28 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 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 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.

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 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 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 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 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 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 invention relates to the technical field of biological analytical chemistry, in particular to a serum perfluorinated compound detection pretreatment method based on acidified protein precipitation and liquid-liquid extraction, which comprises the steps of acidified acetonitrile protein precipitation, nitrogen blowing concentration, composite extractant liquid-liquid extraction and redissolution filtration. According to the method, a methyl tert-butyl ether and ethyl acetate compound extraction system is adopted, the process of first concentration and then extraction is combined, the pretreatment effects of high recovery rate, low matrix effect and high enrichment multiple are achieved in a single centrifugal tube, and the method is suitable for high-flux, low-cost and green detection of C4-C14 perfluorinated compounds in trace serum.

The invention discloses a catalytic synthesis process of methyl tert-butyl ether, and belongs to the technical field of etherification catalytic synthesis, the main raw materials are methanol and C4 before etherification, mesoporous silica is introduced in situ into strongly acidic cation exchange resin, and sulfonic imidazole trifluoromethanesulfonate ionic liquid is loaded in the ion exchange resin, so that the methyl tert-butyl ether is obtained. The obtained modified catalyst can be used for an etherification reaction of methyl tert-butyl ether and a subsequent catalytic rectifying tower process, so that the reaction is balanced and continuously moves towards a product direction, the overall conversion rate of the etherification reaction is improved, and the yield of the methyl tert-butyl ether is improved. According to the process, the raw material conversion rate and the product purity are improved through the synergistic effect of reaction and separation, cyclic utilization of the raw materials is achieved in combination with a methanol recovery system, and the process has high reaction efficiency and good catalyst stability and is suitable for large-scale industrial continuous production.

The invention discloses a green and efficient synthesis method of high-purity 4-chloro-5-fluoro-7-azaindole, which comprises the following steps: by taking 5-fluoro-1H-pyrrolo [2, 3-B] pyridine as a raw material, carrying out high-selectivity reaction on the 5-fluoro-1H-pyrrolo [2, 3-B] pyridine and a composite chlorination system consisting of phosphorus oxychloride and N, N-dimethylformamide in an aprotic polar solvent under the catalysis of Lewis acid, thereby obtaining the high-purity 4-chloro-5-fluoro-7-azaindole. After the reaction is completed, an integrated quenching-neutralization-extraction post-treatment process is adopted, the operation is simplified, and a crude product is finally recrystallized and purified through a stepped solvent system consisting of ethyl acetate, methyl tert-butyl ether and normal hexane. According to the method, chlorination sites are accurately controlled by optimizing a reaction system, so that by-products are remarkably reduced; meanwhile, the used raw materials and solvents are economical and environment-friendly, and the catalyst is high in efficiency and suitable for industrial production.

The present invention relates to a process for the preparation of a compound of formula (II), a stereoisomer, salt, hydrate or solvate thereof, comprising the step of sulfinylating a compound of formula (IV) to produce a compound of formula (II); wherein: R1 and R2 are as defined in the claims; wherein the sulfinylation step is carried out in the presence of a solvent selected from the group consisting of benzene, toluene, ethylbenzene, xylene, chlorobenzene, bromobenzene, fluorobenzene, anisole, nitrobenzene, tetrahydronaphthalene, dichlorobenzene, trimethylbenzene, ethyl acetate, propyl acetate, butyl acetate, propanol, butanol, 2-methyltetrahydrofuran, diethyl ether, methyl tert-butyl ether, cyclopentylmethyl ether, dichloromethane, and tetrachloromethane, pentane, hexane, heptane, cyclohexane, decahydronaphthalene and mixtures thereof.

The utility model relates to the technical field of methyl tert-butyl ether, and discloses a methyl tert-butyl ether recovery device which comprises a protective outer tank, an inner tank is arranged in the protective outer tank, the top end of the inner tank is fixedly connected with a warning lamp, and the top end in the inner tank is fixedly connected with a temperature monitor. Cold air is in contact with the surface of the inner tank to cool the interior of the inner tank. When the temperature in the inner tank is reduced to a specified temperature, the methyl tert-butyl ether in the inner tank begins to react, water drops are generated on the surface of the circulating pipe due to cold air in the refrigeration process, and the water drops fall into a gap between the protective outer tank and the inner tank and then flow out from a liquid outlet pipe. And liquid condensate generated by methyl tert-butyl ether in the inner tank due to cold air can be adhered to the interior of the inner tank and the surface of the filter plate. At the moment, a servo motor drives a rotating shaft to rotate, stirring blades on the rotating shaft stir methyl tert-butyl ether, and meanwhile a first scraper, a second scraper and a third scraper respectively scrape off condensate on the inner wall of the inner tank and the upper surface and the lower surface of a first filter plate.

The utility model relates to the methyl tert -butyl ether recovery field especially relates to a recovery unit for methyl tert -butyl ether, including recovery box, rectangular frame no.

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a method for detecting methyl tert-butyl ether and triethylamine in tofacitinib citrate. Respectively detecting the blank solution, the reference solution and the test solution by headspace gas chromatography, recording chromatograms, and quantitatively analyzing methyl tert-butyl ether and triethylamine in the test solution according to an external standard method; wherein a preparation method of the test solution comprises the following steps: precisely weighing 0.1 g of a tofacitinib citrate sample, putting the tofacitinib citrate sample into a 20ml headspace bottle, adding 2ml of N-methyl pyrrolidone and 0.28 ml of a sodium hydroxide solution with the concentration of 100mg / ml, and sealing. The method realizes effective separation and quantitative detection of methyl tert-butyl ether and triethylamine in tofacitinib citrate, is high in sensitivity, good in repeatability and high in accuracy, makes up for the deficiency of research on methyl tert-butyl ether and triethylamine in tofacitinib citrate, and improves clinical medication safety.

The invention discloses a method for preparing ethylene glycol tert-butyl ether, and belongs to the technical field of petrochemical engineering. According to the method, ethylene glycol or an ethylene glycol aqueous solution, a C4 olefin raw material containing isobutene or methyl tert-butyl ether and a modified solid acid catalyst are subjected to a contact reaction, and ethylene glycol tert-butyl ether is prepared; the modified solid acid catalyst is prepared by the following steps: firstly, loading a hydroxyl pyridine derivative on a molecular sieve, then putting into an acidic aqueous solution for treatment, and roasting. According to the method disclosed by the invention, the selectivity of the ethylene glycol tert-butyl ether can be greatly improved, and the selectivity of the ethylene glycol tert-butyl ether reaches 90% or above; the method is easy to industrially amplify, has a good application prospect and is remarkable in economic benefit.

The invention discloses a method for purifying rocuronium bromide. The method comprises the following steps: reacting a rocuronium bromide crude product with alkali metal bromine in dichloromethane, filtering, mixing the filtrate with methyl tert-butyl ether, and separating out a solid. The method can effectively control the chloride ion residues in rocuronium bromide, and has a good application prospect in industrial production of rocuronium bromide.

The utility model provides a device for efficiently recovering and reusing heavy components in a tertiary butanol dehydration process. The device comprises a rectifying tower; a condenser; a reflux tank; a reflux pump; an extraction column; a feed line; one end of the tower top steam pipeline is connected with a tower top steam outlet of the rectifying tower, and the other end is connected with a condensation inlet of the condenser; a condensate line; one end of the reflux suction pipeline is connected with the liquid outlet of the reflux tank, and the other end is connected with the fluid inlet of the reflux pump; one end of the reflux supply pipeline is connected with a fluid outlet of the reflux pump, a first branch at the other end of the reflux supply pipeline is connected with the upper part of the rectifying tower, and a second branch at the other end of the reflux supply pipeline is connected with an external methyl tert-butyl ether product storage tank; one end of the intermediate material pipeline is connected with the tower kettle material outlet of the rectifying tower, and the other end is connected with the material inlet of the extraction tower; and a water washing agent supply line. According to the utility model, methyl tert-butyl ether and tert-butyl alcohol in heavy components in the tert-butyl alcohol dehydration process can be efficiently recovered and reutilized.

The application belongs to the technical field of environmental monitoring and analytical chemistry, and discloses a detection method for the content of methyl tert-butyl ether in soil. The method uses surface functionalized mesoporous silica adsorbent for solid phase extraction, combines ultrasonic assisted extraction with gas chromatography-mass spectrometry analysis, the adsorbent has a pore size of 2.5-4.0 nm, and a surface grafted with bifunctional ligands containing tertiary amine groups and short chain alkyl groups, and has high selectivity and adsorption capacity for methyl tert-butyl ether; the mass spectrometry detection adopts double ion confirmation and intensity ratio criterion, effectively eliminating the interference of structural analogues. Through the design of special adsorption materials, the optimization of the pretreatment process and the construction of the mass spectrometry confirmation logic, the application realizes high sensitivity, high selectivity and high reproducibility detection of trace methyl tert-butyl ether, and can be widely applied to industrial pollution site investigation, farmland soil safety evaluation, groundwater pollution tracing and emergency monitoring of environmental incidents.

The invention relates to a detection reagent for lipid biomarkers, application and a screening method. The detection reagent comprises a lipid extraction protein precipitation reagent, a redissolving reagent and a chromatographic separation reagent, the lipid extraction protein precipitation reagent is a mixture of methyl tert-butyl ether and methanol in a ratio of 5: 1, and the redissolving reagent is methanol and dichloromethane in a ratio of 1: 1. Injecting the detection reagent into a detection device comprising a liquid chromatography-tandem mass spectrometer, and detecting through liquid chromatography-tandem mass spectrometry to obtain the content of each lipid in the lipid biomarker. The FH neonatal marker is represented through lipidomics characteristics for the first time, the lipid biomarker is screened out and used for evaluating the disease severity of the FH neonatal, and the obtained lipid biomarker has high value for early screening and timely intervention of FH. The lipid biomarker obtained through screening has good biological stability and representativeness, the biological activity of the lipid biomarker can be guaranteed after long-time storage, and the reliability of a detection result can be guaranteed.

This invention discloses a catalytic synthesis process for methyl tert-butyl ether, belonging to the field of etherification catalytic synthesis technology. The main raw materials are methanol and pre-ether C4. By introducing mesoporous silica in situ into a strongly acidic cation exchange resin and loading sulfonic acid imidazole trifluoromethanesulfonate ionic liquid into the ion exchange resin, a composite catalyst with a multi-level pore structure is formed, thereby significantly improving the utilization rate of acidic sites inside the catalyst. The resulting modified catalyst can be used in the etherification reaction of methyl tert-butyl ether and subsequent catalytic distillation process, so that the reaction equilibrium continuously shifts towards the product, thereby improving the overall conversion rate of the etherification reaction. This process also improves the raw material conversion rate and product purity through the synergistic effect of reaction and separation, and realizes the recycling of raw materials by combining a methanol recovery system. This process has high reaction efficiency, good catalyst stability, and is suitable for large-scale industrial continuous production.

The application discloses a method for purifying phosphoramidite monomers, and comprises the following steps: 1) adding a solvent, tetrazole, N-methyl imidazole and a phosphorus reagent under nitrogen protection into a reaction container and stirring; 2) dissolving raw materials in DMF solvent and adding into a reaction system under nitrogen protection; 3) ending when the peak area ratio of raw materials except the solvent on an HPLC spectrum is less than or equal to 0.5% and the purity is more than 95%; 4) concentrating the organic phase to no distillate and dissolving the solvent; 5) adding water and 3wt% NaCl aqueous solution into the reaction container, stirring, separating, and washing the upper organic phase; 6) concentrating the organic phase, centrifuging and crystallizing; 7) dissolving with methyl tert-butyl ether, adding a mixed solvent of DMF and H2O, separating, and washing the organic phase; 8) drying the organic phase, dropping into a solvent for crystallization; and 9) drying under N2. The method can remove trivalent phosphorus by using common chemical purification methods of water washing and crystallization, can wash pentavalent phosphorus with DMF and water, and can purify products, so that industrial production is realized.

The invention relates to the technical field of separation of mutually soluble methyl tert-butyl ether and methanol, in particular to a separation method of methyl tert-butyl ether and methanol based on an ultra-infiltration membrane. The method comprises the following steps: adding a high-polarity inducer into a methyl tert-butyl ether / methanol mixture to induce phase separation of a system so as to form a low-polarity methyl tert-butyl ether phase and a high-polarity methanol / inducer phase; a methyl tert-butyl ether phase selectively permeates through a porous ultra-infiltration membrane with a low-polarity functional layer, and a methanol / inducer phase is blocked, so that efficient separation of the methyl tert-butyl ether phase and the methanol / inducer phase is realized. Compared with traditional membrane separation technologies such as pervaporation, organic solvent reverse osmosis and evaporation osmosis, the method has the advantages of large separation flux, low energy consumption, simplicity and convenience in operation and the like, and has a good application prospect in industrial production of methyl tert-butyl ether.

The invention provides an AOD-9604 polypeptide synthesis method, which comprises: (1) dispersing Fmoc-Phe-OH and Wang resin in a solvent, adding pyridine and 2, 6-dichlorobenzoyl chloride, carrying out a reaction, carrying out suction filtration, washing, and terminating with acetic anhydride to prepare Fmoc-Phe-Wang resin; (2) sequentially coupling amino acids by adopting a solid-phase synthesis method to obtain peptide resin; (3) adding the peptide resin into a lysis solution, reacting, and carrying out solid-liquid separation to obtain a filtrate; adding the filtrate into methyl tert-butyl ether, centrifuging to remove supernate, adding the obtained solid into methyl tert-butyl ether, pulping to suspend, centrifuging, repeating the operation twice, removing supernate, and drying the obtained solid to obtain a linear peptide crude product; and (4) dissolving the linear peptide crude product with a mixed solvent of water, acetic acid and dimethyl sulfoxide, adding water for dilution, adding an oxidizing agent to oxidize and bridge the disulfide bond, reducing with VC to obtain an AOD-9604 polypeptide crude product, and performing reverse preparation and freeze-drying to obtain the AOD-9604 polypeptide. The purity of the solid-phase synthesized simple linear peptide is 86% or above, the cost is low, and side reactions can be controlled.