Abstract

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.

IPC Classes  ?

• C07C 46/00 - Preparation of quinones
• C07C 50/10 - Quinones the quinoid structure being part of a condensed ring system containing two rings
• B01J 31/02 - Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
• C07F 1/08 - Copper compounds
• C07F 9/54 - Quaternary phosphonium compounds

Abstract

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.

IPC Classes  ?

• 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 46/00 - Preparation of quinones
• 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

Abstract

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.

IPC Classes  ?

• B01J 27/24 - Nitrogen compounds
• B01J 37/08 - Heat treatment
• C07C 46/00 - Preparation of quinones
• C07C 50/10 - Quinones the quinoid structure being part of a condensed ring system containing two rings

Abstract

A recombinant microorganism, a preparation method thereof and its application in the production of coenzyme Q10. Specifically, the present disclosure provides a method of exogenously introducing a gene encoding the global regulatory protein irrE to construct a recombinant microorganism. This recombinant microorganism is suitable for producing coenzyme Q10 by fermentation method, and is particularly suitable for producing oxidized coenzyme Q10. The recombinant microorganism of the present disclosure has stress resistance, and has good tolerance against harsh environments including high osmotic pressure and high redox potential, thus making it possible to significantly increase the yield of coenzyme Q10, especially the yield of oxidized coenzyme Q10.

IPC Classes  ?

• C12N 15/74 - Vectors or expression systems specially adapted for prokaryotic hosts other than E. coli, e.g. Lactobacillus, Micromonospora
• C07K 14/245 - Escherichia (G)
• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C12N 1/20 - BacteriaCulture media therefor

Abstract

The present invention relates to a method for preparing an oxazole compound. An additive represented by a formula (I) or (II) or (III) is added into an organic solvent and organic alkali (especially triethylamine), an organic solution of phosgene or diphosgene or triphosgene is dropwise added to perform a cyclization reaction with a compound (IV), and thus a product (V) at a high yield can be obtained and the generation of byproducts can be greatly inhibited. The reaction conditions in the present invention are mild, and compared with a method without addition of additives, the technical solution in the present invention can improve the yield of the product (V) to 95% or more and reduce the byproducts by 10% or more.

IPC Classes  ?

• C07D 263/42 - One oxygen atom attached in position 5

Abstract

The present invention relates to a catalyst for a phosgenation reaction and a phosgenation reaction method. The catalyst for a phosgenation reaction of the present invention is a phosphinyl ionic liquid as represented by general formula (I). In addition, the phosgenation reaction method provided by the present invention is a phosgenation reaction method using phosgene as a chlorination agent, and in the phosgenation reaction method, the catalyst for a phosgenation reaction as provided by the present invention is used. Compared with the use of the catalyst of triphenylphosphine oxide, etc., in a phosgenation reaction, the catalyst provided by the present invention can result in the charge rate of phosgene in a phosgenation reaction being reduced and the reaction time being shortened, thereby indicating a higher reaction efficiency and a higher atomic utilization of phosgene.

IPC Classes  ?

• B01J 31/24 - Phosphines
• C07C 17/00 - Preparation of halogenated hydrocarbons
• C07C 17/013 - Preparation of halogenated hydrocarbons by addition of halogens
• C07C 17/18 - Preparation of halogenated hydrocarbons by replacement by halogens of oxygen atoms of carbonyl groups
• C07C 21/04 - Chloro-alkenes
• C07C 22/00 - Cyclic compounds containing halogen atoms bound to an acyclic carbon atom
• C07C 22/04 - Cyclic compounds containing halogen atoms bound to an acyclic carbon atom having unsaturation in the rings containing six-membered aromatic rings
• C07C 51/60 - Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides into halides with the same carboxylic acid part
• C07H 1/00 - Processes for the preparation of sugar derivatives
• C07H 13/04 - Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
• C07B 39/00 - Halogenation
• C07C 53/38 - Acyl halides

Abstract

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.

IPC Classes  ?

• 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
• C07C 39/08 - Dihydroxy benzenesAlkylated derivatives thereof
• 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
• B01D 9/02 - Crystallisation from solutions
• B01D 19/00 - Degasification of liquids

Abstract

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.

IPC Classes  ?

• B01J 27/232 - Carbonates
• 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

Abstract

1/2. The present invention can efficiently extract two products, namely coenzyme Q10 and a phospholipid, from the coenzyme Q10 fermentation bacterium powder; the process thereof is highly operable, easy to be industrialized, and can provide a product with high purity and yield, having great economic benefit.

IPC Classes  ?

• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C07C 46/10 - SeparationPurificationStabilisationUse of additives

Abstract

Provided is a recombinant microorganism, a preparation method therefor and application thereof in producing coenzyme Q10. Specifically, provided is a method for creating the recombinant microorganism by exogenously introducing a gene coding a global regulation protein irrE. The recombinant microorganism is suitable for producing the coenzyme Q10 by a fermentation method, and is particularly suitable for producing oxidative coenzyme Q10.

IPC Classes  ?

• C12N 15/70 - Vectors or expression systems specially adapted for E. coli
• C12N 1/21 - BacteriaCulture media therefor modified by introduction of foreign genetic material
• C07K 14/195 - Peptides having more than 20 amino acidsGastrinsSomatostatinsMelanotropinsDerivatives thereof from bacteria
• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C12R 1/19 - Escherichia coli

Abstract

A fermentation production method for an oxidized coenzyme Q10 and a high-content oxidized coenzyme Q10 prepared therefrom, which are characterized in that the oxidation-reduction potential ORP of a fermentation broth is controlled to be -50-300 mV during the fermentation process of a production strain, the oxidation-reduction potential ORP of the fermentation broth preferably being controlled to be 50-200 mV. The method enables the content of the oxidized coenzyme Q10 in the coenzyme Q10 produced by microorganisms to reach more than 96%.

IPC Classes  ?

• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C07C 46/10 - SeparationPurificationStabilisationUse of additives
• C12R 1/01 - Bacteria or actinomycetales

Abstract

The present application relates to a method for extracting a coenzyme Q10 and phospholipids from a coenzyme Q10 fermentation bacterial powder. The method is characterized in that a mixed solvent having a three-dimensional Hansen solubility parameter between 21-23(J/cm3)1/2and a hydrogen bond contribution between 10-12(J/cm3)1/2 is used to extract a fermentation bacterial powder of a coenzyme Q10 producing strain. The present invention may efficiently extract the two products of a coenzyme Q10 and phospholipids from a coenzyme Q10 fermentation bacterial powder, the process having high operability, being easy for industrialized production, the product having high purity and a high yield, and the economic benefits being good.

IPC Classes  ?

• C07C 46/10 - SeparationPurificationStabilisationUse of additives
• C07C 50/28 - Quinones containing groups having oxygen atoms singly bound to carbon atoms with monocyclic quinoid structure
• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• A61K 31/685 - Diesters of a phosphorus acid with two hydroxy compounds, e.g. phosphatidylinositols one of the hydroxy compounds having nitrogen atoms, e.g. phosphatidylserine, lecithin

Abstract

The present application relates to a method for fermentative production of oxidized coenzyme Q10 and high-content oxidized coenzyme Q10 prepared therefrom. For the method for fermentative production of oxidized coenzyme Q10, in a fermentation process of a production strain, the oxidation-reduction potential (ORP) of a fermentation broth is controlled to be −50 to 300 Mv, and preferably the oxidation-reduction potential (ORP) of the fermentation broth is controlled to be 50 to 200 mV. By controlling the ORP of the fermentation broth, the method for fermentative production of oxidized coenzyme Q10 enables the oxidized coenzyme Q10 content in the coenzyme Q10 produced by microorganisms to reach 96% or more, and the product is substantially composed of a single component, which makes post-treatment more convenient. Oxidized coenzyme Q10 is more stable than reduced coenzyme Q10, and as compared with the coenzyme Q10 obtained by fermentative production in the prior art, high-content oxidized coenzyme Q10 degrades in a less amount in organisms. In addition, the fermentation method of the present application has a high potency.

IPC Classes  ?

• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure

Abstract

The present invention relates to an optimized fermentation process of coenzyme Q10, particularly to a fermentation process of coenzyme Q10 via flow feeding based on cooperative control of changes of online oxygen consumption rate and conductivity. During the fermentation process of coenzyme Q10 production strains, the oxygen consumption rate is controlled between 30-150 mmol/L·h and the conductivity is maintained between 3.0-30.0 ms/cm via flow feeding, so as to facilitate strain growth and the start of coenzyme Q10 synthesis and accumulation. The present invention can substantially increase output of coenzyme Q10 and greatly reduce the production cost with simple process control and strong operability, thus being applicable to large-scale industrial production.

IPC Classes  ?

• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C12Q 3/00 - Condition-responsive control processes
• C12N 1/20 - BacteriaCulture media therefor
• C12R 1/01 - Bacteria or actinomycetales

Abstract

Disclosed is a fed-batch coordinated-control coenzyme Q10 fermentation production process based on changes in the online oxygen consumption rate and in the online electrical conductivity. In the fermentation process of coenzyme Q10 production strains, the oxygen consumption rate is controlled to be 30-150mmol/L·h the electrical conductivity is maintained at 3.0-30.0ms/cm through fed-batch processing, so as to promote thallus growth and the start and accumulation of coenzyme Q10 synthesis. The method can greatly increase the output of coenzyme Q10 and considerably reduce production cost. The method has the advantages of simple process control and high operability, and is suitable for large-scale industrial production.

IPC Classes  ?

• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C12Q 3/00 - Condition-responsive control processes

Abstract

Disclosed is a fed-batch coordinated-control coenzyme Q10 fermentation production process based on changes in the online oxygen consumption rate and in the online electrical conductivity. In the fermentation process of coenzyme Q10 production strains, the oxygen consumption rate is controlled to be 30-150mmol/L·h the electrical conductivity is maintained at 3.0-30.0ms/cm through fed-batch processing, so as to promote thallus growth and the start and accumulation of coenzyme Q10 synthesis. The method can greatly increase the output of coenzyme Q10 and considerably reduce production cost. The method has the advantages of simple process control and high operability, and is suitable for large-scale industrial production.

IPC Classes  ?

• C12Q 3/00 - Condition-responsive control processes
• C12P 7/66 - Preparation of oxygen-containing organic compounds containing the quinoid structure
• C12R 1/01 - Bacteria or actinomycetales

Abstract

4, and whiteness is over 90, it can satisfy requirements for fiber polyphenylene sulfide resin. C5-C6 fatty acid salt according to the method of the present invention has a higher solubility in NMP, which can better promote polymerization. It is to be fully diverted into the filtrate after filter prior to conversion into free fatty acid again through acidification with hydrochloric acid. C5-C6 fatty acid is available for azeotropy with water, which has a limited solubility in water. Therefore, it is applicable to recycle C5-C6 fatty acid from the filtrate through azeotropy with water, and thereby solve the problem with separation of additive and sodium chloride that are soluble in water.

IPC Classes  ?

• C08G 75/16 - Polysulfides by polycondensation of organic compounds with inorganic polysulfides
• C08G 75/00 - Macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon
• C08G 75/02 - Polythioethers

Abstract

Disclosed is a method for synthesizing a fibre-grade polyphenylene sulphide resin, comprising synthesizing via a polycondensation reaction by using a sodium hydrosulphide solution and p-dichlorobenzene as raw materials, N-methyl-2-pyrrolidone as a solvent, and a C5-C6 fatty acid salt formed by dehydration of a C5-C6 fatty acid and sodium hydroxide as an auxiliary for the polycondensation reaction. The reaction liquid is subjected to acidification and washing to obtain a white polyphenylene sulphide resin, the melt flow rate of the product is less than 125 g/10 min, the weight-average molecular weight measured by GPC is greater than 4.2 × 104, and the whiteness is higher than 90, meeting the requirements of the fibre-grade polyphenylene sulphide resin. In the method of the present invention, the C5-C6 fatty acid salt used has good solubility in NMP and can better promote the polycondensation reaction, all of it enters a filtrate after reaction and filtration, and it is again converted into a free fatty acid through acidification with hydrochloric acid; and the C5-C6 fatty acid can co-boil with water, has low solubility in water, and can be recovered from the filtrate by the method of co-boiling with water, thereby avoiding the problem that both the auxiliary and sodium chloride are dissolved in water and cannot be separated and recovered.

IPC Classes  ?

• C08G 75/02 - Polythioethers