81results about How to "The amount of three wastes is less" patented technology

The invention discloses a preparation method for tenofovir disoproxil fumarate, which comprises the following steps of: A, performing condensation reaction adenine and (R)-propylene carbonate which serve as raw materials to generate (R)-9-(2-hydroxypropyl) adenine; B, performing condensation reaction on the (R)-9-(2-hydroxypropyl) adenine and p-methylphenyl mesyloxy diethyl phosphonate under the catalysis of potassium alcoholate to prepare (R)-9-[2-(diethyl phosphonyl methoxy) propyl] adenine; C, reacting the (R)-9-[2-(diethyl phosphonyl methoxy) propyl] adenine obtained by the step B with para-toluenesulfonate acyl chloride to protect an amino group at bit four to prepare (R)-4-(p-toluenesulfonyl)-9-[2-(diethyl phosphonyl methoxy) propyl] adenine; D, hydrolyzing the (R)-4-(p-toluenesulfonyl)-9-[2-(diethyl phosphonyl methoxy) propyl] adenine obtained by the step C under a strong acid condition to obtain (R)-4-(p-toluenesulfonyl)-9-[2-(dihydroxy phosphonyl methoxy) propyl] adenine; and E, reacting the (R)-4-(p-toluenesulfonyl)-9-[2-(dihydroxy phosphonyl methoxy) propyl] adenine obtained by the step D with mercapto-benzene under a weak alkaline condition to remove a para-toluenesulfonate group to obtain the tenofovir. The invention aims to provide the preparation method for the tenofovir, which is low in cost, safe in process and good in product quality, and is suitable for industrialization.

The invention discloses a preparation method of 2,5-dichlorophenol and relates to the technical field of pesticide intermediate synthesis. The preparation method comprises the following steps: with p-dichlorobenzene as a start raw material, performing a Friedel-Crafts acylation reaction between the p-dichlorobenzene and acetyl chloride in the presence of aluminum trichloride to obtain 2,5-dichloroacetophenone; performing a Baeyer-Villiger oxidation reaction between the 2,5-dichloroacetophenone and a peroxide in the presence of a catalyst at room temperature to obtain 2,5-dichlorobenzene acetate; and performing a hydrolysis reaction between the 2,5-dichlorobenzene acetate and inorganic aqueous alkali in a reflux condition to obtain 2,5-dichlorophenol. The preparation method disclosed by the invention has the characteristics of simple synthesis process, short line, low production cost and high yield; and moreover, with less quantity of generated three wastes and high environmental protection property, the preparation method is more suitable for large-scale industrial production.

The invention provides a method for preparing aromatic amine by using mixed nitrochlorobenzene as a raw material. The method comprises the steps that: mixed nitrochlorobenzene is subjected to ammonolysis, deamination stripping, cooling crystallization, and centrifugal separation, such that a material comprising mixed nitroanilide is obtained; the material can be subjected to catalytic hydrogenation in an alcohol solvent, and p-phenylenediamine and o-phenylenediamine products can be prepared through separation; or before catalytic hydrogenation, part of p-nitroanilide is separated; and hydrogenation is carried out, such that p-phenylenediamine and o-phenylenediamine products can be prepared. According to the aromatic amine preparation method, the mixed nitrochlorobenzene raw material can be used in phenylenediamine production without separation, such that a product material separation process of a traditional production process is simplified, and energy consumption during production process is reduced. The method is economical and highly efficient, and the product has high purity.

The invention discloses a post-treatment method of an enzymatic hydrolysate of L-glufosinate-ammonium. The enzymatic hydrolysate of L-glufosinate-ammonium prepared by a biological enzyme resolution method is treated by four steps of pretreatment, extraction, desalination and crystallization; impurities such as unreacted D-glufosinate-ammonium derivatives, generated organic acids, ammonium salts and sodium salts are removed, and L-glufosinase of which the yield is greater than 98%, the content is greater than 98%, and the ee value is greater than 99% is obtained. According to the method, a traditional cation exchange resin passing mode is replaced with an extraction mode so that the method is simpler, more convenient and feasible, the purification efficiency is high, the extraction agent can be recycled, and the yield of three wastes is greatly reduced.

The invention provides a preparation method of a tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant. Bisphenol S used as a raw material and chloropropene undergo a substitution reaction to obtain a bisphenol S diallyl ether intermediate, and the bisphenol S diallyl ether and liquid bromine undergo addition and substitution reactions to obtain tetrabromobisphenol S bis(2,3-dibromopropyl ether). One-time bromination is adopted to introduce all eight bromine atoms into an aromatic ring and a side chain at the same time, so that the process route is shortened, the operation is simple, the safety is high, and the production cost is low. A solvent can be recycled in the process of preparing the bisphenol S diallyl ether intermediate, and the output of three wastes is greatly reduced, so the pollution to the environment is reduced, and the production cost is saved. The tetrabromobisphenol S bis(2,3-dibromopropyl ether) flame retardant prepared in the invention has high productpurity and improved application quality.

The invention discloses an L-carnitine production process which comprises the raw materials: epichlorohydrin, water, a catalyst, trimethylamine hydrochloride, a 30% sodium cyanide solution, a 30% hydrochloric acid solution and a 20% ammonia water solution. The L-carnitine production process has the following beneficial effects that the raw material epichlorohydrin is firstly split, by-products can be sold, and the reaction yield is high; the product is low in total cost and easy to refine, and an epichlorohydrin synthesis method of a route of splitting, quaternary ammoniation and cyaniding is selected; the production process has the advantages of short synthesis route, high yield, high resource utilization rate, low cost and small three-waste generation amount, ammonia water and hydrochloric acid are used for reacting to adjust the pH value, and excessive alkaline substances are prevented; impurities such as epichlorohydrin, hydrogen chloride, ethanol and isopropanol are injected into water generated by drying, so that pollution caused by leakage is prevented, the generation of wastewater is reduced; and when the temperature is raised to 90 DEG C for centrifugal desalting, a part of heat is provided, so that the heat is recycled.

The invention provides a method for producing bifenthrin with a clean synthesizing process. According to the method, 3-(2-chloro-3,3,3-trifluoro-1-allyl)-2,2-dimethylcyclopropane formyl halide and 2-methyl-3-biphenylmethanol are adopted to directly react in one solvent or mixed solvent of more than two solvents in favor of overflow of halogen hydride, halogen hydride generated in the reaction is removed from tail gas in time by means of negative pressure, and the product is directly cooled and crystallized to obtain bifenthrin. The reaction equation is as shown in a formula (3), wherein X is Cl or Br. The production method has the characteristics of high product content, simple process flow, small output of the 'Three Wastes' and the like, and accords with the requirement for clean production.

The invention relates to the technical field of resource regeneration and recycling, and particularly discloses a treatment process of a ship tail gas denitration waste catalyst. The process mainly comprises the following steps of pretreatment of the ship tail gas denitration waste catalyst, titanium recovery, vanadium recovery and tungsten recovery. By adopting the process to treat the ship tailgas denitration waste catalyst, high-added-value sodium titanate, ammonium metavanadate and sodium tungstate can be efficiently enriched and recovered. Meanwhile, the whole process of the treatment process is a closed cycle, so that the resource waste is avoided, and the utilization rate of resources is improved; and the treatment process is small in three-waste generation amount theoretically, sothat the pollution to the environment is reduced, and the process is a clean recovery process.

The invention discloses a process for preparing a tauroursodeoxycholic acid hydrate, which comprises the steps of reacting chenodeoxycholic acid with acyl chloride compound to obtain chenodeoxycholic acid mixed anhydride in an anhydrous organic solvent with ketone groups and in presence of an acid scavenger; reacting the chenodeoxycholic acid mixed anhydride with igepon with water under an alkaling condition to obtain taurine chenodeoxycholic acid; reacting the taurine chenodeoxycholic acid with an oxidizing agent in presence of water under an alkaling condition to obtain taurine-7-ketone group gallstone acid; leading hydrogen into the taurine-7- ketone group gallstone acid under the condition of chiral catalyst and alkalinity and maintaining a certain pressure and temperature for a hydrogenation reduction reaction to obtain the tauroursodeoxycholic acid; mingling the tauroursodeoxycholic acid with the mixed organic solvent to obtain the tauroursodeoxycholic acid hydrate. The tauroursodeoxycholic acid hydrate has the advantages of being low in cost, safe in process, good in production quality, and applicable to industrialization.

The invention relates to a production method of 1,3-butanediol, in particular to a production process for synthesizing 1,3-butanediol by using propylene and formaldehyde as starting raw materials, andbelongs to the technical field of chemical engineering. The process is characterized in that formaldehyde and the propylene are used as the starting raw materials; prins condensation reaction is performed under the effect of solid acid catalysts; then, the product and methanol are subjected to dehydration reaction to prepare the 1,3-butanediol. The process has the advantages that the raw materialresources are sufficient; the process is suitable for large-scale continuous production; the environment-friendly effect is achieved; three wastes (waste water, waste air and waste solid) are almostnot generated; the comprehensive production cost is low.

The invention discloses a new method for preparing bensulfuron. The preparation method comprises the following steps of: reacting o-methyl formate benzene benzyl sulfamide and ethyl chloroformate in a dried organic solvent to obtain o-methyl formate benzene benzyl sulfamide ethyl formate; and then adding 2-amino-4, 6-dimethoxy pyrimidine and a few amount of catalyst to obtain the bensulfuron. According to the invention, the ethyl chloroformate is used as the amide agent to control the reaction temperature and the speed of dropping the ethyl chloroformate, so that the ethyl chloroformate is reacted with the o-methyl formate benzene benzyl sulfamide in the dried organic solvent to obtain the o-methyl formate benzene benzyl sulfamide ethyl formate; then the o-methyl formate benzene benzyl sulfamide ethyl formate is further reacted with 2-amino-4, 6-dimethoxy pyrimidine under the action of the catalyst to obtain bensulfuron; and the purity of bensulfuron is greater than or equal to 95%. With the adoption of the ethyl chloroformate as the raw material, the preparation method of bensulfuron provided by the invention has the advantages of high output, high producing safety, low cost, and small producing amount of the three wastes compared with the traditional isocyanate method and sodium cyanate method.

The invention relates to the technical field of chemical synthesis and in particular relates to a method for co-producing and preparing methylthio acetate and diethyl thioglycolate by taking methionine as a raw material. The method for co-producing and preparing the methylthio acetate and the diethyl thioglycolate, provided by the invention, takes the methionine and haloacetic acid as raw materials to prepare three chemical products including homoserine lactone hydrohalide (IV), the methylthio acetate (I) and the diethyl thioglycolate (III) at the same time; all the products are easy to separate and purify.

The invention provides a method for preparing 3-methyl-4-aminobenzoic acid through catalytic hydrogenation, belonging to the technical field of chemical synthesis. The method comprises the following steps: adding 3-methyl-4-nitrobenzoic acid and a solvent into a reaction vessel so as to obtain a 3-methyl-4-nitrobenzoic acid solution, and adjusting the pH value of the solution to be alkaline; pouring the obtained alkaline aqueous solution into an autoclave, adding a catalyst, respectively carrying out replacement with nitrogen and hydrogen for three times, introducing ammonia gas for 2 minutes, carrying out pressurizing with hydrogen to 3.45 MPa to 4.50 MPa, and carrying out a reaction under the pressure of 4.50 to 2.50 MPa at 100 to 160 DEG C so as to obtain a reaction solution; and subjecting the reaction solution to post-processing so as to obtain the 3-methyl-4-aminobenzoic acid. The method provided by the invention has the advantages of easily-available raw materials, simple operation, low production amount of three wastes, environmental friendliness, capability of reaching a mole yield up to 90%, and more applicability to industrial production.

The invention discloses an ultra-pure methane chloride production system which comprises a reaction system for producing methane chloride by a methanol gas-phase hydrochlorination dry method and a carbon tetrachloride conversion reaction system. The two systems are sequentially connected with a sulfuric acid drying system and a methane chloride rectification system to obtain a methane chloride finished product; the sulfuric acid drying system is further connected with a compressor, and a gas outlet of the compressor is connected with a top gas outlet of the methane chloride rectification system to be mixed into a reaction system for producing methane chloride from crude methane chloride to methane chloride through a gas-phase thermal chlorination method. With a reaction system for producing methane chloride through the methane chloride gas phase thermal chlorination method, obtained mixed gas obtained after methane chloride and chlorine react sequentially enters a steam generation system, a chiller III, a condensation separation system, a dehydrogenation system, a dichloromethane refining system, a trichloromethane refining system and a carbon tetrachloride refining system. The system provided by the invention realizes full-process coupling energy conservation, energy conservation and emission reduction, the condition of single product proportion is changed, and free adjustmentof the proportion of the whole series of products and composite dehydration of the whole system are realized.

The invention provides a method for preparing an octabromo-S ether flame retardant. The method uses bisphenol S as a raw material to obtain a bisphenol S diallyl ether intermediate through a substitution reaction with allyl chloride, and bisphenol S Diallyl ether and liquid bromine undergo addition and substitution reactions to obtain octabromo-S ether. The preparation method of the invention adopts one-time bromination, simultaneously introduces all eight bromine atoms into the aromatic ring and the side chain, shortens the process route, has simple operation, high safety and low production cost. In the preparation method of the present invention, in the process of preparing the bisphenol S diallyl ether intermediate, the solvent can be recycled and used, the production of three wastes is greatly reduced, the pollution to the environment is reduced, and the production cost is saved at the same time. The octabromo-S ether flame retardant product prepared by the invention has high purity and improves its application quality.

The invention belongs to the field of medicine synthesis, and relates to a preparation method of an amiodarone hydrochloride intermittent. The method is characterized by including the following stepsthat 1, under an alkaline condition, in the presence of a phase transfer catalyst, a compound 1 and a compound 2 are subjected to nucleophilic substitution reaction to obtain a compound 3; 2, under analkaline condition, the compound 3 is hydrolyzed to generate a compound 4; 3, the compound 4 is subjected to intramolecular aldol condensation, decarboxylation and dehydration to obtain a compound 5;4, a compound 6 and thionyl chloride are subjected to heating reaction to obtain a compound 7; 5, under the presence of lewis acid, the compound 5 and the compound 7 are subjected to friede-crafts acylation reaction to obtain a compound 8; 6, under the presence of lewis acid, the compound 8 is subjected to demethylation to generate a compound 9, namely the amiodarone hydrochloride intermittent 2-butyl-3-(4-hydroxybenzoyl)benzofuran. The preparation method of the amiodarone hydrochloride intermittent has the advantages of being short in reaction time, high in product purity and high in yield,and the amiodarone hydrochloride intermittent is suitable for large-scale industrial production.

The invention provides an intermediate compound, carbamazepine and a derivative thereof as well as a preparation method of oxcarbazepine and a derivative thereof. 2-substituted aminophenylacetate or 2-substituted aminophenylacetonitrile and 2-halobenzonitrile are used as raw materials, substitution reaction, intramolecular condensation reaction, hydrolysis and hydrochloric acid acidification are carried out to obtain the oxcarbazepine and the derivative 5-substituent-10-oxa-10, 11-dihydro-5H-dibenzo [b, f] aza thereof, and the derivative of the oxcarbazepine can be used as a raw material to prepare the carbamazepine and the derivative 5-substituted iminostilbene thereof, an intermediate compound iminostilbene and intermediate compounds 5-substituted-10-methoxyiminostilbene and 10-methoxyiminostilbene. The raw materials used in the method are cheap and easy to obtain, and the cost is low; the preparation method is simple, conditions are easy to realize, the method is simple, convenientand safe to operate, and the process flow is short; the production amount of three wastes is small, and thus, the method is environmentally friendly; and a target product has high yield and purity, and is suitable for industrial production.