CN101863785A - Environmental-protection preparation method of betaine hydrochloride - Google Patents
Environmental-protection preparation method of betaine hydrochloride Download PDFInfo
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- CN101863785A CN101863785A CN 201010204233 CN201010204233A CN101863785A CN 101863785 A CN101863785 A CN 101863785A CN 201010204233 CN201010204233 CN 201010204233 CN 201010204233 A CN201010204233 A CN 201010204233A CN 101863785 A CN101863785 A CN 101863785A
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- beet alkali
- calcium
- trimethylamine
- alkali hydrochlorate
- sulfuric acid
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Abstract
The invention belongs to the technical field of fine chemical engineering, in particular to an environmental-protection preparation method of betaine hydrochloride, which is characterized by comprising the following steps: firstly, carrying out neutralization reaction by taking calcium hydroxide or calcium oxide, chloroacetic acid, trimethylamine and sulfuric acid as raw materials to generate calcium chloroacetate; carrying out quaternization reaction with the trimethylamine; and then acidizing with the sulfuric acid to prepare the betaine hydrochloride. The invention does not need expensive alkali and salt, and therefore, the cost is 15-20 percent lower than that of the traditional process; the product has simple and sufficient separation, and three wastes can not be generated, and therefore, the betaine hydrochloride has higher economy and environment protection.
Description
(1) technical field
The invention belongs to the fine chemical technology field, particularly a kind of environment-friendly preparation method of beet alkali hydrochlorate.
(2) background technology
The chemical name of beet alkali hydrochlorate is the hydrochloric acid Trimethyl glycine, is a kind of quaternary ammonium alkaloid, and molecular formula is C
5H
11NO
2HCL can be dissolved in water and alcohol, and it is acid that the aqueous solution becomes, and ability high temperature below 200 ℃ has very strong antioxidant property.Beet alkali hydrochlorate is as a kind of brand-new additive for farm animal feed, and it has a far reaching influence to animal growth and development and carcass quality.
The preparation method of beet alkali hydrochlorate has natural beet sirup extraction method and chemical synthesis.The former makes its application have certain limitation owing to raw material sources are limited; Traditional chemical synthesis process adopts sodium chloroacetate and Trimethylamine 99 reaction, and the sodium-chlor of generation is difficult to remove.In recent years to this research as adopting strong cation-exchanging resin method, solvent method or sodium hydroxide being replaced with method such as calcium hydroxide, all exist cost height, aftertreatment difficulty, supersalinity waste water and problems such as can't handle, this has limited the industrialized development of trimethyl-glycine greatly.
(3) summary of the invention
The present invention is in order to remedy the deficiencies in the prior art, provides that a kind of technology is simple, the environment-friendly preparation method of the beet alkali hydrochlorate of environmental protection.
The present invention is achieved through the following technical solutions:
A kind of environment-friendly preparation method of beet alkali hydrochlorate, it is characterized in that: with calcium hydroxide or calcium oxide, Mono Chloro Acetic Acid, Trimethylamine 99 and sulfuric acid is raw material, carry out neutralization reaction earlier and generate calcium chloroacetate, carry out quaternary ammonium reaction with Trimethylamine 99 again, the sulfuric acid acidation preparation generates beet alkali hydrochlorate then.
The present invention improves original synthetic route, and its synthesis condition has been carried out exploring optimization, and the main technique method that it adopts is:
Calcium hydroxide or calcium oxide and Mono Chloro Acetic Acid obtain calcium chloroacetate solution in reaction below 45 ℃, feeding Trimethylamine 99 below 40 ℃ then, under 30～85 ℃, carry out quaternary ammonium reaction, then use filtering calcium sulfate of sulfuric acid acidation and beet alkali hydrochlorate solution, filtered liquid obtains the target product beet alkali hydrochlorate through condensing crystal; And calcium sulfate further is processed into the high strength gypsum powder of high added value.
The mole proportioning of the reaction mass that adopts among the present invention is: calcium hydroxide or calcium oxide, Mono Chloro Acetic Acid, Trimethylamine 99 and sulfuric acid=1: 1: 1～1.5: 1～1.1, require the calcium oxide or calcium hydroxide content 〉=90% of employing, Mono Chloro Acetic Acid content 〉=98%, the content of Trimethylamine 99 〉=99%.
In acidization, it is 1.0～2.0 that sulfuric acid slowly drips and transfer to pH, refilters; The yield of the beet alkali hydrochlorate that obtains at last is at (with acetometer) more than 95%.
The present invention only needs cheap calcium oxide and sulfuric acid because of not needing the alkali and the hydrochloric acid of costliness, will hang down 15～20% so cost is compared with traditional technology, and product separation is simple and abundant, there is no the three wastes and produces, and therefore has the higher economy and the feature of environmental protection.
(4) embodiment
Embodiment 1:
Adopt the material of following weight proportion: Mono Chloro Acetic Acid (content 〉=98%) 100g, calcium oxide (content 〉=90%) 32g, Trimethylamine 99 (content 〉=99%) 63g, sulfuric acid 50g.
Concrete operations are as follows:
100g Mono Chloro Acetic Acid, water 120ml are added in the reaction flask of 500ml, abundant stirring and dissolving, add then calcium oxide 32g in 30～50 ℃ down reaction 2 hours to pH be 4.0～9.0, feed Trimethylamine 99 63g, continue stirring reaction down in 25～80 ℃, the sulfuric acid of slow Dropwise 5 0g after reaction finishes, transferring pH is 1.0～2.0, filters calcium sulfate, and the filtrate condensing crystal filters, dry pure product beet alkali hydrochlorate 155g, it is 97.3% that chromatography of ions records content.
Embodiment 2:
Adopt the material of following weight proportion: Mono Chloro Acetic Acid (content 〉=98%) 100g, calcium hydroxide (content 〉=90%) 40g, Trimethylamine 99 (content 〉=99%) 70g, sulfuric acid 52g.
Concrete operations are as follows:
100g Mono Chloro Acetic Acid, water 120ml are added in the reaction flask of 500ml, abundant stirring and dissolving, add then calcium hydroxide 40g in 30～50 ℃ down reaction 2 hours to pH be 4.0～9.0, feed Trimethylamine 99 70g, continue stirring reaction down in 25～80 ℃, the sulfuric acid of slow Dropwise 5 2g after reaction finishes, transferring pH is 1.0～2.0, filters calcium sulfate, and the filtrate condensing crystal filters, dry pure product beet alkali hydrochlorate 150g, it is 98.5% that chromatography of ions records content.
Embodiment 3:
Adopt the material of following weight proportion: Mono Chloro Acetic Acid (content 〉=98%) 100g, calcium hydroxide (content 〉=90%) 43g, Trimethylamine 99 (content 〉=99%) 80g, sulfuric acid 55g.
100g Mono Chloro Acetic Acid, water 120ml are added in the reaction flask of 500ml, abundant stirring and dissolving, add then calcium hydroxide 43g in 30～50 ℃ down reaction 2 hours to pH be 4.0～9.0, feed Trimethylamine 99 80g, continue stirring reaction down in 25～80 ℃, the sulfuric acid of slow Dropwise 5 5g after reaction finishes, transferring pH is 1.0～2.0, filters calcium sulfate, and the filtrate condensing crystal filters, dry pure product beet alkali hydrochlorate 149g, it is 99.1% that chromatography of ions records content.
Claims (5)
1. the environment-friendly preparation method of a beet alkali hydrochlorate, it is characterized in that: with calcium hydroxide or calcium oxide, Mono Chloro Acetic Acid, Trimethylamine 99 and sulfuric acid is raw material, carry out neutralization reaction earlier and generate calcium chloroacetate, carry out quaternary ammonium reaction with Trimethylamine 99 again, the sulfuric acid acidation preparation generates beet alkali hydrochlorate then.
2. the environment-friendly preparation method of beet alkali hydrochlorate according to claim 1, it is characterized in that: calcium hydroxide or calcium oxide and Mono Chloro Acetic Acid obtain calcium chloroacetate solution in reaction below 45 ℃, feeding Trimethylamine 99 below 40 ℃ then, under 30～85 ℃, carry out quaternary ammonium reaction, then use filtering calcium sulfate of sulfuric acid acidation and beet alkali hydrochlorate solution, filtered liquid obtains the target product beet alkali hydrochlorate through condensing crystal.
3. the environment-friendly preparation method of beet alkali hydrochlorate according to claim 1 and 2, it is characterized in that: described calcium hydroxide or calcium oxide, Mono Chloro Acetic Acid, Trimethylamine 99 and vitriolic mol ratio are: 1: 1: 1～1.5: 1～1.1.
4. the environment-friendly preparation method of beet alkali hydrochlorate according to claim 1 and 2, it is characterized in that: it is 1.0～2.0 that described sulfuric acid slowly drips and transfer to pH.
5. the environment-friendly preparation method of beet alkali hydrochlorate according to claim 1 and 2, it is characterized in that: the described calcium sulfate that filters out is processed into the high strength gypsum powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010204233 CN101863785A (en) | 2010-06-21 | 2010-06-21 | Environmental-protection preparation method of betaine hydrochloride |
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|---|---|---|---|
| CN 201010204233 CN101863785A (en) | 2010-06-21 | 2010-06-21 | Environmental-protection preparation method of betaine hydrochloride |
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| CN101863785A true CN101863785A (en) | 2010-10-20 |
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| CN 201010204233 Pending CN101863785A (en) | 2010-06-21 | 2010-06-21 | Environmental-protection preparation method of betaine hydrochloride |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807499A (en) * | 2012-08-27 | 2012-12-05 | 陈林世 | Method for preparing betaine hydrochloride |
| 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 |
| CN109593518A (en) * | 2018-12-06 | 2019-04-09 | 古莱特科技股份有限公司 | A kind of solid acid de-plugging system for acidification of oil field de-plugging |
| CN114539082A (en) * | 2022-04-01 | 2022-05-27 | 山东瑞弘生物科技股份有限公司 | Environment-friendly preparation and purification method of betaine hydrochloride |
| CN115368256A (en) * | 2022-09-14 | 2022-11-22 | 宁夏太康药业有限公司 | Preparation method of N, N-dimethylglycine |
| CN115819259A (en) * | 2022-09-02 | 2023-03-21 | 宁夏太康药业有限公司 | Method for preparing sarcosine by chelating calcium |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374293A (en) * | 2002-03-18 | 2002-10-16 | 浙江大学 | Green synthesis process of betaine hydrochloride |
-
2010
- 2010-06-21 CN CN 201010204233 patent/CN101863785A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374293A (en) * | 2002-03-18 | 2002-10-16 | 浙江大学 | Green synthesis process of betaine hydrochloride |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102807499A (en) * | 2012-08-27 | 2012-12-05 | 陈林世 | Method for preparing betaine hydrochloride |
| CN109593518A (en) * | 2018-12-06 | 2019-04-09 | 古莱特科技股份有限公司 | A kind of solid acid de-plugging system for acidification of oil field de-plugging |
| CN114539082A (en) * | 2022-04-01 | 2022-05-27 | 山东瑞弘生物科技股份有限公司 | Environment-friendly preparation and purification method of betaine hydrochloride |
| CN115819259A (en) * | 2022-09-02 | 2023-03-21 | 宁夏太康药业有限公司 | Method for preparing sarcosine by chelating calcium |
| CN115368256A (en) * | 2022-09-14 | 2022-11-22 | 宁夏太康药业有限公司 | Preparation method of N, N-dimethylglycine |
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Application publication date: 20101020 |