CN102382045A - Purification of 2,3-dimethyl pyridine - Google Patents
Purification of 2,3-dimethyl pyridine Download PDFInfo
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- CN102382045A CN102382045A CN2011103297139A CN201110329713A CN102382045A CN 102382045 A CN102382045 A CN 102382045A CN 2011103297139 A CN2011103297139 A CN 2011103297139A CN 201110329713 A CN201110329713 A CN 201110329713A CN 102382045 A CN102382045 A CN 102382045A
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- lutidine
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Abstract
The invention discloses a purification method of 2,3-dimethyl pyridine, which mainly includes the following steps: adding ethanol, ethyl acetate, acetone and dibasic acid in crude 2,3-dimethyl pyridine and then conducting salification, crystallization, washing, resolving, extraction and desolvation in sequence to obtain refined 2,3-dimethyl pyridine. The preparation method is simple; the purification of the 2,3-dimethyl pyridine can be effectively conducted by simple technological operation; and the obtained 2,3-dimethyl pyridine is high in purity.
Description
Technical field
The present invention relates to a kind of chemical purification method, be specifically related to method of purification a kind of 2, the 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 2, the purification of 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:
2, the method for purification of 3-lutidine is characterized in that may further comprise the steps:
(1) salify: successively add in salt oven with diprotic acid 1150-1250kg ethanol 1950-2050kg, ETHYLE ACETATE 450-550kg, 2,3 lutidine bullion 2950-3050kg, acetone 280-320kg; 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 purification of described 2,3-lutidine, it is characterized in that: described diprotic acid can be selected from any diprotic acid.
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 1:2, the method for purification of 3-lutidine may further comprise the steps:
(1) salify: successively add in salt oven with sulfuric acid 1200kg ethanol 2000kg, ETHYLE ACETATE 500kg, 2,3 lutidine bullion 3000kg, acetone 300kg; 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.
Embodiment 2: 2, the method for purification of 3-lutidine may further comprise the steps:
(1) salify: successively add in salt oven with oxalic acid 1200kg ethanol 2000kg, ETHYLE ACETATE 500kg, 2,3 lutidine bullion 3000kg, acetone 300kg; 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)
1.2, the method for purification of 3-lutidine, it is characterized in that may further comprise the steps:
(1) salify: successively add in salt oven with diprotic acid 1150-1250kg ethanol 1950-2050kg, ETHYLE ACETATE 450-550kg, 2,3 lutidine bullion 2950-3050kg, acetone 280-320kg; 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 purification of according to claim 12,3-lutidine, it is characterized in that: described diprotic acid can be selected from any diprotic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103297139A CN102382045A (en) | 2011-10-27 | 2011-10-27 | Purification of 2,3-dimethyl pyridine |
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| CN2011103297139A CN102382045A (en) | 2011-10-27 | 2011-10-27 | Purification of 2,3-dimethyl pyridine |
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| CN102382045A true CN102382045A (en) | 2012-03-21 |
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| CN2011103297139A Pending CN102382045A (en) | 2011-10-27 | 2011-10-27 | Purification of 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962636A (en) * | 2006-11-21 | 2007-05-16 | 浙江大学 | 2,Process for preparing 3-dimethylpyridine |
| CN1966494A (en) * | 2006-10-19 | 2007-05-23 | 沙隆达集团公司 | 2-chloro-5-chloromethyl pyridine refining method |
| CN101648907A (en) * | 2009-09-14 | 2010-02-17 | 南京第一农药集团有限公司 | Purifying method of 2-chloromethyl-4-methoxyl-3,5-dimethylpyridine chloride |
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2011
- 2011-10-27 CN CN2011103297139A patent/CN102382045A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1966494A (en) * | 2006-10-19 | 2007-05-23 | 沙隆达集团公司 | 2-chloro-5-chloromethyl pyridine refining method |
| CN1962636A (en) * | 2006-11-21 | 2007-05-16 | 浙江大学 | 2,Process for preparing 3-dimethylpyridine |
| CN101648907A (en) * | 2009-09-14 | 2010-02-17 | 南京第一农药集团有限公司 | Purifying method of 2-chloromethyl-4-methoxyl-3,5-dimethylpyridine chloride |
Non-Patent Citations (1)
| Title |
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| 谢全安等: "粗轻吡啶精制研究", 《燃料与化工》 * |
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: 20120321 |