CN106010399A - Halogen-free flame retardation electronic pouring sealant - Google Patents

Halogen-free flame retardation electronic pouring sealant Download PDF

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Publication number
CN106010399A
CN106010399A CN201610373118.8A CN201610373118A CN106010399A CN 106010399 A CN106010399 A CN 106010399A CN 201610373118 A CN201610373118 A CN 201610373118A CN 106010399 A CN106010399 A CN 106010399A
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CN
China
Prior art keywords
halogen
parts
free flame
casting glue
resistant electronic
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.)
Pending
Application number
CN201610373118.8A
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Chinese (zh)
Inventor
蔡小连
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Kuikeli Electronic Technology Co Ltd
Original Assignee
Suzhou Kuikeli Electronic Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Suzhou Kuikeli Electronic Technology Co Ltd filed Critical Suzhou Kuikeli Electronic Technology Co Ltd
Priority to CN201610373118.8A priority Critical patent/CN106010399A/en
Publication of CN106010399A publication Critical patent/CN106010399A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • C08K2003/164Aluminum halide, e.g. aluminium chloride
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • C08K2003/166Magnesium halide, e.g. magnesium chloride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention discloses a halogen-free flame retardation electronic pouring sealant. The halogen-free flame retardation electronic pouring sealant comprises nano-modified flame retardation epoxy resin, a filler, a curing agent, a promoter, a reaction diluent, a plasticizer and a silane coupling agent. The halogen-free flame retardation electronic pouring sealant has the advantages of excellent flame retardation property, high temperature resistance, excellent physical performances, high refractive index, environmental protection, high safety, easiness in operation, no addition of extra flame retardants, and cost reduction.

Description

Halogen-free flame-resistant electronic casting glue
Technical field
The present invention relates to a kind of electron pouring sealant, particularly relate to a kind of halogen-free flame-resistant electronic casting glue.
Background technology
Along with America and Europe's raising day by day to environmental requirement, the related substances affecting human security and environment is used and carries out Strict regulations, and formulated " about being limited in electronic and electrical equipment the instruction using some harmful components " in 2006, should The material of standard Main Specification electric equipment products and technological standards, be allowed to advantageously in health and environmental conservation.Should Standard is designed into the application of a lot of material, is extremely difficult to this requirement, has a strong impact on while meeting electric property requirement The outlet of China's part components and parts produces, so the material of Halogen casting glue selects and technologic improvement is extremely urgent.
At present, in terms of halogen-free flameproof casting glue, there are some research reports though domestic, but lay particular stress on interpolation nothing in component more Halogen fire retardant, halogen-free flame retardants can separate out over time, reduces the fire resistance of casting glue.Chinese patent CN102618208 is situated between Continued a kind of halogen-free flame-retarded heat-conducting organic silicon electronic fluid sealant, but does not has high temperature resistant, ageing-resistant function, it is impossible to meets outdoor electricity The embeddings such as sub-components and parts.Chinese patent CN102942889 describes a kind of low halogen epoxy pouring sealant and its preparation method and application, Use low halogen epoxy resin, low halogen epoxide diluent, although can reduce the halogen element content of casting glue, but to environment the most not Enough environmental protection, and do not mention the performances such as high temperature resistant.
Summary of the invention
For above-mentioned weak point, it is an object of the invention to provide a kind of halogen-free flame-resistant electronic casting glue, be characterized in: Not only there is excellent anti-flammability, heat-resisting quantity, excellent physical property and high index of refraction, and Environmental Safety, easily operated, It is not required to add extra fire retardant, reduces the advantages such as cost.
Technical scheme is summarized as follows:
Halogen-free flame-resistant electronic casting glue, it is characterised in that include the material of following weight portion:
Nano modification fire retarding epoxide resin 20 ~ 30 parts;
Filler 5~18 parts;
Firming agent 10~25 parts;
Accelerator 3~15 parts;
Reaction diluent 1~3 parts;
Plasticizer 5~14 parts;
Silane coupler 1~5 parts.
Preferably, the preparation method of described nano modification fire retarding epoxide resin is: S1 is by solubility magnesium salt, soluble aluminum Salt and water are mixed to get mixed solution, then are added drop-wise in sodium dodecyl benzene sulfonate aqueous solution by mixed solution, and keep reaction The pH value of system is 8~13, drip complete after through ageing, be filtrated to get nano modification magnesium-aluminum composite flame-retardant agent;Described mixing Metal ion in solution total concentration is 0.05~2mol/L, and magnalium mol ratio is 2:1;Epoxy resin and described nanometer are changed by S2 Property magnesium-aluminum composite flame-retardant agent blending and modifying prepares nano modification fire retarding epoxide resin.
Preferably, described solubility magnesium salt is magnesium nitrate and/or magnesium chloride, and aluminum soluble salt is aluminum nitrate and/or chlorine Change aluminum.
Preferably, described reaction diluent is selected from, but not limited to, organophosphorus ester, aliphatic glycidyl ether, alicyclic One or more in glycidyl ether, aromatic glycidyl ether, when for time two or more, the ratio of each component is equal portions or Other ratio.
Preferably, described accelerator selected from 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole and 1-cyanoethyl-2-ethyl- One in 4-methylimidazole or its compound.
Preferably, described firming agent faces phthalate anhydride for methyl tetrahydrochysene and methyl hexahydro is faced in phthalate anhydride One or both compound.
Preferably, described filler is selected from aluminium hydroxide and aluminium oxide, silicon dioxide, titanium dioxide, mica powder, charcoal In black, active micro silicon powder silicon powder, blanc fixe one or more.
Preferably, described silane coupler is β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-contracting In water glycerol epoxide propyl trimethoxy silicane, γ mercaptopropyitrimethoxy silane, gamma-aminopropyl-triethoxy-silane A kind of or the most several mixture.
The invention has the beneficial effects as follows:
The present invention is with solubility magnesium salt, aluminium salt as raw material, and dodecylbenzene sodium sulfonate, as intercalator, forms sheet interlayer spacing for receiving The other layer structure of meter level, is more beneficial for the raising of its dispersive property.This nano modification magnesium-aluminum composite flame-retardant agent is efficient halogen-free Fire retardant, the less pollution caused for environment, flame retardant effect highlights, and adds nano modification magnesium-aluminum composite flame-retardant agent, permissible Reduce the viscosity of epoxy resin, make the casting glue good fluidity prepared, be difficult to make moist, water absorption, weatherability and fire-retardant Property.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, to make those skilled in the art with reference to description Word can be implemented according to this.
Embodiment 1
A kind of halogen-free flame-resistant electronic casting glue, including the material of following weight portion: nano modification fire retarding epoxide resin 20 parts;Filler 5 parts;10 parts of firming agent;Accelerator 3 parts;Reaction diluent 1 part;Plasticizer 5~14 parts;Silane coupler 1~5 parts.
Embodiment 2
A kind of halogen-free flame-resistant electronic casting glue, including the material of following weight portion: nano modification fire retarding epoxide resin 25 parts;Filler 5~18 parts;20 parts of firming agent;Accelerator 10 parts;Reaction diluent 2 parts;Plasticizer 8 parts;Silane coupler 3 parts.
Embodiment 3
A kind of halogen-free flame-resistant electronic casting glue, including the material of following weight portion: nano modification fire retarding epoxide resin 30 parts;Filler 18 parts;25 parts of firming agent;Accelerator 15 parts;Reaction diluent 3 parts;Plasticizer 14 parts;Silane coupler 5 parts.
Comparative example 1
A kind of halogen-free flame-resistant electronic casting glue, including the material of following weight portion: nano modification fire retarding epoxide resin 12 parts;Filler 4 parts;6 parts of firming agent;Accelerator 2 parts;Reaction diluent 0.5 part;Plasticizer 4 parts;Silane coupler 0.4 part.
Comparative example 2
A kind of halogen-free flame-resistant electronic casting glue, including the material of following weight portion: nano modification fire retarding epoxide resin 36 parts;Filler 19 parts;29 parts of firming agent;Accelerator 19 parts;Reaction diluent 9 parts;Plasticizer 19 parts;Silane coupler 9 parts.
Wherein, in embodiment 1 ~ 3 and comparative example 1 ~ 2, the preparation method of nano modification fire retarding epoxide resin is:
S1: magnesium nitrate, aluminum nitrate with water, are mixed to get mixed solution, then mixed solution is added drop-wise to dodecylbenzene sodium sulfonate In aqueous solution, and to keep the pH value of reaction system be 8~13, drip complete after through ageing, to be filtrated to get nano modification magnesium-aluminum multiple Close fire retardant;In described mixed solution, metal ion total concentration is 0.05~2mol/L, and magnalium mol ratio is 2:1;
S2: epoxy resin and described nano modification magnesium-aluminum composite flame-retardant agent blending and modifying are prepared nano modification flame retardant epoxy Resin.
Comparative example 3
A kind of halogen-free flame-resistant electronic casting glue, including the material of following weight portion: epoxy resin 20 parts;Filler 5 parts;Firming agent 10 Part;Accelerator 3 parts;Reaction diluent 1 part;Plasticizer 5~14 parts;Silane coupler 1~5 parts.
Following table is the test result of embodiment and comparative example
Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2 Comparative example 3
Viscosity (mPa.s) 5600 6550 7020 5820 5940 8600
Shore A hardness 67 69 70 78 89 82
Fire-retardant rank (UL94) V-0 V-0 V-0 V-0 V-0 V-1
Although embodiment of the present invention are disclosed as above, but it is not restricted in description and embodiment listed Using, it can be applied to various applicable the field of the invention completely, for those skilled in the art, and can be easily Realizing other amendment, therefore under the general concept limited without departing substantially from claim and equivalency range, the present invention does not limit In specific details.

Claims (8)

1. a halogen-free flame-resistant electronic casting glue, it is characterised in that include the material of following weight portion:
Nano modification fire retarding epoxide resin 20 ~ 30 parts;
Filler 5~18 parts;
Firming agent 10~25 parts;
Accelerator 3~15 parts;
Reaction diluent 1~3 parts;
Plasticizer 5~14 parts;
Silane coupler 1~5 parts.
2. halogen-free flame-resistant electronic casting glue as claimed in claim 1, it is characterised in that described nano modification fire retarding epoxide resin Preparation method be: solubility magnesium salt, aluminum soluble salt and water are mixed to get mixed solution by S1, then are added drop-wise to by mixed solution In sodium dodecyl benzene sulfonate aqueous solution, and to keep the pH value of reaction system be 8~13, drip complete after through ageing, filter To nano modification magnesium-aluminum composite flame-retardant agent;In described mixed solution, metal ion total concentration is 0.05~2mol/L, and magnalium rubs That ratio is 2:1;S2 is by epoxy resin and that described nano modification magnesium-aluminum composite flame-retardant agent blending and modifying prepares nano modification is fire-retardant Epoxy resin.
3. halogen-free flame-resistant electronic casting glue as claimed in claim 2, it is characterised in that described solubility magnesium salt is magnesium nitrate And/or magnesium chloride, aluminum soluble salt is aluminum nitrate and/or aluminum chloride.
4. halogen-free flame-resistant electronic casting glue as claimed in claim 1, it is characterised in that described reaction diluent is selected from but does not limits One or many in organophosphorus ester, aliphatic glycidyl ether, cycloaliphatc glycidyl ether, aromatic glycidyl ether Kind, when for time two or more, the ratio of each component is equal portions or other ratio.
5. halogen-free flame-resistant electronic casting glue as claimed in claim 1, it is characterised in that described accelerator is selected from 2-ethyl miaow One in azoles, 2-ethyl-4-methylimidazole and 1-cyanoethyl-2-ethyl-4-methylimidazole or its compound.
6. halogen-free flame-resistant electronic casting glue as claimed in claim 1, it is characterised in that described firming agent is to face for methyl tetrahydrochysene Phthalate anhydride and methyl hexahydro face one or both the compound in phthalate anhydride.
7. halogen-free flame-resistant electronic casting glue as claimed in claim 1, it is characterised in that described filler selected from aluminium hydroxide and In aluminium oxide, silicon dioxide, titanium dioxide, mica powder, white carbon black, active micro silicon powder silicon powder, blanc fixe one or more.
8. halogen-free flame-resistant electronic casting glue as claimed in claim 1, it is characterised in that described silane coupler be β-(3, 4-epoxycyclohexyl) ethyl trimethoxy silane, γ-glycidoxypropyltrimewasxysilane, γ-mercaptopropyi A kind of or the most several mixture in trimethoxy silane, gamma-aminopropyl-triethoxy-silane.
CN201610373118.8A 2016-05-31 2016-05-31 Halogen-free flame retardation electronic pouring sealant Pending CN106010399A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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CN106010399A true CN106010399A (en) 2016-10-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018121048A1 (en) * 2016-12-27 2018-07-05 苏州兴创源新材料科技有限公司 Heat-resistant packaging adhesive for high-power led and manufacturing method thereof
CN112852380A (en) * 2021-01-18 2021-05-28 竹山县秦巴钡盐有限公司 Barium sulfate electronic pouring sealant and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104789177A (en) * 2015-04-08 2015-07-22 浙江大学 Nano-modified flame-retardant epoxy electronic pouring sealant and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104789177A (en) * 2015-04-08 2015-07-22 浙江大学 Nano-modified flame-retardant epoxy electronic pouring sealant and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018121048A1 (en) * 2016-12-27 2018-07-05 苏州兴创源新材料科技有限公司 Heat-resistant packaging adhesive for high-power led and manufacturing method thereof
CN112852380A (en) * 2021-01-18 2021-05-28 竹山县秦巴钡盐有限公司 Barium sulfate electronic pouring sealant and preparation method and application thereof
CN112852380B (en) * 2021-01-18 2022-02-18 竹山县秦巴钡盐有限公司 Barium sulfate electronic pouring sealant and preparation method and application thereof

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Application publication date: 20161012