CN102603626A - Separation and purification process of chinoline with high purity - Google Patents
Separation and purification process of chinoline with high purity Download PDFInfo
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- CN102603626A CN102603626A CN2012100909528A CN201210090952A CN102603626A CN 102603626 A CN102603626 A CN 102603626A CN 2012100909528 A CN2012100909528 A CN 2012100909528A CN 201210090952 A CN201210090952 A CN 201210090952A CN 102603626 A CN102603626 A CN 102603626A
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Abstract
The invention relates to a separation and purification process of chinoline with high purity. The process comprises the following steps of: (1) inputting coarse chinoline into a rectifying tower, carrying out decompress rectify, carrying out sampling analysis per hour, and cutting fractions to a middle slot A when the content of the chinoline rises up to more than 90%; (2) re-inputting materials which are in the middle slot A into the rectifying tower for secondary rectify, carrying out sampling analysis per hour, cutting components to an appointed middle slot B when the content of the chinoline rises up to more than 98%, collecting into an end product slot when the content of the chinoline directly rises up to 99%, and continuously cutting into the middle slot B after the content of the chinoline is lower than 99%; and (3) inputting materials which are in the middle slot B into the rectifying tower for third-time rectify, carrying out sampling analysis per hour, and collecting end products when the content of the chinoline rises up to 99%. Compared with the prior art, the process has the advantages of being low in cost, capable of industrial production and the like.
Description
Technical field
The present invention relates to a kind of quinoline purifying technique, especially relate to a kind of high purity quinoline process for separating and purifying.
Background technology
In the industry, quinoline mainly extracts or chemosynthesis from coal tar wash oil.It is traditional method that coal tar extracts, and coal tar is through acid, alkaline purification, and series of steps such as rectification and purification or recrystallization, produces the quinoline product.Chemical synthesis is a starting raw material with aromatic amine compounds such as aniline or anthranilic acids usually, obtains quinolines with unsaturated aldehydes or ketones generation addition reaction.
Extract the traditional technology of quinoline in the coal tar wash oil, contain impurity such as indoles inevitably, quinoline content is generally below 97%.Synthesis technique, though product purity can reach 99%, production cost is very high, can't industriallization.
Summary of the invention
But the object of the invention is exactly the high purity quinoline process for separating and purifying that the low suitability for industrialized production of a kind of cost is provided for the defective that overcomes above-mentioned prior art existence.
The object of the invention can be realized through following technical scheme: a kind of high purity quinoline process for separating and purifying, it is characterized in that, and may further comprise the steps:
(1) with in the thick quinoline input rectifying tower, in 160～185 ℃ of service temperatures, vacuum tightness-0.08～0.09Mpa; Carry out rectification under vacuum under the condition of reflux ratio 3～8, sampling analysis per hour is after quinoline content rises to greater than 90%; Impurity methylnaphthalene content less than 3% and impurity indoles content less than 2% o'clock, begin to cut cut to medial launder A, when impurity methylnaphthalene content surpass 3% or impurity indoles content surpass 2%; Stop to cut cut to medial launder A, change into conventional medial launder into;
(2), import rectifying tower once more and carry out secondary rectifying, 160～185 ℃ of the service temperatures of secondary rectifying, vacuum tightness-0.08～0.09Mpa with the material among the medial launder A; Reflux ratio 3～8, sampling analysis per hour is when quinoline content rises to 98%; Impurity methylnaphthalene content less than 1.2% and impurity indoles content less than 0.5% o'clock, the beginning cutting of components is to specifying medial launder B, after for some time; If quinoline content directly reaches 99%, then take in pan tank, if quinoline content is lower than 99% and continues to be cut to medial launder B; To impurity methylnaphthalene content surpass 1.2% or impurity indoles content surpass at 0.5% o'clock, stop to cut cut to medial launder B, change into conventional medial launder into;
(3) with the material of medial launder B, the input rectifying tower carries out three rectifying, 160～185 ℃ of the service temperatures of three rectifying, and vacuum tightness-0.08～0.09Mpa, reflux ratio 3～8, sampling analysis per hour, quinoline content rises to 99% and begins to collect finished product.
Described thick quinoline is with coal tar wash oil, obtains through acid, neutralizing treatment.
Described rectifying tower adopts the batch still distillation tower.
Compared with prior art, the present invention has the following advantages:
(1) produce 99% quinoline with conventional synthesis technique, yield is relatively low, and cost is very high; And this process using distil process, cost is low, goes for large industrialized production.
(2) existing former coal tar washing oil separates the purification quinoline, and purity is up to 97%, and this technology then through proprietary technological method and equipment, is rationally cut cut, obtains the product of purity more than 99%.
(3) the present invention is not changing under the original process equipment condition, through reasonable control cut, especially controls the cut foreign matter content, obtains the high purity quinoline, and in daily production, can realize producing in batches.
Embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
Embodiment 1
A kind of high purity quinoline process for separating and purifying may further comprise the steps:
With coal tar wash oil, through the thick quinoline that acid, neutralizing treatment obtain, quinoline component concentration 58% in the thick quinoline, methylnaphthalene content 2.41%, indoles content 1.45%.
(1) with in the thick quinoline input batch still distillation tower, in 160～185 ℃ of service temperatures, vacuum tightness-0.08～0.09Mpa; Carry out rectification under vacuum under the condition of reflux ratio 3～8, sampling analysis per hour, quinoline content rises to 90.31% (greater than 90%); This moment methylnaphthalene content 2.87% (less than 3%), indoles content 1.36% (less than 2%) begins to cut cut to medial launder A; Quinoline content 91.27% after for some time, at this moment, methylnaphthalene content 3.42% (surpassing 3%) or indoles content 2.09% (surpassing 2%); Stop to cut cut to medial launder A, change conventional medial launder into;
(2), import the batch still distillation tower once more and carry out secondary rectifying, 160～185 ℃ of the service temperatures of secondary rectifying with the material among the medial launder A; Vacuum tightness-0.08～0.09Mpa, reflux ratio 3～8, per hour sampling analysis; Quinoline content rises to 98.03% (greater than 98%), this moment methylnaphthalene content 1.18% (less than 1.2%), indoles content 0.14% (less than 0.5%); The beginning cutting of components is to specifying medial launder B, and after for some time, quinoline content directly reaches at 99% o'clock; The income pan tank is if quinoline content is lower than 99% continued and is cut to medial launder B, quinoline content 97.38%; Methylnaphthalene content 1.22% (surpassing 1.2%) or indoles content 0.57% (surpassing 0.5%) stop to cut cut to medial launder B, change into conventional medial launder into;
(3) with the material of medial launder B; Input batch still distillation tower carries out three rectifying, 160～185 ℃ of the service temperatures of three rectifying, vacuum tightness-0.08～0.09Mpa; Reflux ratio 3～8; Sampling analysis per hour, quinoline content rises to 99% and begins to collect finished product, and other cuts are as 98% product except that finished product.
Claims (3)
1. a high purity quinoline process for separating and purifying is characterized in that, may further comprise the steps:
(1) with in the thick quinoline input rectifying tower, in 160～185 ℃ of service temperatures, vacuum tightness-0.08～0.09Mpa; Carry out rectification under vacuum under the condition of reflux ratio 3～8, sampling analysis per hour is after quinoline content rises to greater than 90%; Impurity methylnaphthalene content less than 3% and impurity indoles content less than 2% o'clock, begin to cut cut to medial launder A, when impurity methylnaphthalene content surpass 3% or impurity indoles content surpass 2%; Stop to cut cut to medial launder A, change into conventional medial launder into;
(2), import rectifying tower once more and carry out secondary rectifying, 160～185 ℃ of the service temperatures of secondary rectifying, vacuum tightness-0.08～0.09Mpa with the material among the medial launder A; Reflux ratio 3～8, sampling analysis per hour is when quinoline content rises to 98%; Impurity methylnaphthalene content less than 1.2% and impurity indoles content less than 0.5% o'clock, the beginning cutting of components is to specifying medial launder B, after for some time; If quinoline content directly reaches 99%, then take in pan tank, if quinoline content is lower than 99% and continues to be cut to medial launder B; To impurity methylnaphthalene content surpass 1.2% or impurity indoles content surpass at 0.5% o'clock, stop to cut cut to medial launder B, change into conventional medial launder into;
(3) with the material of medial launder B, the input rectifying tower carries out three rectifying, 160～185 ℃ of the service temperatures of three rectifying, and vacuum tightness-0.08～0.09Mpa, reflux ratio 3～8, sampling analysis per hour, quinoline content rises to 99% and begins to collect finished product.
2. a kind of high purity quinoline process for separating and purifying according to claim 1 is characterized in that described thick quinoline is with coal tar wash oil, obtains through acid, neutralizing treatment.
3. a kind of high purity quinoline process for separating and purifying according to claim 1 is characterized in that, described rectifying tower adopts the batch still distillation tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100909528A CN102603626A (en) | 2012-03-30 | 2012-03-30 | Separation and purification process of chinoline with high purity |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100909528A CN102603626A (en) | 2012-03-30 | 2012-03-30 | Separation and purification process of chinoline with high purity |
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| CN102603626A true CN102603626A (en) | 2012-07-25 |
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| CN2012100909528A Pending CN102603626A (en) | 2012-03-30 | 2012-03-30 | Separation and purification process of chinoline with high purity |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110283083A (en) * | 2019-07-01 | 2019-09-27 | 西北大学 | The enrichment method of basic nitrogen compound in coal tar |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09151176A (en) * | 1995-11-30 | 1997-06-10 | Nippon Steel Chem Co Ltd | Separation and recovery of quinoline |
| CN1259516A (en) * | 1999-01-05 | 2000-07-12 | 鞍山钢铁集团公司 | Method for purifying industrial quinoline to produce fine products |
| CN1974556A (en) * | 2006-12-08 | 2007-06-06 | 鞍钢股份有限公司 | Method for producing refined quinoline by using quinoline fraction as raw material |
| CN101747269A (en) * | 2009-12-23 | 2010-06-23 | 上海新明高新科技发展有限公司 | Purification method of isoquinoline |
| CN101979381A (en) * | 2010-12-05 | 2011-02-23 | 天津市华瑞奕博化工科技有限公司 | Method for refining crude quinoline by continuous rectification |
-
2012
- 2012-03-30 CN CN2012100909528A patent/CN102603626A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09151176A (en) * | 1995-11-30 | 1997-06-10 | Nippon Steel Chem Co Ltd | Separation and recovery of quinoline |
| CN1259516A (en) * | 1999-01-05 | 2000-07-12 | 鞍山钢铁集团公司 | Method for purifying industrial quinoline to produce fine products |
| CN1974556A (en) * | 2006-12-08 | 2007-06-06 | 鞍钢股份有限公司 | Method for producing refined quinoline by using quinoline fraction as raw material |
| CN101747269A (en) * | 2009-12-23 | 2010-06-23 | 上海新明高新科技发展有限公司 | Purification method of isoquinoline |
| CN101979381A (en) * | 2010-12-05 | 2011-02-23 | 天津市华瑞奕博化工科技有限公司 | Method for refining crude quinoline by continuous rectification |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110283083A (en) * | 2019-07-01 | 2019-09-27 | 西北大学 | The enrichment method of basic nitrogen compound in coal tar |
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Application publication date: 20120725 |