CN109293524A - 一种高纯度双丙酮丙烯酰胺的制备方法 - Google Patents
一种高纯度双丙酮丙烯酰胺的制备方法 Download PDFInfo
- Publication number
- CN109293524A CN109293524A CN201710612629.5A CN201710612629A CN109293524A CN 109293524 A CN109293524 A CN 109293524A CN 201710612629 A CN201710612629 A CN 201710612629A CN 109293524 A CN109293524 A CN 109293524A
- Authority
- CN
- China
- Prior art keywords
- diacetone acrylamide
- purity
- added
- preparation
- diacetone
- 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
Links
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 41
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 25
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims abstract description 25
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012043 crude product Substances 0.000 claims abstract description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000005194 fractionation Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003208 petroleum Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000013517 stratification Methods 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 239000012044 organic layer Substances 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000012452 mother liquor Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 239000002994 raw material Substances 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- SHOJXDKTYKFBRD-UHFFFAOYSA-N 4-Methyl-3-penten-2-one, 9CI Chemical compound CC(C)=CC(C)=O SHOJXDKTYKFBRD-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- -1 becomes easy drying Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/06—Preparation of carboxylic acid amides from nitriles by transformation of cyano groups into carboxamide groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims (6)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710612629.5A CN109293524B (zh) | 2017-07-25 | 2017-07-25 | 一种高纯度双丙酮丙烯酰胺的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710612629.5A CN109293524B (zh) | 2017-07-25 | 2017-07-25 | 一种高纯度双丙酮丙烯酰胺的制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN109293524A true CN109293524A (zh) | 2019-02-01 |
CN109293524B CN109293524B (zh) | 2021-08-17 |
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Family Applications (1)
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CN201710612629.5A Active CN109293524B (zh) | 2017-07-25 | 2017-07-25 | 一种高纯度双丙酮丙烯酰胺的制备方法 |
Country Status (1)
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CN (1) | CN109293524B (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112194593A (zh) * | 2020-10-23 | 2021-01-08 | 安徽梁溪环保新材料有限公司 | 双丙酮丙烯酰胺制备中硫酸盐采用氢氧化镁於浆中和方法 |
CN115501839A (zh) * | 2022-10-24 | 2022-12-23 | 广饶瑞尚化工有限公司 | 一种双丙酮丙烯酰胺的合成工艺 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1982839A1 (en) * | 2007-03-27 | 2008-10-22 | FUJIFILM Corporation | Heat-sensitive transfer image-forming method |
WO2008138856A1 (en) * | 2007-05-11 | 2008-11-20 | Dsm Fine Chemicals Austria Nfg Gmbh & Co Kg | Improved process for working up diacetone acrylamide solutions for the preparation of pure diacetone acrylamide |
CN104030939A (zh) * | 2014-07-02 | 2014-09-10 | 山东天一化学股份有限公司 | 一种采用双丙酮醇制备双丙酮丙烯酰胺的方法 |
CN104262190A (zh) * | 2014-08-25 | 2015-01-07 | 安徽梁溪环保新材料有限公司 | 一种水性环保涂料骨料的生产工艺 |
CN106117074A (zh) * | 2016-07-07 | 2016-11-16 | 张华堂 | 制备双丙酮丙烯酰胺的反应后处理方法 |
CN107652163A (zh) * | 2017-09-27 | 2018-02-02 | 荆楚理工学院 | 一种高纯甲基丙烯醇生产方法 |
-
2017
- 2017-07-25 CN CN201710612629.5A patent/CN109293524B/zh active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1982839A1 (en) * | 2007-03-27 | 2008-10-22 | FUJIFILM Corporation | Heat-sensitive transfer image-forming method |
WO2008138856A1 (en) * | 2007-05-11 | 2008-11-20 | Dsm Fine Chemicals Austria Nfg Gmbh & Co Kg | Improved process for working up diacetone acrylamide solutions for the preparation of pure diacetone acrylamide |
CN104030939A (zh) * | 2014-07-02 | 2014-09-10 | 山东天一化学股份有限公司 | 一种采用双丙酮醇制备双丙酮丙烯酰胺的方法 |
CN104262190A (zh) * | 2014-08-25 | 2015-01-07 | 安徽梁溪环保新材料有限公司 | 一种水性环保涂料骨料的生产工艺 |
CN106117074A (zh) * | 2016-07-07 | 2016-11-16 | 张华堂 | 制备双丙酮丙烯酰胺的反应后处理方法 |
CN107652163A (zh) * | 2017-09-27 | 2018-02-02 | 荆楚理工学院 | 一种高纯甲基丙烯醇生产方法 |
Non-Patent Citations (3)
Title |
---|
XIAORUI LI,等: "Synthesis and characterization of self-crosslinked polyurethane/polyacrylate composite emulsion based on carbonyl–hydrazide reaction", 《JOURNAL POLYMER RESEARCH》 * |
司动磊,等: "双丙酮丙烯酰胺的合成", 《化工科技》 * |
王中华,等: "《油田化学品实用手册》", 31 July 2004, 中国石化出版社 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112194593A (zh) * | 2020-10-23 | 2021-01-08 | 安徽梁溪环保新材料有限公司 | 双丙酮丙烯酰胺制备中硫酸盐采用氢氧化镁於浆中和方法 |
CN115501839A (zh) * | 2022-10-24 | 2022-12-23 | 广饶瑞尚化工有限公司 | 一种双丙酮丙烯酰胺的合成工艺 |
Also Published As
Publication number | Publication date |
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CN109293524B (zh) | 2021-08-17 |
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Application publication date: 20190201 Assignee: Yunnan Benyi Biotechnology Co.,Ltd. Assignor: JINGCHU University OF TECHNOLOGY Contract record no.: X2023420000117 Denomination of invention: A Preparation Method of High Purity Diacetone Acrylamide Granted publication date: 20210817 License type: Common License Record date: 20230519 Application publication date: 20190201 Assignee: Yunnan Goudeli Biotechnology Co.,Ltd. Assignor: JINGCHU University OF TECHNOLOGY Contract record no.: X2023420000118 Denomination of invention: A Preparation Method of High Purity Diacetone Acrylamide Granted publication date: 20210817 License type: Common License Record date: 20230519 |
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Application publication date: 20190201 Assignee: Yunnan Weiqiang An Biotechnology Co.,Ltd. Assignor: JINGCHU University OF TECHNOLOGY Contract record no.: X2023420000119 Denomination of invention: A Preparation Method of High Purity Diacetone Acrylamide Granted publication date: 20210817 License type: Common License Record date: 20230522 Application publication date: 20190201 Assignee: Yunnan Benyi Lanche Environmental Protection Technology Co.,Ltd. Assignor: JINGCHU University OF TECHNOLOGY Contract record no.: X2023420000120 Denomination of invention: A Preparation Method of High Purity Diacetone Acrylamide Granted publication date: 20210817 License type: Common License Record date: 20230522 |
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