CN111363197A - Method for recovering thermosetting fiber composite material by supercritical fluid - Google Patents
Method for recovering thermosetting fiber composite material by supercritical fluid Download PDFInfo
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- 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
- C08J11/16—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 by treatment with inorganic material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
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- 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
- C08J11/18—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 by treatment with organic material
- C08J11/22—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 by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/24—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 by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
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- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/06—Unsaturated polyesters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- 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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Abstract
The invention aims to provide a method for recovering thermosetting fiber composite material by supercritical fluid, which can obviously improve the recovery rate of fiber, better preserve the fiber performance, reduce the resource consumption, have no secondary pollution, realize near zero emission of the whole system, reduce the reaction conditions, be easy to control the reaction, and realize the harmless treatment of waste and the high-value reutilization of materials by recycling the collected solid, liquid and gas products after the reaction. The method for recovering the thermosetting fiber composite material by the supercritical fluid comprises the steps of crushing waste articles made of the thermosetting fiber composite material into particles to obtain thermosetting fiber composite material particles; adding thermoset fiber composite particles to a supercritical fluid reactor; opening an exhaust hole at the top of the supercritical fluid reactor, and inputting carbon dioxide from the lower part of the supercritical fluid reactor until the supercritical fluid reactor is filled with the carbon dioxide; adding ethanol, n-propanol or n-butanol to the supercritical fluid reactor.
Description
Technical Field
The invention relates to a method for recycling a thermosetting fiber composite material by using a supercritical fluid.
Background
The thermosetting fiber composite material represented by the wind power fan blade can generate irreversible chemical crosslinking reaction in the heating, curing and molding process, and a chemical bond is formed between molecular chains of the thermosetting fiber composite material to form a three-dimensional network structure, so that the resin has stable performance and is not easy to decompose and can not be melted or remolded again, and therefore, the cyclic recycling is difficult to realize.
Currently, the recycling methods for waste thermosetting fiber composite materials mainly include energy recycling, physical recycling and chemical recycling.
The energy recovery is a technology for recovering energy by taking waste blades as fuel, the combustion calorific value of the thermosetting resin-based composite material is about half of that of hard coal, but glass fiber which is a main material is incombustible, can inhibit the combustion process, can enter flue gas to influence the purification of the flue gas, and generates a large amount of fly ash and residues which need to be treated or used, so that the utilization value of the fiber is lost, and the ecological environment pollution is caused.
The physical recovery mainly adopts a crushing and separating technology to use crushed materials as secondary fillers for manufacturing cement, concrete and the like, but most of the materials obtained by the method are low-value regenerated products and are suitable for recovering glass fiber reinforced composite materials, and for the composite materials doped with high-value carbon fibers, the high-value products can be obtained by further separation and purification in cooperation with a chemical recovery method.
Chemical recovery mainly includes heat recovery and solution recovery processes. The heat recovery is a method for decomposing a resin matrix in the composite material into pyrolysis gas or pyrolysis fuel oil of organic micromolecules by high-temperature heating, and then the recyclable solids such as fibers, fillers, metal pieces and the like are left, and the flux and the strength of part of fibers are lost after the pyrolysis recovery.
Before the supercritical/subcritical fluid dissolution method, the dissolution, separation and recovery treatment process is complex, and a solvent with strong oxidizing property and strong corrosivity is mostly adopted, so that the environment is greatly influenced. As a novel recovery method, the supercritical/subcritical fluid technology has the advantages of clean and pollution-free recovery process, clean regenerated fiber surface, excellent performance and the like, but the application conditions of the technology are more strict, and the supercritical water is mostly adopted as a solvent in the current research, so that the requirements on high reaction temperature, high pressure and strict operation conditions are met.
Disclosure of Invention
The invention aims to provide a method for recovering thermosetting fiber composite material by supercritical fluid, which can obviously improve the recovery rate of fiber, better preserve the fiber performance, reduce the resource consumption, has no secondary pollution, near zero emission of the whole system, reduces the reaction condition, is easy to control the reaction, can recycle the collected solid, liquid and gas products after the reaction and realizes the harmless treatment of waste and the high-valued recycling of materials.
The method for recovering the thermosetting fiber composite material by the supercritical fluid is characterized by comprising the following steps:
A. crushing waste articles made of the thermosetting fiber composite material into particles to obtain thermosetting fiber composite material particles;
B. b, adding the thermosetting fiber composite material particles obtained in the step A into a supercritical fluid reactor;
C. opening an exhaust hole at the top of the supercritical fluid reactor, and inputting carbon dioxide from the lower part of the supercritical fluid reactor until the supercritical fluid reactor is filled with the carbon dioxide;
D. adding ethanol, n-propanol or n-butanol into the supercritical fluid reactor, and soaking the thermosetting fiber composite material particles in the supercritical fluid reactor in the ethanol, n-propanol or n-butanol;
E. heating the thermosetting fiber composite material particles in the supercritical fluid reactor to 280-350 ℃, increasing the pressure in the supercritical fluid reactor to 7-10 Mpa, preserving the heat for 60-100 min, swelling epoxy resin, unsaturated polyester resin and the like in the thermosetting fiber composite material particles under the combined action of supercritical carbon dioxide and ethanol, n-propanol or n-butanol, and further decomposing the resin in the thermosetting fiber composite material particles;
F. separating and recovering carbon dioxide, gaseous and liquid organic matters in the supercritical fluid reactor, wherein the gaseous and liquid organic matters comprise benzene, benzene derivatives, phenol and phenol derivatives;
G. and blowing the glass fiber and/or the carbon fiber downwards from the upper part in the supercritical fluid reactor, removing the glass fiber and/or the carbon fiber adhered to the inner wall of the supercritical fluid reactor, and discharging and recovering the glass fiber and/or the carbon fiber from the lower part of the supercritical fluid reactor.
Preferably, the weight of the thermosetting fiber composite material particles in the step A is less than 5 g;
the adding amount of the thermosetting fiber composite particles added into the supercritical fluid reactor in the step B is not more than 40% of the internal volume of the supercritical fluid reactor;
in the step C, the introduction time of carbon dioxide input from the lower part of the supercritical fluid reactor is 20-50 seconds;
in the step D, adding ethanol, n-propanol or n-butanol into the supercritical fluid reactor in an amount which is not more than 40% of the internal volume of the supercritical fluid reactor;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 290-330 ℃, increasing the pressure in the supercritical fluid reactor to 7.5-9.5 MPa, and keeping the temperature for 70-90 min.
Preferably, the weight of the thermosetting fiber composite material particles in the step A is less than 3 g;
in the step C, the introduction time of carbon dioxide input from the lower part of the supercritical fluid reactor is 25-40 seconds;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 295-320 ℃, increasing the pressure in the supercritical fluid reactor to 7.8-9.0 MPa, and keeping the temperature for 75-85 min.
Preferably, the weight of the thermosetting fiber composite material particles in the step A is less than 2 g;
in the step C, the introducing time of carbon dioxide input from the lower part of the supercritical fluid reactor is 30 seconds;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 300 ℃, increasing the pressure in the supercritical fluid reactor to 8Mpa, and keeping the temperature for 80 min.
Preferably, the step F further comprises recovering heat of the ethanol, n-propanol or n-butanol and the gaseous and liquid organic substances in the supercritical fluid recovery reactor by using a heat exchanger, and using the heat to heat the thermosetting fiber composite particles, the carbon dioxide, the ethanol, the n-propanol or the n-butanol, which are about to enter the supercritical fluid recovery reactor.
The method for recovering the thermosetting fiber composite material by the supercritical fluid has the following beneficial effects:
1. according to the method for recovering the thermosetting fiber composite material by using the supercritical fluid, carbon dioxide and alcohols are used as supercritical solvents, so that the reaction conditions are reduced compared with a supercritical water oxidation reactor, and the method is easy to control;
2. because supercritical carbon dioxide and alcohol are adopted as co-solvents, compared with a single solvent, the treatment efficiency can be improved, and the resin decomposition rate can reach more than 95%;
3. the heat exchanger is arranged, so that the high-temperature product generated by the reaction can be fully utilized to heat the feed, the carbon dioxide and the alcohols entering the reactor, the reaction temperature can be quickly reached, and the energy consumption is saved;
4. by recovering carbon dioxide, benzene, phenol and derivatives thereof and collecting residual solid products, the main components are glass fiber and carbon fiber, the harmless treatment of wastes and the high-value reutilization of materials are realized.
The present invention is described in further detail below.
Detailed Description
The method for recovering the thermosetting fiber composite material by the supercritical fluid comprises the following steps:
A. crushing waste articles made of the thermosetting fiber composite material into particles to obtain thermosetting fiber composite material particles;
B. b, adding the thermosetting fiber composite material particles obtained in the step A into a supercritical fluid reactor;
C. opening an exhaust hole at the top of the supercritical fluid reactor, and inputting carbon dioxide from the lower part of the supercritical fluid reactor until the supercritical fluid reactor is filled with the carbon dioxide;
D. adding ethanol, n-propanol or n-butanol into the supercritical fluid reactor, and soaking the thermosetting fiber composite material particles in the supercritical fluid reactor in the ethanol, n-propanol or n-butanol;
E. heating the thermosetting fiber composite material particles in the supercritical fluid reactor to 280-350 ℃, increasing the pressure in the supercritical fluid reactor to 7-10 Mpa, preserving the heat for 60-100 min, swelling epoxy resin, unsaturated polyester resin and the like in the thermosetting fiber composite material particles under the combined action of supercritical carbon dioxide and ethanol, n-propanol or n-butanol, and further decomposing the resin in the thermosetting fiber composite material particles;
F. recovering n-propanol or n-butanol in the supercritical fluid reactor, and separating and recovering carbon dioxide, gaseous and liquid organic substances in the supercritical fluid reactor, wherein the gaseous and liquid organic substances comprise benzene, benzene derivatives, phenol and phenol derivatives;
G. and blowing the glass fiber and/or the carbon fiber downwards from the upper part in the supercritical fluid reactor, removing the glass fiber and/or the carbon fiber adhered to the inner wall of the supercritical fluid reactor, and discharging and recovering the glass fiber and/or the carbon fiber from the lower part of the supercritical fluid reactor.
As a further improvement of the invention, the weight of the thermosetting fiber composite material particles in the step A is less than 5 g;
the adding amount of the thermosetting fiber composite particles added into the supercritical fluid reactor in the step B is not more than 40% of the internal volume of the supercritical fluid reactor;
in the step C, the introduction time of carbon dioxide input from the lower part of the supercritical fluid reactor is 20-50 seconds;
in the step D, adding ethanol, n-propanol or n-butanol into the supercritical fluid reactor in an amount which is not more than 40% of the internal volume of the supercritical fluid reactor;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 290-330 ℃, increasing the pressure in the supercritical fluid reactor to 7.5-9.5 MPa, and keeping the temperature for 70-90 min.
As a further improvement of the invention, the weight of the thermosetting fiber composite material particles in the step A is less than 3 g;
in the step C, the introduction time of carbon dioxide input from the lower part of the supercritical fluid reactor is 25-40 seconds;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 295-320 ℃, increasing the pressure in the supercritical fluid reactor to 7.8-9.0 MPa, and keeping the temperature for 75-85 min.
As a further improvement of the invention, the weight of the thermosetting fiber composite material particles in the step A is less than 2 g;
in the step C, the introducing time of carbon dioxide input from the lower part of the supercritical fluid reactor is 30 seconds;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 300 ℃, increasing the pressure in the supercritical fluid reactor to 8Mpa, and keeping the temperature for 80 min.
As a further improvement of the present invention, the step F further comprises recovering heat of the ethanol, n-propanol or n-butanol and the gaseous and liquid organic substances in the supercritical fluid recovery reactor by using a heat exchanger, and using the heat to heat the thermosetting fiber composite material particles, carbon dioxide, ethanol, n-propanol or n-butanol which are about to enter the supercritical fluid recovery reactor.
Compared with the prior physical recovery method and heat recovery method, the method for recovering the thermosetting fiber composite material by using the supercritical fluid can obviously improve the recovery rate of the fiber, better preserve the performance of the fiber and reduce the occupied area. Compared with other solvent methods, the method reduces resource consumption, has no secondary pollution and near zero emission of the whole system. According to the method for recovering the thermosetting fiber composite material by using the supercritical fluid, carbon dioxide and alcohols are used as supercritical solvents, so that the reaction conditions are reduced compared with a supercritical water oxidation reactor, and the method is easy to control; the solid, liquid and gas products after the collection reaction can be reused, and the harmless treatment of wastes and the high-valued reutilization of materials are realized.
Claims (5)
1. A method for recovering thermosetting fiber composite material by supercritical fluid is characterized by comprising the following steps:
A. crushing waste articles made of the thermosetting fiber composite material into particles to obtain thermosetting fiber composite material particles;
B. b, adding the thermosetting fiber composite material particles obtained in the step A into a supercritical fluid reactor;
C. opening an exhaust hole at the top of the supercritical fluid reactor, and inputting carbon dioxide from the lower part of the supercritical fluid reactor until the supercritical fluid reactor is filled with the carbon dioxide;
D. adding ethanol, n-propanol or n-butanol into the supercritical fluid reactor, and soaking the thermosetting fiber composite material particles in the supercritical fluid reactor in the ethanol, n-propanol or n-butanol;
E. heating the thermosetting fiber composite material particles in the supercritical fluid reactor to 280-350 ℃, increasing the pressure in the supercritical fluid reactor to 7-10 Mpa, preserving the heat for 60-100 min, swelling epoxy resin, unsaturated polyester resin and the like in the thermosetting fiber composite material particles under the combined action of supercritical carbon dioxide and ethanol, n-propanol or n-butanol, and further decomposing the resin in the thermosetting fiber composite material particles;
F. separating and recovering carbon dioxide, gaseous and liquid organic matters in the supercritical fluid reactor, wherein the gaseous and liquid organic matters comprise benzene, benzene derivatives, phenol and phenol derivatives;
G. and blowing the glass fiber and/or the carbon fiber downwards from the upper part in the supercritical fluid reactor, removing the glass fiber and/or the carbon fiber adhered to the inner wall of the supercritical fluid reactor, and discharging and recovering the glass fiber and/or the carbon fiber from the lower part of the supercritical fluid reactor.
2. The method of supercritical fluid recovery of thermoset fiber composites according to claim 1, characterized in that: the weight of the thermosetting fiber composite material particles in the step A is less than 5 g;
the adding amount of the thermosetting fiber composite particles added into the supercritical fluid reactor in the step B is not more than 40% of the internal volume of the supercritical fluid reactor;
in the step C, the introduction time of carbon dioxide input from the lower part of the supercritical fluid reactor is 20-50 seconds;
in the step D, adding ethanol, n-propanol or n-butanol into the supercritical fluid reactor in an amount which is not more than 40% of the internal volume of the supercritical fluid reactor;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 290-330 ℃, increasing the pressure in the supercritical fluid reactor to 7.5-9.5 MPa, and keeping the temperature for 70-90 min.
3. The method of supercritical fluid recovery of thermoset fiber composites according to claim 2, characterized in that: the weight of the thermosetting fiber composite material particles in the step A is less than 3 g;
in the step C, the introduction time of carbon dioxide input from the lower part of the supercritical fluid reactor is 25-40 seconds;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 295-320 ℃, increasing the pressure in the supercritical fluid reactor to 7.8-9.0 MPa, and keeping the temperature for 75-85 min.
4. A method of supercritical fluid recovery of thermoset fiber composites in accordance with claim 3, wherein: the weight of the thermosetting fiber composite material particles in the step A is less than 2 g;
in the step C, the introducing time of carbon dioxide input from the lower part of the supercritical fluid reactor is 30 seconds;
and E, heating the thermosetting fiber composite particles in the supercritical fluid reactor to 300 ℃, increasing the pressure in the supercritical fluid reactor to 8Mpa, and keeping the temperature for 80 min.
5. The method for supercritical fluid recovery of thermoset fiber composites according to any of claims 1 to 4, characterized in that: and the step F also comprises the step of recovering the heat of the ethanol, the n-propanol or the n-butanol and the gaseous and liquid organic matters in the supercritical fluid reactor by using a heat exchanger, and using the heat to heat the thermosetting fiber composite material particles, the carbon dioxide, the ethanol, the n-propanol or the n-butanol which are about to enter the supercritical fluid reactor.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060116393A (en) * | 2005-05-09 | 2006-11-15 | 충남대학교산학협력단 | Process for preparing fluconazole of specific crystalline form using super critical fluid |
| CN102181071A (en) * | 2011-04-22 | 2011-09-14 | 中国科学院宁波材料技术与工程研究所 | Method for reclaiming carbon fiber reinforced epoxy resin composite material |
| CN103333360A (en) * | 2013-07-10 | 2013-10-02 | 合肥工业大学 | Reinforcement mode based high-performance fiber reinforced resin based composite material recovery method |
| CN106496631A (en) * | 2016-11-03 | 2017-03-15 | 南京工程学院 | The method that overcritical fluid-mixing reclaims carbon fiber enhancement resin base composite material |
| US20190002646A1 (en) * | 2015-07-13 | 2019-01-03 | Sabic Global Technologies B.V. | Process for the preparation of polyolefin particles |
-
2020
- 2020-03-11 CN CN202010164589.4A patent/CN111363197A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20060116393A (en) * | 2005-05-09 | 2006-11-15 | 충남대학교산학협력단 | Process for preparing fluconazole of specific crystalline form using super critical fluid |
| CN102181071A (en) * | 2011-04-22 | 2011-09-14 | 中国科学院宁波材料技术与工程研究所 | Method for reclaiming carbon fiber reinforced epoxy resin composite material |
| CN103333360A (en) * | 2013-07-10 | 2013-10-02 | 合肥工业大学 | Reinforcement mode based high-performance fiber reinforced resin based composite material recovery method |
| US20190002646A1 (en) * | 2015-07-13 | 2019-01-03 | Sabic Global Technologies B.V. | Process for the preparation of polyolefin particles |
| CN106496631A (en) * | 2016-11-03 | 2017-03-15 | 南京工程学院 | The method that overcritical fluid-mixing reclaims carbon fiber enhancement resin base composite material |
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Application publication date: 20200703 |