CN102796560B - Coal tar whole-fraction hydrogenation method - Google Patents
Coal tar whole-fraction hydrogenation method Download PDFInfo
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Abstract
The invention relates to a coal tar whole-fraction hydrogenation method. Medium/low-temperature coal tar whole-fractions are used as raw materials, catalytic hydrogenation and distillation treatments are carried out in a trickle bed reactor through a hydrogenation protective agent, a hydrodemetallization agent, a hydrodesulfurization agent, a hydrodenitrogenation agent and a hydrocracking agent, and then a gasoline fraction and a diesel oil fraction are cut. The coal tar whole-fraction hydrogenation method is simple in process flow; a product is high in conversion rate and high in quality; and the whole process is safe and stable in operation.
Description
Technical field
The invention belongs to coal chemical technology, particularly a kind of take the full cut of medium/low temperature coal tar as raw material, produce the method for fuel oil with trickle-bed reactor shortening.
Background technology
Coal tar is the liquid product that coal obtains in destructive distillation or pyrolysis and gasification.Can obtain following four kinds of coal tar according to the difference of production method: high-temperature coking coal tar, is called for short coal-tar heavy oil (900～1000 ℃); Middle temperature vertical heater coal tar, is called for short coal-tar middle oil (700～900 ℃); Low temperature, middle temperature producer gas coal tar, be called for short medium/low temperature coal tar (600～800 ℃); Low-temperature pyrolyzed coal tar, is called for short coalite tar (450～650 ℃).
In the last few years, along with developing rapidly of China's pyrolysis of coal industry, coal tar annual production was constantly risen.With medium/low temperature coal tar petroleum replacing, produce fuel oil through shortening, under-supply significant to alleviating China's oil.
The oil composition of medium/low temperature coal tar and different in kind, in coal-tar heavy oil, approximately contain 50% alkane and aromatic hydrocarbons in medium/low temperature coal tar, and the content of its tar-bitumen is relatively less, and suitable employing shortening technology is produced vehicular engine fuel oil.
Patent publication No. is the Chinese patent of CN1351130A, its main production method be coal tar first through fractionation by distillation, the 370 ℃ of lighting ends that are less than that fractionate out are carried out to hydro-upgrading, its main weak point is feed coal tar all not to be utilized.
Patent publication No. is the Chinese patent of CN1464031A, has introduced a kind of coal tar hydrogenation process and catalyzer.While mentioning the unprocessed coal tar of direct processing in this patent, before hydrogenator, set up one to four switch protecting reactor.Hydrofining catalyzer is housed in switch protecting reactor.Enter hydrogenator by switch protecting reactor product out, hydrogenator can be suspended-bed reactor, fixed-bed reactor, moving-burden bed reactor or ebullated bed reactor.The weak point of the method is that complex process, catalyst levels are large, running cost is high.
Patent publication No. is the Chinese patent of CN1664068A and CN101429456A, adopts delay coking of coal tar-hydrofining/hydrocracking combined process.Its method is: first full cut coal tar is carried out to delayed coking, obtain gas, coke, benzoline and heavy distillate, then benzoline is carried out to hydrofining, the raw material using heavy distillate as hydrocracking, finally obtains petroleum naphtha and diesel product.The weak point of this technique is: technical process complexity, and part of coal tar is converted into coke, do not make full use of tar resource.
Patent publication No. is the Chinese patent of CN1876767A, first through hydrogenation pretreatment reaction device (1～10 tandem reactor) by full coal tar cut, enter again hydrocracking reactor (1～6 tandem reactor), then the product of generation is made to gasoline and diesel oil after fractionation.The main deficiency of this technique is: required reactor is too many, and technological process is oversize, and investment is large.Wayward.
Patent publication No. is the Chinese patent of CN1766058A, discloses a kind of coal tar hydrogenation of total effluent treatment process.Full coal tar cut is introduced into floating bed hydrogenation device by the present invention, the product that its reaction generates cuts the tail oil of 370 ℃ of water outlet, 370 ℃ of cuts of < and > through water distilling apparatus, wherein 370 ℃ of cuts of < enter fixed-bed reactor after hydrofining reaction, then the product after refining is cut out to 150 ℃ of gasoline of < and 150～370 ℃ of diesel oil, the tail oil of 370 ℃ of > is looped back to suspended-bed reactor simultaneously and further change into light-end products.The deficiency of this technique is that technique is more complicated, investment is larger.
Summary of the invention
Technical problem to be solved by this invention is to overcome the shortcoming of above-mentioned patent, the method for the medium/low temperature coal tar hydrogenation of total effluent of provide that a kind of flow process is simple, transformation efficiency is high, good product quality, safe operation are stable.
Solving the problems of the technologies described above the technical solution used in the present invention comprises the steps:
1) the full cut purifying treatment of coal tar, removes moisture, metal and solid impurity in coal tar;
2) by the coal tar after purifying and hydrogen, 150～250 ℃, 3～8MPa, hydrogen to oil volume ratio in molten hydrogen still are that 800～1800:1, molten hydrogen time are molten hydrogen under 15～40 minutes conditions, obtain the liquid material of vapor liquid equilibrium;
3) liquid material of vapor liquid equilibrium being utilized in the first trickle-bed reactor to the agent of RG-1 type hydrogenation protecting, the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent is 0.28～2.6m at 260～360 ℃, 9～14MPa, liquid volume air speed
3h
-1/ m
3, hydrogen to oil volume ratio is under 900～1800:1 condition, to carry out catalytic hydrogenation reaction for the first time, described RG-1 type hydrogenation protecting agent shared volume ratio in the first trickle-bed reactor is 10%～30%, FZC-200 type hydrodemetallation (HDM) agent shared volume ratio in the first trickle-bed reactor is 10%～40%, RMS-1 type hydrogen desulfurization agent shared volume ratio in the first trickle-bed reactor is 20%～50%, surplus is hydrogen, in the second trickle-bed reactor, utilize again the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent at 360～410 ℃, 9～14MPa, liquid volume air speed 0.28～2.6m
3h
-1/ m
3, carry out catalytic hydrogenation reaction for the second time under hydrogen to oil volume ratio 1000～1800:1 condition, described RSN-1 type hydrodenitrification agent shared volume ratio in the second trickle-bed reactor is that 20%～80%, FC-32 type hydrocracking agent shared volume ratio in the second trickle-bed reactor is 15%～50%, and surplus is hydrogen, obtains lighting product,
4) lighting product is distilled in water distilling apparatus to processing, cut out gasoline fraction, diesel oil distillate and tail oil.
In above-mentioned steps 4) also comprise afterwards step 5), specifically: will in the tail oil of step 4), 70%～80% return to step 2 as circulation tail oil) circular treatment.
Above-mentioned steps 3) described in RG-1 type hydrogenation protecting agent shared preferred volume ratio in the first trickle-bed reactor be 15%～25%; FZC-200 type hydrodemetallation (HDM) agent shared preferably volume ratio in the first trickle-bed reactor is 15%～35%; RMS-1 type hydrogen desulfurization agent shared preferably volume ratio in the first trickle-bed reactor is 25%～40%, and surplus is hydrogen.
Above-mentioned RSN-1 type hydrodenitrification agent shared preferred volume ratio in the second trickle-bed reactor is that 30%～75%, FC-32 type hydrocracking agent shared preferred volume ratio in the second trickle-bed reactor is 24%～45%, and surplus is hydrogen.
Above-mentioned coal tar is coalite tar or coal-tar middle oil or medium/low temperature coal tar.
Above-mentioned RG-1 type hydrogenation protecting agent and the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent, RSN-1 type hydrodenitrification agent, catalyzer branch office of FC-32 type hydrocracking Ji Junshiyou Sinopec Group produce and provide.
The method of coal tar hydrogenation of total effluent of the present invention is take the full cut of medium/low temperature coal tar as raw material; in trickle-bed reactor, passing through shortening, the distillation of hydrogenation protecting agent and hydrodemetallation (HDM) agent, hydrogen desulfurization agent, hydrodenitrification agent, hydrocracking agent processes; cut out gasoline fraction and diesel oil distillate; its technical process is simple, conversion rate of products is high, quality is good, and whole process operating safety is stable.
Embodiment
Now the present invention is further illustrated in conjunction with the embodiments, but the present invention is not limited only to following embodiment.
Embodiment 1
Be example take 100L coalite tar as raw material, the method for coal tar hydrogenation of total effluent comprises the following steps:
Step 1: get 100L coalite tar and remove moisture, metal, solid impurity in refining plant, complete full cut purifying treatment;
Step 2: 180 ℃, 5MPa, hydrogen to oil volume ratio in molten hydrogen still are molten hydrogen processing under 1400:1,25 minutes molten hydrogen time condition by the coal tar after purifying and hydrogen, and hydrogen is fully dissolved in coal tar, obtain the liquid material of vapor liquid equilibrium;
Step 3: the liquid material of vapor liquid equilibrium is utilized in the first trickle-bed reactor the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent 310 ℃, pressure for 12MPa, liquid volume air speed be 1.3m
3h
-1/ m
3, hydrogen to oil volume ratio is under 1300:1 condition, to carry out catalytic hydrogenation reaction for the first time; the percent by volume of shared the first trickle-bed reactor of RG-1 type hydrogenation protecting agent is 20%; the percent by volume of FZC-200 type hydrodemetallation (HDM) agent is 25%; the volume percent of RMS-1 type hydrogen desulfurization agent is 32%; surplus is hydrogen, and catalytic hydrogenation reaction utilizes the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent at 380 ℃, 12MPa, liquid volume air speed 1.3m again in the second trickle-bed reactor after completing for the first time
3h
-1/ m
3, under hydrogen to oil volume ratio 1300:1 condition, carry out catalytic hydrogenation reaction for the second time; In the second trickle-bed reactor, the percent by volume of RSN-1 type hydrodenitrification agent is that the percent by volume of 52%, FC-32 type hydrocracking agent is 35%, and surplus is hydrogen, obtains lighting product;
Step 4: lighting product is distilled in water distilling apparatus to processing, cut out 15L gasoline fraction, 75L diesel oil distillate and 4L tail oil.
The gasoline fraction that coalite tar hydrogenation of total effluent upgrading in the present embodiment produces and the character of diesel oil distillate are respectively in table 1 and table 2.
The main character of table 1 gasoline fraction
The main character of table 2 diesel oil distillate
Can directly be drawn by table 1 and table 2, the gasoline fraction that coal tar hydrogenation of total effluent method of the present invention produces and diesel oil distillate all meet the relevant regulations of GB/T19147-2003, good product quality, and transformation efficiency is high.
Embodiment 2
Be example take 100L coalite tar as raw material, the method for warm coal tar hydrogenation of total effluent comprises the following steps:
Step 1: identical with embodiment 1.
Step 2: by the coal tar after purifying and hydrogen in molten hydrogen still under 250 ℃, 3MPa, hydrogen to oil volume ratio 1800:1,40 minutes molten hydrogen time condition molten hydrogen, obtain the liquid material of vapor liquid equilibrium;
Step 3: the liquid material of vapor liquid equilibrium is utilized in the first trickle-bed reactor the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent temperature be 360 ℃, pressure for 9MPa, liquid volume air speed be 2.6m
3h
-1/ m
3hydrogen to oil volume ratio is under 1800:1 condition, to carry out catalytic hydrogenation reaction for the first time; RG-1 type hydrogenation protecting agent shared percent by volume in the first trickle-bed reactor is 30%; the percent by volume of FZC-200 type hydrodemetallation (HDM) agent is 40%; the volume percent of RMS-1 type hydrogen desulfurization agent is 20%; surplus is hydrogen, and after completing, to utilize in the second trickle-bed reactor the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent be 1.3m at 360 ℃, 14MPa, liquid volume air speed to catalytic hydrogenation reaction again for the first time
3h
-1/ m
3, hydrogen to oil volume ratio is under 1800:1 condition, to carry out catalytic hydrogenation reaction for the second time; In the second trickle-bed reactor, the percent by volume of RSN-1 type hydrodenitrification agent is that the percent by volume of 80%, FC-32 type hydrocracking agent is 15%, and surplus is hydrogen, obtains lighting product;
Step 4: lighting product is distilled in water distilling apparatus to processing, cut out 17L gasoline fraction, 78L diesel oil distillate and 5L tail oil.
Embodiment 3
Be example take 100L coalite tar as raw material, the method for coal tar hydrogenation of total effluent comprises the following steps:
Step 1: identical with embodiment 1.
Step 2: be that 800:1, molten hydrogen time be 15 minute condition under molten hydrogen at 150 ℃, 8MPa, hydrogen to oil volume ratio by the coal tar after purifying and hydrogen in molten hydrogen still, obtain the liquid material of vapor liquid equilibrium;
Step 3: the liquid material of vapor liquid equilibrium is utilized in the first trickle-bed reactor the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent temperature be 260 ℃, pressure for 14MPa, liquid volume air speed be 0.28m
3h
-1/ m
3hydrogen to oil volume ratio is under 900:1 condition, to carry out catalytic hydrogenation reaction for the first time; in the first trickle-bed reactor; the percent by volume of RG-1 type hydrogenation protecting agent is 10%; the percent by volume of FZC-200 type hydrodemetallation (HDM) agent is 10%; the volume percent of RMS-1 type hydrogen desulfurization agent is 50%; surplus is hydrogen, and catalytic hydrogenation reaction utilizes the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent at 410 ℃ of temperature, pressure 9MPa, liquid volume air speed 0.28m again in the second trickle-bed reactor after completing for the first time
3h
-1/ m
3, under hydrogen to oil volume ratio 1000:1 condition, carry out catalytic hydrogenation reaction for the second time; In the second trickle-bed reactor, the percent by volume of RSN-1 type hydrodenitrification agent is that the percent by volume of 20%, FC-32 type hydrocracking agent is 50%, and surplus is hydrogen, obtains lighting product;
Step 4: lighting product is distilled in water distilling apparatus to processing, cut out 18L gasoline fraction, 79L diesel oil distillate and 6L tail oil.
Embodiment 4
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～3, in step 3, the liquid material of vapor liquid equilibrium is utilized in the first trickle-bed reactor to the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent carries out catalytic hydrogenation reaction for the first time, in the first trickle-bed reactor, the percent by volume of RG-1 type hydrogenation protecting agent is 15%, the percent by volume of FZC-200 type hydrodemetallation (HDM) agent is 15%, the volume percent of RMS-1 type hydrogen desulfurization agent is 40%, surplus is hydrogen, in the second trickle-bed reactor, utilize again the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent to carry out catalytic hydrogenation reaction for the second time, described RSN-1 type hydrodenitrification agent shared volume ratio in the second trickle-bed reactor is that 30%, FC-32 type hydrocracking agent shared volume ratio in the second trickle-bed reactor is 45%, and surplus is hydrogen, obtains lighting product, in this step, other operation is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 5
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～3, the liquid material of vapor liquid equilibrium is utilized in the first trickle-bed reactor to the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type hydrodemetallation (HDM) in step 3, RMS-1 type hydrogen desulfurization agent carries out catalytic hydrogenation reaction for the first time, in the first trickle-bed reactor, the percent by volume of RG-1 type hydrogenation protecting agent is 25%, the percent by volume of FZC-200 type hydrodemetallation (HDM) agent is 35%, the volume percent of RMS-1 type hydrogen desulfurization agent is 25%, surplus is hydrogen, in the second trickle-bed reactor, utilize again the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent to carry out catalytic hydrogenation reaction for the second time, described RSN-1 type hydrodenitrification agent shared volume ratio in the second trickle-bed reactor is that 75%, FC-32 type hydrocracking agent shared volume ratio in the second trickle-bed reactor is 24%, and surplus is hydrogen, obtains lighting product, in this step, other operation is identical with corresponding embodiment.
Other step is identical with corresponding embodiment.
Embodiment 6
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～5, after completing, step 4 can also carry out step 5, specifically: using the 75(quality in the tail oil of step 4)) % returns to step 2 as circulation tail oil) molten hydrogen still in circular treatment, with the further utilization ratio of its high raw material.Other step is identical with corresponding embodiment.
Embodiment 7
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～5, after step 4 completes, carry out step 5, by the 70(quality in the tail oil of step 4) % returns to step 2 as circulation tail oil) molten hydrogen still in circular treatment.Other step is identical with corresponding embodiment.
Embodiment 8
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～5, after step 4 completes, carry out step 5, by the 80(quality in the tail oil of step 4) % returns to step 2 as circulation tail oil) molten hydrogen still in circular treatment.Other step is identical with corresponding embodiment.
Embodiment 9
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～8, raw material coalite tar is replaced with isopyknic coal-tar middle oil, and other step is identical with corresponding embodiment.
Embodiment 10
In the method for the coal tar hydrogenation of total effluent of above-described embodiment 1～8, isopyknic medium/low temperature coal tar is replaced for raw material coalite tar, and other step is with embodiment is identical accordingly.
In above-described embodiment 1～10, related raw material coalite tar, coal-tar middle oil and medium/low temperature coal tar oil properties and composition are in table 3.
Table 3 coal tar character and composition/%(massfraction)
Claims (5)
1. a method for coal tar hydrogenation of total effluent, is characterized in that comprising the following steps:
1) the full cut purifying treatment of coal tar, removes moisture, metal and solid impurity in coal tar;
2) by the coal tar after purifying and hydrogen, 150～250 ℃, 3～8MPa, hydrogen to oil volume ratio in molten hydrogen still are 800～1800:1, and the molten hydrogen time is molten hydrogen under 15～40 minutes conditions, obtains the liquid material of vapor liquid equilibrium;
3) liquid material of vapor liquid equilibrium being utilized in the first trickle-bed reactor to the agent of RG-1 type hydrogenation protecting, the agent of FZC-200 type hydrodemetallation (HDM), RMS-1 type hydrogen desulfurization agent is 0.28～2.6m at 260～360 ℃, 9～14MPa, liquid volume air speed
3h
-1/ m
3, hydrogen to oil volume ratio is under 900～1800:1 condition, to carry out catalytic hydrogenation reaction for the first time, described RG-1 type hydrogenation protecting agent shared volume ratio in the first trickle-bed reactor is 10%～30%, FZC-200 type hydrodemetallation (HDM) agent shared volume ratio in the first trickle-bed reactor is 10%～40%, RMS-1 type hydrogen desulfurization agent shared volume ratio in the first trickle-bed reactor is 20%～50%, surplus is hydrogen, in the second trickle-bed reactor, utilize again the hydrodenitrification agent of RSN-1 type and FC-32 type hydrocracking agent at 360～410 ℃, 9～14MPa, liquid volume air speed 0.28～2.6m
3h
-1/ m
3, carry out catalytic hydrogenation reaction for the second time under hydrogen to oil volume ratio 1000～1800:1 condition, described RSN-1 type hydrodenitrification agent shared volume ratio in the second trickle-bed reactor is that 20%～80%, FC-32 type hydrocracking agent shared volume ratio in the second trickle-bed reactor is 15%～50%, and surplus is hydrogen, obtains lighting product,
4) lighting product is distilled in water distilling apparatus to processing, cut out gasoline fraction, diesel oil distillate and tail oil.
2. the method for coal tar hydrogenation of total effluent according to claim 1, it is characterized in that: in step 4) also comprise afterwards step 5), specifically: using step 4) tail oil in 70%～80% return to step 2 as circulation tail oil) circular treatment.
3. the method for coal tar hydrogenation of total effluent according to claim 1; it is characterized in that: step 3) described in RG-1 type hydrogenation protecting agent shared volume ratio in the first trickle-bed reactor be 15%～25%; FZC-200 type hydrodemetallation (HDM) agent shared volume ratio in the first trickle-bed reactor is 15%～35%; RMS-1 type hydrogen desulfurization agent shared volume ratio in the first trickle-bed reactor is 25%～40%, and surplus is hydrogen.
4. the method for coal tar hydrogenation of total effluent according to claim 1, it is characterized in that: described RSN-1 type hydrodenitrification agent shared volume ratio in the second trickle-bed reactor is 30%～75%, FC-32 type hydrocracking agent shared volume ratio in the second trickle-bed reactor is 24%～45%, and surplus is hydrogen.
5. the method for coal tar hydrogenation of total effluent according to claim 1, is characterized in that: described coal tar is coalite tar or coal-tar middle oil.
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| CN103450937B (en) * | 2013-09-13 | 2015-06-24 | 王树宽 | Method for producing low-condensation-point diesel oil and liquid paraffin by using coal tar |
| CN111849552B (en) * | 2019-04-30 | 2021-12-17 | 中国石油化工股份有限公司 | Coal tar full-fraction hydrogenation upgrading method and system |
| CN114437807A (en) * | 2020-10-30 | 2022-05-06 | 中国石油化工股份有限公司 | Pretreatment method of coal tar |
| CN112980484B (en) * | 2021-03-01 | 2022-02-22 | 内蒙古晟源科技有限公司 | Method for producing special marine heavy fuel oil by using coal tar as raw material |
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