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207 results about "Tert-Butanol" patented technology

Tert-Butyl alcohol (TBA), also called tert-butanol or t-butanol, is the simplest tertiary alcohol, with a formula of (CH 3) 3 COH (sometimes represented as t-BuOH).It is one of the four isomers of butanol. tert-Butyl alcohol is a colorless solid, which melts near room temperature and has a camphor-like odor.It is miscible with water, ethanol and diethyl ether

Preparation method of Omarlliptin

The invention relates to Omarlliptin, in particular to a novel method for preparing Istradafylline, and relates to a preparation method of Istradafylline, in particular to a preparation method of Istradafylline. The method comprises the following steps: carrying out coupling reaction on a compound Ia and TMS acetylene to obtain an intermediate Ib; carrying out bromination reaction on the intermediate Ic under the action of NBS (N-bromosuccinimide) to obtain an intermediate Id; carrying out substitution reaction on the intermediate Id and tert-butyl carbamate under the action of potassium tert-butoxide to obtain an intermediate Ie; reacting the intermediate Ie with paraformaldehyde to obtain an intermediate If; carrying out cycloaddition reaction on the intermediate If and the intermediate Ib to obtain a key intermediate Ig; carrying out asymmetric catalytic hydrogenation reduction on the intermediate Ig to obtain an intermediate Ih; and removing a protecting group from the intermediate Ih in a hydrochloric acid and ethyl acetate system to obtain a final product. The method is short in route, simple and convenient to operate, mild in condition, high in reaction yield, environment-friendly and easy for industrial production, and dangerous and highly toxic products are prevented from being used and hazardous chemicals are supervised. # imgabs0 #
Owner:STANDE STANDARD TECH RES (HUBEI) CO LTD

Method and device for preparing tert-butyl alcohol by hydrating isobutene in raffinate C4

The invention provides a method and a device for preparing tert-butyl alcohol by hydrating isobutene in raffinate C4, the raffinate C4 and water are used as raw materials and flow in a hydration reactor in a countercurrent manner, the isobutene in the raffinate C4 and the water react under the action of a catalyst to generate tert-butyl alcohol, the water and the tert-butyl alcohol are extracted from the bottom of the hydration reactor, and the tert-butyl alcohol is obtained. Liquid-phase residual C4 after reaction leaves the reactor from the upper part of the hydration reactor, and gas-phase C4 extracted from the top of the hydration reactor is condensed and gasified or compressed and then returns to the bottom of the reactor to serve as disturbance gas, so that the liquid-liquid-solid three-phase contact area is increased, the reaction rate is increased, and the reaction time is shortened; meanwhile, the generated tert-butyl alcohol product is timely removed from the reaction zone, so that the reaction is carried out in the positive direction, the conversion rate of isobutene is improved, and the method has higher economical efficiency by adopting a lower water-oil ratio and lower operation pressure.
Owner:TIANJIN RUYOU TECH CO LTD

Preparation method of linolenic acid structure ester with synergistic biological activity

The invention discloses a preparation method of linolenic acid structural ester with synergistic biological activity, and relates to the technical field of linolenic acid structural ester preparation.The preparation method comprises the steps that specific lipase is prepared through rhizopus wei, and after an SBA-15 molecular sieve is treated, the lipase is fixed to prepare a composite catalyst; the preparation method comprises the following steps: after hydroxyl protection of quercetin, esterifying quercetin with EPA to obtain quercetin-EPA ester; esterifying glycerol and linolenic acid in the presence of a composite catalyst and microwaves, and purifying to obtain an intermediate product; carrying out microwave catalytic ester exchange on the intermediate product and quercetin-EPA ester in tert-butyl alcohol through a composite catalyst to obtain a crude product; and removing impurities from the crude product by a urea adduction method, and carrying out molecular distillation graded purification, column chromatography, deodorization and filtration to obtain a final product. According to the invention, linolenic acid, quercetin and EPA are combined through molecular design to form a compound structure ester with a multi-target effect, and the linolenic acid, quercetin and EPA achieve functional complementation through a synergistic effect, so that the biological activity of the compound structure ester is enhanced.
Owner:HEZE ZHONGHEJIANYUAN BIOLOGY TECH CO LTD

Double metal cyanide catalyst and preparation method thereof

One form of the present invention provides a double metal cyanide catalyst having excellent catalytic activity and a preparation method thereof. Specifically, the double metal cyanide catalyst according to one form of the present invention is characterized in that it is prepared using a complexing agent comprising tertiary butanol, a linear or cyclic (C2-C12) aliphatic polyol, and a polyalkylene glycol.
Owner:GS CALTEX CORP

4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as synthesis method and application thereof

The invention relates to the technical field of organic synthesis, in particular to 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as a synthesis method and application of the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine. The synthesis method comprises the following steps: (1) synthesizing 2-chloro-3-fluoro-4-iodine-5-methylpyridine from 2-chloro-3-fluoro-5-methylpyridine and an iodine elementary substance to obtain 2-chloro-3-fluoro-4-iodine-5-methylpyridine; (2) synthesizing 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine, the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride, the tripotassium phosphate and the (2-formyl phenyl) boric acid, and further synthesizing the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine and the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride. And (3) synthesizing the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine by using the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde and sodium tert-butoxide. The 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine compound constructed by the invention can be used for detecting the content of pesticide residue glyphosate.
Owner:SHANGHAI LONGSHENG CHEM CO LTD

Preparation method of hydrophobic modified silicon dioxide aerogel with low thermal conductivity

The invention discloses a preparation method of hydrophobic modified silicon dioxide aerogel with low thermal conductivity. The preparation method comprises the following steps: by taking water glass-tetraethoxysilane as a composite silicon source and formamide-ethylene glycol as a retarder, hydrolyzing and mixing, and then adjusting the pH value to trigger sol-gel reaction to form wet gel; after tert-butyl alcohol aging and solvent replacement, hexamethyldisiloxane and hexamethyldisilazane dual modifiers are used for synchronous hydrophobic modification and sodium removal, and the hydrophobic modified low-thermal-conductivity silicon dioxide aerogel with a porous nanostructure is prepared through freeze drying. The method uses the composite silicon source to cooperate with the gel, so that the raw material cost is reduced; a double-modifier synchronous sodium removal process is green and efficient; the obtained aerogel has low thermal conductivity and excellent hydrophobicity, is suitable for the fields of building thermal insulation, industrial thermal insulation, aerospace and the like, and has the advantages of economy and environmental protection.
Owner:FUZHOU UNIV

Catalyst and process for preparing anhydrous tert-butyl alcohol by hydrating isobutene

The invention discloses a catalyst and a process for preparing anhydrous tert-butyl alcohol through isobutene hydration, and belongs to the field of industrial catalysis. The preparation method of the catalyst comprises the following steps: after a polyethylene glycol-polyglycerol-polyethylene glycol triblock polymer, tetraethyl orthosilicate and deionized water are subjected to a first mixing reaction, sodium aluminate and sodium tungstate are added for a second mixing reaction to obtain a mixture, the mixture is sequentially subjected to calcination and HCl treatment to obtain a pretreated catalyst carrier, and the pretreated catalyst carrier is dried to obtain the catalyst. The pretreated catalyst carrier, the modified ionic liquid and N, N-dimethylformamide are subjected to a third mixing reaction, and the catalyst is prepared. In the prepared catalyst, the oleophylic group adsorbs isobutene, the hydrophilic group can interact with water molecules, and the two effects cooperate with each other to form a microenvironment beneficial to reaction on the surface of the catalyst, so that the conversion rate of isobutene and the selectivity of anhydrous tert-butyl alcohol are improved.
Owner:ZIBO KERUN CHEMICAL TECHNOLOGY CO LTD

A catalyst for preparing tert-butyl ethylbenzene and ethylbenzene by alkylating tert-butanol with styrene, and a preparation method and application thereof

This invention discloses a catalyst for the alkylation of tert-butanol with styrene to prepare tert-butylethylbenzene and ethylbenzene, its preparation method, and its application. The catalyst consists of a support and active components loaded on the support. The active components are oxides of rare earth metals and high-valence oxides of transition metals. The support is H-β zeolite. The mass contents of the oxides of rare earth metals and high-valence oxides of transition metals on the support are 3-5% and 2-4%, respectively. This invention makes a breakthrough in the reaction mechanism by loading rare earth metals and transition metals onto a β-molecular sieve and using tert-butanol and styrene as raw materials for alkylation. This avoids the polymerization of styrene (raw material) and the dimerization of isobutylene (intermediate product), reduces the generation of by-products, and makes the catalytic process controllable.
Owner:THE NORTHWEST RES INST OF CHEM IND +1

Anti-fog self-cleaning glass based on cellulose ether coating and preparation method thereof

ActiveCN119059739BGood anti-fog performanceUniform qualityCoatingsEpoxyPolymer science
The present invention relates to an anti-fog self-cleaning glass based on a cellulose ether coating and a preparation method, and belongs to the technical field of glass coatings. The cellulose ether coating comprises, by weight, 100 parts of tetraethyl orthosilicate, 9-12 parts of an active crosslinking agent, 16-24 parts of a modified cellulose ether, 3.2-4.5 parts of nano-silicon dioxide, 0.4-0.5 parts of a leveling agent, and 0.2-0.3 parts of a defoaming agent; the modified cellulose ether uses hydroxypropyl methylcellulose as a raw material, is alkalized by sodium hydroxide, is substituted by an alkyl glycol and trifluoropropylmethyldichlorosilane, and is terminated with an alcohol hydroxyl group, that is, a fluorinated intermediate is obtained, and then the end hydroxyl group of the fluorinated intermediate is opened by epichlorohydrin, and then the ring is closed under the promotion of strongly alkaline potassium tert-butoxide, and epoxy modification is introduced into the end of the fluorinated intermediate, that is, an epoxy modifier is obtained, and the modified cellulose ether is uniformly enriched on the surface during the coating forming process to form a stable protective layer.
Owner:SHANDONG HEAD GRP CO LTD

A method for preparing 9,9-dioctyl-2-fluoreneboric acid

The present invention relates to a method for preparing 9,9-dioctyl-2-fluorene boric acid, industrial 2-bromofluorene, sodium tert-butoxide, n-hexane, 1-bromooctane and activating agent are added to a reaction bottle, reacted at room temperature for 1-3 hours, and then n-hexane, 1-bromooctane and activating agent are extracted in turn by vacuum distillation, and an equal amount of n-hexane solution is added again; the temperature is cooled to 40-80°C, n-butyl lithium is added, and stirred for 0.5-1 hour; trimethyl borate is added again, and stirred for 1-2 hours; after completion of the reaction, the temperature is controlled to be lower than 20-0°C, hydrochloric acid solution is dripped, reacted for 1-4 hours, and then warmed to 0-20°C for reaction for 3-6 hours; liquid separation, organic layer is washed with saturated salt water, and water layer is extracted 3 times with n-hexane; after the organic layers are mixed, the solvent is recovered by vacuum distillation; the filter cake is washed with deionized water to pH=6-7, and the finished product is obtained after drying. The present invention meets the production requirements of economic efficiency and high yield.
Owner:ZHONGWEI NAT ENG RES CTR FOR COKING TECH CO LTD +1

Ruthenium metal complex and preparation method and application thereof

The invention discloses a ruthenium metal complex and a preparation method and application thereof, and belongs to the technical field of organic metal synthesis. The preparation method of the ruthenium metal complex specifically comprises the following steps: (1) under anhydrous and anaerobic conditions, adding ethylene glycol monoethyl ether and RuCl3.H2O into a reaction flask, introducing CO, heating, and reacting; (2) continuously heating, reacting and cooling; and (3) adding 3-chloro-2-methylpropan-1-ene, uniformly mixing, heating, stirring, cooling, adding a potassium tert-butoxide tetrahydrofuran solution, heating until boiling, stirring again, stopping heating, reacting, filtering, cleaning a filter cake with tetrahydrofuran, removing the solvent from the filtrate to obtain a reddish brown oily liquid, and condensing to obtain a Ru (tmm) (CO) 3 product, namely the ruthenium metal complex. The ruthenium metal complex prepared by the method has the advantages of high yield (62.8%), high purity (99.6%), low synthesis cost and simple synthesis steps.
Owner:JIANGSU SHEKOY SEMICONDUCTOR NEW MATERIALS CO LTD

A process for preparing tert-butyl vinyl ether

This application relates to the field of organic synthesis technology, specifically disclosing a process for preparing tert-butyl vinyl ether. The raw materials include solid tert-butanol, acetylene, tetrahydrofuran solvent, and potassium hydroxide catalyst, supplemented with auxiliary materials such as type 3A molecular sieves and activated alumina adsorbents. The preparation method involves: after dehydration and purification of the raw materials, the materials are introduced into a reaction vessel; temperature and pressure are controlled, and the reaction endpoint is monitored using an infrared spectrometer; byproducts are quenched and acetylene is recovered; the process involves multi-stage condensation, water washing to remove impurities, distillation separation, and solvent purification and recycling, with simultaneous integration of waste heat recovery and continuous material feeding. The tert-butyl vinyl ether prepared by this process, as an important fine chemical intermediate, can be used in coatings, adhesives, and polymer material modification, possessing advantages such as high purity and good stability. The preparation method achieves efficient utilization of materials and energy through multi-stage synergistic linkage, combining the advantages of green environmental protection, continuous and stable operation, and high resource utilization.
Owner:JIAOZUO XINJING TECH CO LTD

Production of (meth) acrolein and / or (meth) acrylic acid with reduced amounts of high-boiling byproducts

A reactor for producing (meth) acrolein and / or (meth) acrylic acid from reactants selected from the group consisting of propylene, isobutylene and tertiary butanol. The reactor includes an inlet for the reactant to enter the reactor, an outlet for the reaction product to exit the reactor, and a catalyst bed disposed between the inlet and the outlet. The catalyst bed comprises a mixed oxide catalyst based on molybdenum and bismuth. The catalyst closest to the inlet of the reactor has a molar ratio of bismuth to molybdenum lower than the catalyst closest to the outlet of the reactor has a molar ratio of bismuth to molybdenum.
Owner:ROHM & HAAS CO

Synthesis method of substituted trans-dicyclohexyl alkenyl liquid crystal monomer

The invention discloses a synthetic method of a substituted trans-dicyclohexyl alkenyl liquid crystal monomer, which comprises the following steps: reacting 4, 4 '-dicyclohexyl ketone with chloromethyl ether phosphine salt and potassium tert-butoxide at-10 DEG C to 0 DEG C to form 4, 4'-dicyclohexyl diene methyl ether; reacting with hydroxylamine hydrochloride under the action of a first catalyst to generate 4, 4 '-dicyclohexyl dioxime; under the action of a second catalyst, carrying out unilateral deprotection to generate 4-oxime 4 '-dicyclohexylformaldehyde; the preparation method comprises the following steps: reacting 4-oxime with R1BrPPh3 and potassium tert-butoxide at the temperature of 10 DEG C below zero to 0 DEG C to obtain 4-oxime 4 '-dicyclohexyl alkyl ethylene; reacting with formic acid to generate 4-formaldehyde-4 '-dicyclohexyl alkyl ethylene; the substituted trans-dicyclohexyl alkene liquid crystal monomer is prepared by reacting the substituted dicyclohexyl alkene with R2BrPPh3 and potassium tert-butoxide at the temperature of-10 DEG C to 0 DEG C to obtain a cis-trans mixture and carrying out transposition. The method comprises seven steps of reaction, transposition and purification are not needed in the early stage, transposition crystallization is only needed in the last step, and the total yield can reach 70% or above. The raw materials are cheap, easily available and low in cost.
Owner:ALLCHEMY (TAIXING) CO LTD

Method for improving perfuming quality of megastigmatrienone through alkali regulation and control

The invention discloses a method for improving perfuming quality of megastigmatrienone by alkali regulation, which comprises the following steps of: performing alkali-adding heat treatment on megastigmatrienone, and neutralizing the megastigmatrienone to be neutral by using acid so as to improve the proportion of an isomer D. The alkali is one or more of sodium hydroxide, potassium hydroxide, sodium tert-butoxide and potassium tert-butoxide, preferably sodium hydroxide. According to the method, alkali-adding heat treatment is carried out on the megastigmatrienone, the relative content of isomers A and B of the treated megastigmatrienone is reduced, the content of an isomer D of the treated megastigmatrienone is increased, and the megastigmatrienone is applied to cigarette perfuming and has an obvious perfuming effect. According to the regulation and control method, sodium hydroxide is used as a regulation and control reagent, water is used as a solvent, the regulation and control reagent is cheap and easy to obtain, and acetic acid is added for neutralization removal, so that the problems of various other regulation and control reagents and complex purification are solved. The regulation and control method disclosed by the invention is high in operability and easy to industrially apply. And the regulated isomer is stable in performance during re-storage.
Owner:SICHUAN SANLIAN NEW MATERIAL CO LTD +1

Synthesis method of melam

The invention relates to the technical field of synthesis of carbon nitride flame-retardant materials, and particularly discloses a synthesis method of melam, which comprises the following steps: by taking cyanuric chloride as a raw material, carrying out ammoniation and coupling to obtain a bis-triazine intermediate, and carrying out sealed ammoniation on the bis-triazine intermediate by using ammonia water to obtain melam; the optimal potassium tert-butoxide enables the BDCAT to be obtained at the yield of more than 60% in the second-step reaction, the ammonia water ammoniation process used in the third-step reaction is relatively safe, the synthesis method is simple and efficient, and the harsh requirement of a high-temperature and high-pressure method on equipment is avoided.
Owner:NANJING YUANSHU MEDICAL TECH CO LTD

High-selectivity reduction method for preparing triphenylphosphine from triphenylphosphine sulfide

The invention discloses a high-selectivity reduction method for preparing triphenylphosphine from triphenylphosphine sulfide, and belongs to the technical field of organic synthesis.The method comprises the steps that in the low-oxygen environment with the oxygen content being 5-2000 ppm, triphenylphosphine sulfide, an additive and a metal reducing agent react in methylbenzene at the temperature of 0-250 DEG C; after the reaction is finished, separating and purifying to obtain triphenylphosphine; wherein the additive is ethanol, isopropanol, tertiary butanol, tetrahydrofuran, diphenyl ether, isopropyl ether or diethyl ether, and the metal reducing agent is selected from one or a combination of any more of Li, Na and K. The additive added in the method can overcome the hindering effect of oxygen on the reaction, so that the reaction can be carried out in a low-oxygen environment; and meanwhile, the dosage of a metal reducing agent can be reduced, so that the production cost is reduced.
Owner:ZHEJIANG YANGFAN NEW MATERIALS CO LTD

A bicyclic [2.1.1]hexene compound and its preparation and application

This invention discloses a bicyclic [2.1.1]hexene compound and its preparation and application. The invention uses bicyclic [1.1.0]butanone and phosphate ester as starting materials, and potassium tert-butoxide tetrahydrofuran solution as base. The reaction is carried out under reflux at 80°C to obtain the bicyclic [2.1.1]hexene compound. The prepared compound has certain transpeptidase inhibitory activity and can effectively inhibit the infection and spread of Staphylococcus aureus.
Owner:ZHEJIANG UNIV OF TECH

Intelligent control system and intelligent control method for catalytic-free tert-butane production

This invention provides an intelligent control system and method for the production of tert-butane without catalytic reduction, belonging to the field of tert-butane production control. The intelligent control system includes a host computer and sensing and execution mechanisms electrically connected to the host computer. The sensing mechanisms include a TDLAS analyzer installed at the top outlet of the reactive distillation column, NIR analyzers installed at the tert-butanol inlet of the mixing preheater and the side outlet of the reactive distillation column, temperature sensors installed at the top, bottom, and side outlet of the reactive distillation column, flow meters installed at the feed inlet, top outlet, and reflux inlet of the reactive distillation column, and multiple pressure sensors spaced at equal intervals along the height of the reaction section. The execution mechanisms include electrically operated regulating valves installed at the feed inlet and reflux inlet of the reactive distillation column. The control system integrates multiple sensors and execution mechanisms, enabling closed-loop intelligent control of the entire process.
Owner:MAIQI CHEM CO LTD

Synthesis method of topiromilast

The invention belongs to the technical field of medicine synthesis, and particularly relates to a synthesis method of topiromilast. The preparation method comprises the following steps: reacting 2-cyanopyridine-4-formaldehyde serving as a raw material with hydrazine hydrate to obtain an intermediate product, and further reacting with 4-(aminomethyl) pyridine under the action of iodine and tert-butyl hydroperoxide; and performing post-treatment to obtain a target compound. The used raw materials and reagents are low in price and easy to obtain, and the cost advantage is achieved; the post-treatment and purification steps are simple, and the product yield and purity are high.
Owner:SHANDONG NEW TIME PHARMA CO LTD

Non-aqueous electrolyte and secondary battery

In order to overcome the problems of low initial coulombic efficiency and poor cycle performance caused by insufficient ionic conductivity and large lithium consumption of a solid electrolyte interface film formed by unsaturated carbonate, the invention provides a non-aqueous electrolyte and a secondary battery, the non-aqueous electrolyte comprises a non-aqueous organic solvent, an electrolyte salt and an additive, the additives comprise a first additive, a second additive and a third additive, the first additive comprises a compound as shown in a structural formula 1, and the second additive comprises vinylene carbonate, vinylethylene carbonate, 1, 1, 1, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3, 3 the first additive comprises at least one unsaturated carbonate selected from 1, 2-divinyl ethylidene or 1-methyl-1-vinyl ethylidene carbonate, and the third additive comprises one or two selected from acetone or tert-butyl alcohol; the non-aqueous electrolyte satisfies the following conditions: 10 < = X / Y < = 500, 0.1 < = Z / X < = 30, 10 < = X < = 1000, 1 < = Y < = 5, and 10 < = Z < = 500. The non-aqueous electrolyte provided by the invention can regulate and control the film forming quality of unsaturated carbonate, and effectively improves the first coulombic efficiency and the cycle life of the secondary battery.
Owner:SHENZHEN CAPCHEM TECH CO LTD

Catalysts, methods and applications for the synthesis of imiquimod

This invention relates to the technical field of imiquimod synthesis, specifically to catalysts, methods, and applications for imiquimod synthesis. The invention employs a lipase-immobilized lipase complex carrier to catalyze a transesterification reaction, using vinyl isobutyrate as the acyl donor and tert-butanol as the solvent. The hydroxyl group of 3-(4-amino-1H-imidazo[4,5-C]quinoline-1-yl)-2-methylpropane-1-ol is converted to an isobutyl side chain. Following enzymatic catalysis and pH adjustment, hydrolysis is performed to release the isobutyl group, further generating imiquimod and isobutyric acid. The lipase selectively catalyzes transesterification, avoiding side reactions, and the ester bond is rapidly hydrolyzed to the target product under acidic conditions.
Owner:HUBEI MEDICINE IND RES INST CO LTD

Preparation method of high-purity and high-yield benzyloxypyridine compound

The invention relates to the technical field of medicines, and discloses a preparation method of a high-purity and high-yield benzyloxypyridine compound, which comprises the following steps: by taking 2-fluoropyridine and terephthalyl alcohol as initial raw materials, adding potassium tert-butoxide into a solvent I for catalytic reaction to prepare an intermediate crude product; obtaining a high-purity intermediate through a purification process of dissolving the intermediate crude product under an acidic condition and carrying out alkali neutralization crystallization; and finally, reacting with a chlorination reagent, and carrying out low-boiling-point solvent replacement and post-treatment to obtain the high-purity 2-(4-(chloromethyl) benzyloxy) pyridine. The purity of the product obtained by the preparation method is higher than 99.5%, risky impurities and unreacted initiators are not detected, the safety of the product is ensured, meanwhile, the total yield is increased to more than 75%, and the production cost is remarkably reduced.
Owner:TIANJIN CHENXIN PHARM RES CO LTD +1

Process for preparing double metal cyanide catalysts

The present invention relates to a process for preparing a double metal cyanide (DMC) catalyst, comprising the reaction of an aqueous solution of a cyanide-free metal salt, an aqueous solution of an alkaline metal cyanide salt, an organic complex ligand and optionally a complex-forming component, wherein the metal cyanide salt is one or more compound(s) and is selected from the group consisting of potassium hexacyanocobaltat(III), potassium hexacyanoferrate(II), potassium hexacyanoferrate(III), calcium hexacyanocobaltate(III) and lithium hexacyanocobaltat(III), where the organic complex ligand is one or more compound(s) and is selected from the group consisting of dimethoxyethane, tert-butanol, 2-methyl-3-buten-2-ol, 2-methyl-3-butyn-2-ol, ethylene glycol mono-tert-butyl ether and 3-methyl-3-oxetanemethanol, and wherein the alkaline metal cyanide salt used has an alkalinity by the titration method disclosed in the Experimental of between 0.700% and 3.000% by weight of sodium hydroxide (NaOH) based on the total weight of the alkaline metal cyanide salt used. The invention further relates to double metal cyanide (DMC) catalysts obtainable by the process according to the invention and to the use of DMC catalysts for preparation of polyoxyalkylene polyols.
Owner:COVESTRO DEUTSCHLAND AG

Preparation method of 1-amino-2-cyano-1-cyclopentene

The invention discloses a preparation method of 1-amino-2-cyano-1-cyclopentene, which comprises the following steps: 1, preparing a mixed solution, namely mixing a first organic solvent with super alkali in a protective gas atmosphere, heating by adopting a nano infrared energy-saving electric heating coil, stirring, uniformly mixing and dissolving to obtain the mixed solution; the super base is selected from one of potassium tert-butoxide, sodium tert-butoxide, sodium ethoxide, sodium methoxide and sodium hydroxide; 2, cyclization reaction: dropwise adding adiponitrile into the mixed solution, and continuously carrying out infrared heat preservation reaction for 3-8 hours to obtain a reaction solution of 1-amino-2-cyano-1-cyclopentene; 3, cooling crystallization and filtration: cooling the reaction liquid to-10-5 DEG C, standing for crystallization, and carrying out pressure filtration in a protective gas atmosphere to obtain an ACCP crude product and a filtrate; and 4, recrystallizing and refining to obtain a pure product. The method is mild in reaction condition, low in energy consumption, good in product yield and high in product purity, solves the problems of high solvent toxicity, low yield and high environmental protection pressure in the prior art, and is suitable for production of medicine and pesticide intermediates.
Owner:SHANGHAI CHAOWEI TECHNOLOGY CO LTD

Preparation method of 4-hydroxybenzaldehyde

The invention discloses a preparation method of 4-hydroxybenzaldehyde, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: generating an intermediate from cyclohexanone-4-formaldehyde under the action of a Lewis acid catalyst; and reacting the intermediate under the action of a palladium-carbon catalyst, potassium tert-butoxide and argon, and performing acidolysis to generate the target compound 4-hydroxybenzaldehyde. According to the method, cyclohexanone is converted into phenol under the combined action of the key palladium-carbon catalyst, potassium tert-butoxide and argon, and an effective new path is provided for preparation of 4-hydroxybenzaldehyde.
Owner:安徽英特美科技有限公司

Crystallization tower for preparing potassium tert-butoxide

The invention belongs to the technical field of potassium tert-butoxide preparation, and particularly discloses a potassium tert-butoxide preparation crystallization tower which comprises a crystallization tower body, the lower portion of one side of the crystallization tower body is connected with an air inlet pipe, the upper portion of one side of the crystallization tower body is connected with a liquid conveying assembly, and the lower portion of the inner wall of the crystallization tower body is connected with a collecting assembly. According to the crystallization tower disclosed by the invention, crystals and a solution falling in the crystallization tower can be collected through the arranged collection assembly, a mother solution can be separated from the crystals, the mother solution can be recycled, waste of a solvent and raw materials is reduced, and the crystallization tower is environment-friendly and energy-saving. Meanwhile, residual crystals and solution on the inner wall of the crystallization tower can be conveniently collected and treated through the cleaning assembly, and the residual crystals and solution on the inner wall of the crystallization tower can be prevented from corroding or abrading equipment, so that the service life of the equipment is prolonged.
Owner:CHANGYI RONGXIN CHEM CO LTD

Methods for preparing bimetallic cyanide catalysts

This invention relates to a method for preparing a bimetallic cyanide (DMC) catalyst, comprising a reaction of an aqueous solution of a cyanide-free metal salt, an aqueous solution of a basic metal cyanide salt, an organic complexing ligand, and optionally a component forming a complex, wherein the metal cyanide salt is one or more compounds selected from potassium hexacyanocobalt(III), potassium hexacyanoferrate(II), potassium hexacyanoferrate(III), calcium hexacyanocobalt(III), and lithium hexacyanocobalt(III), wherein the organic complexing ligand is one or more compounds selected from dimethoxyethane, tert-butanol, 2-methyl-3-buten-2-ol, 2-methyl-3-butyn-2-ol, ethylene glycol mono-tert-butyl ether, and 3-methyl-3-oxetane-methanol, and wherein the basic metal cyanide salt used has an alkalinity between 0.700 wt% and 3.000 wt% sodium hydroxide (NaOH) based on the total weight of the basic metal cyanide salt used, determined by titration as disclosed in the experimental section. Another subject of the invention includes a bimetallic cyanide catalyst (DMC) obtainable by the method according to the invention, and the use of said DMC catalyst in the preparation of polyoxyethylene polyols.
Owner:COVESTRO DEUTSCHLAND AG

A catalyst and a process for preparing anhydrous tert-butanol by isobutene hydration

The present invention discloses a catalyst and a process for preparing anhydrous tert-butanol by isobutene hydration, belonging to the field of industrial catalysis. The preparation of the catalyst comprises the following steps: after polyethylene glycol-polyglycerol-polyethylene glycol triblock polymer, tetraethyl orthosilicate and deionized water are subjected to a first mixing reaction, sodium aluminate and sodium tungstate dihydrate are added for a second mixing reaction to obtain a mixture, and the mixture is successively subjected to calcination and HCl treatment to obtain a pretreated catalyst support. The pretreated catalyst support, a modified ionic liquid and N,N-dimethylformamide are subjected to a third mixing reaction to prepare the catalyst. In the catalyst prepared by the present invention, the lipophilic group adsorbs isobutene, and the hydrophilic group can interact with water molecules. The two effects cooperate with each other to form a microenvironment favorable for the reaction on the surface of the catalyst, thereby improving the conversion rate of isobutene and the selectivity of anhydrous tert-butanol.
Owner:ZIBO KERUN CHEMICAL TECHNOLOGY CO LTD

Preparation method of tert-butyl lithium

The invention relates to the technical field of tert-butyllithium preparation, in particular to a tert-butyllithium preparation method which comprises the following steps: preparing raw materials, dissolving lithium and washing oil, mixing the raw materials to start reaction, dropwise adding a modifier, carrying out heat preservation treatment, cooling, settling and taking clear liquid. According to the method, trace impurities on the surface of lithium are removed in the pretreatment link, the PVP coating can block contact of water, oxygen and lithium in a long-acting mode, lithium is prevented from going bad in the earlier stage of storage and reaction, and meanwhile the compatibility of lithium and organic solvents such as n-pentane is enhanced; the interference of impurities on the reaction can be eliminated in a high-purity state of the chlorinated tert-butane, byproducts such as lithium tert-butoxide are prevented from being generated, the moisture in the system is strictly limited by deep dehydration, a stable anhydrous environment is provided for synthesis of the tert-butyllithium, and the reaction efficiency is guaranteed; the operation of deep dehydration and impurity removal by activated aluminum oxide creates a high-cleanliness solvent system for the reaction, avoids the action of water and polar impurities with tert-butyllithium or reaction intermediates, and prevents product decomposition or impurity generation.
Owner:SHANGYU HUALUN CHEM