CN1844082A - Process for preparing betaine - Google Patents

Process for preparing betaine Download PDF

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CN1844082A
CN1844082A CN 200610043770 CN200610043770A CN1844082A CN 1844082 A CN1844082 A CN 1844082A CN 200610043770 CN200610043770 CN 200610043770 CN 200610043770 A CN200610043770 A CN 200610043770A CN 1844082 A CN1844082 A CN 1844082A
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betaine
step
process
alcohol
trimethylamine
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CN 200610043770
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CN100469760C (en
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雷耀辉
陈国民
刘文江
张钦太
马兴群
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潍坊祥维斯化学品有限公司
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Abstract

The invention discloses a technique of beet alkali, using chloroacetic acid and trimethylamine as material, it is getted by completeing preparation step of sodium monochloracetate, reaction step of sodium monochloracetate and trimethylamine, dehydration step and desalin ation step in turn. The technique point is adding desalin ation agent in concentrate that is getted after dehydration step, the desalin ation agent is alcohol dissolvant, the mentioned alcohol dissolvent is ethanol or mixture of carbinol and water or another liquid alcohol, the volumetric ratio of mentioned ethanol or carbinol and water or another liquid alcohol is 1:0-0.3. Filtering removing solid natrii chloridum which not resolved in desalin ation agent, after condensing, chiller crystallizing and drying the rest filtrate, the betaine-completed product will be getted. The betaine produced by this method has high purity, furthermore, the technique is simple, energy consumption is low, and no pollution is diacharged.

Description

制备甜菜碱的工艺方法 Preparation process for betaine

技术领域 FIELD

本发明涉及一种通过化学合成制备甜菜碱的工艺方法,尤其涉及一种用氯乙酸钠和三甲胺为原料制备甜菜碱的工艺方法。 The present invention relates to a process for preparing by chemical synthesis betaine, sodium chloroacetate in particular relates to a process for the preparation of trimethylamine and betaine as a raw material.

背景技术 Background technique

甜菜碱(Betaine),学名三甲胺乙内酯,分子式为(CH3)3NCH2COO,首先发现于欧洲,它主要存在于甜菜糖的糖蜜中,故而得名。 Betaine (, Betaine 1.6 M), scientific name betaine, of the formula (CH3) 3NCH2COO, first discovered in Europe, it is mainly present in the beet sugar molasses, hence the name. 自1939年DUVigneaud发现其营养功能以来,甜菜碱一直成为人们的研究热点,并被广泛地应用于制药、食品、添加剂、化学试剂、化工原料、畜禽养殖、水产养殖等领域。 Since 1939 DUVigneaud find its nutritional function, betaine has become a hot topic, and is widely used in pharmaceutical, food additives, chemical reagents, chemical raw materials, livestock, aquaculture and so on.

目前制备甜菜碱的方法主要有两种:一种是从甜菜糖蜜发酵液中提取,其提取工艺主要是离子排斥法,应用聚乙烯-二乙烯树脂色谱分离柱,洗脱出的甜菜碱母液,经蒸发、浓缩、三段结晶、过滤制得纯度约98%的无水或一水甜菜碱。 The method of preparing the betaine present there are mainly two: one is extracted from sugar beet molasses fermentation broth, extracting process is mainly an ion exclusion process, application of a polyethylene - divinylbenzene resin column chromatography, eluted betaine liquor, by evaporation, condensation, three-stage crystallization, filtration with purity of about 98%, betaine anhydrous or monohydrate. 本方法受到季节和地区的限制,提取工艺也比较烦琐。 This approach is limited by season and region, the extraction process is relatively cumbersome. 另一种是通过化学合成方法制备,采用氯乙酸和三甲胺为原料在碱液中进行反应生成甜菜碱和氯化钠,但是反应生成的氯化钠很难除去。 Another is prepared by chemical synthesis, using trimethylamine and chloroacetic acid as raw materials in the reaction product of betaine and sodium lye, the reaction is difficult to remove sodium chloride. 1994年3月30日,中国专利CN93109224中公开了一种采用强酸性离子交换树脂吸附,稀氨水解吸,然后浓缩,结晶的纯化除盐方法,该法的缺点是不但工艺复杂,生产周期长,效率低,而且能耗很大,离子交换树脂再生时还有大量废水排放。 March 30, 1994, Chinese Patent No. CN93109224 discloses a use of a strongly acidic ion exchange resin, desorption dilute ammonia, and then concentrated and purified by desalting method of crystallization, not only the drawback of this method is the complex process, long production cycle, low efficiency, large power consumption and, when the ion exchange resin regeneration as well as a large amount of wastewater emissions.

发明内容 SUMMARY

本发明所要解决的技术问题是:提供一种制备甜菜碱的工艺方法,使用该工艺方法生产的甜菜碱纯度高,而且工艺简单、能耗低,无污染物排放。 The present invention solves the technical problem are: to provide a process for preparing betaine, the use of high purity process for the production of betaine, and the process is simple, low energy consumption, no pollutant emissions.

为解决上述技术问题,本发明的技术方案是:制备甜菜碱的工艺方法,采用氯乙酸和三甲胺为原料,该工艺方法包括顺序完成的氯乙酸钠溶液制备步骤,氯乙酸钠与三甲胺反应步骤,脱水步骤和除盐步骤;所述的氯乙酸钠溶液制备步骤是,先将氯乙酸配成质量百分比浓度为20~40%的水溶液,置于设有搅拌装置的反应容器中;然后边搅拌边加入质量百分比浓度为15~30%的氢氧化钠或碳酸钠水溶液中和至pH值3.5~5.0,制得氯乙酸钠溶液;所述的氯乙酸钠与三甲胺反应步骤是,将上述步骤制得的氯乙酸钠溶液冷却至10~30℃,加入与所述氯乙酸钠匹配当量的三甲胺,控制温度在30~80℃,反应5~7小时,制得甜菜碱和氯化钠的混合溶液;所述的除盐步骤是,向脱水步骤后得到的浓缩物中加入除盐剂,在50~78℃使甜菜碱充分溶解,将不能溶于除盐剂的氯化钠 To solve the above technical problem, the technical solution of the present invention is: a process for preparing betaine, trimethylamine and chloroacetic acid as raw materials, the process comprising the step of preparing a solution of sodium chloroacetate sequence is complete, the reaction of sodium chloroacetate with trimethylamine step, dehydration step and desalting step; the sodium chloroacetate solution preparation step, the first dubbed the mass concentration of chloroacetic acid is 20 to 40% aqueous solution, placed in a reaction vessel provided with stirring means; then edge stirring, the mass concentration of 15 to 30% aqueous sodium hydroxide or aqueous sodium carbonate solution to pH 3.5 to 5.0, to prepare a solution of sodium chloroacetate; the sodium chloroacetate reaction with trimethylamine step, the above-described sodium chloroacetate step resulting solution was cooled to 10 ~ 30 ℃, sodium chloroacetate is added with the matching equivalents of trimethylamine, controlling the temperature at 30 ~ 80 ℃, reacted for 5 to 7 hours, to obtain betaine, and sodium chloride the mixed solution; the desalting step, the desalting agent is added to the resulting concentrate after dewatering step of the betaine in 50 ~ 78 ℃ fully dissolved, the sodium chloride can not be dissolved in desalted agent 体过滤去除,将滤液浓缩、冷却结晶、抽滤干燥后,得到甜菜碱成品;所述除盐剂是醇溶剂。 Material removed by filtration, the filtrate was concentrated, cooling crystallization, after suction filtration and dried, to give the finished betaine; the desalting agent is an alcohol solvent.

作为一种具体实施方式,所述醇溶剂是乙醇与水或另外一种液体醇的混合物,所述乙醇与水或另外一种液体醇的体积比为1∶0~0.3。 As a particular embodiment, the alcohol solvent is a mixture of ethanol and water or another liquid of alcohol, ethanol and the volume ratio of water or another liquid alcohol is 1-0 to 0.3. 优选为1∶0~0.15。 Preferably 1-0 to 0.15. 所述另外一种液体醇是乙二醇或丙二醇中的一种。 The addition of a liquid alcohol is a glycol or propylene glycol.

作为另一种具体实施方式,所述醇溶剂是甲醇与水或另外一种液体醇的混合物,所述甲醇与水或另外一种液体醇的体积比为1∶0~0.3。 As another specific embodiment, the alcohol solvent is a mixture of methanol and water or another liquid alcohol, the volume ratio of methanol to water or another liquid alcohol is 1-0 to 0.3. 优选为1∶0~0.15。 Preferably 1-0 to 0.15. 所述另外一种液体醇是乙醇或乙二醇或丙二醇中的一种。 Another said alcohol is a liquid alcohol or ethylene glycol or propylene glycol.

由于采用了上述技术方案,只需通过氯乙酸钠溶液制备步骤,氯乙酸钠与三甲胺反应步骤,脱水步骤和除盐步骤就可制得甜菜碱成品,无需添加强酸性离子交换树脂吸附,稀氨水解吸,工艺简单,能耗低。 By adopting the technical solution, simply by sodium chloroacetate solution preparation step, the reaction of sodium chloroacetate with trimethylamine step, a dehydration step and desalting step can be finished prepared betaine, without adding a strongly acidic ion-exchange resin, dilute ammonia desorption process is simple, low energy consumption. 由于其反应产物中只有甜菜碱和氯化钠,通过脱水步骤后得到浓缩物,然后向该浓缩物中加入除盐剂。 Since the only reaction product of betaine and sodium chloride, the concentrate obtained through the dehydration step and then added to the concentrate desalination agent. 该除盐剂是醇溶剂。 The desalting agent is an alcohol solvent. 该醇溶剂是乙醇或甲醇与水或另外一种液体醇按照1∶0~0.3,优选为1∶0~0.15的比例组成的混合溶剂,当采用乙醇作主溶剂时,所述另外一种液体醇是乙二醇或丙二醇等;当采用甲醇作主溶剂时,所述另外一种液体醇是乙醇或乙二醇或丙二醇等;当另外一种液体醇或水为零时,该除盐剂就是无水乙醇或甲醇。 The alcohol solvent is ethanol or methanol and water or another liquid alcohol 1-0 according to 0.3, preferably a mixed solvent composition ratio of 1-0 to 0.15, when using ethanol as the primary solvent, said another liquid alcohol is ethylene glycol or propylene glycol; when using methanol as a main solvent, said another liquid alcohol is ethylene glycol or propylene glycol, ethanol or the like; and when another zero liquid alcohol or water, the desalination agent is ethanol or methanol. 高温时,甜菜碱在该除盐剂中有良好的溶解性,而在低温时,甜菜碱在该除盐剂中的溶解度不大;氯化钠则微溶于该除盐剂,并且其溶解度随温度的降低而降低的幅度很小。 High temperature, the desalination agent betaine good solubility, while at low temperatures, the solubility of betaine little desalination agent; sodium chloride is sparingly soluble in the desalting agent, and their solubility with decreasing temperature decreases only slightly. 无水乙醇在常压下的沸点为78℃左右,甲醇在常压下的沸点为65℃左右,在50~78℃的条件下,大部分的甜菜碱会溶解在该除盐剂中,而大部分的氯化钠则不能溶解于其中。 Ethanol boiling point at atmospheric pressure is about 78 deg.] C, boiling point of methanol at atmospheric pressure is about 65 ℃, at 50 ~ 78 ℃, most of the betaine will be dissolved in the desalting agent, and most of the sodium chloride can not be dissolved therein. 首先通过过滤的方法将这部分不能溶解于除盐剂的氯化钠去除,再将滤液浓缩、冷却结晶、抽滤干燥,从而得到高纯度的甜菜碱成品,实验表明,甜菜碱的纯度可达94%~99.4%,收率可达95%~98.6%。 First, this part of the desalting agent can not be dissolved in the sodium chloride is removed by filtration, the filtrate was concentrated, cooling crystallization, filtration and dried to obtain high-purity betaine products, experimental results show that, up to a purity betaine from 94% to 99.4%, yield of 95% to 98.6%. 在制备过程中,脱水步骤产生的是水;除盐步骤中产生的是氯化钠固体,可以回收利用;作为除盐剂的乙醇以及水或甲醇或乙二醇或丙二醇本身无毒,滤液在浓缩时,被蒸发;因而整个过程无污染物排放,不会造成环境污染。 In the production process, water is produced by the dehydration step; desalting step is produced solid sodium chloride, can be recycled; as water or methanol or ethanol, and ethylene glycol or propylene glycol desalting agent itself toxic, the filtrate upon concentration, it is evaporated; thus the overall process without discharge of pollutants, will not cause environmental pollution.

除盐剂中除了乙醇或甲醇以外,添加另一种液体醇或水的作用是增大除盐剂的极性,其在除盐剂中所占比例越高,除盐剂的极性就越大,其对氯化钠的溶解性就越好;而甜菜碱在这种混合型除盐剂中的溶解度略有提高,但其溶解度随混合型除盐剂组分的含量变化不明显。 In addition to the desalting agent as ethanol or methanol, adding another liquid alcohol or water desalination agent is to increase the effect of polarity, the higher the proportion of its desalination agent, the more polar desalination agent large, the better the solubility of sodium chloride; and betaines such hybrid desalination agent solubility slightly increased, but the content of solubility with component hybrid desalination agent did not change significantly. 采用混合型除盐剂后,在50~78℃的高温除盐时,甜菜碱溶解度的提高,会使滤除的氯化钠盐中的甜菜碱的包结量减少,进入滤液的甜菜碱增加,从而使甜菜碱在高温除盐时损失减小,收率提高。 With hybrid desalination agent, at a high temperature of 50 ~ 78 ℃ desalting, betaine increased solubility, inclusion of an amount of betaine sodium salt was filtered off will decrease, increase into the filtrate betaines , so that the loss is reduced at high temperatures betaine desalting, yield is improved. 同时,另一种溶剂如水或乙二醇或丙二醇等溶剂其沸点都比乙醇或甲醇高,所以在蒸溜浓缩时,乙醇或甲醇的蒸发量大,其在除盐剂中所占比例就会慢慢变小,而另一种溶剂在除盐剂中所占比例就会慢慢变大。 Meanwhile, another solvent such as water or ethylene glycol or propylene glycol solvent having a boiling point higher than ethanol or methanol, when distilled it was concentrated, the evaporation amount of ethanol or methanol, in which the proportion of desalination agent will slow slowly becomes smaller, the proportion of the other solvent will gradually become larger in the desalination agent. 冷却结晶时,由于乙醇或甲醇与另一种溶剂这种相对含量的变化,使氯化钠的溶解度提高,更多的氯化钠盐留在了母液当中,从而使结晶析出的甜菜碱纯度提高。 When cooling crystallization, ethanol or methanol because the relative content of other changes such a solvent, sodium chloride to improve solubility, the more sodium chloride salt which remain in the mother liquor, so that precipitation of crystals improve the betaine purity . 而甜菜碱溶解度随混合型除盐剂组分的含量变化不明显的特点,使母液中的甜菜碱最大限度的析出,保证了收率的提高。 Betaine content of the hybrid desalination solubility with the component characteristics change significantly the maximum betaine precipitation the mother liquor, to ensure the improvement of yield. 实验表明,与单独使用乙醇或甲醇作除盐剂相比,甜菜碱成品的纯度可提高4~5%,收率可提高1~3%。 Experimental results show that, compared with methanol or ethanol alone for desalting agent, betaine purity of the finished product can be increased from 4 to 5 percent, the yield can be increased 1-3%.

作为一种改进,所述除盐步骤中还包括一个滤饼清洗分步骤,所述滤饼清洗分步骤是将过滤时得到的滤饼用除盐剂清洗,并将洗液加入所述滤液中。 As an improvement, the desalting step further comprises a sub-step washing the filter cake, the filter cake is washed substep of filtering the obtained cake was washed with demineralized agent, and the washings added to the filtrate . 其效果是将包结于氯化钠滤饼表面的甜菜碱洗下来,同滤液一起蒸馏浓缩、冷却结晶,提高了甜菜碱成品的收率。 The effect is the inclusion of sodium chloride to betaine cake washed down the surface, together with the filtrate was concentrated by distillation, cooling crystallization, the yield of betaine to improve the finished product.

具体实施方式 Detailed ways

实施例1在装有搅拌装置、气体吸收装置以及温度计的1000ml四口瓶中,加入水160g,用油浴加热,边搅拌边加入质量百分比浓度为99%的氯乙酸100g,使之完全溶解。 Example 1 equipped with a stirring device, a gas absorption device and a thermometer 1000ml four flask was added 160g of water, was heated in an oil bath, was added with stirring the mass concentration of 99% TCA 100g, to completely dissolve. 滴加质量百分比浓度为30%的碳酸钠水溶液中和,终点pH为4~4.5。 Mass concentration of the dropwise addition of 30% aqueous sodium carbonate solution, the final pH of 4 to 4.5. 中和液用冷水冷却至25℃,慢慢通入三甲胺气体约64g,控制温度在60~80℃,搅拌反应约6小时,然后接通真空系统,减压蒸去水。 Neutralized solution was cooled with cold water to 25 ℃, trimethylamine gas was slowly passed through to about 64g, in controlling the temperature 60 ~ 80 ℃, the reaction was stirred for about 6 hours and then the vacuum system is turned on, the water was evaporated under reduced pressure. 物料降温至60℃左右,加入无水乙醇750ml,加热至60~70℃,溶解物料15分钟,然后趁热抽滤,滤饼用少量无水乙醇洗涤,滤液和洗液送回四口瓶,常压浓缩至约150~200mL,冷却至15~25℃,结晶,抽滤干燥得甜菜碱成品,含量94%,收率96%。 Material was cooled to about 60 ℃, was added 750ml of anhydrous ethanol, was heated to 60 ~ 70 ℃, 15 minutes to dissolve the material, and then hot filtration, the filter cake was returned to the four bottle washed with a little ethanol and the filtrate and washings, concentrated under atmosphere pressure to about 150 ~ 200mL, cooled to 15 ~ 25 ℃, crystallization, filtration and dried to obtain the finished betaine, content 94%, yield 96%.

实施例2采用与实施例1同样的步骤,只是除盐剂由无水乙醇改换为无水乙醇与乙二醇的体积比例为1∶0.15的混合液,其它操作指标不变,最后得到甜菜碱的含量为99.4%,收率98.6%。 Example 2 By the same procedure as in Example 1 except desalting agent consists of ethanol and the ethanol is changed to the volume ratio of ethylene glycol 1:0.15 a mixture, the other operation index unchanged, to give the final betaine content of 99.4%, a yield of 98.6%.

实施例3采用与实施例1同样的步骤,只是除盐剂由无水乙醇改换为无水乙醇和丙二醇的比例为1∶0.15的混合液,其它操作指标不变,最后得到甜菜碱含量99.1%,收率98.3%。 Example 3 The same procedure and betaine content in Example 1, except desalting agent consists of ethanol and propylene glycol, ethanol is changed to the ratio of a mixture 1:0.15 other operation index unchanged, to give finally 99.1% a yield of 98.3%.

实施例4采用实施例1同样的步骤,只是除盐剂由无水乙醇改换为无水乙醇与水的比例为1∶0.05的混合液,其它操作指标不变,最后得到甜菜碱含量98.5%,收率92%。 Example 4 The same procedure as in Example 1 except desalting agent consists of ethanol is changed to the ratio of ethanol to water is a mixture 1:0.05 other operation index unchanged, betaine content of 98.5% to give the final, yield 92%.

实施例5采用实施例2同样的步骤,只是碳酸钠水溶液改换为质量百分比浓度30%的氢氧化钠水溶液,三甲胺改换为质量百分比浓度28%的水溶液,其它操作指标不变,最后得到甜菜碱含量95%,收率97.0%。 Example 5 The same procedure as in Example 2, except that the aqueous sodium carbonate solution to change a concentration of 30% by mass percent sodium hydroxide aqueous solution, an aqueous solution of trimethylamine change of mass percent concentration of 28%, the other operation index unchanged, to give the final betaine content of 95% and a yield of 97.0%.

实施例6采用实施例1同样的步骤,只是除盐剂由无水乙醇改换为甲醇,其它操作指标不变,最后得到甜菜碱含量98.5%,收率94%。 Example 6 The same procedure as in Example 1 except desalting agent consists of ethanol, methanol change, the other operation index unchanged, to give the final content of 98.5% Betaine, 94% yield.

实施例7采用实施例1同样的步骤,只是除盐剂由无水乙醇改换为甲醇与乙二醇的体积比例为1∶0.15的混合液,其它操作指标不变,最后得到甜菜碱含量98.5%,收率91%。 Example 7 The same procedure as in Example 1 except desalting agent consists of ethanol is changed to the volume ratio of methanol with ethylene glycol is a mixture 1:0.15 other operation index unchanged, to give the final content of 98.5% Betaine a yield of 91%.

另外,氯乙酸水溶液的浓度太高则反应太过剧烈,太低则反应体积过大,蒸除水能耗增加,因此,以20~40%为宜。 Further, the concentration of chloroacetic acid aqueous solution is too high the reaction is too vigorous, the reaction is too large too low, the energy consumption in addition to increased water vapor, therefore, 20 to 40% is appropriate. 三甲胺常温下为气体,温度太高,损耗增大,但如果反应温度低了则反应进行缓慢,实验表明,30~80℃是经济可行的反应温度,反应温度优选为50~60℃。 Trimethylamine is a gas at room temperature, the temperature is too high, loss increases, but if the reaction temperature is low then the reaction proceeds slowly, experiments show that, 30 ~ 80 ℃ economically feasible reaction temperature, the reaction temperature is preferably 50 ~ 60 ℃.

Claims (10)

1.制备甜菜碱的工艺方法,采用氯乙酸和三甲胺为原料,其特征在于:该工艺方法包括顺序完成的氯乙酸钠溶液制备步骤,氯乙酸钠与三甲胺反应步骤,脱水步骤和除盐步骤;所述的氯乙酸钠溶液制备步骤是,先将氯乙酸配成质量百分比浓度为20~40%的水溶液,置于设有搅拌装置的反应容器中;然后边搅拌边加入质量百分比浓度为15~30%的氢氧化钠或碳酸钠水溶液中和至pH值3.5~5.0,制得氯乙酸钠溶液;所述的氯乙酸钠与三甲胺反应步骤是,将上述步骤制得的氯乙酸钠溶液冷却至10~30℃,加入与所述氯乙酸钠匹配当量的三甲胺,控制温度在30~80℃,反应5~7小时,制得甜菜碱和氯化钠的混合溶液;所述的除盐步骤是,向脱水步骤后得到的浓缩物中加入除盐剂,在50~78℃使甜菜碱充分溶解,将不能溶于除盐剂的氯化钠固体过滤去除,将滤液浓缩、 1. The process for preparing betaine, trimethylamine and chloroacetic acid as raw materials, wherein: the process comprising the step of preparing a solution of sodium chloroacetate sequence is complete, the reaction of sodium chloroacetate with trimethylamine step, dehydration and desalting step the step of; the sodium chloroacetate solution preparation step, the first dubbed the mass concentration of chloroacetic acid is 20 to 40% aqueous solution, placed in a reaction vessel provided with stirring means; added with stirring and then the mass concentration of 15 to 30% aqueous sodium hydroxide or aqueous sodium carbonate solution to pH 3.5 to 5.0, to prepare a solution of sodium chloroacetate; the sodium chloroacetate reaction with trimethylamine step, the above steps gave a sodium chloroacetate the solution was cooled to 10 ~ 30 ℃, added with sodium chloroacetate matching the equivalents of trimethylamine, controlling the temperature at 30 ~ 80 ℃, reacted for 5 to 7 hours, to prepare a mixed solution of sodium chloride and betaine; the desalting step, the desalting agent is added to the resulting concentrate after dewatering step of the betaine in 50 ~ 78 ℃ fully dissolved, the insoluble solid sodium chloride is removed by filtration desalting agent, the filtrate was concentrated 却结晶、抽滤干燥后,得到甜菜碱成品;所述除盐剂是醇溶剂。 But crystals were filtered off with suction and dried, to give the finished betaine; the desalting agent is an alcohol solvent.
2.如权利要求1所述的制备甜菜碱的工艺方法,其特征在于:所述醇溶剂是乙醇与水或另外一种液体醇的混合物,所述乙醇与水或另外一种液体醇的体积比为1∶0~0.3。 2. A process for the preparation of the betaine of claim 1, wherein: said alcohol solvent is a mixture of ethanol and water or another liquid of alcohol, ethanol and the volume of water or another liquid alcohol ratio of 1-0 to 0.3.
3.如权利要求2所述的制备甜菜碱的工艺方法,其特征在于:所述乙醇与水或另外一种液体醇的体积比为1∶0~0.15。 3. A process for the preparation of betaine as claimed in claim 2, wherein: the volume ratio of ethanol to water or another liquid alcohol is 0.15 ~ 1-0.
4.如权利要求2或3所述的制备甜菜碱的工艺方法,其特征在于:所述另外一种液体醇是乙二醇或丙二醇中的一种。 4. The process of claim 2 or claim 3 prepared betaine, wherein: said another liquid alcohol is a glycol or propylene glycol.
5.如权利要求1所述的制备甜菜碱的工艺方法,其特征在于:所述醇溶剂是甲醇与水或另外一种液体醇的混合物,所述甲醇与水或另外一种液体醇的体积比为1∶0~0.3。 5. A process for the preparation of the betaine claim 1, wherein: said alcohol solvent is a mixture of methanol and water or another liquid alcohol, methanol and water or another liquid volume of the alcohol ratio of 1-0 to 0.3.
6.如权利要求2所述的制备甜菜碱的工艺方法,其特征在于:所述甲醇与水或另外一种液体醇的体积比为1∶0~0.15。 6. A process for the preparation of betaine as claimed in claim 2, wherein: the volume ratio of methanol and water or another liquid alcohol is 0.15 ~ 1-0.
7.如权利要求5或6所述的制备甜菜碱的工艺方法,其特征在于:所述另外一种液体醇是乙醇或乙二醇或丙二醇中的一种。 7. The process of claim 5 or claim 6 prepared betaine, wherein: said additional alcohol is a liquid alcohol or ethylene glycol or propylene glycol.
8.如权利要求1所述的制备甜菜碱的工艺方法,其特征在于:所述三甲胺为三甲胺气体或25~45%的三甲胺水溶液。 Process for the preparation of a betaine as claimed in claim 8, wherein: said aqueous trimethylamine or trimethylamine gas is 25 to 45% trimethylamine.
9.如权利要求8所述的制备甜菜碱的工艺方法,其特征在于:所述氯乙酸水溶液的浓度是25~30%,氢氧化钠水溶液的浓度是15~20%,氯乙酸钠与三甲胺反应的温度是50~60℃。 9. A process for the preparation of betaine as claimed in claim 8, wherein: the concentration of the acid aqueous solution is 25 to 30% aqueous sodium hydroxide solution of a concentration of 15 to 20%, with sodium chloroacetate trimethoxyphenyl the reaction temperature of the amine is 50 ~ 60 ℃.
10.如权利要求1所述的制备甜菜碱的工艺方法,其特征在于:所述除盐步骤中还包括一个滤饼清洗分步骤,所述滤饼清洗分步骤是将过滤时得到的滤饼用除盐剂清洗,并将洗液加入所述滤液中。 10. A process for the preparation of the betaine of claim 1, wherein: said desalting step further comprises a sub-step washing the filter cake, the filter cake washed substep is obtained when the filter cake washed with demineralized agent, and the washings added to the filtrate.
CN 200610043770 2006-04-26 2006-04-26 Process for preparing betaine CN100469760C (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101830818A (en) * 2010-05-12 2010-09-15 山东格兰德生物科技有限公司 Method for preparing anhydrous betaine
CN101863784A (en) * 2010-06-07 2010-10-20 房照智 Methods for preparing and extracting betaine and betaine hydrochloride
CN102557970A (en) * 2010-12-27 2012-07-11 山东奥克特化工有限公司 Preparation method of anhydrous betaine
CN102827012A (en) * 2011-06-16 2012-12-19 山东奥克特化工有限公司 Betaine production technology
CN103242184A (en) * 2012-02-14 2013-08-14 北京昕大洋科技发展有限公司 Glycine betaine preparation method
CN105037184A (en) * 2015-05-29 2015-11-11 韩锦超 Preparation method of anhydrous betaine capable of preventing moisture absorption
CN105494951A (en) * 2015-12-02 2016-04-20 山东祥维斯生物科技股份有限公司 Method for producing 650 betaine

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Publication number Priority date Publication date Assignee Title
CN1196351A (en) 1997-12-30 1998-10-21 河北省固安县宏峰化工有限公司 Synthesis and separation of trimethyl glycine (betaine)
CN1065236C (en) 1998-12-16 2001-05-02 山东大学 Method for synthesising betaine hydrochloride

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101830818A (en) * 2010-05-12 2010-09-15 山东格兰德生物科技有限公司 Method for preparing anhydrous betaine
CN101830818B (en) 2010-05-12 2011-05-18 山东格兰德生物科技有限公司 Method for preparing anhydrous betaine
CN101863784A (en) * 2010-06-07 2010-10-20 房照智 Methods for preparing and extracting betaine and betaine hydrochloride
CN101863784B (en) 2010-06-07 2013-02-06 房照智 Methods for preparing and extracting betaine and betaine hydrochloride
CN102557970A (en) * 2010-12-27 2012-07-11 山东奥克特化工有限公司 Preparation method of anhydrous betaine
CN102557970B (en) * 2010-12-27 2015-02-25 山东奥克特化工有限公司 Preparation method of anhydrous betaine
CN102827012A (en) * 2011-06-16 2012-12-19 山东奥克特化工有限公司 Betaine production technology
CN103242184A (en) * 2012-02-14 2013-08-14 北京昕大洋科技发展有限公司 Glycine betaine preparation method
CN105037184A (en) * 2015-05-29 2015-11-11 韩锦超 Preparation method of anhydrous betaine capable of preventing moisture absorption
CN105494951A (en) * 2015-12-02 2016-04-20 山东祥维斯生物科技股份有限公司 Method for producing 650 betaine

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