CN103467302B - The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction - Google Patents
The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction Download PDFInfo
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- CN103467302B CN103467302B CN201310425113.1A CN201310425113A CN103467302B CN 103467302 B CN103467302 B CN 103467302B CN 201310425113 A CN201310425113 A CN 201310425113A CN 103467302 B CN103467302 B CN 103467302B
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- Prior art keywords
- antioxidant
- acid amide
- chlorobenzoic acid
- application
- reaction
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- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 27
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 19
- BLNVISNJTIRAHF-UHFFFAOYSA-N 4-chlorobenzamide Chemical compound NC(=O)C1=CC=C(Cl)C=C1 BLNVISNJTIRAHF-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000004821 distillation Methods 0.000 title claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 4
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000012043 crude product Substances 0.000 claims abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 3
- 239000001257 hydrogen Substances 0.000 claims abstract description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract description 2
- 231100000419 toxicity Toxicity 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000003039 volatile agent Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction, its processing step is as follows: after para-nitrochloro-benzene and hydrogen reaction complete, the crude product p-Chlorobenzoic acid amide generated and antioxidant add in still kettle simultaneously, carry out being obtained by reacting the finished product p-Chlorobenzoic acid amide in still-process.Described antioxidant composition is Sodium Sulphide, and its concentration is 0.1%.The temperature of described distillation reaction is 130 DEG C, and in reaction process, pH value is 10-11.The invention has the advantages that: the application of this kind of antioxidant is compared with other antioxidant, and stability is better, good heat resistance, and oxidation-resistance effect, can preserve color and the outward appearance of material for a long time.Application art of the present invention is simple, and production cost is low, and toxicity is little, and product antioxidant effect is good, is applicable to green industrialized production.
Description
One, technical field
The present invention relates to a kind of technique of producing fine-chemical intermediate, the specifically application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction.
Two, background technology
Product generation oxygenizement avoided by antioxidant, slows down or prevent the material of oxygenizement.Antioxidant uses the change that can not make product that color and outward appearance occur because of rotten to affect the finished product yield.Distillation is a kind of thermodynamic (al) separating technology, and it utilizes each component boiling point in mixing liquid or liquid-solid system different, low boiling component is evaporated, then condensation is to be separated the unit process of whole component, is the associating of evaporation and condensation two kinds of unit operations.In still-process, can there is color and apparent change in material, be in fact there occurs oxidizing reaction, has and have a strong impact on, productive rate can be caused to decline after oxidation to the color and luster of product and face shaping, and income reduces.In production p-Chlorobenzoic acid amide still-process, need to add antioxidant, prevent material generation color and apparent change, to reduce in storage and the oxygenizement in using.In the past, produce antioxidant and the method thereof of p-Chlorobenzoic acid amide application, although play certain antioxidant effect to product, because thermotolerance is bad, poor stability, oxidation-resistance less effective, can not preserve color and the outward appearance of material for a long time.
Three, summary of the invention
In order to overcome deficiency of the prior art, the object of this invention is to provide the application method of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction, material color and outward appearance can be preserved for a long time.
The technical scheme realizing object of the present invention employing is: the application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction, its processing step is as follows: after para-nitrochloro-benzene and hydrogen reaction complete, the crude product p-Chlorobenzoic acid amide generated and antioxidant add in still kettle simultaneously, carry out being obtained by reacting the finished product p-Chlorobenzoic acid amide in still-process.
Described antioxidant composition is Sodium Sulphide (also claiming sodium sulphite), and its concentration is 0.1%.Sodium Sulphide is a kind of inorganic reducing agent, has good oxidation-resistance in the present invention.
The temperature of described distillation reaction is 130 DEG C, and in reaction process, pH value is 10-11.
The invention has the advantages that: the application of this kind of antioxidant is compared with other antioxidant, and stability is better, good heat resistance, and oxidation-resistance effect, can preserve color and the outward appearance of material for a long time.Application art of the present invention is simple, and production cost is low, and toxicity is little, and product antioxidant effect is good, is applicable to green industrialized production.
Four, embodiment
React in the still kettle of p-Chlorobenzoic acid amide mixture that certain content is housed, open steam valve and be warming up to about 140 DEG C to rectifying still, ensure more than vapor pressure 4kg.Sampled by thief hole when backflow appears in attic visor, detect PH.According to the input amount of pH value determination antioxidant, add antioxidant, open and stir.After there is backflow in backflow visor, total reflux 1 hour.A small amount of unlatching front-end volatiles extraction valve, produced quantity is observed by visor, heated up in a steamer normal extraction after can adopting a little bigger 3 hours (produced quantity be have a fine rule in visor or under having liquid stream along Jing Bi) extraction front-end volatiles before initial stage not too fast, control at every still 12-18 hour as well in without cutout situation.Analyze qualified after, close front-end volatiles extraction valve; Open finished product extraction valve, produced quantity controls have backflow to occur at backflow visor, and feed liquid color is colourless.(during as feed liquid color exception, reduce produced quantity, guarantee quality product), when feed liquid in rectifying still is touched less than material to stirring slurries, reaction terminates.The p-Chlorobenzoic acid amide yield that this application method obtains is 99.8%.
Claims (2)
1. the application of antioxidant in p-Chlorobenzoic acid amide distillation reaction, its technique is after para-nitrochloro-benzene and hydrogen reaction complete, the crude product p-Chlorobenzoic acid amide generated and antioxidant add in still kettle simultaneously, carry out being obtained by reacting the finished product p-Chlorobenzoic acid amide in still-process; It is characterized in that: described antioxidant composition is sodium sulphite, its concentration is 0.1%.
2. the application of a kind of antioxidant as claimed in claim 1 in p-Chlorobenzoic acid amide distillation reaction, is characterized in that: the temperature of described distillation reaction is 130 DEG C, and in reaction process, pH value is 10-11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310425113.1A CN103467302B (en) | 2013-09-18 | 2013-09-18 | The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310425113.1A CN103467302B (en) | 2013-09-18 | 2013-09-18 | The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction |
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| Publication Number | Publication Date |
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| CN103467302A CN103467302A (en) | 2013-12-25 |
| CN103467302B true CN103467302B (en) | 2015-08-26 |
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| CN201310425113.1A Active CN103467302B (en) | 2013-09-18 | 2013-09-18 | The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction |
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| CN108218719A (en) * | 2017-12-23 | 2018-06-29 | 杨向党 | A kind of method for being not added with antioxidant continuous rectification parachloroanilinum |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141912A (en) * | 1996-05-09 | 1997-02-05 | 河南省科学院化学研究所 | Preparation aromatic amine compound |
| CN1196831C (en) * | 2001-11-21 | 2005-04-13 | 简琼国际有限公司 | Dyeing process of finished clothes |
| WO2010107404A1 (en) * | 2009-03-16 | 2010-09-23 | Mahmut Bilgic | Stable pharmaceutical combinations |
| CN101879404A (en) * | 2010-07-12 | 2010-11-10 | 华东理工大学 | A resource-based flue gas desulfurization and denitrification method |
-
2013
- 2013-09-18 CN CN201310425113.1A patent/CN103467302B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141912A (en) * | 1996-05-09 | 1997-02-05 | 河南省科学院化学研究所 | Preparation aromatic amine compound |
| CN1196831C (en) * | 2001-11-21 | 2005-04-13 | 简琼国际有限公司 | Dyeing process of finished clothes |
| WO2010107404A1 (en) * | 2009-03-16 | 2010-09-23 | Mahmut Bilgic | Stable pharmaceutical combinations |
| CN101879404A (en) * | 2010-07-12 | 2010-11-10 | 华东理工大学 | A resource-based flue gas desulfurization and denitrification method |
Non-Patent Citations (1)
| Title |
|---|
| 对氟苯胺的合成;徐德忠;《化工生产与技术》;20071231;第14卷(第1期);第4-6页 * |
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| CN103467302A (en) | 2013-12-25 |
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