Synthetic method of beet alkali and beet alkali hydrochlorate

Abstract

The invention provides a synthesis method of betaine and betaine hydrochloride salt, comprising the steps as follows: strong alkali negative ion resin is selected as a carrier and is treated into a hydroxide radical type; elution is carried out by using a chloroactic acid solution; cycle elution is carried out using a trimethylamine solution; scrubbing is carried out by using distilled water, and cleaning solution is combined with cycle eluent, then vacuum distillation is carried out so as to achieve vicidity, and the vacuum distillation is continued until powder or small flake white betaine with water is obtained; the betaine with water is dissolved using absolute ethyl alcohol and is carried out vacuum distillation to obtain betaine anhydrous, with yield of more than 93 percent and purity of more than 98.5 percent; the sticky matter after the vacuum distillation is added with hydrochloric acid and stirred then subjected to the vacuum distillation so as to obtain the powder or small flake white betaine hydrochloride salt, with yield of more than 94 percent and purity of more than 98 percent. The method of the invention has advantages of simple and convenient technique, low production cost, moderate operation condition and environmental-friendliness; the products of the invention are applicable to the application in such fields as feedstuff, food, cosmetics, medicine, biological agent, and chemical industry, etc.

Description

technical field [0001] The invention relates to a quaternary ammonium alkaloid, in particular to a method for synthesizing betaine and betaine hydrochloride. Background technique [0002] Betaine, namely Betaine, chemical name: N, N, N-trimethylglycine inner salt, structural formula: (CH 3 ) 3 N + CH 2 COO - , is a quaternary ammonium alkaloid, which is widely found in animals and plants, and is named for it mainly exists in the molasses of beet sugar. Betaine is a quaternary amphoteric amphoteric compound, so betaine is often used as a surfactant and a leveling agent for vat dyeing. It can be used as a cleaning agent component in the cosmetics industry and is widely used in chemical, pharmaceutical and other industries; because betaine There are three active methyl groups connected to the nitrogen atom of the nitrogen atom, which has a unique physiological activity of the methyl donor. It can replace methionine and choline chloride. feed conversion efficiency. [000...

AI Technical Summary

Problems solved by technology

Because betaine sugar mother liquor is easily restricted by region and season, and the separation and purification process is complex and costly, it is far from meeting the market demand for betaine; chemical synthesis is another and currently the most important betaine production route

Chemical method synthesis technique mainly comprises: the one, produce betaine with the oxidation process of ethoxylated quaternary ammonium compound, C. Blaufeld etc. have expressed a kind of utilization choline chloride as Raw materials, in an alkaline system, the technology of producing betaine by oxidation of oxygen-containing gas under the catalytic conditions of a platinum-containing catalyst, US 5,895,823 discloses a method for preparing a betaine aqueous solution by loading a precious metal catalyst to catalyze choline salt, etc., because the method uses expensive precious metals Catalytically active components, there are problems such as recycling and loss of precious metals, which greatly limit its application and promotion; another important synthetic route is to use chloroacetic acid and trimethylamine as raw materials, and alkali neutralize the chloroacetic acid solution to generate ethyl chloride. acid alkali metal or alkaline earth metal salt, and then react with trimethylamine in a great excess of chloroacetic acid to obtain a mixture of betaine and alkali metal or alkaline earth metal salt, and use electrodialysis, ion exchange, ion exclusion, recrystallization and other separation methods to reduce, Removal of inorganic salts to produce betaine hydrochloride, phosphate or complex betaine products

Ma Lanyu et al. described in the Chinese patent ZL 93109224.8 that sodium chloroacetate and trimethylamine were used as raw materials, and strong acidic cation exchange resin was used as the reaction liquid purification medium to obtain betaine hydrochloride with a purity > 98.5% and a yield > 96%. product, since this method is basically similar to the sugar beet molasses extraction method in terms of separation and post-treatment technology, it obviously also has the same disadvantages as the extraction method, that is, complex process, high energy consumption, environmental pollution, and product purity fluctuations; Xie Xinji et al. Chinese patent ZL 98122140.8 discloses a method for synthesizing betaine hydrochloride by reacting sodium chloroacetate with trimethylamine, through moderate concentration and other processes, with a product yield of about 90% and a purity of 98.15%; US 2,800,502 discloses a Chloroacetic acid and trimethylamine are used as raw materials, and anion resin is used as a synthesis method of betaine hydrate. Compared with the previous method, there are few residual inorganic salts in the product, and the product has high purity, but chlorine is consumed in production. The trimethylamine of 2-3 times of acetic acid amount must exist trimethylamine reclaiming and environmental pollution problem, and needs a large amount of water during this method resin exchange, and cost is higher; Disclosed a kind of chloroacetic acid and sodium carbonate in the And react to generate sodium chloroacetate, react with excess trimethylamine, and synthesize betaine and betaine hydrochloride through processes such as ion exchange resin separation, the product purity is higher than 98%, this method uses sodium carbonate raw material, increases chloroacetic acid The neutralization reaction step increases the cost, and there are sodium salt residues in the product at the same time, which affects product quality; Sun Yuxiu et al. disclose a kind of using chloroacetic acid and trimethylamine as raw materials (trimethylamine and chloroacetic acid molar ratio 1 -3: 1), basic anion resin is the technology of synthesizing betaine hydrochloride under the catalyzed condition of catalyst (addition amount is 0.9-4% of reactant amount), yield 70%-75%, and purity is about 98%, and Compared with the previous several synthetic methods, although this method is easier to operate, it avoids the acid-base neutralization reaction and reduces the pollution of inorganic salts to the product, but because the amount of catalyst anion resin is less in the reaction, a large amount of catalyst is needed in the reaction synthesis process. Trimethylamine, the reaction of trimethylamine and chloroacetic acid may generate trimethylamine chloroacetate and remain in the final product, which not only affects the product quality of betaine hydrochloride, but also reduces the utilization rate of chloroacetic acid, making the process betaine hydrochloride The salt yield is only 70%-75%, and the patented technology cannot directly produce high-purity betaine products, which greatly limits the promotion of this method in food, cosmetics, medicine, biochemical and other high-end betaine production fields

[0004] In summary, the current betaine and betaine hydrochloride production technologies generally have a long reaction time (most inventions include the neutralization reaction step of chloroacetic acid), many reaction by-products, and are difficult to remove (some products may Inorganic salt components of residual alkali metals or alkaline earth metals), electrodialysis (such as Chinese patents: ZL 02159258.6, ZL 200410103519.9) and other separation methods are required, which increases production costs and other shortcomings

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