CN-122010790-A - Vitamin K improving agent3Method for synthesizing yield

Abstract

The invention discloses a method for improving the synthesis yield of vitamin K 3 , which comprises the following steps of S1, taking beta-menaquinone and sodium metabisulfite in a container, adding ethanol as a solvent, stirring and reacting for 1-2 hours, heating to 40-70 ℃ and preserving heat for 10-60min, filtering while the reaction is finished, obtaining filtrate, S2, adding sodium metabisulfite into the filtrate, and then freezing, crystallizing, filtering, washing and drying to obtain a vitamin K 3 finished product. When the vitamin K 3 is prepared by cooling and crystallizing, the crystallization yield of the vitamin K 3 can be effectively improved by adding the sodium metabisulfite into the filtrate to be crystallized.

Inventors

• Xu Ningyan
• Fan Chaoyun
• GAO LIN
• GAO BO
• Li Chongjia
• JIANG YAN
• SHAO QIFENG
• XU SHUGUANG

Assignees

• 云南省陆良和平科技有限公司

Dates

Publication Date

20260512

Application Date

20260120

Claims (4)

1. 1. A method for improving the synthesis yield of vitamin K 3 is characterized by comprising the following steps: s1, taking beta-menadione and sodium metabisulfite, putting the beta-menadione and the sodium metabisulfite into a container, adding a solvent, stirring and reacting for 1-2 hours, heating to the temperature of 30-50 ℃, preserving heat for 10-60min at the temperature of 40-70 ℃, and filtering while the reaction is hot after the reaction is finished to obtain filtrate; s2, adding sodium metabisulfite into the filtrate, and then freezing, crystallizing, filtering, washing and drying to obtain the vitamin K 3 finished product.
2. 2. The method for improving the synthesis yield of vitamin K 3 according to claim 1, wherein the solvent is an 80% ethanol solution.
3. 3. The method for improving the synthesis yield of vitamin K 3 according to claim 2, wherein in the step S1, the mass ratio of beta-menaquinone, sodium metabisulfite and ethanol is 1:0.8-1.2:4-6.
4. 4. The method for improving the synthesis yield of vitamin K 3 according to claim 1, wherein the sodium metabisulfite is added in an amount of 100-1100g per 1L of filtrate in the step S2.

Description

Method for improving synthesis yield of vitamin K 3 Technical Field The invention belongs to the technical field of chemical industry, and particularly relates to a method for improving the synthesis yield of vitamin K 3. Background Vitamin K 3 (also called as sodium bisulphite menaquinone) is a quinone substance, is an important intermediate for synthesizing K-series vitamins, is used as a procoagulant, has a strong blood coagulation effect, acts on liver to synthesize prothrombin and promote liver to synthesize blood coagulation factors, is one of classical hemostatic, can be effectively used for treating tumors by combining with a certain amount of vitamin C clinically, and is an important component of feed additives in animal husbandry. The substance exists in a small amount in green plants in nature, cannot meet the practical production and application, and the currently used vitamin K 3 is obtained by artificial synthesis. The synthetic vitamin K 3 is prepared by taking beta-methylnaphthalene as a raw material, obtaining beta-menaquinone through oxidation reaction, taking beta-menaquinone as a raw material, and carrying out addition reaction. Currently, the method for improving the synthesis yield of vitamin K 3 is mainly used for optimizing the oxidation reaction of the beta-menaquinone synthesized in the first step, changing a reaction solvent (acetic acid, nitrile methyl, acetonitrile and the like), changing an oxidant of the oxidation reaction, replacing chromium salt oxidation by H 2O2 oxidation, using ammonium persulfate as an initiator to participate in the reaction, using a metal and metal molecular sieve catalyst and other methods to improve the oxidation reaction yield, so as to improve the yield of finally produced vitamin K 3, and mainly used for improving the yield in the second step of addition reaction by optimizing the reaction time, the reaction temperature and the raw material proportion. Because the synthesized vitamin K 3 is sensitive to temperature and solvent, in the actual workshop production, if the reaction yield is improved by changing the process conditions (temperature, time, solvent, catalyst, reaction auxiliary agent and the like), continuously reducing the concentration of a reaction product or increasing the concentration of a reactant, the problems that the existing equipment of the workshop cannot meet and increase the production cost, and environmental pollution is caused and the like possibly occur, the method for improving the reaction yield is the current research direction, and the original reaction process (without increasing or decreasing the equipment) is not influenced, the production cost is saved. Disclosure of Invention In order to overcome the problems in the prior art, the invention provides a method for improving the synthesis yield of vitamin K 3. In order to achieve the above purpose, the invention is realized by the following technical scheme: A method for improving the synthesis yield of vitamin K 3, which comprises the following steps: s1, taking beta-menadione and sodium metabisulfite, putting the beta-menadione and the sodium metabisulfite into a container, adding a solvent, stirring and reacting for 1-2 hours, heating to the temperature of 30-50 ℃, preserving heat for 10-60min at the temperature of 40-70 ℃, and filtering while the reaction is hot after the reaction is finished to obtain filtrate; s2, adding sodium metabisulfite into the filtrate, and then freezing, crystallizing, filtering, washing and drying to obtain the vitamin K 3 finished product. Further, the solvent is an ethanol solution with the concentration of 80 percent. Further, in the step S1, the mass ratio of the beta-menaquinone to the sodium metabisulfite to the ethanol is 1:0.8-1.2:4-6. Further, the addition amount of the sodium metabisulfite in the step S2 is 100-1100g per 1L of filtrate. Through the technical scheme, the method has the beneficial effect that when the vitamin K 3 is prepared, the crystallization yield of the vitamin K 3 can be effectively improved by adding sodium metabisulfite into filtrate to be crystallized. Detailed Description Materials and reagents used in the present invention are commercially available unless otherwise indicated. Example 1 Preparation of vitamin K 3 (menaquinone sodium bisulfite): And (3) adding the beta-menaquinone and sodium metabisulfite into a container, adding an ethanol solution with the concentration of 80% as a solvent, stirring and reacting for 1.5 hours, wherein the reaction temperature is 40 ℃, heating to 55 ℃, preserving heat for 35min, and filtering while the reaction is hot after the reaction is finished to obtain a filtrate, wherein the mass ratio of the beta-menaquinone to the sodium metabisulfite to the ethanol is 1:1:5. S2, adding sodium metabisulfite into the filtrate, and then freezing, crystallizing, filtering, washing and drying to obtain a vitamin K 3 (sodium metabisulfite menaquinone) finished product, wherein