CN102408371A - Method for purifying 2,3-dimethyl pyridine - Google Patents
Method for purifying 2,3-dimethyl pyridine Download PDFInfo
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- CN102408371A CN102408371A CN2011103297196A CN201110329719A CN102408371A CN 102408371 A CN102408371 A CN 102408371A CN 2011103297196 A CN2011103297196 A CN 2011103297196A CN 201110329719 A CN201110329719 A CN 201110329719A CN 102408371 A CN102408371 A CN 102408371A
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- lutidine
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Abstract
The invention discloses a method for purifying 2,3-dimethyl pyridine. The method mainly comprises the following steps of: adding ethylene glycol, tetrafluoroethylene and organic carboxylic acid to a crude product of the 2,3-dimethyl pyridine; and then sequentially salifying, crystallizing, washing, analyzing, extracting and precipitating to finally obtain the refined product of the 2,3-dimethyl pyridine. The method disclosed by the invention is simple in operation, and can be used for effectively purifying the 2,3-dimethyl pyridine; and the 2,3-dimethyl pyridine obtained by the method has the advantage of high purity.
Description
Technical field
The present invention relates to a kind of chemical purification method, be specifically related to a kind ofly to purify 2, the method for 3-lutidine.
Background technology
Pyridine is widely used in fields such as medicine, agricultural chemicals; In addition; They also are widely used in rubber industry, tensio-active agent and dyestuffs industries etc., and content is lower than 99% pyridine and is generally known as crude pyridine, can be used as solvent, acid binding agent etc.; Content is higher than 99.5% pyridine and is commonly referred to pure pyridine, can be used for most chemosynthesis.
At present, mainly by chemical synthesis production, chemosynthesis is generally made catalyzer by means of shape-selective molecular sieve to pyridine base; Catalyzed gas condensation reaction by between aldehyde and the ammonia forms, purified pyridine generally adopt sulfuric acid, Pottasium Hydroxide etc. to handle again rectifying obtains, perhaps first potassium permanganate oxidation; The method of handling with sodium hydroxide and quicklime again; Though but these methods purified pyridine more or less, complicated operation is not suitable for large-scale production.
Summary of the invention
For deficiency and the defective of alleviating prior art; The object of the present invention is to provide and a kind ofly purify 2, the method for 3-lutidine; Preparing method of the present invention is simple; Through simple technological operation can effectively carry out 2, the purification of 3-lutidine, obtain 2,3-lutidine purity is high.
The present invention adopts following technical scheme to achieve these goals:
The method of purification 2,3-lutidine is characterized in that may further comprise the steps:
(1) salify: successively add in salt oven with organic carboxyl acid 1150-1250kg terepthaloyl moietie 950-1050kg, 2,3 lutidine bullion 2950-3050kg, tetrafluoroethylene 550-650kg; Be warming up to 170-180 ℃ of backflow; Keep being cooled to normal temperature, stirred crystallization 55-65 minute after-filtration behind the 30-40min;
(2) filtered liq that step (1) is obtained is squeezed into the reaction kettle recrystallize, keeps 55-65 minute down at 4-6 ℃, filters, and solids filtered is incorporated into the salt oven salify into;
(3) salify solids wash: solid behind step (2) salify is soaked 25-35min with 2-3 washing by soaking of ethanol at every turn, and solid-like detection 2,3-lutidine purity are got in press filtration;
(4) resolve: the solid that step (3) press filtration is obtained adds in the extraction-container, and adds 1.8-2.2 times of water dissolution of solid weight, transfers system PH to 7-9 with liquid caustic soda, stirs and detects 2 behind the 15-20min again, 3-lutidine purity, is distilled to no oil droplet and steams;
(5) extraction, precipitation: water is as the distillate of extraction liquid extraction step (4) gained, and oily water separation obtains oil reservoir, puts into precipitation still precipitation to oil reservoir then, obtains 2,3 lutidine elaboration.
The method of purification of described 2,3-lutidine, it is characterized in that: described organic carboxyl acid is selected from YD 30.
Beneficial effect of the present invention:
Preparing method of the present invention is simple, through simple technological operation can effectively carry out 2, the purification of 3-lutidine, obtain 2,3-lutidine purity is high.
Embodiment
Embodiment:The method of purification 2,3-lutidine may further comprise the steps:
(1) salify: successively add in salt oven with YD 30 1200kg terepthaloyl moietie 1000kg, 2,3 lutidine bullion 3000kg, tetrafluoroethylene 600kg; Be warming up to 170-180 ℃ of backflow; Keep being cooled to normal temperature, stirred crystallization 55-65 minute after-filtration behind the 30-40min;
(2) filtered liq that step (1) is obtained is squeezed into the reaction kettle recrystallize, keeps 55-65 minute down at 4-6 ℃, filters, and solids filtered is incorporated into the salt oven salify into;
(3) salify solids wash: solid behind step (2) salify is soaked 25-35min with 2-3 washing by soaking of ethanol at every turn, and solid-like detection 2,3-lutidine purity are got in press filtration;
(4) resolve: the solid that step (3) press filtration is obtained adds in the extraction-container, and adds 1.8-2.2 times of water dissolution of solid weight, transfers system PH to 7-9 with liquid caustic soda, stirs and detects 2 behind the 15-20min again, 3-lutidine purity, is distilled to no oil droplet and steams;
(5) extraction, precipitation: water is as the distillate of extraction liquid extraction step (4) gained, and oily water separation obtains oil reservoir, puts into precipitation still precipitation to oil reservoir then, obtains 2,3 lutidine elaboration.
Claims (2)
- One kind purify 2, the method for 3-lutidine, it is characterized in that may further comprise the steps:(1) salify: successively add in salt oven with organic carboxyl acid 1150-1250kg terepthaloyl moietie 950-1050kg, 2,3 lutidine bullion 2950-3050kg, tetrafluoroethylene 550-650kg; Be warming up to 170-180 ℃ of backflow; Keep being cooled to normal temperature, stirred crystallization 55-65 minute after-filtration behind the 30-40min;(2) filtered liq that step (1) is obtained is squeezed into the reaction kettle recrystallize, keeps 55-65 minute down at 4-6 ℃, filters, and solids filtered is incorporated into the salt oven salify into;(3) salify solids wash: solid behind step (2) salify is soaked 25-35min with 2-3 washing by soaking of ethanol at every turn, and solid-like detection 2,3-lutidine purity are got in press filtration;(4) resolve: the solid that step (3) press filtration is obtained adds in the extraction-container, and adds 1.8-2.2 times of water dissolution of solid weight, transfers system PH to 7-9 with liquid caustic soda, stirs and detects 2 behind the 15-20min again, 3-lutidine purity, is distilled to no oil droplet and steams;(5) extraction, precipitation: water is as the distillate of extraction liquid extraction step (4) gained, and oily water separation obtains oil reservoir, puts into precipitation still precipitation to oil reservoir then, obtains 2,3 lutidine elaboration.
- 2. the method for purification of according to claim 12,3-lutidine, it is characterized in that: described organic carboxyl acid is selected from YD 30.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103297196A CN102408371A (en) | 2011-10-27 | 2011-10-27 | Method for purifying 2,3-dimethyl pyridine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103297196A CN102408371A (en) | 2011-10-27 | 2011-10-27 | Method for purifying 2,3-dimethyl pyridine |
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| CN102408371A true CN102408371A (en) | 2012-04-11 |
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| CN2011103297196A Pending CN102408371A (en) | 2011-10-27 | 2011-10-27 | Method for purifying 2,3-dimethyl pyridine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977005A (en) * | 2012-11-08 | 2013-03-20 | 安徽国星生物化学有限公司 | 2,3,5-trimethylpyridine purification method |
| CN103030592A (en) * | 2012-12-11 | 2013-04-10 | 安徽国星生物化学有限公司 | Purification method of 2, 3, 5-trimethyl pyridine by washing |
| CN104892493A (en) * | 2015-05-13 | 2015-09-09 | 安徽国星生物化学有限公司 | Separation and purification method of 2,3-dimethylpyridine |
-
2011
- 2011-10-27 CN CN2011103297196A patent/CN102408371A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102977005A (en) * | 2012-11-08 | 2013-03-20 | 安徽国星生物化学有限公司 | 2,3,5-trimethylpyridine purification method |
| CN103030592A (en) * | 2012-12-11 | 2013-04-10 | 安徽国星生物化学有限公司 | Purification method of 2, 3, 5-trimethyl pyridine by washing |
| CN104892493A (en) * | 2015-05-13 | 2015-09-09 | 安徽国星生物化学有限公司 | Separation and purification method of 2,3-dimethylpyridine |
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Application publication date: 20120411 |