CN102796560A - 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 with in/the full cut of coalite tar is a raw material, produces the method for fuel oil with the trickle-bed reactor shortening.
Background technology
Coal tar is the liquid product that coal obtains in destructive distillation or pyrolysis and gasification.Difference according to working method can obtain following four kinds of coal tar: high-temperature coking coal tar, be called for short coal-tar heavy oil (900～1000 ℃); In warm vertical heater coal tar, be called for short coal-tar middle oil (700～900 ℃); Low temperature, middle temperature producer gas coal tar, in the abbreviation/coalite tar (600～800 ℃); Low temperature pyrogenation coal tar is called for short coalite tar (450～650 ℃).
In the last few years, along with developing rapidly of China's coal cracking industry, the coal tar YO was constantly risen.With in/coalite tar substitutes oil, produces fuel oil through shortening, and is under-supply significant to alleviating China's oil.
In/composition of coalite tar and different in kind be in coal-tar heavy oil, in/containing 50% alkane and aromatic hydrocarbons approximately in the coalite tar, the content of its tar-bitumen is less relatively, and the suitable shortening technology that adopts is produced the vehicular engine fuel oil.
Patent publication No. is the Chinese patent of CN1351130A, its main working method be coal tar earlier through fractionation by distillation, carry out hydro-upgrading with what fractionate out less than 370 ℃ of lighting ends, 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.When mentioning the unprocessed coal tar of direct processing in this patent, before hydrogenator, set up one to four switch protecting reactor drum.Hydrogenation pre-refining catalyzer is housed in the switch protecting reactor drum.The product that is come out by the switch protecting reactor drum gets into hydrogenator, and hydrogenator can be suspended-bed reactor, fixed-bed reactor, moving-burden bed reactor or ebullated bed reactor.The weak point of this method is that complex process, catalyst levels are big, running cost is high.
Patent publication No. is the Chinese patent of CN1664068A and CN101429456A, adopts delay coking of coal tar-unifining/hydrocracking combined process.Its method is: carry out delayed coking to full cut coal tar earlier, obtain gas, coke, benzoline and heavy distillate, carry out unifining to benzoline then, the raw material of heavy distillate as hydrogen cracking, obtain petroleum naphtha and diesel product at last.The weak point of this technology is: technical process is complicated, and part of coal tar is converted into coke, has not made full use of tar resource.
Patent publication No. is the Chinese patent of CN1876767A; Be earlier through hydrogenation pretreatment reaction device (1～10 tandem reactor) with the full cut of coal tar; Get into hydrocracking reactor (1～6 tandem reactor) again, then the product that generates is made gasoline and diesel oil after fractionation.The main deficiency of this technology is: required reactor drum is too many, and technological process is oversize, and investment is big.Wayward.
Patent publication No. is the Chinese patent of CN1766058A, discloses a kind of coal tar hydrogenation of total effluent treatment process.The present invention is introduced into the floating bed hydrogenation device with the full cut of coal tar; The product that its reaction generates through water distilling apparatus cut water outlet,＜370 ℃ of cuts and＞370 ℃ tail oil; Wherein＜370 ℃ cut gets into fixed-bed reactor behind hydrofining reaction; Product after will making with extra care then cuts out＜150 ℃ of gasoline and 150～370 ℃ of diesel oil, and tail oil that simultaneously will＞370 ℃ loops back suspended-bed reactor and further changes into clean cargo.The deficiency of this technology is that technology is complicated, investment is bigger.
Summary of the invention
Technical problem to be solved by this invention is to overcome the shortcoming of above-mentioned patent, provides that a kind of flow process is simple, transformation efficiency is high, during good product quality, safe operation are stable/method of coalite tar hydrogenation of total effluent.
The technical scheme that solves the problems of the technologies described above the present invention's employing comprises the steps:
1) the full cut purifying treatment of coal tar removes moisture, metal and solid impurity in the coal tar;
2) coal tar after will purifying and hydrogen 150～250 ℃, 3～8MPa, hydrogen to oil volume ratio in molten hydrogen still are 800～1800:1, to dissolve the hydrogen time be to dissolve hydrogen under the condition in 15～40 minutes, obtain the liquid material of vapor liquid equilibrium;
3) liquid material of vapor liquid equilibrium being utilized the agent of RG-1 type hydrogenation protecting, the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent in first trickle-bed reactor is 0.28～2.6m at 260～360 ℃, 9～14MPa, liquid volume air speed
3H
-1/ m
3Hydrogen to oil volume ratio is to carry out the catalytic hydrogenation reaction first time under 900～1800:1 condition; Said RG-1 type hydrogenation protecting agent shared volume ratio in first trickle-bed reactor is 10%～30%; FZC-200 type HDM agent shared volume ratio in first trickle-bed reactor is 10%～40%; RMS-1 type hydrogenating desulfurization agent shared volume ratio in first trickle-bed reactor is 20%～50%, and surplus is a hydrogen, in second trickle-bed reactor, utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent at 360～410 ℃, 9～14MPa, liquid volume air speed 0.28～2.6m again
3H
-1/ m
3, carry out the catalytic hydrogenation reaction second time under hydrogen to oil volume ratio 1000～1800:1 condition; Said RSN-1 type hydrodenitrification agent shared volume ratio in second trickle-bed reactor is 20%～80%, and FC-32 type hydrogen cracking agent shared volume ratio in second trickle-bed reactor is 15%～50%, and surplus is a hydrogen, obtains the lighting product;
4) the lighting product is distilled processing in water distilling apparatus, cut out gasoline fraction, diesel oil distillate and tail oil.
In above-mentioned steps 4) also comprise step 5) afterwards, specifically: with 70%～80% returning step 2 in the tail oil of step 4) as the circulation tail oil) circular treatment.
Above-mentioned steps 3) hydrogenation protecting of RG-1 type described in agent shared preferred volume ratio in first trickle-bed reactor is 15%～25%; FZC-200 type HDM agent shared preferable volume ratio in first trickle-bed reactor is 15%～35%; RMS-1 type hydrogenating desulfurization agent shared preferable volume ratio in first trickle-bed reactor is 25%～40%, and surplus is a hydrogen.
Above-mentioned RSN-1 type hydrodenitrification agent shared preferred volume ratio in second trickle-bed reactor is 30%～75%, and FC-32 type hydrogen cracking agent shared preferred volume ratio in second trickle-bed reactor is 24%～45%, and surplus is a hydrogen.
Above-mentioned coal tar be coalite tar or coal-tar middle oil or in/coalite tar.
Above-mentioned RG-1 type hydrogenation protecting agent and the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent, RSN-1 type hydrodenitrification agent, FC-32 type hydrogen cracking agent all are to be produced by catalyzer branch office of Sinopec Group to provide.
The method of coal tar hydrogenation of total effluent of the present invention with in/the full cut of coalite tar is a raw material; In trickle-bed reactor, passing through shortening, the distillation of hydrogenation protecting agent and HDM agent, hydrogenating desulfurization agent, hydrodenitrification agent, hydrogen cracking agent handles; 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
Combine instance that the present invention is further described, but the present invention is not limited only to following embodiment at present.
Embodiment 1
Is example with the 100L coalite tar as raw material, and the method for coal tar hydrogenation of total effluent may further comprise the steps:
Step 1: get the 100L coalite tar and in refining plant, remove moisture, metal, solid impurity, accomplish full cut purifying treatment;
Step 2: coal tar after will purifying and hydrogen 180 ℃, 5MPa, hydrogen to oil volume ratio in molten hydrogen still are 1400:1, dissolve and dissolve hydrogen under the 25 minutes hydrogen time condition and handle, and hydrogen fully is dissolved in the coal tar, obtain the liquid material of vapor liquid equilibrium;
Step 3: in first trickle-bed reactor, utilize the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent to be 1.3m for 12MPa, liquid volume air speed the liquid material of vapor liquid equilibrium at 310 ℃, pressure
3H
-1/ m
3, hydrogen to oil volume ratio is to carry out the catalytic hydrogenation reaction first time under the 1300:1 condition; The percent by volume of shared first trickle-bed reactor of RG-1 type hydrogenation protecting agent is 20%; The percent by volume of FZC-200 type HDM agent is 25%; The volume percent of RMS-1 type hydrogenating desulfurization agent is 32%; Surplus is a hydrogen, in second trickle-bed reactor, utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent at 380 ℃, 12MPa, liquid volume air speed 1.3m after for the first time catalytic hydrogenation reaction is accomplished again
3H
-1/ m
3, carry out the catalytic hydrogenation reaction second time under the hydrogen to oil volume ratio 1300:1 condition; The percent by volume of RSN-1 type hydrodenitrification agent is 52% in second trickle-bed reactor, and the percent by volume of FC-32 type hydrogen cracking agent is 35%, and surplus is a hydrogen, obtains the lighting product;
Step 4: the lighting product is distilled processing in water distilling apparatus, 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 seen table 1 and table 2 respectively.
The main character of table 1 gasoline fraction
The main character of table 2 diesel oil distillate
Can directly draw by table 1 and table 2, the relevant regulations that gasoline fraction that coal tar hydrogenation of total effluent method of the present invention is produced and diesel oil distillate all meet GB/T19147-2003, good product quality, transformation efficiency is high.
Embodiment 2
Is example with the 100L coalite tar as raw material, and the method for warm coal tar hydrogenation of total effluent may further comprise the steps:
Step 1: identical with embodiment 1.
Step 2: coal tar after will purifying and hydrogen in molten hydrogen still at 250 ℃, 3MPa, hydrogen to oil volume ratio 1800:1, dissolve and dissolve hydrogen under the 40 minutes hydrogen time condition, obtain the liquid material of vapor liquid equilibrium;
Step 3: the liquid material of vapor liquid equilibrium is utilized the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent in first trickle-bed reactor be that 360 ℃, pressure are 2.6m for 9MPa, liquid volume air speed in temperature
3H
-1/ m
3Hydrogen to oil volume ratio is to carry out the catalytic hydrogenation reaction first time under the 1800:1 condition; RG-1 type hydrogenation protecting agent shared percent by volume in first trickle-bed reactor is 30%; The percent by volume of FZC-200 type HDM agent is 40%; The volume percent of RMS-1 type hydrogenating desulfurization agent is 20%, and surplus is a hydrogen, in second trickle-bed reactor, utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent to be 1.3m at 360 ℃, 14MPa, liquid volume air speed after for the first time catalytic hydrogenation reaction is accomplished again
3H
-1/ m
3, hydrogen to oil volume ratio is to carry out the catalytic hydrogenation reaction second time under the 1800:1 condition; The percent by volume of RSN-1 type hydrodenitrification agent is 80% in second trickle-bed reactor, and the percent by volume of FC-32 type hydrogen cracking agent is 15%, and surplus is a hydrogen, obtains the lighting product;
Step 4: the lighting product is distilled processing in water distilling apparatus, cut out 17L gasoline fraction, 78L diesel oil distillate and 5L tail oil.
Embodiment 3
With the 100L coalite tar is that raw material is an example, and the method for coal tar hydrogenation of total effluent may further comprise the steps:
Step 1: identical with embodiment 1.
Step 2: coal tar after will purifying and hydrogen is 800:1 at 150 ℃, 8MPa, hydrogen to oil volume ratio in molten hydrogen still, dissolve the hydrogen time is to dissolve hydrogen under the condition in 15 minutes, obtains the liquid material of vapor liquid equilibrium;
Step 3: the liquid material of vapor liquid equilibrium is utilized the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent in first trickle-bed reactor be that 260 ℃, pressure are 0.28m for 14MPa, liquid volume air speed in temperature
3H
-1/ m
3Hydrogen to oil volume ratio is to carry out the catalytic hydrogenation reaction first time under the 900:1 condition; In first trickle-bed reactor; The percent by volume of RG-1 type hydrogenation protecting agent is 10%, and the percent by volume of FZC-200 type HDM agent is 10%, and the volume percent of RMS-1 type hydrogenating desulfurization agent is 50%; Surplus is a hydrogen, and catalytic hydrogenation reaction utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent at 410 ℃ of temperature, pressure 9MPa, liquid volume air speed 0.28m in second trickle-bed reactor after accomplishing again for the first time
3H
-1/ m
3, carry out the catalytic hydrogenation reaction second time under the hydrogen to oil volume ratio 1000:1 condition; The percent by volume of RSN-1 type hydrodenitrification agent is 20% in second trickle-bed reactor, and the percent by volume of FC-32 type hydrogen cracking agent is 50%, and surplus is a hydrogen, obtains the lighting product;
Step 4: the lighting product is distilled processing in water distilling apparatus, 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 the foregoing description 1～3; In first trickle-bed reactor, utilize the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent to carry out the catalytic hydrogenation reaction first time liquid material of vapor liquid equilibrium in step 3; In 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 HDM agent is 15%; The volume percent of RMS-1 type hydrogenating desulfurization agent is 40%, and surplus is a hydrogen, in second trickle-bed reactor, utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent to carry out the catalytic hydrogenation reaction second time again; Said RSN-1 type hydrodenitrification agent shared volume ratio in second trickle-bed reactor is 30%, and FC-32 type hydrogen cracking agent shared volume ratio in second trickle-bed reactor is 45%, and surplus is a hydrogen, obtains the lighting product; Other operation is identical with respective embodiments in this step.
Other step is identical with respective embodiments.
Embodiment 5
In the method for the coal tar hydrogenation of total effluent of the foregoing description 1～3; Liquid material with vapor liquid equilibrium in step 3 utilizes the hydrogenation protecting agent of RG-1 type and the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent to carry out the catalytic hydrogenation reaction first time in first trickle-bed reactor; In 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 HDM agent is 35%; The volume percent of RMS-1 type hydrogenating desulfurization agent is 25%, and surplus is a hydrogen, in second trickle-bed reactor, utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent to carry out the catalytic hydrogenation reaction second time again; Said RSN-1 type hydrodenitrification agent shared volume ratio in second trickle-bed reactor is 75%, and FC-32 type hydrogen cracking agent shared volume ratio in second trickle-bed reactor is 24%, and surplus is a hydrogen, obtains the lighting product; Other operation is identical with respective embodiments in this step.
Other step is identical with respective embodiments.
Embodiment 6
In the method for the coal tar hydrogenation of total effluent of the foregoing description 1～5;, step 4 can also carry out step 5 after accomplishing; Specifically: % returns step 2 as the circulation tail oil with 75 in the tail oil of step 4) (quality)) molten hydrogen still in circular treatment, with further its high utilization ratio of raw materials.Other step is identical with respective embodiments.
Embodiment 7
In the method for the coal tar hydrogenation of total effluent of the foregoing description 1～5, after step 4 is accomplished, carry out step 5,70 (quality) % that is about in the tail oil of step 4 returns step 2 as the circulation tail oil) molten hydrogen still in circular treatment.Other step is identical with respective embodiments.
Embodiment 8
In the method for the coal tar hydrogenation of total effluent of the foregoing description 1～5, after step 4 is accomplished, carry out step 5,80 (quality) % that is about in the tail oil of step 4 returns step 2 as the circulation tail oil) molten hydrogen still in circular treatment.Other step is identical with respective embodiments.
Embodiment 9
In the method for the coal tar hydrogenation of total effluent of the foregoing description 1～8, the raw material coalite tar is replaced with isopyknic coal-tar middle oil, and other step is identical with respective embodiments.
Embodiment 10
In the method for the coal tar hydrogenation of total effluent of the foregoing description 1～8, the raw material coalite tar with in isopyknic/the coalite tar replacement, other step is identical with respective embodiments.
Related raw material coalite tar in the foregoing description 1～10, coal-tar middle oil and in/character and the composition of coalite tar see table 3.
Table 3 coal tar character and composition/% (massfraction)
Claims (5)
1. the method for a coal tar hydrogenation of total effluent is characterized in that may further comprise the steps:
1) the full cut purifying treatment of coal tar removes moisture, metal and solid impurity in the coal tar;
2) coal tar after will purifying and hydrogen 150～250 ℃, 3～8MPa, hydrogen to oil volume ratio in molten hydrogen still are 800～1800:1, dissolve the hydrogen time and be to dissolve hydrogen under the condition in 15～40 minutes, obtain the liquid material of vapor liquid equilibrium;
3) liquid material of vapor liquid equilibrium being utilized the agent of RG-1 type hydrogenation protecting, the agent of FZC-200 type HDM, RMS-1 type hydrogenating desulfurization agent in first trickle-bed reactor is 0.28～2.6m at 260～360 ℃, 9～14MPa, liquid volume air speed
3H
-1/ m
3, hydrogen to oil volume ratio is to carry out the catalytic hydrogenation reaction first time under 900～1800:1 condition; Said RG-1 type hydrogenation protecting agent shared volume ratio in first trickle-bed reactor is 10%～30%; FZC-200 type HDM agent shared volume ratio in first trickle-bed reactor is 10%～40%; RMS-1 type hydrogenating desulfurization agent shared volume ratio in first trickle-bed reactor is 20%～50%; Surplus is a hydrogen, in second trickle-bed reactor, utilizes hydrodenitrification agent of RSN-1 type and FC-32 type hydrogen cracking agent at 360～410 ℃, 9～14MPa, liquid volume air speed 0.28～2.6m again
3H
-1/ m
3, carry out the catalytic hydrogenation reaction second time under hydrogen to oil volume ratio 1000～1800:1 condition; Said RSN-1 type hydrodenitrification agent shared volume ratio in second trickle-bed reactor is 20%～80%, and FC-32 type hydrogen cracking agent shared volume ratio in second trickle-bed reactor is 15%～50%, and surplus is a hydrogen, obtains the lighting product;
4) the lighting product is distilled processing in water distilling apparatus, cut out gasoline fraction, diesel oil distillate and tail oil.
2. the method for coal tar hydrogenation of total effluent according to claim 1 is characterized in that: after step 4), also comprise step 5), specifically: with 70%～80% returning step 2 as the circulation tail oil in the tail oil of step 4)) circular treatment.
3. the method for coal tar hydrogenation of total effluent according to claim 1; It is characterized in that: the type of RG-1 described in step 3) hydrogenation protecting agent shared volume ratio in first trickle-bed reactor is 15%～25%; FZC-200 type HDM agent shared volume ratio in first trickle-bed reactor is 15%～35%; RMS-1 type hydrogenating desulfurization agent shared volume ratio in first trickle-bed reactor is 25%～40%, and surplus is a hydrogen.
4. the method for coal tar hydrogenation of total effluent according to claim 1; It is characterized in that: said RSN-1 type hydrodenitrification agent shared volume ratio in second trickle-bed reactor is 30%～75%; FC-32 type hydrogen cracking agent shared volume ratio in second trickle-bed reactor is 24%～45%, and surplus is a hydrogen.
5. the method for coal tar hydrogenation of total effluent according to claim 1 is characterized in that: said coal tar be coalite tar or coal-tar middle oil or in/coalite tar.
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| CN103450937A (en) * | 2013-09-13 | 2013-12-18 | 王树宽 | Method for producing low-condensation-point diesel oil and liquid paraffin by using coal tar |
| CN111849552A (en) * | 2019-04-30 | 2020-10-30 | 中国石油化工股份有限公司 | Coal tar full-fraction hydrogenation upgrading method and system |
| CN112980484A (en) * | 2021-03-01 | 2021-06-18 | 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 |
| 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 |
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| 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 |
| CN114437807B (en) * | 2020-10-30 | 2024-06-11 | 中国石油化工股份有限公司 | Pretreatment method of coal tar |
| CN112980484A (en) * | 2021-03-01 | 2021-06-18 | 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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|---|---|
| CN102796560B (en) | 2014-07-09 |
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Inventor after: Shang Jianxuan Inventor after: Yang Zhanbiao Inventor after: Wang Shukuan Inventor before: Yang Zhanbiao Inventor before: Wang Shukuan |