CN109097099B - Method for preparing diesel oil by coal tar hydrogenation and product thereof - Google Patents
Method for preparing diesel oil by coal tar hydrogenation and product thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing diesel oil by coal tar hydrogenation and a product thereof, wherein hydrogen with a hydrogen-oil volume ratio of 850-1100 and coal tar distillate are mixed and then enter a reactor, the reaction temperature is 290-365 ℃, the reaction pressure is 2-9MPa, and the space velocity is 2-4h‑1Reacting under the action of a catalyst, and separating liquid products through gas-liquid separation to obtain the catalyst.
Description
The original invention patent applied by this divisional application has application date of 2015, 06, 15 and application numbers of: 201510330409.4 entitled "a method for preparing diesel oil from coal tar".
Technical Field
The invention relates to a method for preparing diesel oil by coal tar hydrogenation and a product thereof.
Background
Coal tar is generally produced by coal dry distillation and is divided into low-temperature dry distillation, medium-temperature dry distillation and high-temperature dry distillation, wherein the yield of coal tar is the highest in the low-temperature dry distillation of coal, while coal suitable for the low-temperature dry distillation is non-coking coal without cohesiveness, such as lignite or high-volatility bituminous coal, and in China, the coal is rich in reserves and is the basis for producing coal tar and preparing diesel oil by low-temperature dry distillation. The low-temperature dry distillation process is much simpler than the gasification or direct liquefaction of coal, the conditions are mild, and if the low-temperature dry distillation process can be reasonably utilized, the low-temperature dry distillation process can become a good diesel oil production source.
CN88105117 discloses a formula of a diesel oil substituted fuel oil agent and a preparation method thereof, which takes coal tar as raw material, and the fuel oil agent is prepared by the procedures of refining, distilling, emulsifying, water adding, purifying and the like, and is used as fuel oil, but can not replace diesel oil. US4855037 describes a catalyst and a process for the hydrogenation of coal tar for delayed coking by improving mainly the pore size, pore distribution and metal components of the catalyst and by selecting suitable process conditions to increase the stability of the catalyst, which is mainly a pre-treatment for delayed coking and does not produce the desired products. In addition, a protective agent is required to be added in the hydrogenation process of preparing diesel oil from coal tar, so that metal impurities and solid particles in the oil product are effectively removed, substances which are easy to coke in the raw materials are properly hydrogenated, the poisoning and coking of the main catalyst are slowed down, and the service life of the main catalyst is prolonged. Patent CN1147575C discloses a method for producing diesel oil from coal tar, which adds a protective agent, a hydrorefining catalyst and a dearomatization catalyst into a reaction system through a catalyst loading scheme of two-stage grading or three-stage grading, to obtain a certain effect, but the protective agent has a limited effect and cannot maximize the hydrogenation efficiency.
The catalyst for preparing diesel oil by coal tar hydrogenation and the process for preparing diesel oil by using the catalyst have the following application numbers: 200510012554.4 application date: 2005-05-25, the invention is a catalyst for preparing diesel oil by coal tar hydrogenation and a process for preparing diesel oil by using the catalyst. The catalyst for preparing diesel oil by coal tar hydrogenation comprises a first-stage catalyst and a second-stage catalyst, wherein the first-stage catalyst is a hydrodesulfurization and denitrification cracking catalyst, and the second-stage catalyst is a hydrogenation deep dearomatization catalyst. The process for preparing the diesel by using the catalyst for preparing the diesel by hydrogenating the coal tar comprises the steps of atmospheric distillation of the coal tar, primary catalysis of fuel oil, secondary catalysis of the fuel oil, gas stripping and separation; the first-stage catalyst used for the first-stage catalysis of the fuel oil is the hydrodesulfurization denitrification cracking catalyst, and the second-stage catalyst used for the second-stage catalysis of the fuel oil is the hydrogenation deep dearomatization catalyst. The invention greatly improves the temperature resistance of the catalyst for preparing diesel oil by coal tar hydrogenation, enlarges the range of the usable raw material coal tar, reduces the content of aromatic hydrocarbon in the finished product of the diesel oil to the minimum, improves the cetane number, and leads the product to completely reach the national diesel oil standard.
A method for producing high-quality diesel oil by hydrogenation of heavy coal tar distillate is disclosed in the application number: 200710010382.6 application date: 2007-02-09, the invention discloses a method for producing high-quality diesel oil by hydrogenation of heavy coal tar distillate. The method adopts a hydrofining-hydrocracking-upgrading combined process, which comprises the steps of mixing a coal tar heavy fraction with hydrogen and entering a hydrofining reaction zone, enabling a part of obtained diesel fraction and tail oil to enter the hydrocracking/upgrading reaction zone after refined effluent passes through a separation system, recycling part or all of the obtained hydrocracking/upgrading reaction effluent as hydrofining feed, and enabling the rest part to enter the separation system. Compared with the prior art, the method not only can hydrogenate the heavy coal tar distillate to produce high-quality low-freezing diesel products, but also can take the byproduct naphtha as the reformed raw oil, provides an application approach with higher added value for the heavy coal tar oil, and relieves the current situation of supply and demand tension of petroleum-based diesel.
A method for producing diesel oil and heavy fuel oil by coal tar, which has the following application numbers: 200810302167.8 application date: 2008-06-17, the invention discloses a method for producing diesel oil and heavy fuel oil by coal tar, which comprises the following steps of (1) pre-treating coal tar, namely pre-dehydrating the coal tar until the water content is 2-3 WT%, then adding a sodium carbonate solution accounting for 0.5-1% of the weight of the coal tar for desalting treatment, heating to 110-; preheating the pretreated coal tar to 350-400 ℃, then feeding the coal tar into a normal pressure distillation unit, collecting light fractions with the boiling point less than 300 ℃, and obtaining the diesel oil through alkali washing, acid washing, alkali washing and refining; and collecting heavy fractions with the boiling point of above 300 ℃, and carrying out thermal refining treatment to obtain the heavy fuel oil. The invention has the advantages of good product quality and low production cost.
A method for preparing diesel components by catalytic cracking of coal tar light fractions, application No.: 200810302719.5 application date: 2008-07-14. the invention discloses a method for preparing a diesel component by catalytic cracking of coal tar light fraction, which comprises the following steps of placing the coal tar light fraction in a catalytic cracking device, and reacting at the temperature of 400-450 ℃, the pressure of 0.05-0.4MPA and the oil gas airspeed of 0.5-2.5H < -1 > to obtain the diesel component. The method has the advantages of simple process, high conversion rate and stable operation, and belongs to the field of deep processing of coal tar.
Disclosure of Invention
The invention provides a method for preparing diesel oil by coal tar hydrogenation and a product thereof.
A method for preparing diesel oil by coal tar hydrogenation comprises the steps of mixing hydrogen with a hydrogen oil volume ratio of 850-1100 with coal tar distillate, and then feeding the mixture into a reactor, wherein the reaction temperature is 290-365 ℃, the reaction pressure is 2-9MPa, and the space velocity is 2-4h-1Reacting under the action of a catalyst, and separating liquid products through gas-liquid separation to obtain the catalyst.
The reaction temperature is preferably 305-350 ℃; the reaction pressure is preferably 4-6 MPa; the space velocity is preferably 0.5 to 2h-1。
The space velocity mentioned above is the volume space velocity.
The preparation method of the catalyst for preparing diesel oil by coal tar hydrogenation comprises the following steps:
drying the carrier at 110-130 ℃ for 20 minutes, then soaking the carrier in an iodine compound solution, keeping the temperature at 40-60 ℃ for 1 hour, taking out the carrier, and drying the carrier in an oven at 90-120 ℃ for 1 hour; adding acid modified attapulgite with the mass of 2-5% of the carrier into a mixed solution of nitrates of Co, Mo and W, uniformly stirring, soaking the dried carrier into the mixed solution for 2-3 hours at the temperature of 30-45 ℃, stirring and dispersing for 10-60min, drying, and roasting at the temperature of 270-420 ℃ for 3-8 hours to obtain the catalyst powder.
The carrier is Y-type molecular sieve or nano Al2O3
The soluble salts of Co, Mo and W are nitrates.
Nitrate mixed solution of Co, Mo, W: the three nitrates are prepared into a mixed solution, the weight concentrations of the nitrates in the mixed solution are respectively Co 8-14 wt%, Mo 10-16 wt%, and WO32-5wt％。
The iodine-containing compound mixed solution comprises 3-8 wt% of KI, 4-6 wt% of NaI and NaIO3 6-10wt％。
Nano Al2O3The particle diameter of the carrier is 5 to 20nm, preferably 5 to 10 nm.
The invention has the following advantages:
1. the method is a one-step catalytic reaction system, removes S, N, O and other impurities in the coal tar distillate, and simultaneously can saturate or isomerize aromatic hydrocarbon, thereby omitting the complicated steps of two-stage catalytic reaction, and reducing the design difficulty and equipment cost;
the catalytic activity is further improved, the yield can reach 99 percent, the S content is not higher than 120 mu g, the N content is not higher than 200 mu g, the aromatic hydrocarbon content is not higher than 32 percent, and the catalyst can be used as finished fuel oil;
Detailed Description
The space velocity described in the examples below is the volumetric space velocity.
Example 1
A method for preparing diesel oil by coal tar hydrogenation and a product thereof are characterized in that hydrogen with a hydrogen-oil volume ratio of 1000 and coal tar distillate are mixed and then enter a reactor, the reaction temperature is 370 ℃, the reaction pressure is 10MPa, and the airspeed is 2h-1Reacting under the action of a catalyst, and separating liquid products through gas-liquid separation to obtain the catalyst.
The active components of the catalyst are Co, Mo and W, and the carrier is nano Al2O3The carrier and the catalyst composition are 5 wt% of CoO and 17.5 wt% of MoO320% by weight of WO3The balance being nano Al2O3Support, nano Al2O3The particle diameter of the carrier is 5-20nm, most of which is between 5-10 nm.
The product yield can reach 97 percent, the S content is 159 mu g, the N content is 228 mu g, and the aromatic hydrocarbon content is 32.8 percent, and the product can be used as finished fuel oil.
Example 2
The invention provides a method for preparing diesel oil by coal tar hydrogenation and a product thereof.
A method for preparing diesel oil by coal tar hydrogenation comprises the steps of mixing hydrogen with coal tar distillate in a hydrogen-oil volume ratio of 1000, and then feeding the mixture into a reactor, wherein the reaction temperature is 320-345 ℃, the reaction pressure is 2-5MPa, and the space velocity is 2-3h-1Reacting under the action of a catalyst, and separating liquid products through gas-liquid separation to obtain the catalyst.
The preparation method of the catalyst for preparing diesel oil by coal tar hydrogenation comprises the following steps:
drying the carrier at 120 ℃ for 20 minutes, soaking the carrier in an iodine compound-containing solution, keeping the temperature at 50 ℃ for 1 hour, taking out the carrier, and drying the carrier in a 110 ℃ oven for 1 hour; adding acid modified attapulgite with the mass of 4% of the carrier into a mixed solution of nitrates of Co, Mo and W, uniformly stirring, soaking the dried carrier into the mixed solution for 2 hours, controlling the temperature at 40 ℃, stirring and dispersing for 40 minutes, drying, and roasting at 370-410 ℃ for 6 hours to obtain the catalyst powder.
The carrier is a Y-type molecular sieve.
Nitrate mixed solution of Co, Mo, W: the weight concentrations of the nitrates in the mixed solution are respectively Co 14 wt%, Mo 15 wt% and WO34wt％。
The iodine-containing compound mixed solution comprises 5 wt% of KI, 5 wt% of NaI and 5 wt% of NaIO3 8wt％。
Nano Al2O3The particle diameter of the support was 8 nm.
The product yield can reach 99 percent, the S content is 103 mug, the N content is 107 mug, the aromatic hydrocarbon content is 31 percent, and the product can be used as finished fuel oil.
Example 3
The invention provides a method for preparing diesel oil by coal tar hydrogenation and a product thereof.
A method for preparing diesel oil by coal tar hydrogenation comprises the steps of mixing hydrogen with coal tar distillate in a hydrogen-oil volume ratio of 900, and then feeding the mixture into a reactor, wherein the reaction temperature is 310--1Reacting under the action of a catalyst, and separating liquid products through gas-liquid separation to obtain the catalyst.
The preparation method of the catalyst for preparing diesel oil by coal tar hydrogenation comprises the following steps:
drying the carrier at 110 ℃ for 20 minutes, soaking the carrier in an iodine compound-containing solution, keeping the temperature at 40 ℃ for 1 hour, taking out the carrier, and drying the carrier in a 110 ℃ oven for 1 hour; adding acid modified attapulgite with the mass of 3% of the carrier into a mixed solution of nitrates of Co, Mo and W, uniformly stirring, soaking the dried carrier into the mixed solution for 3 hours, controlling the temperature at 45 ℃, stirring and dispersing for 40 minutes, drying, and roasting at 370-410 ℃ for 6 hours to obtain the catalyst powder.
The carrier is a Y-type molecular sieve.
Nitrate mixed solution of Co, Mo, W: the weight concentrations of the nitrates in the mixed solution are respectively Co 14 wt%, Mo 15 wt% and WO34wt％。
The iodine-containing compound mixed solution comprises 5 wt% of KI, 5 wt% of NaI and 5 wt% of NaIO3 8wt％。
Nano Al2O3The particle diameter of the support was 8 nm.
The product yield can reach 95 percent, the S content is 86 mu g, the N content is 125 mu g, the aromatic hydrocarbon content is 29.1 percent, and the product can be used as finished fuel oil.
Example 4
The invention provides a method for preparing diesel oil by coal tar hydrogenation and a product thereof.
A preparation method of diesel oil by coal tar hydrogenation comprises the steps of mixing hydrogen with coal tar distillate in a hydrogen-oil volume ratio of 1100, and then feeding the mixture into a reactor, wherein the reaction temperature is 320-345 ℃, the reaction pressure is 5-7MPa, and the space velocity is 2-3h-1Reacting under the action of a catalyst, and separating liquid products through gas-liquid separation to obtain the catalyst.
The preparation method of the catalyst for preparing diesel oil by coal tar hydrogenation comprises the following steps:
drying the carrier at 120 ℃ for 20 minutes, soaking the carrier in an iodine compound-containing solution, keeping the temperature at 50 ℃ for 1 hour, taking out the carrier, and drying the carrier in a 110 ℃ oven for 1 hour; adding acid modified attapulgite with the mass of 4% of the carrier into a mixed solution of nitrates of Co, Mo and W, uniformly stirring, soaking the dried carrier into the mixed solution for 2 hours, controlling the temperature at 40 ℃, stirring and dispersing for 40 minutes, drying, and roasting at 390-410 ℃ for 6 hours to obtain the catalyst powder.
The carrier is a Y-type molecular sieve.
Nitrate mixed solution of Co, Mo, W: the weight concentrations of the nitrates in the mixed solution are respectively Co 14 wt%, Mo 15 wt% and WO34wt％。
The iodine-containing compound mixed solution comprises 5 wt% of KI, 5 wt% of NaI and 5 wt% of NaIO3 8wt％。
Nano Al2O3The particle diameter of the support was 8 nm.
The product yield can reach 99 percent, the S content is 62 mug, the N content is 178 mug, the aromatic hydrocarbon content is 30.8 percent, and the product can be used as finished fuel oil.
Claims (4)
1. Hydrogenation of coal tarA method for producing diesel, characterized by: the method comprises the following steps: mixing hydrogen with a hydrogen-oil volume ratio of 1000 and coal tar distillate, and introducing the mixture into a reactor, wherein the reaction temperature is 320-345 ℃, the reaction pressure is 2-5MPa, and the volume space velocity is 2-3h-1Reacting under the action of a catalyst, and obtaining a liquid product through gas-liquid separation to obtain a diesel product, wherein the preparation method of the catalyst comprises the following steps:
drying the carrier at 120 ℃ for 20 minutes, soaking the carrier in an iodine compound-containing solution, keeping the temperature at 50 ℃ for 1 hour, taking out the carrier, and drying the carrier in a 110 ℃ oven for 1 hour; the mass concentrations of the nitrates added with the acid modified attapulgite accounting for 4 percent of the mass of the carrier are respectively Co 14 weight percent, Mo 15 weight percent and WO3Uniformly stirring in a 4 wt% nitrate mixed solution, soaking a dry carrier in the mixed solution for 2 hours, controlling the temperature at 40 ℃, stirring and dispersing for 40min, drying, and roasting at the temperature of 370 ℃ and 410 ℃ for 6 hours to prepare catalyst powder, wherein the carrier is a Y-type molecular sieve or nano Al2O3.(ii) a The iodine-containing compound solution comprises 5 wt% of KI, 5 wt% of NaI and 5 wt% of NaIO38wt％。
2. The method for preparing diesel oil by hydrogenating coal tar according to claim 1, wherein the nano Al is2O3The particle diameter of (2) is 8 nm.
3. A diesel fuel produced by the production method according to any one of claims 1 to 2.
4. Use of the diesel fuel of claim 3 in finished fuel oil.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810959538.3A CN109097099B (en) | 2015-06-15 | 2015-06-15 | Method for preparing diesel oil by coal tar hydrogenation and product thereof |
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| CN201810959538.3A CN109097099B (en) | 2015-06-15 | 2015-06-15 | Method for preparing diesel oil by coal tar hydrogenation and product thereof |
| CN201510330409.4A CN104987882B (en) | 2015-06-15 | 2015-06-15 | A method of utilizing preparing diesel from coal tar |
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| CN201510330409.4A Division CN104987882B (en) | 2015-06-15 | 2015-06-15 | A method of utilizing preparing diesel from coal tar |
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| CN109097099B true CN109097099B (en) | 2020-11-17 |
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| CN201810959538.3A Active CN109097099B (en) | 2015-06-15 | 2015-06-15 | Method for preparing diesel oil by coal tar hydrogenation and product thereof |
| CN201810959088.8A Pending CN109097097A (en) | 2015-06-15 | 2015-06-15 | The method and products thereof of diesel oil processed is reacted using the catalysis of one step of coal tar |
| CN201810959090.5A Pending CN109097098A (en) | 2015-06-15 | 2015-06-15 | A kind of method and products thereof of coal tar desulfurization removing nitric diesel oil |
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| CN201810959090.5A Pending CN109097098A (en) | 2015-06-15 | 2015-06-15 | A kind of method and products thereof of coal tar desulfurization removing nitric diesel oil |
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| CN105296001B (en) * | 2015-11-16 | 2017-06-30 | 西北大学 | A kind of coal tar hydrogenating catalytic reforming prepares the system and method for aromatic hydrocarbons |
| CN113522300A (en) * | 2020-04-20 | 2021-10-22 | 广元市天森煤化有限公司 | Catalyst for preparing fuel oil from coal tar and preparation method thereof |
| CN115254119B (en) * | 2021-04-29 | 2024-03-26 | 中国石油化工股份有限公司 | Coal tar hydrogenation catalyst and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5328590A (en) * | 1992-02-27 | 1994-07-12 | Union Oil Company Of California | Hydrocracking process using a catalyst containing zeolite beta and a layered magnesium silicate |
| CN101376816A (en) * | 2007-08-29 | 2009-03-04 | 汉能科技有限公司 | Method for preparing diesel from coal tar |
| CN102002387A (en) * | 2010-11-25 | 2011-04-06 | 邵素英 | Method for preparing fuel oil |
| CN102477310A (en) * | 2010-11-25 | 2012-05-30 | 邵素英 | Method using coal tar to produce fuel oil |
-
2015
- 2015-06-15 CN CN201510330409.4A patent/CN104987882B/en active Active
- 2015-06-15 CN CN201810959538.3A patent/CN109097099B/en active Active
- 2015-06-15 CN CN201810959088.8A patent/CN109097097A/en active Pending
- 2015-06-15 CN CN201810959090.5A patent/CN109097098A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5328590A (en) * | 1992-02-27 | 1994-07-12 | Union Oil Company Of California | Hydrocracking process using a catalyst containing zeolite beta and a layered magnesium silicate |
| CN101376816A (en) * | 2007-08-29 | 2009-03-04 | 汉能科技有限公司 | Method for preparing diesel from coal tar |
| CN102002387A (en) * | 2010-11-25 | 2011-04-06 | 邵素英 | Method for preparing fuel oil |
| CN102477310A (en) * | 2010-11-25 | 2012-05-30 | 邵素英 | Method using coal tar to produce fuel oil |
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| CN104987882A (en) | 2015-10-21 |
| CN104987882B (en) | 2018-11-23 |
| CN109097097A (en) | 2018-12-28 |
| CN109097098A (en) | 2018-12-28 |
| CN109097099A (en) | 2018-12-28 |
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