CN103408901A - Method for irradiation induction modified waste epoxy resin - Google Patents
Method for irradiation induction modified waste epoxy resin Download PDFInfo
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- CN103408901A CN103408901A CN2013103421099A CN201310342109A CN103408901A CN 103408901 A CN103408901 A CN 103408901A CN 2013103421099 A CN2013103421099 A CN 2013103421099A CN 201310342109 A CN201310342109 A CN 201310342109A CN 103408901 A CN103408901 A CN 103408901A
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- epoxy resin
- waste epoxy
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- irradiation
- induced
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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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- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention relates to a method for irradiation induction modified waste epoxy resin. The method comprises the followings: (1), after being crushed and dried, cleaned waste epoxy resin is placed into an irradiation reactor; (2), the irradiation reactor is sent to an irradiation chamber through single rail suspension, and 60 CO gamma rays are used for irradiation, so as to obtain irradiation induced waste epoxy resin; (3), polyvinyl chloride is added into the irradiation induced waste epoxy resin obtained in the step (2), then auxiliaries are added, and the waste epoxy resin, the polyvinyl chloride and the auxiliaries are mixed uniformly, so as to obtain waste epoxy resin mixture; (4), plasticized reaction to the waste epoxy resin mixture obtained is performed so as to obtain the blend of the waste epoxy resin mixture, finally hot pressing and cooling are performed, and the modified waste epoxy resin is obtained. According to the invention, irradiation induction for modification is led into the field of waste epoxy resin regeneration, through accurately controlling the irradiation time and the irradiation dose, the efficiency of the regenerative reaction of waste epoxy resin after irradiation induction and the polyvinyl chloride can be improved, and the heat resistance and the mechanical property of the regenerated composite material are improved greatly.
Description
Technical field
The invention belongs to waste and old thermoset(ting)plastic regeneration field, particularly a kind of method of radiation-induced modified waste epoxy resin.
Background technology
Owing to possessing unique three-dimensional netted crosslinking structure, waste epoxy resin can not reheat fusing, also can't in solvent, dissolve, and the resource utilization difficulty is large.At present, the disposal that waste epoxy resin is commonly used utilizes technology to mainly contain physical method, chemical process and energy recovery method.
Patent CN101580625A has introduced the recycle of discarded thermoset(ting)plastic (epoxy resin) and circulate molding technology and technique again, has realized regeneration waste epoxy resin on general thermoplastic processing units.But owing to differing in the source of waste epoxy resin, the raw material of variant production is all variant on composition and structure, causes with the regenerative response efficiency of polyvinyl chloride and the character of regeneration gained matrix material and also have a great difference.
Radiation-induced modification technology is widely used in the irradiation processing of plastics, mainly contains cross-linking radiation, hardening with radiation, irradiation to crack and irradiation grafting modification etc.Have and the advantage such as be easy to control, technique is simple.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of radiation-induced modified waste epoxy resin, and the method is simple to operate, the matrix material that the waste epoxy resin of preparing and polyvinyl chloride obtain through regenerative response, and shock strength is significantly improved.
The method of a kind of radiation-induced modified waste epoxy resin of the present invention comprises:
(1) to pulverize be the even particulate of 80～120 purpose to the waste epoxy resin after cleaning, 120 ℃ fully dry 40～60min after, be placed in the irradiation reaction device;
(2) above-mentioned irradiation reaction device being hung and is sent to radiation chamber through single track, at normal temperatures, is 0.5～5kGy/h's with radiation dose rate
60The Co gammairradiation, make total dose reach 15～35kGy, obtains the waste epoxy resin after radiation-induced;
(3) step (2) obtain radiation-induced after waste epoxy resin in add polyvinyl chloride, then add auxiliary agent to mix, obtain the waste epoxy resin mixture;
(4) resulting waste epoxy resin mixture is carried out to plastication, obtain the waste epoxy resin blend, finally carry out hot pressing and cold pressing, obtain regenerated composite material.
Waste epoxy resin described in step (1) is to derive from the scrap stock that produce in waste printed circuit board or production process.
Irradiation reaction device described in step (1) is to be applicable to
60The boxlike reactor that the sheet metal of carried of the solid state powder shape sample of Co γ radiation chamber assembles.
Waste epoxy resin after radiation-induced described in step (3) and the mass ratio of polyvinyl chloride are 8:2～5:5.
Waste epoxy resin after radiation-induced described in step (3) and the mass ratio of polyvinyl chloride are 8:2,6:4 or 5:5.
Auxiliary agent described in step (3) accounts for 0.5～3% of waste epoxy resin mixture total mass.
Auxiliary agent described in step (3) is one or more in thermo-stabilizer and lubricant.
The temperature of reaction of the plastication described in step (4) is 205 ℃, and when rotating speed was 45rpm, the time was 3min, and conversion unit is torque rheometer, can obtain the streams varied curve simultaneously.
Hot pressing described in step (4), in temperature, being hot pressing 10min under 185 ℃, the condition of pressure 15Mpa, is colded pressing for the 10min that colds pressing at normal temperatures; Molding apparatus wherein is hydraulic forming machine.
The present invention introduces waste epoxy resin regeneration field by radiation-induced modification, and by the accurate control of irradiation time and irradiation dose, make the efficiency of the waste epoxy resin regenerative response after radiation-induced be improved, thermotolerance, the mechanical property of the matrix material that regeneration makes are taken on a new look greatly.
Beneficial effect:
(1) the present invention is by the accurate control to irradiation time and irradiation dose, utilize gamma-ray irradiation to induce the part side chain binding fracture in the waste epoxy resin molecular structure, active group increases, increase node and the probability of in the regenerative response, being combined with polyvinyl chloride, improved reaction efficiency;
(2) matrix material that obtains through regenerative response of the waste epoxy resin prepared of the present invention and polyvinyl chloride, through thermogravimetric analysis, thermotolerance is significantly improved in the time of 600 ℃;
(3) matrix material that obtains through regenerative response of the waste epoxy resin prepared of the present invention and polyvinyl chloride, shock strength is significantly improved.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention be used to the present invention is described.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) clean waste epoxy resin is crushed to the even particulate of 80 purpose, utilizes vacuum drying oven after under 120 ℃, fully drying 40～60min, be placed in the irradiation reaction device;
(2) the irradiation reaction device being hung and is sent to radiation chamber through single track, at normal temperatures, is 0.5～5kGy/h's with radiation dose rate
60The Co gamma-ray irradiation, make total dose reach 35kGy, obtains the waste epoxy resin after radiation-induced;
(3) in the waste epoxy resin obtained of step (2), add polyvinyl chloride according to different proportioning 8:2, mix with 0.5～3% HSt+Ca/Zn thermo-stabilizer, obtain the waste epoxy resin mixture.
(4) resulting waste epoxy resin mixture being put into to torque rheometer, is 205 ℃, rotating speed while being 45rpm in temperature, and plastication 3min, take out the waste epoxy resin blend, can obtain the streams varied curve simultaneously.
(5) will put into fast prefabricated mould from the blend that rheometer takes out, then be placed in hydraulic forming machine.In temperature, be hot pressing 10min under 185 ℃, the condition of pressure 15Mpa, the 10min that colds pressing at normal temperatures, can obtain regenerated composite material.
As can be known by analysis, when the irradiation total dose was 35kGy, the tensile strength of the regenerated composite material made under these conditions was about 7MPa, and shock strength can reach 3.71KJ/m
2.
Embodiment 2
(1) clean waste epoxy resin is crushed to the even particulate of 80 purpose, utilizes vacuum drying oven after under 120 ℃, fully drying 40～60min, be placed in the irradiation reaction device;
(2) the irradiation reaction device being hung and is sent to radiation chamber through single track, at normal temperatures, is 0.5～5kGy/h's with radiation dose rate
60The Co gamma-ray irradiation, make total dose reach 25～35kGy, obtains the waste epoxy resin after radiation-induced;
(3) in the waste epoxy resin obtained of step (2), add polyvinyl chloride according to different proportioning 6:4, mix with 0.5～3% HSt+Ca/Zn thermo-stabilizer, obtain the waste epoxy resin mixture.
(4) resulting waste epoxy resin mixture being put into to torque rheometer, is 205 ℃, rotating speed while being 45rpm in temperature, and plastication 3min, take out the waste epoxy resin blend, can obtain the streams varied curve simultaneously.
(5) will put into fast prefabricated mould from the blend that rheometer takes out, then be placed in hydraulic forming machine.In temperature, be hot pressing 10min under 185 ℃, the condition of pressure 15Mpa, the 10min that colds pressing at normal temperatures, can obtain regenerated composite material.
As can be known by analysis, when the irradiation total dose was in 25～35kGy scope, the tensile strength of the regenerated composite material made under these conditions was about 27.31MPa, and shock strength can reach 8.17KJ/m
2.And also as can be known through thermogravimetric analysis, the initial decomposition temperature of regenerated composite material is 280 ℃, while surpassing 600 ℃, thermotolerance obviously improves.
Embodiment 3
(1) clean waste epoxy resin is crushed to the even particulate of 80 purpose, utilizes vacuum drying oven after under 120 ℃, fully drying 40～60min, be placed in the irradiation reaction device;
(2) the irradiation reaction device being hung and is sent to radiation chamber through single track, at normal temperatures, is 0.5～5KGy/h's with radiation dose rate
60The Co gamma-ray irradiation, make total dose reach 15kGy, obtains the waste epoxy resin after radiation-induced;
(3) in the waste epoxy resin obtained of step (2), add polyvinyl chloride according to different proportioning 5:5, mix with 0.5～3% HSt+Ca/Zn thermo-stabilizer, obtain the waste epoxy resin mixture.
(4) resulting waste epoxy resin mixture being put into to torque rheometer, is 205 ℃, rotating speed while being 45rpm in temperature, and plastication 3min, take out the waste epoxy resin blend, can obtain the streams varied curve simultaneously.
(5) will from the blend that rheometer takes out, put into fast a certain size mould, then be placed in hydraulic forming machine.In temperature, be hot pressing 10min under 185 ℃, the condition of pressure 15Mpa, the 10min that colds pressing at normal temperatures, can obtain regenerated composite material.
As can be known by analysis, during at 15kGy, the tensile strength of the regenerated composite material made under these conditions is about 30.33MPa when the irradiation total dose, and shock strength can reach 8.88KJ/m
2.
Claims (9)
1. the method for a radiation-induced modified waste epoxy resin comprises:
(1) to pulverize be the even particulate of 80～120 purpose to the waste epoxy resin after cleaning, 120 ℃ fully dry 40～60min after, be placed in the irradiation reaction device;
(2) above-mentioned irradiation reaction device being hung and is sent to radiation chamber through single track, at normal temperatures, is 0.5～5kGy/h's with radiation dose rate
60The Co gammairradiation, make total dose reach 15～35kGy, obtains the waste epoxy resin after radiation-induced;
(3) step (2) obtain radiation-induced after waste epoxy resin in add polyvinyl chloride, then add auxiliary agent to mix, obtain the waste epoxy resin mixture;
(4) resulting waste epoxy resin mixture is carried out to plastication, obtain the waste epoxy resin blend, finally carry out hot pressing and cold pressing, obtain regenerated composite material.
2. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1, it is characterized in that: the waste epoxy resin described in step (1) is to derive from the scrap stock that produce in waste printed circuit board or production process.
3. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1, it is characterized in that: the irradiation reaction device described in step (1) is to be applicable to
60The boxlike reactor that the sheet metal of carried of the solid state powder shape sample of Co γ radiation chamber assembles.
4. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1 is characterized in that: the waste epoxy resin after radiation-induced described in step (3) and the mass ratio of polyvinyl chloride are 8:2～5:5.
5. according to the method for the described a kind of radiation-induced modified waste epoxy resin of claim 1 or 4, it is characterized in that: the waste epoxy resin after radiation-induced described in step (3) and the mass ratio of polyvinyl chloride are 8:2,6:4 or 5:5.
6. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1, it is characterized in that: the auxiliary agent described in step (3) accounts for 0.5～3% of waste epoxy resin mixture total mass.
7. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1, it is characterized in that: the auxiliary agent described in step (3) is one or more in thermo-stabilizer and lubricant.
8. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1, it is characterized in that: the temperature of reaction of the plastication described in step (4) is 205 ℃, and when rotating speed was 45rpm, the time was 3min, and conversion unit is torque rheometer.
9. the method for a kind of radiation-induced modified waste epoxy resin according to claim 1 is characterized in that: the hot pressing described in step (4), in temperature, being hot pressing 10min under 185 ℃, the condition of pressure 15Mpa, is colded pressing for the 10min that colds pressing at normal temperatures; Molding apparatus wherein is hydraulic forming machine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310342109.9A CN103408901B (en) | 2013-08-07 | 2013-08-07 | A kind of method of radiation-induced modified waste epoxy resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310342109.9A CN103408901B (en) | 2013-08-07 | 2013-08-07 | A kind of method of radiation-induced modified waste epoxy resin |
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| CN103408901A true CN103408901A (en) | 2013-11-27 |
| CN103408901B CN103408901B (en) | 2016-05-04 |
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| CN201310342109.9A Expired - Fee Related CN103408901B (en) | 2013-08-07 | 2013-08-07 | A kind of method of radiation-induced modified waste epoxy resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987480A (en) * | 2017-12-14 | 2018-05-04 | 广东机电职业技术学院 | A kind of flame retardant type epoxy/polyvinyl chloride composite foam material and its preparation method and application |
| CN110724973A (en) * | 2019-11-19 | 2020-01-24 | 安徽焦冲矿业有限公司 | Efficient environment-friendly high-purity gold preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3912605A (en) * | 1971-07-26 | 1975-10-14 | Japan Atomic Energy Res Inst | Radiation crosslinked vinyl chloride resin |
| US4336211A (en) * | 1979-11-19 | 1982-06-22 | Agency Of Industrial Science And Technology | Method for the preparation of shaped articles of a vinyl chloride based resin having improved surface properties |
| CN101580625A (en) * | 2008-05-12 | 2009-11-18 | 陆书玉 | Technology and process of cyclic utilization and cyclic remolding of waste thermosetting plastic (epoxide resin) |
-
2013
- 2013-08-07 CN CN201310342109.9A patent/CN103408901B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3912605A (en) * | 1971-07-26 | 1975-10-14 | Japan Atomic Energy Res Inst | Radiation crosslinked vinyl chloride resin |
| US4336211A (en) * | 1979-11-19 | 1982-06-22 | Agency Of Industrial Science And Technology | Method for the preparation of shaped articles of a vinyl chloride based resin having improved surface properties |
| CN101580625A (en) * | 2008-05-12 | 2009-11-18 | 陆书玉 | Technology and process of cyclic utilization and cyclic remolding of waste thermosetting plastic (epoxide resin) |
Non-Patent Citations (1)
| Title |
|---|
| 翁燕青，等: "废旧线路板中环氧树脂的辐射接枝改性", 《宁波化工》, no. 3, 15 September 2008 (2008-09-15), pages 14 - 16 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987480A (en) * | 2017-12-14 | 2018-05-04 | 广东机电职业技术学院 | A kind of flame retardant type epoxy/polyvinyl chloride composite foam material and its preparation method and application |
| CN110724973A (en) * | 2019-11-19 | 2020-01-24 | 安徽焦冲矿业有限公司 | Efficient environment-friendly high-purity gold preparation method |
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| CN103408901B (en) | 2016-05-04 |
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Granted publication date: 20160504 Termination date: 20190807 |