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Preparation method of star polycarboxylic acid high-performance water reducing agent
ActiveCN102887979AExtended Dionon Design-Structure-PropertyExpanding the theoretical connotation of the design-structure-performance of moleculesWater reducerPollution
The invention relates to a preparation method of a star polycarboxylic acid high-performance water reducing agent. Polybasic alcohol and (methyl) acrylic acid used as main raw materials for esterification are esterified and polymerized to prepare the star polycarboxylic acid high-performance water reducing agent material: the (methyl) acrylic acid and polybasic alcohol used as reactants are esterified under the action of a catalyst to firstly prepare a star polymerizable active terminal, and free-radical polymerization reaction is carried out with unsaturated polyethenoxy ether, molecular weight regulator and unsaturated carboxylic acid monomer under the action of an initiator to prepare the star polycarboxylic acid high-performance water reducing agent. The invention is easy to control, and has the advantages of high polymerization degree, low cost and no pollution; the esterification reaction is carried out form an active core, and the free-radical polymerization is carried out to generate the chain arm, thereby implementing the polycarboxylic acid high-performance water reducing agent in a star molecular structure; and under the condition of common doping amount and low doping amount, the star polycarboxylic acid high-performance water reducing agent has better cement paste flowability and holding capacity than the traditional linear and comb polycarboxylic acid water reducing agents, and has favorable cement adaptability and concrete application performance.
Owner:GUIZHOU DR SHI TECH
Synthesis method of polycarboxylic acid high-performance water reducing agent of star-like structure
ActiveCN102911322AExtended Dionon Design-Structure-PropertyExpanding the theoretical connotation of the design-structure-performance of moleculesSynthesis methodsPolyethylene glycol
The invention discloses a synthesis method of a polycarboxylic acid high-performance water reducing agent of a star-like structure, belonging to the field of a water reducing agent. According to the synthesis method, polybasic alcohol, (methyl) acrylic acid, a polyethylene glycol compound and the like are used as esterification raw materials, and the polycarboxylic acid high-performance water reducing agent of the star-like structure is prepared through a sequential esterification and polymerization method, i.e., the (methyl) acrylic acid and the polybasic alcohol are used as reactants, a star-like polymerizable active end is prepared through esterification reaction under the action of a catalyst, and then the polycarboxylic acid high-performance water reducing agent is prepared from the star-like polymerizable active end and esterification macromolecule, a molecular weight regulator and an unsaturated carboxylic acid monomer under the action of an initiator through free radical polymerization reaction. The synthesis method has the advantages of simplicity, easiness in control, high polymerization degree, low cost, no pollution, capability of realizing the polycarboxylic acid high-performance water reducing agent of the star-like structure connected with a plurality of polycarboxylic acid molecules, and more superior cement paste fluidity and holding capacity, good cement adaptability and concrete application performance compared with the conventional linear and comb-shaped polycarboxylic acid water reducing agent in the case of normal and low added amount.
Owner:GUIZHOU DR SHI TECH
Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent
ActiveCN103012694AReduce shipping costsMarket competitiveness and application prospects are goodSolventControllability
The invention discloses a preparation method of a polyester type pure solid polycarboxylic acid high-performance water reducing agent, belonging to the field of water reducing agents. According to the invention, by taking a (methyl) acrylic acid monomer and a polyethylene glycol compound as reactants, a polymerizable macromonomer is prepared through esterification reaction under the effect of a catalyst, and the polymerizable macromonomer conducts a free radical bulk polymerization reaction with an unsaturated carboxylic acid monomer and a chain transfer agent under the effect of an initiator in an environment without any solvent to obtain the polyester type pure solid polycarboxylic acid high-performance water reducing agent. The method disclosed by the invention has strong process controllability, high degree of polymerization and low cost and prevents environmental pollution; a completely anhydrous polyester type pure solid polycarboxylic acid high-performance water reducing agent is prepared through esterification reaction and bulk polymerization, which has neat cement paste liquidity and holding ability, cement adaptability and concrete application performance similar to a traditional solution method; meanwhile, since the polymer product is an anhydrous pure solid, a solution with any concentration can be prepared according to actual needs; and without the after-treatment processes such as heating and drying, solvent separation and the like, the transportation is more convenient, and good market competitiveness and application prospects are realized.
Owner:BEIJING UNIV OF TECH
Reduced-type polycarboxylic acid water reducer and preparation method thereof
The invention relates to a reduced-type polycarboxylic acid water reducer and a preparation method thereof. An esterification method is employed for synthesizing a reduced monomer having a low surfacetension, and the reduced polycarboxylic acid water reducer is prepared through polymerization; acid anhydride or unsaturated carboxylic acid and ethers molecules are subjected to an esterification reaction to prepare the reduced monomer under effect of a catalyst, and then the reduced monomer, nonsaturated polyoxyethylene ether, unsaturated carboxylic acid or a mixture of unsaturated carboxylic acid or its acid anhydride, and a molecular weight conditioning agent are subjected to a free radical copolymerization reaction under effect of an initiator. The method has the advantages of easy control, high yield, low cost, environmental protection, and no pollution. During a polymerization process, a reduced group is introduced, so that the water reducer has low surface tension, an anchoring group is introduced, has good cement slurry-cleaning fluidity under common doping, reduces the surface tension force of a cement aperture solution, and reduces evaporation rate of the solution so as toeffectively reduce the mortar contraction. The obtained water reducer presents good water-reducing and reduction characteristic.
Owner:BEIJING UNIV OF TECH
A method for directly synthesizing pure solid polycarboxylate high-performance water reducer in one step
The invention relates to a method for directly synthesizing a pure solid high-performance polycarboxylate water-reducer in one step, belonging to the field of water-reducers. According to the method, the pure solid high-performance polycarboxylate water-reducer is prepared by taking an acrylic compound and unsaturated polyoxyethylene ether as polymerization reaction monomers, adding a molecular weight regulator and carrying out free-radical polymerization reaction under the action of an initiator and under a solvent-free environment. The method disclosed by the invention is strong in controllability, high in polymerization degree, low in cost, environment-friendly and pollution-free, achieves the purpose of preparing the absolutely anhydrous pure solid polycarboxylate water-reducer by bulk polymerization, not only has the fluidity and holding property of cement paste, cement adaptability and concrete application performance which are similar to those of a polycarboxylate water-reducer prepared from a common solution by polymerization and can be prepared into any concentration of solution according to actual demands as the pure solid high-performance polycarboxylate water-reducer prepared by direct polymerization is an anhydrous pure solid, but also is free of postprocessing working procedures, such as heat drying or solvent separation and is more convenient to transport, saved in transport cost and favorable in market competitiveness and application prospect.
Owner:HUIZHOU JIANKE IND
Preparation method for synthesizing high-performance polycarboxylic acid water reducing agent by undergoing one-step amidation reaction
InactiveCN102181062AApplicable to a wide molecular weight rangeReduce manufacturing costCarboxylic acidMethyl group
The invention relates to a preparation method for synthesizing a high-performance polycarboxylic acid water reducing agent by undergoing a one-step amidation reaction, belonging to the field of water reducing agents. In the invention, a high-performance polycarboxylic acid water reducing agent material is prepared by directly reacting with a one-step amidation method, i.e., the water reducing agent is obtained by undergoing an amidation reaction on reactants which are respectively polymethacrylic acid and methoxyl polyethenoxy ether containing amino at the other end under the action of a catalyst. The method has the advantages of conveniently-controlled process, easiness, practicability, low cost and environmental friendliness. An amide structure and a polyethenoxy ether structure are introduced into the molecular structure of the polycarboxylic acid water reducing agent by undergoing a one-step amidation reaction, so that high flow property of cement is realized, the flow property keeping ability and the cement adaptability are remarkably enhanced, and high flowability can be achieved under the conditions of low cement water factor and low mix proportion.
Owner:BEIJING UNIV OF TECH
Preparation method of star polycarboxylic acid high-performance water reducing agent
ActiveCN102887979BExtended Dionon Design-Structure-PropertyExpanding the theoretical connotation of the design-structure-performance of moleculesSuperplasticizerCarboxylic acid
This invention relates to a method for preparing a star-shaped polycarboxylate superplasticizer by the first esterification step with polyol and (meth)acrylic acid as main reactants and the second polymerization step. In the first step, the star-shaped polymerizable active ends were synthesized by esterification between polyol and (meth)acrylic acid in the presence of catalyst. In the second step, the final star-shaped polycarboxylate superplasticizer was prepared by radical polymerization among the product obtained in first step, unsaturated polyoxyethylene ethers, molecular weight regulator and unsaturated carboxylic acid in the presence of initiator. The production process of this invention exhibits some characteristics including simple, easily controllable, high polymerization degree, low cost and pollution free. The star-shaped molecular structure of polycarboxylate superplasticizer can be achieved through synthesizing active “core” by esterification and “arm” by radical polymerization. It showed better cement paste fluidity and fluidity retention, which manifested as better adaptability to cement and application performance in concrete, than both traditional linear and comb-shaped polycarboxylate superplasticizer at common or lower dosage.
Owner:GUIZHOU DR SHI TECH
Synthesis method of polycarboxylic acid high-performance water reducing agent of star-like structure
ActiveCN102911322BExtended Dionon Design-Structure-PropertyExpanding the theoretical connotation of the design-structure-performance of moleculesSynthesis methodsPolyethylene glycol
The invention discloses a synthesis method of a polycarboxylic acid high-performance water reducing agent of a star-like structure, belonging to the field of a water reducing agent. According to the synthesis method, polybasic alcohol, (methyl) acrylic acid, a polyethylene glycol compound and the like are used as esterification raw materials, and the polycarboxylic acid high-performance water reducing agent of the star-like structure is prepared through a sequential esterification and polymerization method, i.e., the (methyl) acrylic acid and the polybasic alcohol are used as reactants, a star-like polymerizable active end is prepared through esterification reaction under the action of a catalyst, and then the polycarboxylic acid high-performance water reducing agent is prepared from the star-like polymerizable active end and esterification macromolecule, a molecular weight regulator and an unsaturated carboxylic acid monomer under the action of an initiator through free radical polymerization reaction. The synthesis method has the advantages of simplicity, easiness in control, high polymerization degree, low cost, no pollution, capability of realizing the polycarboxylic acid high-performance water reducing agent of the star-like structure connected with a plurality of polycarboxylic acid molecules, and more superior cement paste fluidity and holding capacity, good cement adaptability and concrete application performance compared with the conventional linear and comb-shaped polycarboxylic acid water reducing agent in the case of normal and low added amount.
Owner:GUIZHOU DR SHI TECH
Method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization
The invention relates to a method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a temperature-responsive monomer, unsaturated halogenated hydrocarbon, a small carboxylic acid momonomer and the like as raw materials, a polycarboxylate material is prepared through self-polymerization first, then substitution and then copolymerization; namely, with the temperature-responsive monomer as a reactant, a terminal group-functionalized temperature-responsive polymer chain is produced through the self-polymerization under the actions of an initiator and a terminal group functionalizing agent, then a substitution reaction is performed on the terminal group-functionalized temperature-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a temperature-responsive macromonomer, and finally a copolymerization reaction is performed on the temperature-responsive macromonomer and thesmall carboxylic acid momonomer under the action of the initiator to obtain a comb-structure polymer which uses polycarboxylic acid as a main chain and has a side chain with a temperature-responsive function. By the method, the process is simple, convenient and fast, the molecular weight of a product is controllable, graft polymerization of the temperature-responsive functional macromonomer on polycarboxylic acid is successfully achieved by a terminal group functionalization method, the effects of inhibiting shrinkage and resisting cracking of cement mortar are excellent, and the scientific research value and economic and social benefits are very good.
Owner:BEIJING UNIV OF TECH
Preparation method for cationic side chain esterified-grafted highly-mud-resistant cement dispersing agent
ActiveCN106117564AExpanding the theoretical connotation of the design-structure-performance of moleculesBroaden research ideasPolymer sciencePolyethylene glycol
The invention discloses a preparation method for a cationic side chain esterified-grafted highly-mud-resistant cement dispersing agent, and belongs to the field of dispersing agents. The preparation method comprises the following steps: performing free radical polymerization on an unsaturated carboxylic acid monomer serving as a reactant to obtain a polycarboxylic acid main chain under the action of an initiator and a chain transfer agent, performing free radical polymerization on an unsaturated cationic quaternary ammonium salt monomer serving as a reactant to obtain a hydroxyl-terminated cationic side chain under an oxidization-reduction initiation system formed by high-valence ceric salt and alcohol, and performing esterification-grafting reaction on the polycarboxylic acid main chain, the hydroxyl-terminated cationic side chain and a polyethylene glycol compound in the presence of a catalyst. According to the preparation method, a process is simple and easy to control, and the preparation method is low in cost, energy-saving, efficient, environment-friendly and free of pollution; a composite side chain structure is modified and synthesized by a molecular structure design, so that side chain steric hindrance effects are successfully achieved, cationic charge arrangement is successfully implemented, water reduction and slump retaining characteristics and clay side effect suppression capabilities higher than those of an ordinary polycarboxylic acid water reducing agent are achieved, and the dispersing agent has broad market prospect and great popularization and application potential.
Owner:BEIJING UNIV OF TECH
Method for preparation of high mud resistant polycarboxylic acid dispersant by unsaturated halogenated hydrocarbon copolymerization and grafting with cationic side chain
ActiveCN106188557AThe polymerization process is mild and stableLess side effectsAlcoholPolyethylene glycol
Belonging to the field of dispersants, the invention provides a method for preparation of high mud resistant polycarboxylic acid dispersant by unsaturated halogenated hydrocarbon copolymerization and grafting with a cationic side chain. The method consists of: employing an unsaturated carboxylic acid monomer, an unsaturated halogenated hydrocarbon monomer, an unsaturated cationic quaternary ammonium salt monomer, a polyethylene glycol compound and the like as the raw materials, firstly conducting main chain copolymerization, then polymerizing the cationic side chain, performing functionalization, and finally carrying out etherification grafting so as to synthesize the excellent performance high mud resistant polycarboxylic acid dispersant material with unsaturated halogenated hydrocarbon copolymerized and grafted with cationic side chain, i.e. taking unsaturated carboxylic acid and unsaturated halogenated hydrocarbon as the reactants, conducting free radical polymerization to obtain a carboxylic acid-halogenated hydrocarbon copolymer main chain, using high valence cerium salt-alcohol to initiate polymerization of an unsaturated cationic quaternary ammonium salt monomer so as to obtain a hydroxyl terminated cationic side chain, then modifying the hydroxyl terminated cationic side chain and the polyethylene glycol compound to obtain a functionalized side chain, and carrying out etherification grafting of the functionalized side chain on the carboxylic acid-halogenated hydrocarbon copolymer main chain. The method provided by the invention realizes high water reduction, slump loss resistance, high clay resistance and other multiple effects.
Owner:BEIJING UNIV OF TECH
Preparation method for synthesizing high-performance polycarboxylic acid water reducing agent by undergoing one-step amidation reaction
InactiveCN102181062BApplicable to a wide molecular weight rangeReduce manufacturing costCarboxylic acidMethyl group
The invention relates to a preparation method for synthesizing a high-performance polycarboxylic acid water reducing agent by undergoing a one-step amidation reaction, belonging to the field of water reducing agents. In the invention, a high-performance polycarboxylic acid water reducing agent material is prepared by directly reacting with a one-step amidation method, i.e., the water reducing agent is obtained by undergoing an amidation reaction on reactants which are respectively polymethacrylic acid and methoxyl polyethenoxy ether containing amino at the other end under the action of a catalyst. The method has the advantages of conveniently-controlled process, easiness, practicability, low cost and environmental friendliness. An amide structure and a polyethenoxy ether structure are introduced into the molecular structure of the polycarboxylic acid water reducing agent by undergoing a one-step amidation reaction, so that high flow property of cement is realized, the flow property keeping ability and the cement adaptability are remarkably enhanced, and high flowability can be achieved under the conditions of low cement water factor and low mix proportion.
Owner:BEIJING UNIV OF TECH
Polycarboxylate high-efficiency water reducer and preparation method thereof
The invention discloses a polycarboxylate high-efficiency water reducer and a preparation method thereof. The preparation method comprises the following steps of at normal temperature, dropwise adding components B, C into a component A, cooling to room temperature after dropwise adding the components, and adjusting the pH value to obtain the polycarboxylate high-efficiency water reducer, wherein the component A is obtained by mixing and stirring polyoxyethylene ether, polyethylene glycol and water and then adding a tin or acid catalyst and hydrogen peroxide; the component B is obtained by mixing acrylic acid, a reducing agent and water; and the component C is obtained by mixing sodium methallyl sulfonate, an initiator and water. The water reducer disclosed by the invention is of a multi-arm branch structure with sufficient arm lengths, so that a steric-hinerance effect can be sufficiently developed, the water reduction performance is high, and the working performance of concrete is improved; and the method disclosed by the invention is mild in reaction condition, simple in technology, few in side reactions, safe, environmentally-friendly, low in energy consumption and low in production cost.
Owner:HUNAN UNIV
Method for preparing slump-retaining polycarboxylate water reducer by silylation of amino polyether end groups
The invention relates to a method for preparing a slump loss-resistant type polycarboxylic acid water reducer by silanizing a terminal group of amino polyether. The method provided by the invention takes an amino polyether type compound, a silane coupling agent, an unsaturated carboxylic acid type monomer and the like as main reaction raw materials and a polycarboxylic acid water reducer is prepared through firstly hydrolyzing, substituting, then carrying out condensation, and finally copolymerizing; the method comprises the following steps: firstly hydrolyzing by a halogenated silane coupling agent; then taking the silane coupling agent and the amino polyether type compound to be subjected to substitution reaction; carrying out the condensation on a substituted product and a vinyl silane coupling agent hydrolyzed product; taking a condensed product and unsaturated polyoxyethylene ether, a molecular weight regulator and the unsaturated carboxylic acid type monomer to be subjected to free-radical copolymerization reaction under the action of an initiator to prepare the polycarboxylic acid water reducer with a plurality of branched silane modified polyether side chains. The method provided by the invention has the advantages of simple and easy-to-control process, low cost, energy saving and high efficiency, environmental protection and no pollution; dual modification of the side chains of a main chain of a polycarboxylic acid molecule is successfully realized and more excellent water reduction and slump loss resistance performance, which is better than that of a common polycarboxylic acid water reducer, is represented.
Owner:中铁一局集团工业贸易有限公司
Method for preparing slump-retaining polycarboxylate water reducer by modifying polyether with silane coupling agent
The invention relates to a method using silane coupling agent modified polyether to prepare slump-loss-resistant polycarboxylate superplasticizer. The polycarboxylate superplasticizer is prepared by using a silane coupling agent, a polyether compound, an unsaturated carboxylic acid monomer and the like as the main reaction raw materials and sequentially performing hydrolysis, Williamson etherification, condensation and polymerization. The method specifically includes: hydrolyzing the halogenated silane coupling agent, allowing the hydrolyzed halogenated silane coupling agent to have Williamson etherification reaction with the polyether compound, allowing the etherification product to have condensation reaction with alkenyl silane coupling agent hydrolysate, and allowing the condensation product to have free radical polymerization reaction with unsaturated polyoxyethylene ether, a molecular weight regulator and the unsaturated carboxylic acid monomer under the effect of an initiator to prepare the polycarboxylate superplasticizer with multiple branched silane coupling agent modified polyether side chains. The method has the advantages that the method is simple and easy to control, high in polymerization degree, low in cost, energy-saving, efficient, environmentally friendly and free of pollution, a high steric-hindrance effect is achieved successfully, and the slump loss resistance of the prepared polycarboxylate superplasticizer is better than that of common polycarboxylate superplasticizer.
Owner:BEIJING UNIV OF TECH
Preparation method of high mud-resistant concrete water reducer with graft copolymerized cationic side chains
ActiveCN106117468BAchieving a Transformation in Application PerformanceExpanding the theoretical connotation of the design-structure-performance of moleculesSide chainPolyethylene glycol
The invention discloses a preparation method of a highly mud resistant water reducing agent with graft copolymerization of a cation side chain for concrete, belonging to the field of water reducing agents. The highly mud resistant water reducing agent material with graft copolymerization of a cation side chain for concrete is synthesized by a method of carrying out cation side chain polymerization reesterification first and then graft copolymerization, i.e. an unsaturated cation quaternary ammonium salt monomer as a reactant carries out free radical polymerization in an oxidation-reduction initiation system composed of high-valence cerium salt and alcohols to obtain a terminal hydroxyl cation side chain, then unsaturated carboxylic acid, the terminal hydroxyl cation side chain and methoxy polyethylene glycol carry out esterification under the effect of a catalyst to produce two macromonomers, and then an unsaturated carboxylic acid monomer, a cation side chain macromonomer and a polyether side chain macromonomer as reactants carry out free radical graft copolymerization under the effects of an initiator and a chain transfer agent to obtain the highly mud resistant water reducing agent with graft copolymerization of the cation side chain for concrete. The process of the preparation method has the advantages of simple steps, high efficiency, immediacy, convenience in regulation and control, energy saving and environment protection, a composite side chain structure is synthesized creatively, and the effects of water reducing, slump loss resistance and inhibition in clay side effects are realized.
Owner:中铁一局集团工业贸易有限公司
Preparation method of polyester type pure solid polycarboxylate high-performance water reducer
ActiveCN103012694BReduce shipping costsPrevent the problem of incomplete water concentrationPolyesterPolyethylene glycol
The invention discloses a preparation method of a polyester type pure solid polycarboxylic acid high-performance water reducing agent, belonging to the field of water reducing agents. According to the invention, by taking a (methyl) acrylic acid monomer and a polyethylene glycol compound as reactants, a polymerizable macromonomer is prepared through esterification reaction under the effect of a catalyst, and the polymerizable macromonomer conducts a free radical bulk polymerization reaction with an unsaturated carboxylic acid monomer and a chain transfer agent under the effect of an initiator in an environment without any solvent to obtain the polyester type pure solid polycarboxylic acid high-performance water reducing agent. The method disclosed by the invention has strong process controllability, high degree of polymerization and low cost and prevents environmental pollution; a completely anhydrous polyester type pure solid polycarboxylic acid high-performance water reducing agent is prepared through esterification reaction and bulk polymerization, which has neat cement paste liquidity and holding ability, cement adaptability and concrete application performance similar to a traditional solution method; meanwhile, since the polymer product is an anhydrous pure solid, a solution with any concentration can be prepared according to actual needs; and without the after-treatment processes such as heating and drying, solvent separation and the like, the transportation is more convenient, and good market competitiveness and application prospects are realized.
Owner:GUIZHOU DR SHI TECH
Method for preparing polycarboxylate superplasticizer with main chain modified isocyanate grafted positive ion side chain
The invention relates to a method for preparing a polycarboxylate superplasticizer with a main chain modified isocyanate grafted positive ion side chain and belongs to the field of the superplasticizer. The method comprises the following steps: by taking unsaturated carboxylic acid and unsaturated amide monomer as reactants, acquiring a polycarboxylic acid-amide main chain through free radical polymerization; further modifying the amide group on the main chain as isocyanate group; by taking unsaturated positive ion quaternary ammonium salt monomer as the reactant, performing free radical polymerization under an oxidation-reduction initiating system composed of high-price cerate and alcohol, thereby acquiring an end hydroxy positive ion side chain; performing grafting reaction on polycarboxylic acid main chain containing isocyanate with the end hydroxy positive ion side chain and the polyethylene glycol compound. The method has the advantages of simple and controllable process, low cost, energy-saving effect, high efficiency, polyethylene glycol and no pollution; the main chain modified isocyanate is grafted with the positive ion side chain and the polyether side chain according to a molecular structure design method; the double modification for main chain and side chain of molecule is successfully realized; the water-reducing collapse-protecting property and the capacity of restraining clay side effect are better than those of the common polycarboxylate superplasticizer.
Owner:BEIJING UNIV OF TECH
Method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization
The invention relates to a method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a pH-responsive monomer, unsaturated halogenated hydrocarbon, a small carboxylic acid momonomer and the like as raw materials, a polycarboxylate material is prepared through self-polymerization first, then substitution and then copolymerization; namely, with the pH-responsive monomer as a reactant, a terminal group-functionalized pH-responsive polymer chain is produced through the self-polymerization under the actions of an initiator and a terminal group functionalizing agent, then a substitution reaction is performed on the terminal group-functionalized pH-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a pH-responsive macromonomer, and finally a copolymerization reaction is performed on the pH-responsive macromonomer and the small carboxylic acid momonomer under the action of the initiator to obtain a comb-structure polymer which uses polycarboxylic acid as a main chain and has a side chain with a pH-responsive function. By the method, the process is high-efficiency and energy-saving, the conversion rate of a product is high, the functional modification of the polycarboxylic acid is successfully achieved through introduction of the pH-responsive polymer side chain by a terminal group functionalization method, an excellent characteristic of inhibiting shrinkage of cement mortar is shown, and the market competitiveness and the application prospect are very good.
Owner:BEIJING UNIV OF TECH
Method for preparing macro-monomer synthesized polycarboxylate water reducer through alcoholysis of alkenyl-acyl chloride
ActiveCN106117461AExpand the theoretical connotationThe polymerization process is mild and stableIonEther
A method for preparing a macro-monomer synthesized polycarboxylate water reducer through alcoholysis of alkenyl-acyl chloride belongs to the field of water reducers. The method comprises the following steps: firstly polymerizing a cationic chain, and then reacting with the alkenyl-acyl chloride, thus obtaining a macro-monomer; then carrying out copolymerization on the macro-monomer and a carboxylic acid micro-monomer, i.e., polymerizing under an oxidization-reduction initiating system formed by high-valence cerate and alcohols by taking an unsaturated cationic quaternary ammonium salt monomer as a reactant, thus obtaining a terminal hydroxyl cationic long chain; then respectively enabling the terminal hydroxyl cationic long chain and polyethylene glycol monomothyl ether to react with the alkenyl-acyl chloride respectively, thus preparing macro-monomers with different structures; then carrying out free radical polymerization on the macro-monomers and unsaturated carboxylic acid micro-monomers, thus obtaining the macro-monomer composite polycarboxylate water reducer. According to the method disclosed by the invention, the macro-monomers with different structures and functions are successfully synthesized through ways of polymerizing the cationic chain and respectively reacting with the alkenyl-acyl chloride by combining polyether, and a novel comb-structure polycarboxylate water reducer which takes a polycarboxyl acid as a main chain and the cationic long chain and the polyether as polybasic side chains can be finally obtained. A reaction technology is simple and easy, and multiple excellent effects of retaining slump through reducing water, resisting clay, and the like are realized.
Owner:BEIJING UNIV OF TECH
Method for synthesizing cationic polycarboxylate superplasticizer based on Hoffmann rearrangement reaction
The invention discloses a method for synthesizing a cationic polycarboxylate superplasticizer based on a Hoffmann rearrangement reaction, and belongs to the field of water reducing agents. Unsaturated amide monomers are modified into unsaturated isocyanate, meanwhile, an oxidation-reduction initiating system is formed by high-valence cerate and alcohol to initiate polymeric unsaturated cation quaternary ammonium salt monomers, a hydroxyl-terminated cation side chain is obtained, then isocyanate reacts with the hydroxyl-terminated cation side chain and polyethylene glycol monomethyl ether to obtain cationic macromonomers and polyether macromonomers, then the cationic macromonomers, the polyether macromonomers and small carboxylic acid monomers are subjected to free radical copolymerization, and the cationic polycarboxylate superplasticizer is obtained. Based on the Hoffmann rearrangement reaction principle, unsaturated amide modified amide reacts with the cation side chain and a polyether side chain, the macromonomers with different structures and different functions are designed and synthesized, and the novel pectinated polycarboxylate superplasticizer with polycarboxylic acid as a main chain and cations and polyether as the side chain is obtained finally. The synthesis process is continuous and easy to control, and multiple effects of excellent water reduction, collapse protection, clay resistance and the like are shown.
Owner:中铁一局集团工业贸易有限公司
Method for preparing concrete water reducing agents from polycarboxylic acid modified acyl halide grafted composite side chains
The invention discloses a method for preparing concrete water reducing agents from polycarboxylic acid modified acyl halide grafted composite side chains, and belongs to the field of water reducing agents. By the aid of the method for polymerizing main chains, modifying acyl halide, polymerizing cationic side chains and then carrying out grafting reaction, polycarboxylic acid modified acyl halide grafted composite side chain type concrete reducing agent materials which are excellent in performance can be prepared. The method includes carrying out free radical polymerization on unsaturated carboxylic acid monomers to obtain the polycarboxylic acid main chains; modifying carboxylic acid groups on the main chains to obtain acyl halide groups; forming oxidation-reduction initiation systems from high-valence ceric salt and alcohol, initiating polymerization of unsaturated cationic quaternary ammonium salt monomers by the aid of the oxidation-reduction initiation systems to obtain the hydroxyl-terminated cationic side chains; carrying out the grafting reaction on the polycarboxylic acid main chains with the acyl halide groups, the hydroxyl-terminated cationic side chains and polyethylene glycol compounds to obtain the concrete water reducing agents. The method has the advantages that owing to modes for modifying the acyl halide by polycarboxylic acid and grafting the cationic side chains and polyethylene glycol side chains, composite side chain structures can be synthesized, reaction procedures are simple and are easy to control, energy can be saved, the method is high in efficiency, and excellent water reduction slump retaining and high-resistant clay composite effects can be realized.
Owner:BEIJING UNIV OF TECH
Method for preparing concrete water reducer with styrene sulfonate as monomers
The invention discloses a method for preparing a concrete water reducer with styrene sulfonate as monomers, and belongs to the field of water reducers. The method includes the steps that firstly, styrene sulfonate and unsaturated carboxylic acid monomers are subjected to free radical copolymerization to obtain a polycarboxylic acid-styrene sulfonate main chain, and then benzene sulfonate on the main chain is modified into phenylsulfonyl halide groups; then, an oxidation-reduction initiating system is formed by high-valence cerate and alcohol to initiate polymerization of unsaturated cationic quaternary ammonium monomers to obtain a hydroxyl-terminated cationic long chain; then, the polycarboxylic acid main chain containing the phenylsulfonyl halide groups, the hydroxyl-terminated cationic long chain and a polyethylene glycol compound are subjected to sulfonylation to obtain the concrete water reducer. According to the method, based on the molecular structure design principle, by modifying styrene sulfonate into phenylsulfonyl halide and carrying out sulfonylation on grafted cationic side chains and polyethylene glycol side chains, the novel concrete water reducer containing a double-side-chain structure is successfully synthesized; the reaction process is mild, easy to control, capable of saving energy and efficient, and the concrete water reducer shows multiple excellent effects of water reduction for slump loss resistance, clay resistance and the like.
Owner:BEIJING UNIV OF TECH
A kind of polycarboxylate superplasticizer and preparation method thereof
The invention discloses a polycarboxylate high-efficiency water reducer and a preparation method thereof. The preparation method comprises the following steps of at normal temperature, dropwise adding components B, C into a component A, cooling to room temperature after dropwise adding the components, and adjusting the pH value to obtain the polycarboxylate high-efficiency water reducer, wherein the component A is obtained by mixing and stirring polyoxyethylene ether, polyethylene glycol and water and then adding a tin or acid catalyst and hydrogen peroxide; the component B is obtained by mixing acrylic acid, a reducing agent and water; and the component C is obtained by mixing sodium methallyl sulfonate, an initiator and water. The water reducer disclosed by the invention is of a multi-arm branch structure with sufficient arm lengths, so that a steric-hinerance effect can be sufficiently developed, the water reduction performance is high, and the working performance of concrete is improved; and the method disclosed by the invention is mild in reaction condition, simple in technology, few in side reactions, safe, environmentally-friendly, low in energy consumption and low in production cost.
Owner:HUNAN UNIV
Method for preparing polycarboxylate water-reducer by grafting cationic side chain with modified isocyanate of main chain
The invention relates to a method for preparing a polycarboxylate superplasticizer with a main chain modified isocyanate grafted positive ion side chain and belongs to the field of the superplasticizer. The method comprises the following steps: by taking unsaturated carboxylic acid and unsaturated amide monomer as reactants, acquiring a polycarboxylic acid-amide main chain through free radical polymerization; further modifying the amide group on the main chain as isocyanate group; by taking unsaturated positive ion quaternary ammonium salt monomer as the reactant, performing free radical polymerization under an oxidation-reduction initiating system composed of high-price cerate and alcohol, thereby acquiring an end hydroxy positive ion side chain; performing grafting reaction on polycarboxylic acid main chain containing isocyanate with the end hydroxy positive ion side chain and the polyethylene glycol compound. The method has the advantages of simple and controllable process, low cost, energy-saving effect, high efficiency, polyethylene glycol and no pollution; the main chain modified isocyanate is grafted with the positive ion side chain and the polyether side chain according to a molecular structure design method; the double modification for main chain and side chain of molecule is successfully realized; the water-reducing collapse-protecting property and the capacity of restraining clay side effect are better than those of the common polycarboxylate superplasticizer.
Owner:BEIJING UNIV OF TECH
Method for preparing concrete water reducing agent with p-styrene sulfonate as monomer
Owner:BEIJING UNIV OF TECH
Method for Synthesizing Cationic Polycarboxylate Water Reducer Based on Hoffmann Rearrangement Reaction
The invention discloses a method for synthesizing a cationic polycarboxylate superplasticizer based on a Hoffmann rearrangement reaction, and belongs to the field of water reducing agents. Unsaturated amide monomers are modified into unsaturated isocyanate, meanwhile, an oxidation-reduction initiating system is formed by high-valence cerate and alcohol to initiate polymeric unsaturated cation quaternary ammonium salt monomers, a hydroxyl-terminated cation side chain is obtained, then isocyanate reacts with the hydroxyl-terminated cation side chain and polyethylene glycol monomethyl ether to obtain cationic macromonomers and polyether macromonomers, then the cationic macromonomers, the polyether macromonomers and small carboxylic acid monomers are subjected to free radical copolymerization, and the cationic polycarboxylate superplasticizer is obtained. Based on the Hoffmann rearrangement reaction principle, unsaturated amide modified amide reacts with the cation side chain and a polyether side chain, the macromonomers with different structures and different functions are designed and synthesized, and the novel pectinated polycarboxylate superplasticizer with polycarboxylic acid as a main chain and cations and polyether as the side chain is obtained finally. The synthesis process is continuous and easy to control, and multiple effects of excellent water reduction, collapse protection, clay resistance and the like are shown.
Owner:中铁一局集团工业贸易有限公司
Alkenyl acid chloride alcoholysis to prepare the method of macromonomer synthesis polycarboxylate water reducing agent
ActiveCN106117461BAchieving a Transformation in Application PerformanceExtended Dionon Design-Structure-PropertySide chainPolyethylene glycol
A method for preparing a macro-monomer synthesized polycarboxylate water reducer through alcoholysis of alkenyl-acyl chloride belongs to the field of water reducers. The method comprises the following steps: firstly polymerizing a cationic chain, and then reacting with the alkenyl-acyl chloride, thus obtaining a macro-monomer; then carrying out copolymerization on the macro-monomer and a carboxylic acid micro-monomer, i.e., polymerizing under an oxidization-reduction initiating system formed by high-valence cerate and alcohols by taking an unsaturated cationic quaternary ammonium salt monomer as a reactant, thus obtaining a terminal hydroxyl cationic long chain; then respectively enabling the terminal hydroxyl cationic long chain and polyethylene glycol monomothyl ether to react with the alkenyl-acyl chloride respectively, thus preparing macro-monomers with different structures; then carrying out free radical polymerization on the macro-monomers and unsaturated carboxylic acid micro-monomers, thus obtaining the macro-monomer composite polycarboxylate water reducer. According to the method disclosed by the invention, the macro-monomers with different structures and functions are successfully synthesized through ways of polymerizing the cationic chain and respectively reacting with the alkenyl-acyl chloride by combining polyether, and a novel comb-structure polycarboxylate water reducer which takes a polycarboxyl acid as a main chain and the cationic long chain and the polyether as polybasic side chains can be finally obtained. A reaction technology is simple and easy, and multiple excellent effects of retaining slump through reducing water, resisting clay, and the like are realized.
Owner:BEIJING UNIV OF TECH
Method for preparing high mud-resistant polycarboxylic acid dispersant by grafting cationic side chains by copolymerization of unsaturated halogenated hydrocarbons
ActiveCN106188557BThe polymerization process is mild and stableLess side effectsAlcoholPolyethylene glycol
Owner:BEIJING UNIV OF TECH
Method for preparing ph-responsive comb-like structure polycarboxylic acid by end group functionalization
The invention relates to a method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a pH-responsive monomer, unsaturated halogenated hydrocarbon, a small carboxylic acid momonomer and the like as raw materials, a polycarboxylate material is prepared through self-polymerization first, then substitution and then copolymerization; namely, with the pH-responsive monomer as a reactant, a terminal group-functionalized pH-responsive polymer chain is produced through the self-polymerization under the actions of an initiator and a terminal group functionalizing agent, then a substitution reaction is performed on the terminal group-functionalized pH-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a pH-responsive macromonomer, and finally a copolymerization reaction is performed on the pH-responsive macromonomer and the small carboxylic acid momonomer under the action of the initiator to obtain a comb-structure polymer which uses polycarboxylic acid as a main chain and has a side chain with a pH-responsive function. By the method, the process is high-efficiency and energy-saving, the conversion rate of a product is high, the functional modification of the polycarboxylic acid is successfully achieved through introduction of the pH-responsive polymer side chain by a terminal group functionalization method, an excellent characteristic of inhibiting shrinkage of cement mortar is shown, and the market competitiveness and the application prospect are very good.
Owner:BEIJING UNIV OF TECH
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