CN113651699B - 层式熔融结晶制备高纯2,4-二硝基氯苯的方法 - Google Patents
层式熔融结晶制备高纯2,4-二硝基氯苯的方法 Download PDFInfo
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- CN113651699B CN113651699B CN202110895640.3A CN202110895640A CN113651699B CN 113651699 B CN113651699 B CN 113651699B CN 202110895640 A CN202110895640 A CN 202110895640A CN 113651699 B CN113651699 B CN 113651699B
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- Prior art keywords
- dinitrochlorobenzene
- product
- purity
- temperature
- heating
- 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.)
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- VYZAHLCBVHPDDF-UHFFFAOYSA-N Dinitrochlorobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C([N+]([O-])=O)=C1 VYZAHLCBVHPDDF-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002425 crystallisation Methods 0.000 title claims abstract description 13
- 230000008025 crystallization Effects 0.000 title claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 239000012043 crude product Substances 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 230000035900 sweating Effects 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims abstract description 3
- 239000007791 liquid phase Substances 0.000 claims abstract description 3
- 239000010413 mother solution Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 7
- 210000004243 sweat Anatomy 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract 2
- 239000000498 cooling water Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000006396 nitration reaction Methods 0.000 description 3
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims (2)
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CN202110895640.3A CN113651699B (zh) | 2021-08-05 | 2021-08-05 | 层式熔融结晶制备高纯2,4-二硝基氯苯的方法 |
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CN202110895640.3A CN113651699B (zh) | 2021-08-05 | 2021-08-05 | 层式熔融结晶制备高纯2,4-二硝基氯苯的方法 |
Publications (2)
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CN113651699A CN113651699A (zh) | 2021-11-16 |
CN113651699B true CN113651699B (zh) | 2023-11-21 |
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CN202110895640.3A Active CN113651699B (zh) | 2021-08-05 | 2021-08-05 | 层式熔融结晶制备高纯2,4-二硝基氯苯的方法 |
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Families Citing this family (1)
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CN114507112A (zh) * | 2022-02-25 | 2022-05-17 | 潍坊弘润新材料有限公司 | 一种高纯度均四甲苯的制备方法 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107721878A (zh) * | 2017-10-23 | 2018-02-23 | 天津大学 | 一种采用熔融结晶技术分离提纯丁二腈的方法 |
CN109134310A (zh) * | 2018-10-19 | 2019-01-04 | 天津科技大学 | 层式熔融结晶制备高纯苯胺基乙腈的方法 |
-
2021
- 2021-08-05 CN CN202110895640.3A patent/CN113651699B/zh active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107721878A (zh) * | 2017-10-23 | 2018-02-23 | 天津大学 | 一种采用熔融结晶技术分离提纯丁二腈的方法 |
CN109134310A (zh) * | 2018-10-19 | 2019-01-04 | 天津科技大学 | 层式熔融结晶制备高纯苯胺基乙腈的方法 |
Non-Patent Citations (3)
Title |
---|
Melt crystallization of 2,4-dinitrochlorobenzene: Purification and process parameters evaluation;Shengzhe Jia等;《Separation and Purification Technology》;第259卷;1-10 * |
Purification of 2,4-dinitrochlorobenzene using layer melt crystallization: Model and experiment;Shengzhe Jia等;《Separation andPurificationTechnology》;第270卷;1-10 * |
熊道陵 等.《洗油分离精制应用技术》.冶金工业出版社,2013,218页. * |
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