CN112938982A - Method for preparing liquid oil and silicon carbide through microwave-assisted depolymerization of rice hulls - Google Patents
Method for preparing liquid oil and silicon carbide through microwave-assisted depolymerization of rice hulls Download PDFInfo
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- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 81
- 235000009566 rice Nutrition 0.000 title claims abstract description 81
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 title claims abstract description 29
- 239000003921 oil Substances 0.000 title claims abstract description 28
- 240000007594 Oryza sativa Species 0.000 title 1
- 241000209094 Oryza Species 0.000 claims abstract description 80
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 239000010903 husk Substances 0.000 claims abstract description 29
- 239000002250 absorbent Substances 0.000 claims abstract description 28
- 230000002745 absorbent Effects 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 22
- ADKPKEZZYOUGBZ-UHFFFAOYSA-N [C].[O].[Si] Chemical compound [C].[O].[Si] ADKPKEZZYOUGBZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 238000000197 pyrolysis Methods 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 239000007787 solid Substances 0.000 claims description 19
- 230000035484 reaction time Effects 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- 229910021389 graphene Inorganic materials 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 239000006096 absorbing agent Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 7
- 239000011343 solid material Substances 0.000 abstract 4
- 229910052799 carbon Inorganic materials 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012075 bio-oil Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明公开了一种稻壳微波辅助解聚制备液体油和碳化硅的方法，将稻壳进行粉碎，将粉碎后的稻壳与微波吸收剂混合均匀，经过球磨，获得稻壳与微波吸收剂复合材料；将稻壳与微波吸收剂复合材料在氩气气氛下进行微波辅助解聚；将微波辅助解聚过程产生的热解气进行冷凝获得液体油，产生的固体物质为硅炭氧混合物；将硅炭氧混合物在氩气气氛下继续进行微波加热，得到的固体物质为碳化硅混合物；将得到的碳化硅混合物在空气气氛下进行煅烧，煅烧结束后，获得的固体物质为碳化硅。本发明通过将稻壳与强微波吸收剂混合进行微波辅助解聚，得到高价值的液体油化学品和碳化硅固体材料，为稻壳的高值化利用提供了重要技术支撑。The invention discloses a method for preparing liquid oil and silicon carbide by microwave-assisted depolymerization of rice husks. The rice husks are pulverized, the pulverized rice husks and microwave absorbents are mixed uniformly, and the rice husks and microwave absorbents are obtained by ball milling. composite material; microwave-assisted depolymerization of the rice husk and microwave absorbent composite material in an argon atmosphere; liquid oil is obtained by condensing the pyrolysis gas generated during the microwave-assisted depolymerization process, and the generated solid material is a silicon-carbon-oxygen mixture; The silicon-carbon-oxygen mixture is continuously microwave-heated under an argon atmosphere, and the obtained solid material is a silicon carbide mixture; the obtained silicon carbide mixture is calcined in an air atmosphere, and after the calcination is completed, the obtained solid material is silicon carbide. The invention obtains high-value liquid oleochemicals and silicon carbide solid materials by mixing rice husks with a strong microwave absorbent for microwave-assisted depolymerization, and provides important technical support for high-value utilization of rice husks.
Description
Technical Field
The invention belongs to the technical field of biomass energy and materials, and particularly relates to a method for preparing liquid oil and silicon carbide through microwave-assisted depolymerization of rice hulls.
Background
The rice hulls are one of the important components of biomass and are rich renewable energy sources on the earth. The rice husk is mainly from husked rice, and only China produces more than 5000 million tons of rice husk every year. At present, the rice hulls are mainly utilized by directly burning the rice hulls to supply heat, and the utilization added value is very low, so that a new way for high-value utilization of the rice hulls is urgently needed to be found.
In recent years, scholars at home and abroad have conducted a great deal of research on the pyrolysis mechanism and characteristics of rice hulls, the quality improvement of pyrolysis bio-oil and the like. The method for converting the rice hulls into the bio-oil or the chemical through the pyrolysis is one of the most potential methods for efficiently utilizing the rice hulls and is one of the current research hot directions related to the large-scale utilization of the rice hulls, but the problems of low utilization efficiency, low product conversion added value and the like still exist in the current rice hull utilization aspect due to the characteristics of high ash content and the like, and a high-valued utilization means needs to be found urgently.
Disclosure of Invention
The invention aims to provide a method for preparing liquid oil and silicon carbide by microwave-assisted depolymerization of rice hulls, which aims to overcome the technical problem that the ash content (silicon) of the rice hulls is high and cannot be effectively utilized and converted.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing liquid oil and silicon carbide by rice hull microwave-assisted depolymerization comprises the following steps:
the method comprises the following steps: crushing rice hulls, uniformly mixing the crushed rice hulls with a microwave absorbent, and performing ball milling to obtain a rice hull and microwave absorbent composite material;
step two: carrying out microwave-assisted depolymerization on the rice hull and microwave absorbent composite material in an argon atmosphere;
step three: condensing pyrolysis gas generated in the microwave-assisted depolymerization process to obtain liquid oil, wherein solid matters generated in the microwave-assisted depolymerization process are silicon-carbon-oxygen mixtures;
step four: continuously carrying out microwave heating on the silicon-carbon-oxygen mixture in an argon atmosphere to obtain a solid substance which is a silicon carbide mixture;
step five: and calcining the obtained silicon carbide mixture in an air atmosphere, and obtaining a solid substance of silicon carbide after calcining and sintering.
Further, the grain diameter of the rice hulls in the step one is 0.1-0.5 mm, and the grain diameter of the microwave absorbent is 0.05-0.2 mm.
Further, the microwave absorbent in the step one is activated carbon, carbon black or graphene, and the mass ratio of the rice hull to the microwave absorbent is 1: (0.02-0.5).
Further, the ball milling time in the step one is 2-10 min.
Further, in the second step, microwave power used for microwave-assisted depolymerization is 1500-1700W, and reaction time is 20-60 seconds.
Further, the condensation temperature in the third step is-35 ℃ to 0 ℃.
Furthermore, in the fourth step, the microwave power used for microwave heating is 1800-2000W, and the reaction time is 60-100 seconds.
Furthermore, in the fifth step, the calcining temperature is 800-1000 ℃, and the calcining time is 1-3 hours.
Compared with the prior art, the invention has the following beneficial technical effects:
the method for preparing the liquid oil and the silicon carbide by microwave-assisted depolymerization of the rice hulls provided by the invention realizes high-efficiency depolymerization of the rice hulls, enables the rice hulls to be converted into the silicon carbide to reach theoretical yield, greatly improves the utilization rate and the utilization value of the rice hulls, and has the following specific advantages:
(1) based on the technical problem that the rice hull has high ash content (silicon) and cannot be effectively utilized, the liquid oil and the silicon carbide are obtained by the microwave-assisted depolymerization technology, and the high-value utilization of the rice hull is realized.
(2) Mixing rice hull and microwave absorbent, and ball milling (using ball mill tank rotation and wheel disc rotation opposite direction to give kinetic energy to milling ball)And (6) grinding. The microwave absorbent such as the activated carbon, the carbon black and the graphene is tightly embedded in the rice husk, so that uniform and rapid heat transfer and temperature rise between the rice husk and the microwave absorbent are facilitated, and more importantly, the carbon-based microwave absorbent is tightly embedded in the rice husk, so that carbon thermal reduction reaction under microwave excitation can be promoted, and SiO in the rice husk can be reduced2Can fully contact with the carbon-based microwave absorbent, and is beneficial to SiO2By forming the intermediate product SiO and then further converting the silicon carbide, oxygen is precipitated as CO.
(3) The invention provides a microwave-assisted depolymerization process for carrying out depolymerization twice, and firstly, the rice hull and microwave absorbent composite material is subjected to microwave-assisted depolymerization under an argon atmosphere, the microwave power is 1500-1700W, and the reaction time is 20-60 seconds. The temperature of the rice hull and microwave absorbent composite material is rapidly raised to 500-800 ℃ in a short time, volatile substances in cellulose, hemicellulose and lignin in the rice hull are converted into pyrolysis steam, participated solids are converted into a silicon-carbon-oxygen mixture, and the pyrolysis steam is condensed to obtain high-value liquid oil. And secondly, under the argon atmosphere, the microwave power is 1800-2000W, the reaction time is 60-100 seconds, the temperature is raised to 1400-2000 ℃, the silicon-carbon-oxygen mixture has high dielectric loss tangent and can quickly absorb the microwave and convert the microwave into heat, and under the condition, the silicon-carbon-oxygen mixture and carbon further undergo a carbothermic reduction reaction to generate silicon carbide.
(4) According to the invention, the silicon carbide mixture is calcined in an air atmosphere, and redundant carbon elements are removed through calcination, so that the purity of silicon carbide can be obviously improved; the stability of the silicon carbide crystal structure may also be improved by calcination.
Detailed Description
The invention is further described below.
A method for preparing liquid oil and silicon carbide by rice hull microwave-assisted depolymerization comprises the following steps:
the method comprises the following steps: crushing the rice hulls, uniformly mixing the crushed rice hulls with the microwave absorbent, and performing ball milling for 2-10 min to obtain the rice hulls and microwave absorbent composite material. The grain size of the rice husk is 0.1-0.5 mm, the grain size of the microwave absorbent is 0.05-0.2 mm, the microwave absorbent is activated carbon, carbon black and graphene, and the mass ratio of the rice husk to the microwave absorbent is 1: (0.02-0.5).
Step two: and (3) carrying out microwave-assisted depolymerization on the rice hull and microwave absorbent composite material under an argon atmosphere, wherein the microwave power is 1500-1700W, and the reaction time is 20-60 seconds.
Step three: and (3) condensing pyrolysis gas generated in the microwave-assisted depolymerization process under the condensation condition of-35-0 ℃ to obtain liquid oil, wherein the generated solid matter is a silicon-carbon-oxygen mixture.
Step four: and (3) continuously carrying out microwave heating on the silicon-carbon-oxygen mixture in an argon atmosphere, wherein the microwave power is 1800-2000W, the reaction time is 60-100 seconds, and the obtained solid matter is a silicon carbide mixture.
Step five: and calcining the obtained silicon carbide mixture in a muffle furnace, wherein the calcining atmosphere is air, the calcining temperature is 800-1000 ℃, the calcining time is 1-3 hours, and after calcining, the obtained solid substance is silicon carbide.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
Crushing 10g of rice hulls to obtain the rice hulls with the particle size of 0.1-0.3 mm, uniformly mixing the crushed rice hulls with 5g of activated carbon with the particle size of 0.05-0.1 mm, and performing ball milling for 2min to obtain the rice hulls and activated carbon composite material. And (2) carrying out microwave-assisted depolymerization on the rice hull and activated carbon composite material under the argon atmosphere, wherein the microwave power is 1700W, and the reaction time is 20 seconds. And (3) condensing pyrolysis gas generated in the microwave-assisted depolymerization process at the condensation condition of-35 ℃ to obtain liquid oil, wherein the generated solid matter is a silicon-carbon-oxygen mixture. And (3) continuously carrying out microwave heating on the silicon-carbon-oxygen mixture in an argon atmosphere, wherein the microwave power is 2000W, the reaction time is 60 seconds, and the obtained solid matter is a silicon carbide mixture. And calcining the obtained silicon carbide mixture in a muffle furnace in air at 1000 ℃ for 1 hour to obtain a solid substance of silicon carbide after calcining. The yield of the obtained liquid oil was 32.1%, the yield of the obtained silicon carbide was 45.8%, and the purity of the silicon carbide was 94.1%.
Example 2
Crushing 10g of rice hulls to obtain the rice hulls with the particle size of 0.4-0.5 mm, uniformly mixing the crushed rice hulls with 0.2g of carbon black with the particle size of 0.15-0.2 mm, and performing ball milling for 10min to obtain the rice hulls and carbon black composite material. And (2) carrying out microwave-assisted depolymerization on the rice hull and carbon black composite material under an argon atmosphere, wherein the microwave power is 1500W, and the reaction time is 60 seconds. And (3) condensing pyrolysis gas generated in the microwave-assisted depolymerization process at the condensation condition of 0 ℃ to obtain liquid oil, wherein the generated solid matter is a silicon-carbon-oxygen mixture. And (3) continuously carrying out microwave heating on the silicon-carbon-oxygen mixture in an argon atmosphere, wherein the microwave power is 1800W, the reaction time is 100 seconds, and the obtained solid matter is a silicon carbide mixture. And calcining the obtained silicon carbide mixture in a muffle furnace in air at 800 ℃ for 3 hours to obtain a solid substance of silicon carbide after calcining. The yield of liquid oil obtained was 35.6%, the yield of silicon carbide obtained was 43.4%, and the purity of silicon carbide was 93.7%.
Example 3
Crushing 10g of rice hulls to obtain the rice hulls with the particle size of 0.3-0.4 mm, uniformly mixing the crushed rice hulls with 2g of graphene with the particle size of 0.1-0.15 mm, and performing ball milling for 5min to obtain the rice hulls and graphene composite material. And (2) carrying out microwave-assisted depolymerization on the rice hull and graphene composite material under an argon atmosphere, wherein the microwave power is 1600W, and the reaction time is 40 seconds. And (3) condensing pyrolysis gas generated in the microwave-assisted depolymerization process at a condensation condition of-17 ℃ to obtain liquid oil, wherein the generated solid matter is a silicon-carbon-oxygen mixture. And (3) continuously carrying out microwave heating on the silicon-carbon-oxygen mixture in an argon atmosphere, wherein the microwave power is 1900W, the reaction time is 80 seconds, and the obtained solid matter is a silicon carbide mixture. And calcining the obtained silicon carbide mixture in a muffle furnace in air at 900 ℃ for 2 hours to obtain a solid substance of silicon carbide after calcining. The yield of the obtained liquid oil was 33.5%, the yield of the obtained silicon carbide was 44.6%, and the purity of the silicon carbide was 95.2%.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (8)
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| CN202110188408.6A CN112938982A (en) | 2021-02-18 | 2021-02-18 | Method for preparing liquid oil and silicon carbide through microwave-assisted depolymerization of rice hulls |
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Cited By (1)
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| CN114709405A (en) * | 2022-04-27 | 2022-07-05 | 深圳市寒暑科技新能源有限公司 | A kind of preparation method of hard carbon composite material based on biomass |
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Application publication date: 20210611 |