44 results about "Dichlorobutane" patented technology

The invention discloses a rapid simple efficient method for synthesizing a high-purity spiro quaternary ammonium tetrafluoroborate. The method comprises the following steps: step 1, adding a carbonate, 1,4-dichlorobutane, tetrahydro pyrrole, sodium iodide and a methanol solvent into a reaction kettle to perform reaction, so as to obtain a chloro spiro quaternary ammonium salt; step 2, dissolving the chloro spiro quaternary ammonium salt into ethanol in a reaction kettle, then adding sodium hydroxide to perform ion exchange, and evaporating the solvent to finally obtain a spiro quaternary ammonium base; and step 3, dissolving the spiro quaternary ammonium base into deionized water in a reaction kettle, then adding fluorboric acid for neutralization, then adding active carbon for refluxing decoloring, and then performing pumping filtration, evaporation condensation and drying, so as to finally obtain the high-purity spiro quaternary ammonium tetrafluoroborate with extremely low water content. The step 1 also can be performed as following: adding the raw materials into a ball milling tank for ball milling reaction, so as to obtain the chloro spiro quaternary ammonium salt. The provided synthetic method for the spiro quaternary ammonium tetrafluoroborate is relatively suitable for industrial large-scale production.

The invention discloses a cationic type gemini fluorinated surfactant based on perfluorinated nonene and perfluorinated hexene and a preparation method of the cationic type gemini fluorinated surfactant. The preparation method comprises the following steps of: with the perfluorinated nonene or perfluorinated hexene as a raw material, condensing the perfluorinated nonene or perfluorinated hexene with p-hydroxybenzoic acid, and carrying out chlorination on a matter obtained after condensation and thionyl chloride to prepare perfluorinated alkene oxyl benzoyl chloride; condensing the perfluorinated alkene oxyl benzoyl chloride without separation with 2-dimethylamino ethanol, 3-dimethylamino propanol, 2-dimethylamino ethylamine and 3-dimethylamino propylamine to obtain perfluorinated alkene oxyl benzoate or perfluorinated alkene oxyl benzamide with tertiary amine at an alkanol part or amine part; and finally, condensing the perfluorinated alkene oxyl benzoate or perfluorinated alkene oxyl benzamide with 1,2-dihaloethane, 1,3-dihalopropane, 1,4-dichlorobutane, 1,5-dichloropentane or 3-oxa-1,5-dichloropentane to prepare a quaternary ammonium gemini fluorinated surfactant. The synthesized compound is high in surface activity and is low in critical micelle concentration, has the characteristics of simpleness in synthesization, low cost and the like and has good application prospect.

The invention relates to an aramid fiber surface grafting modification method, belonging to the field of aramid fiber modification field and aiming at solving the problems of low aramid fiber surface activity and poor bonding property with a resin matrix. The aramid fiber surface grafting modification method comprises the steps of carrying out fiber surface cleaning and drying, fiber surface chlorination and fiber surface ammonolysis reaction. High-energy gamma rays with strong penetrability are utilized to excite the activities of fiber surface functional groups and a grafting agent, namely 1,4-dichlorobutane, the grafting reaction is initiated on the fiber surface, and the damage to the fiber surface structure, caused by the other surface treatment methods, can be alleviated; and meanwhile, a sheath core structure of the aramid fiber can be improved by irradiation of the gamma rays, and the phenomenon of reduction of the strength of the aramid fiber after modification treatment is effectively avoided; the process is simple, the efficiency is high, the fiber handling capacity is controllable, and the method is suitable for large-scale industrial production.

A preparation method for 1, 4-butyldisulphonate is to use a 1, 4-dihalogenated butane as materials reacting with a sodium sulfite in an aqueous liquor for 10 to 20 hours under a temperature of 110 to 120 DEG C to generate the 1, 4-butyldisulphonate. The method can use a 1, 4-dibromobutane or a 1, 4-dichlorobutane as raw materials. The invention utilizes the 1, 4-dihalogenated butane and the sodium sulfite to prepare the 1, 4-butyldisulphonate, which is easily operated, does no harm to the environment and has a high yield and a low cost as the 1, 4-dichlorobutane is used as the raw materials.

The invention relates to a preparation method of a symmetric spiro-quaternary ammonium salt electrolyte. The preparation method comprises the following steps: with water as a reaction medium, subjecting ammonium salt and alkyl dihalide to normal pressure reflux reaction for 10-20 hours in the presence of an acid-binding agent, then concentrating the product until the mass of symmetric spiro-quaternary ammonium salt is 15-25% of that of a symmetric spiro-quaternary ammonium salt reaction liquid, and carrying out filtration and purification to obtain the symmetric spiro-quaternary ammonium salt electrolyte, wherein the ammonium salt is any one of ammonium fluoroborate, ammonium trifluoromethanesulfonate and ammonium difluoro(oxalate)borate; alkyl dihalide is any one of 1,4-dichlorobutane, 1,5-dichloropentane, 1,4-dibromobutane and 1,5-dibromopentane; the feed mole ratio of the ammonium salt to alkyl dihalide to the acid-binding agent is 1 to (2-2.2) to (2-2.3); at the beginning of the reaction, the concentration of the ammonium salt is less than or equal to 0.5mol/l. The preparation method has the advantages that the raw materials are cheap; the whole preparation process has high safety; the synthetic reaction is good in selectivity; the product has high yield and high purity; the preparation method is suitable for industrial production.

The invention discloses a synthetic method of 1,1,1,4,4,4-hexafluoro-2-butene, and the synthetic method comprises the steps of carrying out a reaction between hexachlorobutadiene and hydrogen fluoride in the presence of a catalyst to generate 1,1,1,4,4,4-hexafluoro-2,3-dichlorobutane, and carrying out a reductive dechlorination reaction on the 1,1,1,4,4,4-hexafluoro-2,3-dichlorobutane in a solvent by using zinc powder to generate the 1,1,1,4,4,4-hexafluoro-2-butene. According to the synthetic method, the process is simple, the steps are short, the reaction conditions are mild and the product can be obtained through two steps of reaction; and the raw materials are easy to get, the cost is low, and the byproduct hexachlorobutadiene obtained by reducing tetrachloroethylene by carbon tetrachloride at high temperature can be used as a raw material, so that the cost is further reduced.

The invention provides a water-based electrolyte of a super capacitor. The raw materials of the water-based electrolyte include deionized water, a neutral inorganic electrolyte salt, a low-temperature additive and a voltage-resistant additive, wherein the low-temperature additive is an organic alcohol type compound and the volume of the low-temperature additive accounts for 5%-40% of the total volume of the electrolyte, the voltage-resistant additive is at least one of epoxy chloropropane cross-linked intermediate, dichlorobutane cross-linked intermediate, tetramethyldiaminopropane D-13, vanillic aldehyde, benzaldehyde and polyoxyethylene aliphatic alcohol ether, the neutral inorganic electrolyte salt is at least one of Li2SO4.H2O, NH4Cl, NaCl, KCl, (NH4)2SO4, NH4NO3, NaNO3 and KNO3, and the concentration of the neutral inorganic electrolyte salt in the electrolyte is 0.5-3mol/L. The water-based electrolyte of the super capacitor is capable of improving the low temperature property and the working voltage of the super capacitor and advantageous for improving the mass specific capacity of the super capacitor.

A method for modifying aramid fiber with a silane coupling agent, the method comprises four steps of cleaning and drying the fiber surface, chlorination reaction on the fiber surface, hydroxylation reaction on the fiber surface and grafting silane coupling agent reaction on the fiber surface. The invention adopts gamma ray high-energy irradiation to treat aramid fibers, and uses 1,4-dichlorobutane as a grafting agent to irradiate aramid fibers and 1,4-dichlorobutane to initiate grafting on the fiber surface reaction, introduce -Cl functional group, and then use NaOH solution to carry out hydroxylation treatment, convert -Cl to -OH, introduce -OH on the surface of the fiber, and finally react the hydroxylated aramid fiber with the aminosilane coupling agent KH550 to activate Fiber surface, improve fiber interface performance. The process of the invention is simple and efficient, the fibers can be processed in batches, the reaction solvent can be reused many times, the invention is green and environmentally friendly, and is suitable for large-scale industrial production.

The invention discloses a preparation method of spiro quaternary ammonium tetrafluoroborate. The method comprises steps as follows: (1) an acetonitrile solvent, carbonate, a bromine catalyst, pyrrolidine and 1,4-dichlorobutane are added to a reaction kettle to have a reaction, and a chlorinated spiro quaternary ammonium salt solution is obtained; potassium tetrafluoroborate is added to an acetonitrile solution of chlorinated spiro quaternary ammonium salt, the mixture has a reaction and then is subjected to ion exchange and filtration, carbonate is added to a filtrate, the mixture is stirred, filtered and subjected to reduced-pressure distillation, and a crude spiro quaternary ammonium tetrafluoroborate product is obtained; (2) high-purity spiro quaternary ammonium tetrafluoroborate is obtained with a series of purification methods such as extraction, reduced-pressure distillation, recrystallization, drying and the like. The yield and the purity of spiro quaternary ammonium tetrafluoroborate prepared with the method are relatively high, the content of halide ions and water is low, and spiro quaternary ammonium tetrafluoroborate has the remarkable performance advantage when used as a supercapacitor electrolyte.

The invention discloses a MOF-Cd probe for detecting Fe3+ and antibiotic ceftriaxone sodium in water, a preparation method and application thereof. The preparation method comprises the following steps: preparation of ligand bbi: fetching 0.05-0.1 moL of imidazole and 0.05-0.1moL of sodium hydroxide; dissolving the imidazole and the sodium hydroxide in DMSO for reacting for 2h at 60 degrees; then weighing 0.025-0.5moL of 1,4-dichlorobutane; adding the 1,4-dichlorobutane into the solution for multiple times; subjecting the solution to a sustained reaction for 2-3h; pouring the solution into a beaker containing 500 mL of ice water; performing still standing overnight; obtaining a large amount of white needle-like products; performing suction filtration to obtain white products, drying the white products for standby application; fetching and placing 20-40 mg of bbi, 20-40 mg of phenylenediacetic acid, 0.0494-0.1g of Cd(NO3)2 in DMA; stirring; dissolving and placing the mixture in a polytetrafluoroethylene liner; subjecting to a reaction for 40-48h at 80 degrees; and obtaining colorless transparent single crystals, which is the MOF-Cd probe. An analyte can be detected in water, and theeffect of detection is still not affected under different pH conditions and interference of other metal ions and antibiotics.

The invention relates to a one-pot high-yield producing method for tetrahydrothiophene. The method includes adding 164-205 kg of anhydrous sodium sulfide having a content of 60%, 480-800 kg of a solvent and 3.2-9.6 kg of a phase transfer catalyst into an enamel reactor having a volume of 1500 L, heating under stirring, maintaining the reaction temperature to be 50-100 DEG C, adding dropwise 160 kg of 1,4-dichlorobutane into the reactor, maintaining the temperature for 3-6 h after the addition is finished, heating to 115-122 DEG C, and performing atmospheric distillation by adopting an enamel filler column to obtain a tetrahydrothiophene high-quality product. The purity of the product of the method can be 99%, and the yield is higher than 95%. The method is high in product yield and purity, low in environment pollution, low in cost and suitable for industrial production.

The invention relates to the fine chemical engineering field and in particular relates to method for producing a medical intermediate tetraethyl orthocarbonate with coproduction of 5-chlorovaleronitrile. The method comprises the steps of reacting trichloroacetonitrile with sodium ethoxide in absolute ethyl alcohol to obtain the ethyl alcohol solution of the tetraethyl orthocarbonate, and separating out a solid salt sodium chloride and sodium cyanide, evaporating out 70%-75% of absolute ethyl alcohol and then adding water, stirring and standing to split phases, introducing the organic phase to a rectifying tower for rectification, pouring the water phase into a reaction device, and adding 1,4-dichlorobutane and a catalyst for reacting. The method has the advantages that the 5-chlorovaleronitrile is produced while the tetraethyl orthocarbonate is produced, more than 99% of sodium cyanide is utilized and consumed, and as a result, the production efficiency is improved, and the technical problem that the cyanides in the wastewater are difficult to dispose when the tetraethyl orthocarbonate is produced is solved successfully; the method is simple to operate; after being treated, the wastewater is low in toxicity, so that the cost and danger of wastewater treatment are greatly reduced; as a result, the method is especially applicable to industrial production and has tremendous social and economic benefits.

The invention particularly relates to an amine phosphate binder bixalomer intermediate and a preparation method thereof. The preparation method comprises the following steps: reacting a raw material 3,3'-diamidodipropyl amine under the action of benzyl chloroformate to obtain 3,3'-dibenzyloxyamidodipropyl amine, carrying out substitution reaction on the 3,3'-dibenzyloxyamidodipropyl amine and 1,4-dibromobutane or 1,4-dichlorobutane to obtain N,N,N',N'-tetra(3-dibenzyloxyamido)-1,4-butanediamine, and carrying out deprotection by pressure hydrogenation under the action of Pd-C to obtain N,N,N',N'-tetra(3-aminopropyl)-1,4-butanediamine. The method has the advantages of cheap and accessible raw materials, operable reaction, high yield and fewer three wastes, and thus, has excellent industrial prospects.

The invention belongs to the fields of organic and medicine synthesis, and discloses deuterated d8 aripiprazole as well as a preparation method and application thereof. According to the preparation method, 1,4-dichlorobutane-d8 serving as a raw material is subjected to four-step reaction synthesis to obtain deuterated mark d8-aripiprazole. According to the preparation method provided by the invention, the whole process is reasonable in design, high in operability and simple in operation, a deuterated reagent is low in cost, the product is easy to separate and purify, the obtained target product is stable in chemical property, the isotopic abundance is high, the yield is high and the purity can reach to 100 percent. The preparation method provided by the invention can be used for producinga deuterated internal standard substance which is used during analysis and detection of the deuterated aripiprazole, and a test sample can be provided for research on aripiprazole metabolic mechanism,so that the metabolic process and the action mechanism of the aripiprazole in a human body can be known more accurately and conveniently; and the deuterated d8 aripiprazole can be used for preparinga pharmaceutical composition, is applied to a dopamine system stabilizer for treating schizophrenia, schizoaffective psychosis and other psychotic disorders, and has important application value.

The invention relates to a production method of capacitor-grade 2,7-dibutyl octanedioic acid. The method comprises the steps as follows: diester malonate and chlorobutane as raw materials are subjected to alkylation reaction under the action of alkali with a phase transfer catalysis method, and diester butylmalonate is obtained; then, diester butylmalonate and 1,4-dichlorobutane are subjected to alkylation reaction under the action of alkali, 2,7-dibutyl-2,7-dialkoxycarbonyl octanedioic acid diester is obtained and subjected to saponification, acidolysis and decarboxylation reactions, and 2,7-dibutyl octanedioic acid is obtained. According to the method, the speed of the phase transfer catalysis alkylation reaction is high, and reaction time is short; reaction conditions are mild, few byproducts are produced, and no 'three wastes' is emitted. The method is simple in process, high in product yield and low in cost, and industrial production is facilitated.

The invention relates to preparation of organic alkalis of medical and chemical raw materials, particularly to a N-methylpyrrolidine preparation method, which comprises: a) under the catalysis of potassium iodide, carrying out a mixed reaction on 1,4-dichlorobutane and methylamine aqueous solution in an ether solvent to obtain N-methylpyrrolidine, wherein the ether solvent can form a hydrogen bondwith methylamine, and the boiling point of the ether solvent is greater than the azeotropic point of methylamine and water in the mixed system. According to the invention, the preparation method hasadvantages of abundant raw material sources and simple synthesis process route, and does not require high-pressure reaction conditions so as to achieve advantages of equipment investment reducing, production management simplifying, comprehensive cost reducing, excellent economical efficiency and wide popularization prospect compared with the high-pressure method; and the experimental results showthat with the application of the method to prepare N-methylpyrrolidine, the preparation yield is larger than 88%, and the product purity is larger than 99%.

The invention relates to synthesis and application methods of a halogen-free and formaldehyde-emission-free cotton permanent flame retardant of a nitrogen-phosphorus collaboration system. The synthesis method is characterized by comprising the following steps of (1), putting N,N-methylene bisacrylamide into a four-mouth flask, heating, melting, then putting dimethyl methylphosphate, meanwhile, adding a catalyst dibutyltin dilaurate or sodium methoxide, raising a temperature to 75 to 80 DEG C while agitating, carrying out heat preservation, reacting for approximately 2 to 3 hours, and cooling to a room temperature to obtain an intermediate A; (2), putting the obtained intermediate A into the four-mouth flask, adding an aqueous solution, firstly regulating pH (potential of Hydrogen) to be between 8 and 9 by using triethanolamine, raising the temperature of a reaction solution to 85 to 90 DEG C, slowly dropwise adding 1,4-dichlorobutane while agitating, carrying out the heat preservation,and reacting for 2 to 3 hours, so that a final product B can be obtained. The halogen-free and formaldehyde-emission-free cotton permanent flame retardant has the characteristics of being simple in process, high in flame retarding efficiency and a few in the influence on the strength and the hand feeling of a textile.

The invention discloses a method for simultaneously preparing 5-chlorovaleryl chloride and adipoyl chloride by using a one-pot method. Using 1,4-dichlorobutane as a raw material, sodium cyanide is gradually added dropwise into a reaction kettle in the presence of a phase transfer catalyst 1,4-dichlorobutane solution of 5-chlorovaleronitrile and adiponitrile; the obtained organic phase is separated from the aqueous phase, and hydrolyzed to generate 5-chlorovaleric acid and adipic acid 1,4-di Chlorobutane solution; the obtained ammonium chloride solid is added with water to dissolve completely, and the aqueous phase is separated; the 1,4 dichlorobutane solution of the obtained 5-chlorovaleric acid and adipic acid is added to sulfur oxychloride to carry out acid chloride reaction, Obtain the 1,4-dichlorobutane solution of 5-chlorovaleryl chloride and adipoyl chloride; the 1,4-dichlorobutane solution of the above-obtained 5-chlorovaleryl chloride and adipoyl chloride is dropped into a vacuum distillation column Adipoyl chloride products with a distillate temperature of 105-107°C are distilled out of the kettle. The present invention uses 1,4-dichlorobutane as a raw material, adopts "one-pot method" to simultaneously produce two intermediate products of 5-chlorovaleryl chloride and adipoyl chloride, the method has high yield, large single-pot production capacity, and solvent circulation Small amount, low energy consumption, less "three wastes".