CN114478470A - 一种提纯丙交酯的方法 - Google Patents
一种提纯丙交酯的方法 Download PDFInfo
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- CN114478470A CN114478470A CN202011169560.1A CN202011169560A CN114478470A CN 114478470 A CN114478470 A CN 114478470A CN 202011169560 A CN202011169560 A CN 202011169560A CN 114478470 A CN114478470 A CN 114478470A
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- CN
- China
- Prior art keywords
- lactide
- water
- crude
- reaction
- low
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- 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.)
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- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 238000003809 water extraction Methods 0.000 claims abstract description 7
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 23
- 239000004310 lactic acid Substances 0.000 claims description 19
- 235000014655 lactic acid Nutrition 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- 150000007530 organic bases Chemical class 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 3
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000000047 product Substances 0.000 description 50
- JJTUDXZGHPGLLC-IMJSIDKUSA-N 4511-42-6 Chemical compound C[C@@H]1OC(=O)[C@H](C)OC1=O JJTUDXZGHPGLLC-IMJSIDKUSA-N 0.000 description 29
- 239000000126 substance Substances 0.000 description 22
- 239000000203 mixture Substances 0.000 description 21
- 230000003287 optical effect Effects 0.000 description 21
- 238000001514 detection method Methods 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 9
- 229920000747 poly(lactic acid) Polymers 0.000 description 9
- 239000004626 polylactic acid Substances 0.000 description 9
- 239000013638 trimer Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- OZZQHCBFUVFZGT-UHFFFAOYSA-N 2-(2-hydroxypropanoyloxy)propanoic acid Chemical compound CC(O)C(=O)OC(C)C(O)=O OZZQHCBFUVFZGT-UHFFFAOYSA-N 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000006068 polycondensation reaction Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000638 solvent extraction Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000539 dimer Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000007142 ring opening reaction Methods 0.000 description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- JJTUDXZGHPGLLC-ZXZARUISSA-N (3r,6s)-3,6-dimethyl-1,4-dioxane-2,5-dione Chemical compound C[C@H]1OC(=O)[C@H](C)OC1=O JJTUDXZGHPGLLC-ZXZARUISSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229930182843 D-Lactic acid Natural products 0.000 description 2
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229940022769 d- lactic acid Drugs 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 206010057040 Temperature intolerance Diseases 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 1
- 150000003903 lactic acid esters Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D319/00—Heterocyclic compounds containing six-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D319/10—1,4-Dioxanes; Hydrogenated 1,4-dioxanes
- C07D319/12—1,4-Dioxanes; Hydrogenated 1,4-dioxanes not condensed with other rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heterocyclic Compounds That Contain Two Or More Ring Oxygen Atoms (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims (13)
Priority Applications (1)
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CN202011169560.1A CN114478470B (zh) | 2020-10-28 | 2020-10-28 | 一种提纯丙交酯的方法 |
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CN202011169560.1A CN114478470B (zh) | 2020-10-28 | 2020-10-28 | 一种提纯丙交酯的方法 |
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Publication Number | Publication Date |
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CN114478470A true CN114478470A (zh) | 2022-05-13 |
CN114478470B CN114478470B (zh) | 2024-04-19 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114853718A (zh) * | 2022-05-05 | 2022-08-05 | 广东粤港澳大湾区黄埔材料研究院 | L-丙交酯的纯化方法 |
CN116041314A (zh) * | 2023-02-08 | 2023-05-02 | 新沂市永诚化工有限公司 | 一种粗品环酯纯化制备高纯度环酯的工艺 |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1112559A (zh) * | 1993-12-08 | 1995-11-29 | 株式会社武藏野化学研究所 | 丙交酯的提纯方法 |
JPH1025288A (ja) * | 1996-07-12 | 1998-01-27 | Shimadzu Corp | ラクチドの精製法および重合法 |
KR20080018650A (ko) * | 2006-08-25 | 2008-02-28 | 성균관대학교산학협력단 | 광학적으로 순수한 락티드의 분리방법 |
CN101468978A (zh) * | 2007-12-27 | 2009-07-01 | 常熟市长江化纤有限公司 | 丙交酯的提纯方法 |
CN101696204A (zh) * | 2009-10-13 | 2010-04-21 | 常熟市长江化纤有限公司 | 丙交酯的提纯方法 |
CN102875522A (zh) * | 2012-09-29 | 2013-01-16 | 上海绿色盛世生态材料有限公司 | 一种丙交酯的纯化方法 |
CN105646440A (zh) * | 2014-12-05 | 2016-06-08 | 中国石油化工股份有限公司 | 一种丙交酯的精制纯化方法 |
CN106397388A (zh) * | 2016-09-07 | 2017-02-15 | 南京大学 | 一种粗品环酯纯化制备高纯度环酯的工艺 |
CN110128397A (zh) * | 2019-06-12 | 2019-08-16 | 山东谷雨春生物科技有限公司 | 一种高纯度丙交酯的制备方法 |
-
2020
- 2020-10-28 CN CN202011169560.1A patent/CN114478470B/zh active Active
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1112559A (zh) * | 1993-12-08 | 1995-11-29 | 株式会社武藏野化学研究所 | 丙交酯的提纯方法 |
JPH1025288A (ja) * | 1996-07-12 | 1998-01-27 | Shimadzu Corp | ラクチドの精製法および重合法 |
KR20080018650A (ko) * | 2006-08-25 | 2008-02-28 | 성균관대학교산학협력단 | 광학적으로 순수한 락티드의 분리방법 |
CN101468978A (zh) * | 2007-12-27 | 2009-07-01 | 常熟市长江化纤有限公司 | 丙交酯的提纯方法 |
CN101696204A (zh) * | 2009-10-13 | 2010-04-21 | 常熟市长江化纤有限公司 | 丙交酯的提纯方法 |
CN102875522A (zh) * | 2012-09-29 | 2013-01-16 | 上海绿色盛世生态材料有限公司 | 一种丙交酯的纯化方法 |
CN105646440A (zh) * | 2014-12-05 | 2016-06-08 | 中国石油化工股份有限公司 | 一种丙交酯的精制纯化方法 |
CN106397388A (zh) * | 2016-09-07 | 2017-02-15 | 南京大学 | 一种粗品环酯纯化制备高纯度环酯的工艺 |
CN110128397A (zh) * | 2019-06-12 | 2019-08-16 | 山东谷雨春生物科技有限公司 | 一种高纯度丙交酯的制备方法 |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114853718A (zh) * | 2022-05-05 | 2022-08-05 | 广东粤港澳大湾区黄埔材料研究院 | L-丙交酯的纯化方法 |
CN114853718B (zh) * | 2022-05-05 | 2024-03-26 | 广东粤港澳大湾区黄埔材料研究院 | L-丙交酯的纯化方法 |
CN116041314A (zh) * | 2023-02-08 | 2023-05-02 | 新沂市永诚化工有限公司 | 一种粗品环酯纯化制备高纯度环酯的工艺 |
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Publication number | Publication date |
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CN114478470B (zh) | 2024-04-19 |
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Effective date of registration: 20240325 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Country or region after: China Applicant after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Country or region before: China Applicant before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |
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