CN1165813A - Synthetic process for betaine as fodder additive - Google Patents
Synthetic process for betaine as fodder additive Download PDFInfo
- Publication number
- CN1165813A CN1165813A CN 96120087 CN96120087A CN1165813A CN 1165813 A CN1165813 A CN 1165813A CN 96120087 CN96120087 CN 96120087 CN 96120087 A CN96120087 A CN 96120087A CN 1165813 A CN1165813 A CN 1165813A
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- synthesis technique
- synthesis
- catalyzer
- trimethylamine
- betaine
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Abstract
A process for synthesizing betaine from trimethylamine and 2-chloroacetic acid features that during reaction a certain quantity of strong (or weak) alkaline anionic exchange resin is added to make heating unnecessary and shorten reaction time greatly, resulting in high yield increased by 5%, high purity and simple process.
Description
Trimethyl-glycine is that China was as the product innovation of fodder additives over the past two years, and its main physiological function is to participate in metabolism of fat for animal provides methyl donor, regulates Premeabilisation of cells and presses stable vitamin.Because its distinctive physiological function has caused the common concern of domestic and international Animal nutrition and herding circle already.
The method of producing trimethyl-glycine at present has two kinds, and the one, from the by product molasses of sugaring, extract external these methods that adopt more.The 2nd, with the method for chemosynthesis.As far back as the sixties French Patent method of chemosynthesis trimethyl-glycine had once been proposed, but this method long reaction time, power consumption is bigger in the reaction process, byproduct of reaction is more, and difficulty is removed, reaction yield is low, and product cost is higher, so aquaculture wishes that urgently the preparation method that a kind of production technique is simple, production cost is low, product purity is high can be arranged.
The objective of the invention is to overcome the deficiency of existing production technique, provide a kind of and need not to heat, the reaction times shortens greatly, the purity height of product, the preparation method is simple, production cost is low betaine as fodder additive new synthetic process.
Purpose of the present invention can realize by following measure: use 2-Mono Chloro Acetic Acid and Trimethylamine 99 through synthetic, vacuum concentration, acidifying, filtration, drying, obtain the beet alkali hydrochlorate crystal, make catalyzer with strong base or weak base type anionite-exchange resin.
Concrete synthetic method is: add 2-Mono Chloro Acetic Acid and catalyzer in agitation condition downhill reaction device, drip trimethylamine aqueous solution then, the mol ratio of 2-Mono Chloro Acetic Acid and Trimethylamine 99 is 1: 3-1, the addition of catalyzer is the 0.9-4% of total reactant weight, be preferably 2-3%, normal temperature stirs down, reacted 1-2 hour, what can be used as catalyzer of the present invention is strong basic type anion-exchange resin and weak base type anionite-exchange resin, synthesis temperature is 20-40 ℃, be preferably 25-30 ℃, generated time is 0.5-2 hour.After reaction finishes, leach catalyzer and wait until back usefulness, filtrate is carried out vacuum concentration under 50-80 ℃ of condition, and concentrated solution transfers pH value to about the 1-2 with 10-12M hydrochloric acid, and the hydrochloric acid of the most handy 12M is transferred PH to 2.Placement is spent the night, and suction filtration is dry under 50-70 ℃ then, the final beet alkali hydrochlorate crystal that gets.
The product of preparing according to preparation method proposed by the invention has purity height, stable performance, advantage that preparation cost is low.
Accompanying drawing is a synthesis technique FB(flow block) of the present invention.
Embodiment 1:
Add 2-Mono Chloro Acetic Acid 100.0g in having the 500ml there-necked flask of agitator, catalyzer 2.0g starts agitator, drip 30% trimethylamine solution 313.0g, behind reinforced the finishing, under 20 ℃ of conditions, stirred 1 hour, filter, filtrate is carried out vacuum concentration under 50 ℃, to PH=1, spend the night by placement with the 12M hcl acidifying for concentrated solution, and suction filtration gets beet alkali hydrochlorate 114.0g, weight yield is 70%, and purity is 98%.
Embodiment 2:
Preparation process and example 1 are together.But Trimethylamine 99 is reinforced to be 375.0g, and catalyzer is 2.5g, and the reaction times is 1.5 hours, temperature of reaction is 30 ℃, and the vacuum concentration temperature is 70 ℃, and the hcl acidifying of using 11M is to PH=1.5, gained beet alkali hydrochlorate 118.0g, weight yield are 72%, and purity is 98%.
Embodiment 3:
Preparation process and example 1 are together.But Trimethylamine 99 is reinforced to be 250.0g, and catalyzer is 3.0g, and the reaction times is 2 hours, and temperature of reaction is 40 ℃, and the vacuum concentration temperature is 80 ℃, and the hcl acidifying of using 10M is to PH=2.0, and gained beet alkali hydrochlorate 120.0g, weight yield are 75%, and pure rate is 98%.
Claims (9)
1, a kind of synthetic process for betaine as fodder additive uses 2-Mono Chloro Acetic Acid and Trimethylamine 99 through synthetic, vacuum concentration, acidifying, filtration, drying, obtains the beet alkali hydrochlorate crystal, it is characterized in that making catalyzer with strong base or weak base type anionite-exchange resin.
2, synthesis technique as claimed in claim 1 is characterized in that the chloroacetic mol ratio of Trimethylamine 99 and 2-is 1-3: 1.
3, synthesis technique as claimed in claim 1 or 2, the addition that it is characterized in that catalyzer is the 0.9-4% of total reactant weight.
4, synthesis technique as claimed in claim 3, the addition that it is characterized in that catalyzer is the 2-3% of total reactant weight.
5, synthesis technique as claimed in claim 1, the synthesis temperature that it is characterized in that trimethyl-glycine is 20-40 ℃, generated time is 0.5-2 hour.
6, synthesis technique as claimed in claim 5 is characterized in that synthesis temperature is preferably 25-30 ℃.
7, synthesis technique as claimed in claim 1 is characterized in that synthesis reaction solution carries out vacuum concentration under 50-80 ℃ of condition.
8, synthesis technique as claimed in claim 1 is characterized in that said acidifying, is that concentrated solution transfers pH value at 1-2 with the hydrochloric acid of 10-12M.
9, synthesis technique as claimed in claim 1, it is characterized in that concentrated solution the hydrochloric acid of the most handy 12M transfer pH value to 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96120087A CN1054597C (en) | 1996-10-16 | 1996-10-16 | Synthetic process for betaine as fodder additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96120087A CN1054597C (en) | 1996-10-16 | 1996-10-16 | Synthetic process for betaine as fodder additive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1165813A true CN1165813A (en) | 1997-11-26 |
| CN1054597C CN1054597C (en) | 2000-07-19 |
Family
ID=5126129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96120087A Expired - Fee Related CN1054597C (en) | 1996-10-16 | 1996-10-16 | Synthetic process for betaine as fodder additive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1054597C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404117C (en) * | 2005-12-01 | 2008-07-23 | 江南大学 | Preparation method of alpha-alkyl betaine amphoteric surfactant |
| CN101323581B (en) * | 2008-07-18 | 2011-06-15 | 山西大学 | Synthetic method of beet alkali and beet alkali hydrochlorate |
| CN102267918A (en) * | 2011-06-23 | 2011-12-07 | 杭州海尔希畜牧科技有限公司 | Method for preparing betaine hydrochloride |
| CN101531604B (en) * | 2008-09-23 | 2012-02-22 | 宜兴市天石饲料有限公司 | Method for synthesizing betaine |
| CN102827011A (en) * | 2011-06-16 | 2012-12-19 | 山东奥克特化工有限公司 | Preparation method of betaine hydrochloride |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2957919B1 (en) * | 2010-03-23 | 2012-06-01 | Rhodia Operations | CONTINUOUS PROCESS FOR THE PRODUCTION OF AQUEOUS BETAINE SOLUTIONS |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1437540A (en) * | 1965-03-22 | 1966-05-06 | Kuhlmann Ets | Process for the preparation of betaine hydrate |
| FR1471521A (en) * | 1965-03-31 | 1967-03-03 | Orgamol Sa | Process for the synthesis of betaine salts |
| CN1039411C (en) * | 1993-08-05 | 1998-08-05 | 北京市饲料科学技术研究所 | Synthetic method of betaine |
-
1996
- 1996-10-16 CN CN96120087A patent/CN1054597C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404117C (en) * | 2005-12-01 | 2008-07-23 | 江南大学 | Preparation method of alpha-alkyl betaine amphoteric surfactant |
| CN101323581B (en) * | 2008-07-18 | 2011-06-15 | 山西大学 | Synthetic method of beet alkali and beet alkali hydrochlorate |
| CN101531604B (en) * | 2008-09-23 | 2012-02-22 | 宜兴市天石饲料有限公司 | Method for synthesizing betaine |
| CN102827011A (en) * | 2011-06-16 | 2012-12-19 | 山东奥克特化工有限公司 | Preparation method of betaine hydrochloride |
| CN102267918A (en) * | 2011-06-23 | 2011-12-07 | 杭州海尔希畜牧科技有限公司 | Method for preparing betaine hydrochloride |
| CN102267918B (en) * | 2011-06-23 | 2014-05-07 | 杭州海尔希畜牧科技有限公司 | Method for preparing betaine hydrochloride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1054597C (en) | 2000-07-19 |
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