75 results about "Tetrabutylammonium chloride" patented technology

The invention discloses a method for preparing cyclic carbonate. The method specifically comprises the following step: with a quadri-aryloxy bridged rare earth metal compound as a catalyst, catalyzing carbon dioxide and alkylene oxide to react in the present of quaternary ammonium salt, wherein the general formula of the quadriaryloxy bridged rare earth metal compound is LLn(THF), wherein L refers to ethanediamine group bridged quadri-aryloxy, Ln refers to rare earth metal ions, and the quaternary ammonium salt is one of tetrabutylammonium iodide, tetrabutylammonium bromide, tetrabutylammonium chloride, tetraoctyl ammonium bromide, bis(triphenylphosphine) ammonium chloride and benzyl butyl ammonium bromide. The rare earth catalyst in the catalysis system is clear in structure, easy to synthesize, high in catalysis activity, less in using amount, mild in reaction conditions and wide in universality to alkylene oxide. According to the preparation method disclosed by the invention, raw materials are easily available, the reaction conditions are wild, a reaction substrate is wide in universality, the reaction time is short, the yield of the target product, namely the cyclic carbonate is high, and the reaction operation and the posttreatment process are simple.

The invention provides a preparation method of an iron and carbohydrate complex, and particularly relates to a preparation method of ferric carboxymaltose. The preparation method of ferric carboxymaltose comprises the following steps: maltodextrin is oxidized by an oxidant containing tert-butyl hypochlorite in an alkaline aqueous solution in the presence of a phase transfer catalyst; the oxidizedmaltodextrin solution is subjected to a reaction with an aqueous solution of ferric iron salt, wherein the phase transfer catalyst is selected from one or more of quaternary ammonium salts such as trioctylmethylammonium chloride, tributylmethylammonium chloride, tributylmethylammonium bromide, tributylmethylammonium chloride, tetrabutylammonium chloride, and tetrabutylammonium bromide; the oxidantis tert-butyl hypochlorite or a combination of tert-butyl hypochlorite and sodium hypochlorite. Obtained ferric carboxymaltose has MW (molecular weight) of 150-230 kDa, Pd value of 1.2-1.3 and iron content of 26%-31%.

The invention relates to a method for preparing 2-chloro-3-isothiocyanato-prop-1-ene, which is to accomplish the nucleophilic substitution and rearrangement processes of 2,3-dichorproplene and thiocyanate in one step by using 2,3-dichorproplene as a raw material, sodium thiocyanate as a nucleophilic reagent and tetrabutylammonium chloride and potassium iodide as a catalyst. The catalyst used in the invention allows nucleophilic substitution to go smoothly and completely; while the nucleophilic substitution in the system goes smoothly and completely, the rearrangement is also accomplished; andthen, an organic phase is separated, the organic phase is distilled under reduced pressure, and the first distillate is collected. The total yield of the two steps is up to 91 percent. When the method provided by the invention is used, the operation process of the process is simplified considerably, the use of solvent is avoided completely, and the process yield is high; and the cost is reduced, and the production of waste water, water gas and water residue are reduced. Because the system contains little impurity, the yield and purity are not reduced obviously in the process of collecting product under reduced pressure even if the temperature rises to 130 DEG C and the pressure rises to 40mmHg.

The invention relates to a method for extracting benzothiophene by utilizing a deep co-melting solvent composed of tetrabutylammonium chloride and polyethylene glycol. Tetrabutylammonium chloride and polyethylene glycol form the deep co-melting solvent in mole ratio of 1:2, the deep co-melting solvent is mixed with a normal octane solution with the benzothiophene concentration of 200-1600ppm in mixing mass ratio of (0.5-2):1, stirring is carried out for 5-60 minutes at the temperature of 20-50 DEG C and a speed of 600-1000rpm, fully mixing and then standing and layering are carried out, and the benzothiophene concentration of a normal octane layer is detected by adopting a gas chromatographic method, so that extraction rate of benzothiophene is calculated. The method for extracting the benzothiophene by utilizing the deep co-melting solvent composed of tetrabutylammonium chloride and polyethylene glycol has the characteristics of good solubility, mild operating conditions and environmental friendliness and is an efficient and green benzothiphene extraction method.

The invention provides an improved synthesis process for synthesizing rufinamide. The process comprises the following steps of a, reacting 2, 6-difluorobenzyl halide with azide and tetrabutylammonium chloride to obtain 2-(azide methyl)-1,3-difluorobenzene; b, reacting 2-(azide methyl)-1, 3-difluorobenzene with methyl propiolate under the catalyzing of nano-cuprous oxide (Cu2O) to obtain 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-methyl formate; and c, reacting 1-(2,6-difluorobenzyl)-1H-1,2,3-triazole-4-methyl formate with ammonium hydroxide to obtain rufinamide. The process has the advantages of short reaction time and high catalytic efficiency, and is simple and safe to operate.

The invention provides a benzodioxole preparation method, and belongs to the technical field of organic synthesis. The preparation method comprises: mixing catechol, sodium hydroxide, water and dimethyl silicone oil, and carrying out a first reaction to obtain a sodium catechol solution; and mixing the sodium catechol solution, tetrabutylammonium chloride and dichloromethane, and carrying out a condensation reaction to obtain the benzodioxole. According to the present invention, during the preparation of the sodium phenolate solution, dimethyl silicone oil is added, so that the sodium phenolate solution is protected from being oxidized so as to improve the yield of subsequent product; by using tetrabutylammonium chloride as the catalyst, the yield of the benzodioxole is increased comparedwith the use of tetrabutylammonium bromide as the catalyst; and the data of the embodiments show that the preparation method can achieve the molar yield of the benzodioxole of 92-95% and the purity ofthe benzodioxole of greater than 99.9%.

The invention relates to a veratraldehyde preparation method. The method is characterized in that under alkaline condition, vanillin and dimethyl carbonate are subjected to a phase-transfer catalytic reaction, a reaction equation is shown in a specification, wherein, a weight ratio of a phase-transfer catalyst to vanillin is 0.85:1 to 1.27:1, a weight ratio of dimethyl carbonate to vanillin is 2.96:1 to 8.89:1, content of the obtained veratraldehyde is 97-99%, the phase-transfer catalyst can be tetrabutylammonium chloride, tetrabutylammonium bromide, polyethylene glycol, and benzyltrimethylammonium chloride, alkali selects potash, sodium carbonate or sodium acetate, the reaction temperature is 20-120 DEG C, and reaction time is 10-100 hours. Compared with a traditional method, the method has the advantages of no toxicity and environmental protection, and is suitable for industrial production.

The invention discloses a preparation method of a long-chain unsaturated silane coupling agent, and a wood plastic material production technology. The preparation method comprises the following steps that long-chain unsaturated fatty acid and an alkali solution of which the mole amount is the same as the mole amount of the long-chain unsaturated fatty acid undergo a reaction to produce an unsaturated fatty acid salt; and the unsaturated fatty acid salt and chlorosilane of which the mole amount is the same as the mole amount of the unsaturated fatty acid salt undergo a reaction in the presence of tetrabutylammonium chloride to produce the long-chain unsaturated silane coupling agent. 100 parts of thermoplastic plastic, 50 to 150 parts of plant fiber powder, 1 to 15 parts of long-chain unsaturated silane, 1.5 to 5 parts of a lubricant and 0.5 to 1.5 parts of an initiator are subjected to in-situ reaction extrusion in an extruder to produce a wood-plastic composite material. The adopted long-chain unsaturated silane has moderate activity and can fully contact with the plant fiber powder and resin molecules so that the long-chain unsaturated silane and the plant fiber powder and the resin molecules undergo a chemical reaction; and through chemical bonding effects stronger than a dispersion force, high interface bonding strength is obtained and a doping amount and performances of plant fiber powder are greatly improved.

The invention discloses a method for preparing 1-chloro-1-acetylcyclopropylamine by continuous flow reaction, and belongs to the technical field of fine chemical engineering preparation processes. Themethod comprises the following steps: simultaneously pumping a 3,5-dichloro-2-pentanone and chloroform mixed solution, a sodium hydroxide aqueous solution and a tetrabutylammonium chloride mixed solution in a continuous flow device by a metering pump, and after completing reaction at the temperature of 50-60 DEG C, transferring the mixed solution to a low-temperature region and quenching the mixed solution. A continuous flow reactor replaces kettle type reaction, the time of contact between a product and alkali is shortened, side products such as tar are reduced, and the yield is increased.

The invention discloses a synthetic method of doxofylline and belongs to the technical field of organic synthesis. The method comprises the following step: theophylline and 2-chloromethyl-1,3-dioxolane are subjected to a reaction at 60-110 DEG C in an aprotic solvent under the action of alkali and a phase transfer catalyst, and doxofylline is synthesized, wherein the mole ratio of theophylline, 2-chloromethyl-1,3-dioxolane and the alkali is 1:1-2:1-3, the phase transfer catalyst accounts for 3%-5% of the molar weight of theophylline, and the phase transfer catalyst is selected from one or moreof tetrabutylammonium chloride, tetrabutylammonium bromide and tetrabutylammonium fluoride. The provided new synthetic method of doxofylline is short in reaction time and only needs 3-6 h, is low inreaction temperature which is lower by 20-30 DG C than that of the conventional method, is high in yield which is 10% or higher than that of the conventional method, and is beneficial to industrial production of the drug.

The invention discloses a synthetic method of isonicotinic acid. The method comprises the following steps: mixing 4-bromopyridine with N, N-dimethylformamide or acetonitrile and tetraethylammonium chloride or tetraethylammonium bromide or tetraethylammonium iodide or tetraethylammonium tetrafluoroborate or tetrabutylammonium chloride or tetrabutylammonium bromide or tetrabutylammonium iodide to form an electrolyte; introducing carbon dioxide at normal pressure for 30 minutes; and carrying out electrolysis at a constant current, keeping introducing the carbon dioxide during the electrolysis process until the electrolysis is ended, and obtaining the isonicotinic acid after carrying out post-treatments. According to the synthetic method of the isonicotinic acid, the reaction system is simple and easy to control, the rich C1 resource, namely the carbon dioxide is used as one of the raw materials, is cheap and easy to obtain, is low in cost and does not pollute the environment, and therefore a new way is developed for the study of the green isonicotinic acid, an extremely good application prospect of the synthetic method is displayed in the medicine industry, the food industry, the chemical industry and the electronic industry, and the synthetic method of the isonicotinic acid is a process route with high industrial synthetic value.

The invention discloses a bagasse saccharifying method which comprises the following steps: (1) pretreatment of bagasse: sterilizing bagasse with infrared ray, and regulating the moisture content of bagasse to 15%-20% through microwave drying or addition of water; (2) saccharification: adding zymophyte in bagasse, then fermenting at the temperature of 25-30 DEG C, stopping fermentation when ethylalcohol is generated, sterilizing bagasse with infrared ray, then adding citric acid, dimethyl sulfoxide tetrabutylammonium chloride and dimethyl sulfoxide imidazolium salt in the sterilized bagasse,and degrading for 2-6 hours at the room temperature, wherein the zymophyte comprises trichoderma reesei, aspergillus niger, aspergillus aculeatus and kluyveromyce; and (3) enzyme deactivation: puttingthe saccharified bagasse at a high temperature of above 100 DEG C for sterilization for 10-30 min. The bagasse saccharifying method has the advantages that the saccharifying rate is high, and the fermentation end-point is easy to control.

The invention discloses a montmorillonoid modified anti-aging cable insulating material and a manufacturing method thereof. The manufacturing method includes subjecting montmorillonoid, tetrabutylammonium chloride and hydrochloric acid to activating treatment on a condition of decompression, and then filtering to obtain a filter cake to obtain an activated composition; subjecting epoxy resin, neoprene, ethylene-vinyl alcohol copolymer, n-butyl alcohol, hydroxyethyl acrylate, tungsten oxide, tris(dimethylamino)silane, mica powder, diborane, quinoline, dicumyl peroxide, ozocerite, sodium hexametaphosphate and the activating composition to mixing, melting and cooling shaping to obtain the anti-aging cable insulating material. The anti-aging cable insulating material manufactured by the method has excellent insulativity, mechanical property and anti-aging property.

The invention discloses a 1-amino-3-alkyl-1, 2, 3-triazole nitrate compound and its synthesis. The synthesis method consists of: taking glyoxal and hydrazine hydrate as materials to react to obtain glyoxal bishydrazone; taking water as a solvent, adding the glyoxal bishydrazone and a catalyst to react so as to obtain 1-amino-1, 2, 3-triazole; then adopting water as the solvent, in the presence of a phase transfer catalyst tetrabutylammonium chloride or tetrabutylammonium hydrogen sulfate, adding a alkylation reagent dropwisely to undergo reaction to obtain 1-amino-3-alkyl-1, 2, 3-triazole bromide; and finally using water as the solvent, and adding silver nitrate to undergo reaction, thus obtaining the 1-amino-3-alkyl-1, 2, 3-triazole nitrate. The compound 1-amino-3-alkyl-1, 2, 3-triazole nitrate provided in the invention is an energetic surfactant. Adding of the energetic surfactant into mixed explosives can enhance the physicochemical properties and dispersion performance, etc., and has little influence on the overall energy of the mixed explosives. The synthesis process involved in the invention is carried out in a solvent-free condition or in a water solution, the cost is low, and the environmental pollution is small, thus meeting the dual development needs of environment and economy.

The invention discloses a high performance liquid chromatographic analysis method for testing the content of edetate disodium. According to the method, octadecyl silane bonded silica gel is adopted asa filling agent, ferric sulfate is adopted as a diluent, a sodium acetate buffer solution-acetonitrile with tetrabutylammonium chloride is adopted as a mobile phase, the ratio of the buffer solutionto acetonitrile is 4 to 6, a detection wavelength is 350nm, a flowing velocity is 1.0ml/minute, and a feeding volume is 25mu l. By adopting the method, edetic acid radical ions can be effectively separated and accurately quantified. The method is good in specificity, good in precision and high in accuracy, and is capable of rapidly and accurately testing the content of edetate disodium.

The invention relates to a method for extracting thiophene and benzothiophene simultaneously and belongs to the field of extraction separation. The method for extracting the thiophene and the benzothiophene simultaneously comprises steps as follows: an extracting agent is contacted with a mixture, wherein the extracting agent is a deep eutectic solvent comprising N,N-dimethyl-N-nitrilethyl ammonium propionate and tetrabutylammonium chloride in the mass ratio being 1:1; the mixture comprises the thiophene, the benzothiophene and normal octane. According to the method, the extraction efficiency is high, the selectivity is high, desulfurization rates of the thiophene and the benzothiophene can be up to 96.84% and 99.99%, and operation conditions are mild and environment-friendly.

The invention discloses a capacity rapid recovery method for a lead-acid storage battery, and the method comprises the following steps: S1, preparing raw materials of a function repair solution, including a sulfuric acid electrolyte, sodium sulfate, isoascorbic acid, 2-acrylamide-2-methylpropanesulfonic acid and tetrabutylammonium chloride; S2, mixing sodium sulfate, tetrabutylammonium chloride and the sulfuric acid electrolyte to obtain a repair liquid base material, adding isoascorbic acid and 2-acrylamide-2-methylpropanesulfonic acid into ethyl alcohol, performing stirring, performing pressure reduction and vacuumizing to obtain a functional mixture, adding the repair liquid base material into the functional mixture to obtain the functional repair solution; S3, fully discharging the lead-acid storage battery; S4, adding the functional repair solution; S5, fully charging the lead-acid storage battery. The method provided by the invention is low in restoration cost, simple to operate,short in consumed time and good in restoration effect.

The invention discloses a method for preparing dimethyltin chloride, which comprises the following steps of: 1) heating tin, a catalyst and tin tetrachloride with a weight ratio of 1:0.1-0.5:0.1-0.3 to between 100 and 170 DEG C under the airtight condition, wherein the catalyst is tetramethylammonium chloride or tetrabutylammonium chloride; 2) adding chloromethane with stirring, continuing to raise the temperature to between 170 and 250 DEG C under the pressure of 0.9 to 1.7MPa, stopping adding the chloromethane and then continuing to stir for 1 to 5 hours to prepare gaseous dimethyltin chloride; and 3) performing falling film absorption on the gaseous dimethyltin chloride for 1 to 6 hours by using water as absorption liquid under the conditions that the temperature of the gaseous dimethyltin chloride is between 180 and 260 DEG C and the pressure is 0.9 to 1.7MPa to obtain aqueous solution of the dimethyltin chloride. By a direct synthesis method, a process is simple, production cost is greatly reduced and a product is nontoxic and meets the requirement of environmental protection.

The invention discloses a method for preparing hydrophilic nano silica for a silicone sealant and relates to the technical field of nanometer materials. Water glass and concentrated hydrochloric acid are taken as raw materials to manufacture nano silica; and hydrolytic polymaleic anhydride, tetrabutylammonium chloride, polyethylene glycol 400 and polyoxyethylene lauryl ether are utilized to chemically modify the hydrophilic nano silica, to obtain the hydrophilic nano silica. The granularity of the hydrophilic nano silica reaches 20-30 nm. The prepared hydrophilic nano silica is applied to the silicone sealant, not only can shorten curing time of the silicone sealant and water, but also enhances caking property, weather resistance, vibration resistance and high-low temperature resistance, and effectively expands the use range of the sealant.

The invention discloses a method for removing a methyl protecting group from a phenolic hydroxyl under a mild condition. The method is characterized in that a methyl of the phenolic hydroxyl with the amide structure can be completely removed by taking TBACl (Tetrabutylammonium Chloride), TBABr (Tetrabutylammonium Bromide) or TBAI (Tetrabutylammonium Iodide) as a removal agent for the methyl of the phenolic hydroxyl with an amide structure and tetrahydrofuran as a solvent and stirring for four hours at 70 DEG C. The method disclosed by the invention is mild in reaction conditions, less in byproducts, high in yield and simple in operation, and is capable of selectively removing the methyl protecting group of the phenolic hydroxyl with a specific structure.

The invention discloses a novel preparation method of p-fluoronitrobenzene, and relates to the field of organic synthesis. The method concretely comprises the following steps of firstly crushing durian shells; adding ethanol; performing ball milling to prepare durian shell powder; then, mixing the durian shell powder with urea; performing sintering treatment at a certain temperature to obtain mixed powder; adding the mixed powder into a tetrabutylammonium chloride solution for stirring and still standing treatment; then, performing drying to obtain a catalyst; adding reaction raw materials ofpara-nitrochloro-benzene, potassium fluoride and the catalyst into a reaction kettle; performing sealing; performing reaction at a certain temperature; after the reaction is completed, performing water washing and layering treatment; performing organic layer rectification to obtain a target product. The method disclosed by the invention has the advantages that the operation is simple; a solvent isnot used in the reaction process; the cost is effectively reduced; the product yield is high.

The invention belongs to the field of fertilizers, and mainly relates to a flower fertilizer prepared from traditional Chinese medicine residues and used for Chrysalidocarpus lutescens and a preparation method thereof. The preparation method mainly comprises the following steps of (1) drying the medicine residues, (2) adding 0.3 g of tetrabutylammonium chloride into 100 ml of water for dissolving,heating the obtained solution at a constant temperature of 35-45 DEG C, and dropwise adding a KH2PO4/K2H2PO4 buffer solution with the pH value of 6.1-7.8 into the solution for 60 minutes until the system becomes turbid from clear, (3) extraction, (4) re-extracting, and (5) adding sugar alcohol, peat and other components. The fertilizer provided by the invention can promote the content and stability of trace elements in the fertilizer and promote the absorption of nutrient substances in the fertilizer by the Chrysalidocarpus lutescens, and due to components of peat, peat ash, peanut shell andthe like, growth of the Chrysalidocarpus lutescens can be effectively promoted, absorption of the nutrient substances in the fertilizer by the Chrysalidocarpus lutescens is promoted, and the content of chlorophyll in leaves can be significantly improved.