CN101591254B - Method for removing salt in betaine solution - Google Patents
Method for removing salt in betaine solution Download PDFInfo
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- CN101591254B CN101591254B CN2009100323740A CN200910032374A CN101591254B CN 101591254 B CN101591254 B CN 101591254B CN 2009100323740 A CN2009100323740 A CN 2009100323740A CN 200910032374 A CN200910032374 A CN 200910032374A CN 101591254 B CN101591254 B CN 101591254B
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- glycine
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Abstract
The invention discloses a method for removing salt in betaine solution, which comprises the followings steps: firstly removing 70 weight percent of salt in the betaine solution synthesized by taking chloroactic acid, sodium carbonate and trimethylamine as raw materials through concentration; then diluting with water until the mass concentration of the betaine is between 10 and 15 percent; performing a first-stage semi-transparent film nanofiltration on the solution at a temperature of between 60 and 70 DEG C; when the conductivity of the betaine solution reaches between 7,000 and 8,000mu s/cm, diluting the betaine solution again until the mass percentage concentration of the betaine is between 10 and 15 percent; performing a second-stage semi-transparent film nanofiltration on the solution at a temperature of between 50 and 60 DEG C; when the conductivity of the betaine solution reaches between 700 and 800 mu s/cm, finishing the treatment, desalting by a two-stage nanofiltration membrane, and achieving the effect of completely removing the salt, which cannot be achieved in a common concentration process; and performing thickening crystallization to produce betaine crystal containing less than 0.5 percent of salt. The method ensures the production of pure betaine products, saves electricity, and reduces the phenomenon of raw material waste.
Description
Technical field
The present invention relates to a kind of method that removes salt in the alkali solution of beet.
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 is synthetic, carries out concentrating and desalinating then.Because the aqueous solution of trimethyl-glycine can't remove salt with common concentration technology fully, the main synthesizing betaine hydrochloride that adopts is as commodity in the industry.Aspect pure article desalination, mainly contain two kinds of alcohol extracting method and electroosmose processs at present, see accompanying drawing 1." separation method of glycinebetaine and salt compounds in the aqueous solution " disclosed like Chinese patent 200410103519.9; Utilize glycinebetaine easily through the character of semi-permeable membranes dialysis and the special method of electrodialyzer, finally from the aqueous solution of glycinebetaine and salt compounds formation, isolate the solid salt compounds and obtain highly purified glycinebetaine.Electroosmose process needs a large amount of power consumptions, and technology controlling and process is quite harsh in the electrodialytic desalting process; In simple alcohol extracting method demineralising process, the distill repeatedly of solvent reclaims the loss that has strengthened solvent, and the solvent method desalination can not accomplish that pure article content is more than 99% in addition.
Summary of the invention
The present invention provides a kind of improved method that removes salt in the alkali solution of beet just in order to overcome above-mentioned deficiency, and innovative point is to adopt the semipermeability nf membrane to carry out the secondary nanofiltration; The synthetic aqueous solutions of betaine concentrated dilute after removing 70% salt; Carry out secondary circulation nanofiltration then, make the part salt brine solution see through nf membrane, and alkali solution of beet can be dammed by semi-permeable membranes; Through the distillation crystallization, obtain saltiness at last less than 0.5% trimethyl-glycine crystal.It specifically is to implement like this: a kind of method that removes salt in the alkali solution of beet; To be that raw material synthetic alkali solution of beet concentrates the salt that removes 70wt% with Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 earlier; It is characterized in that being diluted with water to then the trimethyl-glycine mass concentration is 10-15%, and solution carries out first step semi-permeable membranes nanofiltration circulation under 60-70 ℃, when the specific conductivity of alkali solution of beet reaches 7000-8000 μ s/cm; The mass percent concentration that dilutes alkali solution of beet to trimethyl-glycine once more is 10-15%; Solution carries out second stage semi-permeable membranes nanofiltration circulation under 50-60 ℃, when the specific conductivity of alkali solution of beet reaches 700-800 μ s/cm, and end treatment.In this technology demineralising process, after usually the trimethyl-glycine liquid concentrator was released for the first time, saltiness was generally about 2%, and one-level nanofiltration circulation can remove 80% of total salt amount in the system, and after the secondary nanofiltration desalination, total salinity is less than 0.1% in the solution.
The semipermeability nf membrane that the present invention adopts is the GEDK4040 type.Alkali solution of beet after the secondary nf membrane removes salt gets into the vacuum concentration still and concentrates, and sloughs the inner a large amount of moisture of system; When the trimethyl-glycine percentage concentration reached 70-75%, in concentration kettle, adding mass concentration was the butyleneglycol more than 99%, and add-on is 1-1.2 a times of pure trimethyl-glycine weight; Cool and separate out the trimethyl-glycine crystal, carry out spinning at last, isolating trimethyl-glycine crystal cleans with ethanol; Spinning again, centrifugal mother liquor recovery set is used.
Pulverize behind the crystal vacuum drying of separating, make commodity trimethyl-glycine crystal.
The present invention adopts the alkali solution of beet after the nanofiltration to carry out crystallization at the concentrated adding butyleneglycol that finishes, and Tc is controlled at 20-37 ℃.
Trimethyl-glycine crystal after centrifugal cleans with edible ethanol, and to guarantee product gas purity, scavenging solution carries out recycle.
Through the desalination of secondary nf membrane; Reached the result that common concentration technology can't remove salt fully, carried out condensing crystal after the combustion, produced saliferous less than 0.5% trimethyl-glycine crystal; The production of the pure article of trimethyl-glycine is guaranteed, and practices thrift power consumption and wastage of material phenomenon.
The present invention has following advantage
1, plant factor improves, and area occupied is few;
2, material loss is few in demineralising process, and yield is high;
3, the process water saving, water resources is carried out recycle through r-o-;
4, the trimethyl-glycine in seeing through film entering salt solution can be recycled;
5, after concentrating, add solvent and carry out crystallization, solvent consumption is low;
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
Interchanger adopts the stainless steel tubular heat exchange; Tubular type semi-permeable membranes (GEDK4040 type), the stainless steel material trough will be that raw material synthetic alkali solution of beet concentrates the salt that removes 70wt% with Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 earlier; Then the trimethyl-glycine liquid concentrator is diluted to 15% (mass percent concentration); Circulate under under meter control with stage pump, solution gets into semi-permeable membranes after through interchanger, and temperature is controlled at 70 ℃; Be back to then in the material trough, the salt brine solution that sees through semi-permeable membranes gets in the salt water collecting groove and reclaims.The specific conductivity of the alkali solution of beet in the stainless steel material trough is during to 7000 μ s/cm, the alkali solution of beet in the material trough got in the secondary semi-permeable membranes circulation groove with pump carried out circular treatment, and temperature is controlled at about 50 ℃; Carry out circular treatment, when specific conductivity met the requirements of 700 μ s/cm, processing finished; Material gets in the concentration kettle and concentrates, and when the trimethyl-glycine mass percent concentration reaches 75%, in concentration kettle, adds the butyleneglycol (mass percent concentration is more than 99%) of 1 times of pure trimethyl-glycine weight; Be cooled to 37 ℃ then, the trimethyl-glycine crystal is separated out, and isolating trimethyl-glycine crystal cleans with ethanol; Spinning again; Centrifugal mother liquor recovery set usefulness, oven dry trimethyl-glycine crystal makes saltiness and is 0.48% commodity trimethyl-glycine crystal.
Embodiment 2
Interchanger adopts the stainless steel tubular heat exchange; Plate and frame semi-permeable membranes (GEDK4040 type), the stainless steel material trough will be that raw material synthetic alkali solution of beet concentrates the salt that removes 70wt% with Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 earlier; Then the trimethyl-glycine liquid concentrator is diluted to 12% (mass percent concentration); Circulate under under meter control with stage pump, solution gets into semi-permeable membranes after through interchanger, and temperature is controlled at 60 ℃; Be back to then in the material trough, the salt brine solution that sees through semi-permeable membranes gets in the salt water collecting groove and reclaims.The specific conductivity of the alkali solution of beet in the stainless steel material trough is got to the alkali solution of beet in the material trough in the secondary semi-permeable membranes circulation groove with pump and to be carried out circular treatment behind 8000 μ s/cm, and temperature is controlled at about 60 ℃; Carry out circular treatment, when specific conductivity met the requirements of 750 μ s/cm, processing finished; Material gets in the concentration kettle and concentrates, and when the trimethyl-glycine mass percent concentration reaches 70%, in concentration kettle, adds the butyleneglycol (mass percent concentration is more than 99%) of 1.1 times of pure trimethyl-glycine weight; Be cooled to 20 ℃ then, the trimethyl-glycine crystal is separated out, and isolating trimethyl-glycine crystal cleans with edible ethanol; Spinning again; Centrifugal mother liquor recovery set usefulness, oven dry trimethyl-glycine crystal makes saltiness and is 0.45% commodity trimethyl-glycine crystal.
Embodiment 3
Interchanger adopts stainless steel tubular heat exchange, spiral wound semi-permeable membranes (GEDK4040 type), stainless steel material trough; The trimethyl-glycine liquid concentrator is diluted to the concentration 10% that needs; Circulate under under meter control with stage pump, solution gets into semi-permeable membranes after through interchanger, and temperature is controlled at 65 ℃; Be back to then in the material trough, the salt brine solution that sees through semi-permeable membranes gets in the salt water collecting groove and reclaims.The specific conductivity of the alkali solution of beet in the stainless steel material trough to about the 7500 μ s/cm after, the alkali solution of beet in the material trough got in the secondary semi-permeable membranes circulation groove with pump carries out circular treatment, temperature is controlled at about 55 ℃; Carry out circular treatment, when specific conductivity met the requirements of the 800 μ s/cm left and right sides, processing finished; Material gets in the concentration kettle and concentrates, and when the trimethyl-glycine mass percent concentration reaches 72%, in concentration kettle, adds the butyleneglycol (mass percent concentration is more than 99%) of 1.2 times of pure trimethyl-glycine weight; Be cooled to 30 ℃ then, the trimethyl-glycine crystal is separated out, and isolating trimethyl-glycine crystal cleans with edible ethanol; Spinning again; Centrifugal mother liquor recovery set usefulness, oven dry trimethyl-glycine crystal makes saltiness and is 0.4% commodity trimethyl-glycine crystal.
Claims (5)
1. method that removes salt in the alkali solution of beet; To be that raw material synthetic alkali solution of beet concentrates the salt that removes 70wt% with Mono Chloro Acetic Acid, yellow soda ash, Trimethylamine 99 earlier; It is characterized in that being diluted with water to then the trimethyl-glycine mass concentration is 10-15%, and solution carries out first step semi-permeable membranes nanofiltration circulation under 60-70 ℃, when the specific conductivity of alkali solution of beet reaches 7000-8000 μ s/cm; The mass percent concentration that dilutes alkali solution of beet to trimethyl-glycine once more is 10-15%; Solution carries out second stage semi-permeable membranes nanofiltration circulation under 50-60 ℃, when the specific conductivity of alkali solution of beet reaches 700-800 μ s/cm, and end treatment.
2. a kind of method that removes salt in the alkali solution of beet according to claim 1 is characterized in that the alkali solution of beet after the secondary nf membrane removes salt, gets into the vacuum concentration still and concentrates; When the trimethyl-glycine percentage concentration reaches 70-75%; In concentration kettle, adding mass concentration is the butyleneglycol more than 99%, and add-on is 1-1.2 a times of pure trimethyl-glycine weight, cools and separates out the trimethyl-glycine crystal; Carry out spinning at last; Isolating trimethyl-glycine crystal cleans with ethanol, spinning again, and centrifugal mother liquor recovery set is used.
3. a kind of method that removes salt in the alkali solution of beet according to claim 2 is pulverized behind the crystal vacuum drying that it is characterized in that separating again, makes commodity trimethyl-glycine crystal.
4. a kind of method that removes salt in the alkali solution of beet according to claim 2 is characterized in that cooling and separates out trimethyl-glycine crystalline Tc and be controlled at 20-37 ℃.
5. a kind of method that removes salt in the alkali solution of beet according to claim 2 is characterized in that the trimethyl-glycine crystal after centrifugal cleans with edible ethanol.
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| CN2009100323740A CN101591254B (en) | 2009-06-11 | 2009-06-11 | Method for removing salt in betaine solution |
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| CN2009100323740A CN101591254B (en) | 2009-06-11 | 2009-06-11 | Method for removing salt in betaine solution |
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| CN101591254B true CN101591254B (en) | 2012-07-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3027298A1 (en) * | 2013-07-31 | 2016-06-08 | Evonik Degussa GmbH | Membrane cascade with falling separating temperature |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104275091A (en) * | 2014-09-25 | 2015-01-14 | 旭泰（太仓）精细化工有限公司 | Continuous nanofiltration membrane desalter |
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2009
- 2009-06-11 CN CN2009100323740A patent/CN101591254B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| 刘久清.纳滤膜脱除高粘度良性表面活性剂中的盐.《华东理工大学学报（自然科学版）》.2005,第31卷(第5期),571-574. * |
| 董爱军.现代分离技术在制糖工业中的应用.《中国甜菜糖业》.2008,(第3期),23-25. * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3027298A1 (en) * | 2013-07-31 | 2016-06-08 | Evonik Degussa GmbH | Membrane cascade with falling separating temperature |
| EP3027298B1 (en) * | 2013-07-31 | 2024-05-15 | Evonik Oxeno GmbH & Co. KG | Membrane cascade with falling separating temperature |
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| CN101591254A (en) | 2009-12-02 |
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Denomination of invention: Method for removing salt in betaine solution Effective date of registration: 20181213 Granted publication date: 20120704 Pledgee: Wuxi rural commercial bank Limited by Share Ltd Yixing branch Pledgor: Tianshi Fodder Co., Ltd., Yixing City Registration number: 2018990001202 |
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Date of cancellation: 20200812 Granted publication date: 20120704 Pledgee: Wuxi rural commercial bank Limited by Share Ltd. Yixing branch Pledgor: SKYSTONE FEED (YIXING) Co.,Ltd. Registration number: 2018990001202 |