904 results about "Chloromethane" patented technology

The invention relates to the technical field of dispersing agents for ceramics, and discloses a preparation method of a dispersing agent for ceramics, and the novel dispersing agent for ceramics is prepared by taking methoxypolyethylene glycol, bromoacetyl bromide, 4-hydroxyphthalic anhydride, 2, 4, 6-diethanolamine amino-1, 3, 5-s-triazine and the like as raw materials. The polyether polyol contains a plurality of carboxyl groups, has strong interaction with the surface of ceramic powder such as aluminum oxide, has a star-shaped multi-arm polyether molecular chain, can well coat the aluminum oxide powder, can effectively inhibit the growth of crystal nucleus particle size of the aluminum oxide powder, reduces the particle size of the aluminum oxide, and avoids agglomeration and sedimentation of the aluminum oxide; the modified aluminum oxide ceramic powder has good activation degree in solvents such as water, ethanol, dichloromethane or N, N-dimethylformamide and the like, is lower in settling volume and shows excellent dispersing performance.

The invention belongs to the technical field of new materials, and discloses a polyolefin dissolving agent as well as a preparation method and application thereof. The cleaning agent is composed of modified long-carbon-chain imidazole dinitrile amine salt, modified long-carbon-chain imidazole long-carbon-chain anion salt, betaine salt, imidazole acetate, imidazole long-carbon-chain anion salt, quaternary ammonium long-carbon-chain anion salt, imidazole bis (fluorosulfonyl) imide salt, imidazole hexafluorophosphate and long-carbon-chain anion and cation liquid. Under the condition of 180-210 DEG C, polyolefin (PP or PE) with the molecular weight of 50-8 million can be dissolved by adopting the polyolefin dissolving agent disclosed by the invention, and effective extrusion can be realized by adopting a twin-screw extruder after dissolution. After PP / PE powder is dissolved by adopting the polyolefin dissolving agent disclosed by the invention, sheet casting or spinning is carried out, casting sheets or PP / PE fibers are washed by using ethanol / dichloromethane / hydrocarbon / tetrachloroethylene to remove ionic liquid, and a polyolefin diaphragm or polyolefin fibers can be prepared.

The invention relates to the technical field of waste gas purification and separation, in particular to a dichloromethane waste gas purification and recovery system which is mainly characterized in that a first auxiliary mechanism and a second auxiliary mechanism are arranged in a pretreatment device main body and are matched for use, so that good pretreatment work is carried out on purification treatment work of waste gas; the positive effect on improving the working efficiency of the purification treatment system is achieved; a rotating control motor in the first auxiliary mechanism drives a storage connecting cylinder to rotate, the storage connecting cylinder drives a fan-shaped plate body arranged on the side wall of the storage connecting cylinder and an impurity removal cotton swab in the second auxiliary mechanism to rotate, and impurity particles in waste gas are adsorbed and filtered in the process; the influence of solid pollutants such as impurity particles on subsequent treatment work is avoided as much as possible; the solid pollutants such as impurity particles can be separated from the waste gas, meanwhile, the stable operation of the subsequent purification treatment work can be ensured, and the device has a positive effect on improving the purification and recovery work benefits.

The invention discloses a self-assembling emulsifier, comprising emulsifier A, emulsifier B and emulsifier C; the mass ratio thereof is (0.05-3):(0.05-1):(0.05-3); emulsifier A comprises at least one of PPG-24-glycerol polyether-24, PPG-decyl tetradecanol polyether-24, and di(PPG-2 myristyl alcohol polyether-10) adipate; emulsifier B comprises at least one of polyquaternium-52, polyquaternium-61, polyquaternium-74, and polyquaternium-37; emulsifier C comprises at least one of PEG-40 hydrogenated castor oil, PEG-80 sorbitan laurate, PPG-5-cetyl alcohol polyether-20, coconut alcohol polyether-7, and PPG-1-PEG-9 lauryl glycol ether. The invention also discloses glabridin liposomes prepared by the self-assembling emulsifier. The self-assembling emulsifier of the invention can self-assemble and emulsify glabridin to form colorless or slightly yellowish clear and transparent glabridin liposomes with uniform particle size and good hydrophilicity; and the preparation process is simple, avoiding the addition of organic solvents such as methanol, ethanol, and chloroform.

The invention relates to the technical field of repair materials, and particularly discloses an extracellular matrix fiber material as well as a preparation method and application thereof. The invention discloses a preparation method of an extracellular matrix fiber material. The preparation method comprises the following steps: taking animal tissues, and carrying out virus inactivation, decellularization and antigen removal, degreasing, drying, grinding and sterilization; the decellularization and antigen removal method comprises the following specific steps: sequentially soaking a sample with a surfactant solution for h; then, soaking treatment is carried out by adopting a salt-alkali solution which contains 0.05-3 mol / L of salt and has the pH value of 8-11; then carrying out soaking treatment by adopting a 0.1-1wt% enzyme solution; and in degreasing, one or more of normal hexane, trichloromethane, dichloromethane, methanol, ethanol, acetone, diethyl ether and ethyl acetate are used for soaking the sample. According to the technical scheme, the ECM powder particle material with high growth factor content is prepared.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for determining a residual solvent in LXH-2103 by headspace gas chromatography. The determination method comprises the following steps: preparing a blank solution, a reference substance solution and a sample solution, respectively injecting the blank solution, the reference substance solution and the sample solution into a headspace for balancing, injecting the solutions into a gas chromatograph in a headspace sample injection manner, recording a chromatogram, and calculating the content according to a peak area by an external standard method; the residual solvent is absolute methanol, absolute ethyl alcohol, isopropanol, dichloromethane and methylbenzene. The method for determining the residual solvents in the LXH-2103 by using the headspace gas chromatography, provided by the invention, is high in sensitivity, good in repeatability and high in accuracy, and can be used for simultaneously detecting various residual solvents in the LXH-2103, so that the quality of the LXH-2103 is ensured, and the safety of clinical medication is improved.

The present invention relates to a method for determining the resin content and fiber surface density content of a prepreg, wherein a mixed solvent of dichloromethane and N-methylpyrrolidone is added to the prepreg sample to be tested after shearing treatment, and after 4 ultrasonic treatments, the resin matrix can be effectively dissolved and the fiber can be separated and obtained; the weights before and after the experiment are weighed respectively, and the resin content and fiber surface density content of the prepreg can be determined. The method of the present invention can achieve effective decomposition of resin and fiber, reduce bonding phenomenon in the fiber after cleaning, no white precipitate is seen, fiber loss is reduced, and the stability and accuracy of determining the resin content and fiber surface density content are higher. Compared with the existing method, the number of cleaning times and the amount of solvent used are significantly reduced, the work efficiency is significantly improved, and the processing cost is significantly reduced.

The invention discloses a fluopyram preparation method, which comprises: S1, carrying out a heating reaction on 2-vinyl-3-chloro-5-trifluoromethylpyridine, ammonia water, a catalyst and a solvent, carrying out reduced pressure distillation after the heating reaction to recover the solvent so as to obtain a residue, and adding dichloromethane and triethylamine to the residue so as to obtain a reaction liquid; and S2, dropwise adding o-trifluoromethyl benzoyl chloride into the reaction liquid in an ice bath, then removing the ice bath, stirring at the room temperature, adding water into the reaction liquid obtained in the step S1, extracting an organic layer, drying with anhydrous magnesium sulfate, recovering the solvent under reduced pressure, and performing vacuum drying to obtain the fluopyram. The method has the advantages of high reaction yield, high product purity, recyclable and reusable solvent, simple and mild production process, and suitableness for mass production.

The invention relates to a covalent organic framework / ionic liquid composite material and a preparation method and application thereof.The preparation method comprises the steps that firstly, through quaternization, part of chlorine atoms of polyether rubber are replaced with ionic liquid groups to prepare polyionic liquid, then part of remaining chlorine atoms on the polyionic liquid are replaced with sulfydryl, and then an alkenyl-containing COFs material is synthesized; and finally, dissolving the sulfydryl-containing polyionic liquid in trichloromethane, stirring, adding the alkenyl-containing COFs material and azodiisobutyronitrile, refluxing and stirring for 60 hours at 72 DEG C under the protection of nitrogen, cooling to room temperature, and centrifuging, washing and vacuum-drying the product to obtain orange powder, namely the covalent organic framework / ionic liquid composite material. The composite material is filled to prepare PT-SPE for simultaneous extraction of four bisphenol substances, the sensitivity of a solid-phase extraction method is greatly improved, the detection limit is as low as 0.06-0.40 ng / L, and the speed and convenience of the solid-phase extraction method are greatly improved.

The invention discloses a headspace gas chromatography detection method for simultaneously determining multiple residual solvents in pharmaceutical adjuvant hydroxypropyl methylcellulose. The headspace gas chromatography detection method comprises the following steps: preparing a reference solution containing the residual solvents; preparing a test solution of hydroxypropyl methylcellulose; respectively injecting the reference solution and the test solution into a headspace gas chromatograph for testing, and calculating the content of each residual solvent by peak area according to an external standard method; through accurate control of gas chromatography conditions, the method can accurately, rapidly and simultaneously detect the contents of residual methanol, isopropanol, dichloromethane, trichloromethane, benzene, trichloroethylene, dioxane and toluene in the pharmaceutical adjuvant hydroxypropyl methylcellulose, and has the advantages of simplicity and convenience in operation, high accuracy and sensitivity, good reproducibility and the like.

The invention discloses a resourceful treatment method for mother liquor in a glycine production process. The method comprises the following steps: introducing hydrogen chloride gas into mother liquor in a glycine production process to obtain hydrolysate; centrifugally separating the hydrolysate to obtain an ammonium chloride product, and treating the primary centrifugal filtrate in the next process; adding urea into the centrifugal filtrate for reaction, and after the reaction is completed, carrying out centrifugal separation to obtain a solid product urea-formaldehyde resin and a secondary centrifugal filtrate; the secondary centrifugal filtrate is heated, methyl alcohol in the filtrate is removed, methyl chloride is recycled, then heating continues, water in the filtrate is removed, evaporation condensate water is obtained, methyl chloride can be collected to serve as a by-product to be sold, the evaporation condensate water is reused for glycine production, and evaporation residual liquid serves as organic matter fertilizer to be treated. Under the condition of low energy consumption, impurities such as urotropin, ammonium chloride and methanol ammonia in the glycine mother liquor are separated, and resources such as urotropin, ammonium chloride and methanol in the mother liquor are recycled.

The invention belongs to the technical field of surface enhanced Raman spectroscopy, and particularly relates to a high-activity surface enhanced Raman scattering substrate as well as a preparation method and application thereof. Comprising the following steps: by utilizing a three-phase liquid-liquid interface self-assembly method, adding dichloromethane into an AuNPs dispersion liquid, uniformly mixing, adding a halide salt solution, uniformly mixing to form a mixed solution, then adding normal hexane into the mixed solution, standing, performing interface self-assembly until a gold nano-film is formed on a liquid surface, fishing out the gold nano-film, and drying to obtain the gold nano-film. The high-activity surface enhanced Raman scattering substrate is obtained. According to the method, the halide salt solution is innovatively introduced in the self-assembly process of the AuNPs, so that the assembly arrangement mode of the AuNPs is remarkably changed, the AuNPs are arranged more tightly, local surface plasma resonance coupling is enhanced, more hot spot areas are generated in a unit area, and the sensitivity of the self-assembly nano array SERS substrate is effectively improved.

The invention discloses an analysis method for simultaneously detecting organochlorine pesticide and polychlorinated biphenyl, which comprises the following steps of: simultaneously extracting organochlorine pesticide and polychlorinated biphenyl in a water sample by adopting a mixed extraction solvent, dehydrating, concentrating and fixing the volume of extract liquor, separating and measuring by adopting a gas chromatography-mass spectrometry method, and quantifying by adopting an internal standard method. When the mixed extraction solvent is n-hexane / dichloromethane with the volume ratio of 9: 1 and 1% by mass of polyethylene glycol 4000 is added, the recovery rates of water samples with the measured concentrations of 5.00 ng / L, 20.0 ng / L, 40.0 ng / L and 80.0 ng / L are 83.6%-95.4%, 91.2%-105.6%, 93.5%-104.7% and 92.8%-106.9% respectively, the relative standard deviations are 6.1%-9.2%, 3.3%-8.2%, 3.2%-6.3% and 3.4%-7.5% respectively, compared with the prior art, the extraction efficiency is remarkably improved, and the method has the advantages that the method is simple, the cost is low, and the method is suitable for industrial production. The accuracy and precision of the method completely meet the determination and analysis requirements for measuring complex water samples.

The invention discloses a method for extracting nicotine-free tar from cigarette butts, which is applied to the field of cigarette butt recovery and comprises the following steps of: adding the cigarette butts into a 30L extraction kettle with a compression device, adding 6.32 kg of cigarette butts in total, adding ethanol, heating and extracting at 78 DEG C for three times, extracting for two hours at each time and 50.0 kg of ethanol in total, and concentrating an ethanol extracting solution to obtain 700.0 g of nicotine-containing tar with the extraction rate of 11% (in terms of cigarette butts). The method comprises the following steps: taking 429.9 g of nicotine-containing tar, adding 750ml of dichloromethane and 330ml of 1 equivalent diluted hydrochloric acid into the tar, stirring overnight at room temperature, adding dichloromethane into the solution, washing with water, and drying with anhydrous sodium sulfate to obtain 190.8 g of a nicotine-free tar product with the yield of 44.4% (metered by tar). According to the method, a feasible way is provided for recycling the effective components in the cigarette butts, after process parameters are further optimized, higher recycling efficiency and better economic benefits are achieved, meanwhile, pollution of the cigarette butts to the environment is reduced, and environmental protection is facilitated.

The invention relates to the technical field of trimethyl boron preparation, in particular to a high-purity trimethyl boron preparation method which comprises the following steps: S1, reaction raw material preparation: magnesium powder and methane chloride react to generate methylmagnesium chloride; reacting boron trifluoride with aluminum trichloride to generate boron trichloride; s2, taking methyl magnesium chloride and boron trichloride as raw materials, and carrying out dry reaction under the conditions that the pressure is 0-1.0 MPa and the temperature is 40-150 DEG C to generate crude trimethyl boron and magnesium chloride; s3, the crude trimethyl boron is subjected to condensation, adsorption and two-stage rectification in sequence, and a high-purity trimethyl boron product is obtained; and S4, magnesium chloride is electrolyzed to obtain magnesium powder and chlorine, and the magnesium powder and the chlorine are recycled. Compared with the prior art, the method has the advantages that the trimethyl boron is prepared by adopting the dry reaction, the reaction is more sufficient, the reaction efficiency is high, the crude trimethyl boron product is purified, the product purity is improved, in addition, the byproduct magnesium chloride can be recycled, and the resource waste is reduced.

The invention discloses an extraction method of silymarin. The extraction method of the silymarin comprises the steps of polar solvent treatment, acid solution treatment, alkaline solution treatment and purification. The polar solvent is selected from one or more of chloroform and dichloromethane, and the alkaline solution comprises one or more of sodium hydroxide and potassium hydroxide. The extraction method of the silymarin provided by the invention has the effects of reducing the extraction difficulty and cost of the silymarin.

A method for catalyzing selective oxidation of 5-hydroxymethylfurfural by ion-doped birnessite belongs to the field of chemical engineering, and comprises the following steps: adding an ion-doped birnessite type catalyst into a solvent, and catalyzing 5-hydroxymethylfurfural to prepare 2, 5-furandicarboxaldehyde and 2, 5-furandicarboxylic acid in the atmosphere of air or oxygen at the temperature of 25-240 DEG C, wherein the solvent is water, methanol, ethanol, acetonitrile, dichloromethane, N, N-dimethylformamide, N, N-dimethylacetamide and the like. The method is simple, few in by-products and environmentally friendly. By adopting ion-doped birnessite as the catalyst, the method has the advantages of economy, environmental protection, mild conditions, high selectivity, easiness in recovery of the catalyst and the like; the ion-doped birnessite catalyst can efficiently and highly selectively catalyze oxidation of 5-hydroxymethylfurfural to prepare 2, 5-furandicarboxaldehyde, catalytic materials are easy to separate, the production cost is low, and the ion-doped birnessite catalyst has remarkable technical and economic effects and application prospects.

The present invention relates to the technical field of eye drops, and specifically discloses a kind of wetting boric acid eye drops. The present invention also discloses a preparation method of the above-mentioned wetting boric acid eye drops, boric acid, chlorhexidine gluconate solution, and calcium disodium edetate are added to water, and stirred at 60-70°C to obtain a boric acid complex; sodium hyaluronate and sodium alginate are added to water and stirred, and hypromellose is added, and stirred at 30-40°C to obtain a hypromellose complex; soy lecithin, cholesterol, and ethylparaben are added to chloroform and stirred to obtain phase A; collagen and carboxymethyl chitosan are added to citric acid aqueous solution and stirred to obtain phase B; phase A is added to phase B under stirring, ultrasonic treatment, 50-60°C vacuum rotary evaporation to remove chloroform, citric acid aqueous solution is added for hydration, ultrasonic treatment, and filtration to obtain liposomes; boric acid complex, hypromellose complex, and liposomes are mixed evenly, and the pH value of the adjustment system is 6.5-7.5.

The invention discloses a method for determining antibiotics in environmental soil, which comprises the following steps: S1, collecting fresh soil, crushing, sieving with a 0.1 mm-0. 2mm sieve, weighing 3 g-5 g of sample, and placing in a centrifuge tube; s2, adding 50-80 mL of a methanol-acetic acid-aqueous solution into the centrifuge tube, oscillating for 3-5 min, then carrying out normal-temperature ultrasonic treatment for 25-30 min, carrying out high-speed centrifugation for 10-15 min at a low temperature of 4-6 DEG C, taking a supernatant, repeatedly extracting residues twice, merging the obtained extract and the supernatant, and concentrating to 10-15 mL to obtain a concentrated solution A; s3, adding 20-25 mL of dichloromethane into the concentrated solution, repeating the extraction operation in the S2 to obtain a concentrated solution B, and adding ultrapure water into the concentrated solution B to dilute the concentrated solution B to 200 mL; and S4, adding 1-1.5 g of disodium ethylene diamine tetraacetate into the diluent obtained in S3, adjusting the pH value to 3.5, enabling the diluent to pass through a small solid-phase extraction column, eluting the small solid-phase extraction column with methanol, blow-drying under nitrogen flow, fixing the volume, passing through a filter membrane, and transferring into a sample bottle for UPLC-MS / MS determination. According to the method, the antibiotic extraction rate and the content determination accuracy are improved.

The invention relates to the technical field of high polymer materials, in particular to a preparation method and application of ternary hydroxyalkyl cellulose ether for a sustained-release coating material.The preparation method comprises the steps that an alkali metal catalyst, purified water, polyhydric alcohol and cellulose are put into a high-pressure reaction kettle, heating and vacuumizing are conducted, firstly, chloromethane and epoxypropane are introduced for an etherification reaction for a certain time, and then the mixture is cooled to the room temperature; the ternary hydroxyalkyl cellulose ether is prepared by adding potassium hydroxide after cooling, vacuumizing, heating, introducing chloroethane, completing an etherification reaction, washing, drying, crushing and synthesizing, has hydrophilic and hydrophobic characteristics of different degrees, is applied to a film coating premix formula, and can be used for preparing a film coating premix. The prepared coating film has excellent properties of slow release, high salt resistance, high release stability and the like.

The invention discloses an organic silicon monomer synthesis material collecting and returning device and process. A gas phase outlet in the top of a fluidized bed is connected with an inlet of a secondary cyclone separator; a gas phase outlet of the second-stage cyclone separator is connected with an inlet of the third-stage cyclone separator, and a solid phase outlet of the second-stage cyclone separator is connected with a receiving hopper of the second-stage cyclone separator; a receiving hopper of the secondary cyclone separator is connected with inlets of the fine powder tank A and the fine powder tank B; silicon powder and chloromethane react in the fluidized bed, most of silicon powder is separated through a built-in cyclone separator and directly returns to the bed through a dipleg, other gas-solid mixtures enter a secondary cyclone to collect fine powder, the fine powder is alternately and continuously returned to the bed, and the efficiency of the secondary cyclone is adjustable. The reaction of the fluidized bed is stabilized, the automation level and intrinsic safety of the device are improved, and the labor intensity is greatly reduced.

The preparation method of the flavone enantiomer compound comprises the following steps: crushing epimedium sagittatum to prepare paste, suspending with water, extracting with petroleum ether, dichloromethane, ethyl acetate and n-butyl alcohol respectively to obtain extractum of each part, carrying out gradient elution separation by using silica gel column chromatography, and concentrating to obtain the flavone enantiomer compound extracted from epimedium sagittatum. Combining the similar parts according to a thin layer chromatography (TLC) color development result to obtain a plurality of polar segments; carrying out chromatography and gradient elution on the target polar section to obtain a plurality of components, and then combining the similar components through thin-layer chromatography (TLC) dot plate absorption to obtain a plurality of sub-components; a target component is eluted and purified, fractions with different retention times are collected and dried, and four compounds are obtained respectively, have a remarkable inhibition effect on the cell viability of human breast cancer cells MCF-7, have anti-breast cancer activity, can be applied to preparation of drugs for treating breast cancer, and have huge social and economic benefits.

The invention discloses a photo-thermal response self-healing coating and a preparation method thereof, and belongs to the technical field of anticorrosive coatings. The preparation method comprises the following steps: dissolving an EVA copolymer in trichloromethane, dropwise adding into an aqueous solution of lauryl sodium sulfate, and stirring until the trichloromethane is evaporated to obtain EVA microspheres; the preparation method comprises the following steps: dispersing MXene in water, and dispersing EVA microspheres in DMF (Dimethyl Formamide); mixing and stirring the two materials to obtain an MXene-coated EVA material; the preparation method comprises the following steps: mixing water-based resin, PPGDGE and a curing agent, adding an MXene-coated EVA material, coating, and curing to obtain the photo-thermal response self-healing coating. Under near-infrared radiation, the photo-thermal response self-healing coating can be rapidly heated, the shape memory process of a coating matrix is started, the EVA material is subjected to phase change to fill the damaged part of the coating, and the MXene nanosheet prolongs the permeation time of electrolyte, so that the coating has efficient damage healing capacity and an anti-corrosion effect.

The utility model relates to a thick edge drying system for a lithium battery diaphragm. The drying mechanism is used for secondarily drying the thick edge part of the diaphragm so as to dry the dichloromethane liquid carried by the thick edge part of the diaphragm; the air supply mechanism is connected with the drying mechanism and used for supplying hot air into the drying mechanism; and the exhaust mechanism is connected with the drying mechanism and is used for recovering dichloromethane gas generated by volatilization of the thick edge part of the diaphragm dried by the drying mechanism to a waste gas treatment system. According to the drying system, secondary heating can be carried out on the thick edge part of the diaphragm, dichloromethane gas is brought out, and the unorganized discharged dichloromethane gas is pumped away and fed into a waste gas treatment system, so that the purposes that operation is safe in the space, the product physical property and appearance qualification rate is increased, and energy consumption is reduced are achieved.

The invention relates to a synthesis method of room-temperature vulcanized methyl phenyl silicone rubber, and belongs to the field of preparation of high polymer materials. The preparation method comprises the following steps: adding alpha, omega-dihydroxy polydimethyldiphenylsiloxane with high phenyl content and low polymerization degree, dimethyl cyclosiloxane and an alkaline resin catalyst into a reaction kettle, stirring, heating and reacting; after the reaction is finished, removing low-boiling-point substances in vacuum to obtain room-temperature vulcanized methyl phenyl silicone rubber; the preparation method comprises the following steps: preparing D201 ion exchange resin (quaternary ammonium salt type), 1-allyl cyclopropanesulfonyl chloride, zinc chloride, bis (1-vinyl imidazole-2-) ketone, mercaptoethyl guanidine dihydrobromide, triethylamine and dichloromethane, so as to obtain guanidine-doped D201 ion exchange resin; loading guanidine-doped D201 ion exchange resin into an ion exchange column for transformation to obtain an alkaline resin catalyst; the room-temperature vulcanized methyl phenyl silicone rubber prepared by the invention has excellent mechanical properties.

The invention relates to the technical field of synthesis of chemical products, in particular to a synthesis method of acryloyloxyethyl trimethyl ammonium chloride. According to the method, a one-pot reaction system is adopted, ethyl acrylate and N, N-dimethylaminoethanol are taken as raw materials and are subjected to quaternization reaction with chloromethane under an alkaline condition, and efficient conversion is realized through the synergistic effect of a composite catalytic system and a polymerization inhibitor. The composite catalyst is constructed by compounding magnetic nanoparticles and a metal organic framework material, forms a multilevel structure through titanate crosslinking, and has high catalytic activity and magnetic separation and recovery characteristics. The method simplifies the traditional step-by-step process, has the advantages of simple and convenient one-pot operation, recyclable catalyst, high raw material utilization rate, environmental friendliness and the like, and is suitable for large-scale preparation of acryloyloxyethyl trimethyl ammonium chloride.

The invention belongs to the technical field of high polymer material detection, and discloses a quantitative detection method for potassium perfluorobutanesulfonate in a high polymer material and application of the quantitative detection method. According to the method, trichloromethane reflux extraction and methanol precipitation are adopted as pretreatment, and specific liquid chromatography-tandem mass spectrometry detection conditions are matched, so that excellent recovery rate and extremely low limit of quantitation are obtained, and the determination requirement of potassium perfluorobutanesulfonate in a high polymer material is met. In addition, the invention further provides a detection method for simultaneously detecting the content of the potassium perfluorobutanesulfonate and the content of the polytetrafluoroethylene in the high polymer material, the content of perfluorine in a sample is detected firstly, then the content of the potassium perfluorobutanesulfonate is detected by adopting the quantitative detection method, and the content of the polytetrafluoroethylene is calculated through the content of the potassium perfluorobutanesulfonate and the content of the polytetrafluoroethylene. The method provided by the invention is simple and easy to implement, high in accuracy and good in reproducibility.

The invention provides a method for detecting environmental pollutants by using a dispersive liquid-liquid microextraction technology. The method is particularly suitable for detecting endocrine disrupters in a urine sample. According to the method, a proper amount of a NaCl solution, a dispersing agent acetonitrile and an extracting agent trichloromethane are added into a urine sample, and target pollutants are rapidly extracted; and after centrifugation and nitrogen blowing drying, redissolving by using a methanol-water mixed solution in a ratio of 1: 1, and finally detecting and quantitatively analyzing through UHPLC (Ultra High Performance Liquid Chromatography). Compared with liquid-liquid extraction and solid-phase extraction, the method has the characteristics of simplicity and convenience in operation, high extraction efficiency and high detection sensitivity, is suitable for detecting bisphenol compounds in various matrixes, conforms to the green chemistry principle, and reduces the use amount of organic solvents. The method can be widely applied to detection and analysis of trace pollutants in environmental samples, and provides reliable technical support for environmental monitoring and pollutant risk assessment.

The invention is suitable for the technical field of organic synthesis, and provides a method for purifying crude polycarbonate diol containing a titanate catalyst, which comprises the following steps: selecting dichloromethane, trichloromethane, tetrahydrofuran or ethyl acetate solvent, and dissolving the crude product according to the mass ratio of crude product PCDL to organic solvent to pure water of 1: (1-10): (1-10) under the condition of jacket hot water heating. Carrying out pressure filtration through high-purity nitrogen, separating filtrate from filter residues, standing and layering the filtrate, and respectively collecting an organic phase and a water phase; and secondly, transferring the organic phase to a concentration kettle, adjusting the temperature and the vacuum degree, recovering and recycling the organic solvent, and finally obtaining a qualified polycarbonate diol product. According to the method, the residual titanate catalyst in the polycarbonate diol product is effectively removed through an innovative purification process, and the production of the high-purity product is realized.

The invention discloses a crystal compound, a preparation method thereof and application of the crystal compound in X-ray detection, imaging and anti-counterfeiting encryption, and belongs to the technical field of crystals. The molecular formula of the crystal compound is [Cu (totp) (CH3CN) 3] [Cu2I3 (totp) (PN)]. (CH3CN), wherein totp is tris (o-tolyl) phosphine; and PN is diphenyl-2-pyridine phosphine. The crystal compound disclosed by the invention is simple in preparation method, and has the characteristics of large mass attenuation coefficient of X-ray energy, high light yield and low detection limit when being used as a material of an X-ray detector. The compound also has the characteristic of structural transformation in solvents such as methanol, ethanol, acetone, dichloromethane, tetrahydrofuran and the like, and meanwhile, the conversion of luminescence color under the excitation of 365nm ultraviolet light and X rays is accompanied. The material can be applied to the aspects of scintillator materials, room-temperature X-ray radiation indirect detection materials, radiation detection dosimeters, X-ray scintillator medical imaging, anti-counterfeiting encryption and the like.