50results about How to "Facilitate the positive reaction" patented technology

The invention provides a method and device for preparing 6-amino-capronitrile from caprolactam by adopting a liquid phase method. In the method for preparing the 6-amino-capronitrile, the caprolactamis taken as a raw material; the method for preparing the 6-amino-capronitrile comprises the following step: S1: mixing the caprolactam, an organic solvent and a catalyst at a certain mass ratio, so asto obtain a mixed solution, adding the mixed solution into a reaction kettle and stirring and heating the mixed solution; S2: when the mixed solution in step S1 reaches certain temperature, introducing ammonia gas into the mixed solution for a reaction; S3, after the reaction in step S2 is ended, rectifying and purifying a reaction product, so as to obtain pure 6-amino-capronitrile. In the methodfor preparing the 6-amino-capronitrile, the caprolactam is taken as the raw material, the reaction conversion rate is comparatively high, and the preparation process is simple.

The invention relates to a method for preparing polycarbonate catalyzed by ionic liquid. The method is characterized in that heterocyclic nitrogen-containing ionic liquid is used as a catalyst, the amount of the catalyst is 5*10<-3>-5% of the mass of a dihydroxy compound, the dihydroxy compound and bis(trichloromethyl) carbonate are taken as raw materials, a feeding mol ratio of the dihydroxy compound to the bis(trichloromethyl) carbonate is 1:0.8-1:10, and the corresponding polycarbonate is obtained by melt polymerization. A synthesis process of the polycarbonate includes two stages of transesterification and polycondensation. In the transesterification stage, a prepolymer is obtained under conditions of a reaction temperature of 90-180 DEG C, an atmospheric pressure and reaction time of0.05-6 h. In the polycondensation stage, the polycarbonate is obtained by synthesizing prepolymer at 200-270 DEG C, a vacuum degree of 4.0*10<-3> MPa-1.0*10<-5> MPa, and reaction time of 0.05-7 h. Thesynthetic method has the advantages of simple catalyst components and molecular structure that can be designed. Moreover, the catalyst is strong in alkalinity and high in activity. By-products can berecycled, which reduces the cost. The synthetic method does not use highly toxic phosgene, dose not require a solvent, is very little in three wastes generation, and conforms to the concept of cleanproduction.

The invention discloses a production method of 3,5-di-tert-butyl-4-hydroxybenzoic acid. The production method sequentially comprises the steps as follows: 2,6-di-tert-butylphenol, a potassium hydroxide aqueous solution and toluene are added to a reactor under protection of nitrogen to be subjected to a reflux reaction under a water distribution condition; CO2 is introduced into the reactor until the pressure is 0.1-3.0 MPa, a Kolbe-Schmitt reaction is conducted under a pressure holding condition, after the reaction, corresponding aftertreatment is carried out, and a crude product of 3,5-di-tert-butyl-4-hydroxybenzoic acid is obtained. The method has short reaction time and high conversion rate, has obvious advantages as compared with traditional gas-solid processes and existing solvent-process synthesis processes and is suitable for further industrialization.

The invention relates to catalytic rectification packing with radial distribution capacity. The interior of a structure A consists of packing sheets; catalysts are filled in the packing, and the exterior is coated by a screen; a structure B refers to regular packing sheets and can be windowing guide packing, plate ripple packing, screen ripple packing, pore plate ripple packing, rolled pore plate ripple packing, cellular packing and other regular packing. The two structures are alternately and circumferentially distributed in a packing disc. The structure A and the structure B are circumferentially arranged in a staggered mode, so that the number of vapor-liquid multi-phase flow channels are increased, the mass transfer process of vapor-liquid multi-phase flow is facilitated, the phenomena of channeling and short circuit of vapor-liquid multi-phase flow are effectively avoided, small bed pressure drop is realized, a multi-phase flow radial diffusion effect is effectively enhanced, the reaction products are timely separated, and forward reaction is promoted, so that the amount of catalysts can be reduced.

The invention relates to a chlorination method for sucrose-6-ethyl ester. The chlorination method comprises the following steps: (1) respectively preparing a chlorination reagent and a solution of sucrose-6-ethyl ester from a polar non-proton solvent; (2) chlorinating the sucrose-6-ethyl ester solution by a chlorination reagent solution; (3) refluxing under reduced pressure; and (4) evaporating the polar non-proton solvent by distilling, recycling, neutralizing the sucrose-6-ethyl ester solution in a distillation kettle, removing the solvent, adding water to dissolve, discoloring and crystallizing to obtain a sucrose-6-ethyl ester crude product, wherein the recycled a polar non-proton solvent is used for the chlorination reagent solution prepared in the step (1). According to the chlorination method, generated hydrogen chloride and sulfur dioxide are discharged by refluxing under reduced pressure to promote reaction to positively perform, and the final reaction temperature is reduced to 105 DEG C which is lower than the highest holding temperature in the existing chlorination technology by 10 DEG C, so that the defects generated by carbonization in the chlorination process are completely avoided; and the used polar non-proton solvent can be recycled for a next-batch chlorination reaction process, and therefore, the chlorination method is especially suitable for industrial production.

The invention discloses a bimetal cobalt oxide-based oxide as well as a preparation method and application thereof. The general formula of the bimetal cobalt oxide-based oxide is MaCobOn, a is 0-3, bis 0-3, a and b do not include 0, n is determined by the oxidation state of other elements, M is selected from one or more of iron, nickel, manganese, zinc or copper, and the surface of the bimetal cobalt oxide-based oxide has defects. The invention also discloses a preparation method and application of the catalyst. The structure of the precursor is controlled by regulating the optimal metal ionratio of the two transition metals and changing the mixed alcohol solvent in the solvothermal reaction, and finally the MaCobOn with different active site distributions can be obtained. As an oxygen reduction catalyst, the MaCobOn has the advantages of proper defects, high activity and stable performance, and meanwhile, the introduction of M metal greatly improves the electron transfer efficiencyand realizes an efficient oxygen reduction process. The preparation process of MaCobOn is simple, the process operability is high, and MaCobOn has good application prospects in the fields of metal-airbatteries, fuel cells, electrolytic cells, super capacitors and the like.

The invention discloses an efficient joint production method of propylene glycol monomethyl ether and propylene glycol monomethyl ether acetate. Propylene oxide, methanol and methyl acetate are takenas raw materials. The method comprises the steps of (1), the preparation of propylene glycol monomethyl ether raw esters: raw materials of the propylene oxide and the methanol are uniformly mixed andpass through a thermostatic reactor and a heat insulation reactor sequentially to generate the propylene glycol monomethyl ether raw esters under the catalytic condition of a medium and strong alkalisolid catalyst, flowing methyl acetate is adopted as a material for a thermal conductive oil pipe in a heat insulation reactor; (2), the preparation of propylene glycol monomethyl ether acetate: partof the propylene glycol monomethyl ether raw esters prepared in the step 1 and the methyl acetate which is preheated in the thermal conductive oil pipe are transferred to an esterification tower to bemixed, and the propylene glycol monomethyl ether acetate is generated by the interesterification reaction of the propylene glycol monomethyl ether raw esters and the methyl acetate which is preheatedin the thermal conductive oil pipe with the presence of acid positive ion resin. The method has the advantages of simple technology, high conversion efficiency and low energy consumption cost.

The invention discloses application of polyester amide as a heat shrinkage film, and relates to the technical field of high polymer materials. Polymer amide is subjected to tabletting and single-axis stretching. The preparation method of polyester amide comprises the following steps: (1) heating and dissolving 30-200 parts by weight of liquid dicarboxylic acid and 15-95 parts by weight of a diamine compound containing beta hydroxyl, and uniformly stirring to form a reaction solution; (2) adding 0.05-0.5 part by weight of a catalyst, heating to 65-100 DEG C in a nitrogen atmosphere, and reacting for 1-6 hours; (3) heating the reaction solution to 100-180 DEG C, and reacting for 3-18 hours; (4) heating the reaction system to 180-240 DEG C, and reacting for 0.5-4 hours; and (5) cooling the reaction system of the reaction solution to 100-180 DEG C to obtain the polyester amide. The polyester amide heat shrinkage film has the advantages that the polyester amide heat shrinkage film not only can replace a PET heat shrinkage film, but also does not melt even at the high temperature of 300 DEG C.

The invention relates to a method for synthesizing resorcinol by m-hydroxybenzoic acid. A one-step synthesis reaction is used, raw materials of m-hydroxybenzoic acid and a solvent are added in a high-pressure reaction vessel for being dissolved according to a mol ratio being 1-8:10-30, a catalyst is added for catalysis, the catalyst is a mixture of ethyl pyruvate and inulase, and m-hydroxybenzoicacid is obtained through steps of extraction and distillation. The reaction reduces soda acid pollution during a traditional technical production process and reduces the usage of a lot of organic solvents, which belongs to the environment friendly chemical reaction; waste water generated by post-treatment is less, and environment pollution is reduced.

The invention belongs to the technical field of synthesis of organic compounds, and specifically relates to a preparation method of bisphenol A diallyl ether. The preparation method of bisphenol A diallyl ether comprises the following steps: (1) adding bisphenol A and a solvent into a reaction kettle, stirring for dissolving, and adding alkali and a water absorbent; (2) dropwise adding allyl halide at a certain temperature, and reacting for a certain time, thus obtaining a crude product; (3) filtering and desalting the crude product, carrying out vacuum distillation, and removing a low-boilingpoint substance, thus obtaining a finished product. The preparation method of bisphenol A diallyl ether, disclosed by the invention, is capable of effectively controlling the water content in a reaction system, reaction is facilitated to proceed forwards, steps for waste treatment in production are greatly reduced, the production cost is reduced, and the preparation method is suitable for large-scale production.

The invention belongs to the field of underground engineering construction, and particularly relates to a tail gas treatment device for underground engineering construction machinery, which comprises a shell and a gas inlet pipe fixedly communicated with the shell; the gas inlet pipe is communicated with the tail end of a tail gas discharge pipe of the underground engineering construction machinery; a horizontally-arranged sieve plate is fixedly connected to the inner side wall of the shell, a plurality of sieve holes are formed in the sieve plate at equal intervals, the interior of the shell is divided into a material storage cavity and a purification cavity through the sieve plate, an annular material storage box is fixedly connected to the top face of the material storage cavity, and purifying agent particles are contained in the annular material storage box. According to the tail gas purification device, an alkaline solution can absorb acid gas in tail gas to generate an acid-base neutralization reaction, and a good tail gas purification effect is achieved; by arranging the wing plates, a purifying agent can be continuously added into the purification cavity; meanwhile, the alkaline solution is stirred and disturbed, the contact area and probability of harmful tail gas and the alkaline solution are increased, and the purification effect of the tail gas purification device is further improved.

The invention discloses a device for producing propylene glycol monomethyl ether acetate by coupling reactive distillation with pervaporation. The device comprises a pre-reactor, a catalytic reactivedistillation tower, a pervaporation feeding buffer tank, a pervaporation membrane assembly and a product refining tower. The invention also discloses a process for producing propylene glycol monomethyl ether acetate by reactive distillation coupled pervaporation. The method disclosed by the invention is simple, good in effect, strong in operability and remarkable in energy-saving effect, and the propylene glycol monomethyl ether acetate can be applied to large-scale industrial production.

The invention relates to an electrochemical hydrogenation device and method and belongs to the technical field of chemical engineering. The device includes a planar laminated assembly. The planar laminated assembly is formed by laminating a hydrogen dissociation catalytic layer, a cation electrolyte membrane layer, an anion electrolyte membrane layer, a water dissociation catalytic layer and a hydrogenation catalytic layer which are planar layers in order. When the device is utilized to perform hydrogenation, the reaction process is stable and controllable, the reaction yield is high, a reactor is self-humidifying, and water management is easy to perform. The device and the method allow a hydrogenation process to be efficient, rapid and stable, do not need high temperature or high pressure, only consume a small amount of electricity, and can perform a catalytic hydrogenation reaction on organic matters at room temperature under atmospheric pressure. A reaction process is economical andenvironmentally friendly.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesizing method of O,O-dimethyl phosphorodithioate. The synthesizing method of the O,O-dimethyl phosphorodithioate has the advantages that on the basis of existing technical method, a proper catalyst is further screened, added into a methanol solution and dripped into a sulfide mother liquid, so that the content and yield of the target product are further increased; the whole methanol dripping process is performed under the micro-negative pressure condition, so that the step of dripping the methanol to react can be performed at lower temperature of 25 to 35 DEG C, and the reaction product of hydrogen sulfide can escape out at micro-negative pressure of 30 to 50mmHg, so as to effectively accelerate the reaction to perform along the positive direction.

The invention relates to a method for synthesizing ethyl tetrazole-5-carboxylate, which belongs to the field of organic synthesis and comprises the following steps of: (1) heating and refluxing by taking ethyl cyanoformate and sodium azide as raw materials and a mixed solution of methylbenzene and water as a solvent to generate ethyl tetrazole-5-carboxylate sodium salt; (2) heating and distillingthe reflux liquid obtained in the step (1) to remove methylbenzene; (3) neutralizing the distillate obtained in the step (2) with an acidic solution, and conducting separating to obtain a crude product of ethyl tetrazole-5-carboxylate; and (4) recrystallizing the crude product of ethyl tetrazole-5-carboxylate through a mixed solvent of low-carbon hydrocarbon and water, and conducting separating toobtain ethyl tetrazole-5-carboxylate. The synthesis method disclosed by the invention is simple to operate and high in yield, and the purity of the prepared ethyl tetrazole-5-carboxylate is high.

The invention relates to the technical field of lubricating oil preparation, in particular, relates to an organic modification method for improving dispersity of graphite phase carbon nitride in lubricating oil, and solves the problem of low compatibility of modified graphite phase carbon nitride and lubricating oil in the prior art. The organic modification method for improving the dispersity of the graphite phase carbon nitride in the lubricating oil comprises the steps: firstly, mixing a certain amount of long carbon chain organic carboxylic acid, triethylamine, 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC.HCL) and 1-hydroxybenzotriazole (HOBT), and adding the mixture into a certain amount of organic solvent. According to the preparation method, an organic long carbon chain is introduced into the surface of graphite phase carbon nitride by utilizing amidation reaction, so that the problem that the graphite phase carbon nitride is difficult to be compatible with an organic matrix is solved, and the compatibility of the graphite phase carbon nitride with oils and lipids is greatly improved. The organically modified graphite phase carbon nitride can be stably dispersed in base oil for a long time, and can be used as a lubricating additive to be applied to the field of lubrication.

The invention provides a camellia oleosa seed oil soap base material and a preparation method thereof. The soap base material comprises the following components in parts by weight: 30-70 parts of camellia oleosa seed oil, 1-10 parts of a solubilizer, 1-13 parts of alkali, 1-4 parts of an emulsifier, 0.01-1 part of an antioxidant, 0.01-2 parts of a preservative and 10-50 parts of deionized water. The preparation method comprises the following steps of: (1) adding alkali into deionized water to prepare alkali liquor; (2) adding a solubilizer into the camellia oleosa seed oil, uniformly stirring,adding the alkali liquor prepared in the step (1), heating to 30-60 DEG C, and quickly stirring and saponifying for 30-90 minutes while keeping the temperature; (3) adding an antioxidant into the saponification liquid obtained in the step (2), and stirring for 5-10 minutes while keeping the temperature; and (4) adding an emulsifier and a preservative, continuing to stir for 5-15 minutes to obtaina soap base material, then stopping heating and stirring, and cooling. The camellia oleosa seed oil soap base material can react in a low temperature range within a short time, active ingredients incamellia oleosa seed oil are effectively reserved, the pH value of the soap base material is close to that of human skin, and the soap base material can be conveniently added into other systems to prepare different types of washing products.

The invention provides a preparation method of 3-methyl-1, 5-pentanediol, which comprises the following steps of: (1) carrying out a condensation reaction on isobutene and formaldehyde as raw materials under the action of an acid catalyst and an auxiliary agent to generate 3-methylene pentane-1, 5-diol and 3-methyl pentyl-2-ene-1, 5-pentanediol; and (2) carrying out a hydrogenation reaction by taking the 3-methylene pentane-1, 5-diol and the 3-methyl pentyl-2-ene-1, 5-pentanediol as raw materials to obtain 3-methyl-1, 5-pentanediol. A sulfoacid pyridinium salt is used as a catalyst and phosphate is used as an auxiliary agent in the condensation reaction of isobutene and formaldehyde, so that the product yield can be obviously improved. The method has the advantages of short process steps, high yield and low cost, and is suitable for industrial amplification.

The invention relates to catalytic rectification packing with radial distribution capacity. The interior of a structure A consists of packing sheets; catalysts are filled in the packing, and the exterior is coated by a screen; a structure B refers to regular packing sheets and can be windowing guide packing, plate ripple packing, screen ripple packing, pore plate ripple packing, rolled pore plate ripple packing, cellular packing and other regular packing. The two structures are alternately and circumferentially distributed in a packing disc. The structure A and the structure B are circumferentially arranged in a staggered mode, so that the number of vapor-liquid multi-phase flow channels are increased, the mass transfer process of vapor-liquid multi-phase flow is facilitated, the phenomena of channeling and short circuit of vapor-liquid multi-phase flow are effectively avoided, small bed pressure drop is realized, a multi-phase flow radial diffusion effect is effectively enhanced, the reaction products are timely separated, and forward reaction is promoted, so that the amount of catalysts can be reduced.

The invention relates to a synthesis method of cyanoacetamide, and belongs to the technical field of organic synthesis. According to the method, a tubular reactor is used as reaction equipment, malonamide is used as a raw material, and cyanoacetamide is generated under the action of triphosgene. The triphosgene with relatively high reaction activity is used, so that the activation energy of the reaction can be reduced, and the forward proceeding of the reaction is promoted; a pipeline reactor is used as reaction equipment, so that the mass and heat transfer effect of a reaction system can be improved, the reaction time and the retention time of a product in the reaction system are further shortened, and the product purity and yield are effectively improved. The atom utilization rate is high, the by-product ammonium chloride can be sold as a product or used for other reactions, and the recovered solvent and the treated rectification base solution can be used for reactions; and only a small amount of activated carbon waste residues are generated, so that the environment-friendly benefit is high.

The invention relates to a method for treating waste DMF in sucralose production, and the method is characterized by comprising the following steps: (1) feeding waste DMF discharged from the bottom of a deacidification tower into a vacuum rectification tower for vacuum rectification, feeding non-condensable gas extracted from the top of the rectification tower into a methanol rectification tower for rectification again, and feeding methanol recovered by rectification into a reaction rectification tower for reaction; (2) feeding an acidic azeotrope extracted from the lower part of the reduced-pressure rectifying tower into a reactive rectifying tower; controlling the volume ratio of the acidic azeotrope to methanol to be 1: (0.9-1.5), returning reaction liquid at the bottom of the reactive distillation tower to the vacuum distillation tower, and returning a mixture of methanol and methyl acetate distilled from the top of the reactive distillation tower to the methanol distillation tower. The method has the advantages that the generated methyl acetate is removed through reactive distillation, the reaction is promoted to proceed forwards, and the yield is increased; acetic acid contained in the raw materials is used as a catalyst, so that the problem of inactivation does not need to be worried about, and excessive decomposition of DMF is avoided; the prepared methyl acetate is high in purity, the product DMF is high in purity, and the production cost of sucralose is reduced.

The invention relates to analysis method for the chiral purity of 1-naphthylethylamine. The analysis method comprises the following two steps of (1) derivatization and (2) separation and detection. The method is mild in condition, convenient and low in price. According to the analysis method, (D)-camphor sulfonyl chloride is taken as a derivatization reagent to carry out derivatization reaction with 1-NEA, the chiral purity of the D-camphor sulfonyl chloride and the derivative of the 1-NEA is analyzed through the combination of reversed-phase high performance liquid chromatography and an ultraviolet detector, so that the chiral purity of the 1-NEA is analyzed.