CN102603537A - Production method of 2,6-dimethylaniline - Google Patents
Production method of 2,6-dimethylaniline Download PDFInfo
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- CN102603537A CN102603537A CN2012100386811A CN201210038681A CN102603537A CN 102603537 A CN102603537 A CN 102603537A CN 2012100386811 A CN2012100386811 A CN 2012100386811A CN 201210038681 A CN201210038681 A CN 201210038681A CN 102603537 A CN102603537 A CN 102603537A
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- xylidine
- catalyst
- xylenol
- consumption
- reaction
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Abstract
The invention discloses a production method of 2,6-dimethylaniline, comprising the following steps: 2,6-dimethylaniline is obtained by a reaction among hydrogen, ammonia and 2,6-dimethylphenol; and a composite catalyst consisting of zirconium oxychloride, barium sulfate or barium hydroxide, aluminum oxide or aluminum nitrate and metal palladium is used as a catalyst in the reaction. The production method provided by the invention is simple and convenient, easy in operation and good in environmental friendliness, and the product yield can be up to above 88%.
Description
Technical field
The present invention relates to a kind of 2, the working method of 6-xylidine.
Background technology
Existing 2, the working method of 6-xylidine, owing to reasons such as catalyzer, the three wastes are many, and energy consumption is big, and yield is low.
Summary of the invention
The object of the present invention is to provide a kind of easy to operate, yield high 2, the working method of 6-xylidine.
Technical solution of the present invention is:
A kind of 2; The working method of 6-xylidine comprises hydrogen, ammonia and 2, and the reaction of 6-xylenol obtains 2; The 6-xylidine; It is characterized in that: the reaction catalyst system therefor is a composite catalyst, and the preparation method of said composite catalyzing is: each component of following weight percent is mixed, obtain mixture:
Zirconium oxychloride 10 ~ 20%
Permanent white or hydrated barta 20 ~ 30%
Aluminium sesquioxide or aluminum nitrate 50 ~ 60%;
Mixture was through 120 ℃ of pre-treatment 8 ~ 12 hours, and behind the removal moisture, warp was fired 8 ~ 12 hours for 500 ~ 600 ℃ again, and the spray of the catalyst surface after firing attaches palladium metal then, and the consumption of palladium metal is 0.5 ~ 1% of a said mixture weight.
Catalyst consumption is 2,2 ~ 3% of 6-xylenol weight.
2, the consumption mol ratio of 6-xylenol and ammonia, hydrogen is 1:1.3:3.
The inventive method is easy, and is easy to operate, and product yield can reach more than 88%, and the feature of environmental protection is good.
Below in conjunction with embodiment the present invention is described further.
Embodiment
Embodiment 1:
A kind of 2, the working method of 6-xylidine comprises 2 after hydrogen, ammonia and the gasification; The 6-xylenol reacts in the reactor drum of catalyzer is arranged, and temperature of reaction is 195 ~ 220 ℃, and reactant gases is through condenser condenses; Reaction obtain 2,6-xylidine bullion to reaction solution basin (thick product yield more than 88%), reaction solution is squeezed into rectifying tower rectifying; Overhead product is behind condensing surface, tail gas condenser; The phlegma partial reflux, rest part removes receiving tank successively by different fractions, packing of product warehouse-in.The reaction catalyst system therefor is a composite catalyst, and the preparation method of said composite catalyzing is: each component of following weight percent is mixed, obtain mixture:
Zirconium oxychloride 15%
Permanent white 25%
Aluminium sesquioxide 60%;
Mixture was through 120 ℃ of pre-treatment 8 ~ 12 hours, and behind the removal moisture, warp was fired 8 ~ 12 hours for 500 ~ 600 ℃ again, and the spray of the catalyst surface after firing attaches palladium metal then, and the consumption of palladium metal is 0.6% of a said mixture weight.
Catalyst consumption is 2,2% of 6-xylenol weight.
2, the consumption mol ratio of 6-xylenol and ammonia, hydrogen is 1:1.3:3.
Embodiment 2:
The preparation method of catalyst system therefor is: each component of following weight percent is mixed, obtain mixture:
Zirconium oxychloride 20%
Hydrated barta 30%
Aluminum nitrate 50%;
Mixture was through 120 ℃ of pre-treatment 8 ~ 12 hours, and behind the removal moisture, warp was fired 8 ~ 12 hours for 500 ~ 600 ℃ again, and the spray of the catalyst surface after firing attaches palladium metal then, and the consumption of palladium metal is 1% of a said mixture weight.
Catalyst consumption is 2,3% of 6-xylenol weight.
Thick product yield is more than 88%, and all the other are with embodiment 1.
Claims (3)
1. one kind 2; The working method of 6-xylidine comprises hydrogen, ammonia and 2, and the reaction of 6-xylenol obtains 2; The 6-xylidine; It is characterized in that: the reaction catalyst system therefor is a composite catalyst, and the preparation method of said composite catalyzing is: each component of following weight percent is mixed, obtain mixture:
Zirconium oxychloride 10 ~ 20%
Permanent white or hydrated barta 20 ~ 30%
Aluminium sesquioxide or aluminum nitrate 50 ~ 60%;
Mixture was through 120 ℃ of pre-treatment 8 ~ 12 hours, and behind the removal moisture, warp was fired 8 ~ 12 hours for 500 ~ 600 ℃ again, and the spray of the catalyst surface after firing attaches palladium metal then, and the consumption of palladium metal is 0.5 ~ 1% of a said mixture weight.
2. according to claim 12, the working method of 6-xylidine is characterized in that: catalyst consumption is 2,2 ~ 3% of 6-xylenol weight.
3. according to claim 1 and 22, the working method of 6-xylidine is characterized in that: 2, and the consumption mol ratio of 6-xylenol and ammonia, hydrogen is 1:1.3:3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100386811A CN102603537A (en) | 2012-02-21 | 2012-02-21 | Production method of 2,6-dimethylaniline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100386811A CN102603537A (en) | 2012-02-21 | 2012-02-21 | Production method of 2,6-dimethylaniline |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102603537A true CN102603537A (en) | 2012-07-25 |
Family
ID=46521387
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100386811A Pending CN102603537A (en) | 2012-02-21 | 2012-02-21 | Production method of 2,6-dimethylaniline |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102603537A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884622A (en) * | 2016-06-03 | 2016-08-24 | 山东崇舜化工有限公司 | Method for preparing 1,5-diaminonaphthlene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590365A (en) * | 2003-09-03 | 2005-03-09 | 中国石油化工股份有限公司 | Method of preparing 2, 6-diisoprogyl aniline |
-
2012
- 2012-02-21 CN CN2012100386811A patent/CN102603537A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590365A (en) * | 2003-09-03 | 2005-03-09 | 中国石油化工股份有限公司 | Method of preparing 2, 6-diisoprogyl aniline |
Non-Patent Citations (1)
| Title |
|---|
| 孙荣华: "《西北大学硕士学位论文》", 31 December 2002, article "2_6_二甲基苯酚气相胺化合成2_6_二甲基苯胺的研究", pages: 35 - 44 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884622A (en) * | 2016-06-03 | 2016-08-24 | 山东崇舜化工有限公司 | Method for preparing 1,5-diaminonaphthlene |
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Application publication date: 20120725 |