Preparation method for 2-methyl-1,4-naphthoquinone and an intermediate thereof. The preparation method for the intermediate 2-methyl-1,4-tetrahydronaphthoquinone comprises: subjecting o-methylbenzoquinone and 1,3-butadiene to an addition reaction under the catalytic action of a metal chelating ionic liquid as represented by formula (I), so as to generate 2-methyl-1,4-tetrahydronaphthoquinone. The method can realize the preparation of 2-methyl-1,4-tetrahydronaphthoquinone with high efficiency, high selectivity and relative safety, and can be used in the preparation of 2-methyl-1,4-naphthoquinone.
Provided are a preparation method for a benzoquinone compound and a preparation method for 2-methyl-1,4-naphthoquinone. A phenolic compound undergoes an oxidation reaction in a catalytic system in the presence of an oxidizing agent to generate a benzoquinone compound; the oxidizing agent is oxygen; the catalytic system contains 4-R-2,2,6,6-tetramethylpiperidinooxy, nitrite, protonic acid, and a solvent; R is -H, -OH, -NHAc, -COOH, -COOPh or (1); the protonic acid is at least one selected from trifluoromethanesulfonic acid, methanesulfonic acid, p-toluenesulfonic acid, a hydrogen chloride alcoholic solution, and sulfuric acid; and the solvent is at least one selected from methanol, ethanol, propanol, tert-butanol, water, and acetonitrile. According to the method, benzoquinone compounds can be obtained in high yields, oxygen can be used as an oxidizing agent, environmental friendliness is achieved, and a metal catalyst is not required, so that the use of a halogen and a transition metal can be avoided, thereby facilitating the preparation of high-quality 2-methyl-1,4-naphthoquinone or other benzoquinone compounds.
C07C 46/08 - Preparation of quinones by oxidation giving rise to quinoid structures of at least one hydroxy group on a six-membered aromatic ring with molecular oxygen
C07C 50/02 - Quinones with monocyclic quinoid structure
C07C 50/10 - Quinones the quinoid structure being part of a condensed ring system containing two rings
B01J 31/26 - Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups
A production process for a heterogeneous nitrogen-doped carbon material supported cobalt catalyst and vitamin K3. A preparation method for the catalyst comprises: mixing well glucosamine hydrochloride, melamine, and cobalt acetate, and sintering in an inert atmosphere, the feeding mass ratio of glucosamine hydrochloride to melamine being 1:25-45, and the feeding mole ratio of glucosamine hydrochloride to cobalt acetate being 1:0.01-0.75; further, subjecting 2-methyl-1,4-tetrahydronaphthoquinone to an oxidative dehydrogenation reaction in a catalytic system in the presence of an oxidizing agent to produce 2-methyl-1,4-naphthoquinone, namely vitamin K3, the catalytic system comprising the described heterogeneous nitrogen-doped carbon material supported cobalt catalyst and a solvent. Practice shows that the catalyst can efficiently catalyze the oxidative dehydrogenation of 2-methyl-1,4-tetrahydronaphthoquinone; the yield is high, and the catalyst is easy to recover, which helps reduce costs.
The present invention discloses a method for preparing taurine. The method comprises: (1) in the presence of an ammonia water complex ion catalyst, subjecting an aqueous sodium isethionate solution and ammonia to an ammonolysis reaction to obtain a reaction solution containing sodium taurate; (2) subjecting the reaction solution containing sodium taurate to deamination, concentration and dewatering, acidification, and crystallization to obtain taurine and a mother solution, wherein the ammonia water complex ion catalyst is obtained by complexing ammonia with a catalyst precursor, and the catalyst precursor comprises one or more metal elements of chromium, zinc, nickel, cobalt, copper, and silver. The method has the advantages of mild process conditions, a short reaction time, a high yield, a simple catalyst source, etc.
C07C 303/30 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfonic acids by reactions not involving the formation of esterified sulfo groups
C07C 309/14 - Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
B01J 31/18 - Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony
5.
Method for preparing taurine and method for recovering mother liquor thereof
The present disclosure relates to a method for preparing taurine and a method for recovering a mother liquor thereof. The method for recovering the taurine mother liquor comprises: providing a taurine mother liquor, and mixing the taurine mother liquor and a treating agent to obtain a solid-containing suspension, wherein the treating agent is a water-soluble organic solvent or a mixture of the water-soluble organic solvent and water; filtering the suspension to obtain a first solid product and a first filtrate; and dissolving the first solid product with an ammonia source, and then filtering same to obtain a second solid product and a second filtrate.
C07C 303/22 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids by reactions not involving the formation of sulfo or halosulfonyl groups
C07C 303/32 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
6.
METHOD FOR PREPARING SODIUM TAURATE AS TAURINE INTERMEDIATE, AND METHOD FOR PREPARING TAURINE
A method for preparing sodium taurine as a taurine intermediate is provided in the present disclosure. The method comprises the following steps: providing sodium hydroxyethyl sulfonate and an ammonia source; and placing the sodium hydroxyethyl sulfonate and the ammonia source in an aminolysis reactor for an aminolysis reaction to obtain a mixture containing sodium taurine as a taurine intermediate, wherein the molar ratio of ammonia in the ammonia source to the sodium hydroxyethyl sulfonate is greater than or equal to 25:1. A method for preparing taurine is further provided.
C07C 309/14 - Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
B01J 19/24 - Stationary reactors without moving elements inside
B01J 3/00 - Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matterApparatus therefor
Provided are a 2,3,5-trimethylhydroquinone synthesis method and device; 2,3,5-trimethylbenzoquinone (TMBQ) is mixed with an alcohol–aromatic hydrocarbon or alcohol–alkane mixed solvent system, then the reaction liquid is thoroughly mixed with hydrogen by way of a hydrogen absorber, then enters a fixed bed equipped with a precious-metal catalyst to carry out a hydrogenation reaction to obtain 2,3,5-trimethylhydroquinone (TMHQ). The technical solution improves the selectivity of the reaction, effectively suppresses side reactions, reducing the impurity content of the product, improving the purity of 2,3,5-trimethylhydroquinone (TMHQ), simplifying the production process, and reducing emission of wastewater, waste gas, and solid waste, and has good environmental protection benefits.
C07C 37/07 - Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by conversion of non-aromatic six-membered rings or of such rings formed in situ into aromatic six-membered rings, e.g. by dehydrogenation with simultaneous reduction of C=O group in that ring
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
Disclosed is an HPLC method for detecting a biotin intermediate diamino substance. The method comprises the following steps: dissolving a cyclization reaction solution in a biotin synthesis process by means of using a mobile phase, and then, carrying out detecting under the following chromatographic conditions: the chromatographic columns being C18-WCX mixed columns, the detection wavelength being 195-220 nm, the test time being 16-20 min, and the mobile phase being an acetonitrile-phosphate buffer solution. According to the detection method, the appearance time of a substance to be detected, a diamino substance, can be stabilized within 10-12 min, so that the problem of peak superposition of the diamino substance and a solvent peak is solved, and testing is more accurate and reliable.
Provided are a continuous ammonolysis reaction system, and a method for preparing taurine alkali metal salt and taurine using the continuous ammonolysis reaction system. The continuous ammonolysis reaction system comprises a high-pressure reaction device, the high-pressure reaction device comprises n ammoniating autoclaves, n≥2, the first ammoniating autoclave to the nth ammoniating autoclave are connected in series in sequence, the ammoniating autoclave is a vessel for the ammonolysis reaction, the ammonolysis reaction uses ammonia as an ammoniating agent, the first ammoniating autoclave is connected with a feeding device, the first ammoniating autoclave to the nth ammoniating autoclave are all connected with a first feed pipe, each ammoniating autoclave is connected with a second feed pipe; a buffer device, the buffer device is connected with the nth ammoniating autoclave, which is used to receive the mixed materials after the ammonolysis reaction in the first ammoniating autoclave to the nth ammoniating autoclave; a flashing device, the flashing device is connected with the buffer device, which is used to receive the mixed materials in the buffer device and obtain the ammonolysis product by means of flashing.
C07C 303/32 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
C07C 303/02 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
C07C 309/14 - Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
10.
CARBON MATERIAL SUPPORTED NANO PALLADIUM ALLOY CATALYST MODIFIED BY CALCIUM CARBONATE, PREPARATION METHOD THEREFOR AND USE THEREOF
The present invention relates to a carbon material supported nano palladium alloy catalyst modified by calcium carbonate, a preparation method therefor, and the use of the carbon material supported nano palladium alloy catalyst modified by calcium carbonate as a catalyst in a reaction for the selective hydrogenation reduction of a C20 alkynol a to C20 enol. The preparation method for the carbon material supported nano palladium alloy catalyst modified by calcium carbonate comprises the following steps: (1) stirring and mixing activated carbon and a carbonate aqueous solution until uniform, heating same and maintaining the temperature, and after the temperature maintaining is over, slowly dropwise adding an acidic calcium salt solution, heating same and maintaining the temperature, and post-treating same to obtain a calcium carbonate modified carbon material; and (2) impregnating the calcium carbonate modified carbon material in a Pd precursor solution, and sequentially subjecting same to stirring, reduction by adding a chemical reagent, a toxifying treatment by adding a cocatalyst, washing and drying, to obtain the carbon material supported nano palladium alloy catalyst modified by calcium carbonate.
C07C 29/17 - Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds
C07C 33/14 - Alcohols containing rings other than six-membered aromatic rings containing six-membered rings
11.
METHOD FOR PREPARING TAURINE AND METHOD FOR RECOVERING MOTHER LIQUOR THEREOF
The present application relates to a method for preparing taurine and a method for recovering a mother liquor thereof. The method for recovering the taurine mother liquor comprises: providing a taurine mother liquor, and mixing the taurine mother liquor and a treating agent to obtain a solid-containing suspension, wherein the treating agent is a water-soluble organic solvent or a mixture of the water-soluble organic solvent and water; filtering the suspension to obtain a first solid product and a first filtrate; and dissolving the first solid product with an ammonia source, and then filtering same to obtain a second solid product and a second filtrate.
C07C 309/14 - Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
The present invention provides an ammonolysis reaction system, comprising: an ammonolysis reactor, which is a vessel for an ammonolysis reaction, the ammonolysis reaction using ammonia as an aminating agent; an ammonia separation device connected to the ammonolysis reactor and used for separating the ammonia that does not participate in the reaction after the ammonolysis reaction to obtain an ammonia-containing gaseous substance; and a compression device separately connected to the ammonia separation device and the ammonolysis reactor, and used for compressing the ammonia-containing gaseous substance obtained by separation to obtain a supercritical fluid, and circulating the supercritical fluid to the ammonolysis reactor. The present invention also provides methods for preparing a taurine intermediate taurine sodium and taurine by using the ammonolysis reaction system.
C07C 303/32 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
C07C 309/14 - Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
13.
METHOD FOR PREPARING SODIUM TAURATE AS TAURINE INTERMEDIATE, AND METHOD FOR PREPARING TAURINE
Provided is a method for preparing sodium taurate as a taurine intermediate. The method comprises the following steps: providing sodium hydroxyethyl sulfonate and an ammonia source; and placing the sodium hydroxyethyl sulfonate and the ammonia source in an aminolysis reactor for an aminolysis reaction to obtain a mixture containing sodium taurate as a taurine intermediate, wherein the molar ratio of ammonia in the ammonia source to the sodium hydroxyethyl sulfonate is 25:1 or above. Also provided is a method for preparing taurine.
C07C 303/32 - Preparation of esters or amides of sulfuric acidsPreparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
C07C 309/14 - Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
Provided is a method for synthesizing keto-isophorone. The method comprising: using 3,5,5-trimethyl-4-hydroxy-2-cyclohexene-1-one (HIP) as a raw material; using a benzoquinone compound (II) as an oxidizing agent and a catalyst; introducing oxygen or air; oxidizing an inert solvent to generate a keto-isophorone (KIP) and a hydroquinone compound (III);
C07C 45/37 - 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 C—O— functional groups to C=O groups
C07C 45/78 - SeparationPurificationStabilisationUse of additives
C07C 49/603 - Unsaturated compounds containing a keto group being part of a ring of a six-membered ring, e.g. quinone methides
patents
