CN107522599A - A kind of neutralization technique of the methylphenol alkane production procedure of 2,6 di-t-butyl 4 - Google Patents
A kind of neutralization technique of the methylphenol alkane production procedure of 2,6 di-t-butyl 4 Download PDFInfo
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- CN107522599A CN107522599A CN201610442025.6A CN201610442025A CN107522599A CN 107522599 A CN107522599 A CN 107522599A CN 201610442025 A CN201610442025 A CN 201610442025A CN 107522599 A CN107522599 A CN 107522599A
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- butyl
- methylphenol
- water
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- reaction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/11—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms
- C07C37/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms by addition reactions, i.e. reactions involving at least one carbon-to-carbon unsaturated bond
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
2, the methylphenol product of 6 di-t-butyl 4 is using p-methyl phenol and isobutene as main raw material(s), reaction is alkylated under acidic catalyst effect, obtained alkide obtains product after alkali neutralizes, washes layering, addition ethanol continuous crystallisation, centrifugation, drying.Solution air-distillation recovery ethanol after centrifugation.The key problem in technology of this technological process includes neutralization reaction technique.
Description
Technical field
The present invention relates to chemical products production technology, neutralized in the reaction of especially 2,6- di-tert-butyl-4-methy phenols alkane
Reaction process.
Background technology
2,6 di tert butyl 4 methyl phenol product is a kind of important chemical products.White or Light yellow crystals.It is readily soluble
In toluene, the organic solutions such as acetone, ethanol, benzene, ether, isopropanol, methanol, 2- butanone, ethylene glycol ethyl ether, petroleum ether are dissolved in,
Not soluble in water and aqueous slkali.It is various lubricating oil in the oil industry, secondary processing of gasoline, paraffin and some other mineral oil
Excellent antioxidant.It is the cheap logical of polypropylene, polyethylene, polystyrene, ABS resin, polyester, celluosic resin and foamed plastics
Use antioxidant；Especially suitable for white or light color article.Especially food grade plastic and polymeric material used for packaging food and day
T PNR, the white of synthetic rubber or the antioxidant and stabilizer of light color article.It is cis-butadiene cement, butadiene-styrene rubber, neoprene, fourth
The antioxidant and stabilizer of eyeball rubber, butyl rubber.Synthetic method：The synthetic method master of 2,6 di tert butyl 4 methyl phenol
Have following several：1. paracresol method.Paracresol purifies after carrying out Friedel-Crafts reaction with alkylating agent.It is domestic generally to be closed using this law
Into.2. mixed phenol method.Rectifying separates after mixed phenol carries out Friedel-Crafts reaction with alkylating agent, finally crystallizes.Technological requirement is higher, mesh
Preceding more applicable this law of German factory.3. Si Jieerda mark's methods.Catalytic hydrogenation can directly obtain after phenol carries out mannich reaction
Product.Because using phenol, for primary raw material, cost is relatively low, but product quality is least stable in three kinds of techniques, Russian work
Factory uses this law more.
The content of the invention
The present invention 2,6- di-tert-butyl-4-methy phenols product using p-methyl phenol and isobutene as main raw material(s),
Reaction is alkylated under acidic catalyst effect, obtained alkide is neutralized through alkali, washes layering, addition ethanol is continuously tied
Brilliant, centrifugation, obtain product after drying.Solution air-distillation recovery ethanol after centrifugation.The key problem in technology of this technological process includes
Neutralization reaction.
Add alkali to neutralize the product after alkylated reaction, add and sodium carbonate and stir in crystallization kettle, make sodium carbonate with it is right
Neutralization reaction occurs for toluenesulfonic acid, generates paratoluenesulfonic acid sodium salt and water.Paratoluenesulfonic acid sodium salt is water-soluble, and phenols is not soluble in water,
Paratoluenesulfonic acid sodium salt can enter in aqueous phase, and phenols can enter in oil phase.
Reaction equation：
Neutralization reaction
。
Claims (2)
1. raw material of the present invention and proportioning.
2. the product of the present invention by after alkylated reaction adds alkali to neutralize, sodium carbonate is added in crystallization kettle and is stirred, is made
With p-methyl benzenesulfonic acid neutralization reaction occurs for sodium carbonate, generates paratoluenesulfonic acid sodium salt and water；Paratoluenesulfonic acid sodium salt is water-soluble, phenols
Not soluble in water, paratoluenesulfonic acid sodium salt can enter in aqueous phase, and phenols can enter flow in oil phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610442025.6A CN107522599A (en) | 2016-06-21 | 2016-06-21 | A kind of neutralization technique of the methylphenol alkane production procedure of 2,6 di-t-butyl 4 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610442025.6A CN107522599A (en) | 2016-06-21 | 2016-06-21 | A kind of neutralization technique of the methylphenol alkane production procedure of 2,6 di-t-butyl 4 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107522599A true CN107522599A (en) | 2017-12-29 |
Family
ID=60733767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610442025.6A Pending CN107522599A (en) | 2016-06-21 | 2016-06-21 | A kind of neutralization technique of the methylphenol alkane production procedure of 2,6 di-t-butyl 4 |
Country Status (1)
| Country | Link |
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| CN (1) | CN107522599A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225644A (en) * | 2020-10-15 | 2021-01-15 | 南京晶典抗氧化技术研究院有限公司 | Production method of alkylphenol liquid antioxidant |
-
2016
- 2016-06-21 CN CN201610442025.6A patent/CN107522599A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225644A (en) * | 2020-10-15 | 2021-01-15 | 南京晶典抗氧化技术研究院有限公司 | Production method of alkylphenol liquid antioxidant |
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Legal Events
| Date | Code | Title | Description |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171229 |