CN108383082B - 硝基甲烷水解制备盐酸羟胺的副产物分离装置和方法 - Google Patents
硝基甲烷水解制备盐酸羟胺的副产物分离装置和方法 Download PDFInfo
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- CN108383082B CN108383082B CN201810101228.8A CN201810101228A CN108383082B CN 108383082 B CN108383082 B CN 108383082B CN 201810101228 A CN201810101228 A CN 201810101228A CN 108383082 B CN108383082 B CN 108383082B
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- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000006227 byproduct Substances 0.000 title claims abstract description 21
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 230000007062 hydrolysis Effects 0.000 title claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 title claims description 10
- 238000000034 method Methods 0.000 title description 13
- 238000002360 preparation method Methods 0.000 title description 3
- 238000000605 extraction Methods 0.000 claims abstract description 157
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 68
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 35
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000019253 formic acid Nutrition 0.000 claims abstract description 34
- 239000012074 organic phase Substances 0.000 claims abstract description 33
- 239000012071 phase Substances 0.000 claims abstract description 31
- 238000011084 recovery Methods 0.000 claims abstract description 24
- 238000000746 purification Methods 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000005292 vacuum distillation Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 24
- 239000002253 acid Substances 0.000 abstract description 18
- 238000004821 distillation Methods 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 6
- 150000007513 acids Chemical class 0.000 abstract description 4
- 239000008346 aqueous phase Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 14
- 239000002699 waste material Substances 0.000 description 9
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 description 8
- 230000005484 gravity Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010812 mixed waste Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0731—Purification ; Separation of hydrogen chloride by extraction
- C01B7/0737—Purification ; Separation of hydrogen chloride by extraction hydrogen chloride being extracted
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Description
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CN201810101228.8A CN108383082B (zh) | 2018-02-01 | 2018-02-01 | 硝基甲烷水解制备盐酸羟胺的副产物分离装置和方法 |
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CN201810101228.8A CN108383082B (zh) | 2018-02-01 | 2018-02-01 | 硝基甲烷水解制备盐酸羟胺的副产物分离装置和方法 |
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CN108383082A CN108383082A (zh) | 2018-08-10 |
CN108383082B true CN108383082B (zh) | 2020-10-16 |
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Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108821938A (zh) * | 2018-08-06 | 2018-11-16 | 江苏沙星化工有限公司 | 一种制备4-氯-2-(三氟乙酰)-苯胺盐酸盐副产物的分离方法 |
CN114906812B (zh) * | 2022-06-01 | 2023-06-23 | 湖南吴赣药业有限公司 | 一种有机混酸分离纯化方法 |
Citations (2)
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CN106422810A (zh) * | 2016-10-17 | 2017-02-22 | 四川久润环保科技有限公司 | 一种热致相分离法制备中空纤维膜的后处理装置及方法 |
CN107474036A (zh) * | 2017-07-03 | 2017-12-15 | 湖北三里枫香科技有限公司 | 一种三聚甲醛生产工艺方法及萃取反应塔 |
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CN101585519B (zh) * | 2008-05-20 | 2011-07-27 | 上海化工研究院 | 15n-硝基甲烷水解制备15n-盐酸羟胺的方法 |
CN101487773B (zh) * | 2009-02-20 | 2011-09-14 | 同济大学 | 饮用水中消毒副产物三氯硝基甲烷的快速分析方法 |
CN103318858B (zh) * | 2013-06-07 | 2016-01-27 | 常州大学 | 一种利用反应-萃取蒸馏耦合技术制备羟胺盐的方法 |
US20160176782A1 (en) * | 2014-12-19 | 2016-06-23 | Uop Llc | Process and apparatus for improving light olefin yield from a fluid catalytic cracking process |
CN106946235B (zh) * | 2017-03-23 | 2019-03-22 | 北京凯瑞英科技有限公司 | 一种由硝基甲烷和盐酸通过相转移合成盐酸羟胺的方法 |
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2018
- 2018-02-01 CN CN201810101228.8A patent/CN108383082B/zh active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106422810A (zh) * | 2016-10-17 | 2017-02-22 | 四川久润环保科技有限公司 | 一种热致相分离法制备中空纤维膜的后处理装置及方法 |
CN107474036A (zh) * | 2017-07-03 | 2017-12-15 | 湖北三里枫香科技有限公司 | 一种三聚甲醛生产工艺方法及萃取反应塔 |
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Effective date of registration: 20191213 Address after: 100084, room 6, building 8, building 1, Zhongguancun East Road, Haidian District, Beijing, Applicant after: Beijing Chemical Reaction Engineering Science AND Technology Co., Ltd. Address before: 100084, room 6, building 8, building 1, Zhongguancun East Road, Haidian District, Beijing, Applicant before: Beijing Chemical Reaction Engineering Science AND Technology Co., Ltd. Applicant before: Shandong rui'ao Mstar Technology Ltd |
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Denomination of invention: Separation device and method for by-product of nitromethane hydrolysis to prepare hydroxylamine hydrochloride Effective date of registration: 20210727 Granted publication date: 20201016 Pledgee: Haihua International Financial Leasing Co.,Ltd. Pledgor: BEIJING CHEMICAL REACTION ENGINEERING SCIENCE & TECHNOLOGY Co.,Ltd. Registration number: Y2021990000651 |
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