CN1869023A - Synthesis of 2-methyl pyridine by acetylene acetonitrile method - Google Patents
Synthesis of 2-methyl pyridine by acetylene acetonitrile method Download PDFInfo
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- CN1869023A CN1869023A CN 200510107312 CN200510107312A CN1869023A CN 1869023 A CN1869023 A CN 1869023A CN 200510107312 CN200510107312 CN 200510107312 CN 200510107312 A CN200510107312 A CN 200510107312A CN 1869023 A CN1869023 A CN 1869023A
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- acetylene
- acetonitrile
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- methylpyridine
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Abstract
A process for preparing 2-methylpyridine by ethyne-acetonitrile method includes such steps as adding acetonitrile and organocobalt into a two-layer reactor, continuously feeding dried and cleaned ethyne gas until it is not absorbed, and cooling.
Description
Technical Field
The invention relates to 2-methylpyridine synthesized and produced by acetylene and acetonitrile at a certain temperature and a certain pressure, in particular to a fine chemical industry synthesized by taking the acetonitrile and the acetylene as raw materials and carrying out trimerization reaction at the temperature of 130-170 ℃ and the pressure of 1.0mpa in the presence of catalyst organic cobalt.
Background
As is known, the prior domestic method for producing 2-methylpyridine mainly extracts coal tar, has low yield and poor quality, and the coal tar resource is quite poor. The method for producing the 2-methylpyridine abroad is an ammonia aldehyde method, the reaction temperature reaches 350-: the boiling points are too close to each other, so that the separation is difficult, the process requirement is difficult, and the quality of the 2-methylpyridine is often influenced.
Disclosure of Invention
The technical scheme of the invention is realized as follows: in the presence of acetonitrile and organic cobalt as raw materials, dry purified acetylene gas is continuously filled into a reaction kettle at the temperature of 130 plus 170 ℃ and the pressure of 1.0mpa until the acetylene gas is not absorbed, the crude product with the temperature reduced to more than 90 percent can be obtained, the catalyst can be filtered and reused, the difference between the product and the acetonitrile as the raw material and a small amount of byproduct benzene is more than 45 ℃, the product with the content of 99.9 percent can be obtained only by a small amount of plate number rectifying towers, and the yield reaches 90 percent.
Drawings
The invention is further described by combining the process flow drawings
Acetonitrile → organic cobalt → thermometer 130 ℃ → pressure 0.1mpa → synthesis kettle → acetylene → temperature reduction 90 ℃ → crude product → catalyst separation → rectification separation → product
The reaction equation is:
Detailed Description
Example 1, 3kg of organic cobalt and 600kg of acetonitrile were charged into a 2000L reactor, ammonia gas and acetylene were substituted 3 times under a vacuum degree of minus 0.09mpa, and 750M was continuously charged at a temperature of 130 ℃ and 170 ℃ and a pressure of 1.0mpa3Stopping charging when the pressure rises suddenly, allowing the pressure to fall below 1.0mpa, cooling, sampling, and performing gas chromatography to obtain the productThe yield of the crude product is more than 90 percent, and the selectivity of acetonitrile is 100 percent.
Example 2A crude sample was analyzed by gas chromatography to find that the content was 96.5%, the yield was 95% and the selectivity to acetonitrile was 100% in a 2000L reactor charged with 1.5kg of cyclopentadienyl cobalt cyclooctadiene under the conditions of example 1.
Claims (4)
1. The synthesis of 2-methylpyridine by acetylene acetonitrile method includes using acetonitrile as raw material, trimerizing reaction at 130-170 deg.C and 1.0mpa in the presence of organic cobalt as catalyst, and only a small number of plate number rectifying towers are needed to obtain product with 99.9% content, and the yield is up to90%.
2. The synthesis of 2-methylpyridine by ethynylacetonitrile according to claim 1, wherein: the reaction is carried out under the anhydrous and anaerobic condition, before the reaction, acetonitrile which is a raw material and organic cobalt which is a catalyst are subjected to non-oxidation treatment, high-purity inert gas and acetylene gas are used for replacement under high vacuum, and then a small amount of acetylene gas is used for pressure maintaining treatment under negative pressure.
3. The synthesis of 2-methylpyridine by acetonitrile acetylene method according to claim 1 and 2, which is characterized in that: when the temperature of the reactor is raised to between 130 ℃ and 170 ℃, the acetylene gas is continuously introduced, the temperature range is controlled, and the pressure is in the range of 1.0mpa for reaction.
The synthesis of 2-methylpyridine by acetylene acetonitrile method according to claim 1, 2, 3, wherein the pressure of the reaction kettle is controlled by an acetylene container and a compressor outside the reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510107312 CN1869023A (en) | 2005-12-23 | 2005-12-23 | Synthesis of 2-methyl pyridine by acetylene acetonitrile method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510107312 CN1869023A (en) | 2005-12-23 | 2005-12-23 | Synthesis of 2-methyl pyridine by acetylene acetonitrile method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1869023A true CN1869023A (en) | 2006-11-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510107312 Pending CN1869023A (en) | 2005-12-23 | 2005-12-23 | Synthesis of 2-methyl pyridine by acetylene acetonitrile method |
Country Status (1)
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| CN (1) | CN1869023A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108821B (en) * | 2007-08-15 | 2011-04-27 | 新乡市恒基化工有限公司 | Method of manufacturing 2-picoline |
-
2005
- 2005-12-23 CN CN 200510107312 patent/CN1869023A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108821B (en) * | 2007-08-15 | 2011-04-27 | 新乡市恒基化工有限公司 | Method of manufacturing 2-picoline |
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| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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