140 results about "Thionyl chloride" patented technology

The invention belongs to the technical field of sulfonamide synthesis, and particularly relates to a green and environment-friendly sulfonamide amidation preparation method. Comprising the following steps: adding chlorosulfonic acid into a reactor, stirring, heating, adding o-nitrochlorobenzene, carrying out staged heat preservation, cooling, and adding thionyl chloride to obtain 2-nitro-4-chlorine sulfonate-chlorobenzene; the method comprises the following steps: separating and filtering 2-nitro-4-chlorine sulfonate-chlorobenzene, adding ammonia water, stirring, preserving heat, and carrying out filter pressing to obtain 2-nitro-4-amine sulfonate-chlorobenzene; the preparation method comprises the following steps: adding liquid caustic soda into 2-nitro-4-amine sulfonate-chlorobenzene, stirring, heating, and adjusting the pH value to obtain 2-nitro-4-amine sulfonate-phenol; the method comprises the following steps: adding water, a catalyst and hydrazine hydrate into 2-nitro-4-amine sulfonate-phenol, heating, stirring, and carrying out filter pressing to obtain 4-sulfonamide-2-amino-phenol. According to the preparation method of sulfonamide, generated tail gas is subjected to falling film absorption treatment, and the product prepared by the preparation method is high in purity.

The invention provides a method for producing 4, 4 '-dichlorodiphenyl sulfone by continuous reaction of a microchannel reactor, which comprises the following steps: uniformly mixing thionyl chloride and aluminum chloride to obtain a solution A; uniformly mixing hydrogen peroxide and glacial acetic acid to obtain a solution B; a first feeding pump and a second feeding pump are adopted for conveying chlorobenzene and a solution A into a first silicon carbide micro-channel reactor for reaction, an outlet of the reactor is connected with a gas-liquid separator, through separation, a gas phase is used for preparing a byproduct hydrochloric acid, and a liquid phase is a chlorobenzene solution of 4, 4 '-dichlorodiphenyl sulfoxide; and continuously conveying the chlorobenzene solution of 4, 4 '-dichlorodiphenyl sulfoxide to the second silicon carbide microchannel reactor by adopting a third feeding pump, and meanwhile, conveying the solution B to the second silicon carbide microchannel reactor by adopting a fourth feeding pump for reaction to prepare 4, 4'-dichlorodiphenyl sulfone. Compared with the prior art, the micro-channel reactor is used for continuous production, the mass and heat transfer effect is good, impurity generation is effectively inhibited, and the reaction time is shortened.

The invention discloses a preparation method of 3-quinuclidinone hydrochloride, which comprises the following steps: carrying out temperature control reaction on 4-picolinic acid and chloroacetic acid under alkaline water conditions to obtain an aqueous solution of a compound a, and directly entering the next reaction without post-treatment after the reaction is finished; adding a reducing agent alkaline water system into the aqueous solution of the compound a, controlling the temperature to react, controlling the temperature to adjust the pH value to 5-5.5 after the reaction is finished, extracting with n-butyl alcohol, and drying to obtain an n-butyl alcohol solution of a compound b, and directly entering the next reaction step; wherein the reducing agent is one of sodium borohydride and potassium borohydride; dropwise adding thionyl chloride into an n-butyl alcohol solution of the compound b, controlling the temperature to react after dropwise adding is ended, and concentrating to remove the solvent and unreacted thionyl chloride after the reaction is ended, so as to obtain a compound c; carrying out Dieckmann condensation reaction on the compound c at controlled temperature under the condition of organic alkali by using toluene as a solvent, carrying out hydrochloric acid quenching reaction after the reaction is finished, and directly carrying out next-step reaction after extracting and removing impurities from a water phase containing a hydrochloride solution of a compound d by using toluene; and carrying out a decarboxylation reaction on the compound d in a hydrochloric acid aqueous solution at controlled temperature, after the reaction is finished, adjusting the pH value to 10-13, extracting, and salifying to obtain a target compound TM, namely 3-quinuclidinone hydrochloride. The preparation method of 3-quinuclidinone hydrochloride provided by the invention has the advantages of economical and easily available raw materials, mild reaction conditions, efficient reaction, simple operation and low cost, and is suitable for industrial application.

This invention provides a method for preparing and applying a highly insecticidal diamide compound, relating to the chemical and pesticide fields. The method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; and, during the reaction under a hydrogen atmosphere, determining the reaction temperature and hydrogen flow rate in each hydrogenation reaction zone based on the concentration of compound B; reacting compound C with paraformaldehyde to obtain compound D; chlorinating 3-chloro-4-fluorobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound E; and amide condensing compound E with compound D to obtain the novel diamide compound of this invention. The diamide compound of this invention exhibits excellent insecticidal effects when used in pesticide compositions.

The invention provides a preparation method of fluoride ether bacteria amide, which comprises the following steps: dissolving pentafluorobenzonitrile in a solvent, dropwise adding a sodium methoxide solution at-10-30 DEG C for 2-15 hours, continuing to carry out heat preservation reaction for 0.5-2 hours after dropwise adding, and carrying out post-treatment to obtain 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile; the preparation method comprises the following steps: jointly dissolving 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile, 3-chloro-5-(trifluoromethyl) pyridine-2-yl) methanol and a catalyst acid in a solvent, reacting at 50-110 DEG C for 5-32 hours, and performing post-treatment on the obtained reaction liquid to obtain fluoride ether bacteria amide, according to the method, sodium methoxide and pentafluorobenzonitrile which are low in price and easy to obtain are subjected to etherification reaction, thionyl chloride and bis (trichloromethyl) carbonate are not used, the green chemical principle is met, and the method has the advantages of being short in step, safe and easy to operate and the like, so that the method has high implementation value and practical production applicability.

This invention discloses a magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd, its preparation method, and its applications. Using an amino alcohol as a starting material, an imidazole derivative containing a hydroxyl group on the N-substituent is obtained through a condensation and ring-closing reaction. This derivative is then subjected to substitution reactions with thionyl chloride and cyclohexanethiol sequentially to obtain an imidazole derivative containing a thioether on the N-substituent. This derivative is then reacted with 1,3-dibromopropane to obtain an N-bromopropyl-N'-cyclohexane thioether-substituted imidazole bromium salt. This salt is then reacted with Pd(OAc)₂ or PdCl₂ via a direct metallization reaction to obtain the N-bromopropyl-substituted thioether-chelated nitrogen heterocyclic carbene palladium complex NHC-Pd. The NHC-Pd complex is then reacted with amino-functionalized magnetic nanoparticles (MNPs-NH₂) to prepare the magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd. It not only possesses the activity of homogeneous nitrogen heterocyclic carbene palladium catalysts, but also has a simple synthesis method, high yield, and is easy to separate and reuse in catalytic C-C bonding reactions, showing good application prospects in the field of catalysis.

The invention discloses a solvent removal process and a crude product post-treatment method in isophthaloyl chloride / paraphthaloyl chloride production, and belongs to the technical field of chemical processes. A three-stage gradient condensation system is adopted, circulating water, chilled water and chilled saline water are respectively introduced, the recovery rate of thionyl chloride is improved, thionyl chloride is prevented from entering a subsequent vacuum unit, the equipment failure rate is reduced, and the annual overhaul frequency is reduced. A top condenser is arranged, hot water at the temperature of 50-55 DEG C (suitable for producing isophthaloyl dichloride) or hot water at the temperature of 85-90 DEG C (suitable for producing paraphthaloyl dichloride) is adopted as a cooling medium, so that isophthaloyl dichloride / paraphthaloyl dichloride is efficiently captured, and coagulum is thoroughly prevented from entering a subsequent system and blocking equipment and pipelines.

The invention belongs to the field of organic chemical synthesis, and particularly relates to a synthesis method of triaryl sulfonium salt, which comprises the following steps: (1) dissolving a catalyst: dissolving the catalyst in an organic solvent in a preparation kettle in advance to form a uniform solution; and (2) continuous feeding and reaction: enabling reactants thionyl chloride and an aromatic hydrocarbon derivative and the catalyst-containing solution obtained in the step (1) to pass through a continuous reactor at a controllable flow rate, firstly carrying out Friedel-Crafts acylation reaction in an all-solvent system, then heating to carry out addition reaction, and finally obtaining the triaryl sulfonium salt. According to the invention, the problem of solid-liquid non-uniformity is eliminated, and the reaction efficiency and reproducibility are improved; the reaction is fast and uniform, and local overheating and out-of-control risks are avoided.

This invention belongs to the field of insecticide technology, specifically relating to a diamide compound, its preparation method, intermediate preparation equipment, and applications. The preparation method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride in the presence of dimethylformamide to generate compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; substituting compound C with formaldehyde to obtain compound D; and condensing compound D with 3,5-dichloro-4-fluorobenzoyl chloride to obtain the diamide compound. The beneficial effects of this invention are: the diamide compound solves the problem of insecticide resistance and possesses high insecticidal activity, exhibiting good insecticidal effect at low doses. Furthermore, the preparation method uses mild reaction conditions, produces few byproducts, and has a high reaction yield, reducing raw material loss and thus lowering production costs.

The invention relates to the technical field of synthesis of ester compounds, in particular to a preparation method of an ester compound based on a sulfur trioxide compound. The method comprises the following steps: by taking a sulfur trioxide compound as a carboxylic acid activating agent and taking a carboxylic acid-containing compound and a hydroxyl-containing compound as raw materials, carrying out esterification reaction at room temperature in a reaction system of an alkali substance, a sodium salt stabilizer and a solvent, activating carboxylic acid by sulfur trioxide to form an active intermediate, and reacting the active intermediate with hydroxyl to generate an ester compound. The ester compound based on the sulfur trioxide compound is obtained, and sodium sulfate precipitate is obtained at the same time. According to the method, acyl chloride, thionyl chloride or unstable condensation reagents with high corrosivity are not used in the reaction, chlorine-containing wastewater is not generated, the reaction is carried out at room temperature, heating or high temperature is not used, the reaction condition is mild, the product is easy to separate, the use of organic solvents can be effectively reduced through post-treatment, and the product yield is relatively high.

A method includes providing, within an etch chamber, a base structure including a target layer disposed on a substrate, and an etch mask disposed on the target layer, dry etching, within the etch chamber, the target layer using thionyl chloride to obtain a processed base structure, and after forming the plurality of features. The processed base structure includes a plurality of features and a plurality of openings defined by the etch mask. The method further includes removing the processed base structure from the etch chamber. In some embodiments, the target layer includes carbon. In some embodiments, the dry etching is performed at a sub-zero degree temperature.

The utility model discloses a continuous reaction device for producing bis (chlorosulfonyl) imide, which belongs to the technical field of chemical equipment and comprises a horizontal reaction tank and a heat preservation tank, a feed port of the reaction tank is connected with a mixed feed liquid pipe, and a discharge port of the reaction tank is connected with the heat preservation tank through a conveying component; heating layers are arranged outside the reaction tank and the heat preservation tank, a plurality of communicated areas are arranged in the reaction tank and the heat preservation tank, a stirrer is arranged in each area, and a chlorosulfonic acid feeding hole is formed in the top of each area of the reaction tank; a discharge hole of the heat preservation tank is connected with the distillation device; exhaust pipes and condensation reflux assemblies are arranged at the tops of the reaction tank and the heat preservation tank. The chlorosulfonic acid is added into each area of the reaction tank in a multi-drop mode, the reaction tank heats materials through the heat preservation layer to ensure the temperature needed by reaction, and the materials enter the heat preservation tank to be subjected to continuous heat preservation to ensure full reaction of the materials; thionyl chloride in gas exhausted from the reaction tank and the heat preservation tank is cooled and recycled through the condensation backflow assembly, the production efficiency is improved, raw material waste is reduced, and the production cost is reduced.

A method of ALE etching of a III-V material including the following steps: a) placing in an enclosure a structure including a layer of III-V material, b) implementing, in the enclosure, at an etching temperature, one or more times the following ALE cycle: oxidizing a surface of the layer of III-V material with an oxidizing gas, whereby an oxide layer is formed, purging the enclosure with an inert gas flow, exposing the formed oxide layer to thionyl chloride vapor to etch the oxide layer, and purging the enclosure with an inert gas flow.

The invention discloses a degradable environment-friendly fiber and a preparation method thereof, and relates to the field of fibers. When the degradable environment-friendly fiber is prepared, triethyl phosphite firstly reacts with 3-(2-bromoethyl) thiophene and then reacts with dimethyl terephthalate and ethylene glycol, and modified polyester is prepared; the preparation method comprises the following steps: enabling chitosan oligosaccharide to react with 4-hydroxy-3-pyridylaldehyde, thionyl chloride and 2-(dimethylaminomethyl) thiophene in sequence, so as to prepare functionalized chitosan oligosaccharide; mixing the functionalized chitosan oligosaccharide, zinc acetate and modified polyester, and performing melt spinning to obtain composite fibers; mixing thiophene, ferric chloride and trichloromethane to prepare a thiophene solution; and immersing the composite fiber in a thiophene solution, and drying to obtain the degradable environment-friendly fiber. The degradable environment-friendly fiber prepared by the invention has excellent flame retardance, antibacterial property, antistatic property and light aging resistance.

The invention discloses a preparation method of an LH-1801 key intermediate, and belongs to the field of medicine synthesis. The preparation method comprises the following steps: enabling SM1 and NBS to react in an acid solution to obtain a compound 1; catalyzing the compound 1 and NBS in an organic solvent in the presence of a catalyst to obtain a compound 2; catalyzing the compound 2 and thionyl chloride in the presence of a catalyst to obtain a compound 3; performing Friedel-Crafts reaction on the compound 3 and 2-ethylthiophene in an organic solvent under the catalysis of a catalyst to obtain a compound 4; reacting the compound 4 with triethyl silane and boron trifluoride diethyl etherate in an organic solvent to obtain a compound 5; reacting the compound 5 with a salt solvent in an organic solvent to obtain a compound 6; and finally, reacting the compound 6 with an alkali solvent in an organic solvent to obtain a compound 7, namely the LH-1801 intermediate. According to the method, 2-chloro-4-methyl benzoic acid is used as a starting material, the intermediate steps are simple and mild reactions, the operation difficulty is low, the reaction risk is low, and the method is suitable for industrial production.

The invention relates to the technical field of organic synthesis, in particular to a method for preparing 4-nitro-N-phenylbenzamide by a one-pot process, which comprises the following steps: under the protection of inert gas, adding an inert solvent, p-nitrobenzoic acid and a composite catalyst into a reactor, and heating to dissolve, the composite catalyst comprising NFM and TPPO; slowly adding thionyl chloride into a reaction system for acylation reaction; then slowly adding aniline into the reaction system to carry out condensation reaction; and after the reaction is finished, carrying out post-treatment to obtain the 4-nitro-N-phenylbenzamide. According to the method, one-pot reaction can be realized, and high-risk intermediates do not need to be separated. In the composite catalyst, NFM efficiently catalyzes acylating chlorination, and TPPO stabilizes an acyl chloride intermediate and promotes condensation, so that the reaction is performed efficiently, stably and highly selectively, and the product is high in yield and purity. And the catalyst is easy to recycle, and the process is green, safe, economical and suitable for industrial production.

The invention discloses a novel bismuth-based chelate CT contrast agent and a preparation method and application thereof. The synthesis method comprises the following steps: reacting 2, 6-pyridine dimethyl carbinol with thionyl chloride to obtain 2, 6-bis (chloromethyl) pyridine; the preparation method comprises the following steps: carrying out a heating reaction on 2-(4-methylphenyl)-1, 2, 4-triazine-2-ketone, N, N ', N'-tri (p-toluenesulfonyl) diethylenetriamine and an inorganic base in a solvent, and carrying out concentrated sulfuric acid deprotection to obtain an intermediate pyclen; the preparation method comprises the following steps: heating and reacting pyrene and halogenated carboxylic ester in a polar organic solvent under an alkaline condition, and hydrolyzing to obtain a ligand product; and heating and chelating the ligand product and a bismuth agent to prepare the target bismuth-based chelate. Laboratory large-scale preparation of the small-molecule bismuth-based chelate CT contrast agent is achieved, and the prepared nonionic contrast agent has low osmotic pressure, high stability, high water solubility and good biological safety and is used for CT imaging of digestion, urinary and circulatory systems.

This invention provides a method for preparing high-purity olaparib, belonging to the field of pharmaceutical synthesis technology. The method uses dimethyl (3-oxo-1,3-dihydroisobenzofuran-1-yl)phosphate as the starting material, reacting it with compound 2 via a Wittig reaction to generate compound 3. Compound 3 reacts with hydrazine hydrate to generate compound 4. Compound 4 is hydrolyzed and acidified to give compound 5. Compound 5 reacts with thionyl chloride to give compound 6. Compound 6 is then condensed with compounds 7 and 9 to obtain olaparib. This invention uses readily available raw materials, is simple to operate and process, has mild reaction conditions, achieves a total yield of up to 90%, a purity >99%, is environmentally friendly, and is suitable for industrial production.

This invention discloses a synthetic process for an empagliflozin intermediate, belonging to the technical field of pharmaceutical intermediate synthesis. The synthetic process is as follows: 2-chloro-5-bromobenzoic acid is first mixed with dichloromethane and N,N-dimethylformamide, and thionyl chloride is added dropwise to obtain a dichloromethane solution of acyl chloride. Then, it is reacted with fluorobenzene under anhydrous aluminum trichloride catalysis to obtain intermediate EGAB-3. Then, it is dehydrated by azeotropic reaction with potassium hydroxide aqueous solution in toluene, and then refluxed with 3-hydroxytetrahydrofuran under tetrabutylammonium bromide catalysis to obtain intermediate EGAB-7. Then, it is reacted with 1,1,3,3-tetramethyldisiloxane under anhydrous aluminum trichloride and nitrogen protection, dried, and tested to be qualified to obtain empagliflozin intermediate. This process achieves high purity, high yield, and low isomer impurities in the preparation of empagliflozin intermediate.

Provided is a method for producing an anhydrous cyclic phosphonic acid by reacting phosphonic acid (A) with a basic compound (B) and at least one type of halogenating agent (C) selected from thionyl chloride, phosphoryl chloride, and oxalyl chloride. Also provided is a method for producing a phosphonic acid monoester by reacting the anhydrous cyclic phosphonic acid obtained by said production method with an alcohol.

The invention relates to a continuous preparation method of pentaerythritol bisulfite, which comprises the following steps: respectively and continuously introducing pentaerythritol emulsion and thionyl chloride into a continuous flow oscillation stirring reactor for continuous flow reaction, controlling the reaction temperature to be 40-90 DEG C, controlling the temperature to be 40-90 DEG C, and controlling the reaction time to be 1-3 hours; the stirring rotating speed is 200 to 800 r / min, the reaction pressure is 0.3 to 0.8 MPa, and the reaction time is 30 to 120 minutes. By using the continuous flow oscillation stirring reactor and specific reaction conditions, the continuous preparation is realized, and the pentaerythritol conversion rate, the product yield and purity, the reaction efficiency and the post-treatment simplicity are considered at the same time. The method has the remarkable advantages of simple process, low reaction operation difficulty, high reaction efficiency and the like, and can meet the comprehensive requirements of large-scale continuous industrial production on efficiency, cost and product quality.

The invention provides a multifunctional bottom film integrated forming machine for a lithium thionyl chloride battery. The workpiece conveying assembly is arranged above the base and comprises two conveying belts which are sequentially arranged and consistent in conveying direction, a machining area is arranged between the two conveying belts in a spaced mode, and the steel shell can be conveyed to the machining area from the previous conveying belt and conveyed to the next conveying belt to be conveyed after being machined in the machining area; the workpiece clamping and lifting assembly is arranged at the machining area between the two conveying belts and comprises a lifting plate capable of ascending and descending, a fixed clamping piece is fixed to the surface of the lifting plate, and a movable clamping piece capable of horizontally moving is arranged on the other side, opposite to the fixed clamping piece, of the surface of the lifting plate. The full-automatic lithium thionyl chloride battery steel shell bottom membrane machining device integrates multiple functions of workpiece conveying, automatic positioning, stable clamping, membrane cutting, accurate membrane pressing and the like, and full-automatic operation in the lithium thionyl chloride battery steel shell bottom membrane machining process is achieved.

A battery health and depassivation testing apparatus includes a timed switch electrically connected to the positive terminal of the battery and a timer circuit to control the timed switch while conducting the battery test, a test initiation switch and a test-in-progress indicator. During the test the battery is connected to a current sink circuit to establish a load condition for a predefined period of time. A comparator is used to test the battery's voltage to a known DC voltage following the load condition. Pass / fail indicator LEDs are provided to display the results of the test. The battery health and depassivation testing apparatus also includes a polarity protection circuit connected to a polarity error indicator to prevent damage to the circuitry due to the battery being installed backwards.

This application provides an apparatus for the acylation synthesis of oxazolidinone, comprising a first reaction vessel, a second reaction vessel, a neutralization vessel, a washing vessel, and a solvent removal vessel connected in series. In the first reaction vessel, a first substrate reacts with thionyl chloride to generate the corresponding acyl chloride. The resulting acyl chloride is then added to the second reaction vessel to react with a second substrate to obtain oxazolidinone. Acid is then added via an acid metering pump for acidification. The acidified reaction is then transferred to the neutralization vessel for neutralization with alkali. Finally, the neutralized reaction solution is subjected to vacuum solvent removal in the solvent removal vessel to obtain dried oxazolidinone. The apparatus of this application, through the combined use of the above equipment, provides an effective industrial production route for oxazolidinone, and is characterized by its ease of operation.

The invention discloses a thionyl chloride device rectification thermal coupling system, which comprises a heavy component removal tower, a light component removal tower and a product tower, the tower bottom of the heavy component removal tower is equipped with a heavy component removal tower reboiler, the tower bottom of the light component removal tower is equipped with a light component removal tower reboiler, and the tower bottom of the product tower is equipped with a product tower reboiler; high-temperature hot steam is introduced into a shell pass inlet of the heavy component removal tower reboiler, steam condensate after heat exchange enters a shell pass of the light component removal tower reboiler, a gas phase at the top of the heavy component removal tower enters a shell pass of the product tower reboiler to supply heat, the temperature of the bottom of the heavy component removal tower is controlled to be 130-135 DEG C, the temperature of the bottom of the light component removal tower is controlled to be 70-75 DEG C, and the temperature of the bottom of the product tower is controlled to be 50-65 DEG C. According to the invention, the defects of the prior art are overcome, the thermal coupling mode is changed, the energy is recycled, the production cost is reduced, the production efficiency is greatly improved, the reaction efficiency and the material utilization rate of the whole production process are optimized, the economic benefits of enterprises are increased, and the method has higher social use value and application prospect.

The invention discloses a novel photoinitiator as well as a preparation method and application thereof, a thiophenol group substituted by methyl, ethyl or isopropyl is introduced into a molecular structure of the photoinitiator, so that the absorption wavelength of the photoinitiator is adaptive to a UV-LED light source of 365-405nm, and the problem that the existing photoinitiator is insufficient in matching with the UV-LED light source is solved. The preparation method comprises the following steps: carrying out acylating chlorination on 2, 4, 6-trimethylbenzoyl phenylphosphonic acid through thionyl chloride, condensing the 2, 4, 6-trimethylbenzoyl phenylphosphonic acid and substituted p-thiophenol in an organic solvent, and purifying to obtain a target product, and the preparation process is simple and convenient to operate and suitable for industrial production. The obtained photoinitiator shows good compatibility and efficient curing efficiency in a UV-LED photocuring system, can be widely applied to the fields of printing ink, photocureable coatings, UV adhesives and the like, and has important significance in promoting popularization of a UV-LED curing technology.

This application provides a method for preparing methyl 5-aminolevulinate hydrochloride and the same, relating to the field of methyl 5-aminolevulinate hydrochloride preparation technology. Methanol is added to a reaction vessel, the temperature is lowered to 0-10°C, and thionyl chloride is added dropwise under controlled temperature. After the addition is complete, the mixture is kept at a constant temperature and stirred to obtain a reaction solution. The pH of the reaction solution is controlled to 1.5-2.5 by vacuum distillation. 5-aminolevulinate salt is added to the reaction solution, the temperature is raised to 60-65°C, and the mixture is refluxed and stirred. A crystallization promoter is added to the system, and crystallization is stirred, filtered, and dried to obtain methyl 5-aminolevulinate hydrochloride. The preparation method of this application allows for sufficient contact between the components in the reaction system, while effectively controlling side reactions and reverse reactions. The purity of the obtained product can reach over 99%, and the yield can reach over 84%. This overcomes the high energy consumption problem caused by traditional high-temperature reactions, significantly reducing energy consumption and production costs.

The invention discloses a quaternized COFs (Covalent Organic Frameworks) material as well as a preparation method and application thereof. The preparation method comprises the following steps: carrying out acylating chlorination reaction on betaine and thionyl chloride to prepare acylating chlorinated betaine; reacting the acylated and chlorinated betaine with dimethyl 2-aminoterephthalate or dimethyl 5-aminoisophthalate, so as to prepare a hydrazide precursor grafted with a quaternary ammonium group; performing hydrazide treatment on the hydrazide precursor grafted with the quaternary ammonium group to prepare a hydrazide monomer containing a quaternary ammonium structure; and enabling the hydrazide monomer containing the quaternary ammonium structure to react with 2, 4, 6-triformyl phloroglucinol by adopting solvothermal, so as to prepare the quaternized COFs material. The quaternized COFs material disclosed by the invention is low in synthesis difficulty, relatively low in cost, uniform in reaction, high in grafting efficiency and suitable for large-scale preparation; meanwhile, the adsorption performance of the prepared quaternized COFs material is greatly improved.

To break passivation coat formed on an electrode of a battery.SOLUTION: An electronic apparatus has: an operation circuit including a thionyl chloride-lithium battery, a coat peeling circuit including a first switching element, energizing the first switching element at an ON state, and peeling coat formed on an electrode of the thionyl chloride-lithium battery by energization, and an operation part including a second switching element, and operated by supplying current from the thionyl chloride-lithium battery when the second switching element is in an ON state; and a switchover part making the second switching element the ON state from an OFF state after making the ON state of the first switching element the OFF state. In a presence of instructions from a user after making the second switching element the OFF state from the ON state, the switchover part makes the first switching element the ON state according to a predetermined condition.SELECTED DRAWING: Figure 1

The invention relates to the technical field of batteries, and discloses an electrolyte preparation method, an electrolyte, an ultrahigh-power lithium thionyl chloride battery and a manufacturing method. The method comprises the following steps: adding solid anhydrous gallium chloride and anhydrous lithium chloride into a round-bottom flask in an argon protection environment, and heating to melt the anhydrous gallium chloride and the anhydrous lithium chloride into liquid; after the round-bottom flask is cooled, thionyl chloride is added into the round-bottom flask and stirred to be partially dissolved, then chlorosulfonic acid is added so that transparent floccules can appear in the solution in the round-bottom flask, a condensation reflux device is installed on the round-bottom flask, and the round-bottom flask is heated so that the transparent floccules in the solution can be completely dissolved. The method comprises the following steps: adding a metal elementary substance lithium sheet into a round-bottom flask in an environment with the relative humidity of less than 1%, installing a condensation reflux device, heating to remove impurities in a solution, cooling the round-bottom flask, enabling sulfur dioxide to sequentially pass through a concentrated sulfuric acid and calcium chloride scrubbing device, and then introducing the sulfur dioxide into the round-bottom flask to remove moisture in the solution so as to prepare the electrolyte.