71 results about "Di-n-butylamine" patented technology

The invention discloses a method for synthesizing SAPO-41 (Silico-Alumino-Phosphate-41) molecular sieve by adopting a novel template agent, relates to a synthesis method of the silico-alumino-phosphate molecular sieve, in particular relates to a synthesis method of the silico-alumino-phosphate molecular sieve SAPO-41, and solves the problems that the method for synthesizing the SAPO-41 molecular sieve by using a conventional DPA (Di-n-Propylamine) as the template agent is high in preparation cost, has mixed crystal and is not beneficial for the realization of large-scale industrial production. The method comprises the following steps: firstly, preparing 85 percent by mass of phosphoric acid, pseudo-boehmite, di-n-butylamine, silica sol and distilled water into initial gel; and secondly, crystallizing, cooling to the room temperature, centrifuging, washing, drying, roasting and naturally cooling the initial gel to the room temperature so as to obtain the SAPO-41 molecular sieve. The method has the advantages that firstly, the product is in pure phase; secondly, the synthesis cost of the molecular sieve is greatly reduced; and thirdly, the large-scale industrial production is realized. The method is mainly used for synthesizing the SAPO-41 molecular sieve.

The invention discloses a high-yield high-purity DAST source powder synthetic process. The synthetic process comprises the following two steps: 1, reacting 4-methylpyridine with methyl p-toluenesulfonate in the presence of absolute ethyl alcohol serving as a solvent to obtain an absolute ethyl alcohol solution of 4-methyl-N-methylpyridine tosilate; and 2, reacting 4-methyl-N-methylpyridine tosilate with p-dimethylaminobenzaldehyde in the presence of absolute ethyl alcohol serving as a solvent and under the catalytic action of di-n-butylamine or piperidine, so as to obtain high-yield (85-95%) high-quality (90-95%) DAST source powder. According to the synthetic process, absolute ethyl alcohol is used as a reaction solvent, harm of poisonous and harmful solvents such as methylbenzene and methyl alcohol to the body of an operator can be avoided and the pollution of waste liquid to the environment can be avoided. The research success of the high-yield high-purity DAST source powder synthetic process is beneficial to culture of high-quality large-sized DAST crystal, thereby laying a good material and theoretical basis for research on the DAST crystal and related products.

The invention provides a preparation process for synthesizing tetrabutyl urea by using di-n-butylamine and carbonyl chloride as major materials in an alkaline organic solvent by means of phosgenation synthesis, wherein the process comprises the following steps: (1) adding di-n-butylamine, carbonyl chloride and organic solvent to a reactor in certain proportion; (2) adjusting the temperature of acylation reaction and controlling the reaction time to obtain crude tetrabutyl urea; (3) standing, separating, distilling and purifying the crude tetrabutyl urea to obtain a final product of tetrabutyl urea. The preparation method provided by the invention is simple in procedure, the raw materials are cheap and easily available, the product is good in quality, the reaction yield is over 90%, and the purity is more than 99%.

The invention provides a method for determining the content of mono-ester aconitum alkaloids in an ephedra-aconitum carmichaelii-liquorice preparation. According to the method, high performance liquid chromatography is used for determining the content of mono-ester aconitum alkaloids, a chromatographic column taking polar ether connected phenyl bonded silica gel as filler, and acetonitrile and 0.05-0.2% phosphoric acid solution which are in a ratio of (19:81)-(25:75) are taken as flowing phases, wherein the phosphoric acid solution comprises 0.02%-0.06% of triethylamine and 0.01-0.03% of di-n-butylamine, the detection wavelength is 222-242nm, the number of theoretical plates is not lower than 6000 if calculated by benzoyl mesaconine peak. The separation degree of target components, peak forms and tailing factors are all improved greatly, and moreover, the specificity, linearity, accuracy, precision and durability are all good.

The invention provides a preparation method of dialkyldithiocarbamate. The preparation method includes following steps: mixing sodium hydroxide, water, di-n-butylamine, alcohol, dichloromethane and carbon disulfide for reaction to obtain a reaction product; adopting solvent oil to extract the reaction product, and separating to obtain an oil phase; mixing the oil phase with a supporter, and filtering to obtain mother liquid; performing depressurizing distillation on the mother liquid to obtain distilled mother liquid; adopting the solvent oil to extract the distilled mother liquid, and performing depressurizing distillation to obtain dialkyldithiocarbamate. The preparation method prepares dialkyldithiocarbamate through a one-step process, the objective of no washing with water is achieved through two times of extraction through the solvent oil, two times of depressurizing distillation and treatment by adopting the supporter before a time of depressurizing distillation, so that generation of wastewater is reduced, and high product yield and product purity are realized. Experiment results show that yield of dialkyldithiocarbamate is higher than 99%, and purity is higher than 98%.

The invention discloses a preparation method for sulfur-containing carbofuran derivative with less than 0.1% of harmful impurity carbofuran. The preparation method comprises the following steps of: using di-n-butylamine or N-isopropyl-beta-alanine ethyl ester derivative and sulfur monochloride as raw materials to prepare into disulphide in the presence of an acid-binding agent triethylamine and an organic solvent 1, 2-dichloroethane; and then reacting with a chlorinating agent sulfuryl chloride to obtain nitrogen sulfur chlorine; and finally reacting with carbofuran under the effect of a cosolvent N-methyl-2-pyrrolidone or dimethylformamide so as to obtain the sulfur-containing carbofuran derivative with not less than 96% of quality percentage composition and less than 0.1% of main harmful impurity carbofuran. By adopting the preparation method, the problem that the carbofuran cannot be completely reacted during being reacted can be solved, the defects due to low content and low yield of sulfur-containing carbofuran derivatives such as benfuracarb and carbosulfan caused by a solid-liquid two-phase reaction can be avoided, the technical problem due to relatively high content of main harmful impurity carbofuran can be solved, and the content of the sulfur-containing carbofuran derivatives such as benfuracarb and carbosulfan can reach a value not less than 96%, and the yield is 97 to 98%, and the main harmful carbofuran in the product is less than or equal to 0.1%, so that the preparation method has a wide popularization and application prospect.

The invention relates to the field of polyurethane and particularly relates to a method for preparing a photo-crosslinking polyurethane film. The method comprises the following steps: adding 24.5g of isophorone diisocyanate and 4 droplets of catalyst into a 250ml four-mouthed bottle, adding 57.1g of polyether polyol into a dropping funnel, carrying out dropwise adding, carrying out a reaction for 1 to 1.5 hours while controlling the temperature to 40 DEG C to 50 DEG C, measuring NCO content by a di-n-butylamine method, adding 3.75g of 2,2-bishydroxymethyl propionate after the NCO content meets requirements, carrying out a reaction for 2 to 3 hours at the reaction temperature of 60 DEG C to 70 DEG C, dropwise adding 3.47g of hydroxyl-2-ethyl methacrylate and a polymerization inhibitor when the NCO content is approximate to a theoretical value, heating the temperature to 70 DEG C, carrying out a reaction for 3 to 4 hours, carrying out sampling, carrying out infrared detection, and obtaining a polyurethane prepolymer when characteristic peaks of an NCO group disappear; loading the prepolymer into a four-mouthed flask, adding triethylamine into the four-mouthed flask according to the mole ratio of 1: 1 in a dropwise adding manner, and carrying out a neutralization reaction for 0.5 to 1 hour at the temperature of 50 DEG C, thereby obtaining a composite nano-emulsion. According to the method, the operation is simple, the operation is convenient, the comprehensive performance of the product is good, and the method is efficient, energy-saving, environmentally friendly, safe and sanitary.

The invention discloses a method for synthesizing a heteroatom substituted MeAPO-31 molecular sieve by microwave heating, relating to a preparation method of a MeAPO-31 molecular sieve. The invention aims to solve the technical problems that the traditional method for preparing the MeAPO-31 molecular sieve has long crystallization time, easy generation of mixed crystals in products, limited type and quantity of the heteroatom introduced into a frameworkd, the narrow adjustable range of the produced acid sites and the like. The method comprises the following steps of: firstly, preparing gel byusing phosphoric acid, water, di-n-butylamine, aluminum isopropoxide (or boehmite) and metal salt; heating with microwaves; and crystallizing, then centrifugally filtering, washing, drying and roasting to obtain the MeAPO-31 molecular sieve. Compared with the traditional hydrothermal process, the method disclosed in the invention obviously shortens the crystallization time of the molecular sieve and does not generate mixed crystals. The MeAPO-31 molecular sieve prepared with the method can be used as catalysts in the fields of petrochemical industry, fine chemical industry and the like.

A poly(2,6-dimethyl-1,4-phenylene ether) prepared using a morpholine-containing polymerization catalyst has a monomodal molecular weight distribution with a reduced content of very high molecular weight species. It also exhibits increased morpholine incorporation in the high molecular weight fraction. Compared to commercially available poly(2,6-dimethyl-1,4-phenylene ether) prepared using a di-n-butylamine-containing polymerization catalyst, the poly(2,6-dimethyl-1,4-phenylene ether) of the invention exhibits reduced odor. Compared to other poly(2,6-dimethyl-1,4-phenylene ether) prepared using a morpholine-containing polymerization catalyst, the poly(2,6-dimethyl-1,4-phenylene ether) of the invention exhibits improved molecular weight build during compounding and improved compatibilization with polyamides.

The invention relates to s preparation method of a fosamprenavir derivative, which comprises the following steps: reacting a compound disclosed as Formula II or ammonium salt thereof with a metallic ion source in a solvent to obtain a compound disclosed as Formula III, separating or purifying, and carrying out catalytic reduction on the compound disclosed as Formula III to obtain a compound disclosed as Formula I, wherein X is a metallic ion, the metallic ion source is preferably a calcium ion source, sodium ion source or potassium ion source, and X is preferably a calcium ion, sodium ion or potassium ion; the solvent is methanol, ethanol, n-propanol, isopropanol, n-butanol or sec-butanol; the catalytic reduction is carried out by using palladium-on-carbon as a catalyst and hydrogen as a reducer; and the ammonium salt is a monomethyl amine salt, dimethyl amine salt, monoethyl amine salt, diethylamine salt, isopropylamine salt, di-n-butylamine salt, dipropyl amine salt, tert-butylamine salt or dicyclohexyl amine salt. The invention also provides a related intermediate of the preparation method of the fosamprenavir derivative. The preparation method of the fosamprenavir derivative saves the cost, enhances the yield, and is suitable for large-scale popularization.