73results about How to "Short synthesis reaction time" patented technology

The invention relates to a preparation method of polybutylene terephthalate/adipate butanediol copolyester, which utilizes a titanium compound and an antimony compound as the composite catalyst, the mole ratio of terephthalic acid to adipate is 3:7-8:2, the ratio of the total mole of the terephthalic acid and the adipate to the mole of 1,4-butanediol is 1:1.0-1.8, esterification is carried out at normal pressure and the temperature of 150-220 DEG C, the pressure is reduced to high vacuum 10-150 Pa for the reaction, the final temperature for the reaction is 265-280 DEG C, and inert gas is utilized to recover the pressure to be normal to obtain the copolyester. The reaction time is shortened, the production amount of tetrahydrofuran is small, the intrinsic viscosity of copolyester chips is 0.90-1.32 dL/g, the hue b value of the product is between 0 and 8, the L value is between 68 and 85, and the product of the polybutylene terephthalate/adipate butanediol copolyester can be used in the fields of various soft package plastic products.

The invention relates to a method for synthesizing water-in-water cation polyacrylamide. The method takes an inorganic salt water solution as a reaction medium, adopts a mixed dispersion stabilizing agent containing polyethylene glycol PEG series, polyvinylpyrrolidone and polyvinyl alcohol (the mass ratio of the polyethylene glycol PEG series to the polyvinylpyrrolidone to the polyvinyl alcohol is 1:1:1) and enables acrylamide and a quaternary ammonium organic compound with double bonds to generate a free radical copolymerization reaction so as to generate water-in-water cation polyacrylamide emulsion. The preparation method of the water-in-water cation polyacrylamide comprises the following steps: (A) adding acrylamide, a cationic monomer, inorganic salt, a dispersant, a screening agent and deionized water into a four-neck flask, dissolving evenly, putting into water bath of 50 DEG C, introducing nitrogen, deoxidizing and stirring at the speed of 1000rpm; (B) when reacting for 0.5 hour and 1.5 hours respectively, adding a certain amount of initiator; and (C) after adding the initiator for the second time, reacting for 3-4 hours continuously so as to obtain a product. The emulsion has the characteristics of high dissolving speed, good stability and convenient use and transportation and can not cause secondary pollution to the environment.

A method for synthesizing a hydrophilic monodisperse carboxyl super paramagnetic microsphere belongs to the inorganic chemistry field. In the invention, soluble iron ion salt, urea, water and carboxylic acid or carboxylate are taken as raw materials, dissolved in ethylene glycol and made into nano-ferroferric oxide super paramagnetic microsphere with carboxylated surface by reduction reaction with polyol at the temperature of 160-250 DEG C, and a series of magnetic microspheres with different diameters and densities of surface carboxyl groups are obtained by controlling reaction parameters. The surface carboxylated microsphere obtained by the method is characterized by uniform size, dispersion stability with a great pH range, high specific saturation magnetization and the like; the raw materials are nontoxic, environmental friendly, cheap; and the method has simple operation, low equipment requirements, high yield, and is applicable to large-scale industrialized production. The application of the bead to the biomedical field can be further expanded by inorganic or polymer surface coating of the super paramagnetic microsphere, on the basis of the bead.

The invention relates to the technical field of preparation of particle reinforced aluminum-based composite materials, in particular to a method for synthesizing a particle reinforced aluminum-based composite material through direct reaction of a melt under the composite action of current and a magnetic field. The method is mainly characterized in that: in the process of synthesizing the particlereinforced aluminum-based composite material by a direct melt reaction method, current is introduced into the melt and the magnetic field is applied so as to promote melt reaction and control the appearance, size, motion and distribution of particles through electromagnetic oscillation effect generated by interaction of the current and the magnetic field. In the scheme, alternating current and a static magnetic field can be composited, and direct current and an alternating magnetic field also can be composited. By the method, the synthesis reaction rate and yield can be obviously improved, obvious effects of controlling the appearance of the particles and promoting dispersion are achieved, and the method is suitable for preparing high-performance particle reinforced composite materials onan industrial scale.

The invention relates to biodegradable copolyester and a preparation method thereof. The preparation method comprises the following steps of: undergoing an esterification reaction on pure terephthalic acid, hexanedioic acid, 1,4-butylene glycol and ethylene glycol under normal pressure at the temperature of between 150 DEG C and 220 DEG C, wherein the molar ratio of the pure terephthalic acid to the hexanedioic acid is (3:7)-(8:2), the molar ratio of the ethylene glycol to the 1,4-butylene glycol is (1:9)-(9:1), and the ratio of the total mole number of the pure terephthalic acid and the hexanedioic acid to the total mole number of the ethylene glycol and the 1,4-butylene glycol is 1:(1.0-1.8); and undergoing condensation polymerization under the pressure of between 10 Pa and 150 Pa to obtain the copolyester, wherein the dosage of a titanium compound is 200-1,200 ppm relative to the total weight of terephthalic acid and the hexanedioic acid, the dosage of an antimony compound is 100-600 ppm relative to the total weight of the terephthalic acid and the hexanedioic acid, and the dosage of a phosphorous compound is 50-400 ppm relative to the total weight of the terephthalic acid and the hexanedioic acid. The biodegradable copolyester has the advantages of low raw material price, reaction at low temperature and under low pressure and high inherent viscosity.

The invention relates to a preparation method for lithium metal. The production method for high-purity lithium metal comprises two steps of synthetic reaction and reducing reaction, the synthetic reaction comprises the steps that raw material lithium carbonate and kalk or aluminium hydroxide are mixed, then are put into a reaction vessel to be calcinated at the temperature of 650 to 850 DEG C, after carbon dioxide and moisture are removed, intermediate products are prepared and are sieved and set aside; the reducing reaction comprises the steps that duriron or aluminium powder are added into the intermediate products prepared during the synthetic reaction to be as reducing agent, after being mixed, the intermediate products are pressed into spherical or cylindrical, then reducing reaction is performed under the vacuum and high-temperature condition, and the lithium metal is prepared. The production method has the advantages that the flow of the synthetic reaction is simplified, the production efficiency is effectively improved, the product purity is greatly enhanced, no waste material is generated, the side product is lithium-containing compound, which can be directly applied to the electrolytic aluminum industry, and all the required raw materials can be solved internally.

The invention relates to a synthetic silicon oxynitride raw material and a preparation method thereof. A technical scheme adopted in the invention is characterized in that the method comprises the following steps: mixing 50-60wt% of elemental silicon with 40-50wt% of silica, and carrying out ball milling in a ball mill until the granularity is 4.5-6.5[mu]m to obtain a ball milled powder; and putting the ball milled powder in an atmosphere furnace, heating in highly pure nitrogen atmosphere at a heating rate of 10-12DEG C/min to 1000-1100DEG C, heating at a heating rate of 6-8DEG C/min to 1400-1500DEG C, and carrying out heat insulation for 4-9h to obtain the synthetic silicon oxynitride raw material. The method has the advantages simplicity, short production period, low cost, and no need of special synthesis devices or processing technologies; and the prepared synthetic silicon oxynitride raw material has the characteristic of high Si2N2O purity and completeness of grown crystal grains.

The invention discloses a method for preparing a photocatalyst with monatomic Pt embedded into a covalent organic framework and application of the photocatalyst. A Pt-containing precursor solution is introduced in the process of preparing TpPa-1-COF, the Pt1 at TpPa-1-COF photocatalyst is obtained through low-temperature calcination and reduction, especially 3% of Pt1 at TpPa-1-COF, and the hydrogen production efficiency reaches 719 molg <-1 > h <-1 > and is 48 times that of water photolysis hydrogen production of a pure TpPa-1-COF catalyst. The preparation process is short in reaction time and mild in reaction condition, characterization tests such as XRD (X-Ray Diffraction) and a spherical aberration corrected high-angle annular dark field scanning transmission electron microscope (AC HAADF-STEM) graph show that the TpPa-1-COF material embedded with the monatomic Pt provides a large number of Pt active sites, favorable conditions are provided for catalyzing water to produce hydrogen, and the application prospect is good.

The invention discloses a method and device for rapidly preparing an ionic liquid by using microwaves to promote synthesis. According to the invention, after mixing methylimidazole and bromobutane, in the first stage, promoting the synthesis of methylimidazole and bromobutane by using microwaves, when the molar ratio of methylimidazole to bromobutane is 1:1, a first stage ionic liquid can be prepared by the synthesis of methylimidazole and bromobutane in only 2 minutes with the yield of 86-99 %, and the time is 1/720 of the required time in traditional technology; in the second stage, after mixing the first stage ionic liquid with potassium hexafluoro hydrogen phosphate, an anion-replacement reaction is carried out, a second stage ionic liquid can be prepared in 2.5 minutes with the yield of 90 %, and the time is 1/576 of the required time in traditional technology. The use of the invention can rapidly synthesized the first stage ionic liquid, and simultaneously can carry out anion-replacement on the first stage ionic liquid rapidly to obtain the second stage ionic liquid, and after the total reaction time of 4.5 minutes, the yield of the ionic liquid can reach to more than 90 %.

The invention discloses 14C-labeled polystyrene (PS) and its synthesis method and belongs to the field of radioactive isotope 14C-labeled compounds. According to the invention, 14C radioactive isotope label is introduced into the structure of polystyrene (PS). A 14C-labeled site is on a branched chain or a phenyl ring, and is respectively named [beta-14C]-PS and [U-ring-14C6]-PS. The general structural formula is as shown in the Figure 1, wherein * indicates the 14C-labeled site. The synthesis method comprises the following steps: adding the 14C-labeled styrene into non-labeled styrene for dilution, putting into a high-temperature and high-pressure reactor and reacting at 118-123 DEG C for 8-12 h; dissolving reaction products with chloroform, washing with methanol, depositing and purifying to obtain the 14C-labeled polystyrene. The synthesis method has the following advantages: reaction materials are easily available, unreacted raw materials can be recovered, and synthesis cost is low; reaction time is short and efficiency is high; and reaction conditions are mild, operation technique is safe, and the preparation technology is simple. Radioactive purity of the 14C-labelled polystyrene synthesized by the method reaches more than 99%.

The invention relates to a preparation method of a polyacrylamide emulsion. The method is characterized by comprising the following steps: taking dimethyl diallyl ammonia chloride (DMDAAC) as the cationic monomer, taking ammonium sulfate and PDMDAAC respectively as the dispersion medium and the dispersion agent for CPAM dispersion polymerization in a saline water medium, and making acrylamide to carry out free radical copolymerization reactions with quaternary ammonium salt organic compounds so as to generate the water-in-water type cationic polyacrylamide emulsion. The appearance of the emulsion is in a milk white color, and the particle size is smaller than 1 [mu]m, which is in the range of emulsion particle size value. The preparation method adopts a novel polymer synthesis method, and overcomes the shortages existing in the prior art that a large amount of organic solvent and surfactant used in the synthesis process generates secondary pollutions to the environment and the product cost is greatly increased. The emulsion can be widely applied to the fields of oil field, industrial or city sewage processing, sludge dehydration, paper making, and personal nursing and cosmetic.

The invention discloses a sodium hydrosulfite synthesizing and continuous producing method. The sodium hydrosulfite synthesizing and continuous producing method comprises the following steps: taking a synthesizing pot as a tubular reactor; after preparing raw materials AE and ME, transferring the raw materials AE and ME into AE and ME storage tanks via inert gas; adding the raw materials AE and ME in a large synthesis dropwise adding pot; opening the pot and inserting a bottom tube into the large synthesis dropwise adding pot to transfer the materials into a small synthesis dropwise adding pot; keeping the liquid level of the materials in the large dropwise adding pot to be stable relatively in a material transferring process; continuing adding the raw materials AE and ME into the large synthesis dropwise adding pot continuously and uniformly; after the small synthesis dropwise adding pot receives a first batch of materials, enabling a second small dropwise adding pot to begin to receive the material from the large synthesis dropwise adding pot, and enabling the rest dropwise adding pot to begin to receive the material from the large synthesis dropwise adding pot in the same way; continuously adding a SO2-CH3OH solution as a raw material at a suitable speed to an end point by the small dropwise adding pots from the time when the small dropwise adding pots begin to receive the material to the time when reaction reaches the end point; and after insulating and ripening are completed, placing the material in a drying process for subsequent use. A repeated operation process of a reaction process is omitted, so that a synthesis process is continuous, and while the efficiency of the device is improved, consumption of sodium formate and sodium pyrosulfite is reduced.

The invention discloses chlorinated rubber prepared by utilizing recycled tire desulfurized rubber. The chlorinated rubber comprises the following raw materials in parts by weight: 40 to 60 parts of a hydrochloric acid solution with a concentration of 10 to 15wt%, 8.0 to 15.0 parts of the recycled tire desulfuized rubber, 3.0 to 9.0 parts of chlorine, 0.07 to 0.25 part of a dispersant, 0.07 to 0.15 part of an emulsifier and 0.01 to 0.03 part of an initiator. The preparation method comprises the following steps: mixing raw materials, directly introducing liquid chlorine, and carrying out a reaction under heating and pressurizing. The chlorinated rubber prepared by using the method provided by the invention adopts the pollution-free recycled tire rubber obtained by utilizing a novel desulfurization technology as a raw material, and an aqueous acid-phase chlorination method is adopted to prepare the chlorinated rubber and an industrial product--hydrogen chloride contained hydrochloric acid with a concentration of 23 to 26wt%; and the method overcomes the problems of large water consumption and high treatment cost of generated acid-contained wastewater in an aqueous phase method, opens up a novel approach for high-value-added utilization of the recycled tire rubber, and has low cost.