CN107903179A - 从ae‑活性酯母液中回收三乙胺和磷酸三乙酯的方法 - Google Patents
从ae‑活性酯母液中回收三乙胺和磷酸三乙酯的方法 Download PDFInfo
- Publication number
- CN107903179A CN107903179A CN201711182112.3A CN201711182112A CN107903179A CN 107903179 A CN107903179 A CN 107903179A CN 201711182112 A CN201711182112 A CN 201711182112A CN 107903179 A CN107903179 A CN 107903179A
- Authority
- CN
- China
- Prior art keywords
- triethylamine
- triethyl phosphate
- recycled
- methoxyiminoacetic
- thiazolyl
- 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.)
- Granted
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 title claims abstract description 120
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 150000002148 esters Chemical class 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012452 mother liquor Substances 0.000 claims abstract description 15
- 239000012074 organic phase Substances 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- COFDRZLHVALCDU-LICLKQGHSA-N s-(1,3-benzothiazol-2-yl) (2e)-2-(2-amino-1,3-thiazol-4-yl)-2-methoxyiminoethanethioate Chemical compound N=1C2=CC=CC=C2SC=1SC(=O)/C(=N/OC)C1=CSC(N)=N1 COFDRZLHVALCDU-LICLKQGHSA-N 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 7
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 13
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N dichloromethane Natural products ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- -1 dichloromethane Alkane Chemical class 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 3
- 229930186147 Cephalosporin Natural products 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229940124587 cephalosporin Drugs 0.000 description 2
- 150000001780 cephalosporins Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- AZZMGZXNTDTSME-JUZDKLSSSA-M cefotaxime sodium Chemical compound [Na+].N([C@@H]1C(N2C(=C(COC(C)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CSC(N)=N1 AZZMGZXNTDTSME-JUZDKLSSSA-M 0.000 description 1
- 229960002727 cefotaxime sodium Drugs 0.000 description 1
- DKOQGJHPHLTOJR-WHRDSVKCSA-N cefpirome Chemical compound N([C@@H]1C(N2C(=C(C[N+]=3C=4CCCC=4C=CC=3)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CSC(N)=N1 DKOQGJHPHLTOJR-WHRDSVKCSA-N 0.000 description 1
- 229960000466 cefpirome Drugs 0.000 description 1
- 229960004755 ceftriaxone Drugs 0.000 description 1
- VAAUVRVFOQPIGI-SPQHTLEESA-N ceftriaxone Chemical compound S([C@@H]1[C@@H](C(N1C=1C(O)=O)=O)NC(=O)\C(=N/OC)C=2N=C(N)SC=2)CC=1CSC1=NC(=O)C(=O)NN1C VAAUVRVFOQPIGI-SPQHTLEESA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims (6)
Priority Applications (1)
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CN201711182112.3A CN107903179B (zh) | 2017-11-23 | 2017-11-23 | 从ae-活性酯母液中回收三乙胺和磷酸三乙酯的方法 |
Applications Claiming Priority (1)
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CN201711182112.3A CN107903179B (zh) | 2017-11-23 | 2017-11-23 | 从ae-活性酯母液中回收三乙胺和磷酸三乙酯的方法 |
Publications (2)
Publication Number | Publication Date |
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CN107903179A true CN107903179A (zh) | 2018-04-13 |
CN107903179B CN107903179B (zh) | 2020-06-09 |
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CN201711182112.3A Active CN107903179B (zh) | 2017-11-23 | 2017-11-23 | 从ae-活性酯母液中回收三乙胺和磷酸三乙酯的方法 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108640844A (zh) * | 2018-05-09 | 2018-10-12 | 国药集团威奇达药业有限公司 | 从工业废水中回收三乙胺的方法 |
CN109052356A (zh) * | 2018-08-09 | 2018-12-21 | 上海应用技术大学 | 一种ae活性酯生产过程产生的含磷残液中磷的分离方法 |
Citations (10)
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CN1552700A (zh) * | 2003-05-30 | 2004-12-08 | 宜兴市化学厂 | 一种苯骈噻唑活性酯合成方法 |
CN101602726A (zh) * | 2009-07-20 | 2009-12-16 | 渤海大学 | 一种12H-苯并[4,5]卓酮并[1,2-b]喹啉类化合物及制备方法 |
CN102060861A (zh) * | 2010-11-04 | 2011-05-18 | 浙江工业大学 | 一种头孢母液的脱盐浓缩方法 |
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CN104387337A (zh) * | 2014-12-15 | 2015-03-04 | 山东鑫泉医药有限公司 | Ae-活性酯残渣合成3-乙基-2-硫乙基苯并噻唑高氯酸盐的方法 |
CN104628199A (zh) * | 2015-01-15 | 2015-05-20 | 珠海保税区丽珠合成制药有限公司 | 一种头孢合成制药生产废水的处理方法 |
CN104803503A (zh) * | 2015-01-15 | 2015-07-29 | 珠海保税区丽珠合成制药有限公司 | 一种头孢合成制药生产废水的处理装置 |
CN107236000A (zh) * | 2017-06-06 | 2017-10-10 | 池正伟 | 磷酸三苯酯的回收方法 |
-
2017
- 2017-11-23 CN CN201711182112.3A patent/CN107903179B/zh active Active
Patent Citations (10)
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CN1552700A (zh) * | 2003-05-30 | 2004-12-08 | 宜兴市化学厂 | 一种苯骈噻唑活性酯合成方法 |
CN101602726A (zh) * | 2009-07-20 | 2009-12-16 | 渤海大学 | 一种12H-苯并[4,5]卓酮并[1,2-b]喹啉类化合物及制备方法 |
CN102060861A (zh) * | 2010-11-04 | 2011-05-18 | 浙江工业大学 | 一种头孢母液的脱盐浓缩方法 |
CN102702233A (zh) * | 2012-05-18 | 2012-10-03 | 苏州中联化学制药有限公司 | 头孢曲松钠的制备方法 |
CN102911202A (zh) * | 2012-10-10 | 2013-02-06 | 山东金城医药化工股份有限公司 | 从ae渣中回收磷酸三乙酯的方法 |
CN104086438A (zh) * | 2014-06-30 | 2014-10-08 | 浙江中山化工集团股份有限公司 | 一种甲基磺草酮溶剂回收工艺 |
CN104387337A (zh) * | 2014-12-15 | 2015-03-04 | 山东鑫泉医药有限公司 | Ae-活性酯残渣合成3-乙基-2-硫乙基苯并噻唑高氯酸盐的方法 |
CN104628199A (zh) * | 2015-01-15 | 2015-05-20 | 珠海保税区丽珠合成制药有限公司 | 一种头孢合成制药生产废水的处理方法 |
CN104803503A (zh) * | 2015-01-15 | 2015-07-29 | 珠海保税区丽珠合成制药有限公司 | 一种头孢合成制药生产废水的处理装置 |
CN107236000A (zh) * | 2017-06-06 | 2017-10-10 | 池正伟 | 磷酸三苯酯的回收方法 |
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李爱军等: "2-(2-氨基噻唑-4-基)-2-(Z)-甲氧亚胺基乙酸苯并噻唑硫酯合成工艺的改进", 《精细化工》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108640844A (zh) * | 2018-05-09 | 2018-10-12 | 国药集团威奇达药业有限公司 | 从工业废水中回收三乙胺的方法 |
CN109052356A (zh) * | 2018-08-09 | 2018-12-21 | 上海应用技术大学 | 一种ae活性酯生产过程产生的含磷残液中磷的分离方法 |
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Publication number | Publication date |
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CN107903179B (zh) | 2020-06-09 |
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Effective date of registration: 20200811 Address after: 256100 Yiyuan Economic Development Zone, Shandong, Zibo Patentee after: SHANDONG XINQUAN PHARMACEUTICAL Co.,Ltd. Address before: 256100 Yiyuan Economic Development Zone, Shandong, Zibo Patentee before: ZIBO XINQUAN PHARMACEUTICAL TECHNOLOGY SERVICE Co.,Ltd. |
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Denomination of invention: Method for recovering triethylamine and triethyl phosphate from AE active ester mother liquor Effective date of registration: 20211216 Granted publication date: 20200609 Pledgee: Commercial Bank of China Yiyuan branch of Limited by Share Ltd. Pledgor: SHANDONG XINQUAN PHARMACEUTICAL Co.,Ltd. Registration number: Y2021980015204 |
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Date of cancellation: 20220721 Granted publication date: 20200609 Pledgee: Commercial Bank of China Yiyuan branch of Limited by Share Ltd. Pledgor: SHANDONG XINQUAN PHARMACEUTICAL Co.,Ltd. Registration number: Y2021980015204 |
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Denomination of invention: Method for recovering triethylamine and triethyl phosphate from AE-active ester mother liquor Effective date of registration: 20221231 Granted publication date: 20200609 Pledgee: Agricultural Bank of China Limited by Share Ltd. Yiyuan county subbranch Pledgor: SHANDONG XINQUAN PHARMACEUTICAL Co.,Ltd. Registration number: Y2022980029922 |
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