CN102259010A - Alkylphenol and phosphorus oxychloride esterification catalyst and preparation method thereof - Google Patents
Alkylphenol and phosphorus oxychloride esterification catalyst and preparation method thereof Download PDFInfo
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- CN102259010A CN102259010A CN2011101199536A CN201110119953A CN102259010A CN 102259010 A CN102259010 A CN 102259010A CN 2011101199536 A CN2011101199536 A CN 2011101199536A CN 201110119953 A CN201110119953 A CN 201110119953A CN 102259010 A CN102259010 A CN 102259010A
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- catalyst
- esterification
- pocl3
- preparation
- alkyl phenol
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention provides an alkylphenol and phosphorus oxychloride esterification catalyst comprising the raw materials in percentage by weight: 70-80% of TiCl4 and 20-30 % of AlCl3. A preparation method of the catalyst comprises the steps of respectively and uniformly grinding the two raw materials, proportionally mixing and then drying. Compared with a single catalyst, the mixed catalyst provided by the invention has the advantages of being better in catalytic performance, shortening the esterification time and increasing the conversion rate of products.
Description
Technical field
The present invention relates to organic matter esterification reaction field, be specifically related to a kind of alkyl phenol and POCl3 esterification catalysts and preparation method thereof.
Background technology
The employed under normal conditions catalyst of alkyl phenol and POCl3 esterification is a magnesium chloride, and with single magnesium chloride as catalyst, the conversion ratio of its catalytic efficiency and product is all not high.
Summary of the invention
The invention provides a kind of alkyl phenol and POCl3 catalyst for esterification reaction and preparation method thereof.Alkyl phenol and POCl3 esterification adopt this catalyst, have improved the speed of esterification, have improved the conversion ratio of product simultaneously.
The present invention adopts following technical scheme for achieving the above object:
A kind of alkyl phenol and POCl3 catalyst for esterification reaction is characterized in that: the percentage by weight of its constitutive material is:
TiCl
4? 70-80%
AlCl
3 20-30%。
Described a kind of alkyl phenol and POCl3 catalyst for esterification reaction is characterized in that: the percentage by weight of its constitutive material is:
TiCl
4 75%
AlCl
3 25%。
The preparation method of described a kind of alkyl phenol and POCl3 catalyst for esterification reaction is characterized in that: the concrete operations step is as follows:
(1) with TiCl
4And AlCl
3Grind respectively evenly;
(2) take by weighing TiCl after the grinding by formula rate
4And AlCl
3, and mixing and stirring;
(3) with the dry materials that stirs, standby.
The advantage that the present invention is compared with prior art had is:
1, shortened the reaction time, used the reaction time of the esterification of the alkyl phenol of this catalyst and POCl3 to compare as catalyst with independent use magnesium chloride, the reaction time has shortened 7-9 hour;
2, improved the conversion ratio of product, the conversion ratio of esterification reaction product that uses the alkyl phenol of this catalyst and POCl3 is up to more than 95%, and the product yield that adopts magnesium chloride to do the esterification of the alkyl phenol of catalyst and POCl3 is 85%-90%.
?
The specific embodiment
Embodiment:
1400 ㎏ alkyl phenols and 1600 ㎏ POCl3s are joined in the reactor, again mixed catalyst 30 ㎏ of the present invention are added in the still, the heating reactor, keeping temperature is under 150 ℃ the condition esterification to take place, reaction time is after 8 hours, and recording reaction conversion ratio is 95.2%.
Comparative Examples:
1400 ㎏ alkyl phenols and 1600 ㎏ POCl3s are joined in the reactor, again catalyst magnesium chloride 30 ㎏ are added in the still, the heating reactor, keeping temperature is under 150 ℃ the condition esterification to take place, reaction time is after 12 hours, and recording reaction conversion ratio is 85.2%.
By contrast catalyst of the present invention as can be seen and existing catalyst mutually specific energy obviously improve esterification speed, the raising conversion ratio.
Claims (3)
1. alkyl phenol and POCl3 catalyst for esterification reaction, it is characterized in that: the percentage by weight of its constitutive material is:
TiCl
4? 70-80%
AlCl
3 20-30%。
2. a kind of alkyl phenol according to claim 1 and POCl3 catalyst for esterification reaction is characterized in that: the percentage by weight of its constitutive material is:
TiCl
4 75%
AlCl
3 25%。
3. the preparation method of a kind of alkyl phenol as claimed in claim 1 and POCl3 catalyst for esterification reaction is characterized in that: the concrete operations step is as follows:
(1) with TiCl
4And AlCl
3Grind respectively evenly;
(2) take by weighing TiCl after the grinding by formula rate
4And AlCl
3, and mixing and stirring;
(3) with the dry materials that stirs, standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101199536A CN102259010A (en) | 2011-05-11 | 2011-05-11 | Alkylphenol and phosphorus oxychloride esterification catalyst and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101199536A CN102259010A (en) | 2011-05-11 | 2011-05-11 | Alkylphenol and phosphorus oxychloride esterification catalyst and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102259010A true CN102259010A (en) | 2011-11-30 |
Family
ID=45005955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101199536A Pending CN102259010A (en) | 2011-05-11 | 2011-05-11 | Alkylphenol and phosphorus oxychloride esterification catalyst and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102259010A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3718699A (en) * | 1969-04-30 | 1973-02-27 | Sagami Chem Res | Process of preparing 4,4'-dithiobis(2,6-di-t-butylphenol) |
| CN1076451A (en) * | 1992-09-29 | 1993-09-22 | 四平市科学技术研究所 | A kind of flame-retardant plasticizer synthetic method |
-
2011
- 2011-05-11 CN CN2011101199536A patent/CN102259010A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3718699A (en) * | 1969-04-30 | 1973-02-27 | Sagami Chem Res | Process of preparing 4,4'-dithiobis(2,6-di-t-butylphenol) |
| CN1076451A (en) * | 1992-09-29 | 1993-09-22 | 四平市科学技术研究所 | A kind of flame-retardant plasticizer synthetic method |
Non-Patent Citations (2)
| Title |
|---|
| 曲敏等: ""AlCl3/TiCl4催化癸烯聚合制润滑油基础油的研究"", 《石油炼制与化工》 * |
| 黄东平等: ""双酚S双(二苯基磷酸酯) ( BSDP)阻燃剂的合成"", 《精细化工》 * |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111130 |