45results about How to "The reaction process is stable and controllable" patented technology

The invention discloses a preparation method of beta-hydroxyphosphonate derivatives. The preparation method comprises that an arylethene derivative, a phosphorus reagent and manganese acetate are dissolved in a solvent and the solution undergoes a reaction at a temperature of 20-60 DEG C to produce the beta-hydroxyphosphonate derivative. Under the action of ammonia water, a beta-aminophosphonate derivative is prepared from the beta-hydroxyphosphonate derivative. The preparation method utilizes the arylethene derivative as an initiator and utilizes multiple easily available raw materials. The beta-hydroxyphosphonate derivatives belong to multiple types and can be directly used and can be used for other further reactions. The preparation method has a short synthesis route, mild reaction conditions, simple reaction and aftertreatment processes and a high yield and is suitable for large-scale production.

The invention discloses a metal ion modified melamine polyphosphate. A molecular formula of the metal ion modified melamine polyphosphate is as shown in formula (I): (as shown in the description) (I), wherein M is metal ions, z is a valence state of metal ions M, n is an average polymerization degree of polyphosphoric acid, and n is greater than or equal to 2. The metal ion modified melamine polyphosphate is good in high-temperature stability, excellent in flame retardant effect and wide in application range. The invention also discloses a preparation method of the metal ion melamine polyphosphate. The preparation method comprises the following steps: (1) slowly adding polyphosphoric acid into melamine at a stirring state, heating to facilitate the reaction, and obtaining a melamine polyphosphate prepolymer; and (2) adding a metal compound into the melamine polyphosphate prepolymer, uniformly stirring, heating to facilitate the reaction, and obtaining the metal ion modified melamine polyphosphate. The preparation method is simple in procedures, moderate in reaction condition, stable and controllable in reaction process, low in energy consumption, small in environmental pollution, and basically free from corroding a device pipeline.

The invention discloses a preparation method for aqueous polyurethane-polyurea dispersion and aims at providing a method for producing polyurethane-polyurea without using cosolvents and solvents in the process of preparation. The method comprises the following steps: 1) weighing water with a mass percent of 60 to 80%, adding the weighed water into a reactor, then adding polyetheramine with a mass percent of 1 to 5%, uniformly mixing the two, adding an anionic surfactant with a mass percent of 0.5 to 2%, and carrying out stirring to realize uniform mixing; 2) weighing polymer polyol with a mass percent of 10 to 25% and polyisocyanate with a mass percent of 2 to 8%, and uniformly mixing the two; 3) adding a substance obtained in step 2) into a substance obtained in step 1), and carrying out stirring to realize uniform mixing; 4) adding an organo-metallic catalyst with a mass percent of 0.001 to 0.1% into a substance obtained in step 3), and allowing an obtained mixture for reaction with stirring for 2 to 6 hours at a temperature of 40 to 80 DEG C so as to produce the aqueous polyurethane-polyurea dispersion. The invention belongs to the technical field of preparation of a chemical disperse system.

The invention discloses a water-oil dual-purpose dispersion agent as well as a preparation method and application thereof and aims at providing a dispersion agent with the advantages of no organic solvent, zero VOC (Volatile Organic Compound), capabilities of meeting the current environment-friendly requirement and being compatible with a waterborne system and a solvent-borne system. The water-oil dual-purpose dispersion agent is prepared by the following steps of: firstly, reacting polyether polyol or polyether polyamine with eta-caprolactone according to the ratio of (4:1)-(1:4) to obtain an intermediate A; secondly, adding 10-25 wt% of polyisocyanates into the intermediate A for reacting to obtain an intermediate B; and thirdly, adding a compound with the molecular formula of YMNH2 into the intermediate B, wherein Y is -OH, -COOH and -SO3H, and M is -Ph and -R; and reacting for 2-5 hours and cooling to be room temperature to obtain the dispersion agent. The water-oil dual-purpose dispersion agent is used for dispersing inorganic pigment, organic pigment and carbon black in a paint and ink system and belongs to the technical field of polymer materials.

The present invention relates to an osimertinib preparation method, which comprises: (1) carrying out a nucleophilic substitution reaction on 3-(2-chloro-4-pyrimidinyl)-1-methyl-1H-indole and 4-fluoro-2-methoxy-5-nitroaniline to prepare a compound 1; (2) carrying out a substitution reaction on the compound 1 and N,N,N-trimethylethylenediamine in the presence of an organic alkali to prepare a compound 2; (3) reducing the compound 2 in the presence of a reducing agent to prepare a compound 3; (4) carrying out condensation on the compound 3 and 3-chloropropionyl chloride in the presence of an alkali to obtain a compound 4; (5) carrying out a heat elimination reaction on the compound 4 through heating in the presence of an alkali to prepare a compound 5; and (6) carrying out salification on the compound 5 and methanesulfonic acid under a heating condition to obtain osimertinib. According to the present invention, the osimertinib synthesis process has characteristics of stability, controllability, no high-toxicity solvent is used, energy saving and environmental protection.

The present invention discloses a direct current cable accessory silicon rubber insulation surface layer molecular structure regulation and control device and method. The method comprises the following steps: (1) employing a vacuum pump to extract internal air of a reactor, closing the vacuum pump after vacuum pumping is completed, opening a nitrogen cylinder reducing valve, injecting nitrogen into the reactor and reaching an environment air pressure, and repeatedly performing the process for at least five times; (2) slowing filling fluorine and nitrogen gas mixture with 20% of volume fraction of fluorine into the reactor to allow the air pressure in the reactor to reach up to 300 mbar; (3) going on filling fluorine into the reactor until the air pressure of the reactor reaches up to 500 mbar to allow the fluorine and nitrogen gas mixture to react with silicone rubber samples, keeping the temperature in the reactor at 25 DEG C, replacing C-H bond in the silicone rubber sample surface layer molecule with C-F bond after a certain reaction time, and obtaining the silicone rubber samples with a surface layer molecular structure forming a space charge shielding layer having electronegativity. The direct current cable accessory silicon rubber insulation surface layer molecular structure regulation and control device and method can enhance the charge screening effect of the direct current cable accessory silicon rubber insulation space.

The invention relates to the technical field of medicine, in particular to a novel sorafenib TsOH crystal form as well as a preparation method and an application thereof, and provides a type E crystal of a sorafenib TsOH monohydrate. In an X-ray powder diffraction pattern, the type E crystal of the sorafenib TsOH monohydrate displays characteristic diffraction peaks when 2-theta is about 8.961 degrees plus / minus 0.2 degrees,13.379 degrees plus / minus 0.2 degrees, 13.939 degrees plus / minus 0.2 degrees, 19.718 degrees plus / minus 0.2 degrees, 20.658 degrees plus / minus 0.2 degrees, 22.761 degrees plus / minus 0.2 degrees, 23.561 degrees plus / minus 0.2 degrees, 24.080 degrees plus / minus 0.2 degrees and 24.881 degrees plus / minus 0.2 degrees. A compound shown in a formula (II) of the type E crystal of the sorafenib TsOH monohydrate is high in product yield and excellent in product quality and has the advantages of good stability, high crystal purity, convenience in storage and the like.

The invention relates to fast-cured, high-performance and low-cost unsaturated polyester prepreg and a preparation method thereof. The fast-cured, high-performance and low-cost unsaturated polyester prepreg comprises a continuous fiber or textile, wherein a resin matrix is impregnated in the continuous fiber or textile; the resin matrix is prepared from vinyltoluene, unsaturated polyester, an initiator, a polymerization inhibitor, organic montmorillonite, silicon dioxide and aluminum hydroxide; the content, in percentage by mass, of the resin matrix is 15 to 60 percent; the unsaturated polyester prepreg is covered with a polyethylene film, a polypropylene film, an aluminum-plated film or silicone release paper; fiber woven fabric and multiple unidirectional fibers are impregnated respectively by adopting a unique high-toughness resin matrix; the prepreg is enabled to have the characteristics of not containing styrene and having low molding cost, low toxicity, low volatility, environmental friendliness, corrosion resistance, flame retardancy and the like; the preparation method is high-efficiency and stable; the fast-cured, high-performance and low-cost unsaturated polyester prepregcan be fast cured and is used for decreasing cost by a wide margin when being applied to a composite material, and the manufacturing efficiency of a component is obviously promoted.

The invention relates to beta-phosphoryl nitrate ester compounds and a preparation method thereof. Novel compounds, namely the beta-phosphoryl nitrate ester compounds as shown in a general formula (I)are synthesized, and the prepared beta-phosphoryl nitrate ester compounds will have a dual property both of nitrate esters and organic phosphines. The invention also discloses the preparation methodof the beta-phosphoryl nitrate ester compounds, and the preparation method is that olefin compounds, phosphorus reagents and an oxidant are dissolved in a solvent, and are allowed to react at 30-60DEGC under a nitrogen atmosphere, so as to prepare and obtain the beta-phosphoryl nitrate ester compounds in one-step with a one-pot method. According to the beta-phosphoryl nitrate ester compounds andthe preparation method thereof, the starting raw material is olefins which are cheap, readily available, low in cost, and have many types for selection; step economy and atom economy are high; the obtained products have various types and generally have high yields; and meanwhile, the preparation method has mild reaction conditions, is safe for operation, is easy to control, has simple post-treatment, and is suitable for large-scale production.

The invention discloses a trap regulation and control method based on POSS modified terpolymer ethylene propylene rubber. The trap regulation and control method based on POSS modified terpolymer ethylene propylene rubber comprises following steps: OVPOSS nanometer material is dried to remove water; a double-roller mixing mill roller is heated, roller distance and blocking plate distance are adjusted, terpolymer ethylene propylene rubber is introduced into the double-roller mixing mill roller for mix milling, an obtained product is taken out from the double-roller mixing mill roller, and the double rollers are washed; terpolymer ethylene propylene raw rubber is introduced for mix milling and roll banding; OVPOSS nanometer is added into terpolymer ethylene propylene rubber matrix for mix milling; 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane is weighed, and is introduced into the double-roller mixing mill for mix milling so as to obtain an unvulcanized rubber material; the unvulcanized rubber material is taken out from the double-roller mixing mill, is placed between two layers of PET film, is introduced into a high temperature hot processing forming machine die for hot pressing, and obtained rubber sheets are taken out from the high temerpature hot processing forming machine die after cooling; the rubber sheets are suspended in an air blast baking oven, sulfuration is carried outso as to obtain modified terpolymer ethylene propylene rubber sample sheets; the functional group composition and section morphology of the modified terpolymer ethylene propylene rubber sample sheetsare analyzed; rubber sample sheet surface potential attenuation characteristics are measured; SPD method is adopted to obtain trap distribution character diagram and charge mobility characteristics ofthe rubber.

The invention discloses a synthesis method of perfluoro-3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride (PSVE), which comprises the following steps: (1) reacting tetrafluoroethane beta sultone with hexafluoropropylene oxide in an organic solvent under the action of a catalyst, and rectifying the reaction solution to obtain an intermediate after the reaction is finished; and (2) mixing alkali carbonate and the intermediate obtained in the step (1) according to a molar ratio of (1-8): 1, carrying out a salt forming reaction at 50-250 DEG C, wherein the contact time of the reaction is 5-10 min, then carrying out a decarboxylation reaction at 260-500 DEG C, wherein the contact time of the reaction is 10-30 min, collecting a decarboxylation reaction product, and carrying out condensation and rectification to obtain the 3, 6-dioxa-4-methyl-7-octenylsulfonyl fluoride product. The method has the advantages of simple process, short reaction route, safety, environmental protection, high yield andhigh purity.

The invention discloses high-solid-content low-viscosity odorless alkyd resin as well as a preparation method and application thereof, and the high-solid-content low-viscosity odorless alkyd resin is prepared from the following raw materials in parts by mass: 29.5 to 33.5 parts of vegetable oil fatty acid, 18.5 to 21.5 parts of anhydride, 2.5 to 4.9 parts of monobasic acid, 20.3 to 24.1 parts of polyhydric alcohol, 2 to 5 parts of aldehyde resin, 3 to 5 parts of xylene and 14 to 15 parts of organic solvent. The structure and performance of the prepared resin are easy to control and adjust, the prepared resin is used for preparing a two-component polyurethane wood lacquer coating, the hardness reaches up to H or above, the adhesive force is grade 0, the residual VOC is lower than 5g / L after a paint film is dried for 2 days, and the resin is odorless and environmentally friendly and has excellent chemical resistance and thermal stability.

The invention discloses a reaction and rectification device and a reaction and rectification method for producing isopropanolamine. In the condition that water is used as a catalyst, ammonia and epoxypropane are used as raw materials to be put into a reaction and rectification tower for reaction, heavy components after the reaction are purified by a stripping section, light components after the reaction are purified by a rectifying section and then enter a condenser to be condensed, a part of distillate in the condenser flows back to the reaction and rectification tower again through a distillate return pipe, and the other part of distillate is discharged out of the tower through a top product discharge pipe and is collected as products; materials at the bottom of the tower enter a reboiler for being heated through a communicating pipe, a part of the materials at the bottom of the tower is discharged out of the tower through a bottom product discharge pipe and is collected as an isopropanolamine mixture, and the other part of the materials at the bottom of the tower flow back to the top of the reaction and rectification tower through a reboiled material circulating return pipe. By using the reaction and rectification device and the reaction and rectification method, the total energy consumption of deamination and dehydration can be reduced, side reactions and by-products are effectively avoided, and the product purity is increased.

The invention discloses a device and a method for preparing silicon rubber for improving quick dissipation of space charges. The device comprises an electron balance, a drying box, a vulcanizing machine and a blending machine, wherein the blending machine is used for blending a silicon rubber substrate and filler and comprises a roll cylinder, a heating device, a rotation speed adjusting device and a timing device. The preparation method comprises the following steps of weighing the silicon rubber matrix and the filler by the electron balance, and adding into the drying box at the temperature of 60 DEG C for further use; sequentially adding the silicon rubber matrix, nanometer silicon dioxide, hexamethyl-disilazane, polyvinylsilicone oil, micrometer silicon carbide, nanometer silicon carbide and 2,5-dimethyl-2,5-di(tert-butyl peroxide)hexane into the roll cylinder, and blending; finally, obtaining a silicon rubber enhanced insulation material with quick dissipation of space charges in the vulcanizing machine. The method has the advantages that the dissipation process of the space charges in the silicon rubber insulation material is obviously improved; the influence on the self mechanical property of the silicon rubber enhanced insulation material in a cable accessory is avoided; the production technology and process are simple, and the reaction process is stable and controllable.

The invention relates to an electrochemical hydrogenation device and method and belongs to the technical field of chemical engineering. The device includes a planar laminated assembly. The planar laminated assembly is formed by laminating a hydrogen dissociation catalytic layer, a cation electrolyte membrane layer, an anion electrolyte membrane layer, a water dissociation catalytic layer and a hydrogenation catalytic layer which are planar layers in order. When the device is utilized to perform hydrogenation, the reaction process is stable and controllable, the reaction yield is high, a reactor is self-humidifying, and water management is easy to perform. The device and the method allow a hydrogenation process to be efficient, rapid and stable, do not need high temperature or high pressure, only consume a small amount of electricity, and can perform a catalytic hydrogenation reaction on organic matters at room temperature under atmospheric pressure. A reaction process is economical andenvironmentally friendly.

The invention relates to a method for preparing polyisocyanate containing allophanate and isocyanurate groups, in particular to a bio-based pentamethylene diisocyanate curing agent as well as a preparation method and application thereof. The preparation method of the bio-based pentamethylene diisocyanate curing agent provided by the invention can be used for preparing a polyisocyanate curing agentcontaining allophanate and isocyanurate groups, and comprises the following steps: mixing a PDI monomer with a hydrolytic chlorine concentration of 0-50ppm with a catalyst A, carrying out pre-reaction for 0-5h, diluting a PDI tripolymer catalyst with a mixed solvent (a solvent B and a solvent C), dropwise adding the PDI tripolymer catalyst at a constant speed section by sections, carrying out polymerization reaction, adding a polymerization inhibitor to terminate the reaction when the conversion rate reaches 30%-40%, adding an antioxidant D, and carrying out two-stage separation by virtue ofa film evaporator and a molecular distiller to obtain a PDI-type polyisocyanate composition.The residual PDI monomer in the product is 0.5% or below, viscosity is low, and color is light. Meanwhile, the curing agent has good compatibility with hydroxyl resin, and has the advantages of being high in reaction activity, high in glossiness, good in chemical medium resistance and the like.

The invention relates to m-benzene type epoxy vinyl ester glass fiber reinforced plastic resin and a synthetic method thereof. The synthetic method includes the following steps that firstly, epoxy resin, m-phthalic acid and a catalyst are sequentially put into a reaction vessel, and stirring is started; secondly, the temperature is increased to 170-175 DEG C, heat preservation is performed, and after the mixture is reacted to be clear, heat preservation continues to be performed for 1 h till the acid value is lower than 5 mgKOH / g; thirdly, the temperature is decreased to 105-115 DEG C, a polymerization inhibitor and a stabilizer are sequentially added, then methacrylic acid is dripped, the methacrylic acid dripping speed is controlled to finish dripping within 1 h, and after dripping is finished, heat preservation is performed at 120-125 DEG C till the acid value is decreased to 20 mgKOH / g or below; fourthly, the temperature is decreased to 85-90 DEG C, styrene is added for dilution, the temperature continues to be decreased to 55-60 DEG C, stirring is performed for 0.5-1 h at the temperature till evenness is achieved, and filtration is performed. The m-benzene type epoxy vinyl ester glass fiber reinforced plastic resin and the synthetic method thereof have the advantages that the reaction process is steady and controllable, no wastewater is produced, and environmental friendliness is achieved.

The invention discloses an adhesion promoter for liquid silicone rubber. The adhesion promoter has a general formula as described in the specification, wherein R1 and R5 are selected from the group consisting of -CH3, -OCH3, -CH2CH3, -OCH2CH3, -CH2CH2CH3 or -OCH2CH2CH3; R2, R3, R6 and R7 are selected from the group consisting of -CH3, -CH2CH3 or -CH2CH2CH3; and R4 is selected from the group consisting of -CH2-, -CH2CH2-, -CH2CH2CH2- or -CH2CH2NHCH2CH2CH2-. The adhesion promoter for the liquid silicone rubber can significantly improve adhesion performance of the liquid silicone rubber to various basic materials, and has good compatibility with the liquid silicone rubber. The invention also discloses a preparation method for the adhesion promoter for the liquid silicone rubber. The method has the advantages of simple process steps, stable and controllable reaction process, low production cost and facilitation to realizing industrial production.

The invention discloses a method for quickly smelting low-nitrogen stainless steel through a vacuum induction furnace, and belongs to the technical field of steel and iron metallurgy. The method comprises the steps of (1) adding steel and iron materials and an alloy material not liable to oxidize into a vacuum induction furnace crucible; (2) firstly, carrying out vacuum pumping, and then, performing energization for heating till the steel and iron materials are melted; (3) after melting, measuring the temperature, and carrying out refining with the vacuum degree and temperature maintained; (4) calculating the required nitrogen pressure, then, filling the furnace with nitrogen with the required pressure, and carrying out nitrogen increase alloying; and (5) carrying out alloying of other alloy materials under the nitrogen atmosphere, and carrying out pouring in the planned steel pouring time. According to the method, nitrogen alloying is carried out through utilizing nitrogen, the alloying of other elements is carried out under the nitrogen atmosphere protection, the reaction process is steady and controllable, the melting cycle is short, and the purpose that the low-nitrogen stainless steel is quickly and accurately smelted is achieved.

The invention discloses a saturated polyester type low-shrinkage additive which is prepared by the following steps: mixing polyhydric alcohols with three or more degrees of functionality with a lactone monomer, and heating to 140-170 DEG C under the protection of nitrogen; dropwise adding a catalyst, and carrying out a reflux reaction for 5-8 h at a temperature of 150-155 DEG C after the dropwiseaddition is completed; cooling to 90-100 DEG C, adding a polymerization inhibitor, uniformly stirring, adding an active diluent for dilution after the polymerization inhibitor is completely dissolved,cooling and filtering to obtain the saturated polyester type low-shrinkage additive. The saturated polyester low shrinkage agent has an excellent shrinkage rate control effect, and can make the coloring property of BMC better.

The invention relates to the technical field of waterborne polyurethane resin, in particular to an internal crosslinking type self-extinction waterborne polyurethane dispersion and a preparation method thereof. The internal crosslinking type self-extinction waterborne polyurethane dispersion comprises the following raw materials in percentage by weight: 7-40% of macromolecular polyol, 5-30% of diisocyanate, 0.4-2.0% of a hydrophilic chain extender, 0.1-5% of a polyol chain extender, 0.05-2% of a neutralizer, 0.1-5% of a post chain extender, 5-25% of aliphatic ketone and the balance of water. According to the invention, macromolecular trihydric alcohol is used as a soft segment, so that the polyurethane emulsion with internal crosslinking property can be obtained without adding a crosslinking agent; the preparation method is high in crosslinking degree and simple in technological process, has a better matting effect and is suitable for products such as leather, paper and films needing matt surfaces.

The invention provides a synthesis method of benzo-p-dipyrrole molecules for hydrogen storage, and belongs to the technical field of hydrogen storage of organic heterocyclic aromatic hydrocarbon molecules. The synthesis method comprises the following steps: preparing benzo-p-dipyrrole molecules by taking N1 molecules as initial reactants; wherein the chemical structural formula of the N1 molecule is shown in the specification, and the chemical structural formula of the benzo-p-dipyrrole molecule is shown in the specification. The N1 molecule is adopted as an initial reactant, so that by-products in the reaction process are reduced, and the yield of an intermediate product and the reaction success rate are greatly improved; finally, the synthesis yield, the yield and the efficiency of the benzo-p-dipyrrole molecule are greatly improved.

The invention discloses a water-soluble low-modulus acrylic resin adhesive and a preparation method thereof, the glass transition temperature of the water-soluble low-modulus acrylic resin adhesive islower than 0 DEG C, the storage state of the water-soluble low-modulus acrylic resin adhesive is a homogeneous, clear and stable aqueous solution, the pH value of the aqueous solution is 6-8, the solid content is 5%-50%, and the viscosity is 10-200000 cp; the dried water-soluble low-modulus acrylic resin adhesive is a solid; when the temperature is higher than 0 DEG C, the tensile modulus and thebending modulus of the water-soluble low-modulus acrylic resin adhesive are lower than 100MPa; the preparation method comprises the following steps: mixing water-soluble acrylate, water-soluble loweralcohol, an initiator and pure water in a reaction container, and fully stirring to obtain a clear aqueous solution which is a reaction solution; and heating the reaction container to 50-80 DEG C, reacting for 2-8 hours, cooling and collecting a product. Compared with the prior art, the water-soluble low-modulus acrylic resin adhesive is an aqueous solution system, and has the advantages of few small molecule residues, good stability, looser requirements on storage conditions and longer storage life.

The invention relates to beta-phosphoryl nitrate ester compounds and a preparation method thereof. Novel compounds, namely the beta-phosphoryl nitrate ester compounds as shown in a general formula (I)are synthesized, and the prepared beta-phosphoryl nitrate ester compounds will have a dual property both of nitrate esters and organic phosphines. The invention also discloses the preparation methodof the beta-phosphoryl nitrate ester compounds, and the preparation method is that olefin compounds, phosphorus reagents and an oxidant are dissolved in a solvent, and are allowed to react at 30-60DEGC under a nitrogen atmosphere, so as to prepare and obtain the beta-phosphoryl nitrate ester compounds in one-step with a one-pot method. According to the beta-phosphoryl nitrate ester compounds andthe preparation method thereof, the starting raw material is olefins which are cheap, readily available, low in cost, and have many types for selection; step economy and atom economy are high; the obtained products have various types and generally have high yields; and meanwhile, the preparation method has mild reaction conditions, is safe for operation, is easy to control, has simple post-treatment, and is suitable for large-scale production.

The invention discloses melamine polyphosphate. The melamine polyphosphate is prepared by mixing dimelamine pyrophosphate and an ammonia source and then carrying out high-temperature heat treatment. The invention also discloses a scheme for preparing a dimelamine pyrophosphate intermediate from melamine, sodium pyrophosphate and inorganic acid, and drying and roasting the intermediate to obtain melamine polyphosphate. The invention also discloses an application of the melamine polyphosphate in flame-retardant modified products. The melamine polyphosphate has the characteristics of high thermalstability, low water solubility and excellent flame retardance, and a flame-retardant modified product prepared by applying the melamine polyphosphate has excellent ageing resistance; the productionprocess of the melamine polyphosphate is simple in step, mild in reaction condition, stable and controllable in reaction process, low in energy consumption and small in environmental pollution.