CN107099052B - Curing epoxy resin dissolving agent and application method thereof - Google Patents
Curing epoxy resin dissolving agent and application method thereof Download PDFInfo
- Publication number
- CN107099052B CN107099052B CN201710274180.6A CN201710274180A CN107099052B CN 107099052 B CN107099052 B CN 107099052B CN 201710274180 A CN201710274180 A CN 201710274180A CN 107099052 B CN107099052 B CN 107099052B
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- CN
- China
- Prior art keywords
- epoxy resin
- dissolving agent
- curing epoxy
- sodium hydroxide
- resin dissolving
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 49
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 49
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 26
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 9
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000003054 catalyst Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000004100 electronic packaging Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 4
- 238000002474 experimental method Methods 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
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 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
- 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
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 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)
- Epoxy Resins (AREA)
- Encapsulation Of And Coatings For Semiconductor Or Solid State Devices (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention provides a curing epoxy resin dissolving agent which is formed by mixing diethylenetriamine, toluene, dichloromethane, ethylene glycol monomethyl ether and sodium hydroxide. The preparation process of the curing epoxy resin dissolving agent comprises the following steps: sequentially adding sodium hydroxide, ethylene glycol monomethyl ether, diethylenetriamine, toluene and dichloromethane, and then stirring until the sodium hydroxide is completely dissolved to obtain a cured epoxy resin dissolving agent; and (3) a cured epoxy resin dissolving process: and (3) putting the electronic device sample containing the cured epoxy resin into a cured epoxy resin dissolving agent for dissolving, and then cleaning with clear water. The invention has the following advantages: 1. the cured epoxy resin for packaging the electronic device can be dissolved, and the metal device in the electronic device is not damaged; 2. the preparation process is simple and can be used for mass preparation; 3. good application effect and high dissolution speed. Therefore, the invention has wide application prospect in the fields of small electronic packaging and epoxy resin-coated metal substrate recovery.
Description
Technical Field
The invention relates to the technical field of dissolving agents, in particular to a curing epoxy resin dissolving agent and an application method thereof.
Background
The molecular structure of the epoxy resin contains active epoxy groups, so that the epoxy resin can react with a plurality of different curing agents to generate a high polymer with a three-dimensional network structure, namely curing. The cured epoxy resin has good physical and chemical properties, and has excellent bonding strength on the surfaces of metal and nonmetal materials, good dielectric property, small deformation shrinkage rate, good product dimensional stability, high hardness and good flexibility, so the cured epoxy resin is widely applied to the fields of packaging, casting and the like of electronic devices. The advantages make it difficult to extract the metal or recyclable material from the epoxy resin package, which runs counter to the strategy of sustainable development in our country. Therefore, it is necessary to produce a solution capable of dissolving the cured epoxy resin.
There are two main types of epoxy resin dissolving agents currently studied: firstly, under the acidic condition, the epoxy resin is dissolved, as in the Chinese patent CN200810303667.3, the method uses a large amount of formic acid and sulfuric acid, and has greater corrosivity to metal equipment; and secondly, organic solvents, such as Chinese patent CN201310456230.4, the method needs to be refluxed and stirred for 0.5 to 1 hour, and the process is relatively complex and long in time.
Disclosure of Invention
The invention aims to provide a curing epoxy resin dissolving agent and an application method thereof, which realize the purposes of reducing the corrosion to other metal devices and improving the dissolving rate by adopting alkaline solution as a condition.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
calculated by volume: the epoxy resin dissolving agent is prepared by mixing 1 to 20 parts of diethylenetriamine, 5 to 20 parts of toluene, 20 to 40 parts of methylene dichloride, 20 to 60 parts of ethylene glycol monomethyl ether and 0.5 to 1.5 parts of sodium hydroxide.
Preferably, the epoxy resin dissolving agent consists of 5 parts of diethylenetriamine, 19 parts of toluene, 25 parts of dichloromethane, 40 parts of ethylene glycol monomethyl ether and 1 part of sodium hydroxide.
Sequentially adding sodium hydroxide, ethylene glycol monomethyl ether, diethylenetriamine, toluene and dichloromethane, stirring in a rotor stirrer for 30min until the sodium hydroxide is completely dissolved to obtain the cured epoxy resin dissolving agent.
Adding the cured epoxy resin dissolving agent into an oil bath pot, adjusting the temperature to 130 ℃, then putting the electronic device sample containing the cured epoxy resin into the cured epoxy resin dissolving agent, taking out the sample after 10min, and cleaning the sample with clear water.
The results of the performance analysis of the prior art solution cured epoxy resin are shown in the following table:
the results of the experiments show that the No. 4 dissolving agent has the most excellent effect, but has certain corrosiveness to metals under acidic conditions.
The performance analysis of the dissolving and curing epoxy resin is detected by experiments, and the results are as follows:
| name of the formulation | A | II | III | Fourthly |
| Dichloromethane (wt%) | 20 | 25 | 25 | 30 |
| Diethylenetriamine (wt%) | 15 | 10 | 5 | 10 |
| Toluene (wt%) | 20 | 20 | 20 | 10 |
| Ethylene glycol methyl ether (wt%) | 45 | 45 | 40 | 50 |
| Sodium hydroxide (g) | 2 | 2 | 2 | 2 |
| Temperature (. degree.C.) | 110 | 110 | 110 | 110 |
| Dissolution Rate(s) | 18 | 16 | 10 | 12 |
Experimental results show that the time for dissolving and curing the epoxy resin is 10-18 minutes, and the dissolving rate is far superior to that of the prior art.
The corrosion condition of the cured epoxy resin dissolving agent on copper in an electronic device is detected by experiments, and the results are as follows:
the experimental result shows that the cured epoxy resin dissolving agent provided by the invention does not corrode copper in electronic devices.
Therefore, compared with the prior art, the invention has the following advantages:
1. the curing epoxy resin for packaging the electronic device can be well dissolved, and the metal device in the electronic device can not be damaged;
2. the preparation process is simple, complex operation is not needed, a sample is added into the solution, and mass preparation can be carried out as long as raw materials are sufficient;
3. the application effect is good, the dissolving speed is high, and the solution can be completely dissolved only after 10 min.
Therefore, compared with the prior art, the epoxy resin dissolving and curing agent can dissolve and cure the epoxy resin in a targeted manner without influencing internal metal devices, improves the dissolving rate, and has wide application prospect in the field of electronic device packaging and recycling.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Examples
1. The preparation process of the curing epoxy resin dissolving agent comprises the following steps:
taking a 50ml beaker, adding 2g of sodium hydroxide, 20ml of ethylene glycol monomethyl ether, 2.5ml of diethylenetriamine, 10ml of toluene and 12.5ml of dichloromethane in sequence, stirring in a rotor stirrer for 30min until the sodium hydroxide is completely dissolved to obtain a solidified epoxy resin dissolving agent;
2. and (3) a cured epoxy resin dissolving process:
adding the cured epoxy resin dissolving agent into an oil bath pot, adjusting the temperature to 130 ℃, then putting the electronic device sample containing the cured epoxy resin into the cured epoxy resin dissolving agent, taking out the sample after 10min, and cleaning the sample with clear water.
Claims (2)
1. A curing epoxy resin dissolving agent is characterized in that: the catalyst is prepared by mixing 1 to 20 parts of diethylenetriamine, 5 to 20 parts of toluene, 20 to 40 parts of dichloromethane, 20 to 60 parts of ethylene glycol monomethyl ether and 0.5 to 1.5 parts of sodium hydroxide.
2. The method for applying a solvent for cured epoxy resin according to claim 1, comprising the steps of:
adding sodium hydroxide, ethylene glycol monomethyl ether, diethylenetriamine, toluene and dichloromethane in sequence in the preparation process of the curing epoxy resin dissolving agent in the step (1), and then stirring until the sodium hydroxide is completely dissolved to obtain the curing epoxy resin dissolving agent;
and (2) adding a curing epoxy resin dissolving agent into the oil bath pot, adjusting the temperature to 130 ℃, then putting the curing epoxy resin sample into the curing epoxy resin dissolving agent, putting the curing epoxy resin sample into the oil bath pot, taking out the sample after the curing epoxy resin is dissolved, and cleaning the sample 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 CN107099052A (en) | 2017-08-29 |
| CN107099052B true CN107099052B (en) | 2020-11-24 |
Family
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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 |
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| CN (1) | CN107099052B (en) |
Families Citing this family (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 |
| CN111660472B (en) * | 2020-06-08 | 2022-08-30 | 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 |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194038A (en) * | 2014-08-29 | 2014-12-10 | 浙江大学 | Epoxy resin composition, and wet-process ultrasonic degradation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH04306272A (en) * | 1991-04-03 | 1992-10-29 | Majitsuku Man Kk | Epoxy resin remover |
| CN101649068B (en) * | 2008-08-12 | 2011-12-14 | 贵州航天林泉电机有限公司 | Epoxy resin dissolving agent and preparing method thereof |
| CN102433043B (en) * | 2011-09-13 | 2013-06-12 | 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104194038A (en) * | 2014-08-29 | 2014-12-10 | 浙江大学 | Epoxy resin composition, and wet-process ultrasonic degradation method and application thereof |
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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 |