CN101993704A - Method for removing quinoline insoluble substances in coal tar pitch - Google Patents
Method for removing quinoline insoluble substances in coal tar pitch Download PDFInfo
- Publication number
- CN101993704A CN101993704A CN2009100567783A CN200910056778A CN101993704A CN 101993704 A CN101993704 A CN 101993704A CN 2009100567783 A CN2009100567783 A CN 2009100567783A CN 200910056778 A CN200910056778 A CN 200910056778A CN 101993704 A CN101993704 A CN 101993704A
- Authority
- CN
- China
- Prior art keywords
- coal
- tar pitch
- quinoline insolubles
- solvent
- removes
- 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.)
- Pending
Links
Landscapes
- Working-Up Tar And Pitch (AREA)
Abstract
The invention provides a method for removing quinoline insoluble substances in coal tar pitch, comprising the following steps of: (1) mixing the coal tar pitch with a solvent and then heating; (2) making a mixture obtained in the step (1) continuously enter into a centrifugal machine, and continuously throwing heavy slag out to obtain light phase liquid; (3) making the light phase liquid obtained in the step (2) continuously enter into the lower part of a settling tank, settling the quinoline insoluble substances, and continuously discharging clear liquid not containing the quinoline insoluble substances from the upper part of the settling tank; (4) distilling the clear liquid not containing the quinoline insoluble substances to obtain a purified product; and (5) recovering the solvent for cycle use. The content of the quinoline insoluble substances in the purified product is 0.06-0.11 percent, the yield of the purified product is 75-88 percent, and the solvent recovery rate is 95.7-98.7 percent. Compared with the prior art, the method has great improvements in the aspects of product quality, device energy consumption, solvent loss, process operation and the like.
Description
Technical field
The present invention relates to field of coal tar deep processing, specifically, the present invention relates to a kind of method that removes the quinoline insolubles in the coal-tar pitch.
Background technology
Formation with contained quinoline insolubles (QI) in the coal-tar pitch is distinguished, and QI can be divided into primary QI and secondary QI.Primary QI forms in the coal tar process, is present in the coal tar, and when coal tar distillation was handled, this part QI transferred in the coal-tar pitch again.Primary QI is made of inorganic QI and organic QI, inorganic QI is that the coal ash particle, furnace wall refractory brick powder, iron filings and the oxide powder thereof that are brought in the coal tar by rising coal gas stream in the coal tar process constitute, this part inorganic QI particle diameter is about 10 μ m, its content is less, adheres to more or is included in bigger organic QI component.The organic moiety of primary QI is mainly formed by the aromatic hydrocarbons thermopolymerization at high temperature that molecular weight is low in contained big aromatic hydrocarbon molecule thermally splitting or the crackate in the coal, and its median size is about 0.5 μ m.
The production of coal-based needle coke, coal-tar pitch based carbon fiber, coal-tar pitch soaker and mesophase pitch preparation all needs the purification coal-tar pitch raw material of low quinoline insolubles content, and is that the impurity of representative can seriously hinder producing of above-mentioned high-quality high added value coal-tar pitch product with primary QI in the coal tar.Simultaneously, the coal tar impurities easily causes the obstruction of coal tar deep processing equipment, thereby influences the quality of coal tar deep processing product, therefore, is necessary coal tar or coal-tar pitch are carried out purifying treatment, to remove its contained primary QI impurity.
The removal methods of the quinoline insolubles in the existing coal-tar pitch mainly contains standing sedimentation separation, centrifugation, thermosol filtration, solvent extraction, solvent flocculation etc.But aforesaid method respectively has shortcoming: the decontamination effect improving of standing sedimentation partition method is poor, and QI content is more than 1%; Centrifugal separation equipment working cost height, treatment capacity are little, the QI content of purified product is more than 0.2%; The thermosol filtration method requires harsh to filter screen, need pressure treatment, and working cost is higher; The solvent treatment method decontamination effect improving is better, but solvent load is big, the big and unclear industrialization difficulty height that causes in two interfaces of the dregs of fat of process energy consumption; The yield of the purified product of solvent extraction and solvent flocculence is low.The common drawback of above method is that industrial value is little.
Chinese patent literature CN1793287 discloses a kind of production method of purifying pitch, this method is the solvent settling process, its main drawback is to adopt stirring tank as the mixing and the QI precipitation apparatus of raw material and solvent, and this just causes following problem: 1, the unclear QI content height that causes purifying pitch in two interfaces of the dregs of fat; 2, to realize the industrialization operate continuously, must have a plurality of stirring tanks to switch and use that so, facility investment is bigger; 3 owing to be periodical operation, pollutes supernatant liquid for fear of the bottom sediment, when extracting the supernatant liquid of stirring tank out, just can not fully it be taken out to the greatest extent, like this, thereby will cause the clear liquid loss to reduce product yield; 4, solvent load is big, causes the energy consumption of solvent recuperation operation higher; 5, settling temperature height, the also corresponding raising of energy consumption of device operation, and the loss through volatilization height of solvent.
Therefore, for overcoming the shortcoming that aforesaid method exists, the object of the present invention is to provide the continuous production technology that removes quinoline insolubles of a kind of new coal-tar pitch etc.
Summary of the invention
The invention provides a kind of method that removes the quinoline insolubles in the coal-tar pitch, may further comprise the steps:
(1) with coal-tar pitch and solvent, heating;
(2) make step (1) gained mixture enter whizzer continuously, will weigh slag and throw away continuously, obtain light phase liquid;
(3) make the light phase liquid of step (2) gained enter the subsider bottom continuously, described quinoline insolubles generation sedimentation, the clear liquid that does not contain quinoline insolubles is discharged continuously by the top of subsider;
(4) the clear liquid distillation that step (3) gained is not contained quinoline insolubles is purified product;
(5) with described solvent recuperation, recycle.
According to the method that removes the quinoline insolubles in the coal-tar pitch of the present invention, preferably, described solvent is selected from aliphatic hydrocarbon and aromatic hydrocarbon, and more excellent is, described aliphatic hydrocarbon is selected from kerosene, hexane or heptane, and the temperature of its air distillation quantity of distillate 95% is not higher than 270 ℃; Described aromatic hydrocarbon is selected from one or more cuts in the tar course of processing, and the temperature of its air distillation quantity of distillate 95% is not higher than 340 ℃.
According to the method that removes the quinoline insolubles in the coal-tar pitch of the present invention, preferably, in described step (1), the weight ratio of described solvent and described coal-tar pitch is 0.4: 1～1.2: 1, and Heating temperature is 60～100 ℃.
According to the method that removes the quinoline insolubles in the coal-tar pitch of the present invention, preferably, in described step (2), the rotating speed of described whizzer is 1000～5500rpm.
According to the method that removes the quinoline insolubles in the coal-tar pitch of the present invention, preferably, in described step (3), described subsider temperature is 60～100 ℃, and the settling time is 1～5 hour.
The technical process of the inventive method following (referring to Fig. 1):
Coal-tar pitch and solvent enter whizzer continuously behind the line mixer thorough mixing, under action of centrifugal force, the heavy slag that is rich in quinoline insolubles in the mixture is thrown away whizzer continuously, and this heavy slag is transported outward as byproduct.Quinoline insolubles content enters the bottom of subsider continuously at 0.03% to 0.20% light phase liquid, in subsider, the quinoline insolubles of trace continues to take place sedimentation, the clear liquid that does not contain quinoline insolubles is discharged continuously by the top of subsider, clear liquid is purified product after the solvent distillation tower is handled, and reclaims solvent.Reclaiming solvent recycles.
In the inventive method, the ratio range of solvent and coal-tar pitch is: 0.4: 1～1.2: 1, by online under meter control; The mixture temperature: 60～100 ℃, by the online interchanger control behind the line mixer; Subsider temperature: 60～100 ℃, control by the subsider internal heater; Mixture is in the residence time of subsider: 1～5 hour, control by the purified liquor outlet and the mixture inlet height difference of subsider; Centrifuge speed: 1000～5500rpm regulates by the whizzer frequency transformer.
Beneficial effect of the present invention:
Adopt method of the present invention, the content of quinoline insolubles is 0.06～0.11% in the gained purified product, and the purified product yield is 75～88%, and solvent recovering rate is 95.7～98.7%.The inventive method compared with prior art, in quality product, aspects such as plant energy consumption, solvent loss, technological operation all are significantly improved.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
Below for a more detailed description to the present invention in conjunction with the accompanying drawings with embodiment.These embodiment only are the descriptions to best mode for carrying out the invention, scope of the present invention are not had any restriction.
Embodiment 1
1) raw material: return and join viscid bitumen
2) processing method:
Raw material and solvent enter whizzer continuously behind the line mixer thorough mixing, under action of centrifugal force, the heavy slag that is rich in quinoline insolubles in the mixture is thrown away whizzer continuously, and this heavy slag is transported outward as byproduct.Light phase liquid enters the bottom of subsider continuously, and in subsider, the quinoline insolubles of trace continues sedimentation takes place, and the clear liquid that does not contain quinoline insolubles is discharged continuously by the top of subsider, and clear liquid is purified product after the solvent distillation tower is handled, and reclaims solvent.Reclaiming solvent recycles.
3) main technologic parameters
Proportioning: the weight ratio of solvent and raw material is: 0.4: 1
Mixture temperature: 60 ℃;
Subsider temperature: 60 ℃;
Mixture is in the residence time of subsider: 5 hours
Centrifuge speed: 1000rpm
After testing, the quinoline insolubles content of light phase liquid is 0.05%, and product yield (purifies back and join viscid bitumen/time join viscid bitumen) is 79%, and solvent recovering rate is 95.7%, and purifying back the content of joining quinoline insolubles in the viscid bitumen is 0.11%.
Embodiment 2
1) raw material: return and join viscid bitumen
2) processing method: same with embodiment 1
3) main technologic parameters
Proportioning: the weight ratio of solvent and raw material is: 0.9: 1
Mixture temperature: 90 ℃;
Subsider temperature: 90 ℃;
Mixture is in the residence time of subsider: 2 hours
Centrifuge speed: 3000rpm
After testing, the quinoline insolubles content of light phase liquid is 0.03%, and product yield (purifies back and join viscid bitumen/time join viscid bitumen) is 82%, and solvent recovering rate is 97.7%, and purifying back the content of joining quinoline insolubles in the viscid bitumen is 0.07%.
Embodiment 3
1) raw material: return and join viscid bitumen
2) processing method: same with embodiment 1
3) main technologic parameters
Proportioning: the weight ratio of solvent and raw material is: 1.2: 1
Mixture temperature: 90 ℃;
Subsider temperature: 90 ℃;
Mixture is in the residence time of subsider: 1 hour
Centrifuge speed: 5500rpm
After testing, the quinoline insolubles content of light phase liquid is 0.02%, and product yield (purifies back and join viscid bitumen/time join viscid bitumen) is 88%, and solvent recovering rate is 96.7%, and purifying back the content of joining quinoline insolubles in the viscid bitumen is 0.06%.
Embodiment 4
1) raw material: straight run viscid bitumen
2) processing method: same with embodiment 1
3) main technologic parameters
Proportioning: the weight ratio of solvent and raw material is: 1.2: 1
Mixture temperature: 95 ℃;
Subsider temperature: 95 ℃;
Mixture is in the residence time of subsider: 5 hours
Centrifuge speed: 5500rpm
After testing, the quinoline insolubles content of light phase liquid is 0.02%, and product yield (purifies back and join viscid bitumen/time join viscid bitumen) is 87%, and solvent recovering rate is 97.2%, and purifying back the content of joining quinoline insolubles in the viscid bitumen is 0.06%.
Embodiment 5
1) raw material: mid-temperature pitch
2) processing method: same with embodiment 1
3) main technologic parameters
Proportioning: the weight ratio of solvent and raw material is: 1.2: 1
Mixture temperature: 100 ℃;
Subsider temperature: 100 ℃;
Mixture is in the residence time of subsider: 5 hours
Centrifuge speed: 5500rpm
After testing, the quinoline insolubles content of light phase liquid is 0.04%, and product yield (purifies back and join viscid bitumen/time join viscid bitumen) is 75%, and solvent recovering rate is 98.7%, and purifying back the content of joining quinoline insolubles in the viscid bitumen is 0.09%.
Adopt the inventive method, the content of quinoline insolubles is 0.06～0.11% in the gained purified product, and the purified product yield is 75～88%, and solvent recovering rate is 95.7～98.7%. The inventive method compared with prior art, in product quality, the aspects such as plant energy consumption, solvent loss, technological operation all are significantly improved.
Claims (7)
1. a method that removes the quinoline insolubles in the coal-tar pitch is characterized in that, may further comprise the steps:
(1) with coal-tar pitch and solvent, heating;
(2) make step (1) gained mixture enter whizzer continuously, will weigh slag and throw away continuously, obtain light phase liquid;
(3) make the light phase liquid of step (2) gained enter the subsider bottom continuously, described quinoline insolubles generation sedimentation, the clear liquid that does not contain quinoline insolubles is discharged continuously by the top of subsider;
(4) the clear liquid distillation that step (3) gained is not contained quinoline insolubles is purified product;
(5) with described solvent recuperation, recycle.
2. the method that removes the quinoline insolubles in the coal-tar pitch as claimed in claim 1 is characterized in that described solvent is selected from aliphatic hydrocarbon and aromatic hydrocarbon.
3. the method that removes the quinoline insolubles in the coal-tar pitch as claimed in claim 2 is characterized in that described aliphatic hydrocarbon is selected from kerosene, hexane or heptane, and the temperature of its air distillation quantity of distillate 95% is not higher than 270 ℃.
4. the method that removes the quinoline insolubles in the coal-tar pitch as claimed in claim 2 is characterized in that, described aromatic hydrocarbon is selected from one or more cuts in the tar course of processing, and the temperature of its air distillation quantity of distillate 95% is not higher than 340 ℃.
5. the method that removes the quinoline insolubles in the coal-tar pitch as claimed in claim 1 is characterized in that, in described step (1), the weight ratio of described solvent and described coal-tar pitch is 0.4: 1～1.2: 1, and Heating temperature is 60～100 ℃.
6. the method that removes the quinoline insolubles in the coal-tar pitch as claimed in claim 1 is characterized in that, in described step (2), the rotating speed of described whizzer is 1000～5500rpm.
7. the method that removes the quinoline insolubles in the coal-tar pitch as claimed in claim 1 is characterized in that, in described step (3), described subsider temperature is 60～100 ℃, and the settling time is 1～5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100567783A CN101993704A (en) | 2009-08-21 | 2009-08-21 | Method for removing quinoline insoluble substances in coal tar pitch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100567783A CN101993704A (en) | 2009-08-21 | 2009-08-21 | Method for removing quinoline insoluble substances in coal tar pitch |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101993704A true CN101993704A (en) | 2011-03-30 |
Family
ID=43784471
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100567783A Pending CN101993704A (en) | 2009-08-21 | 2009-08-21 | Method for removing quinoline insoluble substances in coal tar pitch |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101993704A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952561A (en) * | 2011-08-31 | 2013-03-06 | 上海宝钢化工有限公司 | Method for preparing adjustable high-quinoline-insoluble (QI) coal tar |
| CN103013566A (en) * | 2011-09-23 | 2013-04-03 | 北京三聚创洁科技发展有限公司 | Technology for preparing needle coke raw material from coal-tar pitch |
| CN110317624A (en) * | 2019-08-08 | 2019-10-11 | 平顶山东晟高科实业有限公司 | A kind of method of pitch removing QI |
| CN110408418A (en) * | 2019-08-08 | 2019-11-05 | 平顶山东晟高科实业有限公司 | A kind of preparation method of high regular carbon crystallite pitch coke |
| CN111218294A (en) * | 2018-11-27 | 2020-06-02 | 宝武炭材料科技有限公司 | Method for purifying quinoline insoluble coal-series asphalt with high softening point and high softening point |
| CN111548822A (en) * | 2020-05-15 | 2020-08-18 | 北京先进碳能科技有限公司 | Method for purifying and modifying petroleum residual oil |
| CN113621396A (en) * | 2020-05-07 | 2021-11-09 | 宝武炭材料科技有限公司 | Preparation method of refined medium-temperature asphalt |
| CN114437750A (en) * | 2020-10-30 | 2022-05-06 | 宝武炭材料科技有限公司 | Preparation method of ultra-pure coal tar pitch |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445740A (en) * | 2009-01-04 | 2009-06-03 | 北京石油化工学院 | A preparation method of dipping agent pitch |
| CN101475820A (en) * | 2009-01-23 | 2009-07-08 | 北京石油化工学院 | Purification method for coal pitch |
| CN101508903A (en) * | 2009-03-20 | 2009-08-19 | 上海宝钢化工有限公司 | Process for continuously removing quinoline insoluble substances in coal tar pitch |
-
2009
- 2009-08-21 CN CN2009100567783A patent/CN101993704A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445740A (en) * | 2009-01-04 | 2009-06-03 | 北京石油化工学院 | A preparation method of dipping agent pitch |
| CN101475820A (en) * | 2009-01-23 | 2009-07-08 | 北京石油化工学院 | Purification method for coal pitch |
| CN101508903A (en) * | 2009-03-20 | 2009-08-19 | 上海宝钢化工有限公司 | Process for continuously removing quinoline insoluble substances in coal tar pitch |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952561A (en) * | 2011-08-31 | 2013-03-06 | 上海宝钢化工有限公司 | Method for preparing adjustable high-quinoline-insoluble (QI) coal tar |
| CN102952561B (en) * | 2011-08-31 | 2014-03-12 | 上海宝钢化工有限公司 | Method for preparing adjustable high-quinoline-insoluble (QI) coal tar |
| CN103013566A (en) * | 2011-09-23 | 2013-04-03 | 北京三聚创洁科技发展有限公司 | Technology for preparing needle coke raw material from coal-tar pitch |
| CN103013566B (en) * | 2011-09-23 | 2015-08-05 | 北京宝塔三聚能源科技有限公司 | A kind of technique utilizing coal-tar pitch to prepare needle-shape coke raw material |
| CN111218294A (en) * | 2018-11-27 | 2020-06-02 | 宝武炭材料科技有限公司 | Method for purifying quinoline insoluble coal-series asphalt with high softening point and high softening point |
| CN110408418A (en) * | 2019-08-08 | 2019-11-05 | 平顶山东晟高科实业有限公司 | A kind of preparation method of high regular carbon crystallite pitch coke |
| CN110317624A (en) * | 2019-08-08 | 2019-10-11 | 平顶山东晟高科实业有限公司 | A kind of method of pitch removing QI |
| CN110408418B (en) * | 2019-08-08 | 2021-09-03 | 山西永鑫煤焦化有限责任公司 | Preparation method of high-regular-carbon microcrystalline pitch coke |
| CN113621396A (en) * | 2020-05-07 | 2021-11-09 | 宝武炭材料科技有限公司 | Preparation method of refined medium-temperature asphalt |
| CN111548822A (en) * | 2020-05-15 | 2020-08-18 | 北京先进碳能科技有限公司 | Method for purifying and modifying petroleum residual oil |
| CN111548822B (en) * | 2020-05-15 | 2022-05-17 | 北京先进碳能科技有限公司 | Method for purifying and modifying petroleum residual oil |
| CN114437750A (en) * | 2020-10-30 | 2022-05-06 | 宝武炭材料科技有限公司 | Preparation method of ultra-pure coal tar pitch |
| CN114437750B (en) * | 2020-10-30 | 2024-03-15 | 宝武碳业科技股份有限公司 | Preparation method of ultra-pure coal tar pitch |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101508903B (en) | Process for continuously removing quinoline insoluble substances in coal tar pitch | |
| CN101993704A (en) | Method for removing quinoline insoluble substances in coal tar pitch | |
| CN101294090B (en) | Fine purification method for coal tar pitch | |
| CN102051191B (en) | Production method and system of coal-based needle coke | |
| CN101531909A (en) | Continuous sedimentation process for production of needle coke | |
| CN101824329A (en) | Novel process for eliminating quinoline insoluble substances in coal tar medium temperature pitch | |
| CN101928583A (en) | Method for purifying soft asphalt | |
| CN103113907B (en) | Coal-based needle coke preparation process | |
| CN102399566A (en) | Method for extracting heavy liquefied oil and kerite substance from residue of direct coal liquefaction | |
| CN108410491A (en) | A kind of method and system preparing pitch using coal liquefaction residue | |
| CN104774635A (en) | Treatment method for acid washing and deashing of coal liquefaction residue | |
| CN104046382A (en) | Method for removing catalyst from catalytic cracking oil slurry | |
| CN110194966A (en) | A kind of demetallated method and apparatus of residual oil | |
| CN107892937A (en) | A kind of efficient solvent preparation method of refined bitumen | |
| CN103254933B (en) | Method for separating liquefied heavy oil and asphalt substances from direct coal liquefaction residues | |
| CN108977222B (en) | Separation system and separation method for direct coal liquefaction oil residue | |
| CN103113910B (en) | Pretreatment method for raw material of coal-based needle coke | |
| RU2408652C1 (en) | Procedure and installation for processing tar sand | |
| CN104673369A (en) | Purifying processing method of petroleum slurry for preparing petroleum-based needle coke | |
| CN203440308U (en) | Device for preparing needle coke by using maltha as raw material | |
| CN101220284B (en) | Method for producing electrode impregnation asphalt | |
| CN203079911U (en) | Device for preparing coal based needle coke | |
| CN203440307U (en) | Device adopting maltha as raw material to prepare needle coke | |
| CN107903940A (en) | A kind of catalytic cracked oil pulp removal method of catalyst and system | |
| CN210163381U (en) | Coal tar residue separator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20110330 |