CN1065860C - Technology for extracting betaine hydrochloride - Google Patents
Technology for extracting betaine hydrochloride Download PDFInfo
- Publication number
- CN1065860C CN1065860C CN94109049A CN94109049A CN1065860C CN 1065860 C CN1065860 C CN 1065860C CN 94109049 A CN94109049 A CN 94109049A CN 94109049 A CN94109049 A CN 94109049A CN 1065860 C CN1065860 C CN 1065860C
- Authority
- CN
- China
- Prior art keywords
- betaine hydrochloride
- liquid
- technology
- column
- liter
- 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.)
- Expired - Fee Related
Links
- 229960003403 betaine hydrochloride Drugs 0.000 title claims abstract description 18
- HOPSCVCBEOCPJZ-UHFFFAOYSA-N carboxymethyl(trimethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC(O)=O HOPSCVCBEOCPJZ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000005516 engineering process Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 239000012043 crude product Substances 0.000 claims description 6
- 125000002091 cationic group Chemical group 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229930013930 alkaloid Natural products 0.000 claims description 2
- 150000003797 alkaloid derivatives Chemical class 0.000 claims description 2
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000005342 ion exchange Methods 0.000 claims description 2
- 150000001457 metallic cations Chemical class 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000012085 test solution Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 235000016068 Berberis vulgaris Nutrition 0.000 abstract description 3
- 241000335053 Beta vulgaris Species 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 235000013379 molasses Nutrition 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 2
- 150000001768 cations Chemical class 0.000 abstract 1
- 239000003480 eluent Substances 0.000 abstract 1
- 238000000855 fermentation Methods 0.000 abstract 1
- 230000004151 fermentation Effects 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000012262 fermentative production Methods 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- QCYOIFVBYZNUNW-UHFFFAOYSA-N 2-(dimethylazaniumyl)propanoate Chemical class CN(C)C(C)C(O)=O QCYOIFVBYZNUNW-UHFFFAOYSA-N 0.000 description 1
- 101100476962 Drosophila melanogaster Sirup gene Proteins 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a technology for extracting betaine hydrochloride and belongs to the technical field of chemical industry. The technology comprises the following steps: preparation of waste liquid from wine, liquid filtration, effluent liquid preparation, a B column, eluent liquid preparation, concentrated liquid preparation, crystallization of betaine hydrochloride, liquid filtration and refining of betaine hydrochloride. The technology has the advantages that raw material used for preparing the betaine hydrochloride is, side products in sugar industry, namely that residual alcohol waste liquid generated through fermentation of beet molasses is used as the raw material, the effect of comprehensive utilization is good, and the preparation cost is low; a novel technology of parallel cation exchanging columns is adopted, and the purity of products is 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, raw materials cost height as raw material.
The invention provides a kind of raw material adopts sugar industry byproduct beet honey to produce betaine hydrochloride technology through the remaining waste liquid of fermentative production alcohol.
Technology of the present invention is as follows:
1, 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 hour, filter destainer.
2, remove metallic cation: destainer is passed through cationic exchange coloum A according to 3-10 liter/hour minimum flow velocity, with bismuth potassium iodide test solution monitoring till the alkaloid reaction occurs, discard flow liquid (going up column volume 2/3) just, collect (1/3) back flow liquid, comply with last column flow rate drip washing with the 1.5-2.5 deionized water doubly of ion-exchange column 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/hour minimum flow velocity full dose, discard whole effluent liquid, with the 3-7% ammoniacal liquor wash-out resin column of 2-3 times of column volume (according to the 3-10 liter/hour flow velocity), collect elutriant and put in the concentration tank in 80 ℃ of-90 ℃ of heating, be concentrated into 1/240 of applied sample amount volume, equal 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, the 70-90% ethanol of doubly measuring volume with its 2-3 filters in 60 ℃ of-70 ℃ of following stirring and dissolving, puts recrystallize in the crystallizer, promptly gets and makes with extra care the betaine hydrochloride elaboration.
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 5% ammoniacal liquor with 5-10 liter/hour flow velocity wash-out post B, elutriant is concentrated into 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), cooling is placed to crystallization and finishes, and 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, and add 1% gac, and stir, heating is 1.5-3 hour under 80 ℃ of-90 ℃ of temperature, filter destainer;
B, remove metallic cation: with destainer according to 3-10 liter/hour minimum flow velocity by cationic exchange coloum A, with bismuth potassium iodide test solution monitoring till the alkaloid reaction occurs, discard column volume 2/3 on the first flow liquid, collect 1/3 back flow liquid, comply with last column flow rate drip washing with the 1.5-2.5 deionized water doubly of 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/hour minimum flow velocity full dose, discard whole effluent liquid, with the 3-7% ammoniacal liquor wash-out resin column of 2-3 times of column volume according to the 3-10 liter/hour flow velocity, collect elutriant and put in the concentration tank in 80 ℃ of-90 ℃ of heating, be concentrated into 1/240 of applied sample amount volume, equal 2 with the 8N hcl acidifying to PH, put crystallization in the crystallizer, the betaine hydrochloride crude product;
D, purifying: get the betaine hydrochloride crude product in retort, the 70-90% ethanol of doubly measuring volume with its 2-3 filters in 60 ℃ of-70 ℃ of following stirring and dissolving, puts recrystallize in the crystallizer, promptly gets and makes with extra care the betaine hydrochloride elaboration.
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 CN1117967A (en) | 1996-03-06 |
| CN1065860C true 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) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0012401A1 (en) * | 1978-12-11 | 1980-06-25 | Merck & Co. Inc. | Carboxyalkyl dipeptide derivatives, process for preparing them and pharmaceutical composition 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 |
| CN1084505A (en) * | 1993-08-05 | 1994-03-30 | 北京市饲料科学技术研究所 | The method of synthetic betaine (trimethyl-glycine) |
-
1994
- 1994-08-27 CN CN94109049A patent/CN1065860C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0012401A1 (en) * | 1978-12-11 | 1980-06-25 | Merck & Co. Inc. | Carboxyalkyl dipeptide derivatives, process for preparing them and pharmaceutical composition 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 |
| CN1084505A (en) * | 1993-08-05 | 1994-03-30 | 北京市饲料科学技术研究所 | The method of synthetic betaine (trimethyl-glycine) |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1117967A (en) | 1996-03-06 |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
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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Free format text: CORRECT: APPLICANT; FROM: FANG YOUSHU; ZHAI YUE; LV JINGSHAN; ZHANG ENXUE; WANG DISHU; NIE HAITAO; BAO YUFA; NING YOU TO: WANG DISHU; ZHAI YUE; LV JINGSHAN; LV YAN; ZHAI HONGYE; SI YUNSHAN; LV YONG; ZHAI HONGYU; CHENG DONGYAN |
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Free format text: CORRECT: PATENTEE; FROM: WANG DISHU TO: WANG LISHU |
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| CP01 | Change in the name or title of a patent holder |
Patentee after: Wang Lishu Patentee before: Wang Daishu |
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| C14 | Grant of patent or utility model | ||
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| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |