CN1219570C - Method for separating and reclaiming spent iron based catalyst and heavy hydrocarbon through Fischer-Tropsch Synthesis in slurry bed - Google Patents
Method for separating and reclaiming spent iron based catalyst and heavy hydrocarbon through Fischer-Tropsch Synthesis in slurry bed Download PDFInfo
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- CN1219570C CN1219570C CN 200410012202 CN200410012202A CN1219570C CN 1219570 C CN1219570 C CN 1219570C CN 200410012202 CN200410012202 CN 200410012202 CN 200410012202 A CN200410012202 A CN 200410012202A CN 1219570 C CN1219570 C CN 1219570C
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Abstract
一种浆态床费托合成废铁基催化剂与重质烃的分离回收方法是用初馏点为210℃的轻质液体石蜡对废铁基催化剂与重质烃的混合物在加热和搅拌下抽提分离三到四次即可达到催化剂与重质烃分离的目的，抽提分离出的废铁基催化剂做卫生填埋处理，回收到的轻质液体石蜡与重质烃的混合物无需再分离可直接用于油品加工或返回浆态床反应器作为反应介质循环利用。本发明具有方法简单，工艺流程短，可减少环境污染的优点。本发明重质烃的回收率95～98%，回收的液体石蜡和重质烃的混合物中催化剂的含量小于0.5%。A method for separating and recovering waste iron-based catalysts and heavy hydrocarbons in a slurry bed Fischer-Tropsch synthesis is to use light liquid paraffin with an initial boiling point of 210°C to pump the mixture of waste iron-based catalysts and heavy hydrocarbons under heating and stirring. Three to four times of extraction and separation can achieve the purpose of separating the catalyst and heavy hydrocarbons. The waste iron-based catalyst extracted and separated can be disposed of in a sanitary landfill. The recovered mixture of light liquid paraffin and heavy hydrocarbons can be reused without further separation. It can be directly used in oil processing or returned to the slurry bed reactor as a reaction medium for recycling. The invention has the advantages of simple method, short process flow and reduced environmental pollution. The recovery rate of heavy hydrocarbons in the invention is 95-98%, and the catalyst content in the recovered mixture of liquid paraffin and heavy hydrocarbons is less than 0.5%.
Description
Technical field
The present invention relates to the separation and recovery method of a kind of catalyzer and heavy hydrocarbon, relate in particular to behind a kind of industrial syrup state bed Fischer Tropsch building-up reactions end of run the catalyst based separation and recovery method with heavy hydrocarbon of the scrap iron that goes out from reactor unloading.
Background technology
By synthetic gas (CO+H
2) process of generation hydro carbons is called Fischer-Tropsch synthesis under catalyst action.Iron-based and cobalt-base catalyst are the catalyzer of present most widely used two kinds of Fischer-Tropsch synthesizes industrializations.Coal based synthetic gas (mol ratio 0.5～1.2) Fischer-Tropsch that ferrum-based catalyst is suitable for low hydrogen-carbon ratio synthesizes, and the Fischer-Tropsch that cobalt-base catalyst is suitable for the synthetic gas (mol ratio 2) of Sweet natural gas base synthesizes.
Fischer-Tropsch is synthetic can to carry out in reactors such as fixed bed, fluidized-bed, circulating fluidized bed or slurry attitude bed.Fischer-Tropsch synthesis is a strong exothermal reaction, so it is very important in time removing reaction heat in the Fischer-Tropsch synthesis process, not only can avoid the too high catalyst deactivation that causes sintering of catalyst and cause of temperature, but also can avoid the generation of aromatic hydroxy compound to make the catalyst surface pollution and produce more non-purpose product C H
4For improving the thermo-efficiency of Fischer-Tropsch building-up process, slurry attitude bed technique is widely used.The syrup state bed Fischer Tropsch synthetic technology that gas upwards reacts by the liquid phase inert media that contains powdered catalyst in the bubbling mode, start from people's such as German H.K bel in 1938 and P.Alkermann research, this technology is all studied and has been used in the U.S., Britain and South Africa in succession subsequently.Paste state bed reactor not only has reactant and mixes; Pressure drop is little; Heat-transfer effect is good, but temperature of reaction is controlled characteristics such as isothermal operation easily, and has catalyzer and can onlinely load and unload; Can directly use low H
2The advantages such as coal based synthetic gas of/CO ratio are starched the attitude phase reactor simultaneously and are had few relatively investment, have demonstrated bigger technology, economic advantages, are the synthetic liquid fuel technology of giving priority in the world at present.
When Fischer-Tropsch synthesis carries out in slurry attitude phase reactor, to add the light liquid hydrocarbon compound in the reactor in advance as reaction medium, in entire reaction course, granules of catalyst is suspended in the liquid medium, and the solid content of slurries will maintain in the scope of 5～35wt%.Fischer-Tropsch synthesis can generate the product of gas, liquid and solid three-phase mixture, and solid phase heavy hydrocarbon product is collected by wax trap (180 ℃), but through underpressure distillation production food grade hard wax, lubricant base and detergent raw material; Oil phase and water liquid product are collected by hot trap (105 ℃) and cold-trap (0 ℃), produce gasoline, diesel oil, petroleum naphtha, aviation kerosene through the normal pressure distillation; Gas-phase product that can't condensation is that tail gas returns vapourizing furnace and generates the synthetic gas recycle after low temperature reclaims low-carbon alkene.Along with the carrying out of Fischer-Tropsch synthesis, the heavy hydrocarbon that reaction generates finishes the displacement of light liquid phase hydrocarbon compound medium gradually, and this moment, solid catalyst was suspended in the heavy hydrocarbon mixture of the high boiling point (150-300 ℃) that is in liquid phase under reaction conditions fully.When reaction finished, with liquid-phase mixing together, unloading back Yin Wendu reduction (being lower than 120 ℃) catalyzer was solid-state with the mixed solution that reacts the heavy hydrocarbon that generates very quick setting to the heavy hydrocarbon of catalyzer and reaction generation under temperature of reaction (250～280 ℃).The mixture of the catalyst based and solid-state heavy hydrocarbon of this scrap iron can only be used as waste and it be abandoned contaminate environment if be left intact.So separate with heavy hydrocarbon scrap iron is catalyst based, reclaim heavy hydrocarbon and be used for oil product processing or Returning reactor again as reaction medium, not only turn waste into wealth, and can reduce pollution environment.But through the document investigation, the separation and recovery method about synthetic spent catalyst of industrial syrup state bed Fischer Tropsch and heavy hydrocarbon does not still have bibliographical information at present.
Summary of the invention
The object of the present invention is to provide a kind of industrial syrup state bed Fischer Tropsch building-up reactions to finish the catalyst based separation and recovery method with heavy hydrocarbon of scrap iron that the back goes out from reactor unloading.
Separation and recovery method of the present invention comprises the steps:
1. analyze the content of scrap iron catalyzer of the mixture of the scrap iron catalyzer that unloads out from paste state bed reactor and heavy hydrocarbon;
2. the mixture with scrap iron catalyzer and heavy hydrocarbon adds in the reactor, be that 210 ℃ liquid paraffin,light is made solvent to the initial boiling point that wherein adds 2～5 times of scrap iron catalyzer and heavy hydrocarbon mixture weight then, begin when being heated to 70～100 ℃ to stir, continue to be heated to 120～180 ℃ then, and under this temperature, stirred 60～120 minutes;
3. standing sedimentation 30～90 minutes when settling temperature is 80～120 ℃, solid-liquid separation, and in the time of 80～120 ℃, discharge the liquid paraffin,light on upper strata and the mixed solution of heavy hydrocarbon;
4. the initial boiling point that adds 2～6 times of spent catalyst weight once more in reactor is 210 ℃ a liquid paraffin,light, is heated to 120～180 ℃, stirs 30～90 minutes; Standing sedimentation 30～90 minutes, 80～120 ℃ of settling temperature, solid-liquid separation, and in the time of 80～120 ℃, discharge the liquid paraffin,light on upper strata and the mixed solution of heavy hydrocarbon.
5. repeating step 4 one is to secondary;
6. the liquid paraffin,light that can't discharge with the standing sedimentation solid-liquid separation in the reactor is distilled 210～320 ℃ temperature range;
Aforesaid (2) step is that mixture with heavy hydrocarbon that scrap iron is catalyst based adds in the reactor, be that 210 ℃ liquid paraffin,light is made solvent to wherein adding the catalyst based initial boiling point of scrap iron then with 2～3 times of heavy hydrocarbon mixture weight, begin when being heated to 80～90 ℃ to stir, continue to be heated to 140～150 ℃ then, and under this temperature, stirred 60～90 minutes;
Aforesaid (3) step is when settling temperature is 100～120 ℃, standing sedimentation 60～90 minutes, and solid-liquid separation, and in the time of 80～120 ℃, discharge the liquid paraffin,light on upper strata and the mixed solution of heavy hydrocarbon.
Aforesaid (4) step is that the initial boiling point that adds 2～3 times of the catalyst based weight of scrap iron once more in reactor is 210 ℃ a liquid paraffin,light, is heated to 140～150 ℃, stirs 45～60 minutes; When settling temperature is 100～120 ℃, standing sedimentation 45～60 minutes, solid-liquid separation, and in the time of 80～120 ℃, discharge the liquid paraffin,light on upper strata and the mixed solution of heavy hydrocarbon.
The heavy hydrocarbon that aforesaid method obtains needn't separate with the mixture of liquid paraffin,light, can be directly used in oil product processing or return slurry bed ft synthetic reactor again as reaction medium, and scrap iron is catalyst based to be done sanitary landfill and handle.
The rate of recovery of heavy hydrocarbon of the present invention is 95～98%, and the content of catalyzer is less than 0.5% in the liquid paraffin,light that recovery obtains and the mixed solution of heavy hydrocarbon.
The invention has the advantages that:
1. method is simple, and technical process is short.
2. it is cheap and easy to get to separate the solvent liquid paraffin,light, separates the back and mixes with heavy hydrocarbon, and such mixture does not need any processing directly to utilize.
3. minimizing environmental pollution turns harm into good, and favorable economic benefit is arranged.
Embodiment
Describe several specific embodiments of the present invention below in detail, protection scope of the present invention is not subjected to the restriction of these embodiment.
The analysis test method that the present invention is used:
1. the mensuration of solid content: adopt gravimetric determination.
2. spent catalyst assay in the mixture of liquid paraffin,light of Hui Shouing and heavy hydrocarbon: adopt atomic spectroscopy to measure.
Embodiment 1:
1. the useless Fe/Cu/K/SiO under unloading is carried
2The mixture of catalyzer and heavy hydrocarbon, solid content analytical results: spent catalyst 19.8%, heavy hydrocarbon 80.2%.
2. with 100 kilograms of useless Fe/Cu/K/SiO
2The mixture of catalyzer and heavy hydrocarbon adds and has in the reactor of heated and stirred reflux, be that 210 ℃ liquid paraffin,light is made solvent to the initial boiling point that wherein adds 200 kilograms then, open stirring when being heated to 70 ℃, continue to be heated to 120 ℃ then, and under this temperature, stirred 100 minutes, making heavy hydrocarbon and initial boiling point is that 210 ℃ liquid paraffin,light is fully miscible.
3. 100 ℃ of following standing sedimentations 60 minutes, solid-liquid separation is discharged 225 kilograms of the mixed solutions of the liquid paraffin,light on upper strata and heavy hydrocarbon.
4. the initial boiling point that adds 80 kilograms once more in reactor is 210 ℃ a liquid paraffin,light, is heated to 120 ℃, stirs 60 minutes.
5. repeating step 3, discharge 92 kilograms of mixed solutions.
6. the initial boiling point that adds 65 kilograms for the third time in reactor is 210 ℃ a liquid paraffin,light, is heated to 120 ℃, stirs 60 minutes.
7. repeating step 3, discharge 47 kilograms of mixed solutions.
8. merge three extractings and separate the liquid paraffin,light of discharge and the mixed solution of heavy hydrocarbon, gross weight is 382 kilograms.
9. the liquid paraffin,light that can't discharge with the standing sedimentation solid-liquid separation in the reactor is distilled 210～320 ℃ temperature range, distillation receives 24 kilograms of liquid paraffin,lights.
The rate of recovery of the inventive method heavy hydrocarbon is 97%, and the content of catalyzer is less than 0.5% in the liquid paraffin,light that recovery obtains and the mixed solution of heavy hydrocarbon.
Embodiment 2:
1. get from starching the useless Fe/Mn/K/SiO under the unloading of attitude bed
2Catalyzer, solid content analytical results: spent catalyst 31.5%, heavy hydrocarbon 68.5%.
2. with 150 kilograms of useless Fe/Mn/K/SiO
2The mixture of catalyzer and heavy hydrocarbon adds and has in the reactor of heated and stirred reflux, be that 210 ℃ liquid paraffin,light is made solvent to the initial boiling point that wherein adds 600 kilograms then, open stirring when being heated to 80 ℃, continue to be heated to 140 ℃ then, and under this temperature, stirred 75 minutes, making heavy hydrocarbon and initial boiling point is that 210 ℃ liquid paraffin,light is fully miscible.
3. 80 ℃ of following standing sedimentations 30 minutes, solid-liquid separation is discharged 643 kilograms of the mixed solutions of the liquid paraffin,light on upper strata and heavy hydrocarbon.
4. the initial boiling point that adds 120 kg once more in reactor is 210 ℃ a liquid paraffin,light, is heated to 140 ℃, stirs 50 minutes.
5. repeating step 3, discharge 125 kilograms of mixed solutions.
6. the initial boiling point that adds 120 kg for the third time in reactor is 210 ℃ a liquid paraffin,light, is heated to 140 ℃, stirs 50 minutes.
7. repeating step 3, discharge 122 kilograms of mixed solutions.
8. merge three extractings and separate the liquid paraffin,light of discharge and the mixed solution of heavy hydrocarbon, gross weight is 890 kilograms.
9. the liquid paraffin,light that can't discharge with the standing sedimentation solid-liquid separation in the reactor is distilled 210～320 ℃ temperature range, distillation receives 25 kilograms of liquid paraffin,lights.
The rate of recovery of the inventive method heavy hydrocarbon is 96%, and the content of catalyzer is less than 0.5% in the liquid paraffin,light that recovery obtains and the mixed solution of heavy hydrocarbon.
Embodiment 3:
1. get from starching the useless Fe/Mn/Cu/K/SiO under the unloading of attitude bed
2Catalyzer, solid content analytical results: spent catalyst 17.6%, heavy hydrocarbon 82.4%.
2. with 180 kilograms of useless Fe/Mn/Cu/K/SiO
2The mixture of catalyzer and heavy hydrocarbon adds and has in the reactor of heated and stirred reflux, be that 210 ℃ liquid paraffin,light is made solvent to the initial boiling point that wherein adds 450 kilograms then, open stirring when being heated to 90 ℃, continue to be heated to 160 ℃ then, and under this temperature, stirred 60 minutes, making heavy hydrocarbon and initial boiling point is that 210 ℃ liquid paraffin,light is fully miscible.
3. 110 ℃ of following standing sedimentations 55 minutes, solid-liquid separation is discharged 500 kilograms of the mixed solutions of the liquid paraffin,light on upper strata and heavy hydrocarbon.
4. the initial boiling point that adds 100 kilograms once more in reactor is 210 ℃ a liquid paraffin,light, is heated to 160 ℃, stirs 30 minutes.
5. repeating step 3, discharge 125 kilograms of mixed solutions.
6. the initial boiling point that adds 90 kilograms for the third time in reactor is 210 ℃ a liquid paraffin,light, is heated to 160 ℃, stirs 30 minutes.
7. repeating step 3, discharge 102 kilograms of mixed solutions.
8. merge three extractings and separate the liquid paraffin,light of discharge and the mixed solution of heavy hydrocarbon, gross weight is 727 kilograms.
9. the liquid paraffin,light that can't discharge with the standing sedimentation solid-liquid separation in the reactor is distilled 210～320 ℃ temperature range, distillation receives 33 kilograms of liquid paraffin,lights.
The rate of recovery of the inventive method heavy hydrocarbon is 95.8%, and the content of catalyzer is less than 0.5% in the liquid paraffin,light that recovery obtains and the mixed solution of heavy hydrocarbon.
Embodiment 4:
1. get from starching the useless Fe/La/Cu/K/SiO under the unloading of attitude bed
2Catalyzer, solid content analytical results: spent catalyst 23.9%, heavy hydrocarbon 76.1%.
2. with the useless Fe/La/Cu/K/SiO of 120 kg
2The mixture of catalyzer and heavy hydrocarbon adds and has in the reactor of heated and stirred reflux, be that 210 ℃ liquid paraffin,light is made solvent to the initial boiling point that wherein adds 400 kilograms then, open stirring when being heated to 100 ℃, continue to be heated to 180 ℃ then, and under this temperature, stirred 120 minutes, making heavy hydrocarbon and initial boiling point is that 210 ℃ liquid paraffin,light is fully miscible.
3. 120 ℃ of following standing sedimentations 90 minutes, solid-liquid separation is discharged 425 kilograms of the mixed solutions of the liquid paraffin,light on upper strata and heavy hydrocarbon.
4. the initial boiling point that adds 120 kg once more in reactor is 210 ℃ a liquid paraffin,light, is heated to 180 ℃, stirs 90 minutes.
5. repeating step 3, discharge 128 kilograms of mixed solutions.
6. the initial boiling point that adds 100 kilograms for the third time in reactor is 210 ℃ a liquid paraffin,light, is heated to 180 ℃, stirs 90 minutes.
7. repeating step 3, discharge 106 kilograms of mixed solutions.
8. merge three extractings and separate the liquid paraffin,light of discharge and the mixed solution of heavy hydrocarbon, gross weight is 647 kilograms.
9. the liquid paraffin,light that can't discharge with the standing sedimentation solid-liquid separation in the reactor is distilled 210～320 ℃ temperature range, distillation receives 41 kilograms of liquid paraffin,lights.
The rate of recovery of the inventive method heavy hydrocarbon is 95.3%, and the content of catalyzer is less than 0.5% in the liquid paraffin,light that recovery obtains and the mixed solution of heavy hydrocarbon.
Claims (4)
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410012202 CN1219570C (en) | 2004-03-19 | 2004-03-19 | Method for separating and reclaiming spent iron based catalyst and heavy hydrocarbon through Fischer-Tropsch Synthesis in slurry bed |
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| CN 200410012202 CN1219570C (en) | 2004-03-19 | 2004-03-19 | Method for separating and reclaiming spent iron based catalyst and heavy hydrocarbon through Fischer-Tropsch Synthesis in slurry bed |
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| CN1219570C true CN1219570C (en) | 2005-09-21 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7674369B2 (en) * | 2006-12-29 | 2010-03-09 | Chevron U.S.A. Inc. | Process for recovering ultrafine solids from a hydrocarbon liquid |
| CN110387261B (en) * | 2019-07-03 | 2021-10-22 | 国家能源集团宁夏煤业有限责任公司 | Fischer-Tropsch wax residue treatment device and treatment method |
| CN110369004A (en) * | 2019-07-03 | 2019-10-25 | 国家能源集团宁夏煤业有限责任公司 | Treatment device and treatment method for Fischer-Tropsch waste catalyst |
| CN111303937A (en) * | 2019-08-20 | 2020-06-19 | 武汉兰兆科技有限公司 | Electric separation device and electric separation process for on-line recycling of Fischer-Tropsch synthesis catalyst |
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Owner name: ZHONGKE SYNTHETIC OIL TECHNOLOGY CO., LTD., DISTR Free format text: FORMER OWNER: SHANXI INST. OF COAL CHEMISTRY, CHINESE ACADEMY OF SCIENCES Effective date: 20060818 |
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Effective date of registration: 20060818 Address after: 030006, Shanxi, Taiyuan hi tech Zone, South Central Cyberport 2, port 4, A, B District Patentee after: Zhongke Synthetic Oil Technology Co., Ltd. Address before: 165 mailbox 030001, Shanxi City, Taiyuan Province Patentee before: Shanxi Institute of Coal Chemistry, Chinese Academy of Sciences |
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Assignee: Huainan Catalyst Co., Ltd. of Synfuels China Assignor: Zhongke Synthetic Oil Technology Co., Ltd. Contract record no.: 2010340000069 Denomination of invention: Method for separating and reclaiming spent iron based catalyst and heavy hydrocarbon through Fischer-Tropsch Synthesis in slurry bed Granted publication date: 20050921 License type: Exclusive License Open date: 20050112 Record date: 20100427 |
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Address after: 101407 Beijing city Huairou District Yanqi Economic Development Zone C District No. 1 south two Street Park Patentee after: Zhongke Synthetic Oil Technology Co., Ltd. Address before: 030006, Shanxi, Taiyuan hi tech Zone, South Central Cyberport 2, port 4, A, B District Patentee before: Zhongke Synthetic Oil Technology Co., Ltd. |
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Address after: 101407 No.1, south 2nd Yueyuan street, C District, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Zhongke synthetic oil Technology Co.,Ltd. Address before: 101407 No.1, south 2nd Yueyuan street, C District, Yanqi Economic Development Zone, Huairou District, Beijing Patentee before: SYNFUELS CHINA TECHNOLOGY Co.,Ltd. |
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