CN102226093A - Preparation method of high-purity coal tar pitch from industrial coal tar pitch - Google Patents
Preparation method of high-purity coal tar pitch from industrial coal tar pitch Download PDFInfo
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- CN102226093A CN102226093A CN201110145485XA CN201110145485A CN102226093A CN 102226093 A CN102226093 A CN 102226093A CN 201110145485X A CN201110145485X A CN 201110145485XA CN 201110145485 A CN201110145485 A CN 201110145485A CN 102226093 A CN102226093 A CN 102226093A
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Abstract
A preparation method of high-purity coal tar pitch from industrial coal tar pitch. Industrial coal tar pitch is cracked at a low temperature of 0-15 DEG C, ground wet and treated with liquid-solid separation to obtain coal tar pitch with a granularity less than 100[mu]m. The coal tar pitch with a granularity less than 100[mu]m reacts with carbon tetrachloride with a concentration of 40-70%, and is treated with liquid-solid separation after the reaction. A liquid phase solution enters into a first distillation operation until carbon tetrachloride does not distill into a condensation receiver. Obtained distilled solid coal tar pitch enters into a second distillation operation, and high-purity coal tar pitch is obtained after distillation, wherein a total ash content is less than 0.0008%, and an impurity content is less than 0.0005%. The invention solves insufficiency of a traditional industrial coal tar pitch physical purification method, and enables effective removal of impurities such as zinc, aluminium, titanium and iron etc. in industrial coal tar pitch.
Description
Technical field
The present invention relates to a kind of Wet-process metallurgy method for preparing the high purity coal-tar pitch by industrial coal-tar pitch.
Background technology
Industrial coal-tar pitch, wherein main composition carbon content＜85%, and major impurity zinc, aluminium, titanium, iron equal size height can not satisfy the ingredient requirement of preparation high purity graphite.At present, substantially the removal of impurities measure of not purifying just directly applies to industry for industrial coal-tar pitch, perhaps to demanding relatively technology, only coal-tar pitch is done the processing that simple physics removes mechanical impurity, impurity atom is not wherein removed substantially, does not reach the ingredient requirement of preparation high purity graphite.This requires content＜0.0005% of Zn in the technology of producing high purity graphite, the content of the content of the content of Al＜0.0002%, Fe＜0.0002%, Ti＜0.0001%, and the content of total ash has big gap less than 0.0008%.
Summary of the invention
The present invention proposes a kind of method that is prepared high-purity coal-tar pitch by industrial coal-tar pitch, solved the deficiency of traditional industry coal-tar pitch physical property method of purification, present method effective elimination impurity such as zinc, aluminium, titanium, iron in the industrial coal-tar pitch, make total ash＜0.0008% wherein, and the content of impurity is less than 0.0005%.
The present invention realizes by following step: (1) carries out the coal-tar pitch of liquid-solid separation acquisition＜100um granularity with industrial coal-tar pitch after 0～15 ℃ of cryogenic pulverization, wet-milling, liquid solution is returned low temperature wet-milling operation; Coal-tar pitch material and volumetric concentration are that 40～70% tetracol phenixin is that 3～15:1～10 add in the reactors and carry out first section stripping operation of sizing mixing by weight proportion, 20～70 ℃ of controlled temperature, stirring reaction 4～10h, in reaction process, the coal-tar pitch molecule enters into the organic solvent tetracol phenixin, inorganic impurity then do not enter organic solvent, stay solid mutually in, thereby realized separating of coal-tar pitch molecule and inorganic impurity.Reaction is carried out the liquid-solid separation second time after finishing, and liquid solution is the leaching phase of coal-tar pitch, enters first section distillation process.The fs leaching has obtained 40～50% leaching yield, and this is relevant with the solubleness of coal-tar pitch molecule in tetracol phenixin, and the not molten coal-tar pitch of solid phase remains further to be handled; The organic liquid phase solution of the coal-tar pitch of (2) first sections stripping generations of sizing mixing enters in first section distillation reaction operation, 80～110 ℃ of controlled temperature, reactor pressure＜0.2MPa, the distillation reaction time is 2～5h, till no longer including tetracol phenixin distill out in the condensation receptor.The distillation solid phase coal-tar pitch that obtains enters in second section distillation process, 150～250 ℃ of controlled temperature, and reactor pressure＜0.2MPa, the distillation reaction time is 1～5h.Behind the second distillation, effectively separate tetracol phenixin remaining in the solid phase coal-tar pitch, obtained high-purity coal-tar pitch of main grade 99.999%, total ash＜0.0008% wherein, Zn content＜0.0005%, Al content＜0.0002%, Fe content＜0.0002%, Ti content＜0.0001%.The liquid phase of first section distillation reaction acquisition then is a tetracol phenixin, returns once more and enters first section stripping process flow of sizing mixing, and realizes the recycle of tetracol phenixin in technology.Not molten coal-tar pitch of solid phase that (3) first sections stripping operations of sizing mixing obtain and volumetric concentration are that 80～90% tetracol phenixin is that second section stripping of sizing mixing carried out in 3～10:1～8 by weight proportion, 20～70 ℃ of controlled temperature, stirring reaction 4～10h, carry out liquid-solid separation again, the liquid phase that obtains by volume concentration is to return after 50～70% proportionings in first section stripping operation of sizing mixing, second section leaching yield is 15～20%, and the not molten coal-tar pitch of solid phase then enters the coking treatment process and obtains coke, acts as a fuel.
Method flow provided by the invention is short, process is simple, the reliable easy suitability for industrialized production of going, realize easily, tetracol phenixin separates with coal-tar pitch after distilling, rate of recovery height, coal-tar pitch impurity removal percentage height, and can realize tetracol phenixin cycling and reutilization, reduced production cost, environmental friendliness.High-purity coal-tar pitch that the present invention obtains, wherein impurity Zn, Al, Ti, Fe are effectively removed, reach＜0.0005%.Technological process forms the closed cycle system, and environment is not constituted pollution.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The content 4.2% of embodiment 1, industrial coal-tar pitch Zn, the content 1.25% of Al, the content 0.95% of Ti, the content 1.35% of Fe, total ash is 6.10%.This coal-tar pitch carries out the liquid-solid back of separating and obtains getting the raw materials ready of granularity＜100um earlier through cryogenic pulverization, wet-milling.
The granularity that obtains is reached＜coal-tar pitch of 100um gets the raw materials ready and sizes mixing with 50% tetracol phenixin, adds volume and is in 3 liters the reactor, and 20～25 ℃ of temperature are carried out the 8h reaction, and this is first section stripping of sizing mixing.After the question response time arrives, carry out liquid-solid separation, obtain the solid phase coal-tar pitch after the stripping and contain the organic liquid phase solution of coal-tar pitch molecule.The organic liquid phase solution that obtains packed into enter first section distillation process in the distiller.The heating that heats up, 80～85 ℃ of temperature are carried out 5h after the reaction times under reaction pressure＜0.2Mpa, and no longer include tetracol phenixin steam and come out this moment, emits the solid phase coal-tar pitch after the distillation.Solid phase coal-tar pitch after the distillation is packed in the high-temperature reactor, enter second section distillation process: 150～155 ℃ of controlled temperature, high temperature is sloughed remaining tetracol phenixin, after reaction pressure＜0.2Mpa reacts 2h down, can obtain effectively to slough impurity Zn, Al, the high-purity coal-tar pitch of Fe, Ti, the liquid phase tetracol phenixin then by volume concentration be to return first section stripping operation of sizing mixing after 50～70% the proportioning.
The solid phase coal-tar pitch and the volumetric concentration of first section stripping operation leaching of sizing mixing are that 80% tetracol phenixin enters second section stripping operation of sizing mixing, react, its ratio is 3～10:1～8,20～70 ℃ of controlled temperature, stirring reaction 8h carries out liquid-solid separation again, the liquid solution that obtains by volume concentration is to return after 50～70% proportionings in first section stripping operation of sizing mixing, this section leaching yield is 15～20%, and the solid phase coal-tar pitch then enters the coking treatment process and obtains coke, and the retrieval system that acts as a fuel is used.
The high-purity coal-tar pitch that obtains, the wherein content of the content of the content of the content of Zn＜0.0005%, Al＜0.0002%, Fe＜0.0002%, Ti＜0.0001%, always ash 0.00076%.
The content 3.2% of embodiment 2, industrial coal-tar pitch Zn, the content 1.45% of Al, the content 0.75% of Ti, the content 1.63% of Fe, total ash is 6.50%.This coal-tar pitch carries out liquid-solid separation and obtains getting the raw materials ready of granularity＜100um earlier through cryogenic pulverization, wet-milling.
The coal-tar pitch of granularity＜100um of obtaining got the raw materials ready size mixing with 60% tetracol phenixin, this is first section stripping of sizing mixing: add volume and be in 3 liters the reactor, 30～35 ℃ of temperature, react 7h, after the question response time arrives, carry out liquid-solid separation, obtain the solid phase coal-tar pitch after the stripping and contain the organic liquid phase solution of coal-tar pitch molecule, the organic liquid phase that obtains is packed in the distiller, enter first section distillation process.The heating that heats up, 90～95 ℃ of temperature are reacted 4h under reaction pressure＜0.2Mpa, and no longer include tetracol phenixin steam and come out this moment, emits the solid phase after the distillation.Solid phase after the distillation is packed in the high-temperature reactor, enter second section distillation process.160～165 ℃ of controlled temperature, high temperature is sloughed remaining tetracol phenixin, after reaction pressure＜0.2Mpa reacts 1.5h down, can obtain effectively to slough impurity Zn, Al, the high-purity coal-tar pitch of Fe, Ti, the liquid phase tetracol phenixin then by volume concentration be to return first section stripping operation of sizing mixing after 50～70% the proportioning.
The solid phase coal-tar pitch of first section stripping operation leaching of sizing mixing and the tetracol phenixin of volumetric concentration 85% enter second section stripping operation of sizing mixing and react.Its ratio is 3～10:1～8,30～35 ℃ of controlled temperature, stirring reaction 7h, carry out liquid-solid separation again, the liquid phase that obtains by volume concentration is to return after 50～70% proportionings in first section stripping operation of sizing mixing, this section leaching yield is 15～20%, and the solid phase coal-tar pitch then enters the coking treatment process and obtains coke, acts as a fuel.
The high-purity coal-tar pitch that obtains, the wherein content of the content of the content of the content of Zn＜0.0002%, Al＜0.0002%, Fe＜0.0002%, Ti＜0.0001%, always ash 0.00065%.
The content 2.8% of embodiment 3, industrial coal-tar pitch Zn, the content 1.04% of Al, the content 0.75% of Ti, the content 1.65% of Fe, total ash is 6.10%.This coal-tar pitch is earlier through cryogenic pulverization, wet-milling, obtains granularity after the liquid-solid separation to reach＜the getting the raw materials ready of 100um.
The granularity that obtains is reached＜coal-tar pitch of 100um gets the raw materials ready and sizes mixing with 70% tetracol phenixin, adds volume and is in 3 liters the reactor, and this is first section stripping operation of sizing mixing.40～45 ℃ of temperature are carried out 5h reaction, after the question response time arrives, carry out liquid-solid separation, the solid phase coal-tar pitch after obtaining to leach and contain the organic liquid phase solution of coal-tar pitch molecule.The organic liquid phase that obtains is packed in the distiller, enter first section distillation process.The heating that heats up, 100～105 ℃ of temperature, reaction pressure＜0.2Mpa 3h of following reaction times, no longer include tetracol phenixin steam and come out this moment, emits the solid phase after the distillation.Solid phase after the distillation is packed in the high-temperature reactor, enter second section distillation process.200～210 ℃ of controlled temperature, high temperature is sloughed remaining tetracol phenixin, after reaction pressure＜0.2Mpa reacts 3h down, can obtain effectively to slough impurity Zn, Al, the high-purity coal-tar pitch of Fe, Ti, the liquid phase tetracol phenixin then by volume concentration be to return first section stripping operation of sizing mixing after 50～70% the proportioning.
The solid phase coal-tar pitch of first section stripping operation leaching of sizing mixing and the tetracol phenixin of volumetric concentration 90% enter second section stripping operation of sizing mixing and react.Its ratio is 3～10:1～8,40～45 ℃ of controlled temperature, stirring reaction 4h, carry out liquid-solid separation again, the liquid phase that obtains by volume concentration is to return first section stripping operation of sizing mixing after 50～70% proportionings, this section leaching yield is 15～20%, and the solid phase coal-tar pitch then enters the coking treatment process and obtains coke, acts as a fuel.
The high-purity coal-tar pitch that obtains, the wherein content of the content of the content of the content of Zn＜0.0002%, Al＜0.0002%, Fe＜0.0002%, Ti＜0.0001%, always ash 0.00056%.
Claims (9)
1. the technology that is prepared high-purity coal-tar pitch by industrial coal-tar pitch is characterized in that step is as follows:
(1), industrial coal-tar pitch is carried out the coal-tar pitch that liquid-solid separation obtains granularity＜100um after cryogenic pulverization, wet-milling, liquid solution is returned low temperature wet-milling operation;
(2), the coal-tar pitch of granularity＜100um and volumetric concentration are that 40～70% tetracol phenixin is that first section stripping reaction of sizing mixing carried out in 3～15:1～10 by weight proportion, 20～70 ℃ of controlled temperature, stirring reaction 4～10h, reaction finishes the liquid-solid separation in back, obtains the not molten coal-tar pitch of solid phase and leaches liquid solution;
(3), the leaching liquid solution of step (2) enters first section distillation process, 80～110 ℃ of controlled temperature, reaction pressure＜0.2Mpa, the distillation reaction time is 2～5h, till no longer including tetracol phenixin distill out in the condensation receptor, the solid phase coal-tar pitch enters second section distillation process after the distillation of acquisition, 150～250 ℃ of controlled temperature, reaction pressure＜0.2MPa obtains high-purity coal-tar pitch behind distillation reaction 1～5h.
2. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: said cryogenic pulverization, wet-milling operation are carried out under 0～15 ℃.
3. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: not molten coal-tar pitch of the solid phase of described step (2) and volumetric concentration are that 80～90% tetracol phenixin is that second section stripping reaction of sizing mixing carried out in 3～10:1～8 by weight proportion, 20～70 ℃ of controlled temperature, stirring reaction 4～10h, reaction is carried out liquid-solid separation after finishing, the liquid solution that obtains is returned in first section stripping operation of sizing mixing, and the not molten coal-tar pitch of solid phase obtains coke through the coking treatment process.
4. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: the main by weight grade 99.999% of high-purity coal-tar pitch that obtains behind described second section distillation process, total ash＜0.0008%.
5. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: the content of Zn by weight＜0.0005% in high-purity coal-tar pitch of described acquisition.
6. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: the content of Al by weight＜0.0002% in high-purity coal-tar pitch of described acquisition.
7. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: the content of Fe by weight＜0.0002% in high-purity coal-tar pitch of described acquisition.
8. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: the content of Ti by weight＜0.0001% in high-purity coal-tar pitch of described acquisition.
9. industrial coal-tar pitch according to claim 1 prepares the technology of high-purity coal-tar pitch, it is characterized in that: the tetracol phenixin that described first section distillation process obtains returns first section stripping operation of sizing mixing, realize the recycle of tetracol phenixin in technology, technological process is closed system, and is free from environmental pollution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232135A (en) * | 2014-09-25 | 2014-12-24 | 四川创越炭材料有限公司 | Purification method for coal pitch with high softening point |
| CN109550573A (en) * | 2019-01-15 | 2019-04-02 | 山东交通学院 | The static lossless granulating method of waste asphalt mixture |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3786134A (en) * | 1970-05-29 | 1974-01-15 | Kureha Chemical Ind Co Ltd | Process for producing hollow carbon microspheres |
| CN101294090A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Fine purification method for coal tar pitch |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3786134A (en) * | 1970-05-29 | 1974-01-15 | Kureha Chemical Ind Co Ltd | Process for producing hollow carbon microspheres |
| CN101294090A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Fine purification method for coal tar pitch |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104232135A (en) * | 2014-09-25 | 2014-12-24 | 四川创越炭材料有限公司 | Purification method for coal pitch with high softening point |
| CN109550573A (en) * | 2019-01-15 | 2019-04-02 | 山东交通学院 | The static lossless granulating method of waste asphalt mixture |
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Address after: 650031 No. 86 Yuantong North Road, Yunnan, Kunming Patentee after: Kunming Metallurgical Research Institute Co., Ltd Address before: 650051 No. 86 Yuantong North Road, Wuhua District, Yunnan, Kunming Patentee before: Kunming Metallurgical Research Institute |
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