CN1117967A - Technology for extracting betaine hydrochloride - Google Patents
Technology for extracting betaine hydrochloride Download PDFInfo
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- CN1117967A CN1117967A CN 94109049 CN94109049A CN1117967A CN 1117967 A CN1117967 A CN 1117967A CN 94109049 CN94109049 CN 94109049 CN 94109049 A CN94109049 A CN 94109049A CN 1117967 A CN1117967 A CN 1117967A
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- betaine hydrochloride
- liquid
- technology
- elutriant
- column
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Abstract
The present invention relates to a preparation process for extracting hydrochloride betaine. The liquid waste of wine-making production-filtrate-effluent-Bcolumn-eluate-concentrated solution-hydrochloride betaine crystal-refined hydrochloride betaine. Advantage: it uses the by-product of beet sugar factory, i.e. residual liquid waste of wine-making by fermenting beet molasses as raw material, and its comprehensive utilization effect is good, production cost is low, and the cation exchange column parallel new technology is adopted so as to make its product purity high.
Description
The invention belongs to chemical technology field.
At present, domestic technology of not producing betaine hydrochloride abroad has and adopts molasses to produce trimethyl-glycine as raw material, and raw materials cost is higher.
The invention provides a kind of raw material adopts sugar industry byproduct beet sirup to produce betaine hydrochloride technology through the remaining waste liquid of fermentative production alcohol.
Technology of the present invention is as follows:
1, the decolouring: will make the wine waste liquid and put in the retort, add 1% gac, the stirring, under 80 ℃ of-90 ℃ of temperature, heated 1.5-3 hours, filter destainer.
2, remove metallic cation: destainer is passed through cationic exchange coloum A according to 3-10 liter minimum flow velocities, with bismuth potassium iodide test solution monitoring till the alkaloid reaction occurs, discard flow liquid (going up column volume 2/3 approximately) just, collect (about 1/3) back flow liquid, comply with last column flow rate drip washing with 1.5-2.5 times deionization of about ion-exchange volume again, get elutriant.
3, extract: the back flow liquid of gained, elutriant merges, pass through cationic exchange coloum B according to 3-10 liter minimum flow velocity full doses, discard whole effluent liquid,, collect elutriant and put in dense jar in 80 ℃ of-90 ℃ of heating with 3-7% ammoniacal liquor wash-out resin column (flow velocity is the same) of about 2-3 times of column volumes, be concentrated into 1/240 of about applied sample amount volume, approximate 2 with the 8N hcl acidifying to PH, put crystallization in the crystallizer, the betaine hydrochloride crude product.
4, purifying: get the betaine hydrochloride crude product in retort, in 60 ℃ of-70 ℃ of following stirring and dissolving, filter, put recrystallize in the crystallizer, promptly get and make with extra care the betaine hydrochloride finished product with its 2-3 times 70-90% ethanol of measuring volumes.
Advantage of the present invention is: 1, the raw material system of preparation betaine hydrochloride adopt the sugar industry byproduct be beet sirup through the remaining waste liquid of fermentative production alcohol, fully utilize effectively, production cost is low; 2, adopt the cationic exchange coloum novel process of exchange side by side; 3, product purity height generally can reach 99.6%.
Embodiment:
Adorn two of 732 cation exchange resin columns, each 100 milliliters, with the system wine waste liquid after the decolouring (system wine waste liquid added 1% activated carbon decolorizing 2 hours) upper prop A, the trimethyl-glycine positive reaction appears during 485 milliliters of flow liquid volumes, sample in the continuation, (PH ≈ 7) stops to go up sample (discard the flow liquid of preceding 485 milliliters of no trimethyl-glycines, 215 milliliters of rear portion flow liquids is standby when treating that the flow liquid volume is 700 milliliters, wash post A for 200 milliliters with water, the whole upper prop B of washing lotion and rear portion flow liquid, flow liquid discards, with 280 milliliters of wash-out posts of 5% ammoniacal liquor B, elutriant is concentrated into about 50 milliliters, to PH ≈ 2, cooling is placed with hcl acidifying, and crystallization gets the betaine hydrochloride crude product, the leaching crude product, with 100 milliliters of dissolvings of 80% ethanol (80 ℃ of-90 ℃ of thermosols), it is complete that cooling is placed to crystallization, filters, get pure product 9.9 grams of betaine hydrochloride, productive rate 76%.
Claims (1)
1, a kind of technology for extracting betaine hydrochloride, its technology is:
A, decolouring: will make the wine waste liquid and put in the retort, add 1% gac, stir, under 80 ℃ of-90 ℃ of temperature, heat 1.5-3 hours, filter destainer;
B, remove metallic cation: with destainer according to 3-10 liter minimum flow velocities by cationic exchange coloum A, with bismuth potassium iodide test solution monitoring till the alkaloid reaction occurs, discard flow liquid just, collect the back flow liquid, comply with last column flow rate drip washing with 1.5-2.5 times deionization of red ion-exchange column volume again, get elutriant;
C, extraction: with the back flow liquid of gained, elutriant merges, pass through cationic exchange coloum B according to 3-10 liter minimum flow velocity full doses, discard whole effluent liquid, with 3-7% ammoniacal liquor wash-out resin column of about 2-3 times of column volumes, collect elutriant and put in the concentration tank in 80 ℃ of-90 ℃ of heating, be concentrated into 1/240 of about applied sample amount volume, approximate 2 with the 8N hcl acidifying to PH, put crystallization in the crystallizer, get the betaine hydrochloride crude product;
D, purifying: get the betaine hydrochloride crude product in retort, in 60 ℃ of-70 ℃ of following stirring and dissolving, filter, put recrystallize in the crystallizer, promptly get and make with extra care the betaine hydrochloride finished product with its 2-3 times 70-90% ethanol of measuring volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94109049A CN1065860C (en) | 1994-08-27 | 1994-08-27 | Technology for extracting betaine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94109049A CN1065860C (en) | 1994-08-27 | 1994-08-27 | Technology for extracting betaine hydrochloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1117967A true CN1117967A (en) | 1996-03-06 |
| CN1065860C CN1065860C (en) | 2001-05-16 |
Family
ID=5033741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94109049A Expired - Fee Related CN1065860C (en) | 1994-08-27 | 1994-08-27 | Technology for extracting betaine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1065860C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102669505A (en) * | 2012-06-14 | 2012-09-19 | 中南林业科技大学 | Application of betaine and/or betaine hydrochloride in rice product |
| CN103570569A (en) * | 2013-10-17 | 2014-02-12 | 华南理工大学 | Method for preparing glycine betaine by using beet ethyl alcohol waste liquor |
| CN105566137A (en) * | 2015-12-25 | 2016-05-11 | 安徽丰原发酵技术工程研究有限公司 | Method for separation and purification of betaine from beet molasses |
| CN112624934A (en) * | 2020-12-08 | 2021-04-09 | 武汉美味源生物工程有限公司 | Method for extracting natural betaine from beet molasses |
| CN114957026A (en) * | 2022-06-02 | 2022-08-30 | 上海施聪工业科技有限公司 | Method for extracting natural betaine from yeast wastewater |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL58849A (en) * | 1978-12-11 | 1983-03-31 | Merck & Co Inc | Carboxyalkyl dipeptides and derivatives thereof,their preparation and pharmaceutical compositions containing them |
| CN1049333A (en) * | 1989-08-05 | 1991-02-20 | 新疆石河子八一制糖厂 | From the beet sirup fermented waste fluid, produce trimethyl-glycine |
| CN1039411C (en) * | 1993-08-05 | 1998-08-05 | 北京市饲料科学技术研究所 | Synthetic method of betaine |
-
1994
- 1994-08-27 CN CN94109049A patent/CN1065860C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102669505A (en) * | 2012-06-14 | 2012-09-19 | 中南林业科技大学 | Application of betaine and/or betaine hydrochloride in rice product |
| CN102669505B (en) * | 2012-06-14 | 2014-04-09 | 中南林业科技大学 | Application of betaine and/or betaine hydrochloride in rice product |
| CN103570569A (en) * | 2013-10-17 | 2014-02-12 | 华南理工大学 | Method for preparing glycine betaine by using beet ethyl alcohol waste liquor |
| CN103570569B (en) * | 2013-10-17 | 2015-06-03 | 华南理工大学 | Method for preparing glycine betaine by using beet ethyl alcohol waste liquor |
| CN105566137A (en) * | 2015-12-25 | 2016-05-11 | 安徽丰原发酵技术工程研究有限公司 | Method for separation and purification of betaine from beet molasses |
| CN112624934A (en) * | 2020-12-08 | 2021-04-09 | 武汉美味源生物工程有限公司 | Method for extracting natural betaine from beet molasses |
| CN114957026A (en) * | 2022-06-02 | 2022-08-30 | 上海施聪工业科技有限公司 | Method for extracting natural betaine from yeast wastewater |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1065860C (en) | 2001-05-16 |
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Applicant after: Wang Daishu Applicant after: Di Yue Applicant after: Lv Jingshan Applicant after: Lv Yan Applicant after: Di Hongye Applicant after: Si Yunshan Applicant after: Lv Yong Applicant after: Di Hongyu Applicant after: Cheng Dongyan Applicant before: Fang Youshu Applicant before: Di Yue Applicant before: Lv Jingshan Applicant before: Zhang Enxue Applicant before: Wang Daishu Applicant before: Nie Haitao Applicant before: Bao Yufa Applicant before: Ning You |
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