77 results about "Methylthiobutyric acid" patented technology

The invention discloses a synthesis method of medicinal calcium D,L-2-hydroxyl-4-(methylthio)butyrate. By adopting the existing methods, the product has more impurities and poor quality; and some methods have harsh conditions and low product yield and are not suitable for industrial production. The synthesis method comprises the following steps: using feed grade D,L-2-hydroxyl-4-methylthiobutyricacid of which the content is less than 90% or D,L-2-hydroxyl-4-methylthiobutyric acid of which the content is 75-90% as a starting raw material to react with ammonia and generate an ammonium salt, performing dehydration to obtain D,L-2-hydroxyl-4-methylthiobutyramide, extracting, concentrating, crystallizing and purifying to obtain D,L-2-hydroxyl-4-methylthiobutyramide of which the content is more than 98.5%; and hydrolyzing to generate D,L-2-hydroxyl-4-methylthiobutyrate, and performing the salt forming reaction with CaX2 to generate calcium D,L-2-hydroxyl-4-(methylthio)butyrate. The synthesis method in the invention has mild process conditions, less side reactions and high yield.

The invention discloses a method for preparing a D, L-2-hydroxyl-4-methylthio butanoic calcium salt for medicinal purpose. The method comprises following steps of: a. using a D,L-2-hydroxyl-4-methylthio butanoic acid and an alcohol with a general formula of ROH as the raw materials to carry out esterification to obtain a D, L-2-hydroxyl-4-methylthio butyrate, and; b. hydrolyzing the D, L-2-hydroxyl-4-methylthio butyrate in step a and calcium oxide in a solvent to produce the D, L-2-hydroxyl-4-methylthio butanoic calcium salt. The method provided by the invention for the production of the D, L-2-hydroxyl-4-methylthio butanoic calcium salt has the advantages of short course, readily available the raw materials, low cost, easy control over the quality of the product, and more importantly, the method can prepare high-purity D, L-2-hydroxyl-4-methylthio butanoic calcium salt for medicinal purpose, thereby satisfying the requirements of State Food and Drug Administration Bureau and Good Manufacturing Practice (GMP) for drug production, and facilitating the preparation of pharmaceutical preparations.

The invention provides a preparation method of hydroxy methionine salt and a compound, comprising the following steps: a. feeding metal hydroxide or basic metal oxide or amphoteric metal oxide and 2-hydroxy-4-methylthiobutyricacid into a closed and corrosion resistant reaction kettle to react for 0.5-12h according to a stoichiometric ratio, taking the low-boiling polar organic solvent or the mixed solvent thereof with water as the reaction medium, stirring, separating the target product, washing and drying to obtain the products; and b. recycling the reaction medium. The preparation method of the invention has short route, no consumption of acid or alkali reagent, low cost, easily-controllable product quality, environmental friendliness and the like, thus being applicable to large-scale industrial production.

The invention relates to a preparation method of high-content 2-hydroxy-4-(methylthio) butyl calcium. The content of 2-hydroxy-4-(methylthio) butyl calcium prepared by the traditional synthesis method is lower. The preparation method provided by the invention comprises the following steps of: adding 2-hydroxy-4-methionine nitrile with content higher than 99.0% used as a raw material in concentrated HCl (hydrochloric acid) for carrying out hydrolysis reaction; after the reaction is finished, regulating pH with alkali till pH is between 7.8-8.0, cooling, crystallizing and filtering to obtain a 2-hydroxy-4-(methylthio) butyric amide crude product; recrystallizing with water to obtain high-content 2-hydroxy-4-(methylthio) butyric amide; and dissolving the high-content 2-hydroxy-4-(methylthio) butyric amide in water, adding excess Ca(OH)2 and directly hydrolyzing at 80-100 DEG C to generate 2-hydroxy-4-(methylthio) butyl calcium. The yield of the preparation method is very high, and the content of the prepared 2-hydroxy-4-(methylthio) butyl calcium is higher than 99.0%.

A storage stable mixture containing 86 to 97% by weight of 2-hydroxy-4-methylthiobutyronitrile, 2 to 14% by weight of water, 0.05 to 0.5% by weight of HCN and having a pH of 1 to 4, measured using a pH electrode at 23° C. is provided. A method to produce the storage stable mixture and its use in manufacture of DL-methionine or 2-hydroxy-4-methylthiobutyric acid is also provided.

The invention discloses a method for preparing 2-amino-4-methylthio butyric acid by using recombinant nitrilase, which comprises the following steps: performing water bath shaker reaction (25-40 DEG C, 150-200rpm) on an enzyme source and a substrate in a reaction system of a buffer solution with a pH value of 7.0-9.0, wherein the enzyme source is a wet bacterium obtained through the induced culture of a recombinant engineering bacterium containing nitrilase, and the substrate is 2-amino-4-methylthio butyronitrile; and after the reaction is finished, performing post treatment on the reaction liquid to obtain 2-amino-4-methylthio butyric acid. According to the invention, the gene engineering bacterium is used for experiment of methionine production through biological catalysis and can biologically catalyze methionine production effectively, and the 2-amino-4-methylthio butyronitrile conversion rate within 2 hours is up to 80-100%. Thus, the bacterium has wide application prospects in the field of methionine production through biological catalysis.

The invention discloses a preparation method of MHA (2-hydroxy-4-(methylthio) butyric acid). According to the preparation method, nitrile generated by a reaction of a hydrocyanic acid aqueous solution and (methylthio) propionaldehyde is subjected to acidolysis and then treated to obtain an organic phase containing MHA and an aqueous phase containing ammonium salt, the organic phase is subjected to concentrating under reduced pressure and organic solvent treatment or is subjected to direct centrifugal treatment to remove ammonium salt, and MHA is obtained; and the ammonium salt can be further purified to obtain high-purity ammonium salt by-product, and brine waste is not generated. During the preparation process, the used organic solvent can be recycled for application, the used hydrocyanic acid aqueous solution has no tail gas incineration, hydrocyanic acid rectification is not required, and the energy consumption is low; and the organic phase and the aqueous phase are treated separately, compared with direct water removal without phase-splitting, the influence of the ammonium salt on water distillation is reduced, the condition that mass transfer and heat transfer during water distillation are affected by a great amount of ammonium salt is avoided, so that the water distillation quantity is reduced greatly while energy consumption is reduced, and steam is saved.

The invention belongs to the field of the chemical industry, and relates to a preparation method of large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate. The preparation method of the large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate comprises the following steps that 2-hydroxy-4-(methylthio)butyric acid, a calcium compound and a crystallizing agent are arranged in an aqueous medium, the pH is adjusted to be 5-7, the temperature is 60-80DEG C, stirring and full reactions are carried out, cooling crystallization is carried out to obtain calcium 2-hydroxy-4-(methylthio)butyrate crystals, separation is carried out to obtain crystals and coarse product mother liquid, and the crystals serve as calcium 2-hydroxy-4-(methylthio)butyrate coarse products. The calcium compound is one or more of calcium salt, calcium oxide and calcium hydroxide, and the use amount of the crystallizing agent is 50ppm-3000ppm of the mass of the 2-hydroxy-4-(methylthio)butyric acid. Materials produced through the preparation method of the large-particle crystal type high-bulk-density calcium 2-hydroxy-4-(methylthio)butyrate are high in purity, dehydration is easy, drying is rapid, crystal particles obtained after drying are large, good in mobility and large in bulk density, the amount of dust is low, glossiness is high, and the materials are more applicable to fodder.

The invention is directed at the field of chemical engineering and provides a preparation method for calcium D,L-2-hydroxy-4-methylthiobutyrate. The preparation method comprises the following steps: preparing a hydrocyanic acid gas mixture by using an Andrussow process; preparing a 2-hydroxy-4-methylthiobutyronityile system with the hydrocyanic acid gas mixture and methylthiopropionaldehyde as starting raw materials; hydrolyzing the 2-hydroxy-4-methylthiobutyronityile system with inorganic base so as to obtain D,L-2-hydroxy-4-methylthiobutyrate; and chelating D,L-2-hydroxy-4-methylthiobutyrate with a soluble calcium salt so as to produce calcium D,L-2-hydroxy-4-methylthiobutyrate. The method has the advantages of a few processing step, cheap and easily available raw materials, stable intermediate properties and low total production cost. Prepared calcium D,L-2-hydroxy-4-methylthiobutyrate has the advantages of high yield, high purity, a powder crystal form and great bulk density, can be used as an animal feed additive for effective mixing with a feed so as to supplement trace elements and amino acid in daily ration and improve production performance and immune performance of animals and can also be used as a medicine reagent.

The invention discloses an efficient nutrient supplementation feed for dairy cattle, belongs to the field of feed additives, and in particular relates to a feed additive product for the dairy cattle. The efficient nutrient supplementation feed for the dairy cattle is prepared by adopting the following steps of: crushing calcium carbonate components in a slow release preparation, and mixing the crushed components with alpha-hydroxyl-4-methylthiobutyric acid evenly; mixing the mixture with other components in the slow release preparation evenly; crushing urea, soybean peptide powder, schizophyllum commune and lucid ganoderma to obtain materials with length or grain diameter of being less than 3 mm; mixing the preprocessed mixture with the crushed urea, soybean peptide powder, schizophyllum commune and lucid ganoderma; extruding the mixture by using a feed extruding unit; and mixing the extruded materials with extruded soybean. According to the efficient nutrient supplementation feed for the dairy cattle in the invention, the added edible-medical edible mushroom components not only have nutrient substances such as proteins, polysaccharide and the like, but also have a good lactation promotion effect; and the milk yield of the dairy cattle is effectively increased after the dairy cattle eat the efficient nutrient supplementation feed for the dairy cattle.

The invention relates to a preparation method of a 2-hydroxy-4-methylthio butyric acid metal chelate. The method comprises the following steps: performing a full reaction on hydrocyanic acid mixed gas prepared from an Andrussow method and methylthio propionaldehyde under the catalytic action of an alkali so as to obtain a 2-hydroxy-4-methylthio butyronitrile reaction system; performing a hydrolytic action on the 2-hydroxy-4-methylthio butyronitrile reaction system and sulfuric acid so as to obtain 2-hydroxy-4-methylthio butyric acid; adding an aqueous medium, a metallic compound and a crystallizing agent into the 2-hydroxy-4-methylthio butyric acid; regulating a pH value to reach 5 to 7 by using the alkali; heating to reach 60 DEG C to 90 DEG C; and performing cooling crystallization, thereby obtaining a 2-hydroxy-4-methylthio butyric acid metal chelate crystal. The method is low in production cost, wherein the obtained 2-hydroxy-4-methylthio butyric acid is easy to separate and purify, so that the 2-hydroxy-4-methylthio butyric acid with the high purity and the high yield can be obtained. Thus, the 2-hydroxy-4-methylthio butyric acid metal chelate which is further prepared from the 2-hydroxy-4-methylthio butyric acid has large crystalline particles.

The invention provides a method for clean continuous preparation of 2-hydroxy-4-methylthiobutyric acid. The method comprises preparation of hydrocyanic acid and preparation of 2-hydroxy-4-methylthiobutanoic acid. The method is characterized in that an ammonium phosphate aqueous solution produced by preparation of hydrocyanic acid and preparation of 2-hydroxy-4-methylthiobutanoic acid is treated inan ammonia separation tower and an ammonia purification tower and phosphoric acid and ammonia gas are separated and covered. The ammonia and phosphoric acid can be recycled repeatedly. The method simplifies acid-containing substance emission and treatment. The method has a unique technological process comprising pyrolysis separation of an ammonium phosphate aqueous solution after extraction, recycling of a phosphoric acid aqueous solution in hydrolysis of 2-hydroxy-4-(methylthio)butyronitrile and recycling of ammonium as a hydrocyanic acid preparation raw material. The method is environmentally friendly, reduces an environmental protection cost by 11.5%, has a high atom utilization rate, reduces a production cost by 21.8%, does not produce an ammonium salt by-product and reduces the pressure of sales and environmental protection.

The invention relates to a preparation method of an alkyl butyrate, and particularly discloses a preparation method of a 2-hydroxy-4-methylthioalkyl butyrate, which comprises the following steps: under the catalytic action of phosphoric acid, reacting 2-hydroxyl-4-methylthiobutyric acid and an alcohol, which are used as reaction materials, in an esterification mode; and separating and purifying the reaction products to obtain the 2-hydroxy-4-methylthioalkyl butyrate. The method disclosed by the invention has the advantages of low cost, simple technological process, high yield, high product purity and the like.

The invention aims at the chemical industry field, and relates to a preparation method of calcium D,L-2-hydroxy-4-methylthiobutyrate having a high purity and a high bulk density. The method comprises the following steps: fully reacting a hydrocyanic acid mixed gas prepared through an Andrussow method with methylthiopropionaldehyde under the catalysis of an alkali to obtain a 2-hydroxy-4-methylthiobutyronityile system; hydrating the 2-hydroxy-4-methylthiobutyronityile system in the presence of an inorganic acid to obtain D,L-2-hydroxy-4-methylthiobutyramide; and chelating D,L-2-hydroxy-4-methylthiobutyramide with calcium oxide or calcium hydroxide to prepare calcium D,L-2-hydroxy-4-methylthiobutyrate. The method has the advantages of simple synthesis technology and easily available raw materials, the above obtained product has a large bulk density, a high purity and a good fluency, can be effectively mixed with feeds as an animal feed additive to supplement the calcium element and amino acids in the daily ration and improve the endozoic production and immunity performances, and can also be used as a medicinal reagent.

The invention belongs to the technical field of preparation of feed additives and particularly relates to a preparation method of calcium bis(2-hydroxy-4-(methylthio)butyrate). The preparation methodcomprises the following steps: a calcium compound is uniformly mixed with a dispersant under stirring, the mixture is mixed with bis(2-hydroxy-4-(methylthio)butyrate) for a reaction, a product is dried, and the final product calcium bis(2-hydroxy-4-(methylthio)butyrate) is obtained. The method adopts a few process steps, reaction conditions are mild, the reaction is fast, and the total productioncost is low; the yield of prepared calcium bis(2-hydroxy-4-(methylthio)butyrate) is as high as 96% or higher, the product is loose and good in dispersity, and the problems of low yield and purity of calcium bis(2-hydroxy-4-(methylthio)butyrate), sticky and greasy filter cake, difficult suction filtration, poor smoothness and the like in actual production process are solved; According to the preparation method of calcium bis(2-hydroxy-4-(methylthio)butyrate), the formula is scientific and reasonable, the cost is low, and the preparation process is simple, fast and convenient and has quite greateconomic significance and social significance in industrial preparation of calcium bis(2-hydroxy-4-(methylthio)butyrate).

The invention relates to the technical field of animal feeds, particularly an organic microelement premixed feed for Wuzhishan weaned piglets and a preparation method of the organic microelement premixed feed. The organic microelement premixed feed for Wuzhishan weaned piglets provided by the invention comprises a carrier, a premixing agent and organic microelements, wherein the carrier is one or a mixture of more of rice hull powder, corn flour and mountain flour; the organic microelement comprise 2-hydroxy-4-chelating zinc methylthio butyrate, 2-hydroxy-4-chelating manganese methylthio butyrate, 2-hydroxy-4-chelating copper methylthio butyrate, glycine chelating ferrum and selenium yeast; the premixing agent comprises sodium selenite and calcium iodate. The organic microelement premixed feed for Wuzhishan weaned piglets provided by the invention is suitable for being used in the stage of Wuzhishan weaned piglets and can be used for improving the piglet production performance and obtaining feed conversion; the diarrhea rate of the piglets is reduced by about 33.8%; the discharge of feces copper is reduced by 88.0%; the feed is low in dosage and high in efficiency, the organic copper additive amount in the feed is remarkably reduced, and the ecological environment is protected.

The invention belongs to the field of chemical industry, relates to preparation of D,L-2-hydroxy-4-methylthio butyric ester chemical products, and in particular relates to a preparation method of D,L-2-hydroxy-4-methylthio butyric ester based on silicone sulfonic acid as a catalyst. The method comprises the following step: performing an esterification reaction on D,L-2-hydroxy-4-methylthio butyric acid and an alcohol which are taken as raw materials so as to obtain the D,L-2-hydroxy-4-methylthio butyric ester, wherein the silicone sulfonic acid is taken as the catalyst and the alcohol contains 1 to 12 carbon atoms during the esterification reaction. The silicone sulfonic acid taken as the catalyst is simple to synthesize; and the raw material of the silicone sulfonic acid is cheap and easily-available and high in catalytic activity. The catalyst can be repeatedly recycled in a simple filtration mode, so that the production cost is saved; the corrosion of equipment, caused by sulfuric acid, phosphoric acid and the like, is avoided. The process is high in yield, wherein the conversion rate can reach 95% or more; the subsequent treatment is simple after the reaction is finished; the atom economy of the whole reaction is high, namely, other wastes except water are not generated.

The invention relates to a preparation method of 2-hydroxy-4-methylmercapto butyric acid iron. The specific method is as follows: (1) salifying: pouring 2-hydroxy-4-methylmercapto butyric acid, ferrous sulfate, anti-oxidant, water and sodium hydroxide into a reaction kettle, stirring and heating to 70-80 DEG C to react for 6 to 8h to obtain a crude product solution; and (2) drying: carrying out centrifugal separation on the crude product solution obtained in step (1), putting the granular product obtained from separation in an upper-and-lower ventilate drying sieve and then placing in a drying oven to dry, sieving the obtained crude product to obtain the finished product of 2-hydroxy-4-methylmercapto butyric acid iron. In the production process, the preparation method utilizes the anti-oxidant to ensure the obtained product to be stable, is good for drying, and has the characteristics of simple realization and convenient operation, thus saving the investment on production equipment and improving the production efficiency.

The invention relates to a method for preparing 2-hydroxy-4-methylmercapto copper butyrate, which comprises the following specific steps of: (1) salifying, namely putting 2-hydroxy-4-methylmercapto butyric acid, an initiator and water into a reaction kettle, heating to the temperature of between 70 and 80 DEG C with stirring, adding basic copper carbonate in batches, and reacting under stirring until carbon dioxide bubbles do not overflow to obtain solution of 2-hydroxy-4-methylmercapto copper butyrate; and (2) drying, namely performing centrifugal separation on the product obtained in the step (1), putting the granular product obtained by separation into an up-down ventilated drying sieve, putting the sieve into a dying box to dry for 22 to 26 hours to obtain a crude product, and sieving the crude product to obtain the finished product of the 2-hydroxy-4-methylmercapto copper butyrate. The innovative basic copper carbonate and the initiator are used as raw materials in the production process, so the preparation method has the advantages of convenient operation and easy implementation; and the obtained granular product is more favorable for drying without being crushed, so production equipment investment can be reduced and the production efficiency and economic benefit can be improved.

The invention aims at the chemical industry field, and relates to a preparation method of D,L-2-hydroxy-4-methylthiobutyrate. The method comprises the following steps: fully reacting a hydrocyanic acid gas mixture prepared through an Andrussow method with methylthiopropionaldehyde under the catalysis of an alkali to obtain a 2-hydroxy-4-methylthiobutyronityile reaction system; and mixing the 2-hydroxy-4-methylthiobutyronityile reaction system with alcohol, and carrying out hydrolysis and esterification reactions under the catalysis of an inorganic acid to prepare the D,L-2-hydroxy-4-methylthiobutyrate. Initial raw materials which are not rectified or purified, and are cheap and easily available, an intermediate obtained through a reaction has stable properties, few reaction steps are realized, and a finally obtained product is simply separated and purified to obtain high-purity and high-yield D,L-2-hydroxy-4-methylthiobutyrate.

The invention relates to a method for preparing a solid 2-hydroxy-4-(methylthio) butanoic acid, which comprises the following steps of: a. utizling a methionine hydroxy solution to prepare methionine hydroxy calcium or hydroxy methionine barium; b. mixing the methionine hydroxy calcium or hydroxy methionine barium obtained in a step a with concentrated sulfuric acid according to a stoichiometric ratio, adding a reaction medium B, reacting for 0.5-6h at a temperature of between room temperature and 50 DEG C, stirring and carrying out solid-liquid separation to obtain a methionine hydroxy solution; and c. distilling the methionine hydroxy solution obtained in a step b in a reduced pressure to remove an organic solvent, and after drying the resulting solid, obtaining the solid 2-hydroxy-4-(methylthio) butanoic acid. Compared with the traditional molecular distillation method, the method provided by the invention has the advantages of simple operation, no needs for a short range evaporator or thin film evaporator, and low cost.