CN100537505C - Production method for purifying 2,5-di-tert-butyl hydroquinone - Google Patents
Production method for purifying 2,5-di-tert-butyl hydroquinone Download PDFInfo
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- CN100537505C CN100537505C CNB2007101309188A CN200710130918A CN100537505C CN 100537505 C CN100537505 C CN 100537505C CN B2007101309188 A CNB2007101309188 A CN B2007101309188A CN 200710130918 A CN200710130918 A CN 200710130918A CN 100537505 C CN100537505 C CN 100537505C
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- ditert
- production method
- butyl hydroquinone
- butylhydro quinone
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Abstract
The present invention discloses a production method of purifying the 2, 5-two t-butyl hydroquinone; the 2, 5-two t-butyl hydroquinone is sent to be dried after being boiled in water with the traditional production method. The present invention is characterized in that the dried materials of the 2, 5-two t-butyl hydroquinone are respectively added with ethanol, phosphoric acid, zinc powder, and then the temperature is raised to be between 60 and 85 Celsius system; the temperature is kept for 30 to 60 minutes; the materials are pressed, filtered, cooled, crystallized, taken and mechanical centrifugally dried; then the materials are boiled in water, taken out and treated by rinsing with the hydrochloric acid of 30 to 36 percent; then the materials are taken out and centrifugal. After being dried by the fluidized bed, the qualified product can be made. The present invention lowers the phosphate and the compositions of insoluble impurities in the product; the content of the t-butyl hydroquinone in the 2, 5-two t-butyl hydroquinone is reduced to be less than or equal to 0.1 percent; the content of the hydroquinone is less than or equal to 0.05 percent; the content of the 2, 5-two t-butyl hydroquinone is as high as 99.5 percent. At the same time, the present invention changes the traditional oven into the fluidized bed for drying the materials, and avoids the defects of the caking, the hard breaking, and the inferior crystal model and so on.
Description
Technical field:
The present invention relates to a kind of production method of chemical industry series products, especially a kind of purification 2, the production method of 5-ditert-butylhydro quinone.
Background technology:
2, the 5-ditert-butylhydro quinone is widely used in industry such as synthetic rubber, plastics, resin; Be applicable to natural gum, synthetical glue and latex, the UV light absorber that modifications such as polyolefine and polyoxymethylene are used etc.; All kinds of rubber, developing material, resin, plastics, oils and tackiness agent etc.It is a kind of nontoxic, do not have bad smell, a free of contamination plastics inhibitor.As oxidation inhibitor, 2, the 5-ditert-butylhydro quinone makes the insatiable hunger polyester have satisfactory stability in production and storage.
Traditional production method is: with the Resorcinol and the trimethyl carbinol is that raw material dewaters under the liquid acid as catalyst and generates 2, the 5-ditert-butylhydro quinone, and in water, utilize a spot of Sodium Pyrosulfite to 2, the 5-ditert-butylhydro quinone is purified.
There is defective in traditional production method:
1, reduces Resorcinol and tertiarybutylhydroquinone content in the product with water-boiling method, improved 2, the content of 5-ditert-butylhydro quinone;
2, handle the antioxygen cycle that increases with Sodium Pyrosulfite, the outward appearance part can be turned to be yellow;
3, traditional processing technology adopts baking oven to dry to material, and material easily lumps, and hard broken, crystalline form is bad.
Summary of the invention
The object of the present invention is to provide a kind of above-mentioned shortcoming that overcomes, reduce by 2, the content of tertiarybutylhydroquinone in the 5-ditert-butylhydro quinone in the time of Resorcinol content, improves the outward appearance jaundice, sends out time; Reduce phosphoric acid salt and insoluble impurities composition in the product; A kind of purification 2 of defective such as avoid luming, hard fragmentation and crystalline form are bad, the production method of 5-ditert-butylhydro quinone.
For achieving the above object, the technical solution adopted in the present invention is: with 2, the 5-ditert-butylhydro quinone with traditional production method poach after, send dry by the fire siccative, it is characterized in that: get dry by the fire 2,5-ditert-butylhydro quinone siccative adds ethanol, phosphoric acid, zinc powder respectively, be warming up to 60-85 ℃, be incubated 30-60 minute; Press filtration while hot, cooling, crystallization, suction filtration, mechanical centrifuge dripping; Use traditional method poach, suction filtration once more, handle with 30-36% salt acid rinse, suction filtration is centrifugal; Through the fluidized-bed oven dry, get qualified product.
Described a kind of purification 2, the production method of 5-ditert-butylhydro quinone is characterized in that: the proportioning of weight of material is 2,5-ditert-butylhydro quinone: ethanol: phosphoric acid: zinc powder=1:2-6:0.04-0.1:0.01-0.06.
Described a kind of purification 2, the production method of 5-ditert-butylhydro quinone is characterized in that: the proportioning of weight of material is 2,5-ditert-butylhydro quinone: hydrochloric acid=1:0.02-0.06.
The present invention's beneficial effect compared with prior art:
Owing in traditional water, utilize on the basis of handling with a small amount of pyrosulphite sodium reduction, increase ethanol and made extraction agent, in acidic medium, add zinc powder and separate purification once more.After separating purification, select for use hydrochloric acid to carry out rinsing, the phosphoric acid salt in the product and the composition of insoluble impurities have been reduced, reduced by 2 simultaneously, the content of tertiarybutylhydroquinone≤0.1% in the 5-ditert-butylhydro quinone, Resorcinol content≤0.05%, 2,5-ditert-butylhydro quinone content is up to 99.5%; Changing traditional baking oven simultaneously is fluidized-bed oven dry material, has avoided caking, hard broken, the inferior defective of crystalline form.
Embodiment
Describe the present invention below in detail:
(1), concrete processing method and step;
The 1st the step, get 2, after the 5-ditert-butylhydro quinone carries out poach with traditional method, send dry by the fire siccative;
The 2nd step, get above-mentioned 12 after handling, 5-ditert-butylhydro quinone siccative 150kg adds ethanol 400kg respectively, concentration is 85% phosphoric acid 6kg, zinc powder 2kg, is warming up to 60-85 ℃ of press filtration while hot, cooling, crystallization, suction filtration, mechanical centrifuge dripping;
The 3rd step, use traditional method poach, suction filtration once more, adding concentration is that 36% hydrochloric acid 3kg rinsing is handled, and through the fluidized-bed oven dry, gets material master content 99.1%, Resorcinol 0.05%, tertiarybutylhydroquinone 0.1% and insolubles are qualified; The outward appearance crystalloid is good simultaneously.
(2), principle of work;
Under acidic conditions, in certain temperature range, by with ethanol as extraction agent, carry out antioxygen with zinc powder and handle, increased the antioxygen cycle, outward appearance is improved simultaneously;
Use the salt acid rinse, the phosphoric acid salt in the reduction product and the composition of insoluble impurities;
With fluidized-bed oven dry material the product crystalline form is improved, avoids caking, hard fragmentation and the inferior defective of crystalline form.
Claims (3)
1, a kind of purification 2, the production method of 5-ditert-butylhydro quinone, with 2, the 5-ditert-butylhydro quinone with traditional production method poach after, send dry by the fire siccative, it is characterized in that: get dry by the fire 2,5-ditert-butylhydro quinone siccative, add ethanol, phosphoric acid, zinc powder respectively, be warming up to 60-85 ℃, be incubated 30-60 minute; Press filtration while hot, cooling, crystallization, suction filtration, mechanical centrifuge dripping; Use traditional method poach, suction filtration once more, handle with 30-36% salt acid rinse, suction filtration is centrifugal; Through the fluidized-bed oven dry, get qualified product.
2, a kind of purification 2 according to claim 1, the production method of 5-ditert-butylhydro quinone is characterized in that: the proportioning of weight of material is 2,5-ditert-butylhydro quinone: ethanol: phosphoric acid: zinc powder=1:2-6:0.04-0.1:0.01-0.06.
3, a kind of purification 2 according to claim 1, the production method of 5-ditert-butylhydro quinone is characterized in that: the proportioning of weight of material is 2,5-ditert-butylhydro quinone: hydrochloric acid=1:0.02-0.06.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101309188A CN100537505C (en) | 2007-08-23 | 2007-08-23 | Production method for purifying 2,5-di-tert-butyl hydroquinone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101309188A CN100537505C (en) | 2007-08-23 | 2007-08-23 | Production method for purifying 2,5-di-tert-butyl hydroquinone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101139260A CN101139260A (en) | 2008-03-12 |
| CN100537505C true CN100537505C (en) | 2009-09-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007101309188A Expired - Fee Related CN100537505C (en) | 2007-08-23 | 2007-08-23 | Production method for purifying 2,5-di-tert-butyl hydroquinone |
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| CN (1) | CN100537505C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190564B (en) * | 2011-03-25 | 2013-09-18 | 广州泰邦食品科技有限公司 | Production method of DTBHQ (2-5-di-tert-butylhydroquinone) |
| CN102838454B (en) * | 2012-09-25 | 2014-07-30 | 厦门大学 | Purification method for tertiary butyl hydroquinone |
| CN114890872B (en) * | 2022-06-28 | 2024-04-23 | 翁源广业清怡食品科技有限公司 | Method for improving stability of 2, 5-di-tert-butylhydroquinone |
-
2007
- 2007-08-23 CN CNB2007101309188A patent/CN100537505C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 2,5-二叔丁基对苯二酚的简便脱色方法. 唐渝，张渊明，杨骏.精细化工，第19卷第5期. 2002 |
| 2,5-二叔丁基对苯二酚的简便脱色方法. 唐渝，张渊明，杨骏.精细化工，第19卷第5期. 2002 * |
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| CN101139260A (en) | 2008-03-12 |
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Granted publication date: 20090909 Termination date: 20120823 |