CN114940731A - High-humidity-heat-resistance, long-activation-period, high-hardness and quick-drying resin for aqueous optical diffusion film coating - Google Patents
High-humidity-heat-resistance, long-activation-period, high-hardness and quick-drying resin for aqueous optical diffusion film coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
- C08F283/105—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule on to unsaturated polymers containing more than one epoxy radical per molecule
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates 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
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates 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
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
- C08G59/145—Compounds containing one epoxy group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates 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
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1494—Polycondensates modified by chemical after-treatment followed by a further chemical treatment thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates 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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention belongs to the technical field of optical diffusion films, and particularly relates to a resin for a high-humidity-heat-resistance, long-activation-period, high-hardness and quick-drying type aqueous optical diffusion film coating, which comprises the following components in parts by mass: 10-20 parts of methyl methacrylate, 5-15 parts of hydroxyethyl methacrylate, 3-8 parts of n-butyl methacrylate, 5-20 parts of maleic anhydride novolac epoxy organosilicon adduct, 1-3 parts of acrylic acid, 10-20 parts of styrene, 2.2-9 parts of tert-butyl peroxybenzoate, 0.1-1 part of dodecyl mercaptan, 30-40 parts of ethylene glycol monobutyl ether and 2-5 parts of PMA, and provides a specific preparation method. The invention has the characteristics of low VOC volatilization, environmental friendliness and the like, has long activation period, can keep the activation period for 5h, and solves the defects of the existing light diffusion film.
Description
Technical Field
The invention belongs to the technical field of optical diffusion films, and particularly relates to a high-humidity-heat-resistance, long-activation-period, high-hardness and quick-drying resin for a coating of a water-based optical diffusion film.
Background
The optical diffusion film is mainly applied to a backlight light source part of an LCD module, when light penetrates through the diffusion film taking a polyester film as a substrate, because the surface of the polyester film has a special coating, the coating contains two or more components with different refractive indexes, and media with different refractive indexes can cause the light to generate a plurality of reflection, refraction and scattering phenomena, the phenomena can finally enable the light to be corrected when the light leaves the polyester film, the original light forms an even surface light source, the light radiation area is increased, the light intensity of a unit area is reduced, and a secondary light source with even and soft light is formed.
The key technology of optical films is the coating technology, which can be divided into three categories, namely decorative coatings, protective coatings and functional coatings, depending on the role the coating plays in the optical film. The coating on the optical diffusion film is a functional coating, the components of the optical diffusion film can be divided into coating resin and optical particles, the coating resin is used for fixing particles, and the coating resin is required to be transparent, does not influence the optical performance of the optical particles, and is suitable for being coated on a polyester film. The principle of the particle is that when light passes through a particle with a diameter larger than or equal to the wavelength of the light, most of the light is scattered along the advancing direction, the passing light is scattered continuously, and finally the effect of light homogenization is achieved, and the phenomenon is called meter scattering. The coating formulation technology, the coating process, the coating curing technology and the like are the main problems in the manufacturing process of the optical diffusion film at present. The formula can be divided into three types of polyurethane, organosilicon and acrylic resin according to the type of the resin mainly used; the coating curing technology can be divided into two categories of photocuring and thermocuring, wherein the photocuring has the advantages of environmental protection, energy conservation, high efficiency, economy, strong adaptability and the like, but the photocuring can not completely cure the interior of the coating, so that the bonding strength of the coating and a substrate interface is insufficient. The thermosetting technology utilizes heat to evaporate the solvent in the coating and leaves the resin coated on the surface of the substrate, the method does not affect the strength of the coating, but has long production period, and in the case of a solvent-based formula, the method has large environmental pollution and high VOC content.
Although the problem that VOC exceeds the standard can be solved by taking water as a diluting solvent in the conventional aqueous optical diffusion film resin coating, the problems of low off-line hardness, long curing time, poor boiling resistance and the like of an optical film after coating due to too low volatilization rate and poor corrosion prevention effect of the water can be solved, and the problems of rapid drying of the resin can be solved by increasing the glass transition temperature, but the defects and the defects of poor tensile strength, easy cracking, poor film bottom drying, short activation period and the like are caused.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the resin for the coating of the high-humidity-heat-resistance, long activation period, high-hardness and quick-drying type aqueous optical diffusion film, which has the characteristics of low VOC volatilization, environmental friendliness and the like, has long activation period, can keep the activation period of 5 hours, and overcomes the defects of the existing optical diffusion film.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a resin for a high-humidity heat-resistant, long-activation-period, high-hardness and quick-drying type waterborne optical diffusion film coating comprises the following components in percentage by mass:
10-20 parts of methyl methacrylate, 5-15 parts of hydroxyethyl methacrylate, 3-8 parts of n-butyl methacrylate, 5-20 parts of maleic anhydride novolac epoxy organosilicon adduct, 1-3 parts of acrylic acid, 10-20 parts of styrene, 2.2-9 parts of tert-butyl peroxybenzoate, 0.1-1 part of dodecyl mercaptan, 30-40 parts of ethylene glycol monobutyl ether and 2-5 parts of PMA.
Further, the mass ratio of the resin is as follows:
14 parts of methyl methacrylate, 10 parts of hydroxyethyl methacrylate, 6 parts of n-butyl methacrylate, 12 parts of maleic anhydride novolac epoxy organosilicon adduct, 2 parts of acrylic acid, 16 parts of styrene, 3 parts of tert-butyl peroxybenzoate, 0.3 part of dodecyl mercaptan, 38 parts of butyl cellosolve and 3 parts of PMA.
The preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 10-20 parts of methyl methacrylate, 5-15 parts of hydroxyethyl methacrylate, 3-8 parts of n-butyl methacrylate, 1-3 parts of acrylic acid, 10-20 parts of styrene, 2-7 parts of tert-butyl peroxybenzoate and 0.1-1 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding maleic anhydride novolac epoxy organosilicon adduct and ethylene glycol monobutyl ether, heating and stirring; the ethylene glycol monobutyl ether is based on the proportioning mass of the step 1, the part is 30-40 parts, the part of the maleic anhydride novolac epoxy organosilicon adduct is based on the proportioning mass of the step 1, the part is 5-20 parts, and the temperature for heating and stirring is 136-138 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 0.1-1 part by mass based on the proportioning mass of the step 1, and the third tert-butyl peroxybenzoate is 0.1-1 part by mass based on the proportioning mass of the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
Further, the preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, maleic anhydride novolac epoxy organosilicon adduct, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 14 parts of methyl methacrylate, 10 parts of hydroxyethyl methacrylate, 6 parts of n-butyl methacrylate, 12 parts of maleic anhydride novolac epoxy organosilicon adduct, 2 parts of acrylic acid, 16 parts of styrene, 2.8 parts of tert-butyl peroxybenzoate and 0.3 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding ethylene glycol butyl ether and heating and stirring; the ethylene glycol monobutyl ether is 38 parts based on the proportioning quality in the step 1, and the temperature for heating and stirring is 136-138 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 0.2 part by mass based on the proportioning mass of the step 1, and the third tert-butyl peroxybenzoate is 0.2 part by mass based on the proportioning mass of the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
The viscosity test in the step 3 is a continuous test, the test interval is 15min, and the viscosity change of the two continuous tests is not more than 3 seconds.
When the viscosity is less than 50 seconds, the heat preservation treatment can be continued, a small amount of tert-butyl peroxybenzoate is added, and if the viscosity is more than 60 seconds, ethylene glycol butyl ether is added for dilution.
Further, the mass ratio of the maleic anhydride novolac epoxy organosilicon adduct is as follows:
5-15 parts of maleic anhydride, 10-30 parts of bisphenol A epoxy resin, 30-50 parts of phenolic resin, 1-3 parts of silane coupling agent and 20-40 parts of butyl cellosolve.
Further, the mass ratio of the addition product is as follows: 10 parts of maleic anhydride, 20 parts of bisphenol A epoxy resin, 40 parts of phenolic resin, 2 parts of silane coupling agent and 30 parts of butyl cellosolve.
The preparation method of the adduct comprises the following steps: a1, adding maleic anhydride into a reaction kettle, heating to melt and heat to 140 ℃, adding bisphenol A epoxy resin, controlling the reaction temperature to be about 180 ℃, then adding phenolic resin and a silane coupling agent KH-560, and starting stirring; a2, raising the temperature to 195-200 ℃ for reaction for 3h, and then adding ethylene glycol butyl ether for cooling to obtain an adduct.
According to the invention, due to the introduction of the maleic anhydride novolac epoxy organosilicon adduct, the offline hardness of the final product can reach 2H, the production line efficiency is improved, and the mechanical property and the high-humidity heat resistance are as excellent as those of oiliness; firstly, the double bond in the maleic anhydride and the acrylic acid mixture are copolymerized by free radical initiation, and the addition product is successfully introduced into the acrylic resin; and secondly, unsaturated double bonds in the epoxy resin and acrylic monomers form partial copolymerization through adding an initiator, and an epoxy chain segment is successfully grafted to a main chain of the acrylic resin, most importantly, when an addition product is added to the bottom of a reaction kettle in the reaction process, an acrylic monomer mixture is added into a dropping tank and is dropped, epoxy group organic siloxane and the epoxy resin can generate condensation polymerization reaction with the acrylic monomers in the acrylic mixture at 137 ℃, and the acrylic acid opens epoxy groups in the materials to form links. So that the resin itself forms a multiple network cross-linked structure.
In the reaction process with isocyanate, besides the reaction of conventional NCO and OH, carboxyl in maleic anhydride, phenolic hydroxyl and hydroxymethyl in phenolic resin, hydroxyl in epoxy resin and two hydroxyl groups formed after the ring opening of an ether bond of the epoxy resin, epoxy group and silicon hydroxyl in an organosilicon coupling agent and NCO in an isocyanate curing agent generate multiple chemical crosslinking to form a multiple crosslinking resin network structure, so that the hardness, the surface smoothness, the heat resistance and the crosslinking density of the aqueous optical film are improved to a greater extent.
In addition, due to the introduction of the maleic anhydride novolac epoxy organosilicon adduct, on one hand, the wettability of silicon hydroxyl in an organosilicon monomer to PMMA particles is excellent, and in addition, the resin of a net structure formed by a chain extending structure has excellent wrapping property to the PMMA particles, excellent heat storage stability and high bearing property to the PMMA particles, so that the problems that the conventional water-based acrylic resin prepared optical diffusion film glue filling material has poor bearing property, is easy to settle and needs to be continuously dispersed at high speed to solve industrial pain points of PMMA particle settlement, a water-based optical film prepared by the resin basically can not settle within 3 hours, the problems of bubbles and micropores caused by continuous stirring of PMMA particle settlement in a production line are greatly solved, and the product application range is improved.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention has the characteristics of low VOC volatilization, environmental friendliness and the like, has long activation period, can keep the activation period of 5 hours, and solves the defects of the existing light diffusion film.
2. The hardness of the cable can quickly rise after the cable is off-line, the hardness can reach H after the cable is baked for 1min at 120 ℃, the cable can be directly packaged and bent without curing, and the cable is excellent in boiling resistance.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
Resin for high-humidity-heat-resistance, long-activation-period and high-hardness quick-drying type aqueous optical diffusion film coating
The mass ratio of the maleic anhydride novolac epoxy organosilicon adduct is as follows:
5 parts of maleic anhydride, 10 parts of bisphenol A epoxy resin, 30 parts of phenolic resin, 1 part of silane coupling agent and 20 parts of butyl cellosolve.
The preparation method of the maleic anhydride novolac epoxy organosilicon adduct comprises the following steps: a1, adding maleic anhydride into a reaction kettle, heating to melt and heat to 140 ℃, adding bisphenol A epoxy resin, controlling the reaction temperature to be about 180 ℃, then adding phenolic resin and a silane coupling agent KH-560, and starting stirring; a2, raising the temperature to 195 ℃, reacting for 3 hours, then adding ethylene glycol butyl ether, and cooling to obtain the adduct.
The mass ratio of the resin is as follows:
10 parts of methyl methacrylate, 5 parts of hydroxyethyl methacrylate, 3 parts of n-butyl methacrylate, 5 parts of maleic anhydride novolac epoxy organosilicon adduct, 1 part of acrylic acid, 10 parts of styrene, 2.2 parts of tert-butyl peroxybenzoate, 0.1 part of dodecyl mercaptan, 30 parts of butyl cellosolve and 2 parts of PMA.
The preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 10 parts of methyl methacrylate, 5 parts of hydroxyethyl methacrylate, 3 parts of n-butyl methacrylate, 1 part of acrylic acid, 10 parts of styrene, 2 parts of tert-butyl peroxybenzoate and 0.1 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding maleic anhydride novolac epoxy organosilicon adduct and ethylene glycol monobutyl ether, heating and stirring; the ethylene glycol monobutyl ether is based on the proportioning quality of the step 1, the part is 30 parts, and the part of the maleic anhydride novolac epoxy organic silicon addition compound is based on the proportioning quality of the step 1, the part is 5, and the temperature for heating and stirring is 136 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 0.1 part by mass based on the proportioning mass in the step 1, and the third tert-butyl peroxybenzoate is 0.1 part by mass based on the proportioning mass in the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
The appearance of the maleic anhydride novolac epoxy organosilicon adduct is water white transparent viscous liquid, and the viscosity is 23000cps/25 ℃; the acid value is 50 mgKOH/g.
The results of the basic parameter tests of the resin are as follows
| Verifying items | Test data |
| Adhesion force | 4B |
| Hardness of | f |
| Transmittance (a) | 0.65 |
| Haze/% | 0.87 |
| Surface resistance/omega | 10 12.1 |
Example 2
Resin for high-humidity-heat-resistance, long-activation-period and high-hardness quick-drying type aqueous optical diffusion film coating
The mass ratio of the maleic anhydride novolac epoxy organosilicon adduct is as follows:
15 parts of maleic anhydride, 30 parts of bisphenol A epoxy resin, 50 parts of phenolic resin, 3 parts of a silane coupling agent and 40 parts of butyl cellosolve.
The preparation method of the maleic anhydride novolac epoxy organosilicon adduct comprises the following steps: a1, adding maleic anhydride into a reaction kettle, heating to melt and heat to 140 ℃, adding bisphenol A epoxy resin, controlling the reaction temperature to be about 180 ℃, then adding phenolic resin and a silane coupling agent KH-560, and starting stirring; a2, raising the temperature to 195 ℃, reacting for 3 hours, then adding ethylene glycol butyl ether, and cooling to obtain the adduct.
The mass ratio of the resin is as follows:
20 parts of methyl methacrylate, 15 parts of hydroxyethyl methacrylate, 8 parts of n-butyl methacrylate, 20 parts of maleic anhydride novolac epoxy organosilicon adduct, 3 parts of acrylic acid, 20 parts of styrene, 9 parts of tert-butyl peroxybenzoate, 1 part of dodecyl mercaptan, 40 parts of butyl cellosolve and 5 parts of PMA.
The preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 20 parts of methyl methacrylate, 15 parts of hydroxyethyl methacrylate, 8 parts of n-butyl methacrylate, 3 parts of acrylic acid, 20 parts of styrene, 7 parts of tert-butyl peroxybenzoate and 1 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding maleic anhydride novolac epoxy organosilicon adduct and ethylene glycol monobutyl ether, heating and stirring; the ethylene glycol monobutyl ether is 40 parts by weight based on the proportioning quality of the step 1, the maleic anhydride novolac epoxy organosilicon adduct is 20 parts by weight based on the proportioning quality of the step 1, and the temperature for heating and stirring is 138 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 1 part by mass based on the proportioning mass in the step 1, and the third tert-butyl peroxybenzoate is 1 part by mass based on the proportioning mass in the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
The appearance of the maleic anhydride novolac epoxy organosilicon adduct is water white transparent viscous liquid, and the difficulty is 28000cps/25 ℃; the acid value was 76 mgKOH/g.
The results of the basic parameter tests of the resin are as follows
Example 3
Resin for high-humidity-heat-resistance, long-activation-period and high-hardness quick-drying type aqueous optical diffusion film coating
The mass ratio of the maleic anhydride novolac epoxy organosilicon adduct is as follows:
10 parts of maleic anhydride, 20 parts of bisphenol A epoxy resin, 40 parts of phenolic resin, 2 parts of silane coupling agent and 30 parts of ethylene glycol monobutyl ether.
The preparation method of the maleic anhydride novolac epoxy organosilicon adduct comprises the following steps: a1, adding maleic anhydride into a reaction kettle, heating to melt and heat to 140 ℃, adding bisphenol A epoxy resin, controlling the reaction temperature to be about 180 ℃, then adding phenolic resin and a silane coupling agent KH-560, and starting stirring; a2, raising the temperature to 195 ℃, reacting for 3 hours, then adding ethylene glycol butyl ether, and cooling to obtain the adduct.
The mass ratio of the resin is as follows:
14 parts of methyl methacrylate, 10 parts of hydroxyethyl methacrylate, 6 parts of n-butyl methacrylate, 12 parts of maleic anhydride novolac epoxy organosilicon adduct, 2 parts of acrylic acid, 16 parts of styrene, 3 parts of tert-butyl peroxybenzoate, 0.3 part of dodecyl mercaptan, 38 parts of butyl cellosolve and 3 parts of PMA.
The preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 14 parts of methyl methacrylate, 10 parts of hydroxyethyl methacrylate, 6 parts of n-butyl methacrylate, 2 parts of acrylic acid, 16 parts of styrene, 2.8 parts of tert-butyl peroxybenzoate and 0.3 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding maleic anhydride novolac epoxy organosilicon adduct and ethylene glycol monobutyl ether, heating and stirring; the ethylene glycol monobutyl ether is 38 parts by weight based on the proportioning mass of the step 1, the maleic anhydride novolac epoxy organosilicon adduct is 12 parts by weight based on the proportioning mass of the step 1, and the temperature for heating and stirring is 137 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 0.2 part by mass based on the proportioning mass of the step 1, and the third tert-butyl peroxybenzoate is 0.2 part by mass based on the proportioning mass of the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
The appearance of the maleic anhydride novolac epoxy organosilicon adduct is water white transparent viscous liquid with the difficulty of 26000cps/25 ℃; the acid value is 59 mgKOH/g.
The results of the basic parameter tests of the resin are as follows
| Verifying items | Test data |
| Adhesion force | 4B |
| Hardness of | f |
| Transmittance/% | 0.64 |
| Haze/% | 0.85 |
| Surface resistance/omega | 10 12.0 |
The product of example 3 is used as a test example, the oily hydroxy acrylic resin and the secondary dispersion are used as a comparative example, and the detection data are as follows:
it should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be understood by those skilled in the art that the present invention may be modified and equivalents substituted for elements thereof to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (6)
1. A resin for a high-humidity heat-resistant, long-activation-period, high-hardness and quick-drying type waterborne optical diffusion film coating is characterized in that: the mass ratio is as follows:
10-20 parts of methyl methacrylate, 5-15 parts of hydroxyethyl methacrylate, 3-8 parts of n-butyl methacrylate, 5-20 parts of maleic anhydride novolac epoxy organosilicon adduct, 1-3 parts of acrylic acid, 10-20 parts of styrene, 2.2-9 parts of tert-butyl peroxybenzoate, 0.1-1 part of dodecyl mercaptan, 30-40 parts of ethylene glycol monobutyl ether and 2-5 parts of PMA.
2. The resin for aqueous optical diffusion film coating according to claim 1, characterized in that: the mass ratio of the resin is as follows:
14 parts of methyl methacrylate, 10 parts of hydroxyethyl methacrylate, 6 parts of n-butyl methacrylate, 12 parts of maleic anhydride novolac epoxy organosilicon adduct, 2 parts of acrylic acid, 16 parts of styrene, 3 parts of tert-butyl peroxybenzoate, 0.3 part of dodecyl mercaptan, 38 parts of butyl cellosolve and 3 parts of PMA.
3. The resin for aqueous optical diffusion film coating according to claim 1, characterized in that: the preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 10-20 parts of methyl methacrylate, 5-15 parts of hydroxyethyl methacrylate, 3-8 parts of n-butyl methacrylate, 1-3 parts of acrylic acid, 10-20 parts of styrene, 2-7 parts of tert-butyl peroxybenzoate and 0.1-1 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding maleic anhydride novolac epoxy organosilicon adduct and ethylene glycol butyl ether, heating and stirring; the ethylene glycol monobutyl ether is based on the proportioning mass of the step 1, the part is 30-40 parts, the part of the maleic anhydride novolac epoxy organosilicon adduct is based on the proportioning mass of the step 1, the part is 5-20 parts, and the temperature for heating and stirring is 136-138 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 0.1-1 part by mass based on the proportioning mass of the step 1, and the third tert-butyl peroxybenzoate is 0.1-1 part by mass based on the proportioning mass of the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
4. The resin for aqueous optical diffusion film coating according to claim 3, characterized in that: the preparation method of the resin comprises the following steps:
step 1, uniformly mixing methyl methacrylate, hydroxyethyl methacrylate, n-butyl methacrylate, maleic anhydride novolac epoxy organosilicon adduct, acrylic acid, styrene and a first tert-butyl peroxybenzoate to obtain a mixed solution, and placing the mixed solution into a dropping kettle for later use, wherein the mixed solution comprises the following components in parts by mass: 14 parts of methyl methacrylate, 10 parts of hydroxyethyl methacrylate, 6 parts of n-butyl methacrylate, 12 parts of maleic anhydride novolac epoxy organosilicon adduct, 2 parts of acrylic acid, 16 parts of styrene, 2.8 parts of tert-butyl peroxybenzoate and 0.3 part of dodecyl mercaptan;
step 2, introducing nitrogen into the reaction kettle to form a nitrogen atmosphere; then adding ethylene glycol butyl ether and heating and stirring; the ethylene glycol monobutyl ether is 38 parts based on the proportioning quality in the step 1, and the temperature for heating and stirring is 136-138 ℃;
step 3, dropwise adding the mixed solution obtained in the step 1 into a reaction kettle, adding a second part of tert-butyl peroxybenzoate after dropwise adding is completed within 3 hours, preserving heat for 1 hour, then continuously preserving heat for 1 hour for PMA and a third part of tert-butyl peroxybenzoate until the viscosity is controlled to be 50-60 seconds; the second tert-butyl peroxybenzoate is 0.2 part by mass based on the proportioning mass of the step 1, and the third tert-butyl peroxybenzoate is 0.2 part by mass based on the proportioning mass of the step 1;
and 4, controlling the temperature of the reaction kettle, increasing the temperature from 137 ℃ to 120 ℃ within 0.5h, filtering and packaging to obtain the product.
5. The resin for coating an aqueous optical diffusion film according to claim 3, characterized in that: the viscosity test in the step 3 is a continuous test, the test interval is 15min, and the viscosity change of the two continuous tests is not more than 3 seconds.
6. The resin for coating an aqueous optical diffusion film according to claim 1, characterized in that: the mass ratio of the maleic anhydride novolac epoxy organosilicon adduct is as follows:
5-15 parts of maleic anhydride, 10-30 parts of bisphenol A epoxy resin, 30-50 parts of phenolic resin, 1-3 parts of silane coupling agent and 20-40 parts of butyl cellosolve.
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| CN202210721469.9A CN114940731A (en) | 2022-06-24 | 2022-06-24 | High-humidity-heat-resistance, long-activation-period, high-hardness and quick-drying resin for aqueous optical diffusion film coating |
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| CN202210721469.9A CN114940731A (en) | 2022-06-24 | 2022-06-24 | High-humidity-heat-resistance, long-activation-period, high-hardness and quick-drying resin for aqueous optical diffusion film coating |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070056920A (en) * | 2006-08-02 | 2007-06-04 | 주식회사 카노텍 | Diffusion protecting film and method for preparing the same |
| JP2007138057A (en) * | 2005-11-21 | 2007-06-07 | Soken Chem & Eng Co Ltd | Adhesive composition for optical film and adhesive sheet, and optical member using the same |
| CN104231148A (en) * | 2014-09-28 | 2014-12-24 | 张家港康得新光电材料有限公司 | Hydroxyl acrylic resin and preparation method thereof |
| CN105348998A (en) * | 2015-11-12 | 2016-02-24 | 三棵树涂料股份有限公司 | Organosilicon modified waterborne photo-curing epoxy-acrylic coating and preparation method thereof |
| CN106674441A (en) * | 2017-01-24 | 2017-05-17 | 湘江涂料科技有限公司 | Water-soluble acrylate modified epoxy ester resin and preparation method thereof |
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2022
- 2022-06-24 CN CN202210721469.9A patent/CN114940731A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007138057A (en) * | 2005-11-21 | 2007-06-07 | Soken Chem & Eng Co Ltd | Adhesive composition for optical film and adhesive sheet, and optical member using the same |
| KR20070056920A (en) * | 2006-08-02 | 2007-06-04 | 주식회사 카노텍 | Diffusion protecting film and method for preparing the same |
| CN104231148A (en) * | 2014-09-28 | 2014-12-24 | 张家港康得新光电材料有限公司 | Hydroxyl acrylic resin and preparation method thereof |
| CN105348998A (en) * | 2015-11-12 | 2016-02-24 | 三棵树涂料股份有限公司 | Organosilicon modified waterborne photo-curing epoxy-acrylic coating and preparation method thereof |
| CN106674441A (en) * | 2017-01-24 | 2017-05-17 | 湘江涂料科技有限公司 | Water-soluble acrylate modified epoxy ester resin and preparation method thereof |
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