CN102070453A - Process for producing tetra[beta-(3.5-di-tert-butyl-4-hydroxybenzene)propionic acid]pentaerythritol ester under normal pressure - Google Patents
Process for producing tetra[beta-(3.5-di-tert-butyl-4-hydroxybenzene)propionic acid]pentaerythritol ester under normal pressure Download PDFInfo
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- CN102070453A CN102070453A CN2009102286464A CN200910228646A CN102070453A CN 102070453 A CN102070453 A CN 102070453A CN 2009102286464 A CN2009102286464 A CN 2009102286464A CN 200910228646 A CN200910228646 A CN 200910228646A CN 102070453 A CN102070453 A CN 102070453A
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- tert
- butyl
- propionic acid
- pentaerythritol ester
- hydroxy phenyl
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Abstract
The invention relates to a process for producing tetra[beta-(3.5-di-tert-butyl-4-hydroxybenzene)propionic acid]pentaerythritol ester under normal pressure. The process comprises the following steps of: putting beta-(3.5-di-tert-butyl-4-hydroxybenzene)methyl propionate, pentaerythritol and a catalyst into a reactor according to a certain proportion, heating to melt materials under the condition of keeping introducing N2, stirring to make the materials uniformly mixed, reacting at the temperature of between 160 and 200 DEG C for 6 to 12 hours, dissolving, decolorizing, performing heat filtration, crystallizing and drying to obtain a finished product. The process has the advantages that: 1, methanol serving as a reactant is effectively recycled, so that environmental pollution is reduced; 2, a vacuum pump is saved, so that equipment investment is reduced; and 3, the recycled methanol can be taken as a solvent for production, so that production cost is reduced.
Description
Technical field
The present invention relates to the improvement of four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester production technique,, realize the production of four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester normal pressure by changing technology condition.
Background technology
Four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, its trade name is an antioxidant 1010, traditional processing technology is a decompression method production technique: put into β-(3.5-di-tert-butyl-hydroxy phenyl) methyl propionate, tetramethylolmethane and catalyzer in the reactor by a certain percentage, by the decompression heating, at 140～206 ℃ of reactions of temperature 6h, building-up reactions finishes.
Its shortcoming is: one, for reaction is moved to the positive reaction direction, reaction needs to remove reaction product-methyl alcohol under high vacuum condition, improves product yield.Two, under high vacuum condition, the Methanol Recovery difficulty, emission treatment causes environmental pollution.Though dry vacuum pump can solve this difficult problem, dry vacuum pump costs an arm and a leg, and investment improves.Three, because of the vacuum tightness height of reaction needed, require the equipment resistance to air loss good, improved the equipment installment quality standard.
Summary of the invention
The present invention seeks to overcome the deficiency that exists in the traditional technology, and a kind of four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] production technique that pentaerythritol ester is new that provides, this public affairs skill can be finished under atmospheric pressure state, compare with the decompression method, product yield is with the decompression method, and quality product slightly is better than the decompression method, simultaneously efficient recovery reaction product methyl alcohol, can be directly used in production, reduce production costs.
Technical scheme of the present invention is: four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester non-pressure process production technique
In reactor, drop into β-(3.5-di-tert-butyl-hydroxy phenyl) methyl propionate, tetramethylolmethane, dibutyltin oxide by a certain percentage successively, feed N
2Heating up in the back, after the fusion of question response thing, starts whipping appts and make mixing of materials even, and at 160～200 ℃ of reactions of temperature, 6～12h, reaction finishes.Through dissolving, decolouring, hot filter, crystallization, centrifugal, dry, get finished product four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
All the time feed N in the reaction process
2, and keep certain flow rate, so that take away reaction product-methyl alcohol, gas enters condenser and reclaims methyl alcohol.
The present invention is for reducing N
2Consume, can adopt a plurality of reactors to produce N simultaneously
2Adopt tandem process.
Proportioning raw materials of the present invention is: β-(3.5-di-tert-butyl-hydroxy phenyl) methyl propionate 120g, tetramethylolmethane 13.2g, dibutyltin oxide 0.1～0.8g.
Advantage of the present invention: 1, adopt nitrogen to make medium, remove reaction product methyl alcohol, realize normal pressure production, efficient recovery product methyl alcohol, and conduct is simultaneously produced solvent and is used, and reduces production costs.2, reduce equipment criteria and investment.
Embodiment
With β-(3.5-di-tert-butyl-hydroxy phenyl) methyl propionate 120g, tetramethylolmethane 13.2g, dibutyltin oxide 0.4g drop in the reactor successively, logical people N
2, heat up, treat to start whipping appts behind the material melting, at 160～200 ℃ of reactions of temperature, 6～12h, reaction finishes.Through dissolving, decolouring, hot filter, crystallization, drying, get finished product four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 106g, yield 92.7%; Reclaim methyl alcohol 9g, yield 72.6%.
Reaction equation of the present invention:
Claims (2)
1. one kind four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester non-pressure process production technique, it is characterized in that: β-(3.5-di-tert-butyl-hydroxy phenyl) methyl propionate, tetramethylolmethane, catalyzer are put in the reactor by a certain percentage, kept N
2Under the feeding condition, behind the heat fused material, stirring makes mixing of materials even, at 160～200 ℃ of reactions of temperature 6-12h, through dissolving, decolouring, hot filter, crystallization, dry finished product four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester that gets.
2. four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] according to claim 1 pentaerythritol ester non-pressure process production technique, it is characterized in that: the concrete weight of above-mentioned each raw material is: β-(3.5-di-tert-butyl-hydroxy phenyl) methyl propionate 120g, stearyl alcohol 13.5g, dibutyltin oxide 0.1～0.8g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102286464A CN102070453A (en) | 2009-11-20 | 2009-11-20 | Process for producing tetra[beta-(3.5-di-tert-butyl-4-hydroxybenzene)propionic acid]pentaerythritol ester under normal pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102286464A CN102070453A (en) | 2009-11-20 | 2009-11-20 | Process for producing tetra[beta-(3.5-di-tert-butyl-4-hydroxybenzene)propionic acid]pentaerythritol ester under normal pressure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102070453A true CN102070453A (en) | 2011-05-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102286464A Pending CN102070453A (en) | 2009-11-20 | 2009-11-20 | Process for producing tetra[beta-(3.5-di-tert-butyl-4-hydroxybenzene)propionic acid]pentaerythritol ester under normal pressure |
Country Status (1)
| Country | Link |
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| CN (1) | CN102070453A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701979A (en) * | 2012-07-05 | 2012-10-03 | 营口市风光化工有限公司 | Method for purifying antioxidant 1010 |
| CN114957007A (en) * | 2022-06-15 | 2022-08-30 | 江苏极易新材料有限公司 | Method for recycling 3,5 methyl ester through 1010 alcoholysis of antioxidant |
-
2009
- 2009-11-20 CN CN2009102286464A patent/CN102070453A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701979A (en) * | 2012-07-05 | 2012-10-03 | 营口市风光化工有限公司 | Method for purifying antioxidant 1010 |
| CN114957007A (en) * | 2022-06-15 | 2022-08-30 | 江苏极易新材料有限公司 | Method for recycling 3,5 methyl ester through 1010 alcoholysis of antioxidant |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110525 |