CN102226093B - 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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- CN102226093B CN102226093B CN 201110145485 CN201110145485A CN102226093B CN 102226093 B CN102226093 B CN 102226093B CN 201110145485 CN201110145485 CN 201110145485 CN 201110145485 A CN201110145485 A CN 201110145485A CN 102226093 B CN102226093 B CN 102226093B
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Abstract
The invention relates to 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 that is prepared the high purity coal-tar pitch by industrial coal pitch.
Background technology
Industrial coal-tar pitch, wherein main composition carbon content＜85%, and major impurity zinc, aluminium, titanium, iron equal size are high, 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 pitch, perhaps to relatively demanding technique, only coal-tar pitch is done the processing that simple physical property removes mechanical impurity, impurity atom is not wherein removed substantially, does not reach the ingredient requirement of preparation high purity graphite.In this technique for high purity graphite, require the content of Zn＜0.0005%, the content of the content of the content of Al＜0.0002%, Fe＜0.0002%, Ti＜0.0001%, the content of total ash has larger 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 industrial coal-tar pitch, make wherein total ash＜0.0008%, and the content of impurity is less than 0.0005%.
The present invention realizes by following step: (1) carries out industrial coal-tar pitch the coal-tar pitch of liquid-solid separation acquisition＜100um granularity after 0～15 ℃ of cryogenic pulverization, wet-milling, liquid solution is returned to Low Temperature Wet grinder order; Coal-tar pitch material and volumetric concentration are that 40～70% tetracol phenixin is that 3～15:1～10 add and carry out the first paragraph stripping operation of sizing mixing in reactor by weight proportion, control 20～70 ℃ of temperature, stirring reaction 4～10h, in reaction process, the coal-tar pitch molecule enters into organic solvent carbon tetrachloride, inorganic impurity do not enter organic solvent, stays in solid-phase, thereby realized separating of coal-tar pitch molecule and inorganic impurity.Reaction is carried out liquid-solid separation for the second time after finishing, and liquid solution is the leaching phase of coal-tar pitch, enters the first paragraph 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 processed; (2) the size mixing organic liquid phase solution of the coal-tar pitch that stripping produces of first paragraph enters in first paragraph distillation reaction operation, control 80～110 ℃ of temperature, reactor pressure＜0.2MPa, the distillation reaction time is 2～5h, until till no longer including tetracol phenixin in the condensation receptor and distilling out.The distillation solid phase coal-tar pitch that obtains enters in the second segment distillation process, controls 150～250 ℃ of temperature, reactor pressure＜0.2MPa, and the distillation reaction time is 1～5h.After 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 wherein＜0.0008%, Zn content＜0.0005%, Al content＜0.0002%, Fe content＜0.0002%, Ti content＜0.0001%.The liquid phase that the first paragraph distillation reaction obtains is tetracol phenixin, again returns to enter the first paragraph stripping process flow of sizing mixing, and realizes the recycle of tetracol phenixin in technique.(3) size mixing the not molten coal-tar pitch of solid phase that the stripping operation obtains and volumetric concentration of first paragraph is that 80～90% tetracol phenixin is that the second segment stripping of sizing mixing is carried out in 3～10:1～8 by weight proportion, control 20～70 ℃ of temperature, stirring reaction 4～10h, carry out again liquid-solid separation, the liquid phase that obtains by volume concentration is to return to first paragraph after 50～70% proportionings to size mixing in the stripping operation, the second segment leaching yield is 15～20%, and the not molten coal-tar pitch of solid phase enters the coking treatment process and obtains coke, acts as a fuel.
Method flow provided by the invention is short, process simple, the reliable easy suitability for industrialized production of going, easily realize, tetracol phenixin separates with coal-tar pitch after distillation, the rate of recovery is high, the coal-tar pitch impurity removal percentage is high, 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 consisted of pollution.
Description of drawings
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1, industrial coal pitch Zn content 4.2%, 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 liquid-solid separation and obtains afterwards getting the raw materials ready of granularity＜100um first through cryogenic pulverization, wet-milling.
The granularity that obtains is reached＜coal-tar pitch of 100um gets the raw materials ready and sizes mixing together with 50% tetracol phenixin, and adding volume is that in the reactor of 3 liters, 20～25 ℃ of temperature are carried out the 8h reaction, and this is the first paragraph stripping of sizing mixing.After the question response time arrives, carry out liquid-solid separation, obtain the solid phase coal-tar pitch after stripping and contain the organic liquid phase solution of coal-tar pitch molecule.The organic liquid phase solution that obtains is packed into enter the first paragraph distillation process in 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 out this moment, emits the solid phase coal-tar pitch after distillation.Solid phase coal-tar pitch after distillation is packed in high-temperature reactor, enter the second segment distillation process: control 150～155 ℃ of temperature, high temperature is sloughed remaining tetracol phenixin, after reacting 2h under reaction pressure＜0.2Mpa, can obtain effectively to slough impurity Zn, Al, the high-purity coal-tar pitch of Fe, Ti, the liquid phase tetracol phenixin by volume concentration be to return to the first paragraph stripping operation of sizing mixing after 50～70% proportioning.
The solid phase coal-tar pitch that the stripping operation of sizing mixing first paragraph leaches and volumetric concentration are that 80% tetracol phenixin enters the second segment stripping operation of sizing mixing, react, its ratio is 3～10:1～8, control 20～70 ℃ of temperature, stirring reaction 8h, then carry out liquid-solid separation, the liquid solution that obtains by volume concentration is to return to first paragraph after 50～70% proportionings to size mixing in the stripping operation, this section leaching yield is 15～20%, and the solid phase coal-tar pitch 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%.
Embodiment 2, industrial coal pitch Zn content 3.2%, 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 first through cryogenic pulverization, wet-milling.
The coal-tar pitch of granularity＜100um of obtaining is got the raw materials ready size mixing together with 60% tetracol phenixin, this is the first paragraph stripping of sizing mixing: adding volume is in the reactor of 3 liters, 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 stripping and contain the organic liquid phase solution of coal-tar pitch molecule, the organic liquid phase that obtains is packed in distiller, enter the first paragraph 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 out this moment, emits the solid phase after distillation.Solid phase after distillation is packed in high-temperature reactor, enter the second segment distillation process.Control 160～165 ℃ of temperature, high temperature is sloughed remaining tetracol phenixin, after reacting 1.5h under reaction pressure＜0.2Mpa, can obtain effectively to slough impurity Zn, Al, the high-purity coal-tar pitch of Fe, Ti, the liquid phase tetracol phenixin by volume concentration be to return to the first paragraph stripping operation of sizing mixing after 50～70% proportioning.
The solid phase coal-tar pitch that the stripping operation of sizing mixing first paragraph leaches and the tetracol phenixin of volumetric concentration 85% enter the second segment stripping operation of sizing mixing and react.Its ratio is 3～10:1～8, control 30～35 ℃ of temperature, stirring reaction 7h, carry out again liquid-solid separation, the liquid phase that obtains by volume concentration is to return to first paragraph after 50～70% proportionings to size mixing in the stripping operation, this section leaching yield is 15～20%, and the solid phase coal-tar pitch 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%.
Embodiment 3, industrial coal pitch Zn content 2.8%, 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 first through cryogenic pulverization, wet-milling, and liquid-solid separation obtains afterwards granularity and reaches＜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 together with 70% tetracol phenixin, and adding volume is in the reactor of 3 liters, and this is the first paragraph 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 distiller, enter the first paragraph distillation process.The heating that heats up, 100～105 ℃ of temperature, reaction pressure＜0.2Mpa 3h of lower reaction times, no longer include tetracol phenixin steam out this moment, emits the solid phase after distillation.Solid phase after distillation is packed in high-temperature reactor, enter the second segment distillation process.Control 200～210 ℃ of temperature, high temperature is sloughed remaining tetracol phenixin, after reacting 3h under reaction pressure＜0.2Mpa, can obtain effectively to slough impurity Zn, Al, the high-purity coal-tar pitch of Fe, Ti, the liquid phase tetracol phenixin by volume concentration be to return to the first paragraph stripping operation of sizing mixing after 50～70% proportioning.
The solid phase coal-tar pitch that the stripping operation of sizing mixing first paragraph leaches and the tetracol phenixin of volumetric concentration 90% enter the second segment stripping operation of sizing mixing and react.Its ratio is 3～10:1～8, control 40～45 ℃ of temperature, stirring reaction 4h, carry out again liquid-solid separation, the liquid phase that obtains by volume concentration is to return to the first paragraph stripping operation of sizing mixing after 50～70% proportionings, this section leaching yield is 15～20%, and the solid phase coal-tar pitch 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. prepared the technique of high-purity coal-tar pitch by industrial coal-tar pitch, it 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 to Low Temperature Wet grinder order;
(2), the coal-tar pitch of granularity＜100um and volumetric concentration are that 40～70% tetracol phenixin is that size mixing stripping reaction of first paragraph is carried out in 3～15:1～10 by weight proportion, control 20～70 ℃ of temperature, stirring reaction 4～10h, liquid-solid separation after reaction finishes obtains the not molten coal-tar pitch of solid phase and leaches liquid solution;
(3), the leaching liquid solution of step (2) enters the first paragraph distillation process, control 80～110 ℃ of temperature, reaction pressure＜0.2Mpa, the distillation reaction time is 2～5h, until till no longer including tetracol phenixin in the condensation receptor and distilling out, after the distillation of acquisition, the solid phase coal-tar pitch enters the second segment distillation process, control 150～250 ℃ of temperature, reaction pressure＜0.2MPa obtains high-purity coal-tar pitch after distillation reaction 1～5h.
2. industrial coal-tar pitch according to claim 1 prepares the technique 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 technique of high-purity coal-tar pitch, it is characterized in that: the not molten coal-tar pitch of the solid phase of described step (2) and volumetric concentration are that 80～90% tetracol phenixin is that the second segment stripping reaction of sizing mixing is carried out in 3～10:1～8 by weight proportion, control 20～70 ℃ of temperature, stirring reaction 4～10h, reaction is carried out liquid-solid separation after finishing, the liquid phase that obtains by volume concentration is to return to first paragraph after 50～70% proportionings to size mixing in the stripping operation, 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 technique of high-purity coal-tar pitch, it is characterized in that: the high-purity coal-tar pitch that obtains after described second segment distillation process is main grade 99.999% by weight, total ash＜0.0008%.
5. industrial coal-tar pitch according to claim 1 prepares the technique of high-purity coal-tar pitch, it is characterized in that: the content by weight＜0.0005% of Zn in high-purity coal-tar pitch of described acquisition.
6. industrial coal-tar pitch according to claim 1 prepares the technique of high-purity coal-tar pitch, it is characterized in that: the content by weight＜0.0002% of Al in high-purity coal-tar pitch of described acquisition.
7. industrial coal-tar pitch according to claim 1 prepares the technique of high-purity coal-tar pitch, it is characterized in that: the content by weight＜0.0002% of Fe in high-purity coal-tar pitch of described acquisition.
8. industrial coal-tar pitch according to claim 1 prepares the technique of high-purity coal-tar pitch, it is characterized in that: the content by weight＜0.0001% of Ti in high-purity coal-tar pitch of described acquisition.
9. industrial coal-tar pitch according to claim 1 prepares the technique of high-purity coal-tar pitch, it is characterized in that: the tetracol phenixin that described first paragraph distillation process obtains returns to the first paragraph stripping operation of sizing mixing, realize the recycle of tetracol phenixin in technique, technological process is closed system, and is free from environmental pollution.
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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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| 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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