2177 results about "Chloromethane" patented technology

The invention relates to cationic asphalt emulsifier and preparation method and application thereof. The main agent of the cationic asphalt emulsifier is prepared through the reaction of quaternarization reagent and intermediate at molar ratio of 0.5-3:1, wherein the intermediate is produced in the reaction of organic acid mixture and organic amine at molar ratio of 1: 1-3. The adjuvant agent of the cationic asphalt emulsifier is the combination of, based on the main agent by weight, 0.1-2.5% of nonionic surfactant and 0.1-2.5% of modifier. The organic acid mixture is the mixture of linear, branched or naphthene-containing organic acid with small relative pace steric effect and organic acid with big relative space steric effect at molar ratio of 1: 3- 3: 1. The quaternarization reagent is epichlorohydrin, hydrochloric acid, chloromethane, dimethyl sulfate or chloroacetic acid. The modifier is one or more of aluminum sulfate, ammonium chloride and calcium chloride and the nonionic surfactant is fatty alcohol-polyoxyethylene ether. The emulsifier has no bad effects to the property of the asphalt, has wide application range and can satisfy different construction conditions.

The invention relates to a preparation method of herbicide dicamba. The preparation method includes: (1) liquid potassium hydroxide and 2, 5-dichlorophenol are reacted according to molar ratio of 0.95:1-1:1 to obtain 2, 5-dichlorophenol potassium; (2) at the presence of anhydrous potassium carbonate and catalyst, the 2, 5-dichlorophenol potassium obtained in the step (1) is reacted with CO2 to generate 3, 6-dichlorosalicylic acid, pressure of CO2 is controlled to be 4-6MPa, reaction temperature ranges from 100 DEG C to 160 DEG C, and molar ratio of anhydrous potassium carbonate and 2, 5-dichlorophenol potassium is 1-2:1; and (3) in alkaline condition, at the temperature of 70-100 DEG C, the 3, 6-dichlorosalicylic acid obtained in the step (2) and chloromethane are reacted under the action of the catalyst through a tube fixed-bed reactor according to molar ratio 1:1-3.5, saponification and acidification are performed to obtain 3, 6-dichloro-2-methoxysalicylic acid, namely the dicamba. The process is high in reaction yield, simple in reaction condition, good in product quality, small in three wastes and low in energy consumption.

The invention relates to a method for measuring alkaloid in tobacco and tobacco products, which is characterized by dissociating alkaloid from the tobacco and tobacco products by using sodium hydroxide solution, extracting the alkaloid from samples by using triethylamine/trichloromethane solution, and detecting content of five kinds of alkaloid with GC-MS ( Gas Chromatograph-Mass Spectrum) quantitative analysis. Compared with other methods for analyzing the alkaloid, the invention has the advantages that alkaloid is separated from the tobacco by DB-35MS chromatographic columns so as to separate nornicotine and myosmine in the tobacco and accurately quantify target matters; batch sampling is carried out on the separation of nicotinamide and other alkaloid so as to detect the nicotinamide with high content in the tobacco and meet the quantitative analysis of other alkaloid with low content; the standard working curves of standard matters are separately compounded so as to avoid influence on quantization of other alkaloid by alkaloid catabolite existing in the standard samples. The method is simple and convenient and has the advantages of good repeatability, high analyzing and measuring sensitivity, and accurate quantization.

A process for recovering chloromethane from the tail gas exhausted in the procedure of preparing glyphosate by phosphorus acid-phytanic acid method is disclosed. As said tail gas contains chloromethane (20-90%) and impurities (methanol, methylal, H2O and hydrogen chloride), it uses solvent to absorb impurities, or condenses the impurities, or convents the impurities to chloromethane, so obtaininghigh-purity chloromethane.

The invention relates to a method for detecting multiple residual solvents in a medicament. According to the method, by utilizing a gas chromatographic method, nine organic solvents including methanol, ethanol, acetonitrile, acetone, isopropanol, methylene dichloride, ethyl acetate, tetrahydrofuran and triethylamine in the medicament are simultaneously detected, the sensitivity and the precision are high, and the repeatability is good; by utilizing a standard addition method, other standard substances do not need to serve as internal standard substances, only pure substances of to-be-measured components are needed, the accuracy requirement on the sampling volume is low, and the operation is simple; by utilizing a headspace sampling method, a direct solution sample is prevented from interfering the detection and polluting a chromatographic column; by utilizing a temperature programming method, low-boiling-point organic solvents and high-boiling-point organic solvents can be effectively separated.

The discharged exhaust gas during the glyphosate acid production process through phosphorous acid alkyl acid includes 20-90% of methyl chloride, methanol, formaldehyde dimethyl acetal, water, hydrogen chloride and other foreign matter, by solvent absorption of foreign matter, condensation impurity or charging part of the foreign matter such as methanol, formaldehyde dimethyl acetal into hydrochloride-containing liquid and converting it into methyl chloride, high purity of methyl chloride can be obtained. The process not only solves the problem of environmental pollution in the glyphosate acid production, the production cost can also be lowered substantially.

A monochloro-fluoropropene preparation belongs to the intermediate preparation technical field of coolant, foaming agent and fluorine compounds, which comprises that under catalyst condition, the telomeric reaction on chloromethane and chloroalkene is processed to prepare pentachloro-propane, which is fluorinated with hydrogen fluoride via the catalysis of composite catalyst to prepare trifluoro-dichloropropane, and hydrogen chloride is removed via the alkali alcohol liquid catalysis to obtain monochloro-fluoropropene as final product. The invention has the advantages that the preparation fluorinates pentachloro-propane into trifluoro-dichloropropane, to remove hydrogen chloride to obtain monochloro-fluoropropene, thereby avoiding azeotropic material and sub isomer generated in the fluorination from pentachloro-propane to monochloro-fluoropropene, while the whole process has low reaction temperature to save energy, and the monochloro-fluoropropene product has reach 99.0-99.6% purity and 80.70-88.05% yield, to meet industrial batch production.

In this invention, fatly acid and ethanolamine are proportioned and under ester-aminated, then reacting with dimethyl carbonate to produce ester-amine type quaternary ammonium salt. Said invention p rocess of synthesis has high transforming rate, excellent selectivity, high content of active matter in said product, utilizing no pollution type raw material of dimethyl carbonate, so, no remaining of poison in product, lowering quaternary ammonium salt pollution to environment and to human health.

The invention discloses a preparation method of citrate modified NaYF4:Yb,Er/Mn up-conversion luminescent nano material, a hydrogen peroxide or uric acid detection method and applications. The preparation method comprises the following steps: 1) stirring alkali, water, oleic acid, C1-C3 alcohol, a manganese source, a ytterbium source a yttrium source, an erbium source and NaF, and then carrying out hydrothermal reaction and centrifugal separation to obtain OA-NaYF4:Yb,Er/Mn UCNPs; and 2) dispersing OA-NaYF4:Yb, Er/Mn UCNPs in alcohol, and then carrying out ligand exchange reaction with a trichloromethane and citrate solution to obtain the citrate modified NaYF4:Yb,Er/Mn up-conversion luminescent nano material. The citrate modified NaYF4:Yb,Er/Mn up-conversion luminescent nano material has the advantages of low detection limit, high sensitivity and good selectivity to hydrogen peroxide or uric acid detection, so that the material can be used for detecting uric acid in serum.

The invention discloses a polyaniline nano-fiber electrode material for a super capacitor and a preparation method thereof, belonging to the field of electrochemistry and new energy material. The method is characterized by comprising the steps of: dissolving aniline and initiating agent into dichloromethane organic phase, dissolving oxidizing agent into inorganic acid dope additive water phase, carrying out interfacial polymerization at the temperature of 0-30 DEG C, and obtaining the polyaniline nano-fiber electrode material by separating liquid, washing and drying; wherein the volume ratio between the dichloromethane organic phase and the inorganic acid dope additive water phase is 1:1, the concentration range of the aniline is 0.02-1mol/L, the concentration range of the initiating agent is 0.02-0.002mol/L, and the molar ratio range between the aniline and the oxidizing agent is 1:1-8:1. The polyaniline nano-fiber is controllable in structure as well as good in one-dimensional directivity, electrical conductivity and electrochemical properties. The electrode material has the specific capacitance of 549Fg-1 and the advantage of simple preparing technique.

The discharged exhaust gas during the glyphosate acid production process through phosphorous acid alkyl acid includes 20-90% of methyl chloride, methanol, formaldehyde dimethyl acetal, water, hydrogen chloride and other foreign matter, by solvent absorption of foreign matter, condensation impurity or charging part of the foreign matter such as methanol, formaldehyde dimethyl acetal into hydrochloride-containing liquid and converting it into methyl chloride, high purity of methyl chloride can be obtained. The process not only solves the problem of environmental pollution in the glyphosate acid production, the production cost can also be lowered substantially.

A process for treating the rejected saline generated in preparing hydrazine hydrate from ammonia, sodium hypochlorite and acetone includes such steps as high-pressure and ¿Ctemp hydrolyzing of ketazine in rejected saline, using rectifying tower to collect resultant acetone and ammonia, adding sodium hypochlorite solution, redox reaction between resultant hydrazine hydrate and residual acetone and ammonia to generate sodium chloride, water, N2 and chloromethane, and stirring and blowing with compressed air to carry the gas products away. The removed impurities can be reclaimed.

A process for preparing dimethyl dichlorosilane from the high-boiling-point residue generated in synthesizing methyl chlorosilane includes filling catalyst in gas preheater, passing chloromethane (or hydrogen chloride) gas through it, carrying catalyst into reactor while introducing said residue to it, and separating dimethyl dichlorosilane from the cooled substance at tower top.

The invention relates to a water body, a method for rapidly detecting the residue of malachite green and colorless malachite green in an aquatic product, belonging to the technical field of residue detection in a water body and an aquatic product. The method comprises the following steps: oscillating and mixing a sample to be detected and an extractant I uniformly; adding an extractant II, oscillating and mixing and then standing still; taking and adding an supernatant to an enrichment column; observing color change of a chromogenic reagent on the lowest layer; and determining that the sample contains the malachite green and colorless malachite green if a green circular strap is formed. The extractant I is a mixed solution of acetonitrile, dichloromethane, n-hexane and paratoluenesulfonic acid, the extractant II is a mixture of lead dioxide and acid alumina, and the sample to be detected is a water body sample to be detected or an aquatic product sample to be detected. The invention has the advantages of simple operation and fewer steps, does not need expensive instruments and equipment and can embody the convenience and the flexibility to on-site detection.

The present invention relates to a new process for producing methane chloride by using liquid-phase catalytic method and pressurization process. The hydrogen chloride and methyl alcohol are mixed according to a certain ratio, then placed in a tank reactor with catalyst, and under the condition of a certain temp. and pressure the invented methane chloride can be synthesized. It adopts acid/water washing and alkali-washing processes to remove unreacted methyl alcohol and hydrogen chloride, and adopts concentrated sulfuric acid washing process to remove residual water content and reaction by-product dimethyl ether, then the purified and dried methane chloride gas is undergone the processes of compression and condensation so as to obtain high-purity liquid methane chloride product.

Disclosed is a method for separating a mixed gas of methyl chloride to recover methyl chloride, and the method at least has two absorption tower systems filled with adsorbents, and obtains the methyl chloride gas separated and removed of impurities from discharge ports of the absorption towers through temperature swing adsorption processes of both adsorption and desorption to the mixed gas containing methyl chloride in the absorption towers respectively by means of interlock of time sequence; the adsorbent is at least one of allochroic silicagel, active carbon, aluminum silicate salt zeolite molecular sieve or alumina zeolite molecular sieve; and the method adopts the dry separation and recovery of temperature swing adsorption, one set of apparatus can remove water, methanol, methylal, methyl oxide and air simultaneously, and the methyl chloride product is obtained relying on high purity and/or high rate of recovery, the flow is simple and operation costs are low; and the method can realize the zero discharge of waste sulfuric acid and waste desiccant and green and environment-friendly production compared with the traditional treatment method.

The invention discloses a method for separating a flavone compound from hericium erinaceus by applying a high-speed countercurrent chromatography. The method comprises the following steps: 1) subjecting hericium erinaceus fermented mycelia to extraction by adopting high-purity ethanol, then carrying out filtration, carrying out pressure-reducing concentration so as to recover ethanol, and carrying out extraction with petroleum ether and ethyl acetate so as to obtain a crude extract; 2) mixing chloroform, dichloromethane, methanol and water according to a volume ratio of 4: 2: 3: 2 so as to obtain a mixed solution used as a two-phase solvent system, and carrying out standing and stratifying, wherein the upper phase is used as a stationary phase, and the lower phase is used as a mobile phase; and 3) carrying out separation through the high-speed countercurrent chromatography so as to obtain the flavone compound. The method is simple and convenient, has good reproducibility, can be used for large-scale preparation of compounds, and lays a material foundation for further research on activity.

A method for synthesizing isosorbide dimethyl ether comprises the following steps: (1) adding solvent, isosorbide, alkali and phase transfer catalyst in a reaction vessel; (2) stirring and raising the temperature to 80 to 100 DEG C, reducing the pressure until the gauge pressure is minus 0.095 MPa, and dewatering; (3) leading into chloromethane under the condition of the phase transfer catalyst, and complete the etherification reaction with the pressure 0.1 to 1.0 MPa and the temperature 50 to 90 DEG C; (4) carrying out acid neutralization; (5) filtering and desalting; (6) and carrying out reduced pressure distillation, and collecting fraction with the temperature of 92 to 93 DEG C to get isosorbide dimethyl ether and recovering the solvent. The solvent adopts low molecular polyether with alkyl sealing the ends, in the formulae, R1 and R2 are hydrogen atoms or alkyl; the adopted alkyl comprises 1 to 15 carbon atoms; R3 and R4 are hydrogen atoms or methyl, or other lower alkyl; and m plus n is an integer between 4 to 15. The invention realizes zero discharge, reduces cost and increases production efficiency.

The invention relates to a method for refining a chlorine hydride byproduct and recovering trifluoromethane in production of monochlorodifluoromethane. Refined high-purity chlorine hydride can directly serve as a raw material for synthesizing vinyl chloride monomers; and the trifluoromethane byproduct separated in the refining process can be effectively recovered, wherein the refining of the HCl comprises the following steps of: crude separation, absorption, analysis, condensation, capture of acid mist, and adsorption; and after a F23 byproduct in the production of the monochlorodifluoromethane is separated in the absorption process in the refining of the HCl, the F23 byproduct is subjected to lossless compression and rectification to form the trifluoromethane with the purity of over 99 vol percent. By combining the recovery and comprehensive utilization of the HCl and the recovery of the trifluoromethane, the high consumption of water resources and liquid caustic soda is avoided, and the production cost of the monochlorodifluoromethane is reduced; and the effective recovery of the trifluoromethane prevents environmental pollution, and the chloroalkali, the monochlorodifluoromethane and polyvinyl chloride (PVC) can be circularly produced.

The invention belongs to the technical field of waste gas recovery and treatment, and relates to a dichloromethane waste gas treating method and a system thereof. The dichloromethane waste gas treating system comprises a dichloromethane waste gas inlet pipe, a pretreating system, a condensing system and a recovering system, wherein the pretreating system is formed by a condenser and a gas-to-gas heat exchanger connected with the condenser, the dichloromethane waste gas inlet pipe is connected with the condenser, a fan is arranged on a pipeline connecting the condenser with the gas-to-gas heat exchanger, and the condensing system is formed by two condensing towers including a primary condensing tower and a secondary condensing tower and capable of deeply condensing dichloromethane waste gas so as to enable the same to realize cooling crystallization. The invention further provides the dichloromethane waste gas treating method utilizing the dichloromethane waste gas treating system. The dichloromethane waste gas treating method is a cooling crystallization treating method and includes physical processes of cooling, crystallizing, resolving recovering and the like.

The invention discloses a synthesis and preparation method of fasudil hydrochloride, which comprises the steps of taking 5-isoquinoline sulfoacid as raw material, refluxing in thionyl chloride to obtain 5-isoquinoline sulfonyl chloride hydrochloride, adding dichloromethane after dissolving with ice water, adjusting pH value of the solution to be neutral and performing liquid eparation; washing organic phase with water and edible salt, drying and filtering to obtain dichloromethane solution of 5-isoquinoline sulfonyl chloride; performing reaction of the solution with high purity piperazine in the presence of other alkaline reagents, washing the reaction solution with hydrochloric acid aqueous solution and sodium hydroxide aqueous solution after reaction, and extracting the washing solution respectively with dichloromethane; combining organic phases, washing with water, drying and filtering, and dropwise adding saturated hydrogen chloride ethanol solution to separate out crude product of fasudil hydrochloride; and recrystalizing the crude product with ethanol aqueous solution to obtain fasudil hydrochloride. The method provided by the invention greatly reduces the usage amount of high purity piperazine that is expensive by using deacidifying agents that are low in cost so as to reduce the preparation cost of fasudil hydrochloride effectively.