58 results about "Phase-transfer catalyst" patented technology

This invention discloses a method for synthesizing dialkylphosphinates, belonging to the field of organic synthesis technology. The method uses hypophosphite and haloalkanes as starting materials. First, a hypophosphite is generated through a heated and pressurized reaction under the action of a phase transfer catalyst. The obtained hypophosphite does not require complex purification; it is directly reacted with an olefin under heated and pressurized conditions in the presence of a free radical initiator to obtain the target product, dialkylphosphinate. The method of this invention uses inexpensive and readily available raw materials, has a simple process route, includes only two core reactions, operates under mild conditions, is safe and convenient, produces few and easily treatable byproducts, has a high product yield, and is simple to purify. It is very suitable for large-scale industrial production, providing an economical and efficient synthetic route for the preparation of high-performance halogen-free flame retardants.

The application relates to a preparation method and application of a performance-adjustable reactive cationic polymer, and belongs to the field of textile printing and dyeing. The preparation method of the performance-adjustable reactive cationic polymer comprises the following process steps: mixing an epoxy reactive monomer with concentrated hydrochloric acid, reacting for a certain time under ice bath, and adjusting the pH of the reaction system to be neutral; adding a cationic monomer into the above reaction system, simultaneously adding a phase transfer catalyst or an organic solvent, adding an initiator drop by drop under a nitrogen atmosphere, stirring to carry out a free radical polymerization reaction, naturally cooling after the reaction is completed, and drying to obtain the reactive cationic polymer. According to the application, salt-free high-color-yield dyeing of reactive dyes can be realized when the amount of the cationic polymer is very low.

This invention discloses a method for preparing high-purity Si-75, comprising: S1, adding sodium sulfide, sulfur, and deionized water in a molar ratio of 1:(1.0~1.1):(5~8) to a reaction vessel, adding a buffer, and reacting at 80~90℃ for 1~2h; S2, adding a phase transfer catalyst and a hydrolysis inhibitor to the system, adding γ-chloropropyltriethoxysilane dropwise, and reacting at 85~95℃ for 3~5h, allowing the mixture to stand and separate into layers after the reaction, to obtain an organic phase; S3, subjecting the organic phase to short-path distillation and then filtering to obtain high-purity Si-75. Compared with existing technologies, this invention uses a phosphorus-free buffer system, which simplifies waste treatment. It uses water as the reaction medium and does not use large amounts of organic solvents, making it suitable for continuous industrial production. By adding hydrolysis inhibitors, hydrolysis can be effectively prevented during the reaction, increasing safety. The short-path distillation method provides high purification efficiency and can quickly remove impurities. The product has a disulfide content of ≥98.5% and a color of 0 (Gardner color number), which is of great significance to the light-colored rubber industry.

This invention discloses a low-allergenic, high-activity powder coating curing agent and its preparation method, relating to the field of powder coating technology. The preparation method includes: mixing isocyanuric acid, epichlorohydrin, and an addition reaction catalyst including a phase transfer catalyst to perform an addition reaction; subsequently adding a base to perform a ring-closure reaction; allowing the mixture to stand and separate into layers to obtain a lower crude product; subjecting the lower crude product to vacuum distillation to obtain a distilled product; adding a solvent to the distilled product, stirring to dissolve, and then adding hydrogenated vegetable oil to form a coated crystallization system; followed by cooling crystallization, separation, and drying to obtain the final product. This invention, through the combination of addition ring closure, vacuum distillation, and in-situ oil phase crystallization coating, not only suppresses side reactions at the source and deeply removes harmful residues, significantly reducing the free epichlorohydrin residue in the finished product and almost completely eliminating skin and respiratory sensitization toxicity; but also effectively stabilizes the single-crystal regular crystal form, significantly narrows the melting range, and greatly enhances the activity of the curing agent.

Provided is a method for preparing Compound II, wherein the method includes the following steps: using Compound I as a raw material, performing a reaction under the action of an organometallic catalyst and a phase transfer catalyst, and oxidizing with hydrogen peroxide to obtain Compound II. The catalyst utilized in the present application exhibits remarkably high activity for the oxidation of sulfur ether compounds, leading to the preparation of sulfone compounds. The method for preparing Compound II significantly reduces the amount of catalyst required, effectively diminishing the consumption of non-renewable scarce strategic resources, while concurrently reducing the potential hazards to the natural environment. The novel method exhibits a substantial reduction in the amount of catalyst required, leading to a concurrent decrease in the consumption of non-renewable resources. Concurrently, it significantly mitigates potential harm to the natural environment and human health. The solvent utilized in this method is easy to be recycled and reused, and enhances overall process efficiency by reducing resource consumption, waste generation, and treatment costs, thereby rendering it more suitable for industrial production.

The application discloses a preparation method and application of a naphthalene phenolic epoxy resin, and the preparation method comprises the following steps: performing etherification reaction on a phenol containing a naphthalene ring structure, epichlorohydrin, a cosolvent I and an etherification catalyst, and performing post-treatment to obtain a naphthalene chlorohydrin ether; adding a cosolvent II, an aldehyde compound and a phenolic aldehyde condensation catalyst to perform polycondensation reaction, separating waste water, and obtaining a naphthalene phenolic chlorohydrin ether organic phase solution; adding the cosolvent II and dropwise adding a ring closure catalyst to perform ring closure reaction, and obtaining a naphthalene phenolic epoxy resin crude product; and dissolving the naphthalene phenolic epoxy resin crude product in a cosolvent III, adding a refining catalyst and a phase transfer catalyst to perform refining reaction, and obtaining a naphthalene phenolic epoxy resin finished product. The naphthalene phenolic epoxy resin has a low epoxy equivalent weight, the heat resistance of a cured product is excellent, and the content of hydrolysis chlorine in the resin is low, so that the corrosion risk of a subsequent prepared circuit can be reduced.

This invention discloses a thiophene-based intrinsic flame-retardant epoxy resin and its preparation method, belonging to the field of flame-retardant materials technology. The invention uses thiophene derivatives as raw materials and reacts with epichlorohydrin in the presence of a phase transfer catalyst and alkaline substances via an epoxidation reaction to obtain the target epoxy resin. The sulfur-containing thiophene ring is directly embedded into the main chain framework of the epoxy resin molecule, achieving intrinsic flame-retardant modification at the molecular level. This invention solves the core problems of traditional bisphenol A type epoxy resins being flammable, existing additive flame-retardant modification techniques easily degrading the mechanical properties of the resin, and insufficient environmental friendliness. The prepared epoxy resin does not require the addition of additional flame retardants and possesses excellent flame retardancy, mechanical properties, and environmental friendliness, making it suitable for electronic and electrical packaging, composite material matrices, and other fields, with broad prospects for industrial application.

This invention belongs to the field of organic synthesis technology and discloses a method for preparing trans-3-chloro-2-propenylhydroxylamine hydrochloride. The method involves adding trans-1,3-dichloropropene to a ketoxime, a base, a phase transfer catalyst, and a first solvent for etherification. After the reaction, the mixture is first extracted with an extractant, and the resulting oil phase is then distilled to obtain the oxime ether. The oxime ether, an aqueous hydrochloric acid solution, and a second solvent are mixed and subjected to vacuum distillation in a distillation column to obtain trans-3-chloro-2-propenylhydroxylamine hydrochloride. This invention avoids the use of an aqueous base in the etherification stage, effectively preventing the hydrolysis of the ketoxime. The purified oxime ether obtained in the etherification step is purified by distillation, significantly reducing side reactions during the subsequent hydrolysis. Adding a solvent during the hydrolysis stage allows for better mixing of the aqueous hydrochloric acid solution and the oxime ether, resulting in more uniform acidification, a more complete reaction, and improved conversion and selectivity.

This invention relates to the field of acyclic or carbocyclic compounds and discloses a method for synthesizing sodium methyl methacrylate sulfonate. The method involves introducing an organic phase of methyl methacrylate and an aqueous phase of sodium sulfite into a microchannel reactor. A sulfonation reaction is carried out under the action of a phase transfer catalyst with a crown ether structure and a mixing unit. The reaction effluent is separated into layers by a continuous flow oil-water separator. The aqueous phase is concentrated and crystallized under reduced pressure. The mother liquor and oil phase are combined and extracted through a nanofiltration membrane for the phase transfer catalyst, which is then recycled. This method alleviates the limitations of two-phase mass transfer and local concentration segregation, reduces self-polymerization and eliminates side reactions, maintains the double bond structure of the product, and achieves closed-loop catalyst recycling.

This invention belongs to the field of fine chemical engineering and organic synthesis technology, and relates to a method for preparing high-purity 1,1-difluoro-2-iodoethylene. The method includes: firstly, in an aprotic organic solvent, under controlled low-temperature conditions, allowing vinylidene fluoride to undergo an addition reaction with iodine monochloride to obtain the intermediate 1-chloro-1,1-difluoro-2-iodoethane; subsequently, the intermediate undergoes a controlled elimination reaction in an alkaline aqueous solution, and the product is immediately removed by reactive distillation, finally purified by distillation to obtain the target product. This invention effectively controls the thermal effect of the addition reaction by introducing a specific solvent, suppressing side reactions such as iodine radical coupling, and eliminating the need for expensive metal catalysts or phase transfer catalysts. The process is simple and safe to operate, with an intermediate separation yield of over 95%, high overall yield, and high product purity, making it suitable for large-scale industrial production.

This invention provides a method for preparing pyrogallol A, relating to the field of photoresist materials technology. The method uses 2-phenyl-2-propanol as a starting material and obtains pyrogallol A in a one-pot process. Specifically, aluminum trichloride is added to dichloroethane and stirred to disperse, and acetyl chloride is added dropwise to obtain a complex solution. A dichloroethane solution of 2-phenyl-2-propanol is then added dropwise for reaction. Hydrochloric acid is added for quenching. Phenol, dodecyl mercaptan, and sodium dodecyl sulfate are then added, and the reaction is heated. After the reaction is complete, the mixture is kept at a constant temperature, filtered, washed, and dried to obtain pyrogallol A. The Friedel-Crafts reaction has a high conversion rate, and no post-processing or purification is required after quenching; condensation can be directly performed. Condensation is a heterogeneous reaction, and the reaction time is significantly shortened by adding a catalytic amount of phase transfer catalyst. The preparation method of this invention uses readily available raw materials, produces a product with high purity and high yield, has a short reaction time, is simple to operate, and is low in cost, while also reducing waste, making it suitable for industrial production.

The application discloses a kind of molybdenum bis (dibutyl dithiocarbamate) oxide and preparation method thereof, comprising the following steps: molybdenum trioxide, phase transfer catalyst and water are uniformly mixed, are sent into first-stage mixing reactor, sodium hydrosulfide, sodium thiosulfate and water are uniformly mixed, also are sent into first-stage mixing reactor, and first reaction solution is obtained by reaction;Di-n-butylamine and water are uniformly mixed, are sent into second-stage mixing reactor, carbon disulfide is simultaneously sent, and second reaction solution is obtained by reaction;First reaction solution, second reaction solution are respectively sent into third-stage mixing reactor and are reacted, obtain molybdenum bis (dibutyl dithiocarbamate) oxide solution, solid-liquid separation, drying, obtained immediately.The yield of product obtained by the application is high, the purity is high, the quality is stable, the whole reaction process is continuously carried out in airtight container, there is no gas volatilization, which is conducive to environmental protection, reaction solvent is water, resource consumption is less, can be recycled, clean and environmentally friendly.

This invention provides a method for synthesizing triphenylmethylolmesartan medoxomil, an intermediate of olmesartan medoxomil. The method includes hydrolyzing compound 2 in a toluene / C1-C4 lower alcohol mixed solvent under the action of an alkali to obtain a synthesis solution of an intermediate sodium salt; adding a carbonate and a phase transfer catalyst to the synthesis solution of the intermediate sodium salt to carry out a condensation reaction to obtain triphenylmethylolmesartan medoxomil. This invention effectively controls the content of impurity A in the product by using a toluene / C1-C4 lower alcohol mixed solvent system and inhibiting the high-temperature elimination reaction of hydroxyl groups by a protic alcohol solvent. This invention has a short production cycle, a simple process, and does not require changing or adding new solvents during the process, facilitating solvent recovery and reuse in industrial production and effectively reducing production costs. The synthesis method of triphenylmethylolmesartan medoxomil described in this invention has a high overall yield, high production efficiency, simple product purification, and good quality control.

This invention provides a method for preparing compound II. The method uses compound I as a raw material, reacting it under the action of an organometallic catalyst and a phase transfer catalyst in the presence of hydrogen peroxide oxidation to obtain compound II. The catalyst used in this invention exhibits extremely high activity for the preparation of sulfone compounds from sulfide oxides. This preparation method significantly reduces the amount of catalyst used, effectively reducing the consumption of non-renewable and scarce strategic resources, while greatly reducing potential harm to the natural environment and human health. The solvent used is easily recyclable and reusable. The overall process is more efficient, consumes fewer resources, produces less waste, and has lower waste treatment costs, making it more suitable for industrial production.

The application provides a cobalt phosphosilicotungstate material and a preparation method and application thereof, and the preparation method comprises the following steps: dissolving phosphotungstate in water to obtain solution A; dissolving silicate in the solution A to obtain solution B; dissolving soluble cobalt salt in water to obtain solution C; pouring the solution C into the solution B, adding a phase transfer catalyst, and standing at 25-30 DEG C for 2-12 h to obtain precipitate D; and drying the precipitate D to obtain the cobalt phosphosilicotungstate material. The cobalt phosphosilicotungstate material is added into a Victoria blue B solution with a concentration of 150-350 mg / L, the pH is adjusted to 6-8, and the Victoria blue B is adsorbed by stirring at 20-35 DEG C for 30-70 min. The preparation method is simple, raw materials are easy to obtain, the prepared cobalt phosphosilicotungstate material has good adsorption performance, can be recycled, and can realize industrialized treatment of organic dyes.

This invention proposes a composite complexing agent for ultra-clean polypropylene, its preparation method, and its application. The preparation method includes synthesizing a carboxyl-containing organophosphonate monomer; synthesizing a bisβ-diketone derivative; dissolving the organophosphonate monomer and the bisβ-diketone derivative in hexane solvent, adding a phase transfer catalyst, and mixing to obtain the composite complexing agent. This invention achieves efficient removal of metal ash ions such as titanium, magnesium, and aluminum through a synergistic complexing mechanism, while ensuring that the physical properties of polypropylene are not affected. The phosphonic acid groups in the carboxyl-containing organophosphonate monomer have a significant effect on the removal of titanium ash ions. 4+ Exhibiting strong chelating ability, the β-diketone structure in the bisβ-diketone derivative has a strong effect on Mg. 2+ Al 3+ Exhibiting specific complexing properties, both TBAB and polypropylene work synergistically to achieve highly efficient removal of multi-metal ions. TBAB promotes the diffusion of the complexing agent within polymer particles, significantly improving deashing efficiency. The hexane solvent system is compatible with polypropylene production processes, is easily recyclable, and leaves no residue, meeting green chemistry requirements.

This invention provides a method for synthesizing 3-(4-azidofurazan-3-oxomethyl)-3-azidomethyloxetane, its structural formula is shown below: The method includes the following steps: Step 1, 3-nitro-4-hydroxyfurazan, 3,3-dibromomethyloxetane, a basic donor and a phase transfer catalyst are added to a polar aprotic solvent, and the mixture is stirred at 45-85°C for 0.5-2 hours. Then, the mixture is extracted, washed with water, dried, filtered, the solvent is evaporated, and recrystallized to obtain 3-(4-azidofurazan-3-oxomethyl)-3-azidomethyloxetane. 3-(4-nitrofurazan-3-oxomethyl)-3-bromomethyloxetane; the 3-(4-nitrofurazan-3-oxomethyl)-3-bromomethyloxetane obtained in steps 2 and 1 and the azidating agent are added to a polar aprotic solvent and stirred at room temperature for 0.5-1.5 h. Then, the mixture is extracted, washed with water, dried, filtered, and the solvent is evaporated to obtain the final product. The 3-(4-azidofurazan-3-oxomethyl)-3-azidomethyloxetane prepared by this invention can be used as an energetic binder or an energetic initiator.

The present application relates to the technical field of fine chemical industry, in particular to a kind of perfluoro-2-alkyloxy propionyl fluoride and preparation method thereof, in the presence of polar aprotic solvent, using metal fluoride supported on support agent to catalyze acyl fluoride and hexafluoroepoxy propane reaction, perfluoro-2-alkyloxy propionyl fluoride is obtained.The present application utilizes the loading performance of support agent, metal ion in metal fluoride is fixed, it is beneficial to fluorine ion to be free, increase oligomerization reactivity, without adding phase transfer catalyst, the high yield, high efficiency preparation of perfluoro-2-alkyloxy propionyl fluoride can be realized.

A method can be used for preparing 1,2-propanediol, dipropylene glycol, and tripropylene glycol. The method involves reacting propene with hydrogen peroxide containing nitrate, in the presence of a catalyst mixture containing a phase transfer catalyst and a heteropolytungstate, in a liquid reaction mixture containing an aqueous phase with a maximum apparent pH of 6 and an organic phase. The method then involves separating the reaction mixture into an aqueous phase containing 1,2-propanediol, dipropylene glycol, tripropylene glycol, and nitrate and an organic phase. The method further involves recycling at least part of the separated organic phase to the reaction; hydrogenating the separated aqueous phase using a heterogeneous hydrogenation catalyst to provide a hydrogenated aqueous phase with a reduced nitrate content; and recovering 1,2-propanediol, dipropylene glycol, and tripropylene glycol from the hydrogenated aqueous phase by a sequential multiple-step distillation.

The present application relates to the technical field of organic synthesis, and provides a synthesis method of pepper ring, which comprises the following steps: mixing liquid alkali, catechol, phase transfer catalyst and dichloromethane to carry out reaction, and obtaining the pepper ring; the temperature of the reaction is 100-120 DEG C, and the pressure is 0.6-0.65 MPa.The present application uses catechol and dichloromethane as reaction raw materials to prepare the pepper ring, the conversion rate of raw materials is high, and the yield of product is high; the reaction is carried out under the condition of medium pressure, the selectivity of target product can be significantly improved by accurately controlling the reaction pressure, the side reaction is inhibited, so as to improve the yield and purity of product; and the method provided by the present application can eliminate the generation of a large amount of waste gas, avoid the pollution of waste gas to the environment, produce less waste water, have low production cost, and good economic benefits.

The application relates to the technical field of heat-curable crosslinking agents, in particular to vinylbenzyl fluorene containing a benzocyclobutene group and a preparation method and application thereof, wherein the preparation method of the vinylbenzyl fluorene containing the benzocyclobutene group comprises the following reaction steps: S1. adding fluorene, a solvent, a strong base and a phase transfer catalyst into a reaction container, adding 4-bromobenzocyclobutene dropwise into the reaction container under inert atmosphere, continuous stirring and constant temperature conditions, sequentially performing treatment of solvent removal under reduced pressure, extraction, washing, solvent removal under reduced pressure in the organic phase, and obtaining a target intermediate product; S2. adding the target intermediate product, 4-vinylbenzyl chloride, a solvent, a weak base and a phase transfer catalyst into a reaction container, performing reaction under inert atmosphere, continuous stirring and constant temperature conditions, sequentially performing treatment of solvent removal under reduced pressure, extraction, washing, solvent removal under reduced pressure in the organic phase and recrystallization, and obtaining the vinylbenzyl fluorene containing the benzocyclobutene group.

The application discloses a preparation method of a phenylacetyl acetic acid compound, relates to the technical field of chemical synthesis, and the synthesis route of the phenylacetyl acetyl acid compound is as follows: an aniline compound connected with five groups of R1, R2, R3, R4 and R5 is used as a raw material, a diazotization reagent is added under acidic conditions to perform a diazotization reaction, a phase transfer catalyst, a copper catalyst and divinyl ketone are added to perform a reaction, and hydrolysis is performed under acidic conditions to obtain the phenylacetyl acetic acid compound; wherein R1, R2, R3, R4 and R5 are each independently selected from F, Cl, Br, -CH3, -OCH3, NO2, -C2H5, -C3H7, -CF3 or H, and are not H at the same time; when one or more of R1, R2, R3, R4 and R5 is F, the rest are not all H; and X is selected from Cl or Br. The raw material prepared by the application is easy to obtain, the operation is simple, the reaction condition is mild, the danger is low, the reaction step is short, the production cost and three waste emissions of enterprises are reduced, and large-scale industrial production can be easily realized.

This invention relates to the field of fine chemical technology and discloses a safe and efficient synthesis process for o-p-toluenesulfonamide. The process uses p-toluenesulfonyl chloride and ammonia as raw materials, and tetrabutylammonium bromide as a phase transfer catalyst. In an acetone-water mixed solvent, an amination reaction is carried out in a continuous flow pipeline reactor to generate p-toluenesulfonamide in one step. After continuous extraction and separation in a countercurrent extraction tower, the organic phase is continuously recovered from dichloromethane and acetone via thin-film evaporation and recycled. The crude product is then purified by gradient vacuum distillation to obtain high-purity p-toluenesulfonamide. The aqueous phase is stripped to recover excess ammonia and reused. Wastewater is treated biochemically to meet discharge standards, and solid waste is incinerated for resource utilization. By employing continuous extraction and solvent recovery technologies, the consumption of organic solvents is significantly reduced and recycling is achieved. Simultaneously, gradient distillation instead of recrystallization avoids the generation of saline organic wastewater, thereby reducing wastewater discharge and achieving environmentally friendly production.

The application discloses a concrete reinforcing agent and a preparation method thereof, relates to the technical field of concrete production, and the concrete reinforcing agent is prepared from the following raw materials in parts by mass: 60-70 parts of small-molecule polyacid, 30-45 parts of alcohol amine, 1-4 parts of a catalyst, 0.3-0.5 parts of a chelating agent, 0.1-0.3 parts of a phase transfer catalyst and 0.2-0.5 parts of an antioxidant. The concrete reinforcing agent and the preparation method thereof have the advantages of low mixing amount, good economy, complete water solubility, convenient use, remarkable early and late reinforcing effect and no corrosion to steel bars. The technical scheme effectively solves the technical defects of traditional concrete reinforcing agents and provides a new technical selection for realizing green and low-carbon development of the building industry.