CN103467307B - The application of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction - Google Patents
The application of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction Download PDFInfo
- Publication number
- CN103467307B CN103467307B CN201310425173.3A CN201310425173A CN103467307B CN 103467307 B CN103467307 B CN 103467307B CN 201310425173 A CN201310425173 A CN 201310425173A CN 103467307 B CN103467307 B CN 103467307B
- Authority
- CN
- China
- Prior art keywords
- antioxidant
- application
- bulk powder
- dichlorphenamide bulk
- reaction
- 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.)
- Active
Links
Abstract
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, 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
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:
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 2,5-dichlorphenamide bulk powder 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 2,5-dichlorphenamide bulk powder 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.
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 2,5-dichlorphenamide bulk powder 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: 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, carry out being obtained by reacting the finished product 2,5-dichlorphenamide bulk powder 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.
Embodiment
React in the still kettle of 2,5-dichlorphenamide bulk powder mixtures 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 in without cutout situation every still 12-18 hours as well.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. an antioxidant is 2, application in 5-dichlorphenamide bulk powder distillation reaction, under its technique is: 2, after 5-dichloronitrobenzene and hydrogen reaction complete, by the crude product 2 generated, 5-dichlorphenamide bulk powder and antioxidant add in still kettle simultaneously, carry out being obtained by reacting the finished product 2,5-dichlorphenamide bulk powder in still-process; It is characterized in that: described antioxidant composition is Sodium Sulphide, its concentration is 0.1%.
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: 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 |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103467307A CN103467307A (en) | 2013-12-25 |
| CN103467307B true CN103467307B (en) | 2016-01-06 |
Family
ID=49792388
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103467307B (en) |
Families Citing this family (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 |
-
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 |
|---|
| 二氯苯胺柔性生产技术研究;蔡春;《南京理工大学学报》;20000630;第24卷(第3期);第219-222页 * |
| 催化加氢制备对苯二胺工艺的研究;唐琴;《氯碱工业》;20100930;第46卷(第9期);第23-29页 * |
| 对氟苯胺的合成;徐德忠;《氟化工》;20071231;第14卷(第1期);第4-7页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103467307A (en) | 2013-12-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104445276B (en) | A kind of efficient method preparing cyanamide solution | |
| CN103467245B (en) | Method for complexing and removing water contained in ethanol and water mixed solution by utilizing eutectic solvent | |
| CN103584064B (en) | A kind of containing soy sauce residues soya sauce and production method thereof | |
| CN105368090B (en) | Reduce the preparation method of the caramel colorant of 4 methylimidazole contents | |
| CN103073388B (en) | Method for separating alcohol from water through ion liquid extraction and rectification | |
| CN103709783A (en) | Production process of caramel color | |
| CN105086503A (en) | Common-process production technique of caramel color with color ratio of at least 30000EBC | |
| CN108113047A (en) | It is a kind of to be used to improve the method that the high pressure of thin section for tobacco quality is modified stem extracting solution | |
| CN103467307B (en) | The application of a kind of antioxidant in 2,5-dichlorphenamide bulk powder distillation reaction | |
| CN111269145A (en) | Preparation method of acetamidine hydrochloride | |
| CN103467302B (en) | The application of a kind of antioxidant in p-Chlorobenzoic acid amide distillation reaction | |
| CN102408673B (en) | Epoxidized soybean oil modified phenolic resin and method for producing non-fire-retardant paper based copper clad laminate by using same | |
| CN103664803A (en) | Novel synthesis method of 2, 3, 5, 6-tetramethylpyrazine | |
| CN106083673A (en) | A kind of preparation technology of carbocisteine | |
| CN104621530B (en) | A kind of preparation method of soy sauce | |
| CN105271143A (en) | Recycling and treatment technology for hydroxylamine hydrochloride mother liquor | |
| CN102303887B (en) | Production method for special strontium chloride for liquid crystal | |
| CN106811297A (en) | A kind of preparation method of thermal response tobacco aromaticss with tobacco fruity note and its application in cigarette | |
| CN103740129A (en) | Preparation process of low 4-methylimidazole caramel pigment | |
| CN105295242A (en) | Hydrotalcite composite environmental protection stabilizer for PVC, and preparation method thereof | |
| CN105289210A (en) | Ammonia-carbon separation process | |
| CN102618198B (en) | A kind of modified urea-formaldehyde glue and preparation method thereof | |
| CN107915665A (en) | A kind of preparation method of thermo-sensitive material D 8 | |
| CN107033309A (en) | A kind of preparation method of fiberboard adhesive | |
| CN103932982B (en) | A kind of method controlling alanyl-glutamine injection its related substances |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |