238results about How to "High esterification rate" patented technology

The invention relates to a preparation method of a star polycarboxylic acid high-performance water reducing agent. Polybasic alcohol and (methyl) acrylic acid used as main raw materials for esterification are esterified and polymerized to prepare the star polycarboxylic acid high-performance water reducing agent material: the (methyl) acrylic acid and polybasic alcohol used as reactants are esterified under the action of a catalyst to firstly prepare a star polymerizable active terminal, and free-radical polymerization reaction is carried out with unsaturated polyethenoxy ether, molecular weight regulator and unsaturated carboxylic acid monomer under the action of an initiator to prepare the star polycarboxylic acid high-performance water reducing agent. The invention is easy to control, and has the advantages of high polymerization degree, low cost and no pollution; the esterification reaction is carried out form an active core, and the free-radical polymerization is carried out to generate the chain arm, thereby implementing the polycarboxylic acid high-performance water reducing agent in a star molecular structure; and under the condition of common doping amount and low doping amount, the star polycarboxylic acid high-performance water reducing agent has better cement paste flowability and holding capacity than the traditional linear and comb polycarboxylic acid water reducing agents, and has favorable cement adaptability and concrete application performance.

The invention discloses a preparing method of graft copolymerization carboxylate high-performance dehydragent belonging to dehydragent domain, which comprises the following steps: choosing methoxy carbowax with molecular weight distributing between 1000-2000 and acroleic acid or methacrylic acid as main raw material; adopting total acid method esterified priority method; preparing intermediate (big monomer) with polymerization activity; adding third monomer into polymerization reaction; adjusting polymerization activity of copolymerization system; proceeding technique route synthesis of main chain polymerization in the water solution. The getting big monomer possesses merits of high conversion rate, short reacting time, simple process flow and strong controlling property.

The invention relates to a method for preparing polyol ester lubricating oil by using a composite solid acid catalyst. The method comprises the following steps of: adding a water carrying agent into polyol ester and monobasic fatty acid, performing esterification reaction under the action of the composite solid acid catalyst, and dehydrating and esterfying to obtain raw ester; performing filter pressing on the raw ester to separate the raw ester from the solid acid catalyst, wherein the catalyst can be recycled; and performing reduced pressure distillation on the raw ester to remove the residual fatty acid, and then deacidifying and decolorizing to refine with heating by using a refining adsorption bed layer respectively to obtain low-acid value polyol ester lubricating oil. The method has the advantages that the catalyst can be recycled, the esterification rate is high, an aftertreatment process is simple, and a product is low in acid value, high in purity, environment-friendly and suitable to be produced industrially. The reaction esterification rate can reach over 99 percent, and the acid value of the ester product obtained through refining can be controlled to be less than 0.01mg KOH/g. The product is excellent in visco-temperature performance, high in lubricity and thermal stability, strong in hydrolytic stability, low in volatility and excellent in electrical insulation property.

The invention provides a preparation method and application of a polycarboxylate water reducer containing a phosphate group. According to the preparation method, the defects that the structure and the molecular weight of the water reducer cannot be accurately controlled due to the chain transfer action of the phosphate group can be overcome. The preparation method comprises the steps that an unsaturated polyether macromonomer, unsaturated carboxylic ester and unsaturated alcohol are subjected to a copolymerization reaction in organic solvent to obtain a polycarboxylate water reducer pre-polymer; phosphorylated modification is performed on the polycarboxylate water reducer pre-polymer; on the condition that an acid aqueous solution exists, a carboxylic ester group on a product obtained after phosphorylated modification is hydrolyzed, and the organic solvent is removed; neutralization is performed to obtain the polycarboxylate water reducer containing the phosphate group; the unsaturated polyether macromonomer does not contain hydroxyl, phosphorylated modification is achieved through the step that an alcoholic hydroxyl group in the polycarboxylate water reducer pre-polymer and a phosphate esterification reagent are subjected to an esterification reaction, and the using amount of the phosphate esterification reagent is sufficient to completely esterify the alcoholic hydroxyl group in the polycarboxylate water reducer pre-polymer.

The invention relates to a method and a device for continuously producing terephthalic acid-1,3-propylene glycol ester. In the method, an esterifiction product is obtained by esterfying terephthalic acid-and 1,3-propylene glycol ester in the presence of an esterifiction catalyst, and the terephthalic acid-1,3-propylene glycol ester is obtained by polymerizing in the presence of a polymerization catalyst. The esterifiction is carried out in at least two phases, i.e. an initial first phase and a subsequent second phase, wherein the second phase is carried out in a reactor having a plurality of communicated reaction chambers, and the reaction chambers comprise at least one initial reaction chamber, an intermediate reaction chamber and a final reaction chamber so that the materials after finishing the reaction in the first phase carries out the second phase of esterifiction reaction by sequentially passing through the initial reaction chamber, the intermediate reaction chamber and the final reaction chamber, wherein the esterifiction rate for esterifiction in the intermediate reaction chamber reaches 95-99 percent. The method comprises the steps as follows: the esterifiction catalyst and the polymerization catalyst are added from the intermediate reaction chamber, and part materials in the intermediate reaction chamber circulate to return to the first phase of reactor for esterifiction. By adopting the invention, high-quality terephthalic acid-1,3-propylene glycol ester can be produced with lower cost and higher efficiency.

The invention discloses a preparation method of cationic dyeable flame-retardant polyester resin. The manufacturing method is characterized by comprising the following steps: performing an esterification reaction on a halogen-free copolymerized phosphorus-based flame retardant, ethylene glycol and a composite catalyst to prepare an esterification solution of the halogen-free copolymerized flame retardant; performing ester exchange reaction on sulfoisophthalic acid dimethyl ester and the ethylene glycol to prepare a sulfonate-based bis(hydroxyethyl) isophthalate solution; performing an esterification reaction on terephthalic acid (or dimethyl terephthalate), the ethylene glycol and auxiliaries, then adding a catalyst, a stabilizer, the auxiliaries, the esterification solution of the phosphorus-based flame retardant (or a prepolymer solution of the phosphorus-based flame retardant) and the sulfonate-based bis(hydroxyethyl) isophthalate solution, performing condensation polymerization reaction, and cooling and dicing after the end of reaction to prepare the cationic dyeable flame-retardant polyester resin. The cationic dyeable flame-retardant polyester resin prepared by the method disclosed by the invention has the characteristics of good spinnability, polyester fiber cationic dye boiling dyeing under normal pressure conditions, complete chromatogram and strong dye adhesion.

The invention relates to a method for effectively synthesizing phytosterol ester, belonging to the technical fields of food, medicine and cosmetics. The method has the technical scheme that the high-purity phytosterol ester is synthesized by the steps of directly mixing phytosterol and fatty acid, adding biocatalyst and organic solvent for reaction at the temperature of 35-55 DEG C for 24-96h, and controlling the water activity of a reaction system to be 0.1-0.9. By adopting a biological method to prepare the phytosterol ester, the method has high-efficiency and green processing technique, safety and high conversion rate, and the obtained product has the functional characteristics of reducing cholesterol, preventing and curing cardiovascular and cerebrovascular diseases, antioxidation and the like, so that the invention can be widely applied to multiple fields such as food, medicine, cosmetics and the like.

The invention discloses a method for preparing a polycarboxylic acid water reducer intermediate, namely the method for preparing polyethylene glycol monomethyl ether methacrylate or polyethylene glycol monomethyl ether acrylate, in particular the method for preparing a polycarboxylic acid water reducer macromer. The method for preparing the polycarboxylic acid water reducer macromer comprises the following steps of: putting polyethylene glycol monomethyl ether, methacrylic acid or acrylic acid into a reaction kettle; adding a polymerization inhibitor and a catalyst into the reaction kettle, stirring and heating the mixture; raising the temperature of esterificatin reaction, then introducing inert gas into the reaction kettle, and keeping certain pressure in the reaction kettle; and then preserving the heat for hours to obtain the polyethylene glycol monomethyl ether methacrylate or the polyethylene glycol monomethyl ether acrylate. The invention mainly aims to provide the simple and fast method for preparing the polycarboxylic acid water reducer macromer so as to overcome the defects of the conventional production technique and process of the macromer.

The invention relates to a reduced-type polycarboxylic acid water reducer and a preparation method thereof. An esterification method is employed for synthesizing a reduced monomer having a low surfacetension, and the reduced polycarboxylic acid water reducer is prepared through polymerization; acid anhydride or unsaturated carboxylic acid and ethers molecules are subjected to an esterification reaction to prepare the reduced monomer under effect of a catalyst, and then the reduced monomer, nonsaturated polyoxyethylene ether, unsaturated carboxylic acid or a mixture of unsaturated carboxylic acid or its acid anhydride, and a molecular weight conditioning agent are subjected to a free radical copolymerization reaction under effect of an initiator. The method has the advantages of easy control, high yield, low cost, environmental protection, and no pollution. During a polymerization process, a reduced group is introduced, so that the water reducer has low surface tension, an anchoring group is introduced, has good cement slurry-cleaning fluidity under common doping, reduces the surface tension force of a cement aperture solution, and reduces evaporation rate of the solution so as toeffectively reduce the mortar contraction. The obtained water reducer presents good water-reducing and reduction characteristic.

The invention provides a polycarboxylene high-performance water reducing agent, which is obtained by copolymerization of following monomer components: ester macro monomer, ether macro monomer, micro-molecule monomer and bulking agent. The invention also discloses a preparation method of the polycarboxylene high-performance water reducing agent. The polycarboxylene high-performance water reducing agent of the invention not only can show good adaptability for different concrete construction materials, but also reduces usage of a retarder, improves water-reducing rate, and has good bleeding rate and compressive strength rate. The product has more stable quality; the shortcomings that the polycarboxylene product in the prior art has single type and narrow adaptability is overcome.

The invention discloses a polymerizing production method for transparent amorphous copolyester. The method has the advantages of low esterification temperature, short esterification time and high esterification rate. The method comprises the following steps of: carrying out an esterification reaction and a condensation reaction on dihydric alcohol and dicarboxylic acid to obtain the transparent amorphous copolyester, wherein the esterification reaction comprises the following specific procedures of: breaking various materials into pulp by using a pulping machine and carrying out the esterification reaction on the pulp at the temperature of 220-240DEG C for 1.0-1.5 hours to obtain an esterified product; the condensation reaction comprises the following specific procedures of: polymerizing the esterified product obtained by the esterification reaction at the reaction pressure of 0.2-0.5MPa and the temperature of 250-260DEG C for 1.5-2 hours; then reducing the pressure to be less than 200MPa within 0.5 hour; raising the condensation reaction temperature to be 275DEG C from 260DEG C; adding a thermal stabilizer; and after the condensation reaction, obtaining a polyester copolymer with the inherent viscosity of greater than 0.75dL/g and the carboxyl content of less than 10mol/t.

The invention discloses a method for preparing biodiesel through high-temperature esterification reaction of high acid value oil, belonging to the technical field of biodiesel preparation. The method comprises the following steps: (1) esterification reaction, adding the high acid value oil and a catalyst into an esterification reactor, dripping methanol into the esterification reactor by using a dripping device for esterification reaction, meanwhile, cooling unreacted methanol and moisture generated in reaction by using a condensing device, and after the reaction is finished, removing the methanol and the moisture through distillation to obtain a biodiesel crude product; and (2) distillation treatment, distilling the obtained biodiesel crude product under reduced pressure, and collecting fraction, namely a biodiesel finished product. The method disclosed by the invention realizes the one-step esterification reaction of the high acid value oil under the conditions of normal pressure and high temperature, and the esterification process and the water cooling and removal are carried out simultaneously for the preparation of the biodiesel, so that the method has the advantages of easy process, short production cycle, low energy consumption and the like, is easy to industrially produce, and can significantly increase the yield of the biodiesel per unit time and the output of a single kettle.

The invention relates to octenyl succinic acid starch ester, a lipid-soluble nutrient microcapsule as well as a preparation method application of the lipid-soluble nutrient microcapsule. A preparationmethod of octenyl succinic acid starch ester comprises the step of carrying out esterification reaction on gelatinized starch and octenyl succinic anhydride in a cavitation emulsification process, soas to obtain octenyl succinic acid starch ester. According to the preparation method, the esterification reaction is promoted and intensified by virtue of the cavitation emulsification process, remarkably substitution occurs in a crystallization region and an amorphous region of the starch through the molecular collision of the collision between gelatinized starch and octenyl succinic anhydride,so that the esterification rate of prepared octenyl succinic acid starch ester is increased, and the emulsifying property is greatly improved. The method is rapid and efficient, and a hydrolysis stepis omitted after the esterification, so that the problems that molecular chains are damaged in different degrees due to the hydrolysis, the chain length and content of amylose are remarkably decreased, the compactness of a film formed by octenyl succinic acid starch ester is decreased, and the film easily absorbs moisture and conducts heat and is crispy are avoided, and the application performanceof octenyl succinic acid starch ester is improved.

The invention provides a method for preparing cassava starch octenyl succinate by a sub-gelatinization technology. The method comprises the following steps of: adding cassava starch into an ethanol solution with concentration of 45-65% by volume; gelatinizing at 60-85 DEG C for 1-3 hours while stirring to obtain sub-gelatinized cassava starch emulsion; in a condition with pH value of 7.2-9.2, adding the octenyl succinic anhydride diluted by an organic solvent into the sub-gelatinized cassava starch emulsion to enable esterification reaction; and processing the reaction product to obtain the cassava starch octenyl succinate. According to the method provided by the invention, the raw materials are widely available, and the cost is low; moreover, the technology is simple, the gelatinization degree of starch is proper, the esterification reaction is uniform, and the reaction efficiency is high; and the prepared cassava modified starch has high esterification substation degree and relatively good transparency, thickening property and emulsifying property.

The invention discloses an acidified mesoporous WO3/SiO2 multi-component colloidal sphere, belonging to the field of chemical catalysts. An active component of the colloidal sphere is SO4<2->/WO3/SiO2 of which the structure is like a colloidal sphere; the active component has a mesoporous structure and is high in dispersion property; the particle size is 100-900nm, and the aperture is 3-5nm. The acidified mesoporous WO3/SiO2 multi-component colloidal sphere disclosed by the invention is used as the catalyst; during catalysis of the esterification reaction between different long-chain fatty acids and alcohols, the acidified mesoporous WO3/SiO2 multi-component colloidal sphere is excellent in catalyst performance and high in stability. During esterification reaction in which the long-chain fatty acids are oil acids and the alcohols are methanol, and when the using amount of the colloidal sphere catalyst is 3 percent, the esterification rate of the oil acid can reach 97.0 percent; after the oil acids are continuously and cyclically used for 5 times, the conversion rate of the oil acids can be still kept at about 97 percent.

The invention discloses a synthesis method of trimethylolpropane organic acid ester, which is characterized by comprising the following steps of: taking organic acid and organic alcohol as raw material, further adding proper amount of catalyst, reacting for 3-5 hours under normal pressure at 110-130 DEG C, thereby obtaining the trimethylolpropane organic acid ester; the organic acid is selected from any one of Oleic acid, lauric acid, octanoic acid, stearic acid and palmitic acid, the organic alcohol is trimethylolpropane, and molar ratio of organic acid to organic alcohol is 1:3; the catalyst is N-alkyl pyrrolidone group methyl phosphate ion liquid catalyst. In the synthesis method, the N-alkyl pyrrolidone group methyl phosphate ion liquid catalyst is selected for synthesizing the trimethylolpropane organic acid ester, the synthesis method has the characteristics of low reaction temperature, small dosage of catalyst, short reaction time, high esterification rate, and so on, and products produced by the synthesis method has small acid value.

A preparation method of a super-sustained release ester-ether crosslinking polycarboxylic acid water reducer is provided. The method which combines synthesis of an ester water reducer and synthesis of an ether water reducer allows the polycarboxylic acid water reducer synthesized from large monomers containing different chain lengths and simultaneously containing long side chains and short side chains to be researched and developed, and the method which can guarantee good dispersity and good fluidity keeping ability brings conveniences for the concrete construction process. In the esterification reaction process, hydroxyethyl methacrylate is introduced to increase active hydroxy side chains, and the activity of methacrylic acid is effectively controlled, so the esterification rate of a reaction system is high, product performances are high, and the synthetic method of optimized ester polycarboxylic acid water reducer intermediates is researched and developed through utilizing above principles. A certain synergistic effect is reached by introducing high activity ester monomers in the copolymerization process and combining the long side chains and the short side chains of produced polycarboxylic acid, so performances of the ester-ether crosslinking polycarboxylic acid water reducer of the invention are better than the performances of common ester and ether polycarboxylic acids, and the water reducing rate and the fluidity keeping ability are improved.

The invention discloses a compounding method of allyl polyoxyethylene methyl acrylate, which uses propyl ethylene polyoxyethylene and crylic acid as raw materials. The raw materials are subjected to esterification reaction under the function of a toluenesulfonic acid catalyst and a thiodiphenylamine polymerization resistor, and air dried by silicon gel is supplied to bring out the water generated by the reaction. The invention has the advantages that in the reaction process, the dried air is used for bringing out the water generated by the reaction, the reaction cost is effectively lowered, wet air is discharged, and the environmental pollution is avoided; the paratoluenesulfonic acid is used as the catalyst, the thiodiphenylamine and the oxygen molecules in the air are used as the polymerization resistor, the reaction condition is reasonable, the reaction time is short and the process is simple and easy to control; the allyl polyoxyethylene methyl acrylate compounded by the method has the characteristics of high unsaturation degree, high esterification degree, high reaction activity, and the like, and is suitable for the compounding field of high-performance polycarboxylic-acid water reducer.

The invention discloses a method for synthesizing phenylalanine esterified bagasse xylan-g-CHMA with anti-tumor activity. The method comprises taking bagasse xylan as the raw material, and in an ionicliquid of [Hemim]Cl, taking ammonium persulfate as an initiator and cyclohexyl methacrylate as grafting monomers to synthesize a bagasse xylan-g-CHMA derivative; taking Boc-L-phenylalanine as esterification agent and 4-dimethylaminopyridine as catalysts for catalytic esterification in ionic liquid solvent to synthesize a bagasse xylan esterified grafted derivative phenylalanine esterified bagassexylan-g-CHMA; performing deprotection through trifluoroacetic acid to obtain the product of the phenylalanine esterified bagasse xylan-g-CHMA. Under the reaction environment of the ionic liquid, themethod for synthesizing the phenylalanine esterified bagasse xylan-g-CHMA with the anti-tumor activity introduces active groups to the main chain and the side chain of bagasse xylan through grafting and esterification reaction, thereby enhancing the bioactivity of raw bagasse xylan; the prepared phenylalanine esterified bagasse xylan-g-CHMA has a broad application prospect in the fields of biologyand medicine.

The invention relates to the technical field of biological and medical materials, in particular to a preparation method of injection type modified xanthan gum nano-micelle. The preparation method comprises the steps: performing esterification reaction on phthalic anhydride and xanthan gum, preparing amphipathic modified xanthan gum polymer by a one-step method and then self assembling and preparing modified xanthan nano-micelle by a selective solvent method. The xanthan gum is anhydride modified, so that biocompatibility and oxidation resistance of the xanthan gum are improved. The xanthan gum nano-micelle has a hydrophobic cavity with a benzene ring and a hydrophilic outer layer of the xanthan gum, so that circulation stability of the nano-micelle in a biological body is improved; in addition, the modified xanthan gum contains carboxylic groups, so that the nano-micelle has certain pH response; a charge effect of the nano-micelle can also be utilized to load medicine doxorubicin, so that the medicine loaded nano-micelle has a certain slow-release function. The preparation method disclosed by the invention has simple synthetic steps and is green, and the nano-micelle can be completely degraded in the body and hopefully serves as a carrier of anti-cancer drug to control release.