156 results about "Trimethyl borate" patented technology

Process for preparing an alkoxylated alcohol comprising reacting a starting monohydroxy alcohol selected from secondary alcohols, tertiary alcohols and mixtures thereof with an alkylene oxide in the presence of hydrogen fluoride and a boron-containing compound comprising at least one B—O bond. The alcohol may also be a primary monohydroxy alcohol when the boron containing compound is boric acid or boric acid anhydride or a mixture thereof, or may be a primary mono hydroxy alcohol, except a C14 / C15 alcohol when reacted with ethylene oxide in the presence of HF and trimethyl borate. A phenol may be alkoxylated in the same way instead of the mono-hydroxyalcohol.

The invention provides a novel process method for preparing trimethyl borate through continuous reactive distillation. The process method comprises the following steps of: (1) continuously feeding methyl alcohol and boric acid into a reaction kettle based on ratio to realize initial reaction; (2) continuously feeding reaction liquid into a rough evaporating kettle to evaporate; transferring methyl alcohol, trimethyl borate and water into a reactive distillation tower in form of mixed gas by a evaporating manner; continuously draining water produced in the reaction of methyl alcohol and trimethyl borate from the bottom of the tower; carrying out reaction for producing trimethyl borate after the water is drained until boric acid is completely reacted, so as to improve the one-time conversion rate of boric acid to be more than 99.5% as well as reduce the mixing ratio of methyl alcohol, wherein the energy consumption in preparation of trimethyl borate is greatly lowered down, all discharges from the bottom of the tower are the water produced in the reaction, and little boric acid and methyl alcohol are left; and (3) transferring trimethyl borate output from the reactive distillation tower by an evaporating manner into an azeotropic distillation tower together with methyl alcohol, lowering down the temperature of absolute methanol at the bottom part of the zeotropic distillation tower and recovering the absolute methanol, recovering azeotrope of trimethyl borate and methyl alcohol from the top of the tower, and then separating the azeotrope to obtain trimethyl borate.

The invention belongs to the field of medicine synthesis and specifically relates to a preparation method of an anidulafungin side chain intermediate 4'-orthopentyloxy-1,1':4',1'-terphenyl-4-carboxylic acid. The preparation method comprises the following steps: initiating a 1,4-dibromo-benzene material which serves as a starting material to carry out Grignard reagent reaction with magnesium by iodine; then, preparing 1,4-benzene hypoboric acid by virtue of addition and hydrolysis with trimethyl borate; and preparing 4'-orthopentyloxy-1,1':4',1'- terphenyl-ethyl carboxylate by virtue of Suzuki reaction of 1,4-benzene hypoboric acid, 4-pentyloxy bromobenzene and 4-halogenated ethyl benzoate in dioxane-ethanol liquor under catalysis of [1,1'-bis(diphenyl phosphino) ferrocene] palladium dichloride, and then, hydrolyzing to obtain a target product. The preparation method disclosed by the invention can lower process cost, is simple, convenient, safe and reliable to operate, and suitable for industrial production.

A novel carbinol gasoline fuel relates to an engine fuel, in particular to a novel liquid fuel for a gasoline engine. According to the weight parts, the novel carbinol gasoline fuel is mixed simply by the following raw materials of the composition: 20-80 of gasoline, 20-90 of carbinol, 2-10 of petroleum ether, 1-5 of 2-methylpentane, 0-5 of octane, 0-5 of isooctane, 0-5 of diethyl carbonate, 0-4 of cinnamene, 0.2-4 of trimethyl borate, 0-5 of dibutyl phosphite, 0.5-5 of dimethyl carbonate, 0-5 of methyl tertiary butyl ether, 0-4 of ether, 0-4 of isopropyl ether, 0-6 of acetone, 0-4 of isopropyl alcohol, 0-5 of isobutyl alcohol and 0-4 of anti-oxidant. The antiknock index is reinforced as the octane number is improved; and the compounding is optimized scientifically during the experiment and practice, thus leading the vehicle to keep the best stability on all aspects when the liquid fuel is in use.

The invention relates to a method for fast preparing boron carbide ceramic powder. The method for fast preparing the boron carbide ceramic powder comprises the following steps: 1) choosing raw materials: choosing trimethyl borate and sucrose according to the weight ratio of the trimethyl borate to the sucrose equal to (12:1)-(12:3); choosing methanol, chelating agent acetic acid and water according to the volume ratio of the trimethyl borate, the methanol, the chelating agent acetic acid to the water equal to (6:40:1:1)-(6:80:2:4); and choosing solvent acetic acid according to the ratio of the sucrose to the solvent acetic acid equal to (7-8)g:50ml; 2) preparing dry gel powder; 3) preparing precursor powder; and 4) thermally treating the precursor powder. Under the conditions of high heating speed and short heat preserving time, the carbon thermal reduction reaction is carried out so that the carbon thermal synthesis process of the boron carbide is shortened to dozens of minutes or even several minutes; and, high-purity fine carbon carbide ceramic powder with good sintering property can be obtained without the subsequent carbon removal processes. The carbon carbide ceramic powder is the single carbon carbide phase through X-ray diffraction analysis; the content of free carbon in the product is 1-3%; and, the grains are uniform and fine, and the average grain size is less than 500nm.

A composition comprising a polyepoxide, a hardener, trimethyl borate, and a flame retardant is disclosed. Methods for preparing the composition and its end uses are also disclosed.

The invention relates to a triphyene derivative containing diarylethene and an application thereof. The triphyene derivative is obtained by the way that triphyene derivative halogeneated triphyene and bisthienylethenes containing trimethyl borate are in coupled reaction. The designed and compounded triphyene derivative has the characteristics of being good in heat stability, high in quantum efficiency, short in light response time and the like. In addition, a unique solvation color development phenomenon is shown in triphyene derivative alkane chloride. Consequently, the triphyene derivative containing the diarylethene not only can be used for full color display and information storage but also can be used for trace detection of the alkane chloride.

The invention discloses high-activity washing-free scaling powder. According to the weight percentage, the high-activity washing-free scaling powder includes 45.0 to 80.0 percent of trimethyl borate, 0.01 to 10.0 percent of acetone, 0.001 to 1.0 percent of cesium fluoride or rubidium bifluoride, 0.001 to 2.5 percent of aether; and the rest is carbinol. When the scaling powder produced by the invention is matched with the solders like Cu-P series for soldering, the solder has excellent wetting performance and fluidness on a mother plate, can reduce the soldering defects from generating and can improve the intensity of a soldering seam and still has the characteristics of stopping the metal surface in a soldering area from being oxidized and needing not to be washed by acid after soldering.

The invention discloses a method and a special device for separating trimethyl borate from a carbinol mixture. The method is a salt-adding extraction and rectification method which comprises the following steps of: charging a salt-containing solvent, trimethyl borate and carbinol mixture from the upper part and middle part of an extraction and rectification tower respectively, carrying out salt-adding extraction and rectification, withdrawing pure trimethyl borate from the top of the tower, and obtaining the mixture of carbinol, salt and solvent at a tower kettle; and charging the mixture of carbinol, salt and solvent into a solvent recovering tower from the middle, wherein the distillate on the top of a recovery tower is the carbinol, obtaining the salt-containing solvent at the tower kettle, and repeatedly charging the salt-containing solvent into the extraction and rectification tower to be used. The method is better in effect due to the salt-adding extractant compared with the extractant, has the advantages of being convenient to recycle and easy to realize on the industry, can be used for overcoming the defect that the sold salt in a salt-adding rectification technology is hard to cycle, can be used for greatly improving the separation effect since the relative volatility of the trimethyl borate and the carbinol is increased, has the advantages of being low in equipment investment and low in energy consumption, and can be used for the industrial application for the separation and purification of the trimethyl borate.

The invention provides a preparation method of tri(pentafluorophenyl) borane. The method comprises the following steps: by using pentafluorobromobenzene as a raw material, dissolving the raw material in an organic solvent; adding strong base at a certain temperature; reacting to obtain an intermediate; and performing a reaction on the intermediate and trimethyl borate for a period of time to obtain tri(pentafluorophenyl) borane. The preparation method provided by the invention has the characteristics of shorter reaction process, simpleness and convenience in operation and lower cost of raw materials.

The invention discloses a preparation method of trimethyl borate. The method comprises the following steps of: (1) heating and dehydrating a boric acid solid to prepare metaboric acid and pyroboric acid solids; (2) adding the metaboric acid and pyroboric acid solids which are obtained in the step (1) to methanol to make the mixture react under a stirring state; (3) heating and distilling the reaction solution obtained in the step (2) to obtain an azeotrope solution of the methanol and the trimethyl borate, distilling and cooling raffinate to obtain boric acid; and (4) separating the azeotrope solution of the methanol and the trimethyl borate, which is obtained in the step (3), to obtain a trimethyl borate product. In the invention, by firstly heating and dewatering the boric acid to prepare the metaboric acid and the pyroboric acid and then making the metaboric acid and the pyroboric acid react with the methanol to prepare trimethyl borate, the reaction speed is accelerated, the conversion per pass is improved, the reaction conditions are mild and no risks exist.

The invention provides a synthetic method for tetra(pentafluorophenyl)borate. The synthetic method comprises the following steps: with pentafluorobromobenzene as a starting raw material, treating pentafluorobromobenzene with organic lithium or a Grignard reagent so as to obtain an intermediate A; reacting the intermediate A with trimethyl borate; and carrying out post-treatment so as to obtain the target product tetra(pentafluorophenyl)borate with a structural formula described in the specification. M+ in the product of the method is any one selected from the group consisting of organic carbocation, organic ammonium ion and alkali metal ion. Compared with the prior art, the invention has the following advantages: usage of tri(pentafluorophenyl)borane sensitive to water and oxygen is avoided; product yield is high; and the method has good process and operation practicality, simple steps and low requirements on equipment and is suitable for industrial production.

The invention discloses a preparation method of 4-phenoxyphenylboronic acid, which relates to the technical field of organic synthesis. It uses 4-bromodiphenyl ether as raw material, tetrahydrofuran as solvent, and reacts with magnesium flakes first to prepare Grignard reagent. The crude product of 4-phenoxyphenylboronic acid is obtained by reacting the reagent with trimethyl borate, and then hydrolyzing with hydrochloric acid. Finally, the finished product of 4-phenoxyphenylboronic acid is obtained after purification. The raw materials used in the invention are cheap and easy to obtain, the reaction conditions are mild, the post-processing operation is simple, the production cost is low, the yield is high, and the method is suitable for industrial production.

The invention discloses a synthesis method of a cefpodoxime proxetil intermediate, namely (6R,7R)-7-[2-(2-amino-4-thiazolyl)-(Z)-2-(methoxyimino)acetamido]-3-methoxymethyl-8-oxo-5-thio-1-azabicyclo[4.2.0]oct-2-ene-2-methanoic acid. The synthesis method includes: enabling chlorosulfonic acid and methanol to react to prepare methoxy sulfonic acid; under the action of the methoxy sulfonic acid and dimethylformamide, etherifying 7-ACA (7-aminocephalosporanic acid) and trimethyl borate prior to aftertreatment, adding into a water and methanol solution reversely to guarantee that the obtained intermediate isn't sticky and is loose, drying and grafting with AE active ester so as to obtain a target product, namely the cefpodoxime proxetil intermediate. The synthesis method of the cefpodoxime proxetil intermediate has the advantages that synthesis steps of 3-position and 7-position protection and desorption of 7-ACA can be omitted, so that low step cost, high yield and high purity are achieved, all materials are cheap and available, and industrial production and little pollution are benefited.

A composition comprising a polyepoxide, a hardener, trimethyl borate, and a flame retardant is disclosed. Methods for preparing the composition and its end uses are also disclosed.

The invention discloses a nano silicon dioxide modified wood production method including five steps of pretreatment, preparation of a wood modification agent, preparation of a wood modification fluid, dipping treatment and post-drying treatment, wherein the wood modification agent comprises nano silicon dioxide, fatty alcohol polyoxyethylene ether, distilled water, trimethyl borate, dodecyl dimethyl benzyl ammonium chloride, N-(2-benzimidazole)-methyl carbamate, and imidacloprid. The beneficial effect is that the nano silicon dioxide modified wood production method has the advantages of simple treatment process, easy operation, low cost, good treatment effect, no toxicity, environmental friendliness and the like, the treated wood has no obvious appearance change, and wood dimensional stability, density, surface hardness, bending strength and bending elastic modulus, good processing properties, wear resistance, anti-corrosion flame retardant properties are greatly increased.

The invention discloses a trimethyl borate additive contained high-voltage functional electrolyte and a preparation method and an application therefor. The electrolyte is obtained by adding a functional additive to a common electrolyte; the common electrolyte is formed by a cyclic carbonate solvent, a linear carbonate solvent and a conductive lithium salt; and the functional additive adopts trimethyl borate. According to the functional electrolyte, the trimethyl borate additive is taken as the high-voltage film-forming additive for the lithium ion electrolyte; the additive is relatively low in oxidization and reduction potential, so that a compact and stable SEI film layer can be formed on the surfaces of a positive electrode and a negative electrode in the first charge-discharge process; therefore, the films on the surfaces of the positive electrode and the negative electrode are optimized, the resistance between the positive electrode and the electrolyte is lowered, and the surface activity of the electrodes is restrained, so that the further contact between the electrolyte and the electrode active material is restrained consequently, and the oxidization and decomposition of the electrolyte main body solvent on the electrode surface is lowered; and the cycling performance and the rate capability of the electrolyte additive contained lithium ion battery under 3-4.5V can be improved.

The invention discloses a preparation method for 3-carboxyphenylboronic acid, relating to the technical field of organic synthesis. The preparation method comprises the steps of performing Grignard reaction on m-bromomethyl benzene, magnesium scraps and iodine by using the m-bromomethyl benzene as a starting material, so as to generate a Grignard reagent, performing boronated reaction on the Grignard reagent and trimethyl borate so as to prepare 3-Tolylboronic acid, and oxidizing the 3-Tolylboronic acid with potassium permanganate in an alkaline condition so as to prepare 3-carboxyphenylboronic acid. According to the preparation method, cheap m-bromomethyl benzene easy to obtain is used as the starting material, the 3-carboxyphenylboronic acid is prepared through Grignard reaction, boronated reaction and oxidization reaction, the operations are simple, the average purity of the product 3-carboxyphenylboronic acid reaches 99.3%, and the average total yield reaches 50%. The product yield and purity are ensured at low cost, so that the preparation method is applicable to industrial production.

The invention discloses a preparation method of crisaborole. The method comprises the steps as follows: a compound shown in a formula I and alkali metal borohydride are subjected to a contact reaction, and a compound shown in a formula II is obtained; the compound shown in the formula II and a compound a are subjected to a contact reaction, and a compound III is obtained; or the compound shown inthe formula II and dihydropyran are subjected to a contact reaction, and a compound III is obtained, wherein the compound a is trimethylchlorosilane, tert-butyldimethylsilyl chloride or chloromethyl methyl ether; the compound shown in the formula III and an isopropylmagnesium chloride solution are subjected to a contact reaction, and a standby solution is obtained; then, the standby solution is added to a mixed solution of a compound b and a third organic solvent for a contact reaction, hydrochloric acid is added for a contact reaction, and crisaborole, namely, a compound shown in a formula IV, is obtained, wherein the compound b is 2-alkoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane, triisopropyl borate or trimethyl borate.

The invention relates to a preparation method of boron-10 acid. The preparation method of the boron-10 acid comprises the following steps: heating a prepared lithium carbonate-water solid-liquid mixture to be at 40-80 DEG C, inflating boron trifluoride-10 gas into the lithium carbonate-water solid-liquid mixture, stirring so as to uniformly disperse the boron trifluoride-10 into the solid-liquid mixture, and stopping gas inflation when the mol ratio of the boron trifluoride-10 to the lithium carbonate reaches (1: 1.5)-1.6; conducting an reaction for 10-25 hours to generate the boron-10 acid; separating, and performing ion exchange and crystallization to separate out the boron-10 acid solid. The preparation method is carried out in an aqueous system, thus avoiding ester hydrolysis in the process of generating trimethyl borate; the preparation method is simple in process and can be industrialized easily; the boric acid is high in yield and purity, the yield is above 95% and the purity is above 98%.

Fuel mixtures for direct methanol fuel cells are disclosed. The fuels include methanol and additives that react with water to produce methanol and other easily electro-oxidizable compounds including dimethyloxymethane, methylorthoformate, tetramethylorthocarbonate, trimethylborate, and tetramethylorthosilicate. Other additives to improve safety and efficiency of the fuel cell include sulfonated activated carbon particles and metal hydrides, such as LiAlH4, NaBH4, LiBH4, (CH3)2 NHBH3, NaAlH4, B2H6, NaCNBH3, CaH2, LiH, NaH, KH or sodium bis (2-methoxyethoxy) dihydridaluminate.

The invention discloses a nontoxic environmentally-friendly wood preservative. The nontoxic environmentally-friendly wood preservative is characterized by being prepared through the following raw materials in parts by weight: 15 parts of sodium dodecyl sulfate, 7 parts of trimethyl borate, 6 parts of polyethylene acid ester, 7 parts of butyl carbamate, 4 parts of twain-20, 4 parts of OP-10, 4 parts of lauryl diethanol amine, 5 parts of polyethylene glycol, 6 parts of glycerin, 2 parts of p-hydroxybenzoic acid monosodium salt, 2 parts of potassium sorbate, 8 parts of diatom ooze, and 150 parts of deionized water. The wood preservative has the following advantages: (1) the environment is protected, and no pollution is caused; the production and use do not damage the environment and human body; (2) the self stability is high, and decomposing or falling off in general environment can be avoided; (3) the antibiotic spectrum is wide; general bacteria which can corrode wood can be eliminated and inhibited; and (4) the applicable scope is wide; the nontoxic environmentally-friendly wood preservative is applicable to corrosion prevention of wood used in buildings, furniture, ships and other environments.

A wood treating agent is prepared from the following raw materials in part by weight: 3-10 parts of phenol, 4-7 parts of melamine, 5-10 parts of potassium isopropoxide, 5-8 parts of calcium chloride, 3-8 parts of phosphoric acid, 3-5 parts of boric acid, 1-4 parts of zinc chloride, 6-10 parts of trimethyl borate, 7-10 parts of dodecyl dimethyl benzyl ammonium chloride, 5-9 parts of lignin, 4-8 parts of waterborne zinc stearate emulsion, 5-11 parts of sodium tripolyphosphate, 2-6 parts of folic acid, 3-9 parts of parachlorometaxylenol, 8-11 parts of bronopol, and 6-8 parts of sodium chlorate. The wood treating agent has the benefits that the wood treating agent has good corrosion prevention and insect prevention effects, can form a good breathable layer, and can prolong the service life of wood.

The invention provides a preparation method of diborane, and solves the technical problems of unreasonable preparation method, high raw material price, complex product purification operation, high cost, low yield and unsuitability for industrial production. The preparation method of diborane takes sodium hydride, trimethyl borate and boron trichloride as initial raw materials, and tetrahydrofuran as a reaction solvent, and carries out condensation reaction and a double decomposition reaction to obtain the diborane. The method can be widely applied to the technical field of diborane preparation.

A process for preparing phenylboric acid includes two steps: preparing Grig nard reaction liquid and preparing phenylboric acid. In the second step, the tributyl borate is used to replace trimethyl borate, resulting in high output rate (more than 60%) and low cost.

The invention provides a pickling-free flux, comprising 37-47% of trimethyl borate (by weight); preferably, the weight percentage of the trimethyl borate is 40%. The invention also provides a method used for preparing the pickling-free flux, comprising the steps as follows: under the conditions of temperature of 45-50DEG C, the pressure of 1Pa-1.2Pa and the catalyst of potassium permanganate, boracic acid and carbinol react completely, filtrated and washed to a neutral state, thus gaining the pickling-free flux; furthermore, the pickling-free flux is dried suitably. The pickling-free flux has simple and convenient usage, good film-forming effect, no residues after brazing and no corrosion phenomenon occurring on brazing workpiece, reduces the brazing cost, and protects the environment; the preparation method is simple and convenient and the gained product has high purity.

A method is provided for recovering boric acid from a solution containing boric acid and at least one lithium compound. The method comprises (a) passing the solution through an ion exchange resin such that boric acid accumulates on the resin; (b) removing the boric acid from the resin with an aqueous alcohol solution, thus obtaining a first solution comprising an alcohol, boric acid, and water; (c) converting at least a portion of the boric acid to trimethyl borate, thereby obtaining a second solution; (d) distilling an azeotrope from the second solution, wherein the azeotrope contains trimethyl borate; and (e) recovering boric acid from the azeotrope.

The 7-amino-3-methoxymethyl-3-cephem-4-carboxylic acid of the molecular formula (I) can be obtained by azeotroping the 7-aminocephalosporic acid of the molecular formula (II) with trimethyl borate and methanol. The mixture is readily prepared by reaction in the presence of methanesulfonic acid.

The invention discloses a preparation method of a Crisaborole intermediate. The Crisaborole intermediate has a structure shown as the formula VI. The preparation method comprises the following steps:performing a contact reaction on a compound shown as the formula I and benzyl halide, so as to form a compound shown as the formula II; performing a contact reaction on the compound shown as the formula II and alkali metal borohydride, so as to obtain a compound shown as the formula III; performing a contact reaction on the compound shown as the formula III and a compound a, or performing a contact reaction on the compound shown as the formula III and dihydropyran, so as to obtain a compound shown as the formula IV, wherein the compound a is trimethylchlorosilane, tert-butyldimethylsilyl chloride and chloromethyl methyl ether; performing a contact reaction on the compound shown as the formula IV and an isopropylmagnesium chloride solution; adding an obtained solution into a compound b, performing a contact reaction on the mixture and fourth organic solvent mixed liquor and adding hydrochloric acid into the mixture for contact reaction, so as to obtain a compound shown as the formula V,wherein the compound b is 2-alkoxy-4, 4, 5, 5-tetramethyl-1, 3, 2-dioxaborolane, triisopropyl borate or trimethyl borate; performing a hydrogenation reaction on the compound shown as the formula V toobtain a compound shown as the formula VI.

The invention discloses an unsymmetrical synthesis method of (S)-rivastigmine. The method comprises the following steps of: reacting hydroxyacetophenone with methylethylcarbamoyl chloride to generate N-ethyl-N-methyl-carbamate 3-acetylphenyl formate, carrying out chiral reduction on the N-ethyl-N-methyl-carbamate 3-acetylphenyl formate under the catalysis effect of a complex of (S)-(-)-alpha, alpha-diphenyl prolinol and trimethyl borate, carrying out methanol dissociation to generate N-ethyl-N-methyl- carbamate 3-[(R)-1-hydroxyethyl]phenyl formate, and reacting the N-ethyl-N-methyl- carbamate 3-[(R)-1-hydroxyethyl]phenyl formate with methylsufonyl chloride and dimethylamine hydrochloride to obtain the (S)-rivastigmine. According to the method disclosed by the invention, a target product can be prepared from conventional reagents only through a three-step reaction, the reaction yield reaches 40% and is far higher than that by a racemic resolution method and that by other chiral synthesis methods, the application of virulent reagents and highly corrosive reagents are avoided in the process, and the unsymmetrical synthesis method is easy to operate, environment-friendly, low in production cost, and suitable for industrialized production.