2234 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 discloses a comprehensive method for synthesizing glufosinate and analogue thereof by using phosphorus trichloride, triethyl phosphate and chloromethane as initiative raw materials. The method comprises the following steps of: performing Grignard, disproportionation and coupling; introducing a proper amount of hydrogen halide; and synthesizing to obtain two intermediates, namely methyl diethyl phosphate (intermediate I) and methyl phosphinate (intermediate II), wherein the two intermediates can synthesize the glufosinate and the analogue thereof. By the method, the glufosinate and the analogue thereof are synthesized by completely utilizing the methyl diethyl phosphate and the methyl phosphinate synthesized by a Grignard route; yield is increased; production cost is reduced; and three wastes are reduced.

The invention relates to neutral mononuclear copper (I) complexes for emitting light and with a structure according to formula (A) in which: M represents: Cu(I); L∩L represents: a single, negatively charged, bidentate ligand; N∩N represents: a diimine ligand (substituted with R and FG), in particular a substituted 2,2′-bipyridine derivative (bpy) or a substituted 1,10-phenanthroline derivative (phen); R represents: at least one sterically demanding substituent for preventing the planarisation of the complex in the excited state; FG=functional group, and represents: at least one second substituent for increasing solubility in organic solvents. The substituent can also be used for electron transport or alternatively for hole transport, said functional group being bound to the diimine ligands either directly or by means of suitable bridges; and the copper (I) complex: having a ΔE(S1−T1) value of less than 2500 cm−1 between the lowest excited singlet state (S1) and the triplet state (T1) which lies below; having an emission lifespan of at most 20 μs; having an emission quantum yield of greater than 40%, and a solubility of at least 1 g / L in organic solvents, in particular polar organic hydrocarbons such as acetone, methyl ethyl ketone, benzene, toluene, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, dichloroethane, tetrachloroethylene, alcohols, acetonitrile or water.

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 describes a dust-cleaning technique using wetting method of organic chlorosiline gas. The synthetical gas from double cyclone enters inside from the bottom of washing tower, the discharged liquid from the kettle enters in flash pot, evaporated gas enters in flash condenser, non-condensing gas is entirely discharged after washed by washing tower, condensed liquid enters in liquid-recovery tank and residue is discharged into residual tank. The gas on the top enters in precooling device on top of the tower, after gas-phase is deeply cooled, non-condensing gas goes to chlorine methane buffering pot, condensed liquid enters in rough monomer medium pot, part of which returns to the tower and part of discharging is sent to rough monomer tower for processing.

A rechargeable lithium cell comprising a cathode, an anode, an optional ion-permeable membrane disposed between the anode and the cathode, a non-flammable salt-retained liquefied gas electrolyte in contact with the cathode and the anode, wherein the electrolyte contains a lithium salt dissolved in or mixed with a liquefied gas solvent having a lithium salt concentration greater than 1.0 M so that the electrolyte exhibits a vapor pressure less than 1 kPa when measured at 20° C., a vapor pressure less than 60% of the vapor pressure of the liquefied gas solvent alone, a flash point at least 20 degrees Celsius higher than a flash point of the liquefied gas solvent alone, a flash point higher than 150° C., or no flash point, wherein the liquefied gas solvent is selected from methane, fluoromethane, difluoromethane, chloromethane, dichloromethane, ethane, fluoroethane, difluoroethane, tetrafluoroethane, chloroethane, dichloroethane, tetrachloroethane, propane, fluoropropane, chloropropane, ethylene, fluoroethylene, chloroethylene, or a combination thereof.

The invention discloses a process method used for reducing the content of impurities in gas-phase hydrogen chloride after hydrolysis of dichlorodimethyl silane, comprising the steps as follows: a two-step device is used for separating the impurities; a vapour liquid separator leads the mixed hydrogen chloride gas generated after the hydrolysis of dichlorodimethyl silane to enter a washing tower of a guide structure so as to remove most of impurities; subsequently, the hydrogen chloride gas with most of impurities removed is arranged into the bottom of a demister; the adsorption medium at the internal layer of the demister is porous fiber which is used to adsorb the siloxane impurity in the hydrogen chloride gas; and the hydrogen chloride gas with the siloxane impurity removed is sent to a methyl chloride device to carry out the subsequent process. The method reduces the content of the impurities in the hydrogen chloride gas, improves the yield of hydrolysate of the dichlorodimethyl silane, keeps the pressure of the hydrogen chloride gas at a high level after purification, does not generate a great deal of waste acid, avoids the disposal of waste acid, and has low energy consumption and low equipment expense.

The present invention discloses a solution-processable organic molecule photovoltaic material based on two-dimensional conjugated benzodithiophene, a preparation method and an application thereof. According to the present invention, the molecules adopt thiophene substituted two-dimensional conjugated benzodithiophene as a core, both terminals are symmetrically connected with a thienylethene indene or bithienylethene indene conjugated structure unit, the structure formula is represented by a formula I, the molecules have good dissolubility in common organic solvents (such as dichloromethane, trichloromethane, tetrahydrofuran and the like), and the high-quality film can be prepared by using the solution method; compared with the polymer material, the material of the present invention is easy to purify, and the high purity material can be obtained; and the organic molecules are used for the donor material of organic solar cells, wherein the energy conversion efficiency is more than 6.5%. (Formula I).

The invention belongs to the technical field of acesulfame potassium production and relates to a recovery method of catalyst triethylamine in the acesulfame potassium production. A one-step one-kettle reaction is changed into a two-kettle three-step reaction, and the purpose of recovering triethylamine is achieved by the following steps: (1) preheating, and recovering methylene dichloride; (2) carrying out neutralization reaction; (3) reacting in an alkali separation kettle and dropwise adding sulfuric acid; (4) carrying out heat preservation and water distribution. Compared with a traditional method, the recovery method has the advantages that the recovery rate is greatly improved, the labor intensity of workers is reduced at the same time, and produced wastes also reach the environmental treatment standards.

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 synthesis method of dicamba, which comprises the following steps of: using 2, 5-dichlorophenol as raw materials, conducting sulfonation and bromination reaction to obtain 4-hydroxy-2, 5-dichloro-3-bromobenzenesulfonic acid, treating the 4-hydroxy-2, 5-dichloro-3-bromobenzenesulfonic acid by using alkyl metal complexes of magnesium or lithium, conducting electrophilic addition reaction with CO2 to obtain 5-sulfo-3, 6-diclorsalicylic acid, removing the sulfo of the 5-sulfo-3, 6-diclorsalicylic acid and conducting O-methylation reaction with methyl chloride to obtain the dicamba. The synthesis method of dicamba has the advantages that since the 2, 5-dichlorophenol is used as the raw materials, the raw materials for reaction are easy to obtain, the reaction process is environmental-friendly, the quality of the obtained product is high, the yield is high and the application value is greater.

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.

The invention discloses a preparation method of vinylidene fluoride and a preparation method of a catalyst used by the same. The preparation method of vinylidene fluoride comprises the following steps: mixing methane, oxygen and fluoroform or monochlorodifluoromethane or the mixed gas of fluoroform and monochlorodifluoromethane at any ratio or the mixed gas of multiple gases including fluoroform and monochlorodifluoromethane; adding O2 at a certain proportion, and reacting at a temperature of 550-1,050 DEG C under a total pressure of 1-10bar and at an air speed of 50-10,000h<-1>; and reacting in the presence of a catalyst to generate vinylidene fluoride. According to the method disclosed by the invention, the vinylidene fluoride with relatively high added value is generated under a catalytic action from several waste fluoroform raw materials which are cheap or need forced treatment, has relatively high added value, and brings good economic and social benefits.

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 invention belongs to the technical field of preparation of rare earth europium organic coordination compound and macromolecular polystyrene composite fibers by electrostatic spinning and relates to a method for preparing rare earth fluorescence micro / nano fibers, which comprises: placing europium oxide in an excessive amount of diluted hydrochloric acid to react the europium oxide with the excessive amount of diluted hydrochloric acid completely, allowing the excessive hydrochloric acid to volatilize to obtain europium chloride, reacting the europium chloride, acetylsalicylic acid and phenanthroline, which are in a mass ratio of 1:2.1:0.78, in ethanol in the presence of triethylamine serving as a complexing agent and catalyst, adjusting the pH value to make the chloride, acetylsalicylic acid and phenanthroline react completely, washing, filtering under vacuum and drying to obtain white powdery rare earth coordination compound; and dissolving the rare earth europium coordination compound and a macromolecular material in solution of tetrahydrofuran or trichloromethane respectively, mixing, and uniformly stirring to obtain solution of precursor, and performing electrostatic spinning to obtain micro / nano fibers having smooth appearance and strip structures. In the invention, the preparation process is simple, and the product has low cost, good fluorescence effect and high performance and can be widely used in fields of electrical, optical and chemical materials and the like.

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.

The invention relates to a novel catalyst for hydrotreating and dechlorinating high-level chloromethane as carbon tetrachloride to prepare low-level chloromethane. The catalyst uses one or several of palladium, platinum and nickel as active components, and uses at least two of zircite, titanium oxide and alumina as catalyst carrier. With said catalyst, the carbon tetrachloride is hydrotreated into chloroform which is mainly transferred into carrene, while the produced hydrochloride is reacted with carbinol to obtain methyl chloride.

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 preparation method of Cefozopran Hydrochloric acid, Cefozopran Hydrochloric acid powder for injection and preparation method thereof. The preparation method includes allowing 7-ACA as raw material and compound in the formula (II) to react in the presence of solvent such as dichloromethane, HMDS and TMSI, and post-treating to obtain compound in the formula (III); condensing with the compound in the formula (IV), post-treating to obtain the Cefozopran, salifying with hydrochloric acid to obtain product, centrifuging, water washing, and drying to obtain Cefozopran Hydrochloric acid crude product; and refining to obtain Cefozopran Hydrochloric acid refined product. The preparation method of the Cefozopran Hydrochloric acid provided by the invention has easily available raw material, high yield, and suitability for industrialized production. The Cefozopran Hydrochloric acid is mixed with anhydrous sodium carbonate and sodium chloride, and sub-packaged to obtain powder for injection having good stability. The obtained powder for injection can be used together with 5% glucose injection, and 0.9% sodium chloride injection.