CN102766477B - Method for preparing clean fuel oil from coal tar - Google Patents
Method for preparing clean fuel oil from coal tar Download PDFInfo
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- CN102766477B CN102766477B CN 201210241733 CN201210241733A CN102766477B CN 102766477 B CN102766477 B CN 102766477B CN 201210241733 CN201210241733 CN 201210241733 CN 201210241733 A CN201210241733 A CN 201210241733A CN 102766477 B CN102766477 B CN 102766477B
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Abstract
The invention relates to a method for preparing clean fuel oil from coal tar, belonging to the field of coal tar reprocessing. The method comprises the following steps: mixing coal tar and a specific solvent, holding the mixture in a high-pressure autoclave at constant temperature for several hours, cooling to room temperature, separating the reaction liquid, and extracting to obtain the fuel oil. In the coal tar supercritical extraction process, the solvent has the functions of both extraction and hydrogenation, and the coal tar is lightened under the condition of no need of high-temperaturehigh-pressure catalyst, thereby saving abundant energy sources and hydrogen resources.
Description
Technical field
The present invention relates to a kind ofly prepare the method for clean fuel oil with coal tar, belong to coal tar reprocessing field.
Background technology
The method of oil fuel is produced in coal tar processing, and technology and the method for a lot of maturations arranged both at home and abroad, mainly contains distillation and separation method, extraction separation method etc.Coal tar distillation is more traditional technology, can well cut out each section distillate, and distillation is remaining after 360 ℃ to be pitch, but power consumption is bigger, need be heated to 360-380 ℃ to raw material, also has the part long chain alkane to fail to separate simultaneously.Chinese patent CN101781575A discloses the method that a kind of middle coalite tar is produced high-cleanness fuel oil, be that solvent and coal tar are mixed extraction, upper strata light liquid after leaving standstill is after solvent is reclaimed in evaporation, obtain cleaning light-weight fuel oil, lower floor's heavy-fluid obtains heavy fuel oil (HFO) after solvent is reclaimed in evaporation.Chinese patent CN1664068 provides a kind of technology of producing fuel oil from coal tar, is 500～520 ℃ with coal tar in temperature, and pressure is that 0.22～0.26MPa carries out obtaining oil fuel, liquefied gas and coke product after the delayed coking.Delayed coking gained oil fuel will improve the quality of products through further hydrofining, and hydrofining gained oil product can obtain to meet 90# gasoline ,-20 diesel oil and the oil fuel of national standard after fractionation.
Above-mentioned coal tar lighting prepares oil fuel all need be carried out under the condition of High Temperature High Pressure catalyzer, needs to consume a large amount of energy and valuable hydrogen resource, can pollute environment.And under the condition of high temperature, coal tar causes catalyzer to lose activity easily in the catalyst surface coking.The oil product of aforesaid method gained is nitrogenous, sulphur content is higher, in the use wherein contained sulphur, nitrogen impurity in combustion processes, become SO
x, NO
xSerious environment pollution.
Summary of the invention
To the objective of the invention is in order addressing the above problem, a kind of method for preparing clean fuel oil with coal tar to be provided.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method with producing fuel oil from coal tar of the present invention comprises the following steps:
Step 1, coal tar and solvent mixed according to 1: 3～5 mass ratio after, at sonic oscillation, obtain mixed solution;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement in the reactor and go out air, and the constant 0.1～0.5Mpa of being keep-ups pressure; After displacement is finished, heat up with constant temperature rise rate, when being warming up to 240～350 ℃, feed rare gas element, make pressure remain on 10～20MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.01～-0.1MPa, evaporate solvent under 20～50 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, with the raw fuel stock mixed solution of step 3 gained and thinner by mass ratio 3～5: 1 mixes, and sonic oscillation, leaves standstill, filters; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 80～100 ℃ condition, distill out until absence of liquid impurity, the liquid that is not steamed is clean fuel oil.
Solvent described in the step 1 is any one in methyl alcohol, toluene, ethanol, acetone, the Skellysolve A.
Nitrogen replacement described in the step 2 goes out air, replaces 3～5 times, and each aeration time is 5min～20min;
Thinner described in the step 4 is normal hexane, any one in No. 90 gasoline, No. 0 diesel oil.
Beneficial effect
1, a kind of method with producing fuel oil from coal tar of the present invention, utilize coal tar to be raw material, in the process of supercritical extraction coal tar, solvent not only plays the effect of extraction, can also play the effect of hydrogenation, the clean fuel oil that the obtains use that can directly act as a fuel also can obtain gasoline and diesel oil after fractionation by distillation, all satisfy national standard.
2, a kind of method with producing fuel oil from coal tar of the present invention makes the coal tar lighting under the condition that does not need high temperature catalyst, has saved a large amount of energy and hydrogen resource, and pollution-free, cost is low.
Embodiment
Below in conjunction with embodiment content of the present invention is described further.
Embodiment 1
Step 1, with sonic oscillation 1h after 500g coal tar and the 1500g methanol mixed, obtain mixed solution;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement with the constant pressure of 0.2Mpa in the reaction system and go out air in the reactor, replaces 3 times, and aeration time is 5min at every turn; After displacement is finished, with constant temperature rise rate heat up, when being warming up to 240 ℃, feed rare gas element, make pressure remain on 20MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.01MPa, evaporate methyl alcohol under 20 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, the 400g raw fuel stock mixed solution of step 3 gained is mixed with the 100g normal hexane, sonic oscillation, leave standstill, filter; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 80 ℃ condition, distill out until absence of liquid, the liquid that obtains 298g is clean fuel oil; After fractionation by distillation, obtain 102g gasoline and 97g diesel oil, satisfy No. 89 gasoline and-No. 10 diesel oil national standards respectively.
Embodiment 2
Step 1,500g coal tar is mixed back sonic oscillation 1h with 2000g ethanol, obtain mixed solution;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement with the constant pressure of 0.2Mpa in the reaction system and go out air in the reactor, replaces 3 times, and aeration time is 5min at every turn; After displacement is finished, with constant temperature rise rate heat up, when being warming up to 350 ℃, feed rare gas element, make pressure remain on 10MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.1MPa, evaporate solvent under 50 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, No. 0 diesel oil of 380g raw fuel stock mixed solution and 150g of step 3 gained is mixed, sonic oscillation, leave standstill, filter; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 100 ℃ condition, distill out until absence of liquid, the liquid that obtains 308g is oil fuel; After fractionation by distillation, obtain 153g gasoline and 128g diesel oil, satisfy No. 89 gasoline and-No. 10 diesel oil national standards respectively.
Embodiment 3
Step 1,5kg coal tar is mixed back sonic oscillation 1h with 20kg toluene, obtain mixed solution;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement with the constant pressure of 0.2Mpa in the reaction system and go out air in the reactor, replaces 3 times, and aeration time is 5min at every turn; After displacement is finished, with constant temperature rise rate heat up, when being warming up to 300 ℃, feed rare gas element, make pressure remain on 15MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.05MPa, evaporate solvent under 30 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, the 4.4kg raw fuel stock mixed solution of step 3 gained is mixed with 1kg90 gasoline, sonic oscillation, leave standstill, filter; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 90 ℃ condition, distill out until absence of liquid, the liquid that obtains 3.2kg is oil fuel; After fractionation by distillation, obtain 1.29kg gasoline and 1.08kg diesel oil, satisfy No. 89 gasoline and-No. 10 diesel oil national standards respectively.
Embodiment 4
Step 1,500g coal tar is mixed back sonic oscillation 1h with 1500g acetone, obtain mixed solution;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement with the constant pressure of 0.2Mpa in the reaction system and go out air in the reactor, replaces 3 times, and aeration time is 5min at every turn; After displacement is finished, with constant temperature rise rate heat up, when being warming up to 280 ℃, feed rare gas element, make pressure remain on 12MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.03MPa, evaporate solvent under 25 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, the 320g raw fuel stock mixed solution of step 3 gained is mixed with the 1000g normal hexane, sonic oscillation, leave standstill, filter; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 80 ℃ condition, distill out until absence of liquid, the liquid that obtains 280g is oil fuel; After fractionation by distillation, obtain 112g gasoline and 98g diesel oil, satisfy No. 89 gasoline and-No. 10 diesel oil national standards respectively.
Embodiment 5
Step 1,500g coal tar is mixed back sonic oscillation 1h with the 1500g Skellysolve A, obtain mixed solution;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement with the constant pressure of 0.2Mpa in the reaction system and go out air in the reactor, replaces 3 times, and aeration time is 5min at every turn; After displacement is finished, with constant temperature rise rate heat up, when being warming up to 320 ℃, feed rare gas element, make pressure remain on 18MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.08MPa, evaporate solvent under 35 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, the 380g raw fuel stock mixed solution of step 3 gained is mixed with 1500g0 diesel oil, sonic oscillation, leave standstill, filter; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 100 ℃ condition, distill out until absence of liquid, the liquid that obtains 315g is oil fuel; After fractionation by distillation, obtain 126g gasoline and 112g diesel oil, satisfy No. 89 gasoline and-No. 10 diesel oil national standards respectively.
Claims (2)
1. one kind prepares the method for oil fuel with coal tar, it is characterized in that: comprise the following steps:
Step 1, coal tar and solvent mixed according to 1: 3～5 mass ratio after, at sonic oscillation, obtain mixed solution; Described solvent is any one in methyl alcohol, toluene, ethanol, acetone, the Skellysolve A;
Step 2, the mixed solution that step 1 is obtained join in the autoclave, feed nitrogen replacement in the reactor and go out air, and the constant 0.1～0.5Mpa of being keep-ups pressure; After displacement is finished, with constant temperature rise rate heat up, when being warming up to 240～350 ℃, feed rare gas element, make pressure remain on 10～20MPa; Keep constant temperature and pressure and stirring, the oil fuel composition in the solvent extraction coal tar stops heating after extraction finishes;
Step 3, the reaction system of step 2 is cooled to room temperature, reduces the pressure in the reactor simultaneously; Filter out solution, and join in the rotary evaporation in vacuo instrument ,-0.01～-0.1MPa, evaporate solvent under 20～50 ℃ of conditions, steam until absence of liquid, the liquid that is not evaporated away is the raw fuel stock mixed solution;
Step 4, with the raw fuel stock mixed solution of step 3 gained and thinner by mass ratio 3～5: 1 mixes, and sonic oscillation, leaves standstill, filters; Filtrate is poured in the normal pressure Rotary Evaporators then, evaporate under 80～100 ℃ condition, distill out until absence of liquid, the liquid that is not steamed is clean fuel oil; Described thinner is normal hexane, any one in No. 90 gasoline, No. 0 diesel oil.
2. as claimed in claim 1ly a kind ofly prepare the method for oil fuel with coal tar, it is characterized in that: the nitrogen replacement described in the step 2 goes out air, replaces 3～5 times, and each aeration time is 5min～20min.
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| CN 201210241733 CN102766477B (en) | 2012-07-13 | 2012-07-13 | Method for preparing clean fuel oil from coal tar |
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| CN 201210241733 CN102766477B (en) | 2012-07-13 | 2012-07-13 | Method for preparing clean fuel oil from coal tar |
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| CN102766477B true CN102766477B (en) | 2013-09-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015077045A1 (en) * | 2013-11-19 | 2015-05-28 | Uop Llc | Process for hydrotreating a coal tar stream |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609183A (en) * | 2018-12-11 | 2019-04-12 | 西安交通大学 | Coal tar Method for treatment of oil based on supercritical methanol |
| CN113583756B (en) * | 2021-08-13 | 2024-02-06 | 北京化工大学 | Method for preparing chemicals and fuel oil by mild hydrogenation liquefaction of medium-low rank coal |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033410A (en) * | 2007-02-16 | 2007-09-12 | 西安交通大学 | Method of hydrogenation treatment for coal tar by hypercritical solvent |
| CN101781575A (en) * | 2009-01-21 | 2010-07-21 | 中国科学院工程热物理研究所 | Method for preparing high-cleanness fuel oil from intermediate-temperature and low-temperature coal tar |
| CN101870887A (en) * | 2009-11-24 | 2010-10-27 | 济南开发区星火科学技术研究院 | Method for preparing diesel from coal tar serving as raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080072476A1 (en) * | 2006-08-31 | 2008-03-27 | Kennel Elliot B | Process for producing coal liquids and use of coal liquids in liquid fuels |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033410A (en) * | 2007-02-16 | 2007-09-12 | 西安交通大学 | Method of hydrogenation treatment for coal tar by hypercritical solvent |
| CN101781575A (en) * | 2009-01-21 | 2010-07-21 | 中国科学院工程热物理研究所 | Method for preparing high-cleanness fuel oil from intermediate-temperature and low-temperature coal tar |
| CN101870887A (en) * | 2009-11-24 | 2010-10-27 | 济南开发区星火科学技术研究院 | Method for preparing diesel from coal tar serving as raw material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015077045A1 (en) * | 2013-11-19 | 2015-05-28 | Uop Llc | Process for hydrotreating a coal tar stream |
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