阅读说明：本技术 一种以半乳糖酸钙为原料制备苏糖酸钙的方法 (Method for preparing calcium threonate by using half calcium lactobionate as raw material ) 是由 陈红辉 于 2020-07-02 设计创作，主要内容包括：本发明公开了一种以半乳糖酸钙为原料制备苏糖酸钙的方法,包括如下步骤：S1：降解；将适量的半乳糖酸钙、六水合氯化钴、水依次加入到反应器皿中,加入2mol/L的碳酸氢钠将溶液pH调节至6.5,搅拌反应1-3小时后停止反应,得粗苏糖溶液。溶液通过电渗析回收氯化钴；S2：氧化；将200mL25％苏糖溶液倒入反应器皿中,用恒温加热装置控制反应体系温度在50℃,用20w紫外灯对其照射,搅拌反应体系并导入氧气,滴加30％过氧化氢；S3：脱色；S4：结晶；浓缩滤液,加入15-30mL甲醇溶解,降温至0-10℃,静置,过滤,烘干得苏糖酸钙成品；本工艺不但大大减少了废固的产生,减轻了后处理的压力,而且使得反应更高效。实验过程中用到的原料可回收、降低了生产成本。(The invention discloses a method for preparing calcium threonate by taking calcium hemilactobionate as a raw material, which comprises the following steps: s1: degrading; and (3) sequentially adding a proper amount of calcium hemilactobionate, cobalt chloride hexahydrate and water into a reaction vessel, adding 2mol/L sodium bicarbonate to adjust the pH of the solution to 6.5, stirring and reacting for 1-3 hours, and stopping the reaction to obtain a crude threose solution. Recovering cobalt chloride from the solution by electrodialysis; s2: oxidizing; pouring 200mL of 25% threose solution into a reaction vessel, controlling the temperature of a reaction system at 50 ℃ by using a constant-temperature heating device, irradiating the reaction system by using a 20w ultraviolet lamp, stirring the reaction system, introducing oxygen, and dropwise adding 30% hydrogen peroxide; s3: decoloring; s4: crystallizing; concentrating the filtrate, adding 15-30mL of methanol for dissolving, cooling to 0-10 ℃, standing, filtering, and drying to obtain a finished product of calcium threonate; the process not only greatly reduces the generation of waste solids and lightens the pressure of post-treatment, but also ensures that the reaction is more efficient. The raw materials used in the experimental process can be recovered, and the production cost is reduced.)

1. A method for preparing calcium threonate by taking calcium hemilactobionate as a raw material is characterized by comprising the following steps: the method comprises the following steps:

s1: degrading; and (2) sequentially adding a proper amount of calcium hemilactobionate, cobalt chloride hexahydrate and water into a reaction vessel, stirring and heating to 35 ℃, adding 2mol/L sodium bicarbonate to adjust the pH of the solution to 6.5, controlling the temperature to be 35-40 ℃ in the reaction process, stirring and reacting for 1-3 hours, and stopping the reaction to obtain the crude threose solution. Recovering cobalt chloride from the solution by electrodialysis;

s2: oxidizing; pouring 200mL of 25% threose solution into a reaction vessel, controlling the temperature of a reaction system at 50 ℃ by using a constant-temperature heating device, and irradiating the reaction system by using a 20w ultraviolet lamp; stirring the reaction system, introducing oxygen, dropwise adding 30% hydrogen peroxide, dropwise adding 10% -30% calcium hydroxide suspension solution in the reaction process to control the pH of the reaction system to be 8.5-10.2, stirring for 4-6h, and stopping reaction;

s3: decoloring; adding 10-20g of active carbon into a reaction system, stirring for 1-2h for decolorization, and filtering;

s4: crystallizing; concentrating the filtrate, adding 15-30mL of methanol for dissolving, cooling to 0-10 ℃, standing, filtering, and drying to obtain the finished product of calcium threonate.

2. The method for preparing calcium threonate from calcium hemilactobionate as claimed in claim 1, wherein the method comprises the following steps: the molar ratio of lactose to hydrogen peroxide in step S2 was 1: 3.

Technical Field

The invention relates to the technical field of preparation of calcium threonate, in particular to a method for preparing calcium threonate by taking calcium hemilactobionate as a raw material.

Background

VC hydrogen peroxide is used for oxidation in the traditional preparation process of calcium threonate, a large amount of calcium carbonate needs to be added, and finally generated waste residues are 1.5 times of finished products, so that the preparation process is not environment-friendly and is not beneficial to industrialization.

Disclosure of Invention

The invention aims to provide a method for preparing calcium threonate by taking calcium hemilactobionate as a raw material, which is used for solving the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme:

a method for preparing calcium threonate by using half calcium lactobionate as a raw material comprises the following steps:

s1: degrading; and (2) sequentially adding a proper amount of calcium hemilactobionate, cobalt chloride hexahydrate and water into a reaction vessel, stirring and heating to 35 ℃, adding 2mol/L sodium bicarbonate to adjust the pH of the solution to 6.5, controlling the temperature to be 35-40 ℃ in the reaction process, stirring and reacting for 1-3 hours, and stopping the reaction to obtain the crude threose solution.

Recovering cobalt chloride from the solution by electrodialysis;

s2: oxidizing; pouring 200mL of 25% threose solution into a reaction vessel, controlling the temperature of a reaction system at 50 ℃ by using a constant-temperature heating device, and irradiating the reaction system by using a 20w ultraviolet lamp; stirring the reaction system, introducing oxygen, dropwise adding 30% hydrogen peroxide, dropwise adding 10% -30% calcium hydroxide suspension solution in the reaction process to control the pH of the reaction system to be 8.5-10.2, stirring for 4-6h, and stopping reaction;

s3: decoloring; adding 10-20g of active carbon into a reaction system, stirring for 1-2h for decolorization, and filtering;

s4: crystallizing; concentrating the filtrate, adding 15-30mL of methanol for dissolving, cooling to 0-10 ℃, standing, filtering, and drying to obtain the finished product of calcium threonate.

Preferably, the molar ratio of lactose to hydrogen peroxide in step S2 is 1: 3.

Compared with the prior art, the invention has the beneficial effects that:

the invention provides a method for preparing calcium threonate by taking calcium hemilactobionate as a raw material, which not only greatly reduces the generation of waste solids and lightens the pressure of aftertreatment, but also ensures that the reaction is more efficient. The raw materials used in the experimental process can be recovered, and the production cost is reduced.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.