CN103467307A - Application of antioxidant in distillation reaction of 2, 5-dichloroaniline - Google Patents
Application of antioxidant in distillation reaction of 2, 5-dichloroaniline Download PDFInfo
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- CN103467307A CN103467307A CN2013104251733A CN201310425173A CN103467307A CN 103467307 A CN103467307 A CN 103467307A CN 2013104251733 A CN2013104251733 A CN 2013104251733A CN 201310425173 A CN201310425173 A CN 201310425173A CN 103467307 A CN103467307 A CN 103467307A
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Abstract
The invention relates to an application of an antioxidant in distillation reaction of 2, 5-dichloroaniline. The process comprises the following steps: simultaneously adding a generated crude product, namely the 2, 5-dichloroaniline and the antioxidant into a distillation kettle after the reaction of 2, 5-dichloronitrobenzene and hydrogen is completed and reacting during the distillation process to get a final product, namely p-chloroaniline. The antioxidant comprises the component of sodium sulfide, and the concentration is 0.1%. The temperature of the distillation reaction is 130 DEG C, and the pH value during the reaction process is 10-11. The application disclosed by the invention has the advantages that compared with other antioxidants, the application of the antioxidant has better stability, good heat resistance and good oxidation resistance, and can keep the color and the appearance of the material for a long time. The application disclosed by the invention further has the advantages of simple process, low production cost, low toxicity and good oxidation resistance of the product, and is suitable for green industrial production.
Description
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 2,5-dichlorphenamide bulk powder distillation reaction.
Background technology:
Antioxidant is to avoid product generation oxygenizement, slows down or prevent the material of oxygenizement.Antioxidant is used and can not make product affect the finished product yield because of the rotten change that color and outward appearance occur.Distillation is a kind of thermodynamic (al) separating technology, and it utilizes each component boiling point difference in mixing liquid or liquid-solid system, makes the low boiling component evaporation, then condensation is the associating of evaporation and two kinds of unit operations of condensation to separate the unit process of whole component.Color and apparent variation, in still-process, can occur in material, are in fact that oxidizing reaction has occurred, and after oxidation, the color and luster of product and face shaping are had and have a strong impact on, and can cause productive rate to descend, and income reduces.In producing 2,5-dichlorphenamide bulk powder still-process, need to add antioxidant, prevent material generation color and apparent variation, to reduce the oxygenizement in storing and using.In the past, produced antioxidant and the method thereof of 2,5-dichlorphenamide bulk powder application, although product is played to certain antioxidant effect, because thermotolerance is bad, poor stability, the oxidation-resistance effect is not good enough, color and outward appearance that can not the prolonged preservation material.
Summary of the invention
In order to overcome deficiency of the prior art, the purpose of this invention is to provide the application method of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction, can preserve for a long time material color and outward appearance.
Realize that the technical scheme that purpose of the present invention adopts is: a kind of antioxidant is 2, application in 5-dichlorphenamide bulk powder distillation reaction, its processing step is as follows: 2, after 5-dichloronitrobenzene and hydrogen reaction complete, the crude product 2 generated, 5-dichlorphenamide bulk powder and antioxidant add in still kettle simultaneously, react in still-process and obtain the finished product 2, the 5-dichlorphenamide bulk powder.
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 in the present invention good oxidation-resistance.
The temperature of described distillation reaction is 130 ℃, and in reaction process, the 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, oxidation-resistance effect, but the color of prolonged preservation material and outward appearance.Application art of the present invention is simple, and production cost is low, and toxicity is little, and the product antioxidant effect is good, is applicable to green industrialized production.
Embodiment
2 of certain content is being housed, is being reacted in the still kettle of 5-dichlorphenamide bulk powder mixture, opening steam valve and be warming up to 140 ℃ of left and right to rectifying still, more than guaranteeing vapor pressure 4kg.Sample by thief hole when refluxing appears in the attic visor, detect PH.Determine the input amount of antioxidant according to pH value, add antioxidant, open and stir.After refluxing appears in the backflow visor, total reflux 1 hour.A small amount of front-end volatiles extraction valve of opening, observe produced quantity by visor, heated up in a steamer before initial stage that can to adopt after a little bigger 3 hours normal extraction (produced quantity is a fine rule to be arranged in visor or have liquid to flow down along Jing Bi to get final product) extraction front-end volatiles not too fast, be controlled at every still 12-18 hours in without the cutout situation for well.Analyze qualified after, close front-end volatiles extraction valve; Open finished product extraction valve, produced quantity is controlled at the backflow visor the appearance of backflow, and the feed liquid color is colourless.(during as the feed liquid color exception, reduce produced quantity, guarantee quality product), in rectifying still, feed liquid is when stirring slurries and touch less than material, and reaction finishes.The p-Chlorobenzoic acid amide yield that this application method makes is 99.8%.
Claims (3)
1. an antioxidant is 2, application in 5-dichlorphenamide bulk powder distillation reaction, its processing step is as follows: after 2,5-dichloronitrobenzene and hydrogen reaction complete, the crude product p-Chlorobenzoic acid amide and the antioxidant that generate add in still kettle simultaneously, react in still-process and obtain the finished product p-Chlorobenzoic acid amide.
2. the application of a kind of antioxidant as claimed in claim 1 in 2,5-dichlorphenamide bulk powder distillation reaction is characterized in that: described antioxidant composition is Sodium Sulphide (also claiming sodium sulphite), and its concentration is 0.1%.
3. the application of a kind of antioxidant as claimed in claim 1 in 2,5-dichlorphenamide bulk powder distillation reaction, it is characterized in that: the temperature of described distillation reaction is 130 ℃, in reaction process, the pH value is 10-11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310425173.3A CN103467307B (en) | 2013-09-18 | 2013-09-18 | The application of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310425173.3A CN103467307B (en) | 2013-09-18 | 2013-09-18 | The application of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction |
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| Publication Number | Publication Date |
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| CN103467307A true CN103467307A (en) | 2013-12-25 |
| CN103467307B CN103467307B (en) | 2016-01-06 |
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| CN201310425173.3A Active CN103467307B (en) | 2013-09-18 | 2013-09-18 | The application of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10562841B2 (en) | 2015-10-01 | 2020-02-18 | Monsanto Technology Llc | Process for catalytic hydrogenation of halonitroaromatics |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289631A1 (en) * | 2009-12-29 | 2012-11-15 | Hyojin Lee | Aromatic diamine and method for manufacturing the same, and aramid fiber and method for manufacturing the same |
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2013
- 2013-09-18 CN CN201310425173.3A patent/CN103467307B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120289631A1 (en) * | 2009-12-29 | 2012-11-15 | Hyojin Lee | Aromatic diamine and method for manufacturing the same, and aramid fiber and method for manufacturing the same |
Non-Patent Citations (3)
| Title |
|---|
| 唐琴: "催化加氢制备对苯二胺工艺的研究", 《氯碱工业》 * |
| 徐德忠: "对氟苯胺的合成", 《氟化工》 * |
| 蔡春: "二氯苯胺柔性生产技术研究", 《南京理工大学学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10562841B2 (en) | 2015-10-01 | 2020-02-18 | Monsanto Technology Llc | Process for catalytic hydrogenation of halonitroaromatics |
| US11225454B2 (en) | 2015-10-01 | 2022-01-18 | Monsanto Technology Llc | Process for catalytic hydrogenation of halonitroaromatics |
| US11820725B2 (en) | 2015-10-01 | 2023-11-21 | Monsanto Technology Llc | Process for catalytic hydrogenation of halonitroaromatics |
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| Publication number | Publication date |
|---|---|
| CN103467307B (en) | 2016-01-06 |
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