CN102827012A - Betaine production technology - Google Patents
Betaine production technology Download PDFInfo
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- CN102827012A CN102827012A CN2011101613860A CN201110161386A CN102827012A CN 102827012 A CN102827012 A CN 102827012A CN 2011101613860 A CN2011101613860 A CN 2011101613860A CN 201110161386 A CN201110161386 A CN 201110161386A CN 102827012 A CN102827012 A CN 102827012A
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- glycine
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Abstract
Disclosed is a betaine production technology. According to the technology, chloroacetic acid, sodium carbonate and trimethylamine are used as main raw materials, and the raw materials undergo processes of reaction, condensation, drying, packaging and the like so as to produce anhydrous betaine with its purity being 75-80%. By the adoption of the technology, former methanol dehydration and double cone dryer drying equipment is saved, betaine monohydrate is directly dried by the use of a boiling dryer after the betaine monohydrate is obtained, cost can be reduced by about 1200 yuan per ton, and production power can be raised by 3 ton/day.
Description
Technical field
The present invention relates to a kind ofly prepare the production technique of trimethyl-glycine, relate in particular to a kind of production technique of using Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 to prepare the trimethyl-glycine of 75% one 80% purity as main raw material through chemosynthesis.
Background technology
Trimethyl-glycine is a kind of natural biostearin material, molecular formula (CH
3)
3NCH
2COO, molecular weight 117, nontoxic, water absorbability is extremely strong, flavor is sweet, special odor is arranged, and it extensively is formed in the bodies of aminal and plant and important function is arranged, and it is worth and is affirmed by countless scientific researches, practice.The purposes of trimethyl-glycine is very extensive.For example, aspect medical, trimethyl-glycine can be used for medicine, the antibiotic raw material of production for treating and prevention hepatopathy.Trimethyl-glycine can be used as foodstuff additive, can both play good promoter action to care of aged, upgrowth and development of children.Aspect daily-use chemical industry,, be excellent permeation agent, wetting Agent for Printing Inks and sweeting agent, thereby can add in shampoo, body lotion, hair conditioner, skin care green grass or young crops and the toothpaste because trimethyl-glycine character is extremely gentle.Abominable as do the plant of morning, high salt, high temperature, high humidity etc. or growth that the exogenous betaine administration of crop can promote them, improve their output to growth conditions.
The method for preparing at present trimethyl-glycine mainly contains two kinds: a kind of is from the beet sirup fermented liquid, to extract; Its extraction process mainly is the ion exclusion method; Using polythene-divinyl resin chromatography separator column; The trimethyl-glycine mother liquor that wash-out goes out is through evaporation, concentrate, three sections crystallizations, filter and make anhydrous or trimethylglycine hydroxide.Present method receives season and geographic restriction, and extraction process is also more loaded down with trivial details.Another kind is through the chemical synthesis process preparation, and adopting Mono Chloro Acetic Acid and Trimethylamine 99 is that raw material reacts generation trimethyl-glycine and sodium-chlor in alkali lye, but the sodium-chlor that reaction generates is difficult to remove.Chinese patent CN93109224 discloses a kind of employing strong-acid ion exchange resin absorption, and the weak ammonia desorb concentrates then; Crystalline purification desalination method; The shortcoming of this method is a complex process not only, and the production cycle is long, and efficient is low; And energy consumption is very big, also has the great amount of wastewater discharging during ion exchange resin regeneration.
Trimethyl-glycine and hydrochloride thereof owing to limit by some specific synthesis condition, will inevitably produce a large amount of by product monochlor(in)ate sodium when being prepared by chemical synthesis process, sodium-chlor and principal product generate simultaneously, are doped in the principal product.Simultaneously, also having a small amount of heavy metal substance mixes in product.These impurity have all destroyed the quality of principal product trimethyl-glycine greatly, must it be separated fully and remove.How to accomplish to separate the most completely, be the important subject of trimethyl-glycine industry always.
Deep market study through to domestic and international manufacturing enterprise is found with statistics; The present general preparation process for extracting of employing of trimethyl-glycine, institute of beet alkali hydrochlorate manufacturing enterprise; Thereby the by product doping wherein causes problems such as foreign matter content height in ubiquity such as the product, has restricted enterprise development to a certain extent, extracts anhydrous type crystallization trimethyl-glycine like the domestic vacuum distilling method of generally using; The most outstanding defective of this method is; Because the viscosity of mother liquor is increasingly high when distilling, and the solubility with temperature of sodium-chlor in solution changes and is little, causes by product sodium-chlor all not separate with principal product effectively; This method generally can not obtain highly purified BETAINE anhydrous to the requirement height very of technology control.Comparatively advanced at present ion exchange method can be improved the deficiency of vacuum distillation method to a certain extent, but this method cost is high, and is not suitable for large-scale industrialization production running.And the invention provides a kind of brand-new Production Flow Chart; The product of producing is the BETAINE anhydrous of purity 75%-80%, has realized carrying out according to different requirements of customers the products production of different purity, has filled up the blank of production low-purity trimethyl-glycine; Production process does not have waste liquid and discharges; Low production cost, it is lower to consume energy, and yield of product is high.
Summary of the invention
The present invention provides a kind of trimethyl-glycine production technique; Be intended to solve the ubiquitous investment of existing BETAINE anhydrous production technique big, can't carry out problems such as products production, the product purity of different purity is low, production capacity is low according to customer demand, present method is to advancing large-scale production significant.
Technical scheme of the present invention is:
1, a kind of trimethyl-glycine production technique is characterised in that may further comprise the steps:
(1) reaction
In reaction kettle, squeeze into 2 tons of water, drop into 1450-1550 kilogram Mono Chloro Acetic Acid, be stirred to Mono Chloro Acetic Acid and all dissolve; Slowly drop into 800-900 kilogram soda ash light, attentive response speed when feeding intake is as the criterion not separate out a large amount of carbonic acid gas; When temperature surpasses 50 ℃; Open a spot of water coolant, temperature of charge is remained between 50 ℃ to 60 ℃, stablized 30 minutes after the completion that feeds intake;
Quantitatively throw Trimethylamine 99 900-1000 kilogram; Regulate the logical material speed of Trimethylamine 99 and the confluent of water coolant, temperature of reaction is controlled between 55 ℃-60 ℃, reaction kettle pressure the most very much not allows to surpass 0.1Mpa; When logical material to remaining Trimethylamine 99 when being 150 kilograms; Reduce the confluent of water coolant, temperature of reaction is risen between 60 ℃-70 ℃, feed intake and stablized one hour after finishing;
(2) concentrate
Open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material, and vacuum pressure should be stabilized in-0.08MPa; Trimethyl-glycine concentration reaches at 60% o'clock, stops heating, and this moment, temperature of charge was 115 ℃, stops to stir; Vacuum emptying, stop to stir 30 minutes after, treat the whole sedimentations of salt; Supernatant in the material is moved to another concentration kettle, and remaining salinity dries, and the mother liquor that throws away is squeezed into and concentrated use in the concentration kettle again;
(3) oven dry
Temperature is remained on 110-120 ℃, and pressure remains on-0.15 to-0.2Mpa, dries, and dries to be lower than at 1% o'clock to moisture content and to emit material;
(4) packing
Dried product is put in the big pallet and is cooled off, and temperature is packed material after 40 ℃, detects warehousing after passing.
The invention has the beneficial effects as follows: utilize Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 to be main raw material; Through reaction, concentrate, operations such as oven dry, packing; Produce the BETAINE anhydrous of purity 75%-80%, this technology has been saved original existing methanol dehydration and two vertebra drying machine drying plants, obtains directly drying with boiling drier behind the trimethylglycine hydroxide; Cost-saved about 1200 yuan per ton, improve 3 tons/day of production capacities.
Embodiment
Embodiment 1
(1) reaction
In reaction kettle, squeeze into 2 tons of water, drop into 1450 kilograms of Mono Chloro Acetic Acids, be stirred to Mono Chloro Acetic Acid and all dissolve; Slowly drop into 800 kilograms of soda ash lights, attentive response speed when feeding intake is as the criterion not separate out a large amount of carbonic acid gas; When temperature surpasses 50 ℃; Open a spot of water coolant, make temperature of charge remain on 50 ℃, stablized 30 minutes after the completion that feeds intake;
Quantitatively throw 900 kilograms of Trimethylamine 99s; Regulate the logical material speed of Trimethylamine 99 and the confluent of water coolant, make temperature of reaction be controlled at 55 ℃, reaction kettle pressure the most very much not allows to surpass 0.1Mpa; When logical material to remaining Trimethylamine 99 when being 150 kilograms; Reduce the confluent of water coolant, make temperature of reaction rise to 60 ℃, feed intake and stablized one hour after finishing;
(2) concentrate
Open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material, and vacuum pressure should be stabilized in-0.08MPa; Trimethyl-glycine concentration reaches at 60% o'clock, stops heating, and this moment, temperature of charge was 115 ℃, stops to stir; Vacuum emptying, stop to stir 30 minutes after, treat the whole sedimentations of salt; Supernatant in the material is moved to another concentration kettle, and remaining salinity dries, and the mother liquor that throws away is squeezed into and concentrated use in the concentration kettle again;
(3) oven dry
Temperature is remained on 110 ℃, and pressure remains on-0.15Mpa, dries, and dries to be lower than at 1% o'clock to moisture content and to emit material;
(4) packing
Dried product is put in the big pallet and is cooled off, and temperature is packed material after 40 ℃, detects warehousing after passing.
Through measuring, the purity of gained BETAINE anhydrous is 76.7%, and yield is 98.2%.
Embodiment 2
(1) reaction
In reaction kettle, squeeze into 2 tons of water, drop into 1550 kilograms of Mono Chloro Acetic Acids, be stirred to Mono Chloro Acetic Acid and all dissolve; Slowly drop into 900 kilograms of soda ash lights, attentive response speed when feeding intake is as the criterion not separate out a large amount of carbonic acid gas; When temperature surpasses 50 ℃; Open a spot of water coolant, make temperature of charge remain on 60 ℃, stablized 30 minutes after the completion that feeds intake;
Quantitatively throw 1000 kilograms of Trimethylamine 99s; Regulate the logical material speed of Trimethylamine 99 and the confluent of water coolant, make temperature of reaction be controlled at 60 ℃, reaction kettle pressure the most very much not allows to surpass 0.1Mpa; When logical material to remaining Trimethylamine 99 when being 150 kilograms; Reduce the confluent of water coolant, make temperature of reaction rise to 70 ℃, feed intake and stablized one hour after finishing;
(2) concentrate
Open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material, and vacuum pressure should be stabilized in-0.08MPa; Trimethyl-glycine concentration reaches at 60% o'clock, stops heating, and this moment, temperature of charge was 115 ℃, stops to stir; Vacuum emptying, stop to stir 30 minutes after, treat the whole sedimentations of salt; Supernatant in the material is moved to another concentration kettle, and remaining salinity dries, and the mother liquor that throws away is squeezed into and concentrated use in the concentration kettle again;
(3) oven dry
Temperature is remained on 120 ℃, and pressure remains on-0.2Mpa, dries, and dries to be lower than at 1% o'clock to moisture content and to emit material;
(4) packing
Dried product is put in the big pallet and is cooled off, and temperature is packed material after 40 ℃, detects warehousing after passing.
Through measuring, the purity of gained BETAINE anhydrous is 80%, and yield is 98.8%.
Claims (1)
1. trimethyl-glycine production technique is characterised in that may further comprise the steps:
(1) reaction
In reaction kettle, squeeze into 2 tons of water, drop into 1450-1550 kilogram Mono Chloro Acetic Acid, be stirred to Mono Chloro Acetic Acid and all dissolve; Slowly drop into 800-900 kilogram soda ash light, attentive response speed when feeding intake is as the criterion not separate out a large amount of carbonic acid gas; When temperature surpasses 50 ℃; Open a spot of water coolant, temperature of charge is remained between 50 ℃ to 60 ℃, stablized 30 minutes after the completion that feeds intake;
Quantitatively throw Trimethylamine 99 900-1000 kilogram; Regulate the logical material speed of Trimethylamine 99 and the confluent of water coolant, temperature of reaction is controlled between 55 ℃-60 ℃, reaction kettle pressure the most very much not allows to surpass 0.1Mpa; When logical material to remaining Trimethylamine 99 when being 150 kilograms; Reduce the confluent of water coolant, temperature of reaction is risen between 60 ℃-70 ℃, feed intake and stablized one hour after finishing;
(2) concentrate
Open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material, and vacuum pressure should be stabilized in-0.08MPa; Trimethyl-glycine concentration reaches at 60% o'clock, stops heating, and this moment, temperature of charge was 115 ℃, stops to stir; Vacuum emptying, stop to stir 30 minutes after, treat the whole sedimentations of salt; Supernatant in the material is moved to another concentration kettle, and remaining salinity dries, and the mother liquor that throws away is squeezed into and concentrated use in the concentration kettle again;
(3) oven dry
Temperature is remained on 110-120 ℃, and pressure remains on-0.15 to-0.2Mpa, dries, and dries to be lower than at 1% o'clock to moisture content and to emit material;
(4) packing
Dried product is put in the big pallet and is cooled off, and temperature is packed material after 40 ℃, detects warehousing after passing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101613860A CN102827012A (en) | 2011-06-16 | 2011-06-16 | Betaine production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101613860A CN102827012A (en) | 2011-06-16 | 2011-06-16 | Betaine production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102827012A true CN102827012A (en) | 2012-12-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101613860A Pending CN102827012A (en) | 2011-06-16 | 2011-06-16 | Betaine production technology |
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| CN (1) | CN102827012A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104054912A (en) * | 2014-06-11 | 2014-09-24 | 山东奥克特化工有限公司 | Method for producing betaine powder by residual mother solution in process of extracting betaine hydrochloride |
| CN105037184A (en) * | 2015-05-29 | 2015-11-11 | 韩锦超 | Preparation method of anhydrous betaine capable of preventing moisture absorption |
| CN106883990A (en) * | 2017-03-25 | 2017-06-23 | 河北碧隆化工科技有限公司 | The preparation method of high-efficiency fermenting liquid culture medium |
| CN112342003A (en) * | 2019-08-07 | 2021-02-09 | 沧州中润化学助剂有限公司 | Viscoelastic surfactant for improving recovery ratio and preparation method thereof |
Citations (5)
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|---|---|---|---|---|
| WO1998003467A1 (en) * | 1996-07-22 | 1998-01-29 | Ducoa L.P. | Process for making aqueous betaine solutions |
| US6579904B1 (en) * | 2000-09-22 | 2003-06-17 | K.E.R. Associates, Inc. | Process for making betaine transition metal complexes for use in animal feed supplements and compositions thereof |
| CN1844082A (en) * | 2006-04-26 | 2006-10-11 | 潍坊祥维斯化学品有限公司 | Process for preparing betaine |
| 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 |
-
2011
- 2011-06-16 CN CN2011101613860A patent/CN102827012A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998003467A1 (en) * | 1996-07-22 | 1998-01-29 | Ducoa L.P. | Process for making aqueous betaine solutions |
| US6579904B1 (en) * | 2000-09-22 | 2003-06-17 | K.E.R. Associates, Inc. | Process for making betaine transition metal complexes for use in animal feed supplements and compositions thereof |
| CN1844082A (en) * | 2006-04-26 | 2006-10-11 | 潍坊祥维斯化学品有限公司 | Process for preparing betaine |
| 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 |
Non-Patent Citations (3)
| Title |
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| 李红 等: "甜菜碱的研究进展", 《湖南农业科学》 * |
| 柳恒 等: "三甲胺乙内酯(甜菜碱)的合成", 《陕西化工》 * |
| 高雁 等: "甜菜碱的制备及其应用研究进展", 《新疆农业科学》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104054912A (en) * | 2014-06-11 | 2014-09-24 | 山东奥克特化工有限公司 | Method for producing betaine powder by residual mother solution in process of extracting betaine hydrochloride |
| CN104054912B (en) * | 2014-06-11 | 2016-09-07 | 山东奥克特化工有限公司 | Utilize and remain, after extracting beet alkali hydrochlorate, the method that mother solution produces glycine betaine powder |
| CN105037184A (en) * | 2015-05-29 | 2015-11-11 | 韩锦超 | Preparation method of anhydrous betaine capable of preventing moisture absorption |
| CN106883990A (en) * | 2017-03-25 | 2017-06-23 | 河北碧隆化工科技有限公司 | The preparation method of high-efficiency fermenting liquid culture medium |
| CN112342003A (en) * | 2019-08-07 | 2021-02-09 | 沧州中润化学助剂有限公司 | Viscoelastic surfactant for improving recovery ratio and preparation method thereof |
| CN112342003B (en) * | 2019-08-07 | 2022-01-07 | 沧州中润化学助剂有限公司 | Preparation method of viscoelastic surfactant for improving recovery ratio |
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Application publication date: 20121219 |