46results about How to "Efficient synthesis process" patented technology

The invention discloses a synthesis method of perfluoroisobutyronitrile, comprising the following steps of: (1) carrying out a reaction between oxalyl chloride monoester and fluoride salt in a solventto obtain oxalyl fluoride monoester; (2) carrying out a reaction between oxalyl fluoride monoester and hexafluoropropylene in a solvent by taking fluoride salt as a catalyst to prepare heptafluoro-2-carbonyl-3-methylbutyrate; (3) carrying out catalytic decarbonylation on heptafluoro-2-carbonyl-3-methylbutyrate in a solvent through cesium fluoride, so as to obtain heptafluoroisobutyrate; and (4) carrying out a reaction between heptafluoroisobutyrate and ammonia, and dehydrating to obtain perfluoroisobutyronitrile. The synthetic method has the advantages of easily available raw materials, mildreaction conditions, high raw material conversion rate and product yield, safe and simple process operation, and easy realization of industrial production.

The invention discloses a method for preparing cellulose carbamate through a liquid-solid-phase reaction. The method comprises the following step: performing esterification reaction on cellulose pulp or activated cellulose pulp and urea as raw materials in a high-boiling-point nonprotonic strong-polarity solvent such as dimethyl formamide (DMF), dimethylacetamide (DMAc), dimethyl sulfoxide (DMSO) or N-methylpyrrolidone (NMP) to synthesize cellulose carbamate. In the process of preparing cellulose carbamate by adopting a liquid-solid-phase method, the used solvent is low in toxicity and easy to recover; the preparation process is simple and convenient, environment-friendly, safe, and controllable; prepared cellulose carbamate can be dissolved in a NaOH solution to form a stable solution and can be used for preparing regenerated cellulose fibers, membranes and the like.

The invention belongs to the technical field of polymer synthesis, and in particular relates to a synthesis method of a reproceesable thermosetting polymer. The method adopts a macromolecular cross-linking agent and utilizes reversible cross-linking effect between macromolecular chains and macromolecular chains to synthesize a reproceesable cross-linked polymer. Specifically, the method includes two parts: synthesis of a functionalized copolymer and crosslinking and curing of the copolymer. The copolymer takes vinyl monomers such as (meth) acrylic acid (ester), acrylamide, styrene and derivatives thereof as main components and vinyl monomers having crosslinkable functional groups as secondary components; cross-linking and curing are realized through dynamic chemical bonds formed between functional groups. Compared with thermoplastic materials with similar chemical compositions, the material synthesized by the invention has better mechanical strength, solvent resistance, creep resistance, aging resistance and the like.

The invention discloses a synthesis method of a bidentate phosphorene ligand, and belongs to the technical field of organic chemistry. Biaryl-2-(disubstituent) phosphine 1 and an alkenyl bromide 2 areadopted as raw materials, and react in an organic solvent at 40-180 DEG C in the presence of a ruthenium catalyst, a ligand and an alkali to obtain the bidentate phosphorene ligand 2-(disubstituent)phosphine-2'-olefin 3. The synthesis steps are simple, and the method can be completed only through one step, active functional groups or complex reaction steps do not need to be introduced to construct C-C bonds in the synthesis process, the synthesis process is efficient, and the operation process is simple; and raw materials are cheap and easy to obtain, the product yield reaches 93%, the requirement for process equipment is low, the reaction process is more environmentally friendly, and potential large-scale industrial production and application prospects are achieved.

The invention discloses a process for synthesizing ethyl chloride. In a closed reactor, an ethyl chloride product can be obtained from ethanol and hydrogen chloride gas under the catalytic effect of AlCl3-ZnCl2 double component catalyst by gradually heating for reaction, releasing step by step and recovering. The high activity of AlCl3-ZnCl2 double component catalyst is used in the method, reaction temperature and by-product diethyl ether are reduced, and the yield of the ethyl chloride is increased to above 95%; by the use of the hydrogen chloride for replacement of industrial hydrochloric acid, mother liquor and distillate are directly continuously applied, energy consumption for distillation distillate recovery and hydrogen chloride loss are effectively reduced, environment pollution caused by production of a lot of high salt wastewater and organic waste acid can be avoided; in addition, by use of a closed staged heating reaction way, a catalytic substitution reaction is performed in a liquid phase system, substrate contact reaction time is increased, ethanol conversion rate reduction caused by too fast escaping of excessive hydrogen chloride from the reactor can be avoided, the consumption increase of the hydrogen chloride is avoided, and the atmospheric pollution is reduced.

The invention discloses a synthesis method of alkyl phosphinic acid and aluminium salt thereof under a normal-pressure mild condition. A hypophosphorous acid solution and alcohol are adopted as raw materials, by means of an organic solvent which has an azeotropy point with water, through in-situ reaction of olefin, the alkyl phosphinic acid is synthesized, after reaction is completed, the pH is adjusted, an aluminium salt solution is added, and alkyl aluminum hypophosphite precipitates as a white precipitate. According to the synthesis method of the alkyl phosphinic acid and the aluminium saltthereof under the normal-pressure mild condition, operation is simple and convenient, concentration of the hypophosphorous acid solution is avoided, energy consumption is reduced, and the efficiencyis improved; the alcohol not only can be used as the raw material for in-situ reaction of the olefin, but also can promote homogeneous system generation of the reaction, so that inconvenience of easyauto-agglutination brought by using acetic acid as a solvent and using olefin as an oligomer is eliminated; by using the solvent co-boiling with water, the purposes of solvent recovery and recycle areachieved, and it is easier to obtain the high-quality salt-forming product; the method is implemented under the normal-pressure mild condition, a security coefficient is high, the reaction risk is small, a synthesis technology is more energy-saving, environmentally friendly and efficient, and industrial production is easier to achieve.

The invention relates to a preparation method of an Mn monatomic-loaded N-doped carbon polyhedral catalyst, which comprises the following steps: (1) stirring and dissolving manganese salt and zinc nitrate in a solvent to obtain a solution A, stirring and dissolving an N-containing organic ligand in the solvent to obtain a solution B, stirring and mixing the solution A and the solution B, standing and aging, centrifuging, filtering and washing, and freeze-drying; (2) carrying out primary heat treatment under the protection of inert atmosphere; (3) dispersing in a manganese salt solution, stirring, and freeze-drying; and (4) carrying out secondary heat treatment under the protection of an inert atmosphere to obtain the Mn monatomic-loaded N-doped carbon polyhedral catalyst. The catalyst obtained through the method is good in dispersion, the metal Mn is dispersed in an atomic scale, Mn, N and C elements are evenly distributed, the electro-catalytic oxygen reduction performance is good, the rate performance is superior to that of a commercial Pt/C catalyst, and the catalyst is simple in synthesis process, efficient, low in cost, high in universality and suitable for industrial production.

The invention belongs to the technical field of high polymer materials, and particularly relates to a dynamic covalent cross-linking material for enhancing polyethylene performance and a preparation method and application thereof. The dynamic covalent cross-linking material is prepared from linear polyethylene with a borate group and a borate cross-linking agent through a borate exchange reaction,wherein the borate cross-linking agent is prepared from polybasic boric acid molecules and 1, 2-diol molecules or 1, 3-diol molecules through a dehydration condensation reaction; according to the dynamic covalent cross-linking polyethylene material, conversion and recombination of a polymer network can be realized through reversible exchange reaction among different borate groups. The dynamic covalent cross-linking polyethylene is added into commercial thermoplastic polyethylene to synthesize a polyethylene/dynamic cross-linked polyethylene composite polymer material; the mechanical properties (such as tensile strength and Young's modulus), creep resistance, solvent resistance, heat resistance and the like of the composite polymer material are remarkably enhanced, and the composite polymer material can be used for repeated processing, repeated shaping and 3D printing.

The invention provides a continuous synthesis method of a 2-chloropyrimidine-4-formic acid compound. The 2-chloropyrimidine-4-formic acid compound has a structure represented by a formula I, wherein in the formula I, R1 and R2 are respectively and independently selected from hydrogen, alkoxy, aryl, benzyl or fluorine. The synthesis method comprises the following steps: S1, under the action of a non-noble metal catalyst, carrying out continuous methylation reaction on a compound A and a methyl Grignard reagent B to obtain a compound C, wherein the compound A is a compound shown in the specification, the compound C is a compound shown in the specification, R1 and R2 are respectively and independently selected from hydrogen, alkoxy, aryl, benzyl or fluorine, and the non-noble metal catalyst is one or more of ferric salt, cobalt salt and nickel salt; and S2, carrying out continuous oxidation reaction on the compound C under the action of oxygen, an oxidation catalyst and an additive, and thus obtaining the 2-chloropyrimidine-4-formic acid compound. By adopting the process provided by the invention to synthesize the 2-chloropyrimidine-4-formic acid compound, the aspects of cost, yield,environmental friendliness and the like can be considered.

The invention discloses a preparation method of ketoprofen. The method takes m-bromobenzoic acid and benzene as starting raw materials, and the ketoprofen is prepared through the steps of acylating, protecting a carbonyl group, taking a Grignard reagent, reacting with propylene oxide, oxidizing, de-protecting and the like. The method disclosed by the invention has the characteristics of short reaction route, easiness of obtaining the raw materials, high yield and low cost.

The invention discloses a BaTiO3/BiOIO3 composite material as well as a preparation method and application thereof, belongs to the technical field of photocatalysis, and solves the technical problems that an existing catalytic material is low in solar energy conversion efficiency, only responds to a part of light and the like during photocatalytic reaction. According to the preparation method of the BaTiO3/BiOIO3 composite material disclosed by the invention, BiOIO3 and BaTiO3 with proper energy band structures are selected, a hydrothermal method is adopted, BiOIO3 is introduced to the surface of BaTiO3 powder to prepare and construct the composite material, the hydrothermal reaction condition is mild, the time is short, and the preparation method is suitable for industrial production; the photodegradation efficiency of the obtained BaTiO3/BiOIO3 composite material is far higher than that of pure-phase BaTiO3 and BiOIO3, and the BaTiO3/BiOIO3 composite material is expected to be applied to the fields of sewage treatment and the like.

The invention discloses a method for synthesizing Nitro-PAPS. The chemical structural formula of the Nitro-PAPS is shown in the description. The Nitro-PAPS serves as commercialized hypersensitive colorimetric reagent for detecting Fe(II) in serum, and is also used for detecting zinc in the serum, has the advantages of high sensitivity, good accuracy, simple and stable reagent, small interference,rapid, simple and convenient operation and the like, and is widely used in biochemical detection. The price of the Nitro-PAPS is expensive, and the literature and patent reports for the synthesis method of the Nitro-PAPS are few, therefore, the invention provides a simple efficient synthesis method with high yield, mild reaction condition and very suitable for industrialized production. Accordingto the method, cheap m-aminophenol serves as a raw material, the m-aminophenol, bromopropane and 1,3-propane sultone are subjected to two-step nucleophilic substitution reaction, lastly, the m-aminophenol and diazonium salt of 2-amino-5-nitropyridine are coupled, and the Nitro-PAPS is synthesized by three steps with a high yield. The whole synthesis technology is simple and efficient, has low cost, and is an economically feasible industrialized production method.

The invention relates to an allylated monophosphine ligand and a preparation method thereof, and belongs to the technical field of organic chemistry. A compound 1 and a compound 2 are used as raw materials and react in an inert atmosphere at 60-140 DEG C in the presence of a ruthenium catalyst, a ligand, alkali, an additive and an organic solvent, and the novel allylated monophosphine ligand is prepared after treatment. The preparation method disclosed by the invention is simple in synthesis step, can be completed by only one step, has the advantages of easily available raw materials, simple and convenient process operation, high efficiency, rapidness, reduction of production cost and requirements on equipment and the like, is high in product yield, and is easy to realize industrial large-scale production.

The invention relates to the technical field of production of manganese glutamate, and particularly discloses a production process of feed-grade manganese glutamate. The process adopts a wet synthesis process and comprises the following steps: reacting manganese sulfate with glutamic acid in a solution to obtain a manganese glutamate solution by controlling the reaction temperature and the reaction time, cooling and crystallizing to obtain a manganese glutamate product, performing drying to remove surface moisture, and then screening to remove large-particle products so as to obtain the feed-grade manganese glutamate. The process is low in energy consumption, green and environment-friendly, and does not generate substances polluting the environment, and various indexes such as the product content and heavy metals can meet the quality requirements of the feed-grade manganese glutamate; as only heating and stirring are needed in the production process, complex operations such as ultrasonic are not needed, and the equipment cost is low; the synthesis process is carried out in water, no harmful by-product is generated, mother liquor can be recycled, organic solvent extraction is not needed, the process is green and environment-friendly, post-treatment is simple, and no three wastes are generated; and the synthesis process is environment-friendly, economical and efficient.

The invention relates to the technical field of zinc glutamate production, and particularly discloses a production process of feed-grade zinc glutamate, which comprises the following steps: adopting a wet synthesis process, adopting zinc and glutamic acid to react in a solution, obtaining a zinc glutamate solution by controlling the reaction temperature and the reaction time, obtaining a zinc glutamate product by cooling crystallization, through drying, removing surface moisture, and screening to remove large-particle products, thereby obtaining the feed-grade zinc glutamate. The process is low in energy consumption, green and environment-friendly, and does not generate substances polluting the environment, and various indexes such as product content and heavy metals can meet the quality requirements of feed-grade zinc glutamate; as only heating and stirring are needed in the production process, complex operations such as ultrasonic are not needed, and the equipment cost is low; the synthesis process is carried out in water, no harmful by-product is generated, mother liquor can be recycled, organic solvent extraction is not needed, the process is green and environment-friendly, post-treatment is simple, and no three wastes are generated; and the synthesis process is environment-friendly, economical and efficient.