CN107099052A - A kind of cured epoxy resin lytic agent and its application process - Google Patents
A kind of cured epoxy resin lytic agent and its application process Download PDFInfo
- Publication number
- CN107099052A CN107099052A CN201710274180.6A CN201710274180A CN107099052A CN 107099052 A CN107099052 A CN 107099052A CN 201710274180 A CN201710274180 A CN 201710274180A CN 107099052 A CN107099052 A CN 107099052A
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- cured epoxy
- lytic agent
- parts
- sodium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 40
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 29
- 230000002101 lytic effect Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004090 dissolution Methods 0.000 claims abstract description 9
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 8
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004593 Epoxy Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 230000006378 damage Effects 0.000 abstract 1
- 238000004100 electronic packaging Methods 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Classifications
-
- 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
- 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
- C08J11/28—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 compounds containing nitrogen, sulfur or phosphorus
-
- 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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Encapsulation Of And Coatings For Semiconductor Or Solid State Devices (AREA)
- Epoxy Resins (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention provides a kind of cured epoxy resin lytic agent, is made up of diethylenetriamine, toluene, dichloromethane, ethylene glycol monomethyl ether, sodium hydroxide mixing.The preparation process of cured epoxy resin lytic agent：Sodium hydroxide, ethylene glycol monomethyl ether, diethylenetriamine, toluene and dichloromethane are sequentially added into, then stirs until sodium hydroxide is completely dissolved, obtains cured epoxy resin lytic agent；Cured epoxy resin course of dissolution：Electronic device sample containing cured epoxy resin is put into after being dissolved in cured epoxy resin lytic agent, cleaned with clear water.The present invention has advantages below：1. the cured epoxy resin of electron device package can be dissolved, not the metal device inside destruction；2. preparation technology is simple, can largely it prepare；3. application effect is good, dissolution velocity is fast.Therefore, the present invention has broad application prospects in the metal base recycling field that miniature electric Electronic Packaging and epoxy resin are wrapped up.
Description
Technical field
The present invention relates to lytic agent technical field, and in particular to a kind of cured epoxy resin lytic agent and its application process.
Background technology
Contain active epoxide group in the molecular structure of epoxy resin so that they can be with a variety of different curing agent
React, high polymer of the generation with tridimensional network, here it is solidification.Epoxy resin after solidification has good
Physics, its surface to metal and nonmetallic materials of chemical property has excellent adhesive strength, and dielectric properties are good, deformation
Shrinkage factor is small, and product size stability is good, and hardness is high, and pliability is preferable, so application field is quite varied as electronic device
Encapsulation, cast etc..Exactly these advantages so that be difficult again by the metal or recoverable of the inside after epoxy encapsulation
Material extract again, this runs in the opposite direction with China strategy of sustainable development.Therefore, producing being capable of dissolving cured ring
The solution of oxygen tree fat is extremely necessary.
The research for epoxy resin dissolving agent mainly has two classes at present：First, in acid condition, dissolved epoxy,
Such as Chinese patent CN200810303667.3, this method uses a large amount of formic acid and sulfuric acid, there is larger corrosion to hardware
Property；2nd, organic solvent class, such as Chinese patent CN201310456230.4, this method need return stirring 0.5-1 hours, technique
Relatively complicated, the time is longer.
The content of the invention
It is alkali by condition solution it is an object of the invention to provide a kind of cured epoxy resin lytic agent and its application process
Property condition, realize reduction to the corrosion of other metal devices and improve rate of dissolution.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is：
Calculate by volume：Epoxy resin dissolving agent of the present invention is by 1 part~20 parts of diethylenetriamine, 5 parts of toluene~20 parts, two
20 parts~40 parts of chloromethanes, 20 parts~60 parts of ethylene glycol monomethyl ether, 0.5 part~1.5 parts mixing compositions of sodium hydroxide.
Preferably, above-mentioned epoxy resin dissolving agent is by 5 parts of diethylenetriamine, 19 parts of toluene, 25 parts of dichloromethane, ethylene glycol
40 parts of methyl ether, 1 part of sodium hydroxide composition.
Sodium hydroxide, ethylene glycol monomethyl ether, diethylenetriamine, toluene and dichloromethane are sequentially added into, is then stirred in rotor
Mix in machine and stir, stir 30min, until sodium hydroxide is completely dissolved, obtain cured epoxy resin lytic agent.
Cured epoxy resin lytic agent is added into oil bath pan, by temperature adjustment to 130 DEG C, then will contain cured epoxy tree
The electronic device sample of fat is put into cured epoxy resin lytic agent, after 10min, is taken out sample, is cleaned with clear water.
Properties of Epoxy Resin analysis dissolving cured to prior art, as a result such as following table：
Experimental result understands that the effect of No. 4 lytic agents is ideal, but under acid condition, exists necessarily to metal
Corrosivity.
The dissolving cured Properties of Epoxy Resin analysis through experimental tests of the present invention, as a result such as following table：
| Recipe name | One | Two | Three | Four |
| Dichloromethane (wt%) | 20 | 25 | 25 | 30 |
| Diethylenetriamine (wt%) | 15 | 10 | 5 | 10 |
| Toluene (wt%) | 20 | 20 | 20 | 10 |
| Ethylene glycol monomethyl ether (wt%) | 45 | 45 | 40 | 50 |
| Sodium hydroxide (g) | 2 | 2 | 2 | 2 |
| Temperature (DEG C) | 110 | 110 | 110 | 110 |
| Dissolution velocity (s) | 18 | 16 | 10 | 12 |
Experimental result understands that the dissolving cured epoxy resin time of the invention, rate of dissolution was much better than existing at 10-18 minutes
Technology.
Cured epoxy resin lytic agent of the present invention is as a result as follows to the corrosion condition through experimental tests of copper in electronic device
Table：
Experimental result understands that cured epoxy resin lytic agent of the present invention does not corrode to the copper in electronic device.
Therefore, the present invention is relative to prior art, with advantages below：
1. the cured epoxy resin of electron device package can be dissolved well, and the metal device of the inside will not be destroyed
Part；
2. preparation technology is simple, without too complicated operation, as long as sample is added in solution, as long as and raw material
Abundance just can be prepared largely；
3. application effect is good, dissolution velocity is fast, as long as crossing 10min with regard to that can be completely dissolved.
Therefore, the present invention have compared with prior art can targetedly dissolving cured epoxy resin it is internal without influenceing
Metal device, and improve rate of dissolution, had broad application prospects in electron device package recycling field.
Embodiment
The present invention is described in further detail, but be not limitation of the present invention by embodiment to present invention.
Embodiment
1. the preparation process of cured epoxy resin lytic agent is：
50ml beaker is taken, 2g sodium hydroxide, 20ml ethylene glycol monomethyl ether, 2.5ml divinyl three is sequentially added into
Then amine, 10ml toluene, 12.5ml dichloromethane stirs in rotor mixer, 30min is stirred, until sodium hydroxide
It is completely dissolved, obtains cured epoxy resin lytic agent；
2. cured epoxy resin course of dissolution：
Cured epoxy resin lytic agent is added into oil bath pan, by temperature adjustment to 130 DEG C, then will contain cured epoxy tree
The electronic device sample of fat is put into cured epoxy resin lytic agent, after 10min, is taken out sample, is cleaned with clear water.
Claims (2)
1. a kind of cured epoxy resin lytic agent, it is characterised in that：By 1 part~20 parts of diethylenetriamine, 5 parts~20 parts of toluene,
20 parts~40 parts of dichloromethane, 20 parts~60 parts of ethylene glycol monomethyl ether, 0.5 part ~ 1.5 parts mixing compositions of sodium hydroxide.
2. the application process of cured epoxy resin lytic agent according to claim 1, it is characterised in that comprise the following steps：
Step（1）The preparation process of cured epoxy resin lytic agent, is sequentially added into sodium hydroxide, ethylene glycol monomethyl ether, divinyl
Triamine, toluene and dichloromethane, then stir until sodium hydroxide is completely dissolved, obtain cured epoxy resin lytic agent；
Step（2）Cured epoxy resin course of dissolution, adds oil bath pan by cured epoxy resin lytic agent, temperature adjustment is arrived
130 DEG C, then cured epoxy resin sample is put into cured epoxy resin lytic agent, is put into oil bath pan, epoxy to be solidified
Sample is taken out after resin dissolving, is cleaned with clear water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710274180.6A CN107099052B (en) | 2017-04-25 | 2017-04-25 | Curing epoxy resin dissolving agent and application method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710274180.6A CN107099052B (en) | 2017-04-25 | 2017-04-25 | Curing epoxy resin dissolving agent and application method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107099052A true CN107099052A (en) | 2017-08-29 |
| CN107099052B CN107099052B (en) | 2020-11-24 |
Family
ID=59657483
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710274180.6A Active CN107099052B (en) | 2017-04-25 | 2017-04-25 | Curing epoxy resin dissolving agent and application method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107099052B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111117815A (en) * | 2019-12-31 | 2020-05-08 | 南通曜世新材料科技有限公司 | Resin dissolving solution for resin diamond wire and broken wire connection method thereof |
| CN111547725A (en) * | 2020-05-14 | 2020-08-18 | 湖南太子新材料科技有限公司 | Preparation method for extracting silicon carbide from polyurethane wrapped with silicon carbide |
| CN111660472A (en) * | 2020-06-08 | 2020-09-15 | 西安微电子技术研究所 | Method for cleaning residues in mold cavity of mold box in plastic package mold |
| CN114854385A (en) * | 2022-03-21 | 2022-08-05 | 中国石油化工股份有限公司 | Asphaltene dispersion inhibitor with coating shell and preparation method thereof |
| CN115595133A (en) * | 2021-07-07 | 2023-01-13 | 中国石油化工股份有限公司（Cn） | Composition for dissolving plugging agent and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04306272A (en) * | 1991-04-03 | 1992-10-29 | Majitsuku Man Kk | Epoxy resin remover |
| CN101649068A (en) * | 2008-08-12 | 2010-02-17 | 贵州航天林泉电机有限公司 | Epoxy resin dissolving agent and preparing method thereof |
| CN102433043A (en) * | 2011-09-13 | 2012-05-02 | 天津德高化成电子材料有限公司 | Epoxy resin and silicon resin cured coating and package removing agent and preparation method thereof |
| CN104194038A (en) * | 2014-08-29 | 2014-12-10 | 浙江大学 | Epoxy resin composition, and wet-process ultrasonic degradation method and application thereof |
-
2017
- 2017-04-25 CN CN201710274180.6A patent/CN107099052B/en active Active
Patent Citations (4)
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|---|---|---|---|---|
| JPH04306272A (en) * | 1991-04-03 | 1992-10-29 | Majitsuku Man Kk | Epoxy resin remover |
| CN101649068A (en) * | 2008-08-12 | 2010-02-17 | 贵州航天林泉电机有限公司 | Epoxy resin dissolving agent and preparing method thereof |
| CN102433043A (en) * | 2011-09-13 | 2012-05-02 | 天津德高化成电子材料有限公司 | Epoxy resin and silicon resin cured coating and package removing agent and preparation method thereof |
| CN104194038A (en) * | 2014-08-29 | 2014-12-10 | 浙江大学 | Epoxy resin composition, and wet-process ultrasonic degradation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《涂料工业用原材料技术标准汇编》编写组: "《涂料工业用原材料技术标准汇编》", 31 July 1983, 技术标准出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111117815A (en) * | 2019-12-31 | 2020-05-08 | 南通曜世新材料科技有限公司 | Resin dissolving solution for resin diamond wire and broken wire connection method thereof |
| CN111547725A (en) * | 2020-05-14 | 2020-08-18 | 湖南太子新材料科技有限公司 | Preparation method for extracting silicon carbide from polyurethane wrapped with silicon carbide |
| CN111660472A (en) * | 2020-06-08 | 2020-09-15 | 西安微电子技术研究所 | Method for cleaning residues in mold cavity of mold box in plastic package mold |
| CN115595133A (en) * | 2021-07-07 | 2023-01-13 | 中国石油化工股份有限公司（Cn） | Composition for dissolving plugging agent and preparation method and application thereof |
| CN114854385A (en) * | 2022-03-21 | 2022-08-05 | 中国石油化工股份有限公司 | Asphaltene dispersion inhibitor with coating shell and preparation method thereof |
| CN114854385B (en) * | 2022-03-21 | 2023-11-03 | 中国石油化工股份有限公司 | Asphaltene dispersion inhibitor with wrapping shell and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107099052B (en) | 2020-11-24 |
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Application publication date: 20170829 Assignee: Guangxi Yifang Environmental Protection Technology Co.,Ltd. Assignor: GUILIN University OF ELECTRONIC TECHNOLOGY Contract record no.: X2023980045358 Denomination of invention: A Curing Epoxy Resin Dissolving Agent and Its Application Method Granted publication date: 20201124 License type: Common License Record date: 20231101 |
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