CN113773496A - Production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber - Google Patents
Production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber Download PDFInfo
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- CN113773496A CN113773496A CN202110933435.1A CN202110933435A CN113773496A CN 113773496 A CN113773496 A CN 113773496A CN 202110933435 A CN202110933435 A CN 202110933435A CN 113773496 A CN113773496 A CN 113773496A
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- silicon dioxide
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000002699 waste material Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 20
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 18
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 18
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 16
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000012071 phase Substances 0.000 claims abstract description 19
- 239000000741 silica gel Substances 0.000 claims abstract description 17
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- 238000002485 combustion reaction Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 239000012265 solid product Substances 0.000 claims abstract description 6
- 102000008186 Collagen Human genes 0.000 claims abstract description 5
- 108010035532 Collagen Proteins 0.000 claims abstract description 5
- 229920001436 collagen Polymers 0.000 claims abstract description 5
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 5
- 238000005191 phase separation Methods 0.000 claims abstract description 4
- 239000013589 supplement Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- 238000004132 cross linking Methods 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 38
- 230000008569 process Effects 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 21
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 230000008707 rearrangement Effects 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims 8
- 238000010092 rubber production Methods 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 abstract 1
- 238000004523 catalytic cracking Methods 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0825—Preparations of compounds not comprising Si-Si or Si-cyano linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Silicon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber, which belongs to the technical field of micro-negative pressure, continuous and harmless treatment of organic silicone rubber production, wherein waste silicone collagen materials are recycled and then sorted; crushing the sorted waste silica gel into uniform particles; conveying the silica gel particles into rotary thermal decomposition moving bed equipment after metering, and heating to a certain temperature for decomposition under the conditions of micro-negative pressure, continuous closed loop and indirect heating so as to break the cross-linking state of the silicon rubber polymer; the decomposed main solid phase products are silicon dioxide powder and gas phase products, and the gas phase products are separated out of the moving bed equipment through two-phase separation output equipment; namely, the solid product silicon dioxide powder is continuously output and collected through a material sealing conveying device; collecting the gas-phase product as a methyl cyclosiloxane mixed ring body through a condensation and washing separation system; the non-condensable gas is conveyed to a gas combustion chamber system through a full-wind fan to be fully incinerated and harmlessly treated, and energy supplement is provided for equipment.
Description
Technical Field
The invention relates to the technical field of micro-negative pressure, continuous and harmless treatment of organic silicon rubber production, in particular to a production process for producing dimethyl silicone oil and silicon dioxide by using waste silicon rubber.
Background
The existing waste silica gel treatment methods include a physical crushing method, a catalytic cracking method (including an acid catalytic cracking method and an alkali catalytic cracking method), a batch high-temperature cracking method and the like. The physical crushing method has high requirements on raw materials and can only be suitable for treating waste silica gel of few types. The use of a large amount of acid and alkali in the catalytic cracking method can cause environmental pollution and poor production working condition, and the residue generated after cracking is difficult to treat and has high cost. The intermittent high-temperature cracking method has high energy consumption, low production efficiency, unfriendly environment during production, uncontrollable product quality and difficult effective treatment and utilization of the generated waste.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention provides a production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber, and realizes micro-negative pressure, continuous and harmless treatment of waste silicone rubber on the premise of ensuring safety and product quality, and the treated waste residue is directly produced into a silicon dioxide product to be used as a filler.
In order to achieve the purpose, the invention adopts the following technical scheme: the operation steps are as follows:
step one, sorting the waste silicon collagen material after recovery;
step two, crushing the sorted waste silica gel into uniform particles;
conveying the metered silica gel particles into rotary thermal decomposition moving bed equipment, and heating to a certain temperature for decomposition under the conditions of micro-negative pressure, continuous closed loop and indirect heating to break the cross-linking state of the silicone rubber polymer;
step four, decomposing main solid phase products into silicon dioxide powder and gas phase products, and separating the solid phase products and the gas phase products out of the moving bed equipment through two-phase separation output equipment; namely, the solid product silicon dioxide powder is continuously output and collected through a material sealing conveying device; collecting the gas-phase product as a methyl cyclosiloxane mixed ring body (DMC) through a condensation and washing separation system; and conveying the non-condensable gas in the gas-phase product to a gas combustion chamber system through a full-wind fan to fully burn and perform harmless treatment and provide energy supplement for equipment.
Preferably, the components of the gas phase product are siloxane-based gases such as D3, D4, D5, D6, D7 and D8.
Preferably, the uniform particles in step two have a particle size of less than 10 mm.
Preferably, the uniform particles in the second step are conveyed to a storage tank of a warehouse by a solid particle conveyor according to types and stored.
Preferably, the silica gel particles in the third step are metered and then conveyed to the rotary pyrolysis moving bed equipment through a screw conveying system.
Preferably, the certain temperature in the third step is 300-.
Preferably, the solid product silicon dioxide powder in the fourth step is continuously output to a lower-section high-temperature activation device through a material sealing conveying device to prepare high-purity silicon dioxide.
Preferably, the gas-phase product in the fourth step enters a condenser separation system under a closed condition, is washed and collected into a methyl cyclosiloxane mixed ring body (DMC), and the methyl cyclosiloxane mixed ring body is added with a methyl end capping agent after molecular rearrangement and is subjected to catalytic polymerization reaction with a basic catalyst potassium hydroxide or tetramethyl ammonium hydroxide at the temperature of 150 ℃ to prepare the dimethyl silicone oil.
Preferably, the temperature of the gas combustion system in the fourth step is 1100 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the process realizes the product classification of the waste silica gel and the product quality guarantee in the later production by a mechanical and manual two-stage separation mode;
2. the process realizes the conversion from intermittent production to continuous, intelligent and large-scale production in the waste silica gel treatment industry through screw propulsion, rotary decomposition and solid-gas separation equipment;
3. the continuous and closed network management equipment adopted in the process realizes the environmental problem in the production process, and greatly reduces the labor intensity of workers;
4. the non-condensable gas in the production is effectively introduced into the heating system, so that partial energy self-supply of the production line is realized, the energy is saved, and the carbon emission is reduced;
5. the continuous and constant material temperature control and motion mode in the process ensures that the quality of the produced product is more stable;
6. the process design ensures that the discharge amount of production pollutants is far lower than the national standard and the industrial standard, and the resource recycling rate is far higher than the national standard and the industrial standard.
Description of the drawings:
FIG. 1 is a process flow diagram of the present invention.
The specific implementation mode is as follows:
the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings, and the preferred embodiments in the description are only examples, and all other embodiments obtained by those skilled in the art without any inventive work belong to the protection scope of the present invention.
As shown in fig. 1, the following technical solutions are adopted in the present embodiment: the operation steps are as follows:
step one, recovering waste silicon collagen materials, and then carrying out manual and mechanical mixing and sorting;
secondly, crushing the sorted waste silica gel into solid particles with the particle size of less than 10mm in batches according to the types, and respectively sending the silica gel particles into a storage tank of a warehouse for storage according to the types through a solid particle conveyor;
conveying the metered silica gel particles to rotary thermal decomposition moving bed equipment by a screw conveying system, heating to 300-;
step four, the decomposed main solid phase products are silicon dioxide powder containing impurities, the gas phase products are siloxane gases such as D3, D4, D5, D6, D7 and D8, and the solid phase products and the gas phase products are separated out of the moving bed equipment through two-phase separation output equipment; namely, the solid product silicon dioxide powder is continuously output to a lower-stage high-temperature activation device through a material sealing conveying device to prepare high-purity silicon dioxide; qi (Qi)The phase product enters a condenser separation system under a closed condition, is washed and is collected as a methyl cyclosiloxane mixed ring body (DMC), the DMC is added with a methyl end capping agent after molecular rearrangement and uses an alkaline catalyst potassium hydroxide (KOH) or tetramethyl ammonium hydroxide (C)4H13NO) at 150 ℃ to prepare dimethyl silicone oil by catalytic polymerization; the non-condensable gas is conveyed to a gas combustion chamber (1100 ℃) system through a full wind fan to be fully incinerated and harmlessly treated, and energy supplement is provided for equipment.
After the process is adopted, the beneficial effects of the specific embodiment are as follows:
1. the process realizes the product classification of the waste silica gel and the product quality guarantee in the later production by a mechanical and manual two-stage separation mode;
2. the process realizes the conversion from intermittent production to continuous, intelligent and large-scale production in the waste silica gel treatment industry through screw propulsion, rotary decomposition and solid-gas separation equipment;
3. the continuous and closed network management equipment adopted in the process realizes the environmental problem in the production process, and greatly reduces the labor intensity of workers;
4. the non-condensable gas in the production is effectively introduced into the heating system, so that partial energy self-supply of the production line is realized, the energy is saved, and the carbon emission is reduced;
5. the continuous and constant material temperature control and motion mode in the process ensures that the quality of the produced product is more stable;
6. the process design ensures that the discharge amount of production pollutants is far lower than the national standard and the industrial standard, and the resource recycling rate is far higher than the national standard and the industrial standard.
It will be appreciated by those skilled in the art that modifications and equivalents may be made to the embodiments described above, and that various modifications, equivalents, improvements and the like may be made without departing from the spirit and scope of the invention.
Claims (9)
1. The production process for producing the dimethyl silicone oil and the silicon dioxide by utilizing the waste silicon rubber is characterized by comprising the following steps of: the operation steps are as follows:
the method comprises the following steps of (A) recovering waste silicon collagen materials and then sorting the recovered waste silicon collagen materials;
crushing the sorted waste silica gel into uniform particles;
metering and conveying the silica gel particles into rotary thermal decomposition moving bed equipment, and heating to a certain temperature for decomposition under the conditions of micro-negative pressure, continuous closed loop and indirect heating so as to break the cross-linking state of the silicone rubber polymer;
step four, decomposing main solid-phase products into silicon dioxide powder and gas-phase products, and separating the solid-phase products and the gas-phase products out of the moving bed equipment through two-phase separation output equipment; namely, the solid product silicon dioxide powder is continuously output and collected through a material sealing conveying device; collecting the gas-phase product as a methyl cyclosiloxane mixed ring body (DMC) through a condensation and washing separation system; and conveying the non-condensable gas in the gas-phase product to a gas combustion chamber system through a full-wind fan to fully burn and perform harmless treatment and provide energy supplement for equipment.
2. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: the components of the gas phase product are siloxane gases such as D3, D4, D5, D6, D7, D8 and the like.
3. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: the particle size of the uniform particles in the step (two) is less than 10 mm.
4. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: and (5) respectively conveying the uniform particles in the step (II) into a storage tank of a warehouse for storage according to the types through a solid particle conveyor.
5. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: and (5) conveying the silica gel particles in the step (III) into rotary thermal decomposition moving bed equipment through a screw conveying system after metering.
6. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: the certain temperature in the step (three) is 300-500 ℃.
7. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: and (5) continuously outputting the solid product silicon dioxide powder in the step (IV) to a lower-section high-temperature activation device through material sealing conveying equipment to prepare high-purity silicon dioxide.
8. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: and (3) introducing the gas-phase product in the step (IV) into a condenser separation system under a closed condition, washing, collecting the gas-phase product to form a methyl cyclosiloxane mixed ring body, performing molecular rearrangement on the methyl cyclosiloxane mixed ring body, adding a methyl end-capping agent, and performing catalytic polymerization reaction on potassium hydroxide or tetramethyl ammonium hydroxide serving as an alkaline catalyst at the temperature of 150 ℃ to prepare the dimethyl silicone oil.
9. The process for producing dimethylsilicone oil and silicon dioxide by using waste silicone rubber as claimed in claim 1, wherein the process comprises the following steps: the temperature of the gas combustion system in the step (IV) is 1100 ℃.
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CN202110933435.1A CN113773496A (en) | 2021-08-14 | 2021-08-14 | Production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber |
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CN202110933435.1A CN113773496A (en) | 2021-08-14 | 2021-08-14 | Production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber |
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CN202110933435.1A Withdrawn CN113773496A (en) | 2021-08-14 | 2021-08-14 | Production process for producing dimethyl silicone oil and silicon dioxide by using waste silicone rubber |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114655961A (en) * | 2022-04-11 | 2022-06-24 | 重庆大学 | Simple recovery system and process for waste composite insulator silicone rubber |
CN115156239A (en) * | 2022-07-15 | 2022-10-11 | 山东邦凯新材料有限公司 | Device and processing technology for preparing high-purity silicon dioxide by continuous recovery treatment of hazardous waste silica gel |
-
2021
- 2021-08-14 CN CN202110933435.1A patent/CN113773496A/en not_active Withdrawn
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114655961A (en) * | 2022-04-11 | 2022-06-24 | 重庆大学 | Simple recovery system and process for waste composite insulator silicone rubber |
CN114655961B (en) * | 2022-04-11 | 2023-11-07 | 重庆大学 | Simple recovery system and process for waste composite insulator silicon rubber |
CN115156239A (en) * | 2022-07-15 | 2022-10-11 | 山东邦凯新材料有限公司 | Device and processing technology for preparing high-purity silicon dioxide by continuous recovery treatment of hazardous waste silica gel |
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