83 results about "Methyl t-butyl ether" patented technology

The invention relates to the technical field of adhesives, and discloses an imidazolium ionic liquid and a preparation method and application thereof, the preparation method comprises the following steps: reacting omega-bromoalcohol with 1-(methoxymethyl) imidazole in acetonitrile, and washing with methyl tert-butyl ether to obtain a target ionic liquid precursor; and dissolving the product in acetonitrile, adding 4-trifluoromethyl phenyl isocyanate, and washing with methyl tert-butyl ether after the reaction is finished, thereby obtaining the target imidazolium ionic liquid. The imidazolium ionic liquid disclosed by the invention is applied to a PVB (Polyvinyl Butyral) adhesive, and the PVB adhesive shows excellent adhesion strength in a macroscopic adhesion performance test on the basis of multiple interactions, and particularly has excellent adhesion strength on aluminum. The obtained adhesive can be universally adapted to various substrates such as metal substrates and macromolecule substrates, and finally high-strength and high-durability intelligent adhesion performance is achieved.

The present application relates to the field of environmental protection additives, specifically disclosing a natural gas low-temperature combustion-supporting environmental protection additive and its preparation method. The natural gas low-temperature combustion-supporting environmental protection additive comprises the following substances in parts by weight: 10 to 50 parts of dimethyl carbonate, 0 to 10 parts of methyl tert-butyl ether, 10 to 20 parts of methanol, and 15 to 20 parts of dispersed catalytic particles; the dispersed catalytic particles are carbon aerogels adsorbed with nano-Pt particles. The natural gas low-temperature combustion-supporting environmental protection additive of the present application uses dimethyl carbonate, methyl tert-butyl ether, and methanol as liquid matrices, and a carbon aerogel material adsorbed with the precious metal Pt as a catalytic material. The environmental protection additive material is effectively coated and loaded in the boiling gas phase. A uniform bonding form is formed between the gas-phase environmental protection additive and the natural gas, so that the methane in the natural gas opens the gas-hydrogen-oxygen bond under the action of the environmental protection additive at 80 to 100°C, effectively catalyzing the combustion of natural gas in an oxygen-rich state, further improving the activity of natural gas in a low-temperature environment.

The invention belongs to the technical field of cables, and particularly relates to a weather-proof new energy automobile charging cable which is composed of a cable core, a shielding layer wrapping the cable core and a sheath layer wrapping the shielding layer. Each cable core is composed of a conductor and an insulating layer. The invention discloses a preparation method of a traditional Chinese medicine. A sheath layer of the weather-resistant new energy automobile charging cable is prepared from 70 to 90 parts of thermoplastic elastomer (TPE), 20 to 30 parts of lignin, 25 to 30 parts of propylene oxide, 20 to 25 parts of furfuryl alcohol, 2 to 5 parts of 4-chloromethyl styrene, 1.5 to 3 parts of tetrabutyl ammonium hydroxide, 5 to 6 parts of methylbenzene, 10 to 25 parts of methyl tert-butyl ether, 45 to 7 parts of anhydrous MgSO4, 0.5 to 2.5 parts of initiator, 2 to 3 parts of cross-linking agent, 5 to 8 parts of metal salt additive and 1 to 3 parts of lubricant. 0.3 to 0.6 part of antioxidant and 3 to 4 parts of color master batch.

The invention relates to a device and a method for preparing isobutene and methanol by cracking methyl tert-butyl ether. The device comprises a methyl tert-butyl ether vaporization refining tower, a reactor, a cooling tower, an absorption tower, a methanol extraction tower, an isobutene light component removal tower and an isobutene heavy component removal tower which are sequentially connected along a material conveying direction, a top discharge hole of the cooling tower is connected with a lower gas-phase material inlet of the absorption tower; an absorbent outlet at the bottom of the absorption tower is circularly connected with a cooling absorption liquid inlet at the top of the cooling tower; the bottom extract liquor outlet of the methanol extraction tower is circularly connected with the top absorbent inlet of the absorption tower; an isobutylene discharge hole is formed in the top of the isobutylene heavy component removal tower; the device further comprises a methanol recovery tower and a methanol refining tower which are connected in sequence along the material conveying direction; a bottom cooling absorption liquid outlet of the cooling tower is connected with the methanol recovery tower; a methanol discharge hole is formed in the bottom of the methanol refining tower. The device provided by the invention not only can relax the limitation of the purity of methyl tert-butyl ether in raw materials, but also can prepare high-purity isobutene and high-purity methanol at the same time.

The invention belongs to the field of organic synthesis, and particularly relates to a synthesis method of isoindolone. An N-methylbenzylamine compound as shown in a formula 1 and a 2-fluorobenzoic acid methyl ester compound as shown in a formula 2 are mixed with methyl tert-butyl ether in the presence of bis (trimethylsilyl) lithium amide and cesium fluoride, and the isoindolone as shown in a formula 3 is synthesized through reaction. The isoindolone derivative is synthesized through a one-pot method, and the method has the prominent advantages that raw materials are simple and easy to obtain, operation is easy and convenient, economy and environment friendliness are achieved, and the substrate applicability is wide.

The application discloses a method for determining 15 new psychoactive substances in saliva by solid phase supported liquid-liquid extraction (SLE) combined with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS / MS), which specifically uses a mixed solution of methyl tert-butyl ether and n-hexane as an elution solvent, adopts solid phase supported liquid-liquid extraction to pretreat saliva samples, and then adopts UPLC-MS / MS to detect the collected eluent, so as to realize qualitative and quantitative determination of the new psychoactive substances in saliva. The method has the advantages of rapidness, accuracy, high sensitivity and simple operation, the detection limit of the method is 0.2-0.5 ng / mL, can meet the domestic and foreign limit requirements, and provides technical support for monitoring and investigation of the new psychoactive substances in saliva.

The invention belongs to the technical field of tert-butylamine preparation, and particularly relates to a preparation process for synthesizing tert-butylamine by adopting methyl tert-butyl ether. The preparation process comprises the following steps: preparing calcium alginate microspheres; preparing an SAPO precursor solution; performing composite crystallization; preparing an SAPO-11 carrier; preparing an ammonium type SAPO-11 carrier; preparing a metal supported catalyst; preparing an activated catalyst; methyl tert-butyl ether and liquid ammonia are used as raw materials, and tert-butylamine is prepared under the catalysis of an activated catalyst. According to the preparation process for synthesizing the tert-butylamine by adopting the methyl tert-butyl ether, the process of catalytically synthesizing the tert-butylamine by taking the methyl tert-butyl ether and the ammonia as raw materials follows an acid catalytic cracking nucleophilic addition coupling mechanism, and the prepared hierarchical pore CuZn / HSAPO11 catalyst remarkably reduces the reaction activation energy through the synergistic effect of B acid, L acid and metal active sites; high-activity and high-selectivity catalytic conversion at low temperature is realized, and high-purity tert-butylamine is prepared.

The invention discloses bio-based polyamide with low water absorption and a preparation method thereof, and belongs to the technical field of polyamide preparation. The bio-based polyamide with the low water absorption rate is prepared from the following components in parts by weight: 30 to 50 parts of pentamethylene diamine, 15 to 30 parts of sebacic acid, 5 to 12 parts of citric acid, 5 to 10 parts of hexamethylenediamine, 2 to 5 parts of a hydrophobic auxiliary agent and 1 to 5 parts of a modified high-temperature-resistant additive, the hydrophobic additive is prepared from acetoxybenzoic acid, nonadecanoic acid, m-dimethoxybenzene, trifluoroacetic anhydride and methyl tert-butyl ether as raw materials, and the modified high-temperature-resistant additive is prepared from o-phenylenediamine, chloroacetic acid, vanillin, benzoyl bromide and thiourea as raw materials. The bio-based polyamide prepared from the substances has low water absorption and excellent thermal stability.

The invention relates to a preparation method of a crosslinked benzimidazole and imine connected polymer membrane for methanol / organic matter separation. Cross-linking the benzimidazole and imine connected polymer base membrane prepared on the support in a solution containing a cross-linking agent; the crosslinking time is 0.1 to 72 hours; the crosslinking temperature is 40-80 DEG C; putting the polymer film obtained after crosslinking treatment into a drying oven at 80-300 DEG C, carrying out heat treatment for 1-72 hours, and then naturally cooling to room temperature, so as to obtain a crosslinked benzimidazole and imine connected polymer film; and the thickness of the benzimidazole and imine connection polymer film is 20-2000nm. The method is applied to separation of mixtures such as methanol / dimethyl carbonate, methanol / toluene, methanol / methyl tert-butyl ether and the like for the first time. And for methanol / dimethyl carbonate and methanol / methyl tert-butyl ether, the mass fractions of methanol in the penetrating fluid can respectively reach 98.8% and 99.9% or above.

The utility model discloses a methyl tert -butyl ether sampling detection device relates to methyl tert -butyl ether technical field, including the extraction pipe, the surface fixedly connected with the pivot of extraction pipe, the surface of extraction pipe is opened with the square hole, the fixedly connected with the discharge gate of extraction pipe surface square hole department, the outside of pivot is inserted with the connecting shaft, the outside rotation is connected with the collection box of connecting shaft, the surface fixedly connected with the baffle of collection box. The utility model through baffle divides the inside of collection box into several cabins, through with the specified cabin corresponding mark rotates to the display hole department, then will sample liquid extraction to the inside of extraction pipe, then will device upset, then to the one side rotation limit rod of fixed plate arc shape, through the spring's elasticity, will piston rod push back, and stop moving at the front side of spacing septum, and the sample of extraction flows into the specified cabin inside due to the action of gravity, then rotates the knob to the next mark department again, thereby realizes the sample of multiple extraction and separates storage.

The invention discloses a membrane aeration bioreactor device for removing methyl tert-butyl ether pollution in high-salinity underground water. Comprising an external methyl tert-butyl ether polluted underground water conveying device, a soil sample chamber, a CDI (capacitive deionization) material, a biological function chamber, a dissolved oxygen intelligent control system, a pH intelligent control system, a methyl tert-butyl ether degrading bacterium supply device, a filter material chamber and a purified underground water collection device which are connected in sequence. The underground water polluted by the methyl tert-butyl ether flows into the soil sample chamber through the conveying device, and the soil sample chamber is filled with the soil polluted by the methyl tert-butyl ether to simulate the site environment. Groundwater gradually penetrates through the CDI material through soil pores and enters the biological function chamber, in the CDI material, anions and cations in the underground water move towards electrodes at the two ends under the action of an electric field, a deionization area is formed in the middle to discharge water, and electron donors needed by microorganisms are provided while salinity is removed.

The invention discloses a synthesis and purification method of a nalbuphine intermediate, the synthesis route of the method is as shown in the specification, and the method comprises the following steps: (1) in a reaction solvent, carrying out oxidation reaction on a compound I and peroxide to generate a compound II; (2) quenching, concentrating and extracting the reaction liquid containing the compound II obtained in the step (1), concentrating an extracted organic phase, adding a recrystallization solvent, and recrystallizing at-5 DEG C to 30 DEG C to obtain the compound II; wherein the recrystallization solvent is a mixed solvent of methyl tert-butyl ether and a low-polarity solvent, and the volume ratio of the methyl tert-butyl ether to the low-polarity solvent is (1-9): (1-4). According to the method, the purity of the compound II and the recrystallization yield are remarkably improved, side reactions in the subsequent nalbuphine synthesis process can be reduced, the cost is reduced, and industrial production is facilitated.

This invention discloses a solvate of rememega-2 and its preparation method. The rememega-2 solvate (compound II) provided by this invention has a purity of up to 99.15% compared with the existing rememega-2 methyl tert-butyl ether solvate. The preparation method includes the following steps: adding crude rememega-2 to a binary solvent, heating to 45℃~75℃, adding an antisolvent, stirring, crystallizing, cooling and filtering, and drying under reduced pressure to obtain rememega-2 solvate (compound II). Then, placing rememega-2 solvate (compound II) in ethanol and stirring to obtain rememega-2 (compound I). This route is simple to operate, the process is stable, and it is easy to scale up. Moreover, the rememega-2 (compound I) prepared by this solvate (compound II) has a purity of up to 99.66%, which is higher than that of rememega-2 (compound I) prepared by the existing rememega-2 methyl tert-butyl ether solvate. It also has better fluidity, does not caking, is easy to transfer, and is convenient for later production.

The present invention discloses a pleuromutilin derivative containing a 2-thio-4-thiazolidinone side chain, and its preparation method and application. The preparation method is as follows: first, pleuromutilin and p-toluenesulfonyl chloride are added to methyl tert-butyl ether, sodium hydroxide solution is added dropwise with stirring, and the reaction is refluxed to obtain intermediate 1; then, 2-thio-4-thiazolidinone is added to acetonitrile, anhydrous potassium carbonate is added and stirred at room temperature for 20 minutes, and then intermediate 1 is added, and the reaction is stirred at room temperature for a certain time to obtain intermediate 2; finally, intermediate 2 and an acyl chloride with different group donors are added to dichloromethane, and under the catalysis of triethylamine, stirred at room temperature for a certain time to obtain a pleuromutilin derivative containing a 2-thio-4-thiazolidinone side chain. The present invention synthesizes a pleuromutilin derivative containing a 2-thio-4-thiazolidinone side chain with good antibacterial activity through a simple preparation process, with high yield, good antibacterial activity against drug-resistant bacteria, and good application prospects.

The invention discloses a self-assembled fluorescent probe as well as a preparation method and application thereof. The preparation method comprises the following steps: adding 1-ethyl-2-methylbenzo [cd] indole-1-onium into a mixed solution of 10-[4-(dimethylamino) phenyl]-7-phenyl-3, 11-dithia-7-aza-tricyclo [6.3. 0.02, 6] undec-1 (8), 2 (6), 4, 9-tetraene-4-formaldehyde, acetic acid, acetic anhydride and triethylamine, and then mixing with methyl tert-butyl ether, so as to obtain the small molecule DMA-IN3, and carrying out ultrasonic self-assembly to obtain the nano-particle DINP. The self-assembled fluorescent probe DINP obtained by the invention has fluorescence property and phototoxicity, can be enriched to tumor tissues in a targeted manner, generates a large amount of heat under an illumination condition, realizes visual diagnosis and treatment of tumors, is good in biological safety, and provides a new scheme for clinical tumor treatment.

The purpose of the present invention is to provide a means for obtaining SMTP from a fermentation product including SMTP via a method that can easily be scaled up; to provide an SMTP crystallization method; or to provide a means for obtaining SMTP via a method including SMTP crystallization. The present invention provides an SMTP production method including: a step I for putting a Stachybotrys microspora fermentation product in contact with an aqueous solvent having a pH of 9 or greater and obtaining an extract liquid including SMTP; a step II for supplying the extract liquid obtained in step I for purification and obtaining a purified product; and a step III for crystallizing the SMTP included in the purified product obtained in step II in a crystallization solvent including one or more selected from the group consisting of ethyl acetate, butyl acetate, acetone, 2-butanone, diisopropyl ether, diethyl ether, methyl-tert-butyl ether, and acetonitrile. Alternatively, provided is an SMTP production method including a step for crystallizing SMTP having a purity of 70% or greater in a solvent including one or more selected from the group consisting of ethyl acetate, butyl acetate, acetone, 2-butanone, diisopropyl ether, diethyl ether, methyl-tert-butyl ether, and acetonitrile. Alternatively, provided is an SMTP production method including putting a Stachybotrys microspora fermentation product in contact with an aqueous solvent having a pH of 9 or greater and obtaining an extract liquid including SMTP.

The invention provides a preparation method of annomeline tartrate crystal form A. Cu-K alpha radiation is used, and an X-ray powder diffraction pattern of the crystal form A expressed by a 2 theta angle has characteristic peaks at 9.4 degrees + / -0.2 degrees, 20.4 degrees + / -0.2 degrees and 23.7 degrees + / -0.2 degrees. The preparation method comprises the following steps: (1) adding annomeline and L-tartaric acid into a first organic solvent, and stirring to obtain a second organic solvent; stirring and heating to obtain a clear solution; (2) adding a second organic solvent into the settled solution in the step (1), slowly cooling to 2-8 DEG C while stirring, and separating out crystals; and (3) filtering and collecting crystals, washing with a second organic solvent, and carrying out vacuum drying to obtain the Nomeline tartrate crystal form A. The first organic solvent is selected from methanol, ethanol, isopropanol, n-butanol, acetone or a combination thereof, and the second organic solvent is selected from methyl tert-butyl ether, an ester solvent, acetonitrile, an alkane solvent or a combination thereof. The preparation method of the xanthomeline tartrate is simple to operate, high in yield and high in purity.

The invention provides a cracking process of G-type natriuretic peptide, which is used for cracking synthesized G-type natriuretic peptide resin to obtain a linear peptide crude product, and comprises the following steps: S41, preparing a cracking reagent; s42, performing concentration; s43, carrying out precipitation; s44, filtering is carried out; and S45, drying. The cracking reagent comprises the following components: TFA, H2O, EDTA, TIS, ArOH and ArSCH3, wherein the ratio of TFA to H2O to EDTA to TIS to ArOH to ArSCH3 is 81.5: 5: 2.5: 1: 5: 5 (V / V / V / V / W / V). The dosage ratio of the cracking reagent to the G-type natriuretic peptide resin is 12-15ml / g. And carrying out suction filtration on the cracked reaction liquid, washing with TFA (Trifluoroacetic Acid), combining washing liquids, carrying out reduced pressure concentration on the filtrate at 32 + / -3 DEG C until the volume is 30-40% of the initial volume, and then precipitating with methyl tert-butyl ether. The cracking process of the G-type natriuretic peptide has the advantages that the cracking yield is high and can reach 20.0-30.0%, a stable and reliable process is provided for chemical synthesis of GNP cracking, and a high-quality cracking product is provided for subsequent preparation of GNP raw material medicines.

The invention discloses a refining method of a Pinefibrate intermediate PM02. The method comprises the following steps: 1, carrying out a heating reflux reaction on a reaction solvent, PM01, triethylamine and PM-SM03; 2, adding tetrahydrofuran and saturated saline solution into the reaction product system, and separating liquid to obtain a saline solution phase and a tetrahydrofuran phase; 3, adding tetrahydrofuran into the salt water phase, extracting to obtain tetrahydrofuran phases, combining the tetrahydrofuran phases, washing, drying, carrying out suction filtration, and concentrating to obtain PM02 oily matter; and 4, adding methyl tert-butyl ether into the PM02 oily substance, heating for dissolving, cooling for crystallization, then carrying out suction filtration, leaching a filter cake by using the methyl tert-butyl ether, then carrying out suction drying, and drying to obtain PM02. According to the method, the tetrahydrofuran and the saturated saline solution are adopted for extraction separation, methyl tert-butyl ether is adopted for crystallization, high-yield and high-purity PM02 is obtained, and the problems of equipment corrosion and acid-containing wastewater treatment caused by a large amount of waste liquid generated by column purification and strong acid crystallization are solved.

This invention relates to the fields of environmental and bioanalytical technology, and particularly to a method for simultaneous pretreatment and detection of bisphenol S and bisphenol AF in biological tissues. The technical solution includes a framework process for simultaneous pretreatment and detection of bisphenol S and bisphenol AF in biological tissues. This invention establishes a dual-solvent secondary extraction system composed of n-hexane and methyl tert-butyl ether, achieving differentiated adaptation to different tissue matrices. By combining the advantages of non-polar and moderately polar solvents, it can simultaneously handle the relatively highly polar bisphenol S and the relatively non-polar bisphenol AF in a single extraction process. Furthermore, this method sets key physical parameters during the extraction process according to the histological characteristics of each organ. For heart and lung tissues, specific ultrasonic power is used to ensure thorough cell disruption; while for liver and spleen with high lipid content, different power and time are used to ensure the full release of lipid-bound target substances.

The invention relates to a preparation method of a novel Zr-MOF membrane and organic matter separation application. The preparation method comprises the following steps: adding zirconium oxychloride octahydrate and butynedioic acid into a mixed solvent of water and formic acid, and carrying out ultrasonic treatment at room temperature for 5-15 minutes to completely dissolve solids, so as to prepare a synthetic mother solution; and putting the inorganic support body into a stainless steel reaction kettle containing a polytetrafluoroethylene lining, adding the prepared synthetic mother solution, and reacting in a convection oven at 80-150 DEG C for 12-72 hours to prepare the NUS-36 membrane. The method is applied to separation of mixtures such as methanol / dimethyl carbonate, methanol / toluene, methanol / methyl tert-butyl ether and the like. For methanol / toluene separation, the mass fraction of methanol in the penetrating fluid can reach 99.5% or above. And for methanol / dimethyl carbonate and methanol / methyl tert-butyl ether, the mass fractions of methanol in the penetrating fluid can respectively reach 98.0% and 99.9% or above.

The invention discloses a method and device for preparing low-carbon olefins, and the method comprises the following steps: 1) feeding methyl tert-butyl ether into a catalytic conversion reactor through an atomizing nozzle, and carrying out contact reaction on the methyl tert-butyl ether and a catalytic conversion catalyst under effective conditions to obtain a reaction product containing ethylene, propylene, butylene and C5 + olefins; and 2) feeding the olefin material into an etherification device to obtain methyl tert-butyl ether, and returning the methyl tert-butyl ether and / or etherified olefin to the catalytic conversion reactor. The method can improve the selectivity and yield of low-carbon olefins, obviously reduces the yield of methane in dry gas, and has good economic and social benefits.

The invention discloses a synthesis method for preparing an aryl phosphine-oxazoline ligand, which comprises the following steps: sequentially adding an alkyl alcohol alkali metal compound, a first solvent and a compound B into a reaction container, stirring, continuously adding a compound A, carrying out heat preservation reaction at the reaction temperature of 0-100 DEG C, and synthesizing the aryl phosphine-oxazoline ligand by a one-pot method, the alkyl alcohol alkali metal compound is selected from potassium tert-butoxide, sodium tert-butoxide, lithium tert-butoxide, potassium isopropoxide, sodium isopropoxide, lithium isopropoxide, sodium ethoxide and sodium methoxide; the first solvent is selected from the group consisting of tetrahydrofuran, diethyl ether, 1, 4-dioxane, 2-methyltetrahydrofuran, ethylene glycol dimethyl ether, cyclopentyl methyl ether, methyl tert-butyl ether and isopropyl ether. The method has the advantages of few reaction steps, easily available raw materials, mild reaction conditions, high yield, simple separation and convenient purification.

The present invention discloses a pleuromutilin derivative compound, its preparation method, and application. The method comprises adding pleuromutilin and p-toluenesulfonyl chloride to methyl tert-butyl ether, mixing the mixture, adding sodium hydroxide solution dropwise with stirring, and reacting under reflux to obtain intermediate 1. Intermediate 1 and cysteamine hydrochloride are added to tetrahydrofuran, benzyltributylammonium chloride and sodium hydroxide solution are added dropwise with stirring, and the mixture is reacted with stirring for 4-5 hours to obtain intermediate 2. Intermediate 2, indole acid, and catalyst 2 are added to dichloromethane, and an amidation reaction is carried out at room temperature with stirring for 12-24 hours to obtain the pleuromutilin derivative compound. The pleuromutilin derivative compound of the present invention has a simple preparation process and a high yield. The derivative compound has good in vitro antibacterial activity and is particularly suitable as a new antibacterial drug for preventing and treating infectious diseases caused by bacteria in humans or animals.

The application discloses a synthesis process of tert-butyl ethylbenzene, which comprises the following steps: carrying out a cracking reaction on methyl tert-butyl ether in a cracking reactor, separating and purifying the obtained cracked product to obtain isobutene, drying the isobutene, mixing the isobutene with ethylbenzene, and then feeding the mixture into an alkylation reactor to carry out an alkylation reaction, returning part of the obtained alkylation product to the alkylation reactor, and separating and purifying the other part to obtain tert-butyl ethylbenzene; in the alkylation reaction, an alkylation catalyst used is prepared by mixing modified beta zeolite with H-MCM-22 zeolite. Under the process conditions of the application, isobutene obtained by cracking methyl tert-butyl ether is alkylated with ethylbenzene to generate tert-butyl ethylbenzene, the conversion rate of the isobutene is greater than 97%, the selectivity of the tert-butyl ethylbenzene is greater than 93%, the catalyst has stable activity and long service life, the production cost of the tert-butyl ethylbenzene is low, and the synthesis process can be used for industrial production of the tert-butyl ethylbenzene.

The invention provides a detection method for simultaneously detecting multiple endocrine disrupters, which comprises the following steps: grinding tissue, homogenizing, adding an internal standard, extracting with three solvents: dichloromethane and methyl tert-butyl ether, an ethyl acetate-normal hexane mixed solution, acetonitrile and sodium chloride, combining and collecting the solutions to obtain a comprehensive extracting solution, concentrating and dissolving, degreasing, and drying to obtain the endocrine disrupters. Finally, a liquid chromatograph-mass spectrometer is used for detection, and efficient extraction and accurate analysis of the multiple endocrine disruptors in the tissue are achieved. According to the detection method, multiple organic solvents with different properties are adopted for extraction, detection of multiple endocrine disrupters can be synchronously achieved, the concentration level of the endocrine disrupters in the tissue sample can be directly measured, freeze drying treatment is not needed, operation is easy, and sensitivity and recovery rate are high.

The invention relates to a preparation method of 3-bromobenzotrifluoride, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: taking benzotrifluoride as a raw material, and reacting with liquid bromine under the action of a catalyst and a complexing agent to obtain 3-bromobenzotrifluoride; the catalyst is iron powder, ferric trichloride or ferric tribromide; the complexing agent is at least one of methanol, ethanol, methyl tertiary butyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, acetone or sodium acetate. The compound containing lone pair electrons is added into the reaction liquid to form a complex with ferric iron, so that the activity of the ferric iron catalyst is reduced, and the situation that the bromine substitution selectivity is reduced due to too high activity is avoided; the selectivity of aromatic ring bromine meta-substitution is improved, the generation of para-bromine substituted isomers and polysubstituted impurities is reduced, and the purity and yield of the product are improved.

The invention provides a method for extracting xanthohumol with an antibacterial effect from humulus lupulus, which comprises the following steps: extracting humulus lupulus by adopting methyl tert-butyl ether, and degreasing. Extracting the humulus lupulus raffinate by using n-butyl alcohol to obtain an extracting solution; and concentrating the extracting solution, and carrying out silica gel column chromatography to obtain an eluting solution. The eluting agent comprises three sequentially used volume gradients: methyl tert-butyl ether and n-butyl alcohol in a volume ratio of (4-6): 1, methyl tert-butyl ether and n-butyl alcohol in a volume ratio of (2-3): 1 and n-butyl alcohol. The dosage of the eluting agent is 4-10 times, 4-10 times and 3-6 times of the volume of the concentrated solution at a time. And concentrating and crystallizing the elution solution, and recrystallizing to obtain the xanthohumol. The method for extracting the xanthohumol with the antibacterial effect from the humulus lupulus is simple to operate, high-purity xanthohumol can be prepared without the aid of high-speed counter-current chromatography or ultrafiltration and sodium filtration facilities, and the method is suitable for large-scale process production.

The present invention provides a selective method for separating di- and tri-carboxylic acids from the reaction mixture of oil shale oxidation and for separating even-numbered di-carboxylic acids from odd-numbered di-carboxylic acids and tri-carboxylic acids. This goal is achieved by a method that uses different steps of extraction and crystal separation, the key process being extraction of the neutralized oxidized reaction mixture with dimethyl tert-butyl ether and crystallization of the extract. The noncrystallized part of the concentrated extract is esterified and distilled. The distilled esterified mixture is hydrolyzed with alkali and crystallized, which separates non-crystallized even-numbered dicarboxylic acids and oddnumbered dicarboxylic acids and tricarboxylic acids.

The utility model discloses a methyl tert-butyl ether recycling treatment device, which relates to the technical field of methyl tert-butyl ether recycling and comprises a support plate and a treatment cylinder, the treatment cylinder is mounted at the top of the support plate, a plurality of filter cylinders are arranged on the left side surface of a limiting disc, a rotating shaft is mounted on the left side surface of a transmission shaft, and a speed reducer is mounted on the left side surface of a fixing bolt. A stirring barrel is mounted on the left side face of a mounting rod, a filtering and stirring assembly is arranged in a treatment barrel, a rotating shaft drives the stirring barrel to rotate, unqualified methyl tert-butyl ether is stirred and mixed through stirring teeth on the inner wall of the stirring barrel, and the mixed methyl tert-butyl ether can be filtered and reused through a filtering barrel and a filtering cover. The arranged limiting disc locking screw rod is in threaded connection with the connecting block, installation and use are convenient, the arranged limiting shaft sleeve is used for limiting the rotating shaft, the arranged fixing bolt can facilitate installation of the speed reducer, and the arranged speed reducer can adjust the use speed of the rotating shaft.