147 results about "Insertion reaction" patented technology

The invention discloses a strength determination method for reacted blast furnace coke, which comprises the following steps of: (1) placing a coke sample in a reactor; (2) putting the reactor in an electric heating furnace; (3) inserting a temperature thermocouple into the coke in the reactor;(4) putting an electronic balance on a lifting table and connecting the electronic balance and the reactor through a chain; (5) regulating the electric furnace to heat through a temperature controller and introducing nitrogen when the temperature in the center of a material layer reaches 400 DEG C; (6) introducing carbon dioxide gas when the temperature in the center of the material layer reaches 780 DEG C; (7) cutting the nitrogen and introducing prepared mixed gas when the temperature in the centerof the material layer reaches a certain value, maintaining the temperature of the heating furnace, and when the loss ratio of the coke samples reaches the required value continuously introducing the carbon dioxide gas or the mixed gas, introducing the nitrogen and cooling after the carbon dioxide gas or the mixed gas reaches the specified dissolve loss quantity; and (8) stopping introducing the nitrogen and cooling naturally when below 100 DEG C. The invention more truly reflects the actual conditions of the coke in a blast furnace, and the prediction of the thermal properties of the coke is more accurate.

The invention discloses a method for extracting lithium from a lithium-contained solution based on a LiMn2O4 electrode material. The method comprises the steps that LiMn2O4 powder, a conductive additive and a binding agent are mixed, the surface of a current collector is coated with the mixture, a LiMn2O4 electrode is prepared, lithium extraction treatment is carried out under constant voltage to obtain a Li1-xMn2O4 electrode, the LiMn2O4 electrode and the Li1-xMn2O4 electrode are placed into a recycling solution and an extraction solution which are isolated by an anion exchange membrane, a constant voltage reaction is carried out, lithium ions can be selectively inserted and extracted at the same time, the lithium insertion reaction and the lithium extraction reaction are combined to be carried out at the same time, and finally lithium ion enrichment and extraction are achieved. The electrochemical lithium extraction method is efficient, low in consumption and environmentally friendly.

The present invention relates to surface modifying agents for polymeric and / or textile materials, methods of making and / or using a surface modifying agent to modify and functionalize polymeric and / or textile materials, and / or methods of using surface modified or functionalized polymeric and textile materials, and / or products using or incorporating surface modified or functionalized polymeric and textile materials. For example, the surface modifying agent in precursor form can be styrene sulfonyl azide monomer, polymer or copolymer capable of undergoing a chemical reaction in the presence of heat or light to form one or more styrene sulfonated nitrene monomers, polymers or copolymers, which are capable of chemically reacting with the surface of a polymeric or textile material to endow a specific or desired chemical surface functionality to the surface of a polymeric or textile material. Furthermore, the present invention is possibly preferably directed to a surface modifying agent which comprises a styrene sulfonated nitrene monomer, polymer or polymer containing one or more nitrene functional groups, which are capable of chemically reacting via an insertion reaction into one or more carbon-hydrogen bonds on the surface of a polymeric or textile material in order to chemically attach a specific or desired chemical functionality to the surface of a polymeric or textile material.

The invention discloses a method for preparing methoxyphenylacetic acid by natural anethole; the natural anethole is taken as a raw material and generated into the anisicaldehyde by oxidation reaction, then anisic mandelic acid (salt) is generated by the insertion reaction of carbine; finally the methoxyphenylacetic acid is obtained by reduction. The method has the advantages of reproducible raw material, simple operation and high yield, etc.; furthermore, the method can prepare the methoxyphenylacetic acid which can replace the source of petrochemical industry.

The method for covalent linkage of chitosan on surface of base material includes the following steps: bonding nitrine group on the chitosan, casting the triazo-containing chitosan solution on the base material to form chitosan coating layer containing nitrine group, under the irradiation of UV light photolyzing nitrine group into carbene, making carbene ane base material produce insertion reaction to make chitosan chain produce crosslinking reaction so as to make chitosan bond on the surface of base material. The preparation method of triazo-containing chitosan solution includes the following steps: adding chitosan powder, dicyclohexylcarbimide and 4-azidobenzoic acid into organic solvent stirring, filtering, washing with methyl alcohol or dichloromethane, filtering, drying to obtain triazochitosan, then dissolving it in mixed solvent of dilute acetic acid and glycol methyl ether.

The invention relates to the technical field of synthesis of organic compounds and particularly relates to a preparation method of a beta-hydroxyphenyl selenide compound. The preparation method comprises the step of with aryl boronic acid with a structure presented by a formula (I), elemental selenium and an ethylene oxide derivative presented by a formula (II) as the raw materials, and carrying out insertion reaction on elemental selenium in a reaction solvent under the common effect of a copper catalyst, silver salt and alkali, so as to obtain the beta-hydroxyphenyl selenide compound represented by a formula (III), wherein R1 and R2 are respectively independently selected from one of H, a benzene ring, a naphthalene ring, a heterocyclic ring, a substituted benzene ring, linear alkyl, branched chain, halogen, nitryl and a cyano group.

The invention relates to a spiro bisimine and a preparation method and application thereof. Spiro diamine is adopted as raw material to generate spiro bisimine. The spiro skeleton structure in the spiro bisimine has axial chirality, therefore, the class of compound has two optical isomers, namely, right spiro bisimine and left spiro bisimine; and the commensurable mixture of the two optical isomers become racemization spiro bisimine. The complex compound of the spiro bisimine and copper can be taken as a chiral catalyst which is used in asymmetric insertion reaction of carbene to silicon-hydrogen bond, and has very high activity and enantio selectivity (as high as 99.2 percent ee). The chemical formula of the spiro bisimine is as follows: n=0-3; and the values of R<1>, R<2>, R<3>, R<4>, R<5>, R<6>, R<7>, R<8>, R<9> and R<10> are defined as claim of right 1.

The invention discloses a method for preparing (Z)-3'-hydroxy radical -3,4,4',5-tetra- methoxyl diphenyl ethylene by the material of renewable natural plant resource. Naturally sourced 3,4,5-tri-methoxybenzaldehyde (a derivative extracted from Chinese gall) is taken as the raw material; and 3,4,5-tri-methoyl mandelic acid is obtained through a dichlorocarbene insertion reaction and is reduced to obtain 3,4,5-tri-methoyl phenylacetic acid. The compound can have a Perkin reaction with naturally sourced isovanillin to construct a cis-form diphenyl ethylene backbone, and the (Z)-3'-hydroxy radical -3,4,4',5-tetra- methoxyl diphenyl ethylene is obtained after a decarboxylic reaction. The method adopts the renewable resource-isovanillin and the 3,4,5-tri-methoxybenzaldehyde rich in China to replace increasingly exhausted petrochemical materials, thereby having a good sustainable development capability and remarkable economic, environmental and ecological benefits.

The invention discloses a preparation method for (Z)-3'-hydroxyl-3,4,4',5-tetramethoxyl diphenyl ethylene. A diphenyl ethylene framework structure is built by the Perkin reaction method, and natural aniseed fat-soluble components and propenyl anisole (anethole) are taken as raw materials, and oxidized to obtain anisaldehyde; dichlorocarbene insertion reaction is carried out on the anisaldehyde to obtain p-methoxyl-mandelic acid which is reduced to obtain methoxyl-phenylacetic acid, the methoxyl-phenylacetic acid is brominized to obtain 3-bromo-4-methoxyl-phenylacetic acid. The compound and the natural 3,4,5-trimethoxybenzaldehyde (nutgall extract derivative) carry out Perkin reaction to build a cis-form diphenyl ethylene framework which is further converted and decarboxylated by functional groups to obtain the (Z)-3'-hydroxyl-3,4,4',5-tetramethoxyl diphenyl ethylene. The raw materials of the invention are reproducible natural resources-anethole which are rich in China and 3,4,5-trimethoxybenzaldehyde, and replace non-renewable petrochemical materials which are used by the prior art and become less and less so that the method has the advantages of good sustainable development capability as well as remarkable economic, environmental and ecological benefits.

The invention discloses a preparation method of a mild diazomethane derivative. The preparation method comprises that EWG-substituted benzene sulfonyl chloride and hydrazine hydrate undergo a reaction to produce EWG-substituted benzene sulfonyl chloride, the EWG-substituted benzene sulfonyl chloride and aldehyde or ketone undergo a reaction to produce EWG-substituted benzenesulfonylhydrazone, and the EWG-substituted benzenesulfonylhydrazone, a base and an organic solvent are mixed and undergo a replacement reaction to produce a diazomethane derivative. The diazomethane derivative is not separated and purified and is further used for a tension small ring synthesis reaction and an insertion reaction. The benzene ring of benzenesulfonylhydrazone is introduced with an electron-withdrawing group EWG, and through electron effects and steric hindrance effects, the benzenesulfonyl group on the benzenesulfonylhydrazone is easily separated so that a diazomethane derivative is produced under very mild conditions and especially at the room temperature.

The invention relates to a novel chiral iron complex, in particular to a novel axial chiral iron complex of a nitrogen ligand. The novel chiral iron complex has the following structural formula: wherein m+n is between 2 and 3; m is an integer from 0 to 3; n is an integer from 0 to 3; X and Y are halogens, C1-C8 carboxylate radials, sulfate radicals, perchlorate radicals, 4-(3,5-bi-trifluoromethylphenyl) borate radials, 4-(pentafluoro phenyl) borate radials, 4(perfluoro tert-butoxy ) aluminum ions, 4(hexafluoro isopropoxy) aluminum ions, hexafluoro phosphate radicals, hexafluoro antimonate radials, tetrafluoro borate radials or trifluoro methanesulfonic acid radials; and X and Y are the same or different. The invention also provides a method for preparing the novel chiral iron complex. The novel axial chiral iron complex of the nitrogen ligand can catalyze the insertion reaction of dissymmetrical O-H bonds of alpha-diazotate and show high activity and enantioselectivity.

The invention discloses carbon dioxide based polyurea and a preparation method and application thereof, belongs to the technical field of macromolecular materials, and solves the technical problem in the prior art that the molecular weight of the carbon dioxide based polyurea prepared by the preparation method of the carbon dioxide based polyurea is low, so that the carbon dioxide based polyurea cannot be further applied. The method comprises the following steps: adding a prepolymer or a sliced prepolymer in a reaction device, then continuously blowing carbon dioxide into the reaction device, and completely reacting amino in the prepolymer so as to generate the carbon dioxide based polyurea, wherein the reaction temperature is 120-400 DEG C, the reaction pressure is 0.1-20 MPa, and the reaction time is 0.5-50h. The carbon dioxide which is continuously blown in the method not only can take away a by-product, water, which is not eliminated in the polymerization of the carbon dioxide under a high pressure but also can be inserted into a reaction system, the average molecular weight of the prepared polyurea is between 5000-50000, and the properties are excellent.

The invention relates to a method for synthesizing beta-(3,5-di-tert-butyl-4-hydroxyphenyl)methyl propionate. The technical scheme comprises the following steps of: adding 2,6-di-tert-butyl phenol into a reaction kettle, vacuumizing, displacing hydrogen for more than three times, raising the temperature to be between 55 and 60 DEG C, adding a catalyst, stirring, continuously raising the temperature to be between 90 and 115 DEG C, and dehydrating to obtain slurry; reducing the temperature of the obtained slurry to be between 90 and 97 DEG C, dripping methyl acrylate into the reaction kettle by using an annular dropper which is inserted into the bottom of the reaction kettle, controlling the temperature to be between 95 and 105 DEG C, filling the nitrogen until pressure is between 0.4 and 0.6MPa after dripping is finished, controlling the temperature to be between 95 and 105 DEG C, preserving heat and reacting for 1.5 to 2.5 hours; and reducing the temperature to be between 75 and 85 DEG C, vacuumizing, adding organic acid, reacting for 10 to 20 minutes, filtering, and purifying to obtain a product. By the method, the reaction temperature can be reduced, reaction time is shortened, side reaction is reduced, and the quality and yield of the product are improved.

The invention discloses a method for preparing a novel adsorption material by covalent bonding gelatin on the surface of a non-woven fabric, comprising the following steps of, with a synthetic or nature high polymer non-woven fabric (such as PP (Propene Polymer), PET (Polyester Terephthalate), cellulose and the like) as a substrate, dip-coating the synthetic or nature high polymer non-woven fabric with a polyazide solution to form an activated non-woven fabric substrate, and dip-coating a gelatin solution on the activated non-woven fabric substrate; and utilizing ultraviolet irradiation to photolyze an azide group to form active nitrene, covalently bonding gelatin molecules on the surface of the non-woven fabric through insertion reaction of the active nitrene, and generating partial crosslinking, and finally, removing unbonded or uncrosslinked gelatin by soaking with cold or hot water to prepare the adsorption material. The adsorption material prepared by the method disclosed by the invention has stronger adsorption capacity to tannin, has the balance adsorption capacity of 59.5-134.2mg / g and can reach adsorption balance through about 3h.

The invention relates to light-sensitive nanometer silicon dioxide and a method for preparing the same.The surfaces of the light-sensitive nanometer silicon dioxide contain covalently bonded groups shown as a formula, R1 and R2 in the formula represent independent hydroxyl or ethoxyl or nanometer particle surfaces -O-Si-.The light-sensitive nanometer silicon dioxide and the method have the advantages that the light-sensitive nanometer silicon dioxide contains a benzophenone group which is a photo-initiator, insertion reaction can be carried out on the benzophenone group and C-H bonds under ultraviolet irradiation conditions, accordingly, modified nanometer silicon dioxide and polymer substrates can be combined with one another by chemical bonds, agglomeration among nanometer particles can be prevented, the dispersibility of the nanometer particles in high-polymer matrixes can be improved, and the dispersion stability of the nanometer particles in the high-polymer matrixes can be enhanced; the light-sensitive nanometer silicon dioxide can be used as a filler to be added into high-polymer materials, is excellent in high-polymer matrix compatibility and can be connected with the high-polymer matrixes by covalent bonds after being irradiated by ultraviolet light, and the dispersion stability of the light-sensitive nanometer silicon dioxide in the high-polymer matrixes can be improved.

A thermal cycler includes an attachment unit having an insertion opening for insertion of a reaction container including a channel filled with a reaction solution containing reverse transcriptase enzyme and a liquid having a lower specific gravity than that of the reaction solution and being immiscible with the reaction solution, a first heating unit that heats a first region of the channel, a second heating unit that heats a second region of the channel nearer the insertion opening than the first region, a drive mechanism that switches arrangement of the attachment unit, the first heating unit, and the second heating unit between a first arrangement and a second arrangement, and the control unit performs the first heating unit to be a temperature at which reverse transcription reaction progresses and the second heating unit to be a temperature at which the reverse transcriptase enzyme is not deactivated.

The invention relates to a simple and efficient synthetic method of fexofenadine (chemical name: 4-{1-hydroxyl-4-[4-(hydroxyl benzhydryl)-1-piperidyl]-butyl}-alpha, alpha-dimethyl-phenylacetic acid (I)) and its intermediate. According to the method, isopropyl benzene is used as a raw material. Through a Friedel-Crafts acylation reaction, a halogenation reaction and a carbonyl insertion reaction, a key intermediate 4-(4-chloro-1-butyryl)-alpha, alpha-dimethyl phenylacetic acid (IV) is obtained; the key intermediate reacts with another raw material dibenzyl-(4-pyridyl)-methanol (E) to obtain a key pyridinium intermediate 4-{4-chloro-[4-hydroxydiphenylmethyl]-1-pyridinium]-1-butyryl}-alpha, alpha-dimethyl phenylacetic acid (V); and through catalytic hydrogenation and metallic hydrogen reduction, high-purity fexofenadine is obtained. The synthetic method provided by the invention has advantages of smooth process, simple reaction, short route, convenient post-treatment, high yield and low cost, and is a very ideal preparation method of fexofenadine and industrialization feasible route.

The present invention relates to a polymer-supported rhodium (II) catalyst and its application, which includes addition reaction to carbon-carbon multiple bond in α-diazocarbonyl compounds, insertion reaction to C—H and X—H (X═N, O, S, Se, Si and the like) bonds, or rearrangement and additional cyclization reaction thereofA novel insoluble polymer-supported rhodium (II) complex was prepared through a ligand exchange reaction between an insoluble polymer and a rhodium (II) carboxylato complex, wherein the insoluble polymer was prepared by a copolymerization reaction of (i) a styrene derivative with substituted carboxylic acid, (ii) a stylene, and (iii) a linear alkane with both ends substituted by vinylbenzyloxy groups,Namely, a polymer-supported metal complex catalyst having the following chemical formula 1:wherein M1 and M2 are rhodium, and the like; and X is an oxygen atom, etc; and R4 is an alkyl group, and the like; and k is 1 to 15%, m is 1 to 5% relative to k+l+m, and l is the remainder; and n is 4 and others; and R1 is alkyl-2-(4′-alkyloxy phthalimido methyl), etc, R2 is phenyl, etc; R3 is 4,4′-(1,3-propyrene-1,3-dioxymethyl)phenyl, etc.

Methods and devices for directly measuring the degree of saturation or degree of deactivation of an adsorbent and / or catalytic bed are described herein. The devices contain an inlet, an outlet, a catalytic and / or adsorbent bed, and optionally a support bed for supporting the catalytic and / or adsorbent bed. The devices further contain one or more structures attached to the reactor that allow for insertion of one or more sensors into the reactor. The sensor is used to spectroscopically interrogate the adsorbent and / or catalyst in situ, providing real-time information regarding adsorbant saturation and / or catalyst deactivation. The devices and methods described herein can be used to determine the saturation degree of adsorbent materials or catalyst beds that are involved in gas-liquid and liquid-liquid heterogeneous systems, such as those used in scrubbing and extraction.

Process and a test kit for the detection of drugs of methylenedioxy amphetamine family and derivatives, are disclosed. The process comprises (a) sampling sufficient amount of a material, suspected to be examined comprise of said methylenedioxyphenyl group; (b) admixing said sample with a sufficient amount of a strong acid reagent; and (c) detecting color gradual appearance and determining accordingly the presence of said methylenedioxy amphetamine drugs in predetermined interval of time. The test kit comprises a strong acid reagent; a color vs time chart comprising means for the detection of a specific drug by means of color and time of appearance, a reaction chamber wherein suspected material and said strong acid reagent are admixed and color is indicated; a sampler having means to collect sufficient amount of suspected material to be tested and to insert it to the reaction chamber.

The invention discloses application of a surface-modified sludge carbon catalyst to a carbenoid insertion N-H reaction. An alpha-(phenylamino)methyl ester phenylacetate derivative is generated in onestep from alpha-diazo ester and an amine compound taken as starting raw materials in the presence of a sludge carbon catalyst treated with perchloric acid under a heating condition through formation of metal carbenoid and an N-H insertion reaction. In the method, natural sludge carbon is adopted, and other extra transition metals do not need to loaded, so that the method has the advantages of lowcost, environmental friendliness, ready availability of raw materials, easiness and convenience in operation, mild synthetic reaction condition and high atom utilization rate, gram-grade scale reactions can be realized, recycling of waste is finished, and the requirement on environment-friendly chemistry is met.

Disclosed are dirhodium catalyst compositions. One such dirhodium catalyst composition includes a dirhodium catalyst and a solid support. The dirhodium catalyst includes a Rh—Rh moiety and four bridging ligand moieties. The dirhodium catalyst and the solid support are bound together, but they are not covalently bound together via one or more of the bridging ligand moieties. Another such dirhodium catalyst composition includes a dirhodium tetracarboxylate catalyst and a solid support, and the dirhodium tetracarboxylate catalyst and the solid support are bound together. Yet another such dirhodium catalyst composition includes a dirhodium catalyst and a solid support, where the dirhodium catalyst includes a Rh—Rh moiety and where the dirhodium catalyst and the solid support are bound together via at least one of the rhodiums' axial positions. The compositions can be used in a number of reactions, including insertion reactions (e.g., C—H insertions, Si—H insertions, O—H insertions, and N—H insertions), cyclopropanation reactions, annulations (e.g., [3+2] annulations and [3+4] annulations), and ω,ω-diarylalkanoate synthesis. Methods for making the dirhodium catalyst compositions are also disclosed.

The invention discloses a material surface modification method by combination of plasmas and a chemical method, relates to the technical field of material surface treatment, in particular to a method of performing modification treatment on a material surface by cooperatively utilizing the plasmas and the chemical method, and aims to solve the problem that a material subjected to plasma method surface treatment is low in shear strength. The material surface modification method is characterized in that surface activating treatment is performed on the material by the plasmas, and material surface modification is realized by insertion reaction through utilizing carbyne and the groups such as C-H, O-H and N-H which are inherent in the material and are introduced by plasma treatment. A surface-modified carbon fiber interface prepared by the method has higher shear strength than that of a non-modified carbon fiber interface, and the reaction activity and efficiency of a chemical grafting method are improved, so the surface functional modification degree can be improved. The method is suitable for material surface treatment and enhances the performance of the material.

The invention discloses a preparation method of an organic phosphate polypropylene nucleating agent. In the method, only a single reactor is used as a reactor for reaction, and at the same time, the following reactions are carried out continuously in one reactor: bridging reaction to synthesize an intermediate product substituted diaryl phenol, aromatization to synthesize diaryl organic phosphoric acyl chloride, hydrolysis to produce substituted diaryl organic phosphate and final salt formation reaction to synthesize a substituted diaryl organic phosphate nucleating agent. A suction type filtration pipe with a filter screen is inserted into the reactor to reduce pressure in solid-liquid separation of each step so as to extract filtrate out of the reactor for solid-liquid separation. The multiple steps of reaction operations can be avoided, and the defects of the prior art such as multiple devices, large investment, complex reaction, troublesome operation and the like can be overcome. The operation can be simplified, the cost can be reduced, the reaction yield is high, the operation is safe, no combustion is needed, and the environmental protection can be facilitated.

Disclosed is method for increasing the efficiency of a dirhodium catalyst. The method includes providing a dirhodium catalyst, providing an organic ester, and contacting the dirhodium catalyst and the organic ester under conditions effective to increase the efficiency of the dirhodium catalyst. The organic ester is selected such that it is not a substrate for catalysis by the dirhodium catalyst. Dirhodium catalyst compositions which include a dirhodium catalyst and an organic ester are also disclosed. In these compositions, the organic ester is not a substrate for catalysis by the dirhodium catalyst. The method and compositions can be used in a number of reactions, including insertion reactions (e.g., C—H insertions, Si—H insertions, O—H insertions, and N—H insertions) cyclopropanation reactions, annulations (e.g., [3+2] annulations and [3+4] annulations), and ω,ω-diarylalkanoate syntheses.

The invention discloses an asymmetric synthesis method of a gamma-alkenyl substituted butenolide or butenolactam compound. The method adopts cheap nickel to catalyze a [3+2] asymmetric cycloaddition reaction of a cyclopropenone compound and alpha, beta-unsaturated ketone or imine, the selective insertion reaction of intermolecular C=X after nickel-catalyzed C-C bond activation is realized for thefirst time, wherein X is equal to O or N, the gamma-alkenyl substituted butenolide or butenolactam compound is obtained in a high yield, high enantioselectivity and chirality controllable manner, thesynthesis method is novel, condition mildness, substrate with good applicability, simple and efficient reaction, cheap and readily available catalyst, according to the present invention, the synthesisprocess is simple, the atom economy is good, the synthesis product is easy to derivatize, the method can be widely used in completely-synthesized designed synthesis building blocks and new chiral drug derivatives, and the ligand compound is further provided, and can be used for the asymmetric synthesis of gamma-alkenyl substituted butenolide or butenolactam compounds.

The invention relates to a new synthesis method of a dihydrofuran derivative through a Lewis acid catalyzed insertion reaction to high-effectively form a C-C bond and cyclization with an ionic liquidbeing a solvent and sulfur ylide being a nucleophilic reagent. Compared with other methods, the method of the invention employs feasible raw materials and is simple in steps, avoids use of toxic organic solvent, is a gentle, quick, simple, effective and environment-friendly method of preparing a dihydrofuran parent ring. The method has extensive application prospect.