CN1112345C - Short-path molecular distillation process for refining lactic acid - Google Patents
Short-path molecular distillation process for refining lactic acid Download PDFInfo
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- CN1112345C CN1112345C CN00114432A CN00114432A CN1112345C CN 1112345 C CN1112345 C CN 1112345C CN 00114432 A CN00114432 A CN 00114432A CN 00114432 A CN00114432 A CN 00114432A CN 1112345 C CN1112345 C CN 1112345C
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- lactic acid
- distillation
- short
- evaporator
- temperature
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 title claims abstract description 198
- 235000014655 lactic acid Nutrition 0.000 title claims abstract description 97
- 239000004310 lactic acid Substances 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000000199 molecular distillation Methods 0.000 title claims abstract description 16
- 238000007670 refining Methods 0.000 title claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 238000001944 continuous distillation Methods 0.000 claims abstract 2
- 239000005416 organic matter Substances 0.000 claims abstract 2
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 6
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 238000000526 short-path distillation Methods 0.000 claims 2
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000007790 scraping Methods 0.000 claims 1
- 239000011265 semifinished product Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000008236 heating water Substances 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 238000003303 reheating Methods 0.000 abstract 1
- 229960000448 lactic acid Drugs 0.000 description 67
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 24
- 239000000047 product Substances 0.000 description 16
- 238000000746 purification Methods 0.000 description 15
- 239000006200 vaporizer Substances 0.000 description 11
- 235000013305 food Nutrition 0.000 description 8
- 230000007115 recruitment Effects 0.000 description 5
- LPEKGGXMPWTOCB-UHFFFAOYSA-N 8beta-(2,3-epoxy-2-methylbutyryloxy)-14-acetoxytithifolin Natural products COC(=O)C(C)O LPEKGGXMPWTOCB-UHFFFAOYSA-N 0.000 description 4
- ODQWQRRAPPTVAG-GZTJUZNOSA-N doxepin Chemical compound C1OC2=CC=CC=C2C(=C/CCN(C)C)/C2=CC=CC=C21 ODQWQRRAPPTVAG-GZTJUZNOSA-N 0.000 description 4
- 229940057867 methyl lactate Drugs 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 2
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- MRABAEUHTLLEML-UHFFFAOYSA-N Butyl lactate Chemical compound CCCCOC(=O)C(C)O MRABAEUHTLLEML-UHFFFAOYSA-N 0.000 description 1
- 229930182843 D-Lactic acid Natural products 0.000 description 1
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 229940022769 d- lactic acid Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940116333 ethyl lactate Drugs 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000003903 lactic acid esters Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940017144 n-butyl lactate Drugs 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明涉及乳酸的短程暨分子蒸馏精制工艺。采用分子蒸馏技术，其基本工艺是：1)将乳酸含量为30-80%的乳酸溶液用物料泵送入蒸发器中，保持一个定量，在一定的工作压力下，边加热蒸馏，边馏出水份、冷却收集，使乳酸含量保持在95%以上。2)将浓缩的乳酸用泵均匀地送入短程分子蒸馏蒸发器中，进行再加热蒸馏；根据物料中不同物质在即定的压力温度条件下的不同分子自由程分级冷凝收集水份、乳酸和大分子有机物，并用泵送出，蒸发器内物料温度保持在115℃以内。3)当持续蒸馏过程中料温度高于115℃时，向蒸发器里通入少量水蒸气，当物料温度升至120℃，停止蒸馏，用泵输出残余物。4)将蒸馏出的水份与制得的乳酸进行含量调整，得到含量为88-90%的成品乳酸。The invention relates to a short-range and molecular distillation refining process of lactic acid. Using molecular distillation technology, the basic process is: 1) Pump the lactic acid solution with a lactic acid content of 30-80% into the evaporator, keep a certain amount, and under a certain working pressure, distill while heating Water, cooled and collected to keep the lactic acid content above 95%. 2) Pump the concentrated lactic acid evenly into the short-range molecular distillation evaporator for reheating and distillation; collect water, lactic acid and macromolecules according to the different molecular free paths of different substances in the material under the given pressure and temperature conditions. Molecular organic matter is pumped out, and the temperature of the material in the evaporator is kept within 115°C. 3) When the temperature of the material is higher than 115°C during the continuous distillation process, a small amount of water vapor is introduced into the evaporator, and when the temperature of the material rises to 120°C, the distillation is stopped and the residue is output by a pump. 4) Adjust the content of the distilled water and the prepared lactic acid to obtain a finished lactic acid with a content of 88-90%.
Description
The present invention relates to the short-path molecular distillation process for refining of a kind of complete processing of Chemicals, particularly lactic acid.It is a kind of process for refining of obtain lactic acid, is applicable to the refining processing to food grade or pharmaceutical grade work in-process lactic acid or finished product lactic acid (comprising left-handed or dextrorotation or DL lactic acid), makes it to reach heat-resisting level fine purification of lactic acid.
Lactic acid is a kind of purposes industrial chemicals comparatively widely, and it is mainly used in food service industry and medication chemistry industries such as beer, liquor beverage, and lactic acid is the a-hydroxy-propionic acid again, and its chemical molecular formula is: CH
3CHOHCOOH, molecular weight are 90.8.The price of food grade lactic acid is at 52 cents/pound in the international market, and the price of fine purification of lactic acid is at 1 dollar/pound, and both price differences are very big.The raw material that is used to prepare fine purification of lactic acid now is generally and adopts the food grade that fermentation method produces or the lactic acid of pharmaceutical grade, is substantially devoid of mineral ion, but contains reducing sugar.Its finished product is yellowly owing to contain organic impurity such as thalline degradation product, and multinomial physical and chemical index does not reach the requirement of fine purification of lactic acid, therefore, obtaining fine purification of lactic acid just must reprocess it, remove the organic impurities that wherein contains, wish that simultaneously refining cost of processing is cheap as far as possible, the lactic product quality that obtains is good.According to the knowledge of the applicant, now manufacturer produces fine purification of lactic acid and adopts esterification process usually, the steps include: 1) with food grade or pharmaceutical grade lactic acid under rough vacuum (760-20 mmhg) condition, the heating thickening reaches more than 95% lactic acid content.2) lactic acid behind the general is transferred in the retort, adds an amount of methanol esterification under the effect of catalyzer, generates methyl lactate, go out methyl lactate by vacuum distilling again and change hydrolytic decomposition pot over to, add distilled water, carry out the reflux hydrolysis, generate lactic acid and methyl alcohol, again methyl alcohol is distilled out, obtain fine purification of lactic acid.The weak point of this fine purification of lactic acid technology is: 1. the boiling point of methyl lactate and methyl alcohol is lower, and its methyl alcohol that contains of the purity requirement of the fine purification of lactic acid that will make must not be greater than 1,000,000/, so, the loss in vacuum distillation process of methyl lactate and methyl alcohol is serious, and the yield of product is lower.2. methyl alcohol evaporate in the air in process of production, and on-the-spot and environment are caused certain influence, and is harmful.3. because the deficiency that its technology self exists, make the fine purification of lactic acid of final gained, often, wherein methanol content becomes substandard product owing to exceeding standard.
The objective of the invention is, improve, propose the short-path molecular distillation process for refining of lactic acid at above-mentioned the deficiencies in the prior art.To remove organic impurities in the lactic acid, obtain highly purified fine purification of lactic acid, reduce refining cost of processing simultaneously.
Technical solution of the present invention is, adopts the lactic acid of food grade or pharmaceutical grade or low levels lactic acid work in-process as raw material, it is characterized in that adopt the thermal distillation that adds under the high vacuum state, its basic technology is:
1) will be that the lactic acid solution of 30-80% is sent in the vaporizer with product pump through the lactic acid content of ion-exchange, keep one quantitatively, under certain working pressure, the limit adds thermal distillation, the limit distillates moisture content, cooling is collected, and lactic acid content is remained on more than 95%, on one side spissated lactic acid is evenly exported with certain speed simultaneously, continue on one side to add rare lactic acid, distillate moisture content and should be equal to rare lactic acid magnitude of recruitment with the output lactic acid production;
2) with certain speed equably send in the vaporizer of short-range molecular distillation with mechanical pump spissated lactic acid, remain one and quantitatively under certain working pressure, open the rotation knifing, heat by chuck, the temperature of chuck is controlled at 120-150 ℃, adds thermal distillation; Collect moisture content, lactic acid and larger molecular organics according to the differing molecular free path fractional condensation under the shortly fixed pressure and temp condition of different substances in the material, and send with product pump, all distillate qualities are equal to the magnitude of recruitment of spissated lactic acid, and temperature of charge should remain in 60-115 ℃ in the vaporizer;
When 3) the material temperature is higher than 115 ℃ in continuing still-process, in vaporizer, feed a small amount of water vapor, to slow down the acid by dehydrating lactic auto-polymerization, guaranteeing operating pressure and feeding under the situation of water vapour, temperature of charge rises to 120 ℃, stops distillation, exports resistates with mechanical pump;
4) moisture content that distills out and the lactic acid that makes are carried out the content adjustment, adjusting to lactic acid content is that 88-90% promptly obtains fine purification of lactic acid.
Its feature in, the food grade of employing or the lactic acid of pharmaceutical grade or low levels lactic acid work in-process raw material are food grade or pharmaceutical grade DL or D-lactic acid.
The operating pressure of its feature in, vaporizer is 1 * 1.33322 * 10
3Handkerchief.
Its feature in, the major ingredient of the resistates of output is polymerization lactic acid, reducing sugar.
Its feature in, the resistates of output can utilize again, can add lower alcohol and produce lactic acid ester.
Advantage of the present invention is, adopted molecular distillation technique, obtain lactic acid under high vacuum condition, its process optimization is reasonable, and refining low processing cost is used common raw material, do not add catalyzer, do not add extraction agent, can obtain highly purified fine purification of lactic acid by consumption of power and steam, and can guarantee quality product.The physical and chemical index of fine purification of lactic acid reaches the level of developed countries like product.The resistates of technological process of the present invention can utilize again, can produce ethyl lactate, n-Butyl lactate etc.Use the present invention, the lactic acid overall losses is few.
Below, describe embodiments of the invention in detail.
1. at first, distillation concentrated lactic acid solution.Is that 30% lactic acid solution is sent in the luwa evaporator for 6 tons with product pump with lactic acid content, then opens the rotation knifing, opens the vacuum unit of being made up of lobe pump and water-ring pump, adjusts vacuum 30 * 1.33322 * 10
3About handkerchief, open vaporizer chuck steam, make vapour temperature remain on 130-150 ℃, the moisture content that distills out cooling is collected in the surge tank, send with product pump, and continue to replenish rare lactic acid with product pump simultaneously, magnitude of recruitment and quantity of distillate are equal to substantially, again by adjusting magnitude of recruitment and quantity of distillate, when making lactic acid in the vaporizer contain quality more than 95%, quality continues it to send with toothed gear pump from base of evaporator at the 5-6 ton, and its discharge is 300 kilograms/hour.2. promptly send into the luwa evaporator of short-range molecular distillation after the spissated lactic acid of above-mentioned process is exported by (adjustable speed) toothed gear pump, measure about 3 tons.Open the vacuum unit of forming by lobe pump and water-ring pump, cold-trap, and make the operating pressure in this vaporizer remain on 1.33322 * 10
2-1.33322 * 10
3About handkerchief, start rotatable knifing, open vaporizer chuck steam, make vapour temperature remain on 120-150 ℃, continue distillation, and continue to replenish dense lactic acid with toothed gear pump simultaneously.Magnitude of recruitment and quantity of distillate are equal to, distillate composition three grades of condensations of molecular free path different set according to its various materials under the working unit pressure and temperature, final stage condensation collection moisture content and part lactic acid continue output in surge tank with product pump, and lactic acid content is at 10-30%.B-grade condensation is collected lactic acid in surge tank, and its content continues output more than 95% with product pump.When temperature of charge in the vaporizer is not higher than 115 ℃, not at first level condensation.Behind 20 tons of products of continuous production, stop charging, continue distillation.When temperature of charge surpasses 115 ℃, open elementary condensation, collect organic colour generation thing of polymer and small part lactic acid and export back steaming in surge tank, and continue to feed a little steam from base of evaporator simultaneously, it is reference value that the feeding amount is no more than 120 ℃ with temperature of charge in the vaporizer.When the lactic acid that goes out to heat up in a steamer obviously reduces, when B-grade condensation is collected lactic acid production less than 1 kg/minute, stop distillation, with toothed gear pump resistates is exported, general each about 2.4 tons of salvage stores, the yield of lactic acid is not less than 85%, does not contain the utilization again of resistates.3. the lactic acid goods that the lactic acid that distills out blent into content and be 88-90% are the fine purification of lactic acid finished product.
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
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| CN00114432A CN1112345C (en) | 2000-03-20 | 2000-03-20 | Short-path molecular distillation process for refining lactic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00114432A CN1112345C (en) | 2000-03-20 | 2000-03-20 | Short-path molecular distillation process for refining lactic acid |
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| Publication Number | Publication Date |
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| CN1270953A CN1270953A (en) | 2000-10-25 |
| CN1112345C true CN1112345C (en) | 2003-06-25 |
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| CN00114432A Expired - Fee Related CN1112345C (en) | 2000-03-20 | 2000-03-20 | Short-path molecular distillation process for refining lactic acid |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2534252B1 (en) * | 2010-02-08 | 2015-06-17 | PURAC Biochem BV | Process for manufacturing lactic acid |
| CN102225892A (en) * | 2011-05-10 | 2011-10-26 | 武汉三江航天固德生物科技有限公司 | Preparation method of low-sodium potassium lactate |
| CN102351686B (en) * | 2011-08-16 | 2013-11-06 | 武汉三江航天固德生物科技有限公司 | Lactic acid extraction and purification production method by methanol esterification-vacuum distillation hybrid method |
| CN103724183B (en) * | 2013-12-16 | 2015-10-28 | 河南金丹乳酸科技股份有限公司 | Utilize the method for molecular distillation technique industrial production of lactic acid |
| CN105399622B (en) * | 2015-11-20 | 2017-09-19 | 武汉三江航天固德生物科技有限公司 | A kind of method of use heavy constituent production of lactic acid potassium lactate |
| CN107098808B (en) * | 2017-05-05 | 2020-01-31 | 湖北壮美生物科技有限公司 | Preparation method and production device of high-purity high-content normal-temperature non-crystallized lactic acid products |
| CN109265338A (en) * | 2018-10-09 | 2019-01-25 | 武汉三江航天固德生物科技有限公司 | The production method of medical sodium lactate solution |
| CN109160877A (en) * | 2018-10-09 | 2019-01-08 | 武汉三江航天固德生物科技有限公司 | The production method of medical calcium lactate |
| CN111574360A (en) * | 2020-05-25 | 2020-08-25 | 中粮营养健康研究院有限公司 | Method for separating lactic acid |
| CN114276233A (en) * | 2021-11-01 | 2022-04-05 | 欧尚元(天津)有限公司 | Refining and purifying method and purifying device for crude L-lactic acid |
| CN115970595A (en) * | 2022-12-30 | 2023-04-18 | 河南金丹乳酸科技股份有限公司 | A new continuous fixed-bed catalytic esterification system for preparing high-quality ethyl lactate and its preparation process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995003268A1 (en) * | 1993-07-26 | 1995-02-02 | A.E. Staley Manufacturing Company | Process for recovering organic acids |
| WO1998055442A1 (en) * | 1997-06-06 | 1998-12-10 | 'BRUSSELS BIOTECH' en abrégé '2B' | Method for purifying lactic acid |
-
2000
- 2000-03-20 CN CN00114432A patent/CN1112345C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995003268A1 (en) * | 1993-07-26 | 1995-02-02 | A.E. Staley Manufacturing Company | Process for recovering organic acids |
| WO1998055442A1 (en) * | 1997-06-06 | 1998-12-10 | 'BRUSSELS BIOTECH' en abrégé '2B' | Method for purifying lactic acid |
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| CN1270953A (en) | 2000-10-25 |
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