CN102827011A - Preparation method of betaine hydrochloride - Google Patents
Preparation method of betaine hydrochloride Download PDFInfo
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- CN102827011A CN102827011A CN2011101613803A CN201110161380A CN102827011A CN 102827011 A CN102827011 A CN 102827011A CN 2011101613803 A CN2011101613803 A CN 2011101613803A CN 201110161380 A CN201110161380 A CN 201110161380A CN 102827011 A CN102827011 A CN 102827011A
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Abstract
Disclosed is a preparation method of betaine hydrochloride. According to the preparation method, chloroacetic acid, sodium carbonate and trimethylamine are used as main raw materials and undergo processes of reaction, condensation, drying, packaging, recondensation and the like, so as to produce high-purity betaine hydrochloride. By the adoption of the technology, original methanol dehydration and double-cone dryer drying equipment is saved, cost is saved, and productivity is raised.
Description
Technical field
The present invention relates to a kind ofly prepare the production technique of beet alkali hydrochlorate, relate in particular to a kind of production technique of using Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 to prepare beet alkali hydrochlorate 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 the anhydrous or trimethylglycine hydroxide that evaporates, concentrates, three sections crystallizations, filtrations make purity about 98%.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, like the anhydrous type crystallization trimethyl-glycine of the domestic vacuum distilling method dna purity 98% that generally uses; 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, have advantages such as investment is low, product purity is high, the raw material consumption amount is low, saving cost, raising production capacity with the ordinary method ratio, thereby have good popularization value.
Summary of the invention
The present invention provides a kind of beet alkali hydrochlorate production technique, is intended to solve problems such as the ubiquitous investment of existing beet alkali hydrochlorate production technique is big, product purity is low, production capacity is low, and present method is to advancing large-scale production significant.
Technical scheme of the present invention is:
1, a kind of beet alkali hydrochlorate production technique is characterised in that may further comprise the steps:
(1) in reaction kettle, squeezes 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;
(2) 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 is 150 kilograms to remaining Trimethylamine 99, reduces the confluent of water coolant; Temperature of reaction is risen between 60 ℃-70 ℃, observe the heavy instrument of meter, after the logical material of Trimethylamine 99 finishes; Close the Trimethylamine 99 feed valve; Close the water coolant feedwater valve, keep 60 ℃-70 ℃ of temperature, stablized 1 hour;
(3) open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material; Vacuum pressure should be stabilized in-0.08MPa, and trimethyl-glycine concentration reaches at 50% o'clock, stops heating; This moment, temperature of charge was 115 ℃, stopped to stir vacuum emptying; After stopping to stir 30 minutes, treat the whole sedimentations of salt, the supernatant in the material is moved to another concentration kettle;
(4) high temperature gets rid of the material desalination and suitably uses water washing in 100 ℃; Throwing away mother liquor is extracted at once and cools in the acidifying still to 30 ℃; Add hydrochloric acid up to pH value till the 0.8-1, temperature drops to 25 ℃ and gets rid of material then, and material is put into the Vacuumdrier drying; Vacuum machine jacket steam pressure-controlled is in 3kg, and vacuum tightness is more than-0.07;
(5) dried product is put in the big pallet and is cooled off, and temperature directly packs packing after 40 ℃, detect warehousing after passing, if any big particle, and the back packing of need sieving;
(6) solution that gets rid of material after the cooling in (4) step being driven into mother liquor handles and carries out mother liquor in the still and handle; Step is with (3); Dehydrating amount dewaters according to the 20%--30% of the mother liquor amount that adds, and observes solution colour through window and changes, and when having a large amount of salt to produce in the solution, reaches concentrated condition; Get rid of in 100 ℃ then to squeeze into after the material desalination and get rid of material after being cooled to 25 ℃ in the crystallization kettle, detect and return in the acidifying still after qualified;
(7) repeat step (6), up to mother liquor darken can't use till.
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, reconcentration; Produce the beet alkali hydrochlorate of higher degree; This technology has been saved original existing methanol dehydration and two vertebra drying machine drying plants, has practiced thrift cost, has improved production capacity.
Embodiment
Embodiment 1
(1) in reaction kettle, squeezes 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;
(2) 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 is 150 kilograms to remaining Trimethylamine 99, reduce the confluent of water coolant, make temperature of reaction rise to 60 ℃; Observe the heavy instrument of meter, after the logical material of Trimethylamine 99 finishes, close the Trimethylamine 99 feed valve; Close the water coolant feedwater valve, keep 60 ℃ of temperature, stablized 1 hour;
(3) open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material; Vacuum pressure should be stabilized in-0.08MPa, and trimethyl-glycine concentration reaches at 50% o'clock, stops heating; This moment, temperature of charge was 115 ℃, stopped to stir vacuum emptying; After stopping to stir 30 minutes, treat the whole sedimentations of salt, the supernatant in the material is moved to another concentration kettle;
(4) high temperature gets rid of the material desalination and suitably uses water washing in 100 ℃; Throwing away mother liquor is extracted at once and cools in the acidifying still to 30 ℃; Add hydrochloric acid up to pH value till the 0.8-1, temperature drops to 25 ℃ and gets rid of material then, and material is put into the Vacuumdrier drying; Vacuum machine jacket steam pressure-controlled is in 3kg, and vacuum tightness is more than-0.07;
(5) dried product is put in the big pallet and is cooled off, and temperature directly packs packing after 40 ℃, detect warehousing after passing, if any big particle, and the back packing of need sieving;
(6) solution that gets rid of material after the cooling in (4) step being driven into mother liquor handles and carries out mother liquor in the still and handle; Step is with (3); Dehydrating amount dewaters according to 20% of the mother liquor amount that adds, observes solution colour through window and changes, and when having a large amount of salt to produce in the solution, reaches concentrated condition; Get rid of in 100 ℃ then to squeeze into after the material desalination and get rid of material after being cooled to 25 ℃ in the crystallization kettle, detect and return in the acidifying still after qualified;
(7) repeat step (6), up to mother liquor darken can't use till.
Embodiment 2
(1) in reaction kettle, squeezes 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;
(2) 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 is 150 kilograms to remaining Trimethylamine 99, reduce the confluent of water coolant, make temperature of reaction rise to 70 ℃; Observe the heavy instrument of meter, after the logical material of Trimethylamine 99 finishes, close the Trimethylamine 99 feed valve; Close the water coolant feedwater valve, keep 70 ℃ of temperature, stablized 1 hour;
(3) open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material; Vacuum pressure should be stabilized in-0.08MPa, and trimethyl-glycine concentration reaches at 50% o'clock, stops heating; This moment, temperature of charge was 115 ℃, stopped to stir vacuum emptying; After stopping to stir 30 minutes, treat the whole sedimentations of salt, the supernatant in the material is moved to another concentration kettle;
(4) high temperature gets rid of the material desalination and suitably uses water washing in 100 ℃; Throwing away mother liquor is extracted at once and cools in the acidifying still to 30 ℃; Add hydrochloric acid up to pH value till the 0.8-1, temperature drops to 25 ℃ and gets rid of material then, and material is put into the Vacuumdrier drying; Vacuum machine jacket steam pressure-controlled is in 3kg, and vacuum tightness is more than-0.07;
(5) dried product is put in the big pallet and is cooled off, and temperature directly packs packing after 40 ℃, detect warehousing after passing, if any big particle, and the back packing of need sieving;
(6) solution that gets rid of material after the cooling in (4) step being driven into mother liquor handles and carries out mother liquor in the still and handle; Step is with (3); Dehydrating amount dewaters according to 30% of the mother liquor amount that adds, observes solution colour through window and changes, and when having a large amount of salt to produce in the solution, reaches concentrated condition; Get rid of in 100 ℃ then to squeeze into after the material desalination and get rid of material after being cooled to 25 ℃ in the crystallization kettle, detect and return in the acidifying still after qualified;
(7) repeat step (6), up to mother liquor darken can't use till.
Claims (1)
1. the preparation method of a beet alkali hydrochlorate is characterised in that may further comprise the steps:
(1) in reaction kettle, squeezes 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;
(2) 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 is 150 kilograms to remaining Trimethylamine 99, reduces the confluent of water coolant; Temperature of reaction is risen between 60 ℃-70 ℃, observe the heavy instrument of meter, after the logical material of Trimethylamine 99 finishes; Close the Trimethylamine 99 feed valve; Close the water coolant feedwater valve, keep 60 ℃-70 ℃ of temperature, stablized 1 hour;
(3) open steam valve, make vapor pressure progressively promote, be stabilized in 0.3MPa, heating concentrates to material; Vacuum pressure should be stabilized in-0.08MPa, and trimethyl-glycine concentration reaches at 50% o'clock, stops heating; This moment, temperature of charge was 115 ℃, stopped to stir vacuum emptying; After stopping to stir 30 minutes, treat the whole sedimentations of salt, the supernatant in the material is moved to another concentration kettle;
(4) high temperature gets rid of the material desalination and suitably uses water washing in 100 ℃; Throwing away mother liquor is extracted at once and cools in the acidifying still to 30 ℃; Add hydrochloric acid up to pH value till the 0.8-1, temperature drops to 25 ℃ and gets rid of material then, and material is put into the Vacuumdrier drying; Vacuum machine jacket steam pressure-controlled is in 3kg, and vacuum tightness is more than-0.07;
(5) dried product is put in the big pallet and is cooled off, and temperature directly packs packing after 40 ℃, detect warehousing after passing, if any big particle, and the back packing of need sieving;
(6) solution that gets rid of material after the cooling in (4) step being driven into mother liquor handles and carries out mother liquor in the still and handle; Step is with (3); Dehydrating amount dewaters according to the 20%--30% of the mother liquor amount that adds, and observes solution colour through window and changes, and when having a large amount of salt to produce in the solution, reaches concentrated condition; Get rid of in 100 ℃ then to squeeze into after the material desalination and get rid of material after being cooled to 25 ℃ in the crystallization kettle, detect and return in the acidifying still after qualified;
(7) repeat step (6), up to mother liquor darken can't use till.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101613803A CN102827011A (en) | 2011-06-16 | 2011-06-16 | Preparation method of betaine hydrochloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101613803A CN102827011A (en) | 2011-06-16 | 2011-06-16 | Preparation method of betaine hydrochloride |
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| CN102827011A true CN102827011A (en) | 2012-12-19 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1457923A (en) * | 1973-04-06 | 1976-12-08 | Minnesota Mining & Mfg | Acrylate microsphere-surfaced sheet material |
| CN1165813A (en) * | 1996-10-16 | 1997-11-26 | 中国农业科学院饲料研究所 | Synthetic process for betaine as fodder additive |
| 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) |
| CN1224710A (en) * | 1998-12-16 | 1999-08-04 | 山东大学 | Synthesis of hydrochloride of betaine |
| WO2009073839A1 (en) * | 2007-12-05 | 2009-06-11 | The Cleveland Clinic Foundation | Trimethylamine compounds as risk predictors of cardiovascular disease |
| 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 |
-
2011
- 2011-06-16 CN CN2011101613803A patent/CN102827011A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1457923A (en) * | 1973-04-06 | 1976-12-08 | Minnesota Mining & Mfg | Acrylate microsphere-surfaced sheet material |
| CN1165813A (en) * | 1996-10-16 | 1997-11-26 | 中国农业科学院饲料研究所 | Synthetic process for betaine as fodder additive |
| 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) |
| CN1224710A (en) * | 1998-12-16 | 1999-08-04 | 山东大学 | Synthesis of hydrochloride of betaine |
| WO2009073839A1 (en) * | 2007-12-05 | 2009-06-11 | The Cleveland Clinic Foundation | Trimethylamine compounds as risk predictors of cardiovascular disease |
| 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 |
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Application publication date: 20121219 |