CN1974556A - Method for producing refined quinoline by using quinoline fraction as raw material - Google Patents
Method for producing refined quinoline by using quinoline fraction as raw material Download PDFInfo
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- CN1974556A CN1974556A CN 200610134602 CN200610134602A CN1974556A CN 1974556 A CN1974556 A CN 1974556A CN 200610134602 CN200610134602 CN 200610134602 CN 200610134602 A CN200610134602 A CN 200610134602A CN 1974556 A CN1974556 A CN 1974556A
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- China
- Prior art keywords
- quinoline
- raw material
- refining
- content
- cut
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 title claims abstract description 180
- 239000002994 raw material Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000007670 refining Methods 0.000 claims abstract description 25
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims description 9
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000003245 coal Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 abstract 1
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- ZPHQBFRCXUIIAZ-UHFFFAOYSA-N benzene;hydrochloride Chemical compound Cl.C1=CC=CC=C1 ZPHQBFRCXUIIAZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- JBCOJMLCNNXIIK-UHFFFAOYSA-N phosphoric acid;quinoline Chemical compound OP(O)(O)=O.N1=CC=CC2=CC=CC=C21 JBCOJMLCNNXIIK-UHFFFAOYSA-N 0.000 description 2
- 229910021653 sulphate ion Inorganic materials 0.000 description 2
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- WSZKUEZEYFNPID-UHFFFAOYSA-N hydrogen sulfate;quinolin-1-ium Chemical compound OS(O)(=O)=O.N1=CC=CC2=CC=CC=C21 WSZKUEZEYFNPID-UHFFFAOYSA-N 0.000 description 1
- AVGOEQMXIZKPOL-UHFFFAOYSA-N isoquinoline phosphoric acid Chemical compound P(=O)(O)(O)O.C1=NC=CC2=CC=CC=C12 AVGOEQMXIZKPOL-UHFFFAOYSA-N 0.000 description 1
- PNVXLEZHGVTRFM-UHFFFAOYSA-N isoquinoline;sulfuric acid Chemical compound OS(O)(=O)=O.C1=NC=CC2=CC=CC=C21 PNVXLEZHGVTRFM-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for producing refined quinoline by using quinoline fraction as a raw material in the technical field of coal chemical industry, which comprises the following steps: 1) loading raw material bipyridine with the quinoline content of 25% -35% into a rough rectification kettle for heating, carrying out reduced pressure distillation in a rough rectification tower with the theoretical plate number of 30-40, and collecting quinoline fraction with the quinoline content of more than 65%; 2) and (3) putting the quinoline fraction serving as a raw material into a refining rectifying kettle for heating, and carrying out reduced pressure distillation in a refining rectifying tower with theoretical plate number of 60-90 to obtain refined quinoline with quinoline content of more than 99%. The method takes quinoline fraction as a raw material, the quinoline fraction is rectified for one time to produce rectified quinoline, and an efficient rectifying tower is adopted in the rectification production of the quinoline, and the quinoline content is more than 99 percent.
Description
Technical field
The present invention relates to technical field of coal chemical industry, be a kind of be the method for the refining quinoline of raw material production with the quinoline cut.
Background technology
Existing quinoline production technique is to be raw material with heavy pyridine in the tar, by rectifying extraction quinoline content greater than 55% quinoline cut, be raw material with the quinoline cut then, rectifying obtains technical quinoline, and (quality is that 235 ℃～240 ℃ quantity of distillate are not less than 95%, quinoline content is greater than 90%), technical quinoline is because quinoline content is low, and sale is restricted, and quinoline content is wider greater than 99% refining quinoline purposes, and market sale is better.
The separation and refining method of quinoline, nearly following several: phosphate process, sulphate process, rectification method, hydrochloric acid-benzene counter-current extraction.
(1) phosphate process: this method is that different solubility in water is realized isolating according to phosphoric acid quinoline and phosphoric acid isoquinoline 99.9.Phosphoric acid isoquinoline 99.9 is soluble in water, and the phosphoric acid quinoline is then not soluble in water.
(2) sulphate process: this method is the difference of the solubleness in ethanol according to quinoline sulfate and sulfuric acid isoquinoline 99.9 and isolating.
(3) rectification method:, utilize quinoline to separate with the isoquinoline 99.9 boiling-point difference by rectifying tower.
(4) hydrochloric acid-benzene counter-current extraction: utilize the alkalescence of isoquinoline 99.9 stronger slightly, quinoline is concentrated in the benzene gradually, and isoquinoline 99.9 is concentrated in the hydrochloric acid than quinoline.
Comparatively speaking, all select for use strong acid to do reactant in (1), (2), (4) method, the equipment requirements height, the technology relative complex, and method (3) does not have strong acid, technology is simple relatively, so we select the method for the method of rectifying as development for use.The production of rectifying is used wider at chemical general factory, the particularly use of tray column, but board-like column efficiency is lower, is difficult to satisfy.
Through the domestic literature retrieval, find and three pieces of this project pertinent literatures:
1, Chinese patent " producing the method for smart quinoline from technical quinoline ", the patent No.: ZL99112606.8, publication number: 1259516;
2, Chinese patent " method of refining quinoline from the coal tar crude quinoline ", the patent No.: ZL96117038.7, publication number: 1172106;
3, network information: www.aggroupchem.com/about-c.htm
Check result is with to look into the contrast of new point as follows: it is described to look into new point one, with quinoline cut (content is greater than 65%) is raw material, smart quinoline (content is greater than 98.5%) is produced in a rectifying: wherein be raw material with the quinoline, existing mentioning in document one, but its material content is different with this authorized item with technology.It is described to look into new point two, adopts corrugated-plate packed tower to replace bubble-plate column production, does not see that document mentions.
Conclusion is as follows: this client is a raw material with quinoline cut (content is greater than 65%), and smart quinoline (content is greater than 98.5%) is produced in a rectifying, and adopts corrugated-plate packed tower to replace bubble-plate column in quinoline rectifying is produced, and does not domesticly see bibliographical information.
Summary of the invention
The purpose of this invention is to provide a kind of is the method for the refining quinoline of raw material production with the quinoline cut, this method is to be raw material with quinoline cut (quinoline content is greater than 65%), smart quinoline (quinoline content is greater than 99%) is produced in a rectifying, and adopts high-efficient spiral-screen column in quinoline rectifying is produced.
For achieving the above object, the present invention adopts following technical scheme to realize:
With the quinoline cut is the method for the refining quinoline of raw material production, it is characterized in that this method comprises the steps:
1) the heavy pyridine of the raw material of quinoline content 25%～35% is packed into heat in the rough rectifying still, underpressure distillation in the rough rectifying tower of 30～40 of theoretical stage number, extraction quinoline content is greater than 65% quinoline cut;
2) being that raw material is packed into and heated in the refining rectifying still with the quinoline cut, is underpressure distillation in 60～90 the refining rectifying tower in theoretical stage number, and extraction quinoline content is greater than 99% smart quinoline.
The top vacuum degree of described rough rectifying tower is 0.080～0.095MPa, and the pressure drop of tower vacuum is 0.015～0.035MPa.
The reflux ratio of described rough rectifying tower is 5-10.
The top vacuum degree of described refining rectifying tower is 0.080～0.095MPa, and the pressure drop of tower vacuum is 0.005～0.020MPa.
The reflux ratio of described refining rectifying tower is 5-20.
The present invention's beneficial effect compared with prior art is: this method is to be raw material with the quinoline cut, and smart quinoline is produced in a rectifying, and adopts high-efficient spiral-screen column in quinoline rectifying is produced, and quinoline content is greater than 99%.
Embodiment
With the quinoline cut is the method for the refining quinoline of raw material production, and this method comprises the steps:
1) the heavy pyridine of raw material (quinoline content 25%～35%) is packed into heats underpressure distillation in rough rectifying tower (30～40 of theoretical plate numbers), extraction quinoline cut (quinoline content is greater than 65%) in the rough rectifying still.The top vacuum degree is 0.080～0.095MPa, and the pressure drop of tower vacuum is 0.015～0.035MPa.
2) be that raw material is packed into and heated in the refining rectifying still with the quinoline cut, underpressure distillation in refining rectifying tower (theoretical plate number is 60～90), extraction quinoline cut (quinoline content is greater than 65%), technical quinoline (quinoline content is greater than 90%), smart quinoline (quinoline content is greater than 99%).The top vacuum degree is 0.080～0.095MPa, and the pressure drop of tower vacuum is 0.005～0.020MPa.
Claims (5)
1, is the method for the refining quinoline of raw material production with the quinoline cut, it is characterized in that this method comprises the steps:
1) the heavy pyridine of the raw material of quinoline content 25%～35% is packed into heat in the rough rectifying still, underpressure distillation in the rough rectifying tower of 30～40 of theoretical stage number, extraction quinoline content is greater than 65% quinoline cut;
2) being that raw material is packed into and heated in the refining rectifying still with the quinoline cut, is underpressure distillation in 60～90 the refining rectifying tower in theoretical stage number, and extraction quinoline content is greater than 99% smart quinoline.
2, according to claim 1 is the method for the refining quinoline of raw material production with the quinoline cut, and it is characterized in that: the top vacuum degree of described rough rectifying tower is 0.080～0.095MPa, and the pressure drop of tower vacuum is 0.015～0.035MPa.
3, according to claim 1 is the method for the refining quinoline of raw material production with the quinoline cut, and it is characterized in that: the reflux ratio of described rough rectifying tower is 5-10.
4, according to claim 1 is the method for the refining quinoline of raw material production with the quinoline cut, and it is characterized in that: the top vacuum degree of described refining rectifying tower is 0.080～0.095MPa, and the pressure drop of tower vacuum is 0.005～0.020MPa.
5, according to claim 1 is the method for the refining quinoline of raw material production with the quinoline cut, and it is characterized in that: the reflux ratio of described refining rectifying tower is 5-20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610134602 CN1974556A (en) | 2006-12-08 | 2006-12-08 | Method for producing refined quinoline by using quinoline fraction as raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610134602 CN1974556A (en) | 2006-12-08 | 2006-12-08 | Method for producing refined quinoline by using quinoline fraction as raw material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1974556A true CN1974556A (en) | 2007-06-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610134602 Pending CN1974556A (en) | 2006-12-08 | 2006-12-08 | Method for producing refined quinoline by using quinoline fraction as raw material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1974556A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102603626A (en) * | 2012-03-30 | 2012-07-25 | 上海乾昆化工科技有限公司 | Separation and purification process of chinoline with high purity |
| CN108393022A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | Isoquinoline blending device and process |
| CN108395400A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | Process for industrially producing 2-methylquinoline fraction |
| CN114516816A (en) * | 2022-02-24 | 2022-05-20 | 深圳瑞华泰薄膜科技股份有限公司 | Method and device for recovering DMAC (dimethyl acetamide) and isoquinoline from solution |
-
2006
- 2006-12-08 CN CN 200610134602 patent/CN1974556A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101979381B (en) * | 2010-12-05 | 2012-05-23 | 天津市华瑞奕博化工科技有限公司 | Method for refining crude quinoline by continuous rectification |
| CN102603626A (en) * | 2012-03-30 | 2012-07-25 | 上海乾昆化工科技有限公司 | Separation and purification process of chinoline with high purity |
| CN108393022A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | Isoquinoline blending device and process |
| CN108395400A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | Process for industrially producing 2-methylquinoline fraction |
| CN114516816A (en) * | 2022-02-24 | 2022-05-20 | 深圳瑞华泰薄膜科技股份有限公司 | Method and device for recovering DMAC (dimethyl acetamide) and isoquinoline from solution |
| CN114516816B (en) * | 2022-02-24 | 2023-12-01 | 深圳瑞华泰薄膜科技股份有限公司 | Method and device for recycling DMAC and isoquinoline from solution |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| C12 | Rejection of a patent application after its publication | ||
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Open date: 20070606 |