485 results about "Protic solvent" patented technology

A method for efficiently and safely cleaning an apparatus for tin compound and a highly purified tin compound apparatus are provided. A cleaning method for an apparatus that has been in contact with a tin compound having formula (1) below includes at least steps (A) to (C), in which step (B) is performed after step (A), and step (C) is performed after step (B):(A) a step of cleaning the apparatus with a non-protic solvent,(B) a step of cleaning the apparatus with alcohol, and(C) a step of cleaning the apparatus with ultrapure water having a resistivity value of 17 MΩ·cm at 25° C.RpSnXm  (1)In formula (1), R is a hydrocarbon group, p is an integer from 1 to 3, X is a hydrolyzable substituent, and m=4−p.

A method for efficiently and safely cleaning an apparatus for a tin compound and a highly purified apparatus for a tin compound are provided. A method of cleaning an apparatus that has been in contact with a tin compound having formula (1) includes at least steps (A) to (C) in this order:(A) a step of cleaning the apparatus with a non-protonic solvent,(B) a step of cleaning the apparatus with an acidic aqueous solution and / or alkaline aqueous solution, and(C) a step of cleaning the apparatus with ultrapure water having a resistivity of 17 MΩ·cm at 25° C.RpSnXm  (1)R is a hydrocarbon group, p is an integer of 0 to 3, X is a hydrolyzable substituent, and m=4-p.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of ethylene sulfate and derivatives thereof, which comprises the following steps: S1, taking an aprotic solvent as a reaction solvent, adding urea peroxide, and stirring until the urea peroxide is dissolved; s2, dropwise adding ethylene sulfite or an ethylene sulfite derivative, stirring for reaction, and purifying to obtain ethylene sulfate or an ethylene sulfate derivative; the method has the advantages of reducing the catalyst cost and reducing the wastewater amount.

The invention belongs to the technical field of liquid chromatography-mass spectrometry detection pretreatment, and particularly relates to a pretreatment method for liquid chromatography-tandem mass spectrometry analysis of pesticide and veterinary drug residues in serum, which comprises the following steps: (S1) carrying out heating reaction on Sc (III) salt, Cu (II) salt and 1H-pyrazole-4-formic acid (H2PyC) in a polar aprotic solvent, and cooling to obtain a green crystal, namely MOF-919; the chemical formula of the MOF-919 is [Sc < 3 > (mu3-O) (OH) < 3 >] [Cu3 (mu3-O) (mu-PyC) < 3 > (H2O) < 6 >] < 2 >; (S2) mixing the serum sample with an acetonitrile solution containing formic acid, carrying out ultrasonic treatment, vortex oscillation and centrifugation, taking supernate, and diluting the supernate with an aqueous solution containing formic acid to obtain a to-be-purified solution; and (S3) adding MOF-919 into the to-be-purified liquid, mixing, performing ultrasonic treatment, performing vortex oscillation, centrifuging, and taking supernate, thereby completing the pretreatment of the to-be-purified liquid. According to the method, the MOF-919 is used for adsorbing chemical pollutant residues in serum, especially phospholipids, so that the purpose of removing the chemical pollutant residues in blood is achieved. The method is simple and convenient to operate, small in organic solvent consumption and good in purification effect, and can be widely applied to residue analysis of chemical pollutants in serum.

An improved solvent system for the formulation and application of N-alkyl thiophosphoric triamide urease inhibitors. These formulations provide safety and performance benefits relative to existing alternatives and enable storage, transport and subsequent coating or blending with urea based or organic based fertilizers. These formulations are comprised primarily of environmentally friendly aprotic and protic solvents (particularly dimethyl sulfoxide and alcohols / polyols) to stabilize the urease inhibitor.

Disclosed herein is an aqueous nucleic acid purification buffer comprising a polar aprotic solvent. Also provided herein are using such purification buffers to precipitate nucleic acids from a solution onto a solid support, thereby providing a solid support that binds to nucleic acids. Also provided herein is a method for treating a nucleic acid comprising exposing a sample comprising the nucleic acid to an aqueous medium comprising a polar aprotic solvent in the presence of a solid support; and precipitating the nucleic acid onto the solid support, thereby providing a solid support that binds to the nucleic acid. Further provided herein are kits and compositions comprising such aqueous nucleic acid purification buffers, as well as related nucleic acid analysis devices, and uses of the kits.

The invention belongs to the technical field of polymer electrolyte membrane materials, and particularly relates to a high-ionic-conductivity polymer electrolyte membrane and a preparation method thereof.The preparation method comprises the steps that 1, PEO and lithium salt are added into a polar aprotic solvent, and the mixture is rapidly and violently stirred to be completely dissolved; (2) adding a cross-linking agent and a photoinitiator into the mixed solution, and violently stirring to obtain a mixed solution; and (3) coating the mixed solution in a polytetrafluoroethylene template, heating to remove the solvent, and performing ultraviolet radiation. According to the invention, a three-dimensional cross-linked network is formed by photocuring of an acrylate group of the cross-linking agent, PEO chain segment crystallization is inhibited, and lithium salt anions (such as TFSI-) are physically embedded. A benzene ring structure in a cross-linked network endows the electrolyte membrane with flexibility, mechanical property deterioration caused by a plasticizer or a diluent is avoided, the compact structure of the electrolyte membrane can inhibit lithium dendrite growth, the ionic conductivity reaches 1.7 * 10 <-4 > S / cm, and the electrochemical window reaches 4.9 V. The method is simple in process and suitable for large-scale preparation of the high-energy-density solid-state lithium battery.

The invention provides a solvent-assisted aminolysis method of a waste polyurethane material, which comprises the following steps: mixing a catalyst with an aminolysis reagent to form an aminolysis solution, mixing the aminolysis solution with an aprotic solvent, then adding the waste polyurethane material, and carrying out aminolysis reaction under a heating condition to degrade the waste polyurethane material. And separating the aprotic solvent and the aminolysis reagent from the degradation liquid, and cleaning the obtained solid product to obtain the degradation product of the waste polyurethane material. According to the method, the degradation temperature of the existing aminolysis method for degrading the waste polyurethane material can be reduced, and the degradation speed of the existing aminolysis method for degrading the waste polyurethane material can be increased. The invention also provides a method for preparing the supramolecular adhesive by recovering the degradation product of the waste polyurethane material, which comprises the following steps: fully mixing the degradation product of the waste polyurethane material obtained by the method with the polyphenol compound at 60-120 DEG C to obtain the supramolecular adhesive. According to the method, the aminolysis temperature of the waste polyurethane material can be reduced, and the reutilization operation of the waste polyurethane degradation product is simplified.

The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to a two-dimensional fullerene covalent network, an electrochemical synthesis method and a photoelectric detector. The method comprises the following steps: by taking a fullerene superlattice material as a cathode, an inert material as an anode and a mixed solution of quaternary ammonium salt containing hydrogen protons and a polar aprotic solvent as an electrolyte solution, performing electrochemical stripping under constant potential to obtain a large batch of two-dimensional fullerene networks within a short time. Based on intercalation and expansion of layered fullerene superlattices, in combination with an in-situ reduction assisting effect of solvated protons at the edge of Mg4C60 crystals, quaternary ammonium salt cations are electrically driven to perform rapid intercalation expansion, generated hydrogen bubbles destroy relatively strong interaction force between layers, rapid and uniform intercalation of the quaternary ammonium salt cations between the layers is promoted, and the performance of the Mg4C60 crystal is improved. The stripping efficiency is as high as 83%, the single-layer stripping rate is as high as 30%, and the stripped two-dimensional C60 covalent network keeps a complete crystal structure and a large size.

An inhibited aqueous fertilizer composition and methods of use thereof.

The invention provides a high-strength anti-ultraviolet regenerated PET fiber and a preparation method thereof. The preparation method comprises the following steps: in a nitrogen atmosphere, dissolving 2, 2 '-methylenebis [6-(benzotriazolyl)-tetramethylbutylphenol] and hexamethylene diisocyanate in N-methyl pyrrolidone, adding a catalyst for reaction, then heating to remove residual monomers, cooling, dropwise adding into ice methanol to separate out a product, washing, and carrying out vacuum drying to obtain an anti-ultraviolet auxiliary agent; the preparation method comprises the following steps: dissolving an anti-ultraviolet aid and hexamethylenediamine in an aprotic solvent, adding a catalyst, carrying out condensation reaction in a nitrogen atmosphere, and carrying out centrifugal washing and vacuum drying to obtain the anti-ultraviolet composite chain extender, the preparation method comprises the following steps: mixing an anti-ultraviolet composite chain extender with recycled PET fragments, adding an antioxidant, a hydrolysis-resistant solution and a lubricant, and carrying out blending spinning through a double-screw extruder to obtain the high-strength anti-ultraviolet regenerated PET fiber. According to the invention, through anti-ultraviolet-chain extension chemical bonding, the bottleneck that the strength and the function of the regenerated PET fiber are difficult to synergistically improve is broken through.

The invention discloses a method for preparing 1-chloro-2, 3, 3-trifluoropropene through resource utilization of 1, 1, 2-trifluoroethane, which comprises the following steps: (1) dehydrofluorination: 1, 1, 2-trifluoroethane is subjected to a dehydrofluorination process under the action of a gas-phase dehydrofluorination catalyst to obtain 1, 2-difluoroethylene; (2) telomerization: under the combined action of the prefluorinated telomerization catalyst, the accelerant and the polar aprotic solvent, telomerization is performed on the 1, 2-difluoroethylene and the dichlorofluoromethane to obtain 3, 3-dichloro-1, 1, 2-trifluoropropane; and (3) a dehydrochlorination step: carrying out dehydrochlorination on the 3, 3-dichloro-1, 1, 2-trifluoropropane to obtain the 1-chloro-2, 3, 3-trifluoropropene. The method has the advantages of easily available raw materials, high product selectivity, high purity, easiness in separation, suitability for industrial application and the like.

The present invention discloses a method for preparing furfural, which includes: under the action of a heteropolyacid-based phase transfer catalyst, an intramolecular dehydration reaction occurs for xylose-based carbohydrates in a ternary two-phase reaction medium composed of a low-boiling organic solvent, a protic solvent, and an ionic organic ammonium chloride. The catalyst used in the present invention has the property of phase transfer, that is, its solubility in the reaction medium increases at high temperature, and it catalyzes the dehydration of xylose in the form of a liquid acid; after the reaction, the solubility decreases and it precipitates in the form of a solid, which is convenient for the recovery and separation of the catalyst, and largely solves the problems of low efficiency of solid acid catalysts and difficult separation of liquid acid catalysts. And an advanced reaction medium is coupled to increase the solubility of xylose-based carbohydrates and the solvation effect on xylose. Through the optimization of the catalyst and the reaction medium, the reaction performance of the reaction system is effectively improved.

A pattern formation method may use a resist composition. The resist composition may include an organometallic compound represented by any one of Formulae 1-1 to 1-4, an additive represented by Formula 2, and a solvent. The solvent may include a non-polar solvent, a polar aprotic solvent, or a combination thereof.Refer to the specification for the descriptions of M11, L11 to L14, a11 to a14, R11 to R14, b11 to b14, Y11 to Y13, X11 to X13, Y21, Y22, L21, and a21 in Formulae 1-1 to 1-4 and 2.

The invention relates to the technical field of high-molecular polymerization and molding, in particular to a modified para-aramid stock solution, a preparation method and para-aramid fibers.The preparation method comprises the steps that under the inert gas condition, diamine and a chlorosilane polycondensation agent react in a weakly-alkaline polar aprotic solvent, and a silanization modified diamine solution is obtained; the diamine comprises diaminodiphenyl ether and p-phenylenediamine; adding paraphthaloyl chloride into the silanization modified diamine solution to carry out a copolymerization reaction, and after the reaction is finished, carrying out neutralization treatment to obtain the modified para-aramid stock solution. According to the preparation method of the modified para-aramid stock solution, the modified diamine does not need to be independently purified, the high-viscosity modified para-aramid stock solution can be directly obtained, and the modified para-aramid stock solution is high in polymer specific concentration logarithmic viscosity and high in molecular weight, so that a high-quality and stable-quality para-aramid fiber product is more favorably obtained.

The invention also is directed to a new process for making the bis-polyisobutylene alcohol amine by reacting a polyisobutylene epoxide with a polyamine, optionally in the presence of a catalyst, a protic solvent initiator and / or a diluent. In addition, the invention further relates to the many uses of the bis-polyisobutylene alcohol amine including but not limited to its use in lubricants, surfactants, emulsifiers, resins, and the like.

The invention relates to a synthesis method of milobalin or acid salt thereof, and belongs to the technical field of medicine synthesis. In order to solve the problem that chiral resolution needs to be adopted in the prior art, the invention provides a synthesis method of miloabalin or an acid salt thereof, which comprises the following steps: under the action of an organic strong base, carrying out Michael addition reaction on a compound shown as a formula III and acetonitrile in a non-polar organic solvent at a low temperature of-50 DEG C or below to obtain an intermediate product; under the alkaline condition, the intermediate product is subjected to an oxidation reaction and a hydrolysis reaction under the action of an oxidizing agent, after the reaction is finished, an intermediate product is obtained through acidification, and the intermediate product is subjected to a high-temperature decarboxylation reaction in an aprotic solvent to obtain a compound of a formula VI; and carrying out Hofmann degradation reaction on the compound of formula VI to obtain the compound of formula I miloabalin or miloabalin acid salt. The method has the advantages of high stereoselectivity, no need of chiral resolution operation, avoidance of the problem of large material loss caused by resolution, high chiral purity and high yield.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of octocrylene serving as a main component of a sun-screening agent. The invention provides a preparation method of octocrylene serving as a main component of a sun-screening agent, which comprises the following steps: dissolving benzophenone in a polar aprotic solvent, adding zinc powder, heating to 50-70 DEG C under an inert condition, and dropwise adding 2-bromo-2-ethyl cyanoacetate for reaction to obtain a solution containing an intermediate etocrylene; under an ice bath condition, acidifying the solution containing the intermediate etocrilene by using a protonic acid aqueous solution, adding isooctanol, and slowly heating to 15-30 DEG C for reaction; and after the reaction is finished, extracting, washing, drying, filtering and concentrating the reaction liquid to obtain the octocrylene. According to the preparation method, reaction steps are reduced, the preparation process is simple, the operation method is convenient and fast, high-purity octocrylene can be obtained without purifying an intermediate, and large-scale industrial production is facilitated.

The invention provides a stripping method of a negative pole piece in a metal battery and a testing method of the metal battery. The stripping method comprises the following steps: disassembling the metal battery to obtain a negative pole piece with a diaphragm on the surface; the negative pole piece comprises an active metal layer; applying the treating fluid to the negative pole piece with the diaphragm on the surface, enabling the treating fluid to at least act on an interface between the active metal layer and the diaphragm, and stripping the negative pole piece from the diaphragm; wherein the treating fluid comprises a polar aprotic solvent, the dielectric constant of the polar aprotic solvent at 25 DEG C is larger than or equal to 7, and the standard reduction potential of the polar aprotic solvent relative to a standard hydrogen electrode is smaller than-1.1 V. According to the stripping method, the risks of metal adhesion and oxidation blackening can be reduced, the deposition morphology integrity of the metal layer of the cathode pole piece obtained by stripping is improved, and the accuracy of judging the metal deposition condition on the cathode interface of the metal battery is improved.

The invention relates to a preparation method of a lithium difluoro-bis (oxalate) phosphate concentrated solution, the lithium difluoro-bis (oxalate) phosphate concentrated solution is composed of lithium difluoro-bis (oxalate) phosphate and an aprotic solvent, the aprotic solvent comprises any one or a combination of at least two of diethyl carbonate, ethyl methyl carbonate, ethylene carbonate or propylene carbonate, the concentration of the lithium difluoro-bis (oxalate) phosphate in the lithium difluoro-bis (oxalate) phosphate concentrated solution is 10-35 wt%. The lithium difluoro bis (oxalate) phosphate concentrate provided by the invention exists in a non-proton electrolyte state, so that an evaporative crystallization process is omitted, and the production cost is reduced; the product transportation cost can be reduced through pipeline transportation; and compared with a lithium phosphate solid difluoro bis (oxalate), the process of re-dissolution during use is omitted, the risk of impurity introduction is avoided, and the use cost is reduced.

The invention discloses a ketoazine-based polymer, an anion exchange membrane and a preparation method and application of the ketoazine-based polymer and the anion exchange membrane. A first linking group and a second linking group are mixed and then mixed with an aryl monomer A in an aprotic solvent of halogen atoms; slowly adding a super acid mixture; performing polymerization reaction in an environment of-5 to 3 DEG C to obtain a reaction solution; pouring the reaction liquid into a first mixed solvent to obtain PAAz; carrying out primary quaternization reaction on PAAz through carbonate, bicarbonate or hydroxide salt of alkali metal, and adding an organic base catalyst to assist the primary quaternization reaction; in the first quaternization reaction, a quaternization reagent is added; and pouring into a second mixed solvent, and precipitating to obtain purified PAAz. Under the condition of super acid catalysis, two or more alicyclic amine derivatives containing ketone groups react with one or more aromatic fused rings to generate a polymer containing secondary or tertiary amine. And carrying out quaternization treatment to finally form the cationic polymer.

The present invention discloses a nicotine-tartrate complex, a preparation method and an application, which relate to the technical field of chemical synthesis. The preparation method provided by the present invention includes: Step 1: Completely dissolve tartaric acid in a protic solvent to obtain a tartaric acid solution; Step 2: Dropwise add nicotine to the solution obtained in Step 1, and stir at room temperature until a white solid precipitates. Then, add an aprotic solvent to the reaction system, and the amount of the precipitated solid increases. Continue to stir for 16-24 hours. When the amount of the white solid no longer increases, filter, and wash the filter cake with the aprotic solvent 2-3 times to obtain a white solid; Step 3: Vacuum-dry the white solid obtained in Step 2 to obtain a white solid powder of tartaric acid-nicotine salt complex. This method well solves the problems that the nicotine-tartrate complex is not easy to form a solid and the solid is not easy to dry. The obtained nicotine-tartrate complex solid is a uniform white fluffy powder, which is more convenient to use.

The invention relates to a polyisobutylene polyether alcohol amine compounds and compositions thereof. The invention also is directed to a new process for making the polyisobutylene polyether alcohol amine compound(s) by reacting a polyisobutylene epoxide with a specific polyetheramine, a protic solvent, a diluent, and optionally a catalyst. In addition, the invention further relates to the many uses of the polyisobutylene polyether alcohol amine compound(s) and composition(s) including but not limited to its use in lubricants, surfactants, emulsifiers, adhesives, resins, and the like.

The invention discloses a preparation method of a molybdenum extraction reagent NP192 for an alkaline system, and belongs to the technical field of hydrometallurgy. The preparation method comprises the following steps: adding 1-2mol / L of a 1, 2, 3-triazole reagent and a solvent into a reaction container, stirring and dissolving, and cooling to 0-5 DEG C; dropwise adding 2-4mol / L of sulfonating reagent, and controlling the dropwise adding speed to enable the temperature of the reaction system to be less than or equal to 0 DEG C; after dropwise adding, continuously reacting at 0-5 DEG C for 2-4 hours; and then adjusting the pH value of the reaction system to 6.5-7.5, precipitating and separating out the product, filtering out the precipitate, and washing off impurities. And dissolving the obtained solid with a polar protic solvent to form a solution with the concentration of 50%, and mixing the solution with a non-polar solvent according to the volume ratio of 1: 1 to obtain the target molybdenum extraction reagent NP192 for the alkaline system. The molybdenum extraction reagent NP192 prepared through the method is high in separation efficiency, good in selectivity, good in long-term stability and wide in applicable pH value range, the recovery efficiency of molybdenum can be remarkably improved, meanwhile, raw materials are easy to obtain, the technological process is simple, the waste liquid treatment cost is low, and the method has extremely high application and popularization value.

The present invention is directed to a method for preparing a cell penetrating peptide-cargo formulation, said method comprising providing the cell penetrating peptide in ethanol without an aprotic solvent, associating the cell penetrating peptide with a nucleic acid cargo in an association buffer comprising 30-90% sucrose (in particular 50-90% sucrose) at a ratio of 3:1 to the cell penetrating peptide in ethanol, and storing the cell penetrating peptide-cargo formulation at -70°C or below, wherein associating is performed in a volume between 0.5x and 0.1x the final volume at which the formulation is prepared for administration. The formulation may also be lyophilised. Also provided are cell penetrating peptide-cargo formulations obtainable and / or obtained by the method herein, pharmaceutical compositions comprising the formulations, and said formulations and pharmaceutical compositions for use in the transport of the cargo across a lipid membrane and delivery of the cargo into a cell or for use in raising an immune response in a subject.

The invention provides bio-based polyimide as well as a preparation method and application thereof, and belongs to the technical field of polyimide. The preparation method comprises the following steps: adding a dianhydride monomer containing tetrahydrocurcumin and a diamine monomer containing tetrahydrocurcumin into a polar aprotic solvent, heating to a first temperature for reaction, then heating to a second temperature for reaction, cooling to room temperature, pouring the system into ethanol, filtering, precipitating ethanol Soxhlet extraction, and drying to obtain the bio-based polyimide. The bio-based polyimide material prepared in the invention has good flexibility, gas permeability, light transmittance, solvent resistance and corrosion resistance, not only has good mechanical properties, electrical properties and high and low temperature resistance, but also has good antibacterial and antioxidant effects, high biocompatibility and wide application prospects.

The invention discloses a preparation and purification method of high-purity tris (dimethylamino) silane. The preparation and purification method comprises the steps of reactive distillation, crude product separation, product purification, desolvation recovery and neutralization recovery. Through aprotic solvent solubility and hydrodynamic design, the problem of blockage is radically solved; the T3 tower high vacuum is adopted to guarantee the purity of a thermosensitive substance, and the T4 high vacuum is adopted to realize near zero loss of a solvent; by adopting triple material circulation, the raw material utilization rate is greater than or equal to 98%, the solvent recovery rate is greater than or equal to 99.8%, and the industrial cost can be reduced by 32%.

The invention relates to the technical field of p-fluorobenzaldehyde production, and particularly discloses a production process of high-purity p-fluorobenzaldehyde. The invention relates to a production process of high-purity p-fluorobenzaldehyde. The production process comprises the following steps: S1, carrying out a chlorination reaction by taking p-fluorotoluene and chlorine as raw materials to prepare a mixed chlorination solution of p-fluoromethyl benzyl monochloride, p-fluoromethyl benzyl dichloride and p-fluoromethyl benzyl trichloride; s2, adding an organic complexing agent, which is a water-soluble aprotic solvent, into the mixed chlorinated liquid prepared in the step S1, and then performing vacuum rectification to obtain distillate and residual liquid; rectifying by taking the residual liquid as a raw material to obtain kettle liquid and rectified liquid; and S3, carrying out hydrolysis reaction by taking the rectification liquid and water as raw materials, separating, and drying to obtain the product. The production process of the high-purity p-fluorobenzaldehyde has the advantages of high raw material conversion rate, high product purity and few three-waste products.

The present application relates to the technical field of chemical medicine preparation, and particularly relates to a preparation method of tetrabromophenol tetrahalosulfonophthalein, which is prepared from 3,4,5,6-tetrahalophenol sulfonophthalein as raw material, organic carboxylic acid in aqueous solution, liquid bromine, oxidation by hydrogen peroxide to obtain tetrabromophenol tetrahalosulfonophthalein crude product, then salification with alkali salt in an aprotic solvent to obtain tetrabromophenol tetrahalosulfonophthalein salt; and then acid conversion with organic carboxylic acid in aqueous solution, recrystallization to obtain tetrabromophenol tetrahalosulfonophthalein pure product; the present application provides a preparation method of tetrabromophenol tetrahalosulfonophthalein, which is low in cost, high in yield and purity, simple in method, mild in condition, high in yield and purity, and beneficial to mass production.

The invention provides a preparation method of 3-trifluoromethylpyridine, and relates to the technical field of preparation of trifluoromethylpyridine intermediates. 3-methylpyridine (3MP) and a polar aprotic solvent are mixed and then introduced into a micro-channel reactor to react with fluorine / nitrogen mixed gas, and the product 3-trifluoromethylpyridine (3-TF) is separated from the solvent through a three-stage vacuum distillation process. Compared with the conventional synthesis technology, the method provided by the invention has the advantages of high reaction yield, easiness in operation, low energy consumption, solvent recycling, high economical efficiency and the like.