CN104449517A - Ultraviolet cured repair adhesive and preparation method thereof - Google Patents
Ultraviolet cured repair adhesive and preparation method thereof Download PDFInfo
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- CN104449517A CN104449517A CN201410806277.3A CN201410806277A CN104449517A CN 104449517 A CN104449517 A CN 104449517A CN 201410806277 A CN201410806277 A CN 201410806277A CN 104449517 A CN104449517 A CN 104449517A
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Abstract
The invention provides ultraviolet cured repair adhesive and a preparation method thereof, belongs to the technical field of quick ultraviolet cured repair adhesive, and solves the problems that the curing time is long, the bonding strength is low, the oil resistance is poor or the aging degree is serous, the service cycle is short and the like in the prior art. The ultraviolet cured repair adhesive is characterized by comprising a component A and a component B, wherein the component A comprises epoxy modified acrylate resin, ultraviolet cured epoxy resin, room-temperature cured silicone rubber, methylsilicone oil, zinc carbonate powder and fumed silica; the component B comprises an ultraviolet initiator and a curing agent. The preparation method of the ultraviolet cured repair adhesive comprises the steps of preparing the component A, preparing the component B and mixing the component A and the component B. The ultraviolet cured repair adhesive can be cured within 90s without heating, is convenient in field operation, and can be used for quickly and highly effectively repairing leaking parts without shutting down, pressure leakage and oil/gas discharge, so that the labor, material and financial resource investment is effectively saved.
Description
Technical field
The invention belongs to ultraviolet light fast solidification repair sheets technical field, be specifically related to ultraviolet light polymerization repair sheets and preparation method thereof.
Background technology
For a long time, Leakage in Transformer oil/gas problem annoyings the normal operation of transformer and the power supply safety of power system always, causes the extensive concern of domestic and international those skilled in the relevant art.Domestic relevant publication there is the report in a large number about Leakage in Transformer point producing cause and treatment measures.Yang Zhi waits by force people's proposition modified acrylic ester adhesion agent to process breakthrough.Yan Tao proposes with " 302 " seal gum or " can fill in new " that metal repairing agent carries out leak stopping, but " 302 " seal gum is more fragile, easily unsticking or fracture after repairing, and " can fill in new " metal repairing agent can not be with oil to operate, and set time is longer.All there are repair sheets product, 826 repair sheets as prosperous in justice and the urgent healant of TS858 pasta of Tai Sheng for the treatment of breakthrough in Yantai Yi Chang Fine Chemical Co., Ltd and the Tai Sheng novel material company limited that refines.Above measure is based on existing repair sheets product substantially, and specific aim is not strong, even if repair efficiency is better in a short time, but effect is not lasting, can not meet application requiring.
Also there is related products abroad, consult the data display that internet obtains, the FasMetal of ITW Devcon company
tMputty product (a kind of epoxy glue adding aluminum oxide can solidify within 5 minutes) and
80Putty product (a kind of polyurethane adhesive), polywater company of the U.S.
system's putty series product, and the related products of THE COLT GROUP company, all can be used for repairing Leakage in Transformer position.External product is expensive, and result of use is also not fully up to expectations.
The subject matter that prior art exists is: set time is long, cohesive strength is not high, oil-proofness is poor, or seriously aging, the problems such as life cycle is short.
Summary of the invention
Present patent application technical problem underlying to be solved is that development is a kind of for fast setting and the more lasting repair sheets formula of effect, to adapt to the repairing demand at Leakage in Transformer position in power system, and other ultraviolet light polymerization repair sheets needing the Application Areas of Rapid-Repair and preparation method thereof.
The present invention solves the problems of the technologies described above the technical scheme taked to be:
Ultraviolet light polymerization repair sheets, be characterized in: these repair sheets are made up of component A and B component two portions, component A comprises epoxy modified acrylic resin, UV-curable epoxy and room curing silicon rubber, and methyl-silicone oil, zinc carbonate powder and aerosil, B component comprises ultraviolet initiator and solidifying agent.
The preparation method of ultraviolet light polymerization repair sheets, comprises the step of preparation component A, the step of preparation B component and the step of component A and B component mixing, it is characterized in that: the concrete steps of these repair sheets preparation method are as follows:
(1) preparation of epoxy acrylic resin
Take epoxy resin and vinylformic acid in proportion, by epoxy resin and the mixing of a small amount of Resorcinol, be heated to 80-90 DEG C, then slowly drip the mixture of vinylformic acid and benzyl triethyl ammonium bromide, control temperature of reaction below 100 DEG C, drip after terminating, be warmed up to 100-105 DEG C, react two hours; After reaction terminates, be cooled to less than 80 DEG C, be mixed into thinner tri (propylene glycol) diacrylate (TPGDA);
(2) reinforcing filler aerosil is mixed into
Take a certain amount of aerosil, be mixed in appropriate dehydrated alcohol, by ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C;
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into a certain amount of UV-curable epoxy and room curing silicon rubber successively, fully stir, make it mix;
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into methyl-silicone oil and zinc carbonate powder successively, obtain the repair sheets component A of slightly thickness;
(5) preparation of repair sheets B component
The proportioning of B component is relevant to repair sheets component A, comprises light trigger, photo-curing epoxy resin, silicon rubber solidifying agent, above component is mixed, be the B component of repair sheets;
(6) preparation of ultraviolet light polymerization repair sheets
Take appropriate repair sheets component A, add B component (light trigger and solidifying agent) in proportion, mix, obtain ultraviolet light polymerization repair sheets.
The present invention has following beneficial effect:
(1) ultraviolet light polymerization repair sheets of the present invention can solidify in 90 seconds, and did not need heating.Domestic existing self-vulcanizing repair sheets product, set time is longer, generally could solidify completely after several hours.And before this, the oil/gas of seepage place cannot be avoided to penetrate in repair sheets, cause degradation.
(2) due to quick solidifying; ultraviolet light polymerization repair sheets of the present invention can play the effect of fast blockage; be convenient to execute-in-place, when not shutting down, not pressure release, fast and effeciently repair seepage place when not putting oil/gas, effectively save the input of human and material resources, financial resources.
(3) ultraviolet light polymerization repair sheets of the present invention formula, be suitable for using under condition out of doors, repair efficiency is more lasting.
Embodiment
Ultraviolet light polymerization repair sheets, these repair sheets are made up of component A and B component two portions, component A mainly comprises epoxy modified acrylic resin, UV-curable epoxy and room curing silicon rubber, and methyl-silicone oil, zinc carbonate powder and aerosil, B component mainly comprises ultraviolet initiator and solidifying agent.
The preparation method of ultraviolet light polymerization repair sheets, comprise the step of preparation component A, the step of preparation B component and the step of component A and B component mixing, the concrete steps of these repair sheets preparation method are as follows:
(1) preparation of epoxy acrylic resin
Take epoxy resin and vinylformic acid in proportion, wherein: the mol ratio of epoxide group and carboxyl is 1 ~ 5:1, by epoxy resin and the mixing of a small amount of Resorcinol, described dihydroxy-benzene content is 0.1wt%-0.3wt%, is heated to 80-90 DEG C, then the mixture of vinylformic acid and benzyl triethyl ammonium bromide is slowly dripped, wherein benzyl triethyl ammonium bromide content is 0.6wt%-1.5wt%, controls temperature of reaction below 100 DEG C, drips after terminating, be warmed up to 100-105 DEG C, react two hours.After reaction terminates, be cooled to less than 80 DEG C, be mixed into thinner tri (propylene glycol) diacrylate (TPGDA), its content is the 10wt%-30wt% of epoxy acrylic resin;
(2) reinforcing filler aerosil is mixed into
Take a certain amount of aerosil, be mixed in appropriate dehydrated alcohol, wherein: described aerosil content is the 1wt%-8wt% of epoxy acrylic resin; By ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C;
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into a certain amount of UV-curable epoxy and room curing silicon rubber successively, wherein: the mass ratio of described UV-curable epoxy and epoxy acrylic resin is 1:1 ~ 3, the mass ratio of described room curing silicon rubber and epoxy acrylic resin is 1:3 or 2:1, abundant stirring, makes it mix;
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into the methyl-silicone oil of 5wt% ~ 20wt% and the zinc carbonate powder of 5wt% ~ 50wt% successively, obtain the repair sheets component A of slightly thickness;
(5) preparation of repair sheets B component
The proportioning of B component is relevant to repair sheets component A, light trigger 1173 and 184 2 ~ 5:1 mixing in mass ratio, the ratio that need add 2-5wt% with 100 mass unit epoxy acrylic resins adds, the ratio that initiator S-6976 need add 2 ~ 5wt% with 100 mass unit photo-curing epoxy resins adds, the ratio that silicon rubber solidifying agent need add 2 ~ 5wt% with 100 mass unit silicon rubber adds, above component is mixed, is the B component of repair sheets;
(6) preparation of ultraviolet light polymerization repair sheets
Take appropriate repair sheets component A, add the B component of 20wt%-35wt%, mix, obtain ultraviolet light polymerization repair sheets.
Embodiment 1:
(1) 25 grams of epoxy resin and 9 grams of vinylformic acid are taken, the addition of Resorcinol is 0.2wt%, the addition of benzyl triethyl ammonium bromide is 0.9wt%, by epoxy resin and Resorcinol mixing, be heated to 80-90 DEG C, then slowly drip the mixture of vinylformic acid and benzyl triethyl ammonium bromide, control temperature of reaction below 100 DEG C, after dropping terminates, be warmed up to 100-105 DEG C, react two hours.After reaction terminates, be cooled to less than 80 DEG C, be mixed into 9 grams of thinner tri (propylene glycol) diacrylates (TPGDA).
(2) 1.2 grams of aerosils are taken, be mixed in 20 milliliters of dehydrated alcohols, by ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C.
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into 44 grams of UV-curable epoxy and 22 grams of silicon rubber component A successively, fully stir, make it mix.
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into 15 grams of methyl-silicone oils and 30 grams of zinc carbonate powder successively, obtain the repair sheets component A of slightly thickness.
(5) preparation of repair sheets B component
Take each 0.66 gram and 0.22 gram of light trigger 1173 and 184 respectively, take initiator S-6976 and each 1.32 grams and 22 grams of silicon rubber B component respectively, above component is mixed, is the B component of repair sheets.
(6) preparation of ultraviolet light polymerization repair sheets
Take appropriate repair sheets component A, add the B component of 20wt%, mix, obtain ultraviolet light polymerization repair sheets.
Embodiment 2
(1) 25 grams of epoxy resin and 5.3 grams of vinylformic acid are taken, the addition of Resorcinol is 0.2wt%, the addition of benzyl triethyl ammonium bromide is 0.9wt%, by epoxy resin and Resorcinol mixing, be heated to 80-90 DEG C, then slowly drip the mixture of vinylformic acid and benzyl triethyl ammonium bromide, control temperature of reaction below 100 DEG C, after dropping terminates, be warmed up to 100-105 DEG C, react two hours.After reaction terminates, be cooled to less than 80 DEG C, be mixed into 6 grams of thinner tri (propylene glycol) diacrylates (TPGDA).
(2) 1 gram of aerosil is taken, be mixed in 20 milliliters of dehydrated alcohols, by ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C.
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into 29 grams of UV-curable epoxy and 18 grams of silicon rubber component A successively, fully stir, make it mix.
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into 15 grams of methyl-silicone oils and 30 grams of zinc carbonate powder successively, obtain the repair sheets component A of slightly thickness.
(5) preparation of repair sheets B component
Take each 0.54 gram and 0.18 gram of light trigger 1173 and 184 respectively, take initiator S-6976 and each 0.9 gram and 18 grams of silicon rubber B component respectively, above component is mixed, is the B component of repair sheets.
(6) preparation of ultraviolet light polymerization repair sheets
Take appropriate repair sheets component A, add the B component of 25wt%, mix, obtain ultraviolet light polymerization repair sheets.
Using method:
1, the cleaning of seepage place
Adopt scavenger specially, the spot that cleaning leaking surface adheres to, if necessary, can the auxiliary meanss such as scraper be adopted, remove stain.Also can increase sand papering operation, increase surfaceness, to improve cohesive strength.
2, gluing and ultraviolet light polymerization operation
The ultraviolet light polymerization repair sheets prepared are evenly coated in seepage place, irradiate 90 seconds with ultra-violet lamp, namely curable.If necessary, this operation can also repeatedly be repeated.
Four, the coating protection on surface is repaired
For improving the oxidation-resistance of repairing surface, protective coating can be imposed.
Claims (4)
1. ultraviolet light polymerization repair sheets, it is characterized in that: these repair sheets are made up of component A and B component two portions, component A mainly comprises epoxy modified acrylic resin, UV-curable epoxy and room curing silicon rubber, and methyl-silicone oil, zinc carbonate powder and aerosil, B component mainly comprises ultraviolet initiator and solidifying agent.
2. the preparation method of ultraviolet light polymerization repair sheets, comprises the step of preparation component A, the step of preparation B component and the step of component A and B component mixing, it is characterized in that: the concrete steps of these repair sheets preparation method are as follows:
The step of preparation component A:
(1) preparation of epoxy acrylic resin
Take epoxy resin and vinylformic acid in proportion, wherein: the mol ratio of epoxide group and carboxyl is 1 ~ 5:1, by epoxy resin and the mixing of a small amount of Resorcinol, described Resorcinol content is 0.1wt%-0.3wt%, is heated to 80-90 DEG C, then the mixture of vinylformic acid and benzyl triethyl ammonium bromide is slowly dripped, wherein benzyl triethyl ammonium bromide content is 0.6wt%-1.5wt%, controls temperature of reaction below 100 DEG C, drips after terminating, be warmed up to 100-105 DEG C, react two hours; After reaction terminates, be cooled to less than 80 DEG C, be mixed into thinner tri (propylene glycol) diacrylate (TPGDA), its content is the 10wt%-30wt% of epoxy acrylic resin;
(2) reinforcing filler aerosil is mixed into
Take a certain amount of aerosil, be mixed in appropriate dehydrated alcohol, wherein: described aerosil content is the 1wt%-8wt% of epoxy acrylic resin; By ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C;
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into a certain amount of UV-curable epoxy and room curing silicon rubber successively, wherein: the mass ratio of described UV-curable epoxy and epoxy acrylic resin is 1:1 ~ 3, the mass ratio of described room curing silicon rubber and epoxy acrylic resin is 1:3 or 2:1, abundant stirring, makes it mix;
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into the methyl-silicone oil of 5wt% ~ 20wt% and the zinc carbonate powder of 5wt% ~ 50wt% successively, obtain the repair sheets component A of slightly thickness;
The step of preparation B component:
Light trigger 1173 and 184 2 ~ 5:1 mixing in mass ratio, the ratio that need add 2-5wt% with 100 mass unit epoxy acrylic resins adds, the ratio that initiator S-6976 need add 2 ~ 5wt% with 100 mass unit photo-curing epoxy resins adds, the ratio that silicon rubber solidifying agent need add 2 ~ 5wt% with 100 mass unit silicon rubber adds, above component is mixed, is the B component of repair sheets;
The step of component A and B component mixing:
Take appropriate repair sheets component A, add B component in proportion, mix, obtain ultraviolet light polymerization repair sheets.
3. the preparation method of ultraviolet light polymerization repair sheets according to claim 2, is characterized in that: comprise following concrete steps:
(1) 25 grams of epoxy resin and 9 grams of vinylformic acid are taken, the addition of Resorcinol is 0.2wt%, the addition of benzyl triethyl ammonium bromide is 0.9wt%, by epoxy resin and Resorcinol mixing, be heated to 80-90 DEG C, then slowly drip the mixture of vinylformic acid and benzyl triethyl ammonium bromide, control temperature of reaction below 100 DEG C, after dropping terminates, be warmed up to 100-105 DEG C, react two hours; After reaction terminates, be cooled to less than 80 DEG C, be mixed into 9 grams of thinner tri (propylene glycol) diacrylates;
(2) 1.2 grams of aerosils are taken, be mixed in 20 milliliters of dehydrated alcohols, by ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C;
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into 44 grams of UV-curable epoxy and 22 grams of silicon rubber component A successively, fully stir, make it mix;
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into 15 grams of methyl-silicone oils and 30 grams of zinc carbonate powder successively, obtain the repair sheets component A of slightly thickness;
(5) preparation of repair sheets B component
Take each 0.66 gram and 0.22 gram of light trigger 1173 and 184 respectively, take initiator S-6976 and each 1.32 grams and 22 grams of silicon rubber B component respectively, above component is mixed, is the B component of repair sheets;
(6) preparation of ultraviolet light polymerization repair sheets
Take appropriate repair sheets component A, add the B component of 20wt%, mix, obtain ultraviolet light polymerization repair sheets.
4. the preparation method of ultraviolet light polymerization repair sheets according to claim 2, is characterized in that: comprise following concrete steps:
(1) 25 grams of epoxy resin and 5.3 grams of vinylformic acid are taken, the addition of Resorcinol is 0.2wt%, the addition of benzyl triethyl ammonium bromide is 0.9wt%, by epoxy resin and Resorcinol mixing, be heated to 80-90 DEG C, then slowly drip the mixture of vinylformic acid and benzyl triethyl ammonium bromide, control temperature of reaction below 100 DEG C, after dropping terminates, be warmed up to 100-105 DEG C, react two hours; After reaction terminates, be cooled to less than 80 DEG C, be mixed into 6 grams of thinner tri (propylene glycol) diacrylates;
(2) 1 gram of aerosil is taken, be mixed in 20 milliliters of dehydrated alcohols, by ul-trasonic irradiation, white carbon black is made to be dispersed in ethanol, then by the reaction solution of gained in its impouring step (1), reflux 10-20 minute, afterwards underpressure distillation, removing ethanol wherein, is cooled to about 60 DEG C;
(3) UV-curable epoxy and room curing silicon rubber is mixed into
In the mixture of step (2) gained, be mixed into 29 grams of UV-curable epoxy and 18 grams of silicon rubber component A successively, fully stir, make it mix;
(4) methyl-silicone oil and zinc carbonate powder is mixed into
In the mixture of step (3) gained, be mixed into 15 grams of methyl-silicone oils and 30 grams of zinc carbonate powder successively, obtain the repair sheets component A of slightly thickness;
(5) preparation of repair sheets B component
Take each 0.54 gram and 0.18 gram of light trigger 1173 and 184 respectively, take initiator S-6976 and each 0.9 gram and 18 grams of silicon rubber B component respectively, above component is mixed, is the B component of repair sheets;
(6) preparation of ultraviolet light polymerization repair sheets
Take appropriate repair sheets component A, add the B component of 25wt%, mix, obtain ultraviolet light polymerization repair sheets.
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Cited By (2)
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CN106281176A (en) * | 2016-07-28 | 2017-01-04 | 孙涛 | A kind of windshield renovation agent and preparation method thereof |
CN111826109A (en) * | 2020-06-22 | 2020-10-27 | 上海回天新材料有限公司 | UV-curable two-component epoxy adhesive |
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US7232850B2 (en) * | 2003-10-03 | 2007-06-19 | Huntsman Advanced Materials Americas Inc. | Photocurable compositions for articles having stable tensile properties |
CN101812278A (en) * | 2010-05-20 | 2010-08-25 | 上海西怡新材料科技有限公司 | Ultraviolet curable organic silicon-acrylic resin electronic adhesive and application thereof |
CN103755889A (en) * | 2014-01-10 | 2014-04-30 | 上海那恒新材料有限公司 | Light-emitting high precision three-dimensionally moulded photosensitive resin composition |
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2014
- 2014-12-22 CN CN201410806277.3A patent/CN104449517B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US7232850B2 (en) * | 2003-10-03 | 2007-06-19 | Huntsman Advanced Materials Americas Inc. | Photocurable compositions for articles having stable tensile properties |
CN101812278A (en) * | 2010-05-20 | 2010-08-25 | 上海西怡新材料科技有限公司 | Ultraviolet curable organic silicon-acrylic resin electronic adhesive and application thereof |
CN103755889A (en) * | 2014-01-10 | 2014-04-30 | 上海那恒新材料有限公司 | Light-emitting high precision three-dimensionally moulded photosensitive resin composition |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106281176A (en) * | 2016-07-28 | 2017-01-04 | 孙涛 | A kind of windshield renovation agent and preparation method thereof |
CN106281176B (en) * | 2016-07-28 | 2019-04-19 | 孙涛 | A kind of windshield renovation agent and preparation method thereof |
CN111826109A (en) * | 2020-06-22 | 2020-10-27 | 上海回天新材料有限公司 | UV-curable two-component epoxy adhesive |
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