CN101979381A - Method for refining crude quinoline by continuous rectification - Google Patents
Method for refining crude quinoline by continuous rectification Download PDFInfo
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- CN101979381A CN101979381A CN 201010572864 CN201010572864A CN101979381A CN 101979381 A CN101979381 A CN 101979381A CN 201010572864 CN201010572864 CN 201010572864 CN 201010572864 A CN201010572864 A CN 201010572864A CN 101979381 A CN101979381 A CN 101979381A
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Abstract
The invention discloses a method for refining crude quinoline by continuous rectification. The method comprises the following working steps of: making the crude quinoline into a heavy component removing rectifying tower; removing heavy component impurities from the bottom of the tower; extracting steam from the top of the tower; transferring the steam into a heat exchanger; refluxing part of fluid which is condensed by using the heat exchanger; making the other part of the fluid which is condensed by using the heat exchanger enter a light component removing rectifying tower in a feeding form; vaporizing light component impurities from the liquid which enters the light component removing rectifying tower from the top of the tower; making part of a material flow enter the heat exchanger from the bottom of the tower; making the other part of the material flow enter a quinoline rectifying tower; and extracting a refined quinoline product from the top of the tower and extracting a crude isoquinoline product from the bottom of the tower from the material flow which enters the quinoline rectifying tower. In the method, the refined quinoline product with the purity of 99.5 percent is obtained by taking the crude quinoline separated from coal tar as a raw material, removing the heavy component impurities and the light component impurities by using the heavy component removing rectifying tower and the light component removing rectifying tower respectively, and refining by using the quinoline rectifying tower. The method has the advantages that: the method is simple and is easy to operate, the quality of a product is improved, and the energy source and the production cost are saved.
Description
Technical field
The present invention relates to a kind of method of refining thick quinoline, in particular, the present invention relates to a kind of method of producing smart quinoline by thick quinoline.
Background technology
Quinoline is a kind of important organic synthesis raw material, and being used for tobacco curing acid system, oxine system and quinine in medicine industry is medicine, also can make Nikethamide and wormer, control pyelonephritis medicine and analgesic agent etc.; Also can produce photopigment raw material, thiofide, flotation agent, restrainer and the agricultural chemicals etc. of dyestuff and photograph usefulness.Since synthesis method building-up process complexity, the expense costliness, and can not satisfy the needs that industry increases.Existing quinoline is mainly derived from the coal tar chemical industry, and directly from coal tar isolated quinoline purity lower, can not satisfy the needs of medicine, dyestuff and rubber industry, therefore, design a kind of novel quinoline process for refining and have great significance.
Existing thick quinoline process for purification has, phosphate process, sulphate process, hydrochloric acid-benzene counter-current extraction, azeotropic distillation and batch fractionating method.Phosphate process wherein, sulphate process and hydrochloric acid-benzene counter-current extraction all has strong acid to participate in separating, and to having relatively high expectations of equipment performance, the production technique relative complex produces waste water simultaneously, increases production cost; Azeotropic distillation wherein though avoided the generation of waste water, need to add a large amount of entrainers, and entrainer easily remains in the quinoline product, influences product quality.
Summary of the invention
Problem to be solved by this invention overcomes the defective of prior art exactly, and provides a kind of for this reason can make with extra care and obtain the method for purity greater than the refining thick quinoline of the continuous rectification of 99.5% quinoline product to the thick quinoline that obtains from coal tar wash oil.
The method of the refining thick quinoline of continuous rectification of the present invention, the system component that is adopted comprise takes off heavy rectifying tower, takes off light rectifying tower and quinoline rectifying tower; Be provided with the weight-removing column reboiler at the bottom of the described tower that takes off heavy rectifying tower; Describedly take off light rectifying tower
Cat head is provided with condenser of light component removal column, and is provided with the condensation reboiler at the bottom of its tower; The cat head of described quinoline rectifying tower is provided with quinoline tower condenser, and is provided with quinoline tower reboiler at the bottom of its tower; Its algorithm comprises two kinds of flow processs:
First kind of workflow is atmospheric tower or pressurizing tower to take off heavy rectifying tower, and taking off light rectifying tower is vacuum distillation tower, and its algorithm is as follows:
(1) thick quinoline enters and takes off heavy rectifying tower 1, gets rid of heavy constituent impurity at the bottom of the tower of this tower, and overhead vapours is then from the cat head extraction and enter the condensation reboiler;
(2) through the condensed liquid of condensation reboiler, partial reflux, part enters with the charging form takes off light rectifying tower;
(3) enter the liquid that takes off light rectifying tower, steam light constituent impurity in this column overhead, the tower base stream part enters the condensation reboiler and vaporizes at the bottom of tower, and part enters the quinoline rectifying tower;
(4) enter the logistics of quinoline rectifying tower, in the smart quinoline product of this column overhead extraction, thick isoquinoline 99.9 product extraction at the bottom of tower of by-product.
Second kind of workflow is vacuum distillation tower to take off light rectifying tower, and taking off heavy rectifying tower is atmospheric tower or pressurizing tower, and its step is as follows:
(1) thick quinoline enters and takes off light rectifying tower, and at the cat head extraction light constituent of this tower, the tower base stream part enters the condenser vaporization of boiling again at the bottom of tower, and part enters with the form of charging takes off heavy rectifying tower;
(2) enter the logistics of taking off heavy rectifying tower, extraction heavy constituent at the bottom of this Tata, overhead vapours is through the condenser condenses of boiling again, and partial reflux partly enters the quinoline rectifying tower;
(3) enter the logistics of quinoline rectifying tower, in the smart quinoline product of this column overhead extraction, thick isoquinoline 99.9 product extraction at the bottom of tower of by-product.
The method of the refining thick quinoline of continuous rectification of the present invention compared with prior art has following advantage:
(1) adopt the mode of continuous rectification to carry out removing of light constituent impurity and heavy constituent impurity, process is continuous, locates
The reason amount is big, and equipment and operation are all fairly simple.
(2) processing mode of employing double-effect rectification not only can make the quinoline product purity that obtains greater than 99.5%, and reach energy-conservation 30% effect.
(3) when obtaining the smart quinoline of high purity, isolate thick isoquinoline 99.9 product, can make the content of thick isoquinoline 99.9 reach 99%.
Description of drawings
Fig. 1 is the synoptic diagram of first kind of flow process of the present invention;
Fig. 2 is the synoptic diagram of second kind of flow process of the present invention.
Reference numeral: 1-take off heavy rectifying tower; 2-take off light rectifying tower; 3-quinoline treating tower; 4-weight-removing column reboiler; 5-condensation reboiler; 6-condenser of light component removal column; 7-quinoline tower condenser; 8-quinoline tower reboiler.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
The method of the refining thick quinoline of continuous rectification of the present invention comprises Fig. 1, two kinds of workflows shown in Figure 2.
In the embodiment of workflow shown in Figure 1, be atmospheric tower or pressurizing tower to take off heavy rectifying tower 1, take off light rectifying tower 2 and be vacuum distillation tower; The described cat head that takes off heavy rectifying tower 1 has the steam heating effect, and Qi Tadi is provided with weight-removing column reboiler 4; The described cat head that takes off light rectifying tower 2 is provided with condenser of light component removal column 6, and Qi Tadi is provided with condensation reboiler 5; Press by adjusting tower, can make described vapor temperature of taking off heavy rectifying tower 1 cat head higher more than 15 ℃ than described stream temperature of taking off at the bottom of light rectifying tower 2 towers, its step is as follows:
(1) thick quinoline enters and takes off heavy rectifying tower 1, gets rid of heavy constituent impurity at the bottom of the tower of this tower, and overhead vapours is then from the cat head extraction and enter condensation reboiler 5;
(2) through described condensation reboiler 5 condensed liquid, partial reflux, part enters the described light rectifying tower 2 that takes off with the charging form;
(3) enter the described liquid that takes off light rectifying tower 2, steam light constituent impurity in this column overhead, stream portions at the bottom of the tower enters condensation reboiler 5 and vaporizes at the bottom of tower, part enters quinoline rectifying tower 3, the cat head of described quinoline rectifying tower 3 is provided with quinoline tower condenser 7, and Qi Tadi is provided with quinoline tower reboiler 8;
(4) enter the logistics of described quinoline rectifying tower 3, in the smart quinoline product of this column overhead extraction, thick isoquinoline 99.9 product extraction at the bottom of tower of by-product.
In the embodiment of workflow shown in Figure 2, be vacuum distillation tower to take off light rectifying tower 2, take off heavy rectifying tower 1 and be atmospheric tower or pressurizing tower; The described cat head that takes off heavy rectifying tower 1 has the steam heating effect, and Qi Tadi is provided with weight-removing column
Reboiler 4; The described cat head that takes off light rectifying tower 2 is provided with condenser of light component removal column 6, and Qi Tadi is provided with condensation reboiler 5; Press to make and take off heavy rectifying tower overhead vapours temperature ratio to take off light rectifying tower tower base stream temperature high more than 15 ℃ by adjusting tower, its step is as follows:
(1) thick quinoline enters and takes off light rectifying tower 2, and at the cat head extraction light constituent of this tower, the tower base stream part enters condenser 5 vaporizations of boiling again at the bottom of tower, and part enters with the form of charging takes off heavy rectifying tower 1;
(2) enter described logistics of taking off heavy rectifying tower 1, extraction heavy constituent at the bottom of this Tata, the steam of cat head is through condenser 5 condensations of boiling again, and partial reflux partly enters quinoline rectifying tower 3; The cat head of described quinoline rectifying tower 3 is provided with quinoline tower condenser 7, and Qi Tadi is provided with quinoline tower reboiler 8;
(3) enter the logistics of described quinoline rectifying tower 3, in the smart quinoline product of this column overhead extraction, thick isoquinoline 99.9 product extraction at the bottom of tower of by-product.
The refining thick quinoline of continuous rectification of the present invention method adopted takes off heavy rectifying tower 1, take off light rectifying tower 2 and quinoline rectifying tower 3, both can be that packing tower also can be a tray column.For packing tower, its filler should preferred double-deck screen waviness structured packing.
The method of the refining thick quinoline of continuous rectification of the present invention, with the thick quinoline of isolated lower concentration from coal tar is raw material, remove heavy constituent impurity and light constituent impurity through taking off heavy rectifying tower and taking off light rectifying tower respectively, make with extra care by the quinoline rectifying tower again, obtain the smart quinoline product of purity 99.5%.The mode of producing of its double-effect rectification has not only improved product quality, and has saved the energy and production cost.
Below in conjunction with the accompanying drawings and embodiments the method for the refining thick quinoline of continuous rectification of the present invention is schematically described.Those skilled in the art will be understood that under enlightenment of the present invention other staff also may make and its similar methods design.Special needs to be pointed out is that only otherwise break away from aim of the present invention, the design that all are similar to the present invention is all within the present invention's scope required for protection.
Claims (2)
1. the method for the refining thick quinoline of a continuous rectification, the system component that is adopted comprise takes off heavy rectifying tower, takes off light rectifying tower and quinoline rectifying tower; Be provided with the weight-removing column reboiler at the bottom of the described tower that takes off heavy rectifying tower; The described cat head that takes off light rectifying tower is provided with condenser of light component removal column, and is provided with the condensation reboiler at the bottom of its tower; The cat head of described quinoline rectifying tower is provided with quinoline tower condenser, and is provided with quinoline tower reboiler at the bottom of its tower; Its algorithm comprises two kinds of flow processs:
First kind of workflow is atmospheric tower or pressurizing tower to take off heavy rectifying tower, and taking off light rectifying tower is vacuum distillation tower, and its algorithm is as follows:
Thick quinoline enters and takes off heavy rectifying tower 1, gets rid of heavy constituent impurity at the bottom of the tower of this tower, and overhead vapours is then from the cat head extraction and enter the condensation reboiler;
Through the condensed liquid of condensation reboiler, partial reflux, part enters with the charging form takes off light rectifying tower;
Enter the liquid that takes off light rectifying tower, steam light constituent impurity in this column overhead, the tower base stream part enters the condensation reboiler and vaporizes at the bottom of tower, and part enters the quinoline rectifying tower;
Enter the logistics of quinoline rectifying tower, in the smart quinoline product of this column overhead extraction, thick isoquinoline 99.9 product extraction at the bottom of tower of by-product;
Second kind of workflow is vacuum distillation tower to take off light rectifying tower, and taking off heavy rectifying tower is atmospheric tower or pressurizing tower, and its step is as follows:
(1) thick quinoline enters and takes off light rectifying tower, and at the cat head extraction light constituent of this tower, the tower base stream part enters the condenser vaporization of boiling again at the bottom of tower, and part enters with the form of charging takes off heavy rectifying tower;
(2) enter the logistics of taking off heavy rectifying tower, extraction heavy constituent at the bottom of this Tata, overhead vapours is through the condenser condenses of boiling again, and partial reflux partly enters the quinoline rectifying tower;
(3) enter the logistics of quinoline rectifying tower, in the smart quinoline product of this column overhead extraction, thick isoquinoline 99.9 product extraction at the bottom of tower of by-product.
2. the method for the refining thick quinoline of continuous rectification according to claim 1 is characterized in that, that adopts in this method describedly takes off heavy rectifying tower, takes off light rectifying tower and the quinoline rectifying tower is packing tower or tray column.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105728642A CN101979381B (en) | 2010-12-05 | 2010-12-05 | Method for refining crude quinoline by continuous rectification |
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| CN2010105728642A CN101979381B (en) | 2010-12-05 | 2010-12-05 | Method for refining crude quinoline by continuous rectification |
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| CN101979381A true CN101979381A (en) | 2011-02-23 |
| CN101979381B CN101979381B (en) | 2012-05-23 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107648976A (en) * | 2017-09-22 | 2018-02-02 | 杭州杭氧股份有限公司 | A kind of cryogenic separation produces the method and cryogenic separation system of ultra-pure gases |
| CN108276315A (en) * | 2017-12-29 | 2018-07-13 | 中国船舶重工集团公司第七八研究所 | A kind of purification process of trifluoromethanesulfonic acid |
| CN108393022A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | Isoquinoline blending device and process |
| CN110980648A (en) * | 2019-12-31 | 2020-04-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen bromide purification device and method |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61161265A (en) * | 1985-01-09 | 1986-07-21 | Sumikin Coke Co Ltd | Recovery of quinoline |
| 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 |
-
2010
- 2010-12-05 CN CN2010105728642A patent/CN101979381B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61161265A (en) * | 1985-01-09 | 1986-07-21 | Sumikin Coke Co Ltd | Recovery of quinoline |
| 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 |
Non-Patent Citations (1)
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| 《科技情报开发与经济》 19951231 米杰等 喹啉的加工和利用 20 1-2 第5卷, 第6期 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108393022B (en) * | 2017-02-08 | 2021-04-02 | 鞍钢股份有限公司 | Isoquinoline blending device and process |
| CN107648976A (en) * | 2017-09-22 | 2018-02-02 | 杭州杭氧股份有限公司 | A kind of cryogenic separation produces the method and cryogenic separation system of ultra-pure gases |
| CN107648976B (en) * | 2017-09-22 | 2020-10-09 | 衢州杭氧气体有限公司 | Method for preparing ultra-high-purity gas through low-temperature separation and low-temperature separation system |
| CN108276315A (en) * | 2017-12-29 | 2018-07-13 | 中国船舶重工集团公司第七八研究所 | A kind of purification process of trifluoromethanesulfonic acid |
| CN110980648A (en) * | 2019-12-31 | 2020-04-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen bromide purification device and method |
| 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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| CN101979381B (en) | 2012-05-23 |
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Granted publication date: 20120523 Termination date: 20211205 |