CN111057515B - Block-type-structure UV adhesive for sensing coil and preparation method thereof - Google Patents

Block-type-structure UV adhesive for sensing coil and preparation method thereof Download PDF

Info

Publication number
CN111057515B
CN111057515B CN201911140799.3A CN201911140799A CN111057515B CN 111057515 B CN111057515 B CN 111057515B CN 201911140799 A CN201911140799 A CN 201911140799A CN 111057515 B CN111057515 B CN 111057515B
Authority
CN
China
Prior art keywords
resin matrix
temperature
acrylate resin
adhesive
sensing coil
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.)
Active
Application number
CN201911140799.3A
Other languages
Chinese (zh)
Other versions
CN111057515A (en
Inventor
吴晓乐
赵小明
罗巍
马林
史英桂
左文龙
刘伯晗
王玥泽
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.)
707th Research Institute of CSIC
Original Assignee
707th Research Institute of CSIC
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 707th Research Institute of CSIC filed Critical 707th Research Institute of CSIC
Priority to CN201911140799.3A priority Critical patent/CN111057515B/en
Publication of CN111057515A publication Critical patent/CN111057515A/en
Application granted granted Critical
Publication of CN111057515B publication Critical patent/CN111057515B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/14Polyurethanes having carbon-to-carbon unsaturated bonds
    • C09J175/16Polyurethanes having carbon-to-carbon unsaturated bonds having terminal carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67Unsaturated compounds having active hydrogen
    • C08G18/671Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1433Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • C08G59/1455Monocarboxylic acids, anhydrides, halides, or low-molecular-weight esters thereof
    • C08G59/1461Unsaturated monoacids
    • C08G59/1466Acrylic or methacrylic acids
    • 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
    • C09J163/10Epoxy resins modified by unsaturated compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Emergency Medicine (AREA)
  • General Chemical & Material Sciences (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Macromonomer-Based Addition Polymer (AREA)

Abstract

The invention relates to a block-type structure UV adhesive for a sensing coil, which comprises a polyurethane acrylate resin matrix, an epoxy acrylate resin matrix, an active monomer, a photoinitiator, a sensitizer and an auxiliary agent. According to the UV adhesive for the sensing coil and the preparation method thereof, provided by the invention, the low-temperature toughness and high-temperature rigidity of the adhesive can be improved, and the stability of the full-temperature performance of the coil is greatly enhanced; the UV adhesive can realize stable winding and deep curing of the coil, and has a wide working temperature range.

Description

UV adhesive with block type structure for sensing coil and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of fiber-optic gyroscope optical fiber loops, and particularly relates to a block-type structure UV adhesive for a sensing coil and a preparation method thereof.
Background
The optical fiber gyroscope is a novel all-solid-state angular rate sensor, has the advantages of low cost, long service life, large dynamic range, high reliability and the like, and is widely applied to the military and civil fields.
The sensing coil is a core sensing element of the optical fiber gyroscope, the application performance of the optical fiber gyroscope is directly influenced by the environmental adaptability of the sensing coil, and whether the optical fiber sensing coil can quickly adapt to the external high-low temperature environment or not is an important factor for determining the full-temperature stability of the coil in the working process after the optical fiber sensing coil is subjected to the environmental change of minus 45-70 ℃.
The UV adhesive is a high polymer material, occupies a high proportion of the ring, and has physical and chemical properties which are greatly related to the full-temperature stability of the optical fiber coil. As a key composition material of a fiber optic gyroscope sensitive element, the UV adhesive is required to have good mechanical property and durability, and also to have good temperature adaptability. The UV adhesive with the soft-segment-hard-segment block-type structure can encapsulate and cure the sensing coil, plays a role in fixing and size keeping, simultaneously ensures that the coil always works in a glass state under the full-temperature condition, simultaneously keeps certain flexibility at a low temperature of-45 ℃ and has better rigidity at a high temperature of 70 ℃, can fully keep stable performance when the coil experiences high and low temperatures, effectively reduces the low-temperature brittleness and internal stress of the optical fiber coil, improves the high-temperature rigidity and size keeping capability, and reduces the full-temperature error of the coil.
The high-vitrification adhesive generally shows brittleness at low temperature and has poor flexibility, and low-temperature thermal stress is not easy to absorb and release after being cured; the adhesive is softer under the high-temperature condition, and the coil cannot well keep dimensional deformation, so that the whole product has uneven thermal stress and larger change in the full-temperature range, and the application of the product is influenced.
Therefore, many researchers have studied the heat conductivity of the adhesive, and usually the glass transition temperature of the adhesive is increased to improve the defect of high-temperature softness, or the toughening means is used to improve the low-temperature brittleness, but the two adjusting means have opposite effects, and the ideal effect is difficult to achieve.
Therefore, the UV curing adhesive for the sensing coil needs to be designed and prepared, and has high-temperature rigidity and low-temperature toughness, so that the stability of the full-temperature performance of the fiber-optic gyroscope is improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the UV adhesive with the block-type structure for the sensing coil and the preparation method thereof, so that the low-temperature toughness and the high-temperature rigidity of the adhesive can be effectively improved, and the stability of the full-temperature performance of the coil is greatly enhanced; the UV adhesive can realize stable winding and deep curing of the coil, and the working temperature range is wide.
The technical problem to be solved by the invention is realized by the following technical scheme:
the utility model provides a block-type structure UV gluing agent for sensing coil which characterized in that: the UV adhesive with the block-type structure for the sensing coil comprises the following components in parts by weight:
Figure GDA0002385233970000021
and the epoxy acrylate resin matrix is independently synthesized and consists of epoxy resin E-51 and acrylic acid.
And the polyurethane acrylate resin matrix is independently synthesized and consists of xylylene diisocyanate, diethylene glycol phthalate and hydroxyethyl acrylate.
And the active monomer is one or more of hydroxyethyl acrylate, dipentaerythritol pentaacrylate, glycidyl methacrylate, polyethylene glycol (400) diacrylate, dipropylene glycol diacrylate, 1, 6-hexanediol diacrylate, polyethylene glycol terephthalate glycol diacrylate, trimethylolpropane triacrylate, ditrimethylolpropane tetraacrylate and hydroxypropyl methacrylate.
The photoinitiator is one or more of 2-hydroxy-2-methyl-phenyl acetone, 1-hydroxy-cyclohexyl benzophenone, 2-hydroxy-2-methyl-p-hydroxyethyl ether phenyl acetone, 2-methyl 1- (4-methylmercaptophenyl) -2-morpholinyl acetone-1 and bis (2, 4, 6-trimethylbenzoyl) phenyl phosphorus oxide.
The sensitizer is one or more of double EPD, double 225 and double ITX.
Furthermore, the auxiliary agent is digaku Dispers710 or FoamexN or the combination of the two.
A preparation method of a block-type structure UV adhesive for a sensing coil is characterized by comprising the following steps: the preparation method comprises the following steps:
1) synthesis of polyurethane acrylate resin matrix: placing a mixture of xylylene diisocyanate and a catalyst into an inclined four-neck flask, heating in a water bath, setting the temperature to be 50-70 ℃, slowly dripping diethylene glycol phthalate into a reaction system under a closed condition, and stirring and reacting for 3-6 hours after dripping is finished; after the reaction is finished, setting the temperature to be 80-100 ℃, slowly dripping the mixture of hydroxyethyl acrylate and a polymerization inhibitor into the reaction system, continuously reacting for 3-6 h after dripping is finished, then cooling the system to 60 ℃, and discharging to obtain a polyurethane acrylate resin matrix;
2) synthesis of epoxy acrylate resin matrix: placing a mixture of E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone in an inclined four-neck flask, heating in an oil bath at the temperature of 70-90 ℃, slowly dripping acrylic acid into the inclined four-neck flask, slowly heating to 100 ℃, continuously reacting for 2-5 h, heating to 110-120 ℃, continuously reacting for 2h, and discharging when the temperature is reduced to 70 ℃ to obtain an epoxy acrylate resin matrix;
3) adding the urethane acrylate resin matrix obtained in the step 1), the epoxy acrylate resin matrix obtained in the step 2) and an active monomer into a four-neck flask, controlling the rotating speed to be 300-800 r/min, stirring and mixing for 20min, then heating to 60-80 ℃, and preserving heat for 2h to obtain a mixed resin matrix;
4) cooling the mixed resin matrix obtained in the step 3) to 65 ℃, adding a photoinitiator, a sensitizer and an auxiliary agent under the condition of keeping out of the sun, stirring and mixing uniformly at a constant temperature of 200-500 r/min, and finally naturally cooling to room temperature to obtain the block-structured UV adhesive for the sensing coil.
The invention has the advantages and beneficial effects that:
1. the UV adhesive prepared by the invention realizes a high-modulus and high-vitrification design technology, and a block type molecular structure containing a benzene ring hard segment chain link and a polyurethane soft segment is prepared.
2. The UV adhesive prepared by the invention has a soft segment (PUA) -hard segment (benzene ring) block type molecular structure, has low-temperature toughness and high-temperature rigidity thermo-mechanical properties, and effectively ensures the temperature property stability of the sensing coil in the high-temperature and low-temperature range.
3. The UV adhesive prepared by the invention is used for packaging the sensing coil, the full-temperature stability of the ring is greatly improved, and the error of the full-temperature of the sensing coil using the UV adhesive is less than 0.06 degree/h at minus 45-70 ℃, and is improved by nearly 1 time compared with the improvement.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative, not limiting and are not intended to limit the scope of the invention.
The utility model provides a block-type structure UV gluing agent for sensing coil which characterized in that: the UV adhesive with the block-type structure for the sensing coil comprises the following components in parts by weight:
Figure GDA0002385233970000031
Figure GDA0002385233970000041
a preparation method of a soft-segment-hard-segment embedded structure UV adhesive for a sensing coil comprises the following steps:
1) weighing 40% of xylylene diisocyanate and catalyst mixture, 35% of diethylene glycol phthalate, 25% of hydroxyethyl acrylate and polymerization inhibitor mixture according to the mass percentage;
placing a mixture of xylylene diisocyanate and a catalyst in an inclined four-neck flask, heating in a water bath at the temperature of 50-70 ℃, slowly dripping diethylene glycol phthalate into a reaction system under a closed condition, and stirring and reacting for 3-6 hours after dripping is finished; and after the reaction is finished, setting the temperature to be 80-100 ℃, slowly dropwise adding a mixture of hydroxyethyl acrylate and a polymerization inhibitor into the reaction system, continuously reacting for 3-6 h after dropwise adding is finished, then cooling the system to 60 ℃, and discharging to obtain the polyurethane acrylate resin matrix.
2) Respectively weighing 74% of a mixture of E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone and 26% of acrylic acid according to the mass percentage;
placing a mixture of E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone in an inclined four-neck flask, heating in an oil bath at the temperature of 70-90 ℃, slowly dropwise adding acrylic acid into the four-neck flask, slowly heating to 100 ℃, continuously reacting for 2-5 h, heating to 110-120 ℃, continuously reacting for 2h, and discharging when the temperature is reduced to 70 ℃ to obtain the epoxy acrylate resin matrix.
3) Respectively weighing 20-40% of a polyurethane acrylate resin matrix, 10-30% of an epoxy acrylate resin matrix and 15-60% of an active monomer according to the mass percentage, respectively adding the materials into a reaction kettle, controlling the rotating speed to be 300-800 r/min, stirring and mixing for 20min, then heating to 60-80 ℃, and preserving heat for 2h to obtain a mixed prepolymer;
4) cooling the mixed prepolymer obtained in the step 3) to 65 ℃, adding 0.1-7% of photoinitiator, 0.1-1% of sensitizer and 0.2-3% of auxiliary agent under the condition of keeping out of the sun, placing the mixture at 200-500 r/min, stirring and mixing the mixture uniformly under the constant temperature condition, and finally naturally cooling the mixture to room temperature to obtain the UV adhesive for the sensing coil.
The process of the invention is illustrated below by way of specific examples:
the first embodiment is as follows:
1) placing 40g of a mixture of xylylene diisocyanate and a catalyst into an inclined four-neck flask, heating in a water bath at the temperature of 70 ℃, slowly dripping 35g of diethylene glycol phthalate into a reaction system under a closed condition, and stirring for reaction for 4 hours after dripping is finished; after the reaction is finished, setting the temperature to 95 ℃, slowly dripping 25g of a mixture of hydroxyethyl acrylate and a polymerization inhibitor into the reaction system, continuing to react for 6 hours after the dripping is finished, then cooling the system to 60 ℃, and discharging to obtain the polyurethane acrylate resin matrix.
2) Placing 74g of a mixture of epoxy resin E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone in a four-neck flask, heating in an oil bath at 85 ℃, slowly dripping 26g of acrylic acid into the four-neck flask, slowly heating to 100 ℃, continuously reacting for 4 hours, then heating to 115 ℃, continuously reacting for 2 hours, and discharging when the temperature is reduced to 70 ℃ to obtain the epoxy acrylate resin matrix.
3) Respectively adding 40g of urethane acrylate resin matrix, 10g of epoxy acrylate resin matrix and 39g of dipropylene glycol diacrylate into a reaction kettle, stirring and mixing for 20min at the rotating speed of 800r/min, then heating to 80 ℃, and preserving heat for 2h to obtain a mixed prepolymer;
4) and cooling the mixed prepolymer to 65 ℃, respectively adding 4g of 2-methyl 1- (4-methylmercaptophenyl) -2-morpholinopropanone-1, 3g of 2-hydroxy-2-methyl-p-hydroxyethyl ether phenyl propanone, 1g of double 225 and 3g of dispers710 under the condition of keeping out of the sun, placing at 200r/min, stirring and mixing uniformly under the constant temperature condition, and finally naturally cooling to room temperature to obtain the UV adhesive for the sensing coil.
Example two:
1) placing 10g of a mixture of xylylene diisocyanate and a catalyst into an inclined four-neck flask, heating in a water bath at 50 ℃, slowly dripping 8.75g of diethylene glycol phthalate into a reaction system under a closed condition, and stirring for reacting for 6 hours after dripping is finished; after the reaction is finished, setting the temperature to 100 ℃, slowly dripping 6.25g of a mixture of hydroxyethyl acrylate and a polymerization inhibitor into the reaction system, continuing to react for 3 hours after the dripping is finished, then cooling the system to 60 ℃, and discharging to obtain the polyurethane acrylate resin matrix.
2) Placing a mixture of 18.5g of epoxy resin E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone in a four-neck flask, heating in an oil bath at 70 ℃, slowly dropwise adding 6.5g of acrylic acid into the four-neck flask, slowly heating to 100 ℃, continuously reacting for 5 hours, then heating to 110 ℃, continuously reacting for 2 hours, and discharging when the temperature is reduced to 70 ℃ to obtain the epoxy acrylate resin matrix.
3) Respectively adding 20g of urethane acrylate resin matrix, 30g of epoxy acrylate resin matrix and 49.6g of trimethylolpropane triacrylate into a reaction kettle, stirring and mixing for 20min under the condition of the rotating speed of 300r/min, then heating to 60 ℃, and preserving heat for 2h to obtain a mixed prepolymer;
4) and cooling the mixed prepolymer to 65 ℃, respectively adding 0.1g of 2-hydroxy-2-methyl-phenyl acetone, 0.1g of double EPD and 0.2g of Foamex N under the dark condition, placing at 500r/min, stirring and mixing uniformly at a constant temperature, and finally naturally cooling to room temperature to obtain the UV adhesive for the sensing coil.
Example three:
1) placing 20g of a mixture of xylylene diisocyanate and a catalyst into a four-neck flask, heating in a water bath at a temperature of 60 ℃, slowly dripping 17.5g of diethylene glycol phthalate into a reaction system under a closed condition, and stirring for reaction for 5 hours after dripping is finished; after the reaction is finished, setting the temperature to 95 ℃, slowly dripping a mixture of 12.5g of hydroxyethyl acrylate and a polymerization inhibitor into the reaction system, continuing the reaction for 4 hours after the dripping is finished, then cooling the system to 60 ℃, and discharging to obtain the polyurethane acrylate resin matrix.
2) Placing a mixture of 37g of epoxy resin E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone in a four-neck flask, heating in an oil bath at 80 ℃, slowly dropwise adding 13g of acrylic acid into the four-neck flask, slowly heating to 100 ℃, continuously reacting for 3h, then heating to 120 ℃, continuously reacting for 2h, and discharging when the temperature is reduced to 70 ℃ to obtain the epoxy acrylate resin matrix.
3) Respectively adding 35g of urethane acrylate resin matrix, 20g of epoxy acrylate resin matrix and 37g of trimethylolpropane triacrylate into a reaction kettle, stirring and mixing for 20min at the rotation speed of 300r/min, heating to 60 ℃, and preserving heat for 2h to obtain a mixed prepolymer;
4) and cooling the mixed prepolymer to 65 ℃, respectively adding 5g of bis (2, 4, 6-trimethylbenzoyl) phenyl phosphorus oxide, 0.5g of double EPD and 2.5g of Foamex N under the condition of keeping out of the sun, placing the mixture at 350r/min, stirring and mixing the mixture uniformly at a constant temperature, and finally naturally cooling the mixture to room temperature to obtain the UV adhesive for the sensing coil.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the embodiments disclosed.

Claims (1)

1. The utility model provides a block-type structure UV gluing agent for sensing coil which characterized in that: the UV adhesive with the block-type structure for the sensing coil comprises the following components in parts by weight:
20-40% of polyurethane acrylate resin matrix
10-30% of epoxy acrylate resin matrix
15-60% of active monomer
0.1 to 7 percent of photoinitiator
0.1 to 1 percent of sensitizer
0.2-3% of an auxiliary agent;
the epoxy acrylate resin matrix is independently synthesized and consists of epoxy resin E-51 and acrylic acid;
the polyurethane acrylate resin matrix is independently synthesized and consists of xylylene diisocyanate, diethylene glycol phthalate and hydroxyethyl acrylate;
the active monomer is one or more of hydroxyethyl acrylate, dipentaerythritol pentaacrylate, glycidyl methacrylate, polyethylene glycol diacrylate, dipropylene glycol diacrylate, 1, 6-hexanediol diacrylate, polyethylene glycol terephthalate diacrylate, trimethylolpropane triacrylate, trimethylolpropane diacrylate and hydroxypropyl methacrylate;
the photoinitiator is one or more of 2-hydroxy-2-methyl-phenyl acetone, 1-hydroxy-cyclohexyl benzophenone, 2-hydroxy-2-methyl-p-hydroxyethyl ether phenyl acetone, 2-methyl 1- (4-methylmercaptophenyl) -2-morpholine acetone-1 and bis (2, 4, 6-trimethylbenzoyl) phenyl phosphorus oxide;
the sensitizer is one or more of double EPD, double 225 and double ITX;
the auxiliary agent is Digao Dispers710 or Foamex N or the combination of the two;
the preparation method of the block-type structure UV adhesive for the sensing coil comprises the following steps:
1) synthesis of polyurethane acrylate resin matrix: placing a mixture of xylylene diisocyanate and a catalyst into an inclined four-neck flask, heating in a water bath, setting the temperature to be 50-70 ℃, slowly dripping diethylene glycol phthalate into a reaction system under a closed condition, and stirring and reacting for 3-6 hours after dripping is finished; after the reaction is finished, setting the temperature to be 80-100 ℃, slowly dripping the mixture of hydroxyethyl acrylate and a polymerization inhibitor into the reaction system, continuously reacting for 3-6 h after dripping is finished, then cooling the system to 60 ℃, and discharging to obtain a polyurethane acrylate resin matrix;
2) synthesis of epoxy acrylate resin matrix: placing a mixture of E-51, N-dimethylaniline and 2, 5-dimethyl hydroquinone in an inclined four-neck flask, heating in an oil bath at the temperature of 70-90 ℃, slowly dripping acrylic acid into the inclined four-neck flask, slowly heating to 100 ℃, continuously reacting for 2-5 h, heating to 110-120 ℃, continuously reacting for 2h, and discharging when the temperature is reduced to 70 ℃ to obtain an epoxy acrylate resin matrix;
3) adding the urethane acrylate resin matrix obtained in the step 1), the epoxy acrylate resin matrix obtained in the step 2) and an active monomer into a four-neck flask, controlling the rotating speed to be 300-800 r/min, stirring and mixing for 20min, then heating to 60-80 ℃, and preserving heat for 2h to obtain a mixed resin matrix;
cooling the mixed resin matrix obtained in the step 3) to 65 ℃, adding a photoinitiator, a sensitizer and an auxiliary agent under the condition of keeping out of the sun, stirring and mixing uniformly at a constant temperature of 200-500 r/min, and finally naturally cooling to room temperature to obtain the block-structured UV adhesive for the sensing coil.
CN201911140799.3A 2019-11-20 2019-11-20 Block-type-structure UV adhesive for sensing coil and preparation method thereof Active CN111057515B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911140799.3A CN111057515B (en) 2019-11-20 2019-11-20 Block-type-structure UV adhesive for sensing coil and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911140799.3A CN111057515B (en) 2019-11-20 2019-11-20 Block-type-structure UV adhesive for sensing coil and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111057515A CN111057515A (en) 2020-04-24
CN111057515B true CN111057515B (en) 2022-06-17

Family

ID=70298569

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911140799.3A Active CN111057515B (en) 2019-11-20 2019-11-20 Block-type-structure UV adhesive for sensing coil and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111057515B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114933886B (en) * 2021-06-04 2024-04-02 东莞市瑞辉新材料技术有限公司 High-flexibility UV transfer printing adhesive and preparation method and application thereof
CN114874742A (en) * 2022-05-20 2022-08-09 长春艾德斯新材料有限公司 Ultraviolet curing adhesive with low volume shrinkage and preparation method thereof
CN115160975B (en) * 2022-06-21 2023-12-22 武汉长盈鑫科技有限公司 Dual-cured metal surface primer and use method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018160564A1 (en) * 2017-03-03 2018-09-07 3M Innovative Properties Company High performance photocurable optically clear adhesive

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0570404A (en) * 1991-09-13 1993-03-23 Chisso Corp New acrylate
CN103555210A (en) * 2013-10-26 2014-02-05 深圳市中显微电子有限公司 Liquid optical adhesive and preparation method thereof
CN104559811B (en) * 2015-01-13 2017-12-05 武汉长盈通光电技术有限公司 A kind of radiation-hardenable fiber optic loop tail optical fiber encapsulating adhesive
CN106634789B (en) * 2016-11-09 2020-11-06 东莞市贝特利新材料有限公司 Ultraviolet light curing adhesive and preparation method thereof
CN107828368A (en) * 2017-11-16 2018-03-23 广州日高新材料科技有限公司 Ultraviolet photo-curing cementing agent and preparation method thereof
CN109439269B (en) * 2018-10-31 2020-04-24 中国船舶重工集团公司第七0七研究所 High-thermal-conductivity ultraviolet curing adhesive for potting optical fiber coil and preparation method thereof
CN110184023A (en) * 2019-05-31 2019-08-30 长飞光纤光缆股份有限公司 A kind of ultraviolet light solidification fiber optic loop adhesive
CN110172327B (en) * 2019-05-31 2021-09-14 山东领科新材料科技有限公司 Photocuring composite adhesive and production process thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018160564A1 (en) * 2017-03-03 2018-09-07 3M Innovative Properties Company High performance photocurable optically clear adhesive

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Preparation of UV-curable epoxy acrylate adhesive toughened by polyurethane acrylate;Li Guo-qiang等;《Electroplating & Finishing 32》;20130630;第32卷(第6期);第65-68页 *
UV固化环氧丙烯酸酯涂料研究进展;王锋等;《热固性树脂》;20070731;第22卷(第04期);第39-43页 *

Also Published As

Publication number Publication date
CN111057515A (en) 2020-04-24

Similar Documents

Publication Publication Date Title
CN111057515B (en) Block-type-structure UV adhesive for sensing coil and preparation method thereof
CN105086916B (en) A kind of double curing adhesives of high printing opacity UV moistures
CN102076806B (en) Active-energy-ray-curing adhesive composition
CN108383974A (en) A kind of ultraviolet light solidification high-strength polyurethane acrylate and preparation method thereof
CN109439269B (en) High-thermal-conductivity ultraviolet curing adhesive for potting optical fiber coil and preparation method thereof
CN105885002A (en) Preparation method of waterborne polyurethane capable of selfreparing
CN108530602B (en) Color-changing polyurethane acrylic dye resin and preparation method thereof
CN110358020A (en) A kind of photosensitive resin and a kind of method of 3D printing polyureas
CN103374323B (en) Preparation method of yellowing resistant liquid optical adhesive
CN104098999A (en) UV-heat dual-curing polyurethane coating, and preparation method and application thereof
CN104531045A (en) Preparing method for reaction type polyurethane hot melt adhesive with multiple curing modes
CN105400251B (en) Hard coating composition, polarizing film using same and display
CN109517513A (en) A kind of production method with the room temperature self-repair type aqueous polyurethane car clothing from extinction effect
CN103382381A (en) Yellowing resistant liquid optical adhesive
CN103408713A (en) Preparation method and application of supramolecular liquid crystal shape memory polyurethane
CN115181535B (en) Ultraviolet light-moisture dual-curing polyurethane hot melt adhesive and preparation method thereof
Ma et al. A Self-repairing transparent film with reprocessable, ultra-high strength and outstanding elasticity based on interlocking hydrogen bonds and reversible topological networks
WO2019006694A1 (en) Method for preparing shape memory polyurethane
CN103030767A (en) Degradable radiation-curable polyurethane acrylate oligomer and preparation method thereof
CN113493654A (en) Photo-thermal dual-curing adhesive and preparation method thereof
CN112029043B (en) Photosensitive elastic resin, preparation method thereof and application thereof in photocuring 3D printing technology
CN110684175B (en) High-light-transmittance super-tough room-temperature intrinsic self-repairing elastomer material and preparation method thereof
CN105542121B (en) UV-cured polyurethane acrylate and preparation method thereof
CN112552862A (en) Dual-curing glue, intelligent terminal shell and manufacturing method
CN108977071A (en) A kind of fiber outer layer coating of interpenetrating net polymer structure and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant