CN115446078B - Treatment method for microwave pyrolysis of waste camphor tree branches and leaves - Google Patents
Treatment method for microwave pyrolysis of waste camphor tree branches and leaves Download PDFInfo
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- 241000723346 Cinnamomum camphora Species 0.000 title claims abstract description 104
- 238000000197 pyrolysis Methods 0.000 title claims abstract description 72
- 239000002699 waste material Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 65
- 238000005336 cracking Methods 0.000 claims abstract description 59
- 239000007787 solid Substances 0.000 claims abstract description 35
- 239000012263 liquid product Substances 0.000 claims abstract description 33
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims abstract description 30
- 239000000779 smoke Substances 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 4
- 239000012634 fragment Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 29
- 238000001179 sorption measurement Methods 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 238000001994 activation Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000446 fuel Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 229960000411 camphor oil Drugs 0.000 claims description 9
- 239000010624 camphor oil Substances 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000005188 flotation Methods 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000711 cancerogenic effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 231100000315 carcinogenic Toxicity 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 83
- 230000008569 process Effects 0.000 description 27
- 239000010813 municipal solid waste Substances 0.000 description 13
- 230000000391 smoking effect Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 238000012216 screening Methods 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 235000013305 food Nutrition 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000004227 thermal cracking Methods 0.000 description 5
- 229960000846 camphor Drugs 0.000 description 4
- 229930008380 camphor Natural products 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 239000002023 wood Substances 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 244000082946 Tarchonanthus camphoratus Species 0.000 description 3
- 235000005701 Tarchonanthus camphoratus Nutrition 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 235000013622 meat product Nutrition 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- -1 sawdust Substances 0.000 description 3
- 238000001256 steam distillation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000020994 smoked meat Nutrition 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 241000723347 Cinnamomum Species 0.000 description 1
- 241001483108 Cinnamomum longipaniculatum Species 0.000 description 1
- 235000019542 Cured Meats Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000218195 Lauraceae Species 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
- B09B3/35—Shredding, crushing or cutting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/50—Destroying solid waste or transforming solid waste into something useful or harmless involving radiation, e.g. electro-magnetic waves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
-
- 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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a treatment method for microwave pyrolysis of waste camphor tree branches and leaves, which comprises the following steps: s1, crushing the waste Cinnamomum camphora branches and leaves to obtain Cinnamomum camphora branch and leaf fragments; s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps to obtain pyrolysis solids and pyrolysis gas; condensing the cracking gas to obtain a crude product of the liquid smoke, and preparing the cracking solid into the activated carbon. In the step S2, the pyrolysis gas is condensed to obtain a gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigating liquid product and separated gas. The method for treating the camphor tree branches and leaves has the characteristics of high speed, high efficiency, low energy consumption, low cost and the like, and the prepared active carbon product has the advantages of low ash content and high adsorptivity, and the prepared smoke liquid product has the advantages of high phenol content and no cancerogenic substances such as tar. The effect of reducing the influence of waste camphor tree branches and leaves on the environment and improving the utilization rate of the camphor tree branches and leaves is achieved.
Description
Technical Field
The invention belongs to the technical field of utilization of Cinnamomum camphora, and particularly relates to a treatment method for microwave pyrolysis of branches and leaves of waste Cinnamomum camphora.
Background
Cinnamomum camphora (academic: cinnamomum longipaniculatum (Gamble) N.Chaoex H.W.Li) is a evergreen arbor of Cinnamomum genus of Lauraceae family, and Cinnamomum camphora has the characteristics of rapid growth, strong sprout tillering, more leaf carrying, less disease and insect, beautiful tree shape, male-like posture, flexible wood, compact texture, and long service life reaching thousands of years, and is the preferred tree species for sheeting forestation and four-side greening.
The camphor oil is prepared by a steam distillation method, and can be further separated into camphor and camphor oil which are important chemical raw materials and are increasingly used in domestic and foreign markets.
The Cinnamomum camphora is distributed in Sichuan Yibin of China, and is also called as "Cinnamomum camphora kingdom", and 45 ten thousand mu of Cinnamomum camphora forests are produced in one year, namely 6000 tons of Cinnamomum camphora oil. 35 ten thousand tons of oil-distilled waste camphor branches and leaves are produced each year. At present, the comprehensive utilization of the branches and leaves of the camphor trees is less, and after the camphor oil is processed and prepared by the existing steam distillation method, leaf residues and residues in the process are generally discarded as waste or directly burnt, so that on one hand, environmental protection burden is caused, on the other hand, resources are wasted, and the method is not in accordance with the current energy-saving and environment-friendly policy.
The traditional smoking mainly utilizes the mixture of gas and particulate solid generated by smoldering wood, sawdust, charcoal and other plant materials to smoke the meat product, so that a part of moisture of the meat product is lost, and meanwhile, the smoke is absorbed, so that the meat product has corresponding smoking flavor and smoking color. While foods acquire a smoky flavor, some other desirable properties are available, such as: removing the smell of mutton or other abnormal flavors; forming a layer of film on the surface of the food to prevent water and grease from overflowing; sterilizing and resisting oxidation, and prolonging storage period; the meat has attractive color and luster and the like. However, the conventional smoking technology has some unavoidable disadvantages, such as giving products with excessive polycyclic aromatic hydrocarbon, which is a fat-soluble compound, and can enter human body through respiration, skin contact and food contact, thus having carcinogenic effect, and the smoking process also pollutes the air. In addition, researches have shown that the surface of smoked meat products also contains a large amount of formaldehyde, which is mainly because methanol is generated by dry distillation of wood in an anoxic state in the smoking process, and the methanol is further oxidized into formaldehyde which is adsorbed and accumulated on the surface of the products, and the smoked meat products have an antibacterial effect but also have a great toxic effect. In addition, the wood can generate tar particles, dust and other impurities which are attached to the surface of food to pollute the surface of the food in the smoking process, and the factors such as different areas, raw materials, auxiliary materials and the like can also cause a series of problems such as unstable flavor of the cured meat product. Therefore, the traditional smoking method has safety and sanitation problems, and along with the improvement of health consciousness of people, higher requirements are also put on food safety, and a safe and sanitary method is urgently needed to generate smoking color.
Currently, little research is done on the comprehensive utilization of the branches and leaves of Cinnamomum camphora. The Chinese patent No. 201410608098.9 discloses a method for comprehensively utilizing Cinnamomum camphora leaves: extracting volatile oil from Cinnamomum camphora leaves by steam distillation, extracting total flavone from the residue by alcohol extraction, extracting total polysaccharide from the residue by water extraction and alcohol precipitation, and using the residue as biofertilizer raw material. The Chinese patent No. 201210004494.1 discloses a garbage microwave pyrolysis treatment method, which comprises the following treatment processes: (1) Pretreating garbage to obtain structured garbage suitable for microwave pyrolysis; (2) microwave pyrolysis of garbage; and (3) recycling the cracked product.
However, a treatment method for performing microwave pyrolysis on the branches and leaves of the waste camphor trees to prepare the smoke liquid and the activated carbon so as to reduce the influence of the smoke liquid and the activated carbon on the environment, improve the utilization rate of the branches and leaves of the camphor trees and realize the recycling of wastes has not been reported yet.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a treatment method for microwave pyrolysis of waste camphor tree branches and leaves, which is used for preparing smoke liquid and active carbon so as to reduce the influence of the waste camphor tree branches and leaves on the environment, improve the utilization rate of the camphor tree branches and leaves and realize the effect of recycling waste.
The aim of the invention is realized by the following technical scheme:
a treatment method for microwave pyrolysis of waste camphor tree branches and leaves comprises the following steps:
s1, crushing the waste Cinnamomum camphora branches and leaves to obtain Cinnamomum camphora branch and leaf fragments;
s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps to obtain pyrolysis gas and pyrolysis solid, condensing the pyrolysis gas to obtain a crude fumigated liquid product, and carrying out smashing, flotation, acid washing and activation processes on the pyrolysis solid to prepare active carbon;
wherein the cracking temperature is 250-650 ℃, further, the cracking temperature is preferably 420-500 ℃, the cracking time is 20-40 minutes, further, the cracking time is preferably 30 minutes.
In the step S2, the pyrolysis gas is condensed to obtain a gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigating liquid product and separated gas.
Further, in step S1, the waste camphor tree branches and leaves are camphor tree branches and leaves after camphor oil extraction or branch and leaf waste of trimmed camphor tree.
Further, in step S1, the waste camphor branches and leaves are washed and dried before being crushed.
Further, the moisture content of the dried waste camphor tree branches and leaves is less than or equal to 7.0 percent.
Further, in the step S1, the granularity of the camphor tree branch and leaf scraps is 10-18 meshes.
In step S2, the temperature of the crude liquid smoke after condensation is 10 ℃ or lower, and preferably 5 to 8 ℃.
Furthermore, the separated gas is combustible gas after drying and dust removal, and can be used as fuel for drying the waste camphor tree branches and leaves.
Further, in step S2, the crude product of the liquid smoke is allowed to stand, the supernatant is taken, and the liquid smoke is obtained through adsorption by activated carbon, filtration and refining, and the standing time is preferably 24 hours.
The invention relates to a method for preparing active carbon by crushing, floatation, acid washing and activation processes of active carbon, which refers to a method for preparing active carbon by microwave pyrolysis of solid residues of municipal solid waste in the document CN 102275913A.
The beneficial effects of the invention are as follows:
1. according to the invention, waste camphor tree branches and leaves are subjected to microwave pyrolysis to prepare the smoke liquid and the activated carbon, so that the harm to the environment is reduced, the utilization rate of the camphor tree branches and leaves is improved, and the recycling of waste is realized;
2. 88.6g of active carbon can be prepared from every 200g of waste camphor branches and leaves, and more than 940mg of iodine can be adsorbed per gram of the prepared active carbon, so that the adsorption is good, and the active carbon can be used for refining smoked liquid;
3. according to the invention, 69.4g of high-quality smoked liquid can be prepared from every 200g of waste camphor tree branches and leaves, the total phenol content of the prepared smoked liquid is more than or equal to 16.32mg/mL, the carboxyl compound content is more than or equal to 15.56g/100mL, and compared with the commercially available smoked liquid, the smoked liquid has the advantages of high phenol content and no cancerogenic substances such as tar, and can better meet the requirements of a smoking process.
Drawings
FIG. 1 is a diagram of a microwave pyrolysis system according to the present invention;
in the figure, a 1-cracking furnace; 2-a microwave generator; a 3-condenser; 4-a feeding bin; 5-a vapor-liquid separator; 6-a storage tank; 7-scraping plates; 8-a solids storage tank; 9-screw conveyor; a-a cooling medium inlet; b-a cooling medium outlet; c-a gas outlet; d-shielding gas inlet.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to the accompanying drawings, but the scope of the present invention is not limited to the following description.
According to the invention, a cracking furnace 1 is transversely arranged, a screw conveyor 9 is positioned in the cracking furnace 1, a feeding bin 4 is positioned at the upper part of the cracking furnace 1 and is close to the front end of the screw conveyor 9, a solid storage tank is positioned at the lower part of the cracking furnace 1 and is close to the tail end of the screw conveyor 9, a microwave generator 2 and a scraping plate 7 are arranged at the upper side of the cracking furnace, and the microwave generator 2 and the scraping plate 7 are opposite to the screw conveyor 9. The upper side of the cracking furnace 1 is provided with a cracking gas outlet, the cracking gas outlet is connected with a condenser 3, the condenser 3 is communicated with a storage tank 6 and a gas-liquid separator 5, and a liquid outlet of the gas-liquid separator is also connected with the storage tank 6.
The invention relates to a microwave pyrolysis method for waste camphor tree branches and leaves, which comprises the following steps:
before cracking, nitrogen is introduced into the cracking furnace 1 through the protective gas inlet d for replacement, and after 5 minutes, the introduction is stopped. The pretreated camphor tree branch and leaf scraps are continuously fed into a cracking furnace through a feed inlet 4 and fall on a screw conveyor 9 positioned in the cracking furnace, the screw conveyor conveys the camphor tree branch and leaf scraps from right to left, a microwave generator 2 generates microwaves with the frequency of 2450+/-50 MHz in the conveying process, the microwaves are heated and cracked, and meanwhile, a scraping plate 7 is continuously stirred to fully irradiate the camphor tree branch and leaf scraps and facilitate the overflow of cracking gas;
after the pyrolysis is completed, the solid product enters a solid storage tank 8, and the gas product is simultaneously introduced into a condenser 3 for condensation as own shielding gas. After condensation, the condensate enters a storage tank 6, the uncondensed gas enters a gas-liquid separator 5 for gas-liquid separation, the separated liquid enters the storage tank 6, and the separated gas is led out through a gas outlet c.
The cracking process can be used for continuous feeding and continuous discharging, has high production efficiency, does not decompose violently in the cracking treatment process, and is stable in gas production, and suitable for large-scale treatment of the camphorwood branches and leaves.
The outer cylinder of the microwave cracking furnace is made of metal material and can be operated under vacuum and positive pressure operation conditions. Except the feed inlet, the cracking gas outlet and the solid product discharge outlet, other parts are subjected to sealing treatment, so that accidents such as combustion and explosion are prevented from occurring when oxygen enters the reactor. The pyrolysis gas is used as the protective gas in the pyrolysis process, so that the concentration of combustible gas in the pyrolysis gas is improved, the pyrolysis gas is recovered, purified and recycled, and the microwave treatment process is simplified.
Specific examples of the invention are as follows
Example 1
A processing method of microwave pyrolysis of camphorwood branches and leaves after camphor oil extraction comprises the following steps:
s1, cleaning and drying branches and leaves of the Cinnamomum camphora subjected to extraction of 200 g+/-5 g camphor oil until the moisture content is less than or equal to 7.0%, and then crushing the branches and leaves of the Cinnamomum camphora until the granularity is 10-18 meshes to obtain chips of the branches and leaves of the Cinnamomum camphora;
s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps, wherein the pyrolysis temperature is 350 ℃, and the pyrolysis time is 20 minutes, so as to obtain pyrolysis solids and pyrolysis gas;
condensing the cracking gas to obtain crude smoke liquid at 5 deg.c.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking solid residues of municipal solid waste) to obtain the product activated carbon.
And condensing the pyrolysis gas to obtain gas-liquid mixed gas, and performing gas-liquid separation on the gas-liquid mixed gas to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 24 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Example 2
A treatment method for microwave pyrolysis of branch and leaf wastes of trimmed camphor trees comprises the following steps:
s1, cleaning 200 g+/-5 g of branch and leaf waste of a trimmed camphor tree, drying until the moisture content is less than or equal to 7.0%, and then crushing the branch and leaf waste to 10-18 meshes to obtain camphor tree branch and leaf scraps;
s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps, wherein the pyrolysis temperature is 435 ℃, and the pyrolysis time is 25 minutes, so as to obtain pyrolysis solids and pyrolysis gas;
condensing the cracking gas to obtain crude smoke liquid at 8 ℃.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking solid residues of municipal solid waste) to obtain the product activated carbon.
And condensing the pyrolysis gas to obtain gas-liquid mixed gas, and performing gas-liquid separation on the gas-liquid mixed gas to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 28 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Example 3
A treatment method for microwave pyrolysis of branch and leaf wastes of trimmed camphor trees comprises the following steps:
s1, cleaning 200 g+/-5 g of branch and leaf waste of a trimmed camphor tree, drying until the moisture content is less than or equal to 7.0%, and then crushing the branch and leaf waste to 10-18 meshes to obtain camphor tree branch and leaf scraps;
s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps, wherein the pyrolysis temperature is 520 ℃, and the irradiation time is 40 minutes to obtain pyrolysis solids and pyrolysis gas;
condensing the cracking gas to obtain crude smoke liquid at 8 ℃.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking of solid residues of municipal solid waste) to obtain the product of the activated carbon.
And the pyrolysis gas is condensed to obtain gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 48 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Example 4
A treatment method for microwave pyrolysis of branch and leaf wastes of trimmed camphor trees comprises the following steps:
s1, cleaning 200 g+/-5 g of branch and leaf waste of a trimmed camphor tree, drying until the moisture content is less than or equal to 7.0%, and then crushing the branch and leaf waste to 10-18 meshes to obtain camphor tree branch and leaf scraps;
s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps, wherein the pyrolysis temperature is 650 ℃, and the irradiation time is 35 minutes, so as to obtain pyrolysis solids and pyrolysis gas;
condensing the cracking gas to obtain crude fumigating liquid at 2 ℃.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking of solid residues of municipal solid waste) to obtain the product of the activated carbon.
And the pyrolysis gas is condensed to obtain gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 36 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Comparative example 1
A thermal cracking treatment method of camphorwood branches and leaves after camphor oil extraction comprises the following steps:
s1, cleaning and drying branches and leaves of the Cinnamomum camphora subjected to extraction of 200 g+/-5 g camphor oil until the moisture content is less than or equal to 7.0%, and then crushing the branches and leaves of the Cinnamomum camphora until the granularity is 10-18 meshes to obtain chips of the branches and leaves of the Cinnamomum camphora;
s2, heating the camphor tree branch and leaf scraps to 350 ℃ by adopting an electric furnace for cracking, wherein the cracking time is 20 minutes, and cracked solids and cracked gas are obtained;
condensing the cracking gas to obtain crude smoke liquid at 5 deg.c.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking solid residues of municipal solid waste) to obtain the product activated carbon.
And the pyrolysis gas is condensed to obtain gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 24 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Comparative example 2
A thermal cracking treatment method for branch and leaf wastes of trimmed camphor tree comprises the following steps:
s1, cleaning 200 g+/-5 g of branch and leaf waste of a trimmed camphor tree, drying until the moisture content is less than or equal to 7.0%, and then crushing the branch and leaf waste to 10-18 meshes to obtain camphor tree branch and leaf scraps;
s2, heating the camphor tree branch and leaf scraps to 435 ℃ by adopting an electric furnace for cracking for 25 minutes to obtain cracking solids and cracking gas;
condensing the cracking gas to obtain crude smoke liquid at 8 ℃.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking solid residues of municipal solid waste) to obtain the product activated carbon.
And the pyrolysis gas is condensed to obtain gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 28 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Comparative example 3
A thermal cracking treatment method for branch and leaf wastes of trimmed camphor tree comprises the following steps:
s1, cleaning 200 g+/-5 g of branch and leaf waste of a trimmed camphor tree, drying until the moisture content is less than or equal to 7.0%, and then crushing the branch and leaf waste to 10-18 meshes to obtain camphor tree branch and leaf scraps;
s2, heating the camphor tree branch and leaf scraps to 520 ℃ by adopting an electric furnace for cracking, wherein the cracking time is 40 minutes, and cracked solids and cracked gas are obtained;
condensing the cracking gas to obtain crude smoke liquid at 8 ℃.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking of solid residues of municipal solid waste) to obtain the product of the activated carbon.
And the pyrolysis gas is condensed to obtain gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 48 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
Comparative example 4
A thermal cracking treatment method for branch and leaf wastes of trimmed camphor tree comprises the following steps:
s1, cleaning 200 g+/-5 g of branch and leaf waste of a trimmed camphor tree, drying until the moisture content is less than or equal to 7.0%, and then crushing the branch and leaf waste to 10-18 meshes to obtain camphor tree branch and leaf scraps;
s2, heating the camphor tree branch and leaf scraps to 650 ℃ by adopting an electric furnace for cracking, wherein the cracking time is 35 minutes, and cracked solids and cracked gas are obtained;
condensing the cracking gas to obtain crude fumigating liquid at 2 ℃.
The cracking solid is subjected to multistage screening, floatation, acid washing and steam activation processes (the process described in the process reference CN102275913A for preparing the activated carbon by microwave cracking of solid residues of municipal solid waste) to obtain the product of the activated carbon.
And the pyrolysis gas is condensed to obtain gas-liquid mixed gas, and the gas-liquid mixed gas is subjected to gas-liquid separation to obtain a crude fumigated liquid product and separated gas.
And drying and dedusting the separated gas to be used as fuel for drying the waste camphor tree branches and leaves.
Standing the crude fumigating liquid product for 36 hours, taking supernatant, adding activated carbon (7%wt) for adsorption, and filtering to obtain the fumigating liquid product.
The experimental results are shown in tables 1 and 2:
TABLE 1 results of liquid smoke products prepared by various groups of experiments
TABLE 2 results of activated carbon products prepared in various groups of experiments
| Group of | Yield (g) | Iodine value (mg/g) | Ash content (%) |
| Example 1 | 81.2 | 952 | 3.1 |
| Example 2 | 88.6 | 1103 | 4.3 |
| Example 3 | 87.4 | 1089 | 4.9 |
| Example 4 | 84.5 | 1056 | 5.2 |
| Comparative example 1 | 41.2 | 940 | 3.2 |
| Comparative example 2 | 48.9 | 983 | 4.9 |
| Comparative example 3 | 50.2 | 1032 | 5.1 |
| Comparative example 4 | 51.3 | 1029 | 5.5 |
Comparing the embodiments 1, 2, 3 and 4 of the invention with the comparative examples 1, 2, 3 and 4, compared with the traditional electric furnace heating mode, the scheme of the invention for carrying out microwave pyrolysis on the waste camphor tree branches and leaves can increase the smoke liquid product yield by 78.2 percent (formula (65.6-36.8)/36.8 x 100 percent) to the maximum, and increase the active carbon product yield by 81.2 percent (formula (886.4-489.3)/489.3 x 100 percent) to the maximum, which proves that the scheme of the invention greatly improves the utilization rate of the waste camphor tree branches and leaves. And the smoke liquid product prepared in the embodiment 2 of the invention has higher carboxyl compound content and total phenol content than the comparison examples; the iodine value of the activated carbon product prepared in the example 2 is 1103mg/g, which is higher than that of each example, the ash content is 4.3%, and the adsorption is good, which indicates that the prepared smoke liquid product and the activated carbon product have more excellent performance compared with the traditional thermal cracking mode.
The foregoing is merely a preferred embodiment of the invention, and it is to be understood that the invention is not limited to the form disclosed herein but is not to be construed as excluding other embodiments, but is capable of numerous other combinations, modifications and environments and is capable of modifications within the scope of the inventive concept, either as taught or as a matter of routine skill or knowledge in the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (8)
1. The treatment method for microwave pyrolysis of the waste camphor tree branches and leaves is characterized by comprising the following steps of: s1, crushing the waste Cinnamomum camphora branches and leaves to obtain Cinnamomum camphora branch and leaf fragments;
s2, carrying out microwave pyrolysis on the camphor tree branch and leaf scraps to obtain pyrolysis gas and pyrolysis solid, condensing the pyrolysis gas to obtain a crude fumigated liquid product, and carrying out smashing, flotation, acid washing and activation processes on the pyrolysis solid to prepare active carbon;
wherein the cracking temperature is 350-650 ℃, and the cracking time is 20-40 minutes;
and S2, standing the crude product of the liquid smoke, taking supernatant, and carrying out adsorption, filtration and refining by using active carbon to obtain the product of the liquid smoke.
2. The method for treating waste camphor tree branches and leaves by microwave pyrolysis according to claim 1, wherein in the step S2, a gas-liquid mixture is obtained after the pyrolysis gas is condensed, and the gas-liquid mixture is subjected to gas-liquid separation to obtain a crude fumigated liquid product and a separated gas.
3. The method according to claim 1 or 2, wherein in step S1, the waste camphor tree branches and leaves are camphor tree branches and leaves after camphor oil extraction or branch and leaf waste of trimmed camphor tree.
4. The method according to claim 1 or 2, wherein in step S1, the waste camphor tree branches and leaves are washed and dried before being crushed.
5. The method for treating waste camphor tree branches and leaves by microwave pyrolysis according to claim 4, wherein the moisture content of the waste camphor tree branches and leaves after drying is less than or equal to 7.0%.
6. The method for treating waste camphor tree branches and leaves by microwave pyrolysis according to claim 1 or 2, wherein in the step S1, the granularity of the camphor tree branches and leaves scraps is 10-18 meshes.
7. The method according to claim 2, wherein in step S2, the temperature of the condensed crude product of the liquid smoke is 10 ℃ or lower.
8. The method for treating the waste camphor tree branches and leaves by microwave pyrolysis according to claim 2, wherein the separated gas is used as fuel for drying the waste camphor tree branches and leaves after drying and dust removal.
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