CN101531604A - Method for synthesizing betaine - Google Patents
Method for synthesizing betaine Download PDFInfo
- Publication number
- CN101531604A CN101531604A CN200810157064A CN200810157064A CN101531604A CN 101531604 A CN101531604 A CN 101531604A CN 200810157064 A CN200810157064 A CN 200810157064A CN 200810157064 A CN200810157064 A CN 200810157064A CN 101531604 A CN101531604 A CN 101531604A
- Authority
- CN
- China
- Prior art keywords
- controlled
- acetic acid
- mono chloro
- chloro acetic
- amination
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229960003237 betaine Drugs 0.000 title claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 title abstract 3
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000005576 amination reaction Methods 0.000 claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims abstract description 7
- RMQUNZQRHHMDIW-UHFFFAOYSA-N 2-chloroacetic acid;magnesium Chemical compound [Mg].OC(=O)CCl RMQUNZQRHHMDIW-UHFFFAOYSA-N 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 9
- 239000001095 magnesium carbonate Substances 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 6
- 229960001708 magnesium carbonate Drugs 0.000 claims description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 6
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 6
- 238000010924 continuous production Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 3
- 239000013505 freshwater Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract 1
- 229910052749 magnesium Inorganic materials 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for synthesizing betaine, which is characterized in that the method uses trimethylamine and chloroacetic magnesium at the molar ratio of 1.02-1.03:1 for amination and synthesis; the reaction temperature of synthesis is controlled between 40 and 60 DEGC; the optimum reaction temperature is controlled between 53 and 55 DEG C; a pH value is controlled to be between 8 and 9; synthesis time is between 2.5 and 5 hours; continuous feeding and continuous discharging are adopted; and the feeding and discharging of reaction are regulated and controlled by use of a pH meter. The method has the advantages of eliminating frequent operation for feeding, synthesis and discharging during batch production, as well as unsafe factors possibly caused by the frequent operation, increasing production yield, treating and recycling water after the concentration of betaine solution and reducing the waste of freshwater resources.
Description
Technical field
The present invention relates to a kind of method of synthesizing betaine.
Technical background
Trimethyl-glycine is to use a kind of widely additive at present, is applied in aspects such as feed, food, makeup, medicine, is that employing sodium chloroacetate, Trimethylamine 99 are that raw material carries out the synthetic trimethyl-glycine, and process flow sheet is seen Fig. 1.This technology exists following deficiency: 1) batch production, and the charging of production process, synthetic, the frequent operation of blowing yield poorly, plant factor is low, safe handling process holding time is many, may cause unsafe factor because of frequent operation in addition; 2) sodium-chlor that comes out through concentrating and separating of reaction solution is difficult to carry out industrial utilization, and production technique water does not make full use of, the production cost height, and the equipment blowing, charging emptying causes environmental pollution.
Summary of the invention
The present invention is just in order to overcome above-mentioned deficiency, and providing a kind of is the method for raw material synthesizing betaine with Mono Chloro Acetic Acid magnesium, Trimethylamine 99, and it can continuous production, the plant factor height, and waste of raw materials is few, and water resources can rationally make full use of.Specifically implement like this: a kind of method of synthesizing betaine, it is characterized in that with mol ratio being that the Trimethylamine 99 of 1.02-1.03:1 and the amination of Mono Chloro Acetic Acid magnesium are synthetic, synthesis reaction temperature is controlled at 40-60 ℃, the reaction optimum temps is controlled at 53-55 ℃, pH value is controlled to be 8-9, and generated time is 2.5-5 hour.
The present invention adopts the continuous production method, be communicated with by reaction tower, amination still, amination liquid recycle pump, trimethyl-glycine storage tank pipeline successively, be equipped with the feed-pipe of Trimethylamine 99 and Mono Chloro Acetic Acid magnesium on the reaction tower respectively, the amination liquid recycle pump inserts reaction tower after being communicated with condenser by circulating line, and the PH meter is installed on the described circulating line.Carry out continuous detecting by the meter of the PH on the circulating line and control the input and output material amount, material reacts in reaction tower, and reacted material enters reactor, carries out external forced circulation and cooling by recycle pump then, removes reaction heat, obtains the ideal transformation efficiency.
The Mono Chloro Acetic Acid magnesium that the present invention adopts is by in Mono Chloro Acetic Acid, the magnesiumcarbonate and generate, and the neutralization reaction controlled temperature is 25-40 ℃ in the Mono Chloro Acetic Acid magnesium neutralizing well.
When amination liquid in the trimethyl-glycine storage tank reach a certain amount of after, amination liquid concentrated get final product, the phlegma that obtains when concentrating amination liquid cools off, water coolant is transported to Mono Chloro Acetic Acid magnesium neutralizing well, magnesium chloride can be used as additive for farm animal feed.
The present invention adopts continuously feeding and discharging continuously, react the adjusting control of input and output material with the PH meter, eliminated the frequent operation of charging at batch production process, synthetic, blowing, with the unsafe factor that may cause because of frequent operation, and improved production output, water after alkali solution of beet concentrates recycles through handling, and has reduced the waste of Freshwater resources.Concrete advantage is:
1, plant factor improves 40%;
2, utilization rate of raw materials improves, 300 yuan/ton of cost savings;
3, the process water saving, per ton 60% aqua is saved 600 kilograms in tap water;
4, factory utilization ratio height, the workman is simple to operate;
5, magnesium chloride can be used as additive for farm animal feed;
6, the technology three-waste pollution significantly reduces.
Description of drawings
Fig. 1 is the background process flow sheet.
Fig. 2 is a process flow sheet of the present invention
Embodiment
Embodiment 1, a kind of method of synthesizing betaine, with mol ratio is that the Trimethylamine 99 of 1.02:1 and the amination of Mono Chloro Acetic Acid magnesium are synthetic, synthesis reaction temperature is controlled at 53 ℃, pH value is controlled to be 8.5, generated time is 3 hours, and wherein Mono Chloro Acetic Acid magnesium is by in Mono Chloro Acetic Acid, the magnesiumcarbonate and generate, and the neutralization reaction temperature is controlled to be 40 ℃
Embodiment 2, a kind of method of synthesizing betaine, adopt the continuous production method, be communicated with by reaction tower, amination still, amination liquid recycle pump, trimethyl-glycine storage tank pipeline successively, be equipped with the feed-pipe of Trimethylamine 99 and Mono Chloro Acetic Acid magnesium on the reaction tower respectively, the amination liquid recycle pump inserts reaction tower after being communicated with condenser by circulating line, and the PH meter is installed on the described circulating line.
With mol ratio is that the Trimethylamine 99 of 1.03:1 and the amination of Mono Chloro Acetic Acid magnesium are synthetic, synthesis reaction temperature is controlled at 55 ℃, and pH value is controlled to be 8.5, and generated time is 2.5 hours, wherein Mono Chloro Acetic Acid magnesium is by in Mono Chloro Acetic Acid, the magnesiumcarbonate and generate, and the temperature of neutralization reaction is controlled to be 30 ℃ in the neutralizing well
Embodiment 3, reference example 2, and the mol ratio of Trimethylamine 99 and Mono Chloro Acetic Acid magnesium is 1.025:1, synthesis reaction temperature is controlled at 40 ℃, and pH value is controlled to be 8, and generated time is 4 hours, in Mono Chloro Acetic Acid, the magnesiumcarbonate and generate Mono Chloro Acetic Acid magnesium, the temperature of the reaction of neutralizing well is controlled to be 25 ℃
Embodiment 4, reference example 2, and the mol ratio of Trimethylamine 99 and Mono Chloro Acetic Acid magnesium is 1.03:1, synthesis reaction temperature is controlled at 60 ℃, and pH value is controlled to be 9, and generated time is 5 hours, in Mono Chloro Acetic Acid, the magnesiumcarbonate and generate Mono Chloro Acetic Acid magnesium, the temperature of the reaction of neutralizing well is controlled to be 28 ℃
Claims (4)
1. the method for a synthesizing betaine, it is characterized in that with mol ratio being that the Trimethylamine 99 of 1.02-1.03:1 and the amination of Mono Chloro Acetic Acid magnesium are synthetic, synthesis reaction temperature is controlled at 40-60 ℃, and the reaction optimum temps is controlled at 53-55 ℃, pH value is controlled to be 8-9, and generated time is 2.5-5 hour.
2. the method for synthesizing betaine according to claim 1, it is characterized in that adopting the continuous production method, be communicated with by reaction tower, amination still, amination liquid recycle pump, trimethyl-glycine storage tank pipeline successively, be equipped with the feed-pipe of Trimethylamine 99 and Mono Chloro Acetic Acid magnesium on the reaction tower respectively, the amination liquid recycle pump inserts reaction tower after being communicated with condenser by circulating line, and the PH meter is installed on the described circulating line.
3. the method for synthesizing betaine according to claim 1 and 2 is characterized in that Mono Chloro Acetic Acid magnesium is by in Mono Chloro Acetic Acid, the magnesiumcarbonate and generate.
4. the method for synthesizing betaine according to claim 3 is characterized in that Mono Chloro Acetic Acid magnesium carries out in neutralizing well, and reaction control temperature is 25-40 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101570647A CN101531604B (en) | 2008-09-23 | 2008-09-23 | Method for synthesizing betaine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101570647A CN101531604B (en) | 2008-09-23 | 2008-09-23 | Method for synthesizing betaine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101531604A true CN101531604A (en) | 2009-09-16 |
| CN101531604B CN101531604B (en) | 2012-02-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101570647A Active CN101531604B (en) | 2008-09-23 | 2008-09-23 | Method for synthesizing betaine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101531604B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126964A (en) * | 2010-12-10 | 2011-07-20 | 江南大学 | Method for preparing high-content alpha-lauryl betaine by solvent-free quaternization |
| CN105130830A (en) * | 2015-09-14 | 2015-12-09 | 宜兴市天石饲料有限公司 | Preparation method of betaine |
| CN109134288A (en) * | 2018-08-29 | 2019-01-04 | 宜兴市天石饲料有限公司 | A kind of device and method of synthesizing betaine |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4412481A1 (en) * | 1994-04-12 | 1995-10-19 | Witco Surfactants Gmbh | Process for the preparation of highly concentrated flowable aqueous solutions of betaines |
| CN1054597C (en) * | 1996-10-16 | 2000-07-19 | 中国农业科学院饲料研究所 | Synthetic process for betaine as fodder additive |
-
2008
- 2008-09-23 CN CN2008101570647A patent/CN101531604B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126964A (en) * | 2010-12-10 | 2011-07-20 | 江南大学 | Method for preparing high-content alpha-lauryl betaine by solvent-free quaternization |
| CN105130830A (en) * | 2015-09-14 | 2015-12-09 | 宜兴市天石饲料有限公司 | Preparation method of betaine |
| CN109134288A (en) * | 2018-08-29 | 2019-01-04 | 宜兴市天石饲料有限公司 | A kind of device and method of synthesizing betaine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101531604B (en) | 2012-02-22 |
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Application publication date: 20090916 Assignee: Jiangsu Tianshi Biotechnology Co., Ltd. Assignor: Tianshi Fodder Co., Ltd., Yixing City Contract record no.: 2013320000672 Denomination of invention: Method for synthesizing betaine Granted publication date: 20120222 License type: Exclusive License Record date: 20130814 |
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Assignee: Jiangsu Tianshi Biotechnology Co., Ltd. Assignor: Tianshi Fodder Co., Ltd., Yixing City Contract record no.: 2013320000672 Date of cancellation: 20140305 |
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Denomination of invention: Method for synthesizing betaine Effective date of registration: 20140530 Granted publication date: 20120222 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Tianshi Fodder Co., Ltd., Yixing City Registration number: 2014990000426 |
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Date of cancellation: 20150323 Granted publication date: 20120222 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Tianshi Fodder Co., Ltd., Yixing City Registration number: 2014990000426 |
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Denomination of invention: Method for synthesizing betaine Effective date of registration: 20150324 Granted publication date: 20120222 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Tianshi Fodder Co., Ltd., Yixing City Registration number: 2015990000222 |
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Date of cancellation: 20161214 Granted publication date: 20120222 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Skystone Feed (Yixing) Co., Ltd. Registration number: 2015990000222 |
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Denomination of invention: Method for synthesizing betaine Effective date of registration: 20161214 Granted publication date: 20120222 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Skystone Feed (Yixing) Co., Ltd. Registration number: 2016990001109 |
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Date of cancellation: 20181221 Granted publication date: 20120222 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Tianshi Fodder Co., Ltd., Yixing City Registration number: 2016990001109 |