CN102766427A - Epoxy resin optical fiber adhesive glue doped by nano ultraviolet absorbing agent - Google Patents

Epoxy resin optical fiber adhesive glue doped by nano ultraviolet absorbing agent Download PDF

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Publication number
CN102766427A
CN102766427A CN201210293451XA CN201210293451A CN102766427A CN 102766427 A CN102766427 A CN 102766427A CN 201210293451X A CN201210293451X A CN 201210293451XA CN 201210293451 A CN201210293451 A CN 201210293451A CN 102766427 A CN102766427 A CN 102766427A
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CN
China
Prior art keywords
optical fiber
adhesive glue
epoxy resin
absorbing agent
component
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Pending
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CN201210293451XA
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Chinese (zh)
Inventor
曹祥来
孔庆茹
乔毅
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SHANGHAI ZHONGXIN YUXIANG CHEMICAL CO Ltd
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SHANGHAI ZHONGXIN YUXIANG CHEMICAL CO Ltd
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Priority to CN201210293451XA priority Critical patent/CN102766427A/en
Publication of CN102766427A publication Critical patent/CN102766427A/en
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Abstract

The invention relates to epoxy resin optical fiber adhesive glue doped by a nano ultraviolet absorbing agent. The optical fiber adhesive glue is composed of a main agent A and a curing agent B, the component A and the component B are mixed based on a ratio of 1: (0.01-0.02) to be used for a construction, the component A is composed of 96.5%-97.5% of organosilicon modified cycloaliphatic epoxy resins, 2%-3.2% of flexibilizer and 0.3%-0.5% of antifoaming agents, and the component B is composed of 95% of cationic curing agent aromatic diazonium salts and 5% of nano ultraviolet absorbing agents. The optical fiber adhesive glue is transparent, good in uvioresistant aging performance, high in cohesive force, uneasy to craze, resistant to high temperature, high corrosion and low temperature, and capable of being widely applied to optical fiber optical cable connectors, optical components and optical communication by serving as a high-quality adhesive glue, besides, the preparation process is simple, the production cost is low, and the optical fiber adhesive glue is suitable for industrialization mass production.

Description

The adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue
Technical field
The present invention relates to a kind of optical fiber adhesive glue, be specifically related to the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue, its cohesive force is strong, the anti-ultraviolet ageing performance is good, bonding quality is high, can be used for fixing between optical fiber cable and the junctor.
Background technology
Opticfiber communication is one of important way of present information transmission, and it has, and capacity is big, repeater span length, good confidentiality, do not receive advantages such as EMI and saving copper material.The optical fiber tackiness agent is to be used for a kind of tackiness agent of being adhesively fixed between optical fiber cable and the junctor; Because its special use range; Therefore it is had relatively high expectations, below needing to satisfy some: cohesive force that ⑴ is stronger and persistence, can be after bonding because of the ectocine mobile phenomenon that occurs coming unstuck; ⑵ high light transmittance can not produce light conduction refraction action after the use, can not cause transmission loss; ⑶ stability is high, and high temperature resistant high erosion and low temperature resistant has good resistivity.
Common having in practical application: AB glue, thermocoagulation epoxy resin glue, ultraviolet solidification adhesive, inject thermosol and anaerobic glue etc. in advance.In recent years; Anaerobic glue obtains using more widely because of its setting rate needs curing oven soon and not; But it in use, and must use ionic catalyst to handle can solidify, if tackiness agent does not touch ionic catalyst; Then will can not solidify, and cause optical fiber to be fixed and produce piston effect.AB glue is made up of host and solidifying agent two portions, and its host adopts epoxy resin more, have with low cost, the transparency is good, advantages such as the good and complete processing maturation of mechanics and thermal property.Aromatic epoxy resin contains can absorb ultraviolet phenyl ring; Meeting oxidation flavescence after the absorption ultraviolet ray, and cycloaliphatic epoxy resin can form stiff molecule structure closely because epoxy group(ing) directly is connected on the alicyclic ring; Solidifying the back cross-linking density increases; Make the material after solidifying have higher heat-drawn wire, because of not containing phenyl ring, show good anti-UV performance and agent of low hygroscopicity in the molecular structure.
The adulterated cycloaliphatic epoxy resin optical fiber of the nanometer uv-absorbing agent adhesive glue of two-pack among the present invention; Cycloaliphatic epoxy resin is earlier through organic-silicon-modified in the one side A component; In structure, introduce the Si-O key, have more advantages such as transmittance height, heat-resistant stability is good, ultraviolet resistance is strong, water absorbability is low after the curing; Improve the anti-ultraviolet ageing performance of this optical fiber adhesive glue through adding the uv-absorbing agent nano titanium oxide in the B component on the other hand; And the photopolymerization that cation curing agent causes has advantages such as not receiving oxygen inhibition, volumetric shrinkage are little, thick film; It is bonding reliably both to have guaranteed that optical fiber cable and junctor formed; Can play again and fill up the device space and prevent effects such as high loading pressurized, make it be more suitable for being used for being adhesively fixed of optical fiber cable as high-quality adhesive glue.
Summary of the invention
The purpose of this invention is to provide a kind of transparent, the anti-ultraviolet ageing performance is good, cohesive force is strong, high temperature resistant high erosion and low temperature resistant optical fiber adhesive glue; Optical fiber, metal, glass, pottery and most plastic cement are had good sticking power, can be used as high-quality adhesive glue and be widely used in photo-fibre and light cable jointer, optical component and optical communication.
Content of the present invention is the adulterated epoxy resin optical fiber of an a kind of nanometer uv-absorbing agent adhesive glue; This adhesive glue is made up of host A and solidifying agent B two components; Through A, B component by mass ratio 1: (0.01-0.02) be used for construction after mixing, it is characterized in that each method for preparing ingredients thereof is following:
The preparation of component A: with mass percent be 96.5%~97.5% organic-silicon-modified cycloaliphatic epoxy resin, 2%~3.2% toughner and 0.3%~0.5% skimmer weighing is good in proportion, under 70-80 ℃ of condition, stir 3-4h to mixing;
The preparation of B component: with mass percent be 95% cationic solidifying agent aromatic diazo salt and 5% nanometer uv-absorbing agent weighing is good in proportion, under 70-90 ℃ of condition, stir 3-4h, mix.
Press the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue of such scheme, it is characterized in that the preparation method of described organic-silicon-modified cycloaliphatic epoxy resin is: in reaction unit, add 70%~75% epoxy resin composition, by 3; 4-epoxy cyclohexylmethyl-3; 4-epoxy cyclohexyl carbonic ether with gather [(2-Oxyranyle)-1,2-cyclohexanediol] 2-ethyl-2-(methylol)-1, ammediol ether is formed with the ratio of 3:1; Behind the heating and melting; Add 0.5%~1% catalyzer triphenyl phosphorus and 20%~30% silicone resin midbody, be warming up to 120 ℃ of reaction 4h after, the water that underpressure distillation removes the dereaction generation gets final product.
Press the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue of such scheme, it is characterized in that described silicone resin midbody is methyl phenyl silicone resin, methyl silicon resin, low phenyl methyl silicone resin, phenmethyl silicone resin, epoxy modified silicone resin, organosilicon polyester modified resin, gathers in methyl silicon resin, the amino silicone one or more.
Press the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue of such scheme, it is characterized in that described toughner is toughness reinforcing dose of organosilicon.
Press the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue of such scheme, it is characterized in that described nanometer uv-absorbing agent is that particle diameter is the titanium oxide of 16nm.
The adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent adhesive glue; This optical fiber adhesive glue has following characteristics: (1) outward appearance is a transparent liquid, no segregation, particle and gel, and light transmission is good; Can not produce light conduction refraction action after the use, avoid causing transmission loss; (2) cycloaliphatic epoxy resin after organic-silicon-modified because of introducing the Si-O key in the structure, has more advantages such as excellent transmittance, heat-resistant stability, toughness and agent of low hygroscopicity after the curing; (3) nano titanium oxide of doping trace just can have good shield effectiveness to ultraviolet region, has good anti-ultraviolet ageing performance; (4) after A, B two components are mixed by a certain percentage, under UV-irradiation, get final product fast setting, and have stronger cohesive force and persistence after solidifying; (5) shock strength>12.8 KJ/m 2, bending strength>14J, second-order transition temperature>423K; (6) thermal shock :-70 ℃ of (30min) → 100 ℃ (30min) circulations 200-300 time, no change; (7) cross twice Reflow Soldering (peak temperature: 260-265 ℃, time 10-30s), glue does not have and comes off and the xanthochromia phenomenon; (8) 85 ℃, 85% relative humidity, 100 ℃ of digestion 1h of red ink or soak at room temperature 30 days all do not have infiltration, the high-temp resisting high-humidity resisting excellent performance.
Embodiment
Further introduce the present invention through embodiment below, but embodiment can not be construed as limiting the invention.
96.5%~97.5% organic-silicon-modified cycloaliphatic epoxy resin, 2%~3.2% toughner and 0.3%~0.5% skimmer
Embodiment 1
(1) prepare organic-silicon-modified cycloaliphatic epoxy resin: in reaction unit, add 10.48Kg 3,4-epoxy cyclohexylmethyl-3,4-epoxy cyclohexyl carbonic ether and 3.6Kg gather [(2-Oxyranyle)-1; The 2-cyclohexanediol] 2-ethyl-2-(methylol)-1; Ammediol ether behind the heating and melting, adds 0.2Kg catalyzer triphenyl phosphorus and 5.4Kg methyl phenyl silicone resin; After being warming up to 120 ℃ of reaction 4h, underpressure distillation removes the water that dereaction generates;
(2) component A: take by weighing the above-mentioned organic-silicon-modified cycloaliphatic epoxy resin of 9.7Kg, toughness reinforcing dose of 0.25 Kg organosilicon and 0.05 Kg skimmer, under 70 ℃ of conditions, stir 3.5h to mixing;
(3) B component: take by weighing 0.19 Kg aromatic diazo salt and 0.01Kg nano titanium oxide, under 70 ℃ of conditions, stir 3.5h to mixing;
(4) with being used for construction behind above-mentioned A, the B two component mixings.
Embodiment 2
(1) prepare organic-silicon-modified cycloaliphatic epoxy resin: in reaction unit, add 10.48Kg3,4-epoxy cyclohexylmethyl-3,4-epoxy cyclohexyl carbonic ether and 3.6Kg gather [(2-Oxyranyle)-1; The 2-cyclohexanediol] 2-ethyl-2-(methylol)-1; Ammediol ether behind the heating and melting, adds 0.2Kg catalyzer triphenyl phosphorus and 5.4Kg methyl phenyl silicone resin; After being warming up to 120 ℃ of reaction 4h, underpressure distillation removes the water that dereaction generates;
(2) component A: take by weighing the above-mentioned organic-silicon-modified cycloaliphatic epoxy resin of 9.7 Kg, toughness reinforcing dose of 0.25Kg organosilicon and 0.05 Kg skimmer, under 80 ℃ of conditions, stir 3h to mixing;
(3) B component: take by weighing 0.19 Kg aromatic diazo salt and 0.01Kg nano titanium oxide, under 80 ℃ of conditions, stir 3h to mixing;
(4) with being used for construction behind above-mentioned A, the B two component mixings.
Embodiment 3
(1) prepare organic-silicon-modified cycloaliphatic epoxy resin: in reaction unit, add 10.48Kg 3,4-epoxy cyclohexylmethyl-3,4-epoxy cyclohexyl carbonic ether and 3.6Kg gather [(2-Oxyranyle)-1; The 2-cyclohexanediol] 2-ethyl-2-(methylol)-1; Ammediol ether behind the heating and melting, adds 0.2Kg catalyzer triphenyl phosphorus and 5.4Kg methyl phenyl silicone resin; After being warming up to 120 ℃ of reaction 4h, underpressure distillation removes the water that dereaction generates;
(2) component A: take by weighing the above-mentioned organic-silicon-modified cycloaliphatic epoxy resin of 9.65Kg, toughness reinforcing dose of 0.3 Kg organosilicon and 0.05 Kg skimmer, under 70 ℃ of conditions, stir 3.5h to mixing;
(3) B component: 0.095 Kg aromatic diazo salt and 0.005Kg nano titanium oxide, stir 3.5h to mixing under 70 ℃ of conditions;
(4) with being used for construction behind above-mentioned A, the B two component mixings.

Claims (3)

1. the adulterated epoxy resin optical fiber of nanometer uv-absorbing agent adhesive glue; This adhesive glue is made up of host A and solidifying agent B two components; Through A, B two components by mass ratio 1: (0.01-0.02) be used for construction after mixing; It is characterized in that; The A method for preparing ingredients thereof is: with mass percent be 93%~95.5% organic-silicon-modified cycloaliphatic epoxy resin, 0.5%-1% silane coupling agent, 4%~6% toughner and 0.3%~0.5% skimmer weighing is good in proportion, under 70-80 ℃ of condition, stir 3-4h to mixing; The B method for preparing ingredients thereof is: with mass percent be 99% cationic solidifying agent aromatic diazo salt and 1% nanometer uv-absorbing agent weighing is good in proportion, under 70-90 ℃ of condition, stir 3-4h, mix.
2. the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent as claimed in claim 1 adhesive glue is characterized in that described nanometer uv-absorbing agent is that particle diameter is the titanium oxide of 16nm.
3. the adulterated epoxy resin optical fiber of a kind of nanometer uv-absorbing agent as claimed in claim 1 adhesive glue is characterized in that described solidifying agent is cationic solidifying agent aromatic diazo salt.
CN201210293451XA 2012-08-17 2012-08-17 Epoxy resin optical fiber adhesive glue doped by nano ultraviolet absorbing agent Pending CN102766427A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114409875A (en) * 2022-02-28 2022-04-29 万华化学集团股份有限公司 Reactive ultraviolet absorbent and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114409875A (en) * 2022-02-28 2022-04-29 万华化学集团股份有限公司 Reactive ultraviolet absorbent and preparation method and application thereof
CN114409875B (en) * 2022-02-28 2023-10-20 万华化学集团股份有限公司 Reactive ultraviolet absorber, preparation method and application thereof

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Application publication date: 20121107