CN105820784A - Flame-retardant epoxy resin pouring sealant - Google Patents
Flame-retardant epoxy resin pouring sealant Download PDFInfo
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- CN105820784A CN105820784A CN201610263356.3A CN201610263356A CN105820784A CN 105820784 A CN105820784 A CN 105820784A CN 201610263356 A CN201610263356 A CN 201610263356A CN 105820784 A CN105820784 A CN 105820784A
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- epoxy resin
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- silica fume
- casting glue
- fire retarding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a flame-retardant epoxy resin pouring sealant which is prepared from the following components: polyphenol type glycidyl ether epoxy resin, methyl silicone resin, glycidyl ester epoxy resin, mica powder, triepoxypropane propyl ether, diepoxypropane ethyl ether, aluminum hydroxide powder, adjuvant, a mixture of triethylene tetramine diamino diphenylmethane and silica fume. As production processes and formulas are improved, the prepared flame-retardant epoxy resin pouring sealant is relatively low in viscosity, good in infiltration property, good in flowability, easy to dye, low in curing heat radiation and small in shrinkage rate, a cured product is smooth and bright in surface, good in hardness, excellent in insulating property, excellent in mechanical property, good in heat resistance, small in water absorption and thermal expansion coefficient and good in flame retardancy, heat conduction, high-low temperature alternating resistance and weather resistance, the flame retardancy of the cured product is UI94-Vo grade, and the flame-retardant epoxy resin pouring sealant is applicable to pouring sealing of various IC plastic membrane capacitors and transformers and insulation, dampproof pouring sealing and confidential pouring sealing of other electronic components.
Description
Technical field
The present invention relates to casting glue field, particularly relate to a kind of fire retarding epoxide resin casting glue.
Background technology
Epoxy resin is a kind of thermosetting resin, has excellent chemical stability, corrosion resistance, and its adhesive property is good, mechanical strength is high, electrical insulating property is strong, industrially it is widely used, especially in terms of the cast, encapsulation of the device such as electronic device, transformator, is widely used especially.But, pure epoxy resin has high cross-linked structure, thus there is the shortcomings such as matter is crisp, fatiguability, thermostability are the best, toughness is poor, and epoxy resin embedding adhesive overcomes disadvantages mentioned above, in the actual application of electronic device embedding the most extensive, but existing epoxy resin embedding adhesive exists the shortcomings such as hardness is low, thermal deformation is poor, proof voltage performance is weak, fire resistance is poor, need existing epoxy resin embedding adhesive is improved.
Summary of the invention
It is an object of the invention to provide a kind of fire retarding epoxide resin casting glue.
The present invention is achieved through the following technical solutions:
A kind of fire retarding epoxide resin casting glue, it is made up of following component by weight, many phenolic tetraglycidel ether epoxy resin 102 parts, methyl silicon resin 3 parts, glycidyl ester type epoxy resin 20 parts, mica powder 0.2 part, three expoxy propane propyl ether 2 parts, diepoxy propane ethylether 1.5 parts, aluminium-hydroxide powder 1.1 parts, adjuvant 1 part, triethylene tetramine and two 16 parts of amido diphenyl-methane mixture, SILICA FUME 2 parts.
Further, described many phenolic tetraglycidel ether epoxy resin and glycidyl ester type epoxy resin process through premix: many phenolic tetraglycidel ether epoxy resin and glycidyl ester type epoxy resin are mixed and put in reactor, stirring 30 minutes at 56 DEG C, mixing speed is 800r/min.
Further, described mica powder is to be mixed by 3:1 mass ratio with without the mica powder of calcining by through low temperature calcination mica powder, it can improve heatproof and decay resistance, mica powder calcining heat through low temperature calcination is 150 DEG C, calcination time is 40 minutes, and the granularity of described mica powder is 450-480 mesh.
Further, the granularity of described aluminium-hydroxide powder is 450-480 mesh, and aluminium-hydroxide powder is through pretreatment, is put into by aluminium-hydroxide powder in the caprylic acid solution that mass fraction is 0.55%, after soaking 15 minutes, filters, is dried.
Further, described adjuvant is made up of following component in percentage terms: attapulgite modified 20%, isocyanates 80%, and the two is mixed under 4-8 DEG C of low temperature；Described attapulgite modified it is made up of following methods: first soak attapulgite 2-3 hour with 1.5% mass concentration sodium hydroxide solution, filter, be dried, then with 280 DEG C calcining 0.5 hour after, attapulgite is put in clear water soak 15 minutes, filter, placing into mass concentration is to soak after 10 minutes in 6.5% hydrogen peroxide solution, and filtration drying is crushed to 300-350 mesh,, the shock resistance flexibility after casting glue solidifies can be improved by adding adjuvant.
Further, in described triethylene tetramine and two amido diphenyl-methane mixture, triethylene tetramine and two amido diphenyl-methanes are mixed by 2:3 mass ratio.
Further, described SILICA FUME is to be mixed by 1:1 mass ratio with without the SILICA FUME of calcining by through high-temperature calcination SILICA FUME, SILICA FUME calcining heat through high-temperature calcination is 450 DEG C, and calcination time is 10 minutes, and the granularity of described SILICA FUME is 450-480 mesh.
A kind of preparation method of fire retarding epoxide resin casting glue, it is made up of following making step:
1) the many phenolic tetraglycidel ether epoxy resin processed through premix and glycidyl ester type epoxy resin mixture being heated to 60 DEG C in a kettle., add methyl silicon resin, be stirred, mixing speed is 350-380r/min；
2) until temperature arrive 70 DEG C time, add mica powder, three expoxy propane propyl ethers, diepoxy propane ethylether, be continuously heating to after be incubated 1-2 hour 200-220 DEG C stir and add aluminium-hydroxide powder carry out react 4-6 hour；
3) adding adjuvant, triethylene tetramine and two amido diphenyl-methane mixture, SILICA FUME in reactor, control temperature to 80-85 DEG C, pressure is 7-8MPa, and is stirred, and mixing speed is 450-500r/min, keeps 8-10 hour,.
Temperature during fire retarding epoxide resin casting glue of the present invention solidification is 60 DEG C, and hardening time is 1.85 hours.
The invention has the beneficial effects as follows, compared with prior art:
The present invention is by improving production technology and formula, and the fire retarding epoxide resin casting glue of preparation, viscosity is relatively low, infiltration property is good, and mobility is good, easy dyeing；In solidification process, will not produce layering, curing rate is fast；Curing exotherm amount is low, and shrinkage factor is little；Solidfied material surfacing, light, hardness are high, and solidfied material excellent insulation performance, anti-flammability reach UI94-V0 level, good mechanical performance, and heat-resist, water absorption and thermal coefficient of expansion are little；Solidfied material is fire-retardant, heat conduction, high-low temperature resistant alternation, weatherability requirement；It is applicable to all kinds of IC plastic film capacitor, the embedding of transformator and the insulation of other electronic component, moistureproof embedding and the embedding for secrecy.
Detailed description of the invention
A kind of fire retarding epoxide resin casting glue, it is made up of following component by weight, many phenolic tetraglycidel ether epoxy resin 102 parts, methyl silicon resin 3 parts, glycidyl ester type epoxy resin 20 parts, mica powder 0.2 part, three expoxy propane propyl ether 2 parts, diepoxy propane ethylether 1.5 parts, aluminium-hydroxide powder 1.1 parts, adjuvant 1 part, triethylene tetramine and two 16 parts of amido diphenyl-methane mixture, SILICA FUME 2 parts.
Further, described many phenolic tetraglycidel ether epoxy resin and glycidyl ester type epoxy resin process through premix: many phenolic tetraglycidel ether epoxy resin and glycidyl ester type epoxy resin are mixed and put in reactor, stirring 30 minutes at 56 DEG C, mixing speed is 800r/min.
Further, described mica powder is to be mixed by 3:1 mass ratio with without the mica powder of calcining by through low temperature calcination mica powder, it can improve heatproof and decay resistance, mica powder calcining heat through low temperature calcination is 150 DEG C, calcination time is 40 minutes, and the granularity of described mica powder is 450-480 mesh.
Further, the granularity of described aluminium-hydroxide powder is 450-480 mesh, and aluminium-hydroxide powder is through pretreatment, is put into by aluminium-hydroxide powder in the caprylic acid solution that mass fraction is 0.55%, after soaking 15 minutes, filters, is dried.
Further, described adjuvant is made up of following component in percentage terms: attapulgite modified 20%, isocyanates 80%, and the two is mixed under 4-8 DEG C of low temperature；Described attapulgite modified it is made up of following methods: first soak attapulgite 2-3 hour with 1.5% mass concentration sodium hydroxide solution, filter, be dried, then with 280 DEG C calcining 0.5 hour after, attapulgite is put in clear water soak 15 minutes, filter, placing into mass concentration is to soak after 10 minutes in 6.5% hydrogen peroxide solution, and filtration drying is crushed to 300-350 mesh,, the shock resistance flexibility after casting glue solidifies can be improved by adding adjuvant.
Further, in described triethylene tetramine and two amido diphenyl-methane mixture, triethylene tetramine and two amido diphenyl-methanes are mixed by 2:3 mass ratio.
Further, described SILICA FUME is to be mixed by 1:1 mass ratio with without the SILICA FUME of calcining by through high-temperature calcination SILICA FUME, SILICA FUME calcining heat through high-temperature calcination is 450 DEG C, and calcination time is 10 minutes, and the granularity of described SILICA FUME is 450-480 mesh.
A kind of preparation method of fire retarding epoxide resin casting glue, it is made up of following making step:
1) the many phenolic tetraglycidel ether epoxy resin processed through premix and glycidyl ester type epoxy resin mixture being heated to 60 DEG C in a kettle., add methyl silicon resin, be stirred, mixing speed is 350-380r/min；
2) until temperature arrive 70 DEG C time, add mica powder, three expoxy propane propyl ethers, diepoxy propane ethylether, be continuously heating to after be incubated 1-2 hour 200-220 DEG C stir and add aluminium-hydroxide powder carry out react 4-6 hour；
3) adding adjuvant, triethylene tetramine and two amido diphenyl-methane mixture, SILICA FUME in reactor, control temperature to 80-85 DEG C, pressure is 7-8MPa, and is stirred, and mixing speed is 450-500r/min, keeps 8-10 hour,.
Temperature during fire retarding epoxide resin casting glue of the present invention solidification is 60 DEG C, and hardening time is 1.85 hours.
Fire retarding epoxide resin casting glue performance parameter of the present invention:
| Viscosity CP/S | Proportion g/cm | Pot-life (moon) |
| 6.5×10³ | 1.053 | 8 |
Table 1
Condensate performance parameter:
| Shore hardness (25 DEG C) shore-D | Water absorption rate %(24h) | Heat distortion temperature 0.45MPa/ DEG C | Proof voltage KV/mm |
| 96±3 | ＜ 0.1 | 138-156 | 8-10 |
Table 2
As can be seen from Table 1 and Table 2, this fire retarding epoxide resin casting glue superior performance.
Claims (8)
1. a fire retarding epoxide resin casting glue, it is characterized in that, it is made up of following component by weight, many phenolic tetraglycidel ether epoxy resin 102 parts, methyl silicon resin 3 parts, glycidyl ester type epoxy resin 20 parts, mica powder 0.2 part, three expoxy propane propyl ether 2 parts, diepoxy propane ethylether 1.5 parts, aluminium-hydroxide powder 1.1 parts, adjuvant 1 part, triethylene tetramine and two 16 parts of amido diphenyl-methane mixture, SILICA FUME 2 parts.
A kind of fire retarding epoxide resin casting glue the most according to claim 1, it is characterized in that, described many phenolic tetraglycidel ether epoxy resin and glycidyl ester type epoxy resin process through premix: many phenolic tetraglycidel ether epoxy resin and glycidyl ester type epoxy resin are mixed and put in reactor, stirring 30 minutes at 56 DEG C, mixing speed is 800r/min.
A kind of fire retarding epoxide resin casting glue the most according to claim 1, it is characterized in that, described mica powder is to be mixed by 3:1 mass ratio with without the mica powder of calcining by through low temperature calcination mica powder, mica powder calcining heat through low temperature calcination is 150 DEG C, calcination time is 40 minutes, and the granularity of described mica powder is 450-480 mesh.
A kind of fire retarding epoxide resin casting glue the most according to claim 1, it is characterized in that, the granularity of described aluminium-hydroxide powder is 450-480 mesh, and aluminium-hydroxide powder is through pretreatment, aluminium-hydroxide powder is put in the caprylic acid solution that mass fraction is 0.55%, after soaking 15 minutes, filter, be dried.
A kind of fire retarding epoxide resin casting glue the most according to claim 1, it is characterised in that described adjuvant is made up of following component in percentage terms: attapulgite modified 20%, isocyanates 80%, and the two is mixed under 4-8 DEG C of low temperature；Described attapulgite modified it is made up of following methods: first soak attapulgite 2-3 hour with 1.5% mass concentration sodium hydroxide solution, filter, it is dried, after again with 280 DEG C of calcinings 0.5 hour, attapulgite is put in clear water and soak 15 minutes, filter, placing into mass concentration is to soak after 10 minutes in 6.5% hydrogen peroxide solution, filtration drying, is crushed to 300-350 mesh,.
A kind of fire retarding epoxide resin casting glue the most according to claim 1, it is characterised in that in described triethylene tetramine and two amido diphenyl-methane mixture, triethylene tetramine and two amido diphenyl-methanes are mixed by 2:3 mass ratio.
A kind of fire retarding epoxide resin casting glue the most according to claim 1, it is characterized in that, described SILICA FUME is to be mixed by 1:1 mass ratio with without the SILICA FUME of calcining by through high-temperature calcination SILICA FUME, SILICA FUME calcining heat through high-temperature calcination is 450 DEG C, calcination time is 10 minutes, and the granularity of described SILICA FUME is 450-480 mesh.
8. according to the preparation method of a kind of fire retarding epoxide resin casting glue described in any one of claim 1-7, it is characterised in that it is made up of following making step:
1) the many phenolic tetraglycidel ether epoxy resin processed through premix and glycidyl ester type epoxy resin mixture being heated to 60 DEG C in a kettle., add methyl silicon resin, be stirred, mixing speed is 350-380r/min；
2) until temperature arrive 70 DEG C time, add mica powder, three expoxy propane propyl ethers, diepoxy propane ethylether, be continuously heating to after be incubated 1-2 hour 200-220 DEG C stir and add aluminium-hydroxide powder carry out react 4-6 hour；
3) adding adjuvant, triethylene tetramine and two amido diphenyl-methane mixture, SILICA FUME in reactor, control temperature to 80-85 DEG C, pressure is 7-8MPa, and is stirred, and mixing speed is 450-500r/min, keeps 8-10 hour,.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610263356.3A CN105820784A (en) | 2016-04-26 | 2016-04-26 | Flame-retardant epoxy resin pouring sealant |
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| CN201610263356.3A CN105820784A (en) | 2016-04-26 | 2016-04-26 | Flame-retardant epoxy resin pouring sealant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502283A (en) * | 2017-08-18 | 2017-12-22 | 佛山市永恒达新材料科技有限公司 | A kind of preparation method of fire-proof plate binder in use for jointing |
Citations (5)
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| CN101851480A (en) * | 2010-05-11 | 2010-10-06 | 华烁科技股份有限公司 | Halogen-free and phosphorous-free flame-retardant synthetic resin adhesive used for flexible copper clad laminate |
| CN102516914A (en) * | 2011-11-21 | 2012-06-27 | 烟台德邦电子材料有限公司 | Halogen-free flame-retardant epoxy resin electronic pouring sealant |
| CN102942889A (en) * | 2012-11-29 | 2013-02-27 | 宜兴市江南药用化工厂 | Low-halogen epoxy potting adhesive, and preparation method and application thereof |
| CN103361019A (en) * | 2013-08-05 | 2013-10-23 | 安徽康瑞鑫电子科技有限公司 | Epoxy resin pouring sealant |
| CN104152093A (en) * | 2014-08-16 | 2014-11-19 | 烟台德邦科技有限公司 | Flame-retardant heat-conducting double-component epoxy resin pouring sealant and preparation method thereof |
-
2016
- 2016-04-26 CN CN201610263356.3A patent/CN105820784A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851480A (en) * | 2010-05-11 | 2010-10-06 | 华烁科技股份有限公司 | Halogen-free and phosphorous-free flame-retardant synthetic resin adhesive used for flexible copper clad laminate |
| CN102516914A (en) * | 2011-11-21 | 2012-06-27 | 烟台德邦电子材料有限公司 | Halogen-free flame-retardant epoxy resin electronic pouring sealant |
| CN102942889A (en) * | 2012-11-29 | 2013-02-27 | 宜兴市江南药用化工厂 | Low-halogen epoxy potting adhesive, and preparation method and application thereof |
| CN103361019A (en) * | 2013-08-05 | 2013-10-23 | 安徽康瑞鑫电子科技有限公司 | Epoxy resin pouring sealant |
| CN104152093A (en) * | 2014-08-16 | 2014-11-19 | 烟台德邦科技有限公司 | Flame-retardant heat-conducting double-component epoxy resin pouring sealant and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502283A (en) * | 2017-08-18 | 2017-12-22 | 佛山市永恒达新材料科技有限公司 | A kind of preparation method of fire-proof plate binder in use for jointing |
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