CN101643655B - Method for preparing gas-liquid fuels by scrap tire vacuum pyrolysis - Google Patents
Method for preparing gas-liquid fuels by scrap tire vacuum pyrolysis Download PDFInfo
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- CN101643655B CN101643655B CN2009101832358A CN200910183235A CN101643655B CN 101643655 B CN101643655 B CN 101643655B CN 2009101832358 A CN2009101832358 A CN 2009101832358A CN 200910183235 A CN200910183235 A CN 200910183235A CN 101643655 B CN101643655 B CN 101643655B
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Abstract
The invention discloses a method for preparing gas-liquid fuels by scrap tire vacuum pyrolysis, and the method is to carry out vacuum pyrolysis on an integral device by a fixed bed containing high efficient desulfuration and to carry out vacuum pyrolysis on a scrap tire under the condition of load-type solid base catalyst to prepare the gas-liquid fuels. By using the method of the invention, sulphur in the volatile matter can be effectively removed, the obtained gas-liquid products can be directly taken as fuel for using, and the load-type solid catalyst not only can increase heat transfer efficiency of the scrap tires, but also can improve the content of high value-added products in fluid oil phase. The method is economical and feasible, has no discharging of the three wastes, and realizes zero pollution on the environment, and meanwhile, wastes are changed into wealth, which conforms to sustainable developmental tendency of the future resources.
Description
Technical field
The present invention relates to the solid waste safe disposal and utilize technical field, relate in particular to a kind of containing the high-efficiency desulfurization effect fixed bed vacuum cracking integrated apparatus and the condition of load type solid body base catalyst under junked tire is carried out vacuum cracking, prepare the method for gas-liquid fuels.
Background technology
Along with being on the rise of energy dilemma and environmental problem, the recycling of organic solid castoff (such as junked tire) becomes the focus of people's research gradually in recent years.China is the tire production big country that is only second to the U.S., the rough estimates of announcing on January 22nd, 2009 according to State Statistics Bureau show, China's accumulative total was produced 5.4614 hundred million on tire in 2008, increase by 6.7% on a year-on-year basis, 2,380,000 tons of synthetic rubber accumulative totals, increase by 9.2% on a year-on-year basis, the junked tire generation is above 1.5 hundred million.How the effective recycling junked tire prevents that to environment this is a global problem, also is the new problem that China's utilization of the recycling of renewable resources faces.Damaged tire has very strong heat impedance, antibiont and anti-mechanicalness, is called by people " black pollution ".Owing to lack effectively management, many junked tires flow in the local method refiner hand, have not only wasted resource but also contaminate environment.And waste rubber (tire) is that (28～37MJ/Kg), the calorific value that damaged tire is every kilogram is higher by 69%, higher by 10%, higher by 4% than coke than bituminous coal than timber for a kind of high heating value material.But the thermal conductivity of tire only is 0.16～0.22W/ (m ℃), is the poor conductor of heat.The present invention is according to these characteristics of junked tire, invent a kind of containing the high-efficiency desulfurization effect fixed bed vacuum cracking integrated apparatus and in the condition of load type solid body base catalyst junked tire is carried out vacuum cracking, prepare the method for gas-liquid fuels.Patent CN1760333 discloses a kind of damaged tire vacuum catalytic cracking and has produced Limonene, and the method for fuel oil and carbon black and device fail to remove the sulfur in the liquid product, can not get liquid phase sample online and condensation effect is undesirable.Patent CN1834206 discloses a kind for the treatment of process of waste and used rubber tyre, is the method for a kind of pyrolytic decomposition system, and this method power consumption is large, and product quality is not high.
Summary of the invention
Technical problem: the purpose of the method for the present invention is that provides a kind of method that contains the preparing gas-liquid fuels by scrap tire vacuum pyrolysis of high-efficiency desulfurization effect, efficiently removes the sulfur of fugitive constituent, improves condensation effect and realizes the online sampling of sample; Increase simultaneously the heat transfer efficiency between junked tire, also improve the content of high value added product in the liquid oil phase; The non-condensable gas product circulation utilizes, and removes to greatest extent acidic substance.
Technical scheme: preparation method of the present invention adopts the preparation of vacuum cracking device, specifically may further comprise the steps:
1. the pre-treatment of raw material: the junked tire starting material are cut into be of a size of 5mm * 10mm～8mm * 15mm block rubber;
2. the supported solid ferric oxide desulfurizer is filled in the desulfurizer, then desulfurizer is installed on the boss flange face;
3. through step 1. pretreated block rubber and load type solid body base catalyst join in the vacuum cracking reactor after mixing, good seal boss flange face starts vacuum pump, checks the system resistance to air loss;
4. open the 14 stopping valve, treat that the reading of vacuum meter reaches-0.098～-0.090MPa, close the 14 stopping valve, open the first stopping valve, pass into N
2, when the reading for the treatment of vacuum meter makes zero, close the first stopping valve; Again open the 14 stopping valve, the reading for the treatment of vacuum meter reaches-0.098～-0.090MPa, close the 16 stopping valve, start compression pump, open the 18 stopping valve, start small circulating pump, regulate the first variable valve on the absorption bottle, obtain suitable bubbling rate by the switch size of regulating the first variable valve, realized the circulation of non-condensable gas, can remove to greatest extent acidic substance wherein;
5. start and regulate temperature controller, the control furnace temperature rises to 400～450 ℃ of final temperatures with 10～30 ℃/min speed; By opening the second stopping valve, close the 3rd stopping valve, the 4th stopping valve, then open the 5th stopping valve, get online the liquid oil phase sample of the first collector, similarly the liquid oil phase sample of the second collector and the 3rd collector is got in operation online; Open the 19 stopping valve and get online the gas phase sample, the liquid and gas sample is sent into respectively LC and GC, the computer record data; Condensed product is collected in the first collector, the second collector, the 3rd collector, and compressed being pumped in the collection and confinement of gases tank of condensable gases do not collected.
Beneficial effect:
1, the inventive method can efficiently remove the sulfur in the fugitive constituent that the vacuum cracking junked tire produces, and utilization can directly act as a fuel;
2, the inventive method not only can increase the heat transfer efficiency between material, reduces the reaction times, but also can improve the content of high value added product in the liquid oil phase;
3, the inventive method passes into nitrogen before and after reaction, effectively reduces the oxygen content of whole reaction system, has reduced the oxygen level in the fugitive constituent, has increased the product calorific value;
4, the inventive method immerses cooling medium with three grades of coil heat exchangers, has increased contact area, has improved condensation effect, has increased the productive rate of liquid phase fuel;
5, the inventive method can be implemented in the line sampling, and the liquid and gas product is sent into respectively LC and GC, the computer record data;
6, the inventive method is used small circulating pump, absorption bottle, and the switch size of regulating the first variable valve obtains suitable bubbling rate, has realized the circulation of non-condensable gas, can remove to greatest extent acidic substance wherein.
Description of drawings
Fig. 1 is the apparatus structure synoptic diagram that the inventive method adopts,
Have among the figure: 1, the first stopping valve, 2, the boss flange face, 3, desulfurizer, 4, reactor, 5, temperature controller, 6, the second stopping valve, 7, the 3rd stopping valve, 8, the 4th stopping valve, 9, the 5th stopping valve, 10, the 6th stopping valve, 11, the 7th stopping valve, 12, the 8th stopping valve, 13, the 9th stopping valve, 14, the tenth stopping valve, 15, the 11 stopping valve, 16, the 12 stopping valve, 17, the first collector, 18, the second collector, 19, the 3rd collector, 20, the 13 stopping valve, 21, the first variable valve, 22, absorption bottle, 23, drying tower, 24, the 14 stopping valve, 25, the 15 stopping valve, 26, the 16 stopping valve, 27, vacuum pump, 28, compression pump, 29, the 17 stopping valve, 30, the collection and confinement of gases tank, 31, the 18 stopping valve, 32, small circulating pump the 4th branch road, 33, the 19 stopping valve, 34, the 20 stopping valve, 35, vacuum meter, 36, thermopair, 37, coil heat exchanger.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments:
1. raw materials pretreatment: the junked tire starting material are cut into the block rubber that is of a size of 5mm * 10mm～8mm * 15mm;
2. the supported solid ferric oxide desulfurizer is filled in the desulfurizer, then desulfurizer is installed on the boss flange face;
3. through step 1. pretreated block rubber and load type solid body base catalyst join in the vacuum cracking reactor after mixing, good seal boss flange face starts vacuum pump, checks the system resistance to air loss;
4. open the 14 stopping valve, treat that the reading of vacuum meter reaches-0.098～-0.090MPa, close the 14 stopping valve, open the first stopping valve, pass into N
2, when the reading for the treatment of vacuum meter makes zero, close the first stopping valve.Open the 14 stopping valve, the reading for the treatment of vacuum meter reaches-0.098～-0.090MPa, close the 16 stopping valve, start compression pump, open the 18 stopping valve, start small circulating pump, regulate the first variable valve on the absorption bottle, obtain suitable bubbling rate by the regulated valve switch size, realized the circulation of non-condensable gas, can remove to greatest extent acidic substance wherein;
5. start and regulate temperature controller, the control furnace temperature rises to 400～450 ℃ of final temperatures with 10～30 ℃/min speed.Condensed product is collected in the first collector, the second collector, the 3rd collector, and compressed being pumped in the collection and confinement of gases tank of condensable gases do not collected;
When 6. taking a sample online, by opening the second stopping valve, close the 3rd stopping valve, the 4th stopping valve, then open the 5th stopping valve, get online the liquid oil phase sample of the first collector.Similarly the liquid oil phase sample of the second collector and the 3rd collector is got in operation online.Open the 19 stopping valve and get online the gas phase sample, the liquid and gas product is sent into respectively LC and GC, the computer record data;
7. after question response finishes, close successively the 18 stopping valve, small circulating pump, the first variable valve, the 14 stopping valve, the 17 stopping valve and compression pump, open the 15 stopping valve and prevent pump oil suck-back, close vacuum pump.Open the first stopping valve and be filled with nitrogen, when the reading for the treatment of vacuum meter makes zero, close the first stopping valve; Open the 5th stopping valve, the 9th stopping valve, the 12 stopping valve collection liquid fuel.
Embodiment 1:
Pretreated 5mm * 10mm～8mm * 15mm junked tire and load type solid body base catalyst in 1000g: the 40g ratio joins in the vacuum cracking reactor 4 after mixing, 400g supported solid ferric oxide desulfurizer is filled in the desulfurizer 3, then desulfurizer 3 is installed on the boss flange face 2.Good seal boss flange face 2 starts vacuum pump 27, checks the system resistance to air loss.Open the 14 stopping valve 24, treat that the reading of vacuum meter 35 reaches-0.090MPa, close the 14 stopping valve 24, open the first stopping valve 1, pass into N
2, when the reading for the treatment of vacuum meter 35 makes zero, close the first stopping valve 1.Open the 14 stopping valve 24, the reading for the treatment of vacuum meter 35 reaches-0.090MPa, close the 16 stopping valve 26, start compression pump 28, open the 18 stopping valve 31, start small circulating pump 32, regulate the first variable valve 21 on the absorption bottle 22, obtain suitable bubbling rate by the regulated valve switch size.Start and adjusting temperature controller 5, the control furnace temperature rises to 400 ℃ of final temperatures with 10 ℃/min speed.Condensed product is collected in the first collector 17, the second collector 18, the 3rd collector 19, and the compressed pump 28 of condensable gases is not pressed in the collection and confinement of gases tank 30 and collects; During online sampling, by opening the second stopping valve 6, close the 3rd stopping valve 7, the 4th stopping valve 8, then open the 5th stopping valve 9, get online the liquid oil phase sample of the first collector 17.Similarly the liquid oil phase sample of the second collector 18 and the 3rd collector 19 is got in operation online.Open the 19 stopping valve 33 and get online the gas phase sample.The liquid and gas product is sent into respectively LC and GC, the computer record data.Question response is closed the 18 stopping valve 31, small circulating pump 32, the first variable valve 21, the 14 stopping valve 24, the 17 stopping valve 29 and compression pump 28 after finishing successively, opens the 15 stopping valve 25 and prevents pump oil suck-back, closes vacuum pump 20.Open the first stopping valve 1 and be filled with nitrogen, when the reading for the treatment of vacuum meter 35 makes zero, close the first stopping valve 1; Open the 5th stopping valve 9, the 9th stopping valve 13 and the 12 stopping valve 16 and collect liquid fuel.Question response still temperature is down to room temperature, collects solid phase carbon black and steel wire, the cleaning reactor.
Gas phase fuel accounts for 23.5wt%, and liquid phase fuel accounts for 46.2wt%, and the sulphur content of liquid phase fuel accounts for 0.2wt%, and the sulphur content of gas phase fuel accounts for 0.05wt%.
Embodiment 2:
Pretreated 5mm * 10mm～8mm * 15mm junked tire and load type solid body base catalyst in 1000g: the 50g ratio joins in the vacuum cracking reactor 4 after mixing, 450g supported solid ferric oxide desulfurizer is filled in the desulfurizer 3, then desulfurizer 3 is installed on the boss flange face 2.Good seal boss flange face 2 starts vacuum pump 27, checks the system resistance to air loss.Open the 14 stopping valve 24, treat that the reading of vacuum meter 35 reaches-0.094MPa, close the 14 stopping valve 24, open the first stopping valve 1, pass into N
2, when treating that vacuum meter 35 makes zero, close the first stopping valve 1.Open the 14 stopping valve 24, the reading for the treatment of vacuum meter 35 reaches-0.094MPa, close the 16 stopping valve 26, start compression pump 28, open the 18 stopping valve 31, start small circulating pump 32, regulate the first variable valve 21 on the absorption bottle 22, obtain suitable bubbling rate by the regulated valve switch size.Start and adjusting temperature controller 5, the control furnace temperature rises to 450 ℃ of final temperatures with 20 ℃/min speed.Condensed product is collected in the first collector 17, the second collector 18, the 3rd collector 19, and the compressed pump 28 of condensable gases is not pressed in the collection and confinement of gases tank 30 and collects; During online sampling, by opening the second stopping valve 6, close the 3rd stopping valve 7, the 4th stopping valve 8, then open the 5th stopping valve 9, get online the liquid oil phase sample of the first collector 17.Similarly the liquid oil phase sample of the second collector 18 and the 3rd collector 19 is got in operation online.Open the 19 stopping valve 33 and get online the gas phase sample.The liquid and gas product is sent into respectively LC and GC, the computer record data.Question response is closed the 18 stopping valve 31, small circulating pump 32, the first variable valve 21, the 14 stopping valve 24, the 17 stopping valve 29 and compression pump 28 after finishing successively, opens the 15 stopping valve 25 and prevents pump oil suck-back, closes vacuum pump 20.Open the first stopping valve 1 and be filled with nitrogen, when treating that vacuum meter 35 makes zero, close the first stopping valve 1; Open the 5th stopping valve 9, the 9th stopping valve 13, the 12 stopping valve 16 collection liquid fuels.Question response still temperature is down to room temperature, collects solid phase carbon black and steel wire, the cleaning reactor.
Gas phase fuel accounts for 24.8wt%, and liquid phase fuel accounts for 48.1wt%, and the sulphur content of liquid phase fuel accounts for 0.1wt%, and the sulphur content of gas phase fuel accounts for 0.03wt%.
Embodiment 3:
Pretreated 5mm * 10mm～8mm * 15mm junked tire and load type solid body base catalyst in 1000g: the 80g ratio joins in the vacuum cracking reactor 4 after mixing, 500g supported solid ferric oxide desulfurizer is filled in the desulfurizer 3, then desulfurizer 3 is installed on the boss flange face 2.Good seal boss flange face 2 starts vacuum pump 27, checks the system resistance to air loss.Open the 14 stopping valve 24, treat that the reading of vacuum meter 35 reaches-0.098MPa, close the 14 stopping valve 24, open the first stopping valve 1, pass into N
2, when treating that vacuum meter 35 makes zero, close the first stopping valve 1.Open the 14 stopping valve 24, the reading for the treatment of vacuum meter 35 reaches-0.098MPa, close the 16 stopping valve 26, start compression pump 28, open the 18 stopping valve 31, start small circulating pump 32, regulate the first variable valve 21 on the absorption bottle 22, obtain suitable bubbling rate by the regulated valve switch size.Start and adjusting temperature controller 5, the control furnace temperature rises to 450 ℃ of final temperatures with 30 ℃/min speed.Condensed product is collected in the first collector 17, the second collector 18, the 3rd collector 19, and the compressed pump 28 of condensable gases is not pressed in the collection and confinement of gases tank 30 and collects; During online sampling, by opening the second stopping valve 6, close the 3rd stopping valve 7, the 4th stopping valve 8, then open the 5th stopping valve 9, get online the liquid oil phase sample of the first collector 17.Similarly the liquid oil phase sample of the second collector 18 and the 3rd collector 19 is got in operation online.Open the 19 stopping valve 33 and get online the gas phase sample.The liquid and gas product is sent into respectively LC and GC, the computer record data.Question response is closed the 18 stopping valve 31, small circulating pump 32, the first variable valve 21, the 14 stopping valve 24, the 17 stopping valve 29 and compression pump 28 after finishing successively, opens the 15 stopping valve 25 and prevents pump oil suck-back, closes vacuum pump 20.Open the first stopping valve 1 and be filled with nitrogen, when the reading for the treatment of vacuum meter 35 makes zero, close the first stopping valve 1; Open the 5th stopping valve 9, the 9th stopping valve 13, the 12 stopping valve 16 collection liquid fuels.Question response still temperature is down to room temperature, collects solid phase carbon black and steel wire, the cleaning reactor.
Gas phase fuel accounts for 26.4wt%, and liquid phase fuel accounts for 52.1wt%, and the sulphur content of liquid phase fuel accounts for 0.05wt%, and the sulphur content of gas phase fuel accounts for 0.02wt%.
Claims (1)
1. the method for a preparing gas-liquid fuels by scrap tire vacuum pyrolysis, it is characterized in that the method adopts the preparation of vacuum cracking device, reactor (4), the first collector (17), the second collector (18), the 3rd collector (19), absorption bottle (22), drying tower (23), vacuum pump (27), compression pump (28), collection and confinement of gases tank (30) are linked in sequence; Be provided with boss flange face (2) above the reactor (4), be provided with the first stopping valve (1), desulfurizer (3), vacuum meter (35), thermopair (36) at boss flange face (2), temperature controller (5) is connected with thermopair (36); Coil heat exchanger (37) is connected between desulfurizer (3) and the absorption bottle (22); Output terminal at drying tower (23) is connected to the 14 stopping valve (24), be connected to respectively the 3rd stopping valve (7), the 4th stopping valve (8), the 5th stopping valve (9) on the first collector (17), the second stopping valve (6) is connected between the 3rd stopping valve (7), the 4th stopping valve (8); The output terminal of compression pump (28) is connected to respectively the 17 stopping valve (29), the 19 stopping valve (33), the output terminal of collection and confinement of gases tank (30) is connected to respectively the 18 stopping valve (31), the 20 stopping valve (34), and the 16 stopping valve (26) is connected on the pipe connecting of vacuum pump (27), compression pump (28);
Specifically may further comprise the steps:
1. the pre-treatment of raw material: the junked tire starting material are cut into be of a size of 5mm * 10mm～8mm * 15mm block rubber;
2. the supported solid ferric oxide desulfurizer is filled in the desulfurizer (3), then desulfurizer (3) is installed on the boss flange face (2);
3. through step 1. pretreated block rubber and load type solid body base catalyst join in the reactor (4) after mixing, good seal boss flange face (2) starts vacuum pump (27), checks the system resistance to air loss;
4. open the 14 stopping valve (24), the reading for the treatment of vacuum meter (35) reaches-0.098～-0.090MPa, close the 14 stopping valve (24), open the first stopping valve (1), pass into N
2, when the reading for the treatment of vacuum meter (35) makes zero, close the first stopping valve (1); Again open the 14 stopping valve (24), the reading for the treatment of vacuum meter (35) reaches-0.098～-0.090MPa, close the 16 stopping valve (26), start compression pump (28), open the 18 stopping valve (31), start small circulating pump (32), regulate the first variable valve (21) on the absorption bottle (22), obtain suitable bubbling rate by the switch size of regulating the first variable valve (21), realize the circulation of non-condensable gas, can remove to greatest extent acidic substance wherein;
5. start and regulate temperature controller (5), the control furnace temperature rises to 400～450 ℃ of final temperatures with 10～30 ℃/min speed; By opening the second stopping valve (6), close the 3rd stopping valve (7), the 4th stopping valve (8), then open the 5th stopping valve (9), get online the liquid oil phase sample of the first collector (17), similarly the liquid oil phase sample of the second collector (18) and the 3rd collector (19) is got in operation online; Open the 19 stopping valve (33) and get online the gas phase sample; The liquid and gas sample is sent into respectively LC and GC, the computer record data; Condensed product is collected in the first collector (17), the second collector (18), the 3rd collector (19), and the compressed pump of condensable gases (28) is not pressed in the collection and confinement of gases tank (30) and collects.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101832358A CN101643655B (en) | 2009-07-23 | 2009-07-23 | Method for preparing gas-liquid fuels by scrap tire vacuum pyrolysis |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101832358A CN101643655B (en) | 2009-07-23 | 2009-07-23 | Method for preparing gas-liquid fuels by scrap tire vacuum pyrolysis |
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| CN101643655A CN101643655A (en) | 2010-02-10 |
| CN101643655B true CN101643655B (en) | 2013-04-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105400539B (en) * | 2015-10-28 | 2017-05-10 | 贵州安泰再生资源科技有限公司 | Oil preparation method via waste tire degradation |
| CA3061184A1 (en) * | 2017-03-27 | 2018-10-04 | Scanship As | Microwave pyrolysis reactor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1982411A (en) * | 2006-05-22 | 2007-06-20 | 刘建有 | Method and apparatus for manufacturing fuel oil, carbon black and natural gas by waste tyre |
| CN101381612A (en) * | 2008-11-04 | 2009-03-11 | 黄术坤 | Processing technology for oil refining by scrap tire distillation |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1982411A (en) * | 2006-05-22 | 2007-06-20 | 刘建有 | Method and apparatus for manufacturing fuel oil, carbon black and natural gas by waste tyre |
| CN101381612A (en) * | 2008-11-04 | 2009-03-11 | 黄术坤 | Processing technology for oil refining by scrap tire distillation |
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