CN1948258A - 乙酰氯联产羟基亚乙基二膦酸的制备方法及装置 - Google Patents
乙酰氯联产羟基亚乙基二膦酸的制备方法及装置 Download PDFInfo
- Publication number
- CN1948258A CN1948258A CN 200610097146 CN200610097146A CN1948258A CN 1948258 A CN1948258 A CN 1948258A CN 200610097146 CN200610097146 CN 200610097146 CN 200610097146 A CN200610097146 A CN 200610097146A CN 1948258 A CN1948258 A CN 1948258A
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- Prior art keywords
- acetyl chloride
- kettle
- tower
- reaction kettle
- temperature
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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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- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000012346 acetyl chloride Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VPTUPAVOBUEXMZ-UHFFFAOYSA-N (1-hydroxy-2-phosphonoethyl)phosphonic acid Chemical compound OP(=O)(O)C(O)CP(O)(O)=O VPTUPAVOBUEXMZ-UHFFFAOYSA-N 0.000 title 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 148
- 238000006243 chemical reaction Methods 0.000 claims abstract description 64
- 229960000583 acetic acid Drugs 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 33
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000009833 condensation Methods 0.000 claims abstract description 17
- 230000005494 condensation Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- MXPRZOBRBIVDGQ-UHFFFAOYSA-N C(C)(=O)O.P1(=O)OC(CO)OP(O1)=O Chemical compound C(C)(=O)O.P1(=O)OC(CO)OP(O1)=O MXPRZOBRBIVDGQ-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000010521 absorption reaction Methods 0.000 claims description 59
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 56
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 39
- 230000007062 hydrolysis Effects 0.000 claims description 31
- 238000006460 hydrolysis reaction Methods 0.000 claims description 31
- 238000010025 steaming Methods 0.000 claims description 24
- 238000010992 reflux Methods 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 22
- LGDNGCWFLSOZDD-UHFFFAOYSA-N acetic acid (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound C(C)(=O)O.OCC(P(O)(O)=O)P(O)(O)=O LGDNGCWFLSOZDD-UHFFFAOYSA-N 0.000 claims description 20
- 239000011552 falling film Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000011010 flushing procedure Methods 0.000 claims description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 15
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 239000002351 wastewater Substances 0.000 claims description 8
- 239000012267 brine Substances 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 238000004042 decolorization Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 3
- URWIWRCHIPAGBL-UHFFFAOYSA-N OCC1OP(=O)OP(=O)O1 Chemical compound OCC1OP(=O)OP(=O)O1 URWIWRCHIPAGBL-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 20
- 239000000047 product Substances 0.000 description 20
- 239000002994 raw material Substances 0.000 description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- 229910052698 phosphorus Inorganic materials 0.000 description 8
- 239000011574 phosphorus Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 6
- 239000006096 absorbing agent Substances 0.000 description 5
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 5
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 238000003965 capillary gas chromatography Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- FAKJFAMIABOKBW-UHFFFAOYSA-N 1-(2,4-dichloro-5-fluorophenyl)ethanone Chemical compound CC(=O)C1=CC(F)=C(Cl)C=C1Cl FAKJFAMIABOKBW-UHFFFAOYSA-N 0.000 description 1
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- UKASRNSYWPGSDQ-UHFFFAOYSA-N acetic acid;trichlorophosphane Chemical compound CC(O)=O.ClP(Cl)Cl UKASRNSYWPGSDQ-UHFFFAOYSA-N 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 125000003668 acetyloxy group Chemical group [H]C([H])([H])C(=O)O[*] 0.000 description 1
- 230000010933 acylation Effects 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229960001680 ibuprofen Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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CNB2006100971468A CN100443459C (zh) | 2006-10-28 | 2006-10-28 | 乙酰氯联产羟基亚乙基二膦酸的制备方法及装置 |
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CNB2006100971468A CN100443459C (zh) | 2006-10-28 | 2006-10-28 | 乙酰氯联产羟基亚乙基二膦酸的制备方法及装置 |
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CN1948258A true CN1948258A (zh) | 2007-04-18 |
CN100443459C CN100443459C (zh) | 2008-12-17 |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101386628B (zh) * | 2008-10-29 | 2010-12-15 | 河南清水源科技股份有限公司 | 砷含量≤3ppm的羟基亚乙基二膦酸及其制取工艺 |
WO2011023280A1 (en) * | 2009-08-28 | 2011-03-03 | Synthon B.V. | Process for making 1-hydroxyalkylidene-1,1-biphosphonic acids |
CN102278868A (zh) * | 2011-08-02 | 2011-12-14 | 济南圣泉集团股份有限公司 | 异硫氰酸酯制备中的废气回收工艺及装置 |
CN103570760A (zh) * | 2013-11-25 | 2014-02-12 | 山东化友化学有限公司 | 羟基亚乙基二膦酸生产方法 |
CN106366124A (zh) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | 一种利用乙酰氯废液制备羟基亚乙基二膦酸的生产工艺 |
CN107602611A (zh) * | 2017-09-11 | 2018-01-19 | 南通意特化工有限公司 | 一种利用乙酰氯废液制备羟基亚乙基二膦酸的生产工艺 |
CN109956969A (zh) * | 2019-04-25 | 2019-07-02 | 山东泰和水处理科技股份有限公司 | 一种羟基亚乙基二膦酸的制备方法 |
CN111318244A (zh) * | 2020-02-26 | 2020-06-23 | 青岛长荣化工科技有限公司 | 一种膦酸酯水解装置及方法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1043044C (zh) * | 1993-02-16 | 1999-04-21 | 化学工业部天津化工研究院 | 羟基乙叉二膦酸的生产方法 |
CN1616469A (zh) * | 2004-09-20 | 2005-05-18 | 张益军 | 羟基乙叉二膦酸联产乙酰氯的方法 |
-
2006
- 2006-10-28 CN CNB2006100971468A patent/CN100443459C/zh not_active Expired - Fee Related
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101386628B (zh) * | 2008-10-29 | 2010-12-15 | 河南清水源科技股份有限公司 | 砷含量≤3ppm的羟基亚乙基二膦酸及其制取工艺 |
WO2011023280A1 (en) * | 2009-08-28 | 2011-03-03 | Synthon B.V. | Process for making 1-hydroxyalkylidene-1,1-biphosphonic acids |
CN102278868A (zh) * | 2011-08-02 | 2011-12-14 | 济南圣泉集团股份有限公司 | 异硫氰酸酯制备中的废气回收工艺及装置 |
CN103570760A (zh) * | 2013-11-25 | 2014-02-12 | 山东化友化学有限公司 | 羟基亚乙基二膦酸生产方法 |
CN103570760B (zh) * | 2013-11-25 | 2015-12-09 | 山东化友化学有限公司 | 羟基亚乙基二膦酸生产设备及其方法 |
CN106366124A (zh) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | 一种利用乙酰氯废液制备羟基亚乙基二膦酸的生产工艺 |
CN107602611A (zh) * | 2017-09-11 | 2018-01-19 | 南通意特化工有限公司 | 一种利用乙酰氯废液制备羟基亚乙基二膦酸的生产工艺 |
CN109956969A (zh) * | 2019-04-25 | 2019-07-02 | 山东泰和水处理科技股份有限公司 | 一种羟基亚乙基二膦酸的制备方法 |
CN111318244A (zh) * | 2020-02-26 | 2020-06-23 | 青岛长荣化工科技有限公司 | 一种膦酸酯水解装置及方法 |
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CN100443459C (zh) | 2008-12-17 |
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Application publication date: 20070418 Assignee: Nanjing Chemical Engineering Institute Changzhou Wujin Water Quality Stabilizer Factory Assignor: Zhou Hui Contract record no.: 2010320000097 Denomination of invention: Preparation method and device of acetyl chloride and hydroxy ethylene diphosphonic acid coproduction Granted publication date: 20081217 License type: Exclusive License Record date: 20100222 |
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Effective date of registration: 20171114 Address after: 213000, No. 3, building 65, No. 1206 Guan Zhong Road, Tianning District, Changzhou, Jiangsu Patentee after: Changzhou technology and Trade Co., Ltd. Xiao boat Address before: 213119 Hengshan City, Changzhou province Wujin district town of stars village Patentee before: Zhou Hui |
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