CN101735844A - Method for preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way - Google Patents
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002671 adjuvant Substances 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000004215 Carbon black (E152) Substances 0.000 claims description 26
- 238000005336 cracking Methods 0.000 claims description 26
- 235000007164 Oryza sativa Nutrition 0.000 claims description 20
- 235000009566 rice Nutrition 0.000 claims description 20
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000010903 husk Substances 0.000 claims description 13
- -1 hydro carbons compounds Chemical class 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 9
- 239000005416 organic matter Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
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- 238000002360 preparation method Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 3
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- 150000004645 aluminates Chemical class 0.000 claims description 3
- 239000011425 bamboo Substances 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
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- 241000209140 Triticum Species 0.000 claims description 2
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- 150000003839 salts Chemical class 0.000 claims description 2
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- 240000007594 Oryza sativa Species 0.000 claims 3
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 229920002223 polystyrene Polymers 0.000 claims 1
- 239000010812 mixed waste Substances 0.000 abstract description 10
- 238000000197 pyrolysis Methods 0.000 abstract description 7
- 229920000642 polymer Polymers 0.000 abstract description 4
- 229910021417 amorphous silicon Inorganic materials 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000000047 product Substances 0.000 description 36
- 241000209094 Oryza Species 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 13
- 230000009466 transformation Effects 0.000 description 5
- 239000003921 oil Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
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- 239000000446 fuel Substances 0.000 description 3
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
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- 230000002153 concerted effect Effects 0.000 description 2
- 238000012962 cracking technique Methods 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 125000002015 acyclic group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000007233 catalytic pyrolysis Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 230000007246 mechanism Effects 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a method for preparing hydrocarbon compounds in a biomass self-catalysis copyrolysis way, which is realized in a way as follows: biomass and polymer waste are used as raw materials, and a catalyst adjuvant is added to prepare the hydrocarbon compounds by using a biomass self-catalysis copyrolysis technique; the pyrolysis is carried out in a normal pressure reactor; and the reaction is carried out in the reaction atmosphere of hydrogen, nitrogen or vacuum without oxygen at the pyrolysis temperature of 400-550 DEG C for 1-6 hours. In the invention, the total conversion rate of mixed waste reaches 65-81%, and the content of hydrocarbonaceous gases in the total product is 10-20%; and the hydrocarbon compounds contain 38-56% of liquid, 19-25% of oxygenic organic substances and 14-19% of residues. The hydrocarbon compound products of the invention comprise gas hydrocarbons, oily hydrocarbons, oxygenic organic substances and amorphous silicon.
Description
Technical field
The present invention relates to a kind of technology of utilizing mixed waste to prepare the hydro carbons thing, being specially with biomass and polymkeric substance waste is that raw material prepares the hydro carbons thing by autocatalysis copyrolysis technology.
Background technology
At present, Chinese big city meets with the rubbish predicament, and people also are faced with resource and shortage of energy sources problem simultaneously.In a lot of countries, solid waste mainly consist of 65% Mierocrystalline cellulose and xylogen derived material, 15% polymer materials and 20% inorganic materials.Polymkeric substance is to be raw material with natural resourcess such as oil, Sweet natural gas, coals, the high molecular polymer of synthetic, and the general character of they and biomass is all to belong to the bulk material that is rich in hydrocarbon element.China is maximum in the world paddy rice plantation country, and according to the statistics of the Ministry of Agriculture, China's rice yield was 18,059 ten thousand tons in 2005, and rice husk accounts for 20% of paddy usually, calculates like this, produces more than 3,600 ten thousand tons of rice husks, and the rice husk resource is very abundant.The main composition of rice husk is cellulose family, lignin and silicon class, rice kind and place of production difference, it forms difference to some extent, roughly consists of: robust fibre 35.5%～45% (polycondensation pentose 16%～22%), wooden rope 21%～26%, silica 1 0%～21%.
The liquid that biomass pyrolytic obtains mainly is hydro carbons and the compound fragrant hydrocarbon that contains oxygenatedchemicalss such as the higher type organic of oxygen such as phenol, cresols and C10～C16.Oxygen is higher, calorific value is lower because of containing, and problems such as stronger burn into ignition delay and storage instability that engine is produced remain certain difficulty.Also exist biological heat to separate the liquid oils that obtains simultaneously, the problems such as intermiscibility difference with traditional fuel mix hinder its widespread use.Have above-mentioned defective for overcoming the liquid that the independent pyrolysis of biomass produces, the present invention with it with copyrolysis such as other material such as polymkeric substance.Also there are problems such as paraffin productive rate height, the lightweight oil productive rate is low, the liquid oil octane value is low in the independent pyrolysis of waste of polymeric, hinders its widespread use.The pyrolysis that the copyrolysis of biomass and multipolymer mainly can be it based on biomass provides the oxygen of hydrogen source and trace, helps the fracture of C-C, c h bond.
Biomass and polymkeric substance copyrolysis have very strong synergy, and the biomass pyrolytic solid product mainly is the acyclic oligo thing that has oxygen-containing functional group, dewater lentamente in this temperature range, deoxidation and polyreaction.In reaction, played the effect that stores and provide living radical, represented that with simple formula its mechanism is: biomass → solid+free radical → free radical+polymkeric substance → chain rupture → light liquid phase product.
Early stage cleavage method is simple thermal-cracking method.But this method has obvious defects, and promptly power consumption is high, efficient is low, productive rate is not high, selectivity is not strong.Therefore people have developed catalytic thermocracking process rapidly, add catalyzer in the thermo-cracking stage, one can reduce the required activation energy of raw material cracking, cut down the consumption of energy, raise the efficiency, but also can improve product selectivity, therefore this method has remarkable advantages with respect to pyrolysis method, but owing to adopt catalyzer to improve cost, and catalyst themselves is difficult for reclaiming.
Summary of the invention
The object of the invention provides a kind of technology of utilizing mixed waste to prepare the hydro carbons thing, and being specially with biomass and polymkeric substance waste is that raw material prepares the hydro carbons thing by autocatalysis copyrolysis technology.The present invention makes full use of the silicon resource of biomass, realizes the resource circulation use, and the cost of catalyzer is low; The cracking condition gentleness belongs to the environmental friendliness technology.
The invention provides the method for preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, with biomass and polymkeric substance waste is raw material, prepare hydrocarbon compound by adding catalyst aid and biomass autocatalysis copyrolysis technology, cracking is carried out in normal pressure reactor, and concrete preparation process is as follows:
The 1st step: the mixed with polymers waste is gone foreign matter and biomass, and through pulverizing and dry, by dried biomass: polymkeric substance waste weight ratio is to mix at 10～1: 1, is 0.5～3.5% adding catalyst adjuvant of raw material weight by consumption.
The 2nd step: feed hydrogen or nitrogen, discharge the air of reactor.Be warming up at 400～550 ℃ and carry out scission reaction, the reaction times is 1～6 hour.
The 3rd step: gaseous product is collected on cracking limit, limit.Contain liquefiable gas in the hydrocarbon gas of C1～C4, handle, obtain hydro carbons liquefiable product through liquefiable gas preprocessor.The gas of not liquefiable imports the combustion chamber, for copyrolysis provides energy.
The 4th step: product liquid is collected on cracking limit, limit, and product liquid is collected through after the condenser condenses.Product liquid obtains hydrocarbon liquids product and water soluble organic substance through layering.The hydrocarbon liquids product can obtain variant production after stepwise distillation, or continues meticulous cracking and obtain the light hydrocarbons compound.Water soluble organic substance obtains different oxygen-bearing organic matters through upgrading.
The 5th step: residue obtains unformed silicon through aftertreatment.
The kind of mixed waste of the present invention: biomass comprise agricultural processing wastes such as rice husk, rice bar, bamboo class, wheat straw; The polymkeric substance waste comprises polystyrene (PS), polyethylene (PE), polypropylene (PP), damaged tire and daily waste plastic etc.
Biomass of the present invention are pulverized the back 110 ℃ of dry half an hour; The polymkeric substance waste removes foreign matter, pulverizes, 110 ℃ of dry half an hour.
The present invention utilizes the self-catalysis of the unformed silicon of biomass and the common concerted catalysis cracking technique of catalyst adjuvant.Catalyst adjuvant is a metal oxide, aluminate, an alkali metal salt and alkaline earth salt; The catalyst adjuvant consumption is 0.5～3.5% of a raw material weight; Be preferably 2.5%.
Reaction atmosphere of the present invention is hydrogen or nitrogen, vacuum anaerobic.Preferred hydrogen.
Reaction conditions of the present invention is: carry out under the normal pressure, reaction gas is hydrogen or nitrogen, vacuum anaerobic.Pyrolysis temperature is preferably 450～520 ℃ at 400～550 ℃.
In 1～6 hour reaction times of the present invention, be preferably 3～4.5 hours.
The method that the present invention prepares the hydro carbons thing can obtain: gas hydro carbons, oily hydro carbons, oxygen-bearing organic matter and unformed silicon multiple product can not liquefied gas can act as a fuel when copyrolysis and utilize.The oily hydrocarbon product can directly utilize, and also can obtain variant production after stepwise distillation, or continues meticulous cracking and obtain the light hydrocarbons compound.Water soluble organic substance obtains different oxygen-bearing organic matters through upgrading.
The transformation efficiency of the total mixed waste of the present invention reaches 65～81%, hydrocarbon-containifirst gas comprises 10～20% in the total product, hydrocarbon compound liquid 38～56%, oxygen-bearing organic matter 19～25%, residue 14～19%.
The present invention utilizes the principle of biomass self silicon oxide-containings such as rice husk.SiO in the rice husk
2Be undefined structure, and the most SiO of occurring in nature
2All be crystal form and exist, paddy rice is with unformed SiO rare in the soil
2Be enriched in the rice husk, it is a kind of of great value resource.In the rice hull ash SiO
2By adding catalyst aid, biomass self silicon oxide-containing such as rice husk plays the catalytic pyrolysis effect when the copyrolysis of biomass and polymkeric substance, and residue obtains unformed silicon again through aftertreatment in the copyrolysis process.The copyrolysis of biomass and polymkeric substance can be converted into the useful industrial chemicals and the energy to these wastes effectively, thereby realizes the resource circulation use, and has protected environment.Copyrolysis of the present invention has reduced the cost of catalyzer, and can make full use of the silicon resource of biomass.
Advantage of the present invention: (1) the present invention utilizes the self-catalysis of the unformed silicon of biomass and the common concerted catalysis cracking technique of catalyst adjuvant, and copyrolysis has reduced the cost of catalyzer, and can make full use of the silicon resource of biomass.(2) transformation efficiency of total mixed waste improves.(3) obtain gas hydro carbons, oily hydro carbons, oxygen-bearing organic matter and unformed silicon multiple product, can not liquefied gas can when copyrolysis, act as a fuel and utilize again.(4) whole process is carried out in normal pressure, the cracking condition gentleness, and no serious " three wastes " have made full use of resource, belong to the environmental friendliness technology.The present invention is subsidized by Zhejiang Province's key research project (2005C12023).
Embodiment
Embodiment 1
The 1st step: mixed waste is removed foreign matter, pulverize dryly, by dry rice husk: polymer weight ratio is to mix at 10～1: 1, is 0.5～3.5% adding catalyst adjuvant of raw material weight by consumption;
The 2nd step: feed hydrogen or nitrogen, discharge the air of reactor;
The 3rd step: be warming up at 400～550 ℃ and carry out scission reaction, the reaction times is 1～6 hour;
The 4th step: gaseous product is collected on cracking limit, limit.The hydrocarbon gas that contains C1～C4 obtains liquefiable gas through cryogenic condensation;
The 5th step: product liquid is collected on cracking limit, limit, and product liquid is collected through after the condenser condenses.Obtain the hydrocarbon liquids product through layering again;
The 6th step: will contain in the hydrocarbon gas of C1～C4 liquefiable gas and handle, and obtain hydro carbons liquefiable product through liquefiable gas preprocessor.The gas of not liquefiable imports the combustion chamber, for copyrolysis provides energy;
The 7th step: product liquid is obtained hydrocarbon liquids product and water soluble organic substance through layering.The hydrocarbon liquids product can obtain variant production after stepwise distillation, or continues meticulous cracking and obtain the light hydrocarbons compound.Water soluble organic substance obtains different oxygen-bearing organic matters through upgrading.
The 8th step: residue obtains unformed silicon through aftertreatment.
The transformation efficiency of the total mixed waste of the present invention reaches 65～81%, hydrocarbon-containifirst gas comprises 10～20% in the total product, hydrocarbon compound liquid 38～56%, oxygen-bearing organic matter 19～25%, residue 14～19%.
Embodiment 2
According to preparation process and the method for embodiment 1, cracking is carried out in normal-pressure reaction kettle.Rice husk is 110 ℃ of dry half an hour, and waste polypropylene removes foreign matter, pulverizes, and 110 ℃ of dry half an hour, respectively gets 0.125 kilogram, presses the alumina catalyzation agent aid that 2.5% of raw material weight adds metal oxide, logical H
2Emptying gas is warming up to 460 ℃, cracking 3 hours, and gaseous product is collected on cracking limit, limit, and the hydrocarbon gas that contains C1～C4 obtains liquefiable gas through cryogenic condensation; Product liquid is collected on cracking limit, limit, and product liquid is collected through after the condenser condenses, obtains the hydrocarbon liquids product through layering again; Obtain water-soluble oxygen-bearing organic matter and residue simultaneously.Residue obtains unformed silicon through aftertreatment.Product liquid is analyzed by gas chromatograph-mass spectrometer.The transformation efficiency 68% of total mixed waste, hydrocarbon gas accounts for 20% in the total product, hydrocarbon liquids 50%, oxygen-bearing organic matter 12%, residue 16%.The hydrocarbon liquids product can directly utilize, and also can continue meticulous cracking after distilling and obtain light hydrocarbon.
Embodiment 3
According to preparation process and the method for embodiment 1, cracking is carried out in normal-pressure reaction kettle.The bamboo powder is 110 ℃ of dry half an hour, and plastic waste: waste polyethylene (removing foreign matter) weight ratio is 1: 1, pulverizes, and 110 ℃ of dry half an hour, presses 3% of raw material weight and adds the aluminate catalyst auxiliary agent, is warming up to 500 ℃, cracking 4 hours.Gaseous product is collected on cracking limit, limit, and the hydrocarbon gas that contains C1～C4 obtains liquefiable gas through cryogenic condensation; Product liquid is collected on cracking limit, limit, and product liquid is collected through after the condenser condenses, obtains the hydrocarbon liquids product through layering again; Obtain water-soluble oxygen-bearing organic matter and residue simultaneously.Residue obtains unformed silicon through aftertreatment.Product liquid is analyzed by gas chromatograph-mass spectrometer.The transformation efficiency 72% of total mixed waste, hydrocarbon gas accounts for 18% in the total product, hydrocarbon liquids 52%, oxygen-bearing organic matter 10%, residue 17%.The hydrocarbon liquids product can directly utilize, and also can continue meticulous cracking after distilling and obtain light hydrocarbon.
Claims (7)
1. the method for a preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, with biomass and polymkeric substance waste is raw material, prepare the hydro carbons compounds by adding catalyst adjuvant and biomass autocatalysis copyrolysis technology, cracking is carried out in normal pressure reactor, and preparation process is as follows:
(1), biomass and polymkeric substance waste are removed foreign matter, pulverize back, dry, by dried biomass: polymkeric substance waste weight ratio is to mix at 10～1: 1, is 0.5～3.5% adding catalyst adjuvant of raw material weight by consumption, is added in the normal pressure reactor;
(2), in normal pressure reactor, feed hydrogen or nitrogen, the air of discharge reactor; Be warming up at 400～550 ℃ and carry out scission reaction, the reaction times is 1～6 hour;
(3), cracking limit, limit collects gaseous product, contains liquefiable gas in the hydrocarbon gas of C1～C4, handles through liquefiable gas preprocessor, obtains hydro carbons liquefiable product; The gas of not liquefiable imports the combustion chamber, and the scission reaction energy is provided;
(4), cracking limit, limit collects product liquid, product liquid is collected through after the condenser condenses, product liquid obtains hydrocarbon liquids product and water soluble organic substance through layering; The hydrocarbon liquids product obtains variant production after stepwise distillation; Or continue meticulous cracking, obtain the light hydrocarbons compound; Water soluble organic substance obtains different oxygen-bearing organic matters through upgrading.
(5), residue obtains unformed silicon through aftertreatment.
2. according to the method for claim 1 preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, it is characterized in that the polymkeric substance waste comprises: waste plastic, polystyrene, polypropylene, polyethylene, damaged tire.
3. according to the method for claim 1 preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, it is characterized in that biomass comprise: the rice husk of agricultural processing waste, rice bar, bamboo class, wheat straw.
4. according to the method for claim 3 preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, it is characterized in that biomass are rice husk.
5. according to the method for claim 1 preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, it is characterized in that catalyst adjuvant comprises: metal oxide, aluminate, an alkali metal salt, alkaline earth salt.
6. according to the method for claim 1 preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, it is characterized in that biomass pulverizing back is 110 ℃ of dry half an hour; The polymkeric substance waste removes foreign matter, pulverizes, 110 ℃ of dry half an hour.
7. according to the method for claim 1 preparing hydrocarbon compounds in biomass self-catalysis copyrolysis way, it is characterized in that the product that obtains the hydro carbons thing comprises: gas hydro carbons, oily hydro carbons, oxygen-bearing organic matter and unformed silicon.
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| CN103080274A (en) * | 2010-07-26 | 2013-05-01 | 埃米尔·A·J·维泽尔-林哈特 | System and method for producing fuels from biomass/plastic mixtures |
| JP2013170224A (en) * | 2012-02-21 | 2013-09-02 | Nihon Univ | Method for producing petroleum alternative liquid fuel |
| CN103316647A (en) * | 2013-07-04 | 2013-09-25 | 东南大学 | Method for preparing supported solid-base catalyst and bio-oil |
| CN103695021A (en) * | 2014-01-03 | 2014-04-02 | 北京林业大学 | Method for preparing pyrolytic oil by co-heated pyrolysis and liquefaction of biomass and waste tire |
| CN104046374A (en) * | 2014-06-12 | 2014-09-17 | 江苏大学 | Device and method for quickly preparing bio-oil by catalytically cracking biomass pyrolysis vapor on line |
| CN104178188A (en) * | 2014-08-08 | 2014-12-03 | 南京理工大学 | Method for reducing pyrolysis activation energy of rice hulls |
| CN105419839A (en) * | 2015-11-03 | 2016-03-23 | 交通运输部公路科学研究所 | Modified biological asphalt and preparation method therefor |
| CN105745311A (en) * | 2013-09-11 | 2016-07-06 | 研究三角协会 | Reactive catalytic fast pyrolysis process and system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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