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54 results about "Metacresol" patented technology

Tazobactam synthesis method

The invention relates to a tazobactam synthesis method which comprises the steps of: with 6-APA(Amino Penicillanic Acid) as raw material, preparing a key intermediate 6,6-dihydro penam sulphoxide acid diphenylcarbinol ester through successive reactions of esterification, oxidation, reduetive debromination and the like without separation; then, reacting with 2-triphenyl silicon-1,2,3-triazole; introducing a triazole ring; and finally obtaining the final product of tazobactam through potassium permanganate oxidation and metacresol deprotection. The tazobactam synthesis method is mainly characterized in that a phase transfer catalyst is introduced in the first step, therefore, the reaction rate and the product purity are improved; since an environment-friendly hydrogen peroxide-cobalt acetate catalytic oxidation system is adopted in the third step, the characteristics of good reaction selectivity, high yield, catalyst recyclability and the like are achieved; a method for synthesizing 2 alpha-methyl-2 beta-(1,2,3- triazole-1- radical) methyl penam-3 alpha-carboxylic acid diphenylcarbinol ester by using 2-triphenyl silicon-1,2,3-triazole is adopted in the fifth step, and the tazobactamsynthesis method is simple and convenient to operate, is safe and reliable, shortens the reaction route and improves the total yield. Compared with the traditional process, the tazobactam synthesis method greatly reduces the production cost and the environment pollution and has greater implementation value and economic benefits.
Owner:YIYUAN XINQUAN CHEM

Preparation of glyoxalinyl-containing sulphonation polyimides covalence-ionomer membrane

InactiveCN101407592AExcellent anti-free radical oxidation performanceHigh proton conductivityCell component detailsFuel cell detailsBenzoic acidCross-link
The invention relates to a preparation method of a covalent-ion cross-linked film of sulfonated polyimide containing imidazolyl. The preparation method comprises the following steps: 1, 4, 5, 8-naphthoic tetracarboxylic dianhydride, sulfonated diamine, common non-sulfonated diamine and diamine containing imidazolyl are added into a metacresol medium, the sulfonated polyimide containing imidazolyl is obtained by copolycondensation under the presence of triethylamine and benzoic acid and the protection of nitrogen; a solution casting method and proton exchange are adopted to prepare non-covalent cross-linked sulfonated polyimide film containing imidazolyl which is then processed by methane-sulfonic acid/phosphorus pentoxide solution or phosphoric acid solution or polyphosphoric acid containing phosphorus petoxide so as to prepare the covalent-ion cross-linked film of sulfonated polyimide containing imidazolyl. The covalent-ion cross-linked film obtained by the preparation method has anti-free radical oxidation susceptibility which is far better than the common sulfonated polyimide or non-covalent cross-linked film without containing imidazolyl and has potential application prospect in the fields of fuel cells and the like.
Owner:SHANGHAI JIAO TONG UNIV

Tazobactam synthesis method

ActiveCN102643292ASteps to increase monoxidationBlocking affinityOrganic chemistryMetacresolSynthesis methods
The invention discloses a tazobactam synthesis method, which belongs to the technical field of medicines, and includes the steps: firstly, enabling 6,6-dihydropenam sulfoxide acid diphenylmethyl ester serving as raw materials to undergo thermal cracking and chloromethylation reaction to obtain 2beta-chloromethyl penicillanic acid diphenylmethyl ester; secondly, adding oxidizing agent to oxidize the 2beta-chloromethyl penicillanic acid diphenylmethyl ester-1beta-oxide, enabling the oxidized 2beta-chloromethyl penicillanic acid diphenylmethyl ester-1beta-oxide to react with sodium azide to generate 2beta-hydrazoic methyl penicillanic acid diphenylmethyl ester-1beta- oxide, and then generating 2beta-hydrazoic methyl penicillanic acid diphenylmethyl ester-1,1- dioxide by means of oxidization under the action of potassium permanganate and acetic acid; and finally, preparing the tazobactam by means of deprotection under the action of acetylene cyclization and metacresol. Compared with a past 6-APA (aminopenicillanic acid) route, the tazobactam synthesis method has the advantages that the step of sulfur atom single oxidization is added, so that possibility of ring expansion due to affinity of lone pair electrons on a sulfur atom is blocked, and transformation of five-membered ring products to six-membered ring by-products during hydrazoic reaction can be effectively controlled.
Owner:山东安信制药有限公司 +1

Technology for complexing, crystallizing, separating and purifying metacresol

The invention provides a technology for complexing, crystallizing, separating and purifying metacresol, belonging to the field of separation and purification in a chemical industry. The technology comprises the steps of dissolving urea in mixed phenol: adding the mixed phenol into a reactor, wherein the mixed phenol comprises 10.907wt% of o-cresol, 34.276wt% of p-cresol, 53.176wt% of m-cresol and 1.641% of dimethyl phenol; adding the urea into the reactor, wherein the mole ratio of the urea to the m-cresol is 1.0-1.8; heating and rising the temperature to be 85-105DEG C in a water bath or an oil bath for 40-80min, so that the urea is completely dissolved in the mixed phenol; cooling, adding normal hexane under the temperature of 60DEG C, and crystallizing for 1-2h under the temperature from -10DEG C to -20DEG C; transporting crystallized serous fluid into a filter to separate solid from liquid; recovering filter liquor in a rectifying way, adding water into crystalline solid, and hydrolyzing during heating at 40DEG C to obtain water phase and organic phase; and recovering the water phase, so that the organic phase is the m-cresol. In the technology, methylbenzene is replaced by normal hexane to be taken as a dissolvent for complexing and crystallizing reaction, so that the technology is higher in the yield of the cresol, the usage amount of the dissolvent can be reduced by one third, and the dissolvent can be covered by less energy consumption.
Owner:BEIJING UNIV OF CHEM TECH

Polyphenol mixture recycling purification technology

ActiveCN108558609AReduce pollutionRealize sequential separation and purificationOrganic chemistryOrganic compound preparationMetacresolPhase splitting
The invention provides a polyphenol mixture recycling purification technology which comprises the steps of alkalization and phase splitting: heating a polyphenol mixture to react with a sodium carbonate solution to general phenol sodium salt, conveying reaction liquid into an alkalization and phase splitting tower for continuous reaction to generate the phenol sodium salt and phase splitting and obtaining a water phase rich in the phenol sodium salt and an organic light component, acidification, water washing and phenol extraction: conveying the water phase into an acidification tower for acidification, allowing an organic phase on the upper layer in the acidification tower to overflow into a water washing tower for washing treatment, ethanol crystallization mixing and adding the organic phase after the water washing and ethanol into a crystallizer for crystallization to form 2,3-dimethyl phenol, and rectification and separation: continuously conveying primary mother liquid into a primary rectification tower for rectification till a metacresol finished product with a content greater than 98% is generated continuously in the primary rectification tower, and conveying kettle liquid with a 3,5-dimethyl phenol content greater than 80% from the primary rectifying tower into a secondary rectification tower for continuous rectification and purification to form a product with the 3,5-dimethyl phenol content greater than 98%.
Owner:JIANGSU HUANXIN NEW MATERIAL CO LTD

Method for measuring content of seven harmful phenol in mainstream flue gas by high efficiency liquid chromatography

The invention provides a method for measuring the content of seven harmful phenol in the mainstream flue gas by high efficiency liquid chromatography, comprising the steps of mainstream flue gas collection, flue gas sample preparation and high efficiency liquid chromatography fluorescence detection. Firstly, the fluorescence detection spectrum data output by a high efficiency liquid chromatographyfluorescence detector of different mixed concentration sample is processed with a partial least square method, and a mathematical model is built, and then the fluorescence detection spectrum data ofthe metacresol and the paracresol in high efficiency liquid chromatography fluorescence detection data of the flue gas sample is input into the mathematical model to obtain the concentration of the metacresol and the paracresol. The method can be used for simultaneously analyzing the content of seven harmful phenol compounds in the mainstream flue gas and realizes the measurement of the metacresolcompound and the paracresol compound with a chemometrics method without adopting any other instrument, equipment or reagent, has accurate mausruing result, simple measure process and rapid calculation speed.
Owner:CHINA TOBACCO GUIZHOU IND +1

Synthesis method for 2-methoxy-4-methylbenzylamine

The present invention discloses a synthesis method for 2-methoxy-4-methylbenzylamine. The method comprises the following three steps that: 1, metacresol and formaldehyde are mixed in a solvent A, the resulting solution is subjected to a carbonylation reaction under an alkaline condition through a catalytic action of a Lewis acid catalyst to generate 2-hydroxy-4-methyl-benzaldehyde; 2, the 2-hydroxy-4-methyl-benzaldehyde and a methylating regent are subjected to heating reflux in a solvent B to carry out a methylation reaction to generate 2-methoxy-4-methyl-benzaldehyde; 3, the 2-methoxy-4-methyl-benzaldehyde and ammonium formate are subjected to a reductive amination reaction under a heating condition to generate the 2-methoxy-4-methylbenzylamine. According to the synthesis method provided by the present invention, the used raw materials are mass industrial products, such that the production cost is low; in the third step of the reductive amination reaction, a hazardous reducing agentof lithium aluminum hydride is prevented from using; the reaction conditions are mild, the operation is safe and convenient; the yield of the final product is high, the generated three waste are less, and the method is applicable for the industrial production.
Owner:SHANGHAI INST OF TECH +1

Method for preparing metacresol by directly hydrolyzing meta-aminotoluene

The invention discloses a method for preparing metacresol by directly hydrolyzing meta-aminotoluene. The method comprises the following steps: acid, meta-aminotoluene and water are made into a solution which is put into a reactor; nitrogen is introduced into the reactor; heating and stirring are carried out, so that the hydrolysis reaction is carried out fully; when the reaction is finished, the temperature is cooled to room temperature, the material is extracted by an organic solvent to obtain the metacresol crude product. The hydrolysis of the invention is carried out by one step or multiple steps of continuous reactions, the method is simple and practicable with low cost, the product of primary hydrolysis is removed, a plurality of hydrolyses of the mixture can improve the yield; after metacresol is extracted, the residual mixed liquor is added with reactant which are heated to hydrolysis temperature, and multiple times of hydrolysis reactions are carried out, which is capable of effectively reducing waste water; the reaction processes are shortened, the treatment of waste water is greatly reduced, the conversion rate of the reaction is up to 100%, and the yield is up to above 80%; the invention is a new method for synthesizing metacresol and can remarkably reduce the production cost of metacresol.
Owner:NANJING UNIV OF SCI & TECH

Carbon/carbon composite material preform and preparation method thereof

InactiveCN105859303AMeet the requirements of opennessHigh strengthFiberCarbon composites
The invention relates to a carbon/carbon composite material preform. The carbon/carbon composite material preform comprises 40-70wt% of short carbon fibers, and the balance of a carbon nano-adhesive. The invention provides a preparation method of the preform. The method comprises the following steps: dispersing the short carbon fibers in a polyoxyethylene and hydroxypropyl methyl cellulose ether dispersed aqueous solution; standing the obtained solution, and removing a supernatant; heating and drying the obtained material to obtain a carbon fiber preform; carrying out vacuum impregnation to make a n-propanol solution of phenol-metacresol-furfural-acetyl chloride be impregnated into the carbon fiber preform, heating the obtained carbon fiber preform to carry out in situ polymerization in order to form a phenolic aldehyde-based nano-adhesive, and drying the phenolic aldehyde-based nano-adhesive to volatilize n-propanol in order to obtain a phenolic resin nano-adhesive reinforced carbon fiber preform; and carbonizing the phenolic resin nano-adhesive reinforced carbon fiber preform to obtain the carbon nano-adhesive reinforced short carbon fiber preform. The preparation method has the advantages of no need of expensive long carbon fibers, no need of a complex knitting technology, convenient operation, short period, low cost, excellent performances and easy industrial production.
Owner:SHANGHAI INST OF TECH

Tazobactam synthesis method

ActiveCN102643292BSteps to increase monoxidationBlocking affinityOrganic chemistryMetacresolSynthesis methods
The invention discloses a tazobactam synthesis method, which belongs to the technical field of medicines, and includes the steps: firstly, enabling 6,6-dihydropenam sulfoxide acid diphenylmethyl ester serving as raw materials to undergo thermal cracking and chloromethylation reaction to obtain 2beta-chloromethyl penicillanic acid diphenylmethyl ester; secondly, adding oxidizing agent to oxidize the 2beta-chloromethyl penicillanic acid diphenylmethyl ester-1beta-oxide, enabling the oxidized 2beta-chloromethyl penicillanic acid diphenylmethyl ester-1beta-oxide to react with sodium azide to generate 2beta-hydrazoic methyl penicillanic acid diphenylmethyl ester-1beta- oxide, and then generating 2beta-hydrazoic methyl penicillanic acid diphenylmethyl ester-1,1- dioxide by means of oxidization under the action of potassium permanganate and acetic acid; and finally, preparing the tazobactam by means of deprotection under the action of acetylene cyclization and metacresol. Compared with a past 6-APA (aminopenicillanic acid) route, the tazobactam synthesis method has the advantages that the step of sulfur atom single oxidization is added, so that possibility of ring expansion due to affinity of lone pair electrons on a sulfur atom is blocked, and transformation of five-membered ring products to six-membered ring by-products during hydrazoic reaction can be effectively controlled.
Owner:山东安信制药有限公司 +1

Preparation method of single-component high-ortho-position-content thermosetting phenolic resin used for extrusion

The invention discloses a preparation method of a single-component high-ortho-position-content thermosetting phenolic resin used for extrusion, and belongs to the field of phenolic resin preparation method. The preparation method comprises following steps: complete pyrolysis of paraformaldehyde is carried out so as to obtain a formaldehyde solution; a certain amount of acetic acid is added, phenol and zinc oxide are added to control pH value of an obtained reaction liquid to be 5 to 7, and reaction is carried out for 120 to 180min at 80 to 95 DEG C; other aldehyde raw materials and an alkali catalyst are added for reaction; when the Abbe refractive index of an obtained mixed reaction liquid ranges from 1.460 to 1.470, temperature is reduced to 50 to 70 DEG C quickly, a mixed phenol composed of resorcinol, metacresol, and 3,5-xylenol is added for reaction; vacuum dehydration is carried out, an auxiliary material is delivered into a reaction still, and discharging is carried out after viscosity adjusting so as to obtain a finished product. The single-component high-ortho-position-content thermosetting phenolic resin used for extrusion is friendly to the environment, is low in curing temperature, high in curing speed, long in storage duration, high in product strength, stable in performance, and excellent in comprehensive properties; and no bubble is generated in curing.
Owner:洛阳双瑞橡塑科技有限公司

Tazobactam synthesis method

The invention relates to a tazobactam synthesis method which comprises the steps of: with 6-APA(Amino Penicillanic Acid) as raw material, preparing a key intermediate 6,6-dihydro penam sulphoxide acid diphenylcarbinol ester through successive reactions of esterification, oxidation, reduetive debromination and the like without separation; then, reacting with 2-triphenyl silicon-1,2,3-triazole; introducing a triazole ring; and finally obtaining the final product of tazobactam through potassium permanganate oxidation and metacresol deprotection. The tazobactam synthesis method is mainly characterized in that a phase transfer catalyst is introduced in the first step, therefore, the reaction rate and the product purity are improved; since an environment-friendly hydrogen peroxide-cobalt acetate catalytic oxidation system is adopted in the third step, the characteristics of good reaction selectivity, high yield, catalyst recyclability and the like are achieved; a method for synthesizing 2 alpha-methyl-2 beta-(1,2,3- triazole-1- radical) methyl penam-3 alpha-carboxylic acid diphenylcarbinol ester by using 2-triphenyl silicon-1,2,3-triazole is adopted in the fifth step, and the tazobactamsynthesis method is simple and convenient to operate, is safe and reliable, shortens the reaction route and improves the total yield. Compared with the traditional process, the tazobactam synthesis method greatly reduces the production cost and the environment pollution and has greater implementation value and economic benefits.
Owner:YIYUAN XINQUAN CHEM
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