CN102040518A - Method for producing antioxidant of tetra[Beta-(3.5-ditertiary butyl-4-hydroxyphenyl) propanoic acid] pentaerythritol ester - Google Patents
Method for producing antioxidant of tetra[Beta-(3.5-ditertiary butyl-4-hydroxyphenyl) propanoic acid] pentaerythritol ester Download PDFInfo
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- CN102040518A CN102040518A CN2009100708245A CN200910070824A CN102040518A CN 102040518 A CN102040518 A CN 102040518A CN 2009100708245 A CN2009100708245 A CN 2009100708245A CN 200910070824 A CN200910070824 A CN 200910070824A CN 102040518 A CN102040518 A CN 102040518A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to a method for producing an antioxidant of tetra[Beta-(3.5-ditertiary butyl-4-hydroxyphenyl) propanoic acid] pentaerythritol ester, comprising the following steps of: placing 3.5 methyl ester, pentaerythritol and a catalyst in a normal pressure reaction kettle; introducing N2 to replace air in a system for 0.5-1 h; raising the temperature; stirring after the materials are completely dissolved; controlling the reaction temperature to be 16-200 DEG C; keeping the flow rate of N2 in the reaction process to flow out the generated methanol; introducing the methanol to a condenser for condensing and recycling; reacting for 6-12 h, then stopping reacting; sampling and analyzing. The method has the advantages that the methanol has high recovery rate, for example, the tail oxygen and cold well can reach more than 90%, the pollution (water or atmosphere) on the environment is reduced, and the raw material cost for production is also lowered; the whiteness and the light transmittance of a product are improved; the noise on a station and the vacuum operation energy consumption are reduced because a vacuum pump is replaced; and the reaction kettle is replaced by a normal pressure apparatus.
Description
Technical field:
The present invention relates to a kind of production technique of oxidation inhibitor, particularly a kind of non-pressure process is produced the method for four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester.
Background technology:
Four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, general oxidation inhibitor by name " 1010 ".Carrying out transesterification reaction by β (3.5-di-tert-butyl-hydroxy phenyl) methyl propionate and tetramethylolmethane obtains.
Production technique in the past is the decompression reaction, carries out at absolute pressure＜10mmHG post, and the methyl alcohol that reaction generates is taken away by vacuum, and the balance of reaction reaches gratifying substantially terminal point to the right.
The reaction shortcoming of decompression state is: 1, the methyl alcohol of reaction generation, difficulty is reclaimed in cooling under vacuum state, thereby the rate of recovery is on the low side, and then water or air polluted, though dry vacuum pump can solve this problem, but the dry vacuum high price has increased one-time investment greatly, and also need work hard to the maintenance of pump.2, react under the high vacuum, the bearing capacity and the equipment installment quality (the close property of oxygen) of equipment also proposed high standard.
Summary of the invention:
Purpose of the present invention just is to overcome above-mentioned the deficiencies in the prior art, and provide the production method of a kind of oxidation inhibitor four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, the Methanol Recovery rate height of this method, reduced pollution, reduced production cost simultaneously environment.
Technical scheme of the present invention is: the production method of a kind of oxidation inhibitor four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester is characterized in that: after in normal-pressure reaction kettle, dropping into 3.5 methyl esters, tetramethylolmethane and catalyzer, and logical N
2Air 0.5-1 in the exchange system hour, heat up, start in the complete molten back of material and stir, 160 ℃-200 ℃ of control reaction temperature keep N in reaction process
2Flow velocity so that the methyl alcohol that generates is taken out of, enters condenser, carries out condensation and reclaims, and after reaction 6-12 hour, gets final product stopped reaction, sampling analysis.
Aforesaid reaction vessel can adopt a plurality of reactors to be connected in series.
Drop into 3.5 methyl esters, 200 grams, tetramethylolmethane 21.9 grams in the aforesaid reaction vessel, catalyst oxidation two zinc-base tin 1.0 grams.
Of the present invention have following advantage and a positively effect:
1, Methanol Recovery rate height adds cold well as tail oxygen and can reach more than 90%, reduces the pollution (water and atmosphere) to environment, has reduced the raw materials cost of producing simultaneously.
2, whiteness, the transmittance of product have been improved.
3, replace vacuum pump, reduce noise and vacuum running energy consumption on the post.
4, reactor was pressure regulating equipment originally, and available normal pressure equipment replaces.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
As shown in the figure: I, II, III are reactor, 1. are methanol tank; 2. be receiving tank; 3. be receiving tank; 4. be condenser.
Drop into 3.5 methyl esters, 200 grams, tetramethylolmethane 21.9 grams in 3 reactors that are connected in series, after catalyst oxidation two zinc-base tin 1.0 grams finished, series connection fed N
2Air in the exchange system (about 0.5 hour, according to the logical N of the size of still
2Speed is adjusted), heat up, after material is molten entirely, starts and stir, 160 ℃-200 ℃ of control reaction temperature keep N in reaction process
2Flow velocity so that the methyl alcohol that generates is taken out of, enters condenser, and condensation is reclaimed, and after reaction 6-12 hour, gets final product stopped reaction, and sampling analysis carries out post-processing operation.Last still N
2Suggestion is then discharged by cold well before the emptying.
The present invention adopts synthesis under normal pressure, 64 ℃ of methyl alcohol boiling points, and the condensation that can obtain comparison safety in condenser is reclaimed, and reduces the pollution to environment, reclaims the raw materials cost that methyl alcohol can reduce production simultaneously.
Claims (3)
1. the production method of an oxidation inhibitor four [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester is characterized in that: drop into 3.5 methyl esters, tetramethylolmethane and catalyzer in normal-pressure reaction kettle after, lead to N
2Air 0.5-1 in the exchange system hour, heat up, start in the complete molten back of material and stir, 160 ℃-200 ℃ of control reaction temperature keep N in reaction process
2Flow velocity so that the methyl alcohol that generates is taken out of, enters condenser, carries out condensation and reclaims, and after reaction 6-12 hour, gets final product stopped reaction, sampling analysis.
2. the production method of oxidation inhibitor four according to claim 1 [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, aforesaid reaction vessel can adopt a plurality of reactors to be connected in series.
3. the production method of oxidation inhibitor four according to claim 1 [β-(3.5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester drops into 3.5 methyl esters, 200 grams, tetramethylolmethane 21.9 grams in the aforesaid reaction vessel, catalyst oxidation two zinc-base tin 1.0 grams.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100708245A CN102040518A (en) | 2009-10-16 | 2009-10-16 | Method for producing antioxidant of tetra[Beta-(3.5-ditertiary butyl-4-hydroxyphenyl) propanoic acid] pentaerythritol ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100708245A CN102040518A (en) | 2009-10-16 | 2009-10-16 | Method for producing antioxidant of tetra[Beta-(3.5-ditertiary butyl-4-hydroxyphenyl) propanoic acid] pentaerythritol ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102040518A true CN102040518A (en) | 2011-05-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100708245A Pending CN102040518A (en) | 2009-10-16 | 2009-10-16 | Method for producing antioxidant of tetra[Beta-(3.5-ditertiary butyl-4-hydroxyphenyl) propanoic acid] pentaerythritol ester |
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| CN (1) | CN102040518A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112538204A (en) * | 2020-12-02 | 2021-03-23 | 广州市奇胜电线电缆有限公司 | Wear-resistant and tensile-resistant halogen-free wire and cable and manufacturing method thereof |
| CN112661633A (en) * | 2020-12-24 | 2021-04-16 | 青岛科技大学 | Method for continuously preparing antioxidant 1010 |
-
2009
- 2009-10-16 CN CN2009100708245A patent/CN102040518A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112538204A (en) * | 2020-12-02 | 2021-03-23 | 广州市奇胜电线电缆有限公司 | Wear-resistant and tensile-resistant halogen-free wire and cable and manufacturing method thereof |
| CN112661633A (en) * | 2020-12-24 | 2021-04-16 | 青岛科技大学 | Method for continuously preparing antioxidant 1010 |
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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: 20110504 |