CN1935764A - Method for preparing 2, 6-di-tert.-butyl phenol alkylating solution - Google Patents
Method for preparing 2, 6-di-tert.-butyl phenol alkylating solution Download PDFInfo
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- CN1935764A CN1935764A CNA2006101173821A CN200610117382A CN1935764A CN 1935764 A CN1935764 A CN 1935764A CN A2006101173821 A CNA2006101173821 A CN A2006101173821A CN 200610117382 A CN200610117382 A CN 200610117382A CN 1935764 A CN1935764 A CN 1935764A
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- tert
- phenol
- butylphenol compounds
- butylene
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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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 2, 6-di-ter-butyl phenol alkylating liquor preparing method, weighing phenol in the ratio of phenol to aluminum scraps 1 to 0.001-0.01 and mixing with the catalyst fully, then charging isobutylene into a reacting kettle in the given proportion, under the action of the catalyst, keeping a certain temperature, pressure and time to complete the reaction, and then by resolution and filtering, removing the catalyst and obtaining pure 2, 6-di-ter-butyl phenol alkylating liquor. As compared with the existing technique, it has characters of low cost and high yield.
Description
Technical field
The present invention relates to the intermediate manufacturing technology field of 2.6-DI-tert-butylphenol compounds, relate in particular to a kind of preparation method of intermediate 2.6-DI-tert-butylphenol compounds alkylation liquid of 2.6-DI-tert-butylphenol compounds.
Background technology
Phenol and iso-butylene carry out alkylated reaction under the effect of phenol Al catalysts, generate 2.6-DI-tert-butylphenol compounds alkylation liquid, are called for short 26 alkylation liquids.26 alkylation liquids are intermediates of 2.6-DI-tert-butylphenol compounds, just can obtain 2.6-di-tert-butyl phenolic product through rectification and purification.These product are important source material of multiple hindered phenol antioxygen, and the manufacture method of its optimization can reduce the production cost of oxidation inhibitor to a great extent.
At present, the production method of 26 alkylation liquids has a variety of, but mostly transformation efficiency is lower, and promptly 2.6-DI-tert-butylphenol compounds content is lower in 26 alkylation liquids, generally about 70%～78%, and also long reaction time, the production cost height.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of preparation method who improves reaction yield, shortens the 2.6-DI-tert-butylphenol compounds alkylation liquid in reaction times for the weak point that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of 2.6-DI-tert-butylphenol compounds alkylation liquid, it is characterized in that, by phenol: the aluminium bits are that 1: 0.001～0.01 proportioning adds reactor with phenol and aluminium bits, intensification is risen pressure, when rising suddenly, reacting kettle inner pressure stops, preparation phenol Al catalysts, then according to phenol: iso-butylene is that 1: 0.9～1.9 ratio feeds iso-butylene in this reactor, controlled temperature is 80 ℃～120 ℃, reacted 1.0～2.0 hours, after insulation reaction finishes, question response still internal pressure descends when slow, and iso-butylene excessive in the reactor is carried out parse operation, adds the water destruct catalyzer then, filter and remove catalyzer, obtain purified 2.6-DI-tert-butylphenol compounds alkylation liquid.
Described suitable phenol: the aluminium bits are 1: 0.002～0.006.
Described phenol: iso-butylene is 1: 1.1～1.4.
Described alkylated reaction temperature is 90 ℃～120 ℃.
The described alkylated reaction time is 1～2 hour.
Enforcement of the present invention is by changing raw material and catalyzer ingredient proportion, and temperature of reaction, pressure, time is optimized control, improved transformation efficiency greatly, the content of 2.6-DI-tert-butylphenol compounds can reach 84%～88% in 26 alkylation liquids of being produced, and is worth 3 of proposition to shorten the reaction times greatly especially.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
The phenol and the aluminium bits of specified amount are pressed phenol: the proportioning of aluminium bits=1: 0.003 adds preparation phenol Al catalysts, intensification is upgraded to suddenly up to reacting kettle inner pressure and ends, then according to phenol: the ratio of iso-butylene=1: 1.35 feeds iso-butylene, 90 ℃ of reactions of controlled temperature 0.5 hour, further control reaction temperature is carried out insulation reaction for 120 ℃.After insulation reaction finished, question response still internal pressure descended when slow, and iso-butylene excessive in the reactor is carried out parse operation, adds water subsequently, filters and removes catalyzer, obtains 26 alkylation liquids, and the content of 2.6-DI-tert-butylphenol compounds is 85.33% by analysis.
Described alkylated reaction equation is:
Embodiment 2
The phenol and the aluminium bits of specified amount are pressed phenol: the proportioning of aluminium bits=1: 0.004 adds preparation phenol Al catalysts, intensification is upgraded to suddenly up to reacting kettle inner pressure and ends, then according to phenol: the ratio of iso-butylene=1: 1.3 feeds iso-butylene, 90 ℃ of reactions of controlled temperature 0.5 hour are warmed up to 110 ℃ of insulation reaction 1 hour again.After insulation reaction finished, question response still internal pressure descended when slow, and iso-butylene unnecessary in the reactor is carried out parse operation.Add entry subsequently and filter the removal catalyzer, obtain 26 alkylation liquids, the content of 2.6-DI-tert-butylphenol compounds is 84.16% by analysis.
Described alkylated reaction equation is:
Embodiment 3
The phenol and the aluminium bits of specified amount are pressed phenol: the proportioning of aluminium bits=1: 0.006 adds preparation phenol Al catalysts, intensification is upgraded to suddenly up to reacting kettle inner pressure and ends, then according to phenol: the ratio of iso-butylene=1: 1.4 feeds iso-butylene, 100 ℃ of reactions of controlled temperature 0.5 hour, control reaction temperature was carried out insulation reaction 1.5 hours for 120 ℃ again, after insulation reaction finished, question response still internal pressure descended when slow, and iso-butylene unnecessary in the reactor is carried out parse operation.Add water filtration subsequently and remove catalyzer, obtain 26 alkylation liquids, the content of 2.6-DI-tert-butylphenol compounds is 86.02% by analysis.
Described alkylated reaction equation is:
Claims (5)
1. the preparation method of a 2.6-DI-tert-butylphenol compounds alkylation liquid, it is characterized in that, by phenol: the aluminium bits are that 1: 0.001～0.01 proportioning feeds intake, intensification is till reacting kettle inner pressure sharply rises, insulation reaction 0.5～1.0 hour, then according to phenol: iso-butylene is that 1: 0.9～1.9 ratio feeds iso-butylene in this reactor, controlled temperature is 80 ℃～120 ℃, carried out alkylated reaction 2.0～4.0 hours, afterwards iso-butylene unnecessary in the reactor is carried out parse operation, filter and remove catalyzer, obtain purified 2.6-DI-tert-butylphenol compounds alkylation liquid.
2. the preparation method of a kind of 2.6-DI-tert-butylphenol compounds alkylation liquid according to claim 1 is characterized in that, described phenol: the aluminium bits are 1: 0.002～0.006.
3. the preparation method of a kind of 2.6-DI-tert-butylphenol compounds alkylation liquid according to claim 1 is characterized in that, described phenol: iso-butylene is 1: 1.1～1.4.
4. the preparation method of a kind of 2.6-DI-tert-butylphenol compounds alkylation liquid according to claim 1 is characterized in that, described alkylated reaction temperature is 90 ℃～120 ℃.
5. the preparation method of a kind of 2.6-DI-tert-butylphenol compounds alkylation liquid according to claim 1 is characterized in that, the described alkylated reaction time is 1～2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101173821A CN1935764A (en) | 2006-10-20 | 2006-10-20 | Method for preparing 2, 6-di-tert.-butyl phenol alkylating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2006101173821A CN1935764A (en) | 2006-10-20 | 2006-10-20 | Method for preparing 2, 6-di-tert.-butyl phenol alkylating solution |
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| CN1935764A true CN1935764A (en) | 2007-03-28 |
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| CNA2006101173821A Pending CN1935764A (en) | 2006-10-20 | 2006-10-20 | Method for preparing 2, 6-di-tert.-butyl phenol alkylating solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108026010A (en) * | 2015-09-11 | 2018-05-11 | 巴斯夫欧洲公司 | Alkylated method for phenol |
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2006
- 2006-10-20 CN CNA2006101173821A patent/CN1935764A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108026010A (en) * | 2015-09-11 | 2018-05-11 | 巴斯夫欧洲公司 | Alkylated method for phenol |
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