CN112679372A - Process for recovering betaine from beet waste honey - Google Patents
Process for recovering betaine from beet waste honey Download PDFInfo
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- CN112679372A CN112679372A CN202011501951.9A CN202011501951A CN112679372A CN 112679372 A CN112679372 A CN 112679372A CN 202011501951 A CN202011501951 A CN 202011501951A CN 112679372 A CN112679372 A CN 112679372A
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- betaine
- waste honey
- beet
- honey
- resin
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- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229960003237 betaine Drugs 0.000 title claims abstract description 71
- 239000002699 waste material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 235000012907 honey Nutrition 0.000 title claims abstract description 24
- 230000008569 process Effects 0.000 title claims abstract description 23
- 235000016068 Berberis vulgaris Nutrition 0.000 title claims abstract description 19
- 241000335053 Beta vulgaris Species 0.000 title claims abstract description 19
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 title claims abstract 19
- 239000011347 resin Substances 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 239000008394 flocculating agent Substances 0.000 claims abstract description 7
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 7
- 239000012498 ultrapure water Substances 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 239000008186 active pharmaceutical agent Substances 0.000 claims abstract description 4
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 4
- 239000000919 ceramic Substances 0.000 claims abstract description 4
- 238000013375 chromatographic separation Methods 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 125000002091 cationic group Chemical group 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000005457 optimization Methods 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 235000013379 molasses Nutrition 0.000 claims 3
- 239000000047 product Substances 0.000 abstract description 7
- 238000012216 screening Methods 0.000 abstract description 2
- 238000010828 elution Methods 0.000 description 11
- 238000001179 sorption measurement Methods 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000012086 standard solution Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005303 weighing Methods 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000019737 Animal fat Nutrition 0.000 description 1
- 208000003495 Coccidiosis Diseases 0.000 description 1
- 208000004930 Fatty Liver Diseases 0.000 description 1
- 206010019708 Hepatic steatosis Diseases 0.000 description 1
- 206010023076 Isosporiasis Diseases 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 208000010706 fatty liver disease Diseases 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 1
- 235000013923 monosodium glutamate Nutrition 0.000 description 1
- 239000004223 monosodium glutamate Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 231100000240 steatosis hepatitis Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for recovering betaine from beet waste honey, which comprises the following specific steps: 1) insoluble component removal process: adding a flocculating agent and a filter aid into the beet waste honey, standing for 12-24 hours, adsorbing impurities and suspended matters, filtering the supernatant by a plate frame or ceramic membrane to obtain a beet waste honey water solution with Ca and Mg ions less than 550ppm/DS, dry matter less than 55% and zero suspended solids; 2) the chromatographic separation process comprises the following steps: optimizing and screening out the betaine in the waste honey extracted in series in a cationic three-stage way by using 5 kinds of resins, wherein the flow rate of the resins is required to be controlled at 20-50 mL/min; 3) the betaine detection method comprises the following steps: decolorizing the betaine extractive solution with active carbon, concentrating, crystallizing to obtain crude betaine, dissolving with ultrapure water, filtering with 0.22 μm water phase membrane, and detecting with high performance liquid chromatography to obtain betaine with purity of 98%. The invention can more effectively obtain high-purity betaine and meet the requirement of high-purity products.
Description
Technical Field
The invention relates to a process for recovering betaine, in particular to a process for recovering betaine from waste beet honey.
Background
Betaine, also known as trimethylglycine, is a quaternary ammonium alkaloid, and has a simple chemical molecular structure: (CH3)3N + CH2COO-, with a molecular weight of 117.15, and usually contains a crystal water. Is a colorless or slightly brown crystallized compound, has sweet taste, good stability and strong antioxidant capacity. Betaine has multiple functions, and can be used as a donor of high-efficiency methyl, promote animal fat metabolism, relieve stress, regulate osmotic pressure, promote livestock growth, increase body weight and egg yield, stabilize vitamins, prevent coccidiosis, prevent fatty liver, and improve feed utilization rate. A large amount of waste honey is generated in the process of preparing sugar by using the beet, the waste honey is usually used for fermenting and producing products such as alcohol, monosodium glutamate, yeast, citric acid and the like, and the betaine is not damaged in the production process and finally enters waste liquid. At present, most of the waste liquid is discharged, so that the environment is polluted and resources are wasted. With the continuous development of economy and the continuous improvement of the living standard of people in China, the domestic demand of betaine tends to rise year by year, and domestic products can not meet the market demand, so that the development scene of betaine is very wide.
Disclosure of Invention
The invention aims to provide a process for recovering betaine from beet waste honey, which is environment-friendly, saves resources and meets market demands.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the process for recovering betaine from beet waste honey comprises the following specific steps:
1) insoluble component removal process: adding a flocculating agent and a filter aid into the waste honey, standing for 12-24 hours, adsorbing impurities and suspended matters, filtering supernatant by a plate frame or ceramic membrane to obtain a beet waste honey water solution with Ca and Mg ions less than 550ppm/DS, dry matter less than 55% and zero suspended solids;
2) the chromatographic separation process comprises the following steps: 2 kinds of cation resin are screened through optimization of 5 kinds of resin, betaine in waste liquid is extracted in a three-stage series connection mode, and the flow rate of the resin is required to be controlled to be 20-50 mL/min; through the adsorption and elution research of 5 kinds of resin on betaine standard solution, the 001x7 or D001 resin is screened to have the strongest adsorption capacity on betaine at the flow rate of 20-50mL/min and the largest resolution on betaine at the hydrochloric acid concentration of 1.0-1.5 mol/L.
3) The betaine detection method comprises the following steps: decolorizing the betaine extractive solution with active carbon, evaporating for concentration, extracting with ethanol, freeze drying to obtain crude betaine, dissolving with ultrapure water, filtering with 0.22 μm water phase membrane, and detecting with high performance liquid chromatography to obtain betaine with purity of 98%;
preferably, the flocculating agent in the step 1) is any one of polyaluminium chloride, polyacrylamide, bentonite and chitosan; the filter aid is any one of calcium carbonate and diatomite.
Preferably, the resin types in step 2) 5 are: d314, D001, 001x7, 201x7, ZGC 108.
Preferably, the 2 cationic resins in step 2) are D001 and 001x7, respectively.
Preferably, the betaine in the step 2) is extracted by using any one of cation three-stage resin series extraction or sequential simulated moving bed extraction of D001 or 001x 7.
Preferably, in the step 2), betaine can be resolved with 1.0 to 1.5mol/L hydrochloric acid or pure water.
Compared with the prior art, the invention has the advantages that: the invention can more effectively obtain high-purity betaine; through researching the optimization of the 5 kinds of resins on the adsorption quantity, the elution quantity and the elution efficiency of the betaine, the transition of the extraction technology from a laboratory level to an industrial level is realized; provides new methods for the high-value utilization of the beet waste honey, and provides new ways for food fermentation, extraction and application of active ingredients.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a HPLC chart of betaine standard;
FIG. 3 is a HPLC chart of crude betaine.
Detailed Description
The invention will be further explained with reference to the drawings.
Referring to fig. 1, the process for recovering betaine from beet waste honey of the invention comprises the following specific steps:
1) insoluble component removal process: adding a flocculating agent and a filter aid into the waste honey, standing for 12-24 hours, adsorbing impurities and suspended matters, filtering supernatant by a plate frame or ceramic membrane to obtain a beet waste honey water solution with Ca and Mg ions less than 550ppm/DS, dry matter less than 55% and zero suspended solids;
2) the chromatographic separation process comprises the following steps: through optimization screening of 5 kinds of resins, betaine in the waste honey extracted in a cation three-stage series mode is extracted, the flow rate of the resins is required to be controlled to be 20-50mL/min, and through adsorption and elution research on 5 kinds of resins on a betaine standard solution, the 001x7 type resin is screened to have the strongest adsorption capacity on the betaine at the flow rate of 20-50mL/min and have the largest resolution rate on the betaine at the hydrochloric acid concentration of 1.0-1.5 mol/L;
3) the betaine detection method comprises the following steps: the method comprises resolving waste beet honey 001 × 7 or D001 cation resin with 5-10% ammonia water solution at flow rate of 20-50mL/min and temperature of 35 deg.C to obtain effluent containing betaine, decolorizing, evaporating for concentration, extracting with ethanol, freeze drying to obtain crude betaine product, dissolving with ultrapure water, filtering with 0.22 μm water phase membrane, and detecting with high performance liquid chromatography to obtain betaine with purity of 98%.
The flocculating agent in the step 1) is any one of polyaluminium chloride, polyacrylamide, bentonite and chitosan; the filter aid is any one of calcium carbonate and diatomite.
The 5 types of resins in the step 2) are as follows: the D314, D001, 001x7, 201x7, ZGC108, 001x7 type resins may be replaced with D001 resins.
In the step 2), the betaine is extracted by adopting a sequential simulated moving bed, and the cation three-section series resin can be replaced by the sequential simulated moving bed.
In the step 2), 1.0-1.5mol/L hydrochloric acid or pure water can be used for resolving betaine.
Study on adsorption and elution Properties of cation exchange resin
TABLE 1 adsorption and elution results of the resins for betaine Standard solutions
| Resins and their use | Adsorption amount mg/ml | Elution amount mg/ml | Elution efficiency type |
| D314 | 14.65 | 12.52 | 85.46％ |
| D001 | 24.77 | 22.15 | 89.42％ |
| 001×7 | 15.46 | 13.78 | 89.13％ |
| 201×7 | 18.64 | 16.36 | 87.76％ |
| ZGC108 | 17.63 | 15.4 | 87.46％ |
As shown in Table 1, the elution efficiency of each resin was 85% or more, but the adsorption amount and elution amount of the 001X7 and D001 type resins were 89% or more, and the elution efficiency was higher than those of the other 3 types of resins. The content change of betaine in effluent after D001 and 001 × 7 resin exchange is determined to show that the adsorption performance on betaine is better, and the saturated exchange amount on betaine is larger.
High performance liquid chromatography for measuring betaine
Chromatographic conditions
A chromatographic column: waters Xbridge C18 (4.6X 150mm,3 μm);
mobile phase: methanol/water (30: 70);
flow rate: 1.0-1.5 mL/min;
column temperature: at room temperature
Detection wavelength: 200 nm;
temperature of analytical column: 30-40 ℃;
sample introduction volume: 10-20 μ L.
Preparation of betaine solution
(1) Preparation of standard solution
Weighing 8g of betaine standard, dissolving with ultrapure water, transferring to a 400mL volumetric flask, and preparing 20mg/mL betaine standard solution for later use.
(2) Preparation of test solutions
Precisely weighing a certain amount of crude betaine product by an electronic analytical balance, dissolving with ultrapure water, and filtering with a 0.22 μm water phase filter membrane for use.
Drawing of betaine standard curve
Precisely measuring prepared betaine standard solution with the concentration of 20mg/mL, wherein the concentration of the betaine standard solution is 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL and 9mL, placing the solution in a 10mL volumetric flask, fixing the volume by using ultrapure water, shaking up, filtering by using a 0.22 mu m water-phase filter membrane, collecting filtrate, detecting by using a high performance liquid chromatograph, and calculating a regression equation according to the peak area and the concentration of the betaine.
Determination of the concentration of crude betaine
As can be seen from FIG. 2, the peak time of the betaine standard product is 4.1785min, and as can be seen from FIG. 3, the peak time of the crude betaine product is 4.1785 min. The peak-out time is consistent, and the purity of the extracted betaine is calculated to be 98% by adopting a peak area method.
Claims (5)
1. A process for recovering betaine from beet waste honey is characterized by comprising the following specific steps:
1) insoluble component removal process: adding a flocculating agent and a filter aid into the waste honey, standing for 12-24 hours, adsorbing impurities and suspended matters, filtering supernatant by a plate frame or ceramic membrane to obtain a beet waste honey water solution with Ca and Mg ions less than 550ppm/DS, dry matter less than 55% and zero suspended solids;
2) the chromatographic separation process comprises the following steps: 2 kinds of cation resin are screened through optimization of 5 kinds of resin, betaine in waste honey is extracted in a three-stage series connection mode, and the flow rate of the resin is required to be controlled to be 20-50 mL/min;
3) the betaine detection method comprises the following steps: decolorizing the betaine extractive solution with active carbon, evaporating for concentration, extracting with ethanol, freeze drying to obtain crude betaine, dissolving with ultrapure water, filtering with 0.22 μm water phase membrane, and detecting with high performance liquid chromatography to obtain betaine with purity of 98%.
2. The process for recovering betaine from beet molasses as claimed in claim 1, wherein: the flocculating agent in the step 1) is any one of polyaluminium chloride, polyacrylamide, bentonite and chitosan; the filter aid is any one of calcium carbonate and diatomite.
3. The process for recovering betaine from beet molasses as claimed in claim 1, wherein: the types of the resin in the step 2) 5 are as follows: d314, D001, 001x7, 201x7, ZGC 108.
4. The process for recovering betaine from beet molasses as claimed in claim 1 or 3, wherein: the 2 kinds of cationic resins in the step 2) are D001 and 001x7 respectively.
5. The process for recovering betaine from waste honey as claimed in claim 1, wherein: in the step 2), the betaine is extracted by adopting any one of D001 or 001x7 cation three-stage resin series extraction or sequential simulated moving bed extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011501951.9A CN112679372A (en) | 2020-12-18 | 2020-12-18 | Process for recovering betaine from beet waste honey |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011501951.9A CN112679372A (en) | 2020-12-18 | 2020-12-18 | Process for recovering betaine from beet waste honey |
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| CN112679372A true CN112679372A (en) | 2021-04-20 |
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| CN202011501951.9A Pending CN112679372A (en) | 2020-12-18 | 2020-12-18 | Process for recovering betaine from beet waste honey |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113698309A (en) * | 2021-09-10 | 2021-11-26 | 中南民族大学 | Method for extracting and separating betaine ester from bolete |
| CN113976075A (en) * | 2021-10-19 | 2022-01-28 | 恒枫食品科技有限公司 | Material and system for removing caffeine in solution |
| 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107602404A (en) * | 2017-09-25 | 2018-01-19 | 新疆绿原糖业有限公司 | A kind of method from molasses alcohol waste liquid extraction high-purity betaine |
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2020
- 2020-12-18 CN CN202011501951.9A patent/CN112679372A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602404A (en) * | 2017-09-25 | 2018-01-19 | 新疆绿原糖业有限公司 | A kind of method from molasses alcohol waste liquid extraction high-purity betaine |
Non-Patent Citations (2)
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| 张书文等: "甜菜糖蜜发酵废液中提取甜菜碱新工艺研究", 《精细化工》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113698309A (en) * | 2021-09-10 | 2021-11-26 | 中南民族大学 | Method for extracting and separating betaine ester from bolete |
| CN113698309B (en) * | 2021-09-10 | 2024-02-06 | 中南民族大学 | Method for extracting and separating betaine fat from bolete |
| CN113976075A (en) * | 2021-10-19 | 2022-01-28 | 恒枫食品科技有限公司 | Material and system for removing caffeine in solution |
| CN113976075B (en) * | 2021-10-19 | 2023-09-19 | 恒枫食品科技有限公司 | Material and system for removing caffeine in solution |
| 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 |
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Application publication date: 20210420 |