A porous polymer has a pore volume of 0.3 to 2.5 cm3/g and comprises a pore having a first pore diameter and a pore having a second pore diameter. A ratio of pore volume of the pore having a first pore diameter to pore volume of the pore having a second pore diameter is 1 to 10:1. The porous polymer is obtained by self-polymerization or copolymerization of at least one of the phosphorus ligands, and phosphorous content of the porous polymer is 1 to 5 mmol/g. The porous polymer-nickel catalyst made of the porous polymer has a significant increase in water resistance, which may reduce the consumption of phosphorus ligands, eliminating the steps of removing water from raw materials and reaction system water control, which greatly saves process equipment investment. When used in the preparation of adiponitrile from butadiene, it has high catalytic activity, high reaction selectivity, and high linearity.
B01J 31/06 - Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
C08F 30/02 - Homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
C08J 9/14 - Working-up of macromolecular substances to porous or cellular articles or materialsAfter-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
B01J 31/28 - Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups of the platinum group metals, iron group metals or copper
B01J 35/10 - Solids characterised by their surface properties or porosity
B01J 35/00 - Catalysts, in general, characterised by their form or physical properties
C07C 253/10 - Preparation of carboxylic acid nitriles by addition of hydrogen cyanide or salts thereof to unsaturated compounds to compounds containing carbon-to-carbon double bonds
2.
ADDITIVE USED IN METHIONINE PREPARATION PROCESS, AND METHIONINE PREPARATION METHOD
The present disclosure relates to an additive used in a methionine preparation process, and a methionine preparation method. The additive provided by the present disclosure is a mixture containing components A, B, and C; component A has a structure represented by the following general formula (1); component B has a structure represented by the following general formula (2); component C is silicone oil; RCON(CH3)CH2CH2SO3Na (1). The methionine preparation method provided in the present invention comprises subjecting methionine to crystallization and/or recrystallization in the presence of the additive provided by the present disclosure. The additive provided by the present disclosure results in uniform emulsification, has good stability, can be used stably for a long time, and is suitable for a continuous crystallization process. The prepared methionine crystal has a good crystal form, a large bulk density, and good flowability. In addition, according to the methionine preparation method of the present disclosure, a crystallization system can operate continuously and stably for a long time without obvious foaming, and the crystallization process of the methionine product can proceed smoothly.
The present disclosure relates to an additive used in a methionine preparation process, and a methionine preparation method. The additive provided by the present disclosure is a mixture containing components A, B, and C; component A has a structure represented by the following general formula (1); component B has a structure represented by the following general formula (2); component C is silicone oil; RCON(CH3)CH2CH2SO3Na (1). The methionine preparation method provided in the present invention comprises subjecting methionine to crystallization and/or recrystallization in the presence of the additive provided by the present disclosure. The additive provided by the present disclosure results in uniform emulsification, has good stability, can be used stably for a long time, and is suitable for a continuous crystallization process. The prepared methionine crystal has a good crystal form, a large bulk density, and good flowability. In addition, according to the methionine preparation method of the present disclosure, a crystallization system can operate continuously and stably for a long time without obvious foaming, and the crystallization process of the methionine product can proceed smoothly.
A porous polymer having a pore volume of 0.3-2.5 cm3/g, the porous polymer comprising pores having a first pore diameter and pores having a second pore diameter, wherein the pore volume ratio of the pores having the first pore diameter to the pores having the second pore diameter is 1-10:1. The porous polymer is obtained by means of self-polymerization or copolymerization of at least one phosphorus ligand, and the phosphorus content of the porous polymer is 1-5 mmol/g. A porous polymer-nickel catalyst prepared from the porous polymer has significantly improved water resistance, can reduce the consumption of phosphorus ligands, omits the steps of water removal of raw materials and water control of a reaction system, and greatly saves on process equipment investment. In addition, when used for preparing adiponitrile by using butadiene, the catalyst has a high catalytic activity, a high reaction selectivity and high linearity, and is easy to recycle and reuse.
C08F 230/02 - Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
C08J 9/00 - Working-up of macromolecular substances to porous or cellular articles or materialsAfter-treatment thereof
B01J 31/18 - Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony
C07C 253/10 - Preparation of carboxylic acid nitriles by addition of hydrogen cyanide or salts thereof to unsaturated compounds to compounds containing carbon-to-carbon double bonds
C07C 255/04 - Carboxylic acid nitriles having cyano groups bound to acyclic carbon atoms of an acyclic and saturated carbon skeleton containing two cyano groups bound to the carbon skeleton
B01J 35/10 - Solids characterised by their surface properties or porosity
C08L 43/02 - Homopolymers or copolymers of monomers containing phosphorus
4.
ADDITIVE USED IN METHIONINE PREPARATION PROCESS, AND METHIONINE PREPARATION METHOD
32233Na (1). The methionine preparation method provided in the present invention comprises crystallization and/or recrystallization of methionine in the presence of the additive provided by the present invention. The additive provided by the present invention results in uniform emulsification, has good stability, can be used stably for a long time, and is suitable for a continuous crystallization process. The prepared methionine crystal has a good crystal form, a large bulk density, and good fluidity. In addition, according to the methionine preparation method of the present invention, a crystallization system can operate continuously and stably for a long time without obvious foaming, and the crystallization process of the methionine product can proceed smoothly.
C07C 323/58 - Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atoms of the thio groups bound to acyclic carbon atoms of the carbon skeleton the carbon skeleton being further substituted by nitrogen atoms, not being part of nitro or nitroso groups with amino groups bound to the carbon skeleton
C07C 319/26 - SeparationPurificationStabilisationUse of additives
5.
Method and device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof
Provided by the present disclosure are a method and a device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile. The method for preparing 2-hydroxy-4-methylthiobutyric acid provided by the present disclosure comprises: step (1), a step of reacting acrolein with methyl mercaptan to prepare 3-methylthiopropionaldehyde; step (2), a step of reacting 3-methylthiopropionaldehyde with hydrocyanic acid to prepare 2-hydroxy-4-methylthiobutyronitrile; and step (3), a step of hydrating 2-hydroxy-4-methylthiobutyronitrile by using sulfuric acid and then hydrolyzing to prepare 2-hydroxy-4-methylthiobutyric acid; wherein in steps (1), (2) and (3), the reaction status of the materials is detected online, and the proportions of the materials are controlled according to the detection results such that reactions are performed completely.
C07C 319/20 - Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by reactions not involving the formation of sulfide groups
C07C 319/18 - Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by addition of thiols to unsaturated compounds
B01J 19/24 - Stationary reactors without moving elements inside
C07C 323/52 - Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atoms of the thio groups bound to acyclic carbon atoms of the carbon skeleton the carbon skeleton being acyclic and saturated
6.
Method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine
SHANDONG NHU FINE CHEMICAL SCIENCE AND TECHNOLOGY COMPANY LTD. (China)
Inventor
Chen, Zhirong
Mao, Jianyong
Hu, Baishan
Li, Guanbing
Li, Haoran
Wang, Yu
Yang, Yingkuo
Liu, Qing
Tang, Jiyu
Chen, Weiyong
Abstract
The present disclosure relates to a method for preparing isophorone diamine by means of a hydrogenation reduction of isophorone nitrile imine. The hydrogenation reduction is continuously carried out in a multi-stage bubble column reactor loaded with a supported alkaline cobalt-based catalyst, wherein isophorone nitrile imine is successively in countercurrent contact with hydrogen in each stage of the reactor to carry out a hydrogenation reduction reaction, so as to obtain the isophorone diamine. The preparation method solves the problem of back-mixing, and further improves the conversion rate and the cis/trans ratio of the product.
C07C 209/52 - Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of imines or imino-ethers
B01J 23/78 - Catalysts comprising metals or metal oxides or hydroxides, not provided for in group of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups with alkali- or alkaline earth metals or beryllium
C07C 209/48 - Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of nitriles
7.
CATALYST FOR PREPARING ACRYLIC ACID OR ACROLEIN AND PREPARATION METHOD THEREFOR
abcdeff, where X is selected from at least one of Fe, Co, and Ni, Y is selected from at least one of Na, K, Cs, Ba, La, and Ce, Z is selected from at least one of V, W, and Cr, a:b:c:d:e = 12:(0.5-2.5):(0.5-3):(0.005-0.5):(0.5-10), and f is the total number of oxygen atoms required to satisfy the valences of other elements.
B01J 23/78 - Catalysts comprising metals or metal oxides or hydroxides, not provided for in group of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups with alkali- or alkaline earth metals or beryllium
C07C 27/12 - Processes involving the simultaneous production of more than one class of oxygen-containing compounds by oxidation of hydrocarbons with oxygen
C07C 45/35 - Preparation of compounds having C=O groups bound only to carbon or hydrogen atomsPreparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties in unsaturated compounds in propene or isobutene
xx, where 0 < x ≤ 3, and the carrier is a metal oxide having an oxygen vacancy on the surface thereof; the elementary Mo in the active component molybdenum is combined with the oxygen vacancy to form a Mo-[O]-M structure, wherein [O] represents the oxygen vacancy, and M is a metal element in the carrier, and the active component molybdenum is distributed on the surface of the carrier in the form of nanoparticles.
Provided by the present invention are a method and device for preparing 2-hydroxy-4-methylthiobutyric acid and intermediates thereof; the intermediates for preparing 2-hydroxy-4-methylthiobutyric acid comprise 3-methylthiopropionaldehyde and 2-hydroxy-4-methylthiobutyronitrile. The method for preparing 2-hydroxy-4-methylthiobutyric acid provided by the invention comprises: step (1), a step of causing acrolein to react with methyl mercaptan to prepare 3-methylthiopropionaldehyde; step (2), a step of causing 3-methylthiopropionaldehyde to react with hydrocyanic acid to prepare 2-hydroxy-4-methylthiobutyronitrile; step (3), a step of hydrating 2-hydroxy-4-methylthiobutyronitrile by using sulfuric acid, and then rehydrolyzing to prepare 2-hydroxy-4-methylthiobutyric acid; in steps (1), (2), and (3), the reaction conditions of the materials are detected online, and the proportions of the materials are controlled according to the detection results such that reactions are performed completely.
C07C 319/20 - Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides by reactions not involving the formation of sulfide groups
SHANDONG NHU FINE CHEMICAL SCIENCE AND TECHNOLOGY COMPANY LTD. (China)
SHANDONG NHU PHARMACEUTICAL CO., LTD. (China)
Inventor
Chen, Zhirong
Liu, Jinlong
Qiu, Guisheng
Wang, Zhixuan
Ma, Xiao
Zhou, Yougui
Chen, Weiyong
Liu, Xiaoqing
Abstract
Provided by the present invention is a device used for evaporation and crystallization. The device comprises an evaporation container and a crystallization container. The device used for evaporation and crystallization further comprises a first circulation unit and a second circulation unit. The first circulation unit comprises a first branch pipe, a first circulation pump, and a first circulation inlet pipe that are successively connected. The second circulation unit comprises a second branch pipe, a second circulation pump, a heater, and a second circulation inlet pipe that are successively connected. The first circulation inlet pipe and the second circulation inlet pipe are connected to the evaporation container. By means of providing an additional first circulation loop, a portion of fine crystals are reintroduced into the crystallization container as a crystal nucleus, and a product that has more uniform particles and a controllable particle size is finally obtained.
SHANDONG NHU FINE CHEMICAL SCIENCE AND TECHNOLOGY COMPANY LTD. (China)
Inventor
Chen, Zhirong
Mao, Jianyong
Hu, Baishan
Li, Guanbing
Li, Haoran
Wang, Yu
Yang, Yingkuo
Liu, Qing
Tang, Jiyu
Chen, Weiyong
Abstract
The present invention relates to a method for preparing isophorone diamine by means of a hydrogenation reduction of isophorone nitrile imine. The hydrogenation reduction is continuously carried out in a multi-stage bubble column reactor loaded with a supported alkaline cobalt catalyst, wherein isophorone nitrile imine is successively in countercurrent contact with hydrogen in each stage of the reactor, so as to obtain the isophorone diamine. The preparation method solves the problem of back-mixing, and further improves the conversion rate and the cis:trans product ratio.
C07C 209/52 - Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of imines or imino-ethers
C07C 209/48 - Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers by reduction of nitriles
C07C 211/36 - Compounds containing amino groups bound to a carbon skeleton having amino groups bound to carbon atoms of rings other than six-membered aromatic rings of a saturated carbon skeleton containing at least two amino groups bound to the carbon skeleton
B01J 8/02 - Chemical or physical processes in general, conducted in the presence of fluids and solid particlesApparatus for such processes with stationary particles, e.g. in fixed beds
Grains [cereals]; live animals; seeds for planting; animal
foodstuffs; by-products of the processing of cereals, for
animal consumption; stall food for animals; mash for
fattening livestock; cattle food; malt for brewing and
distilling; litter for animals.
Grains [cereals]; live animals; seeds for planting; animal
foodstuffs; by-products of the processing of cereals, for
animal consumption; stall food for animals; mash for
fattening livestock; cattle food; malt for brewing and
distilling; litter for animals.
14.
Method for continuous preparation of high bulk density methionine crystal
The present disclosure relates to a method for continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate solution, which is obtained from a reaction of 5-(β-methylmercaptoethyl) hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after being cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer and is sprayed in the form of liquid droplet or trickle into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the obtained mixture grows on fine crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a deposition area in the middle part of the crystallization region, the crystals having larger particle diameters deposits into an elutriation leg, while the fine crystals circulate with the external circulation material, and a part of the external circulation material is used to elutriate the crystals in the elutriation leg, while another part of the same is used to be mixed with the hydrolysate solution; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.
C07C 323/58 - Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atoms of the thio groups bound to acyclic carbon atoms of the carbon skeleton the carbon skeleton being further substituted by nitrogen atoms, not being part of nitro or nitroso groups with amino groups bound to the carbon skeleton
15.
METHOD FOR CONTINUOUS PREPARATION OF HIGH BULK DENSITY METHIONINE CRYSTAL
The present invention relates to a method for the continuous preparation of high bulk density methionine crystals. The process of the method is as follows: a hydrolysate, which is obtained from a reaction of 5-(β-methylthioethyl)hydantoin and a potassium carbonate solution, is mixed with an external circulation material from a DTB neutralization crystallizer having a gas phase neutralization section; after the mixture is cooled, the mixture enters a liquid distributor of a neutralization region in the upper part of the crystallizer; the mixture is sprayed in liquid droplets or trickles into carbon dioxide gas for neutralization reaction, and then naturally falls into a crystallization region in the lower part to be mixed with a material in the region; the mixture grows on small crystals in a system to form crystals having larger particle diameters, and meanwhile new crystal nucleuses are formed; in a settling region in the middle part of the crystallization region, the crystals having larger particle diameters sink into an elutriation leg, while the small crystals circulate with the external circulation material, and a part of the external circulation material is used for elutriating the crystals in the elutriation leg, and another part of the same is used for mixing with the hydrolysate; and the crystals in the elutriation leg are separated, washed and dried to obtain the high bulk density methionine product.
C07C 323/58 - Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atoms of the thio groups bound to acyclic carbon atoms of the carbon skeleton the carbon skeleton being further substituted by nitrogen atoms, not being part of nitro or nitroso groups with amino groups bound to the carbon skeleton
