CN102676064B - Matte adhesive and preparation method thereof - Google Patents
Matte adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a matte adhesive and a preparation method thereof. The matte adhesive is composed of a component A and a component B according to weight proportion as 1:10-10:1. The method includes the steps of first, preparing the component A and the component B respectively and then evenly mixing the component A and the component B according to the weight ratio as 1:10-10:1 during use.The matte adhesive has the advantages of being high in adhesion reliability, toughness, corrosion resistance and strength, wide in application range, and the like.
Description
Technical field
The present invention relates to a kind of inferior light sizing agent and preparation method thereof, belong to the agent of Resins, epoxy gluing and CALCIUM ACRYLATE sizing agent field.
Background technology
People liked as bright as a sixpence high gloss high-brightness surface material more in the past, but along with the raising of people to the living environment requirement, realize that high-gloss surface is under the irradiation of light, eyes to the people have hormesis, the sensation that is in this class environment people for a long time can be uncomfortable, therefore people begin gloss softly, and the inferior luminescent material that human eye is had no stimulation causes the demand.Inferior luminescent material refers to surfacing, but delustring processing, the material more weak to reflection of light were carried out in the surface.More representational is lacquer class coating, the glossiness of clear lacquer is very high, if surface-treated is good, then has the sensation of minute surface, if but the surface is smooth inadequately, as long as some flaws are arranged, will be easy to be found, clear lacquer is in case damaged, will produce inharmonic sensory handicaps, and be in for a long time in the high reflective environment, it is nervous tired out that people can feel, so begin to produce the demand to inferior optical coating.Usual finishing is used sub-gloss varnish, and softer on the sense organ, the people is in such environment, feels also pleasant.This raising to the people living environmental requirement, beginning expands every field gradually to, and in the electronic enterprises, people also begin to have proposed the demand to inferior light aspect.
Esters of acrylic acid sizing agent and epoxy adhesive that electronic apparatus is commonly used, because solidifying the rear surface, it presents the light state, can not satisfy the requirement of inferior light, therefore in component design, need to consider to realize inferior light by specific method, modal is to add matting agent, adds oarse-grained filler, adopts the methods such as solidifying agent of inferior light.And we know that these class methods are done like this and can be met the demands in the application of aspects such as coating, but, at the electronic apparatus production field, in order to raise the efficiency, generally take to improve the method that solidification value improves curing speed, present common inferior optical cement, though be inferior light to a certain extent, with the raising of solidification value, its surface presents the trend of light gradually, therefore can not satisfy client's demand, between the two, have very big contradiction in production efficiency and product quality.
In order to solve the problem of appearance, we must seek new method, method is at first wanted the surface property of research material, and how the surface of inferior light and light occurs actually, and data shows, whether the surface of material is light, relevant with its surperficial reflective function, if the smooth surface of material is smooth, when incident light touches material surface, be easy to be reflected, thereby cause the shinny sensation in surface to the people; On the contrary, if the surface is hackly, incident light forms diffuse-reflectance on the surface, and the reflectivity that causes is so disperseed, and people just can not feel more intense reflected light on sense organ, thereby sense-data is inferior light.
Can know from the analysis of above optics, in order to realize inferior light, need start with from forming shaggy direction, and traditional methods such as interpolation matting agent, also be to realize same purpose, but in order also to satisfy inferior light under the situation that can be implemented in hot setting, then must consider new direction.
Characteristic from sizing agent, form diffuse-reflectance in order to realize the coarse of solidified surface, best mode is to cause the variation of the cure shrinkage of system by ad hoc approach, thereby produces the coarse of surface, so the present invention has designed two kinds of cure systems that the cure shrinkage degree is different of existence in the curing system, thereby be implemented in the solidification process, two system's shrinking percentage differences interact in the solidification process, cause the coarse injustice on surface, form the diffuse-reflectance basis, thereby realized inferior light.
Summary of the invention
Technical problem to be solved by this invention provides a kind of inferior light sizing agent and preparation method thereof, solidify the rear surface light to overcome common sizing agent, perhaps heat up to solidify the back and produce the problem of light, to satisfy people simultaneously because the demand of enhancing productivity needs intensification fast setting and solidifying the inferior light in back.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of inferior light sizing agent is that 1: 10～10: 1 A component and B component formed by weight proportion,
Described A component is made up of following each raw material in the percentage composition of A component gross weight: Resins, epoxy accounts for 30～60%, thinner accounts for 2～15%, filler accounts for 25～40%, the active coupling agent of silane accounts for 0～1%, dyestuff accounts for 0～1%, defoamer accounts for 0～1%, solidifying agent accounts for 5～20%;
Described B component is made up of following each raw material in the percentage composition of B component gross weight: CALCIUM ACRYLATE accounts for 20～75%, filler accounts for 25～78%, the BPO initiator accounts for 0.1～1%, stabilizer comprises 0～0.9%.
The invention has the beneficial effects as follows: adopt epoxy-resin systems, after curing, have the high tenacity of Resins, epoxy gluing agent in its structure, erosion resistance, advantages such as water tolerance; Adopt the CALCIUM ACRYLATE system, after curing, have the high strength of CALCIUM ACRYLATE sizing agent in its structure, high-modulus, advantages such as weather resisteant.After the two was mixing cured, the material after the curing had had the advantage of two class sizing agents concurrently, and has produced micron-scale phase separation in solidification process, had formed fine and close phase and loose alternate two-phase network structure, caused the coarse of solidified surface, had reached the effect of inferior light.And the system after solidifying, gluing reliability height, the scope of application is extensive.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described Resins, epoxy is the organic compound that contains two or more epoxide groups, typically refers to a kind of or several mixing arbitrarily in bisphenol A epoxide resin, bisphenol F epoxy resin, multi-functional epoxy's basic ring epoxy resins, the phenol aldehyde type epoxy resin.
Adopt the beneficial effect of above-mentioned further scheme to be: to adopt Resins, epoxy, can after curing, have the high tenacity of Resins, epoxy gluing agent in its structure, erosion resistance, advantages such as water tolerance.
Further, described thinner is the epoxy resin diluent of difunctionality;
Further, described epoxy resin diluent is ethylene glycol bisthioglycolate contracting glyceryl ether, butanediol diglycidyl ether, 1, a kind of or several mixing arbitrarily in 2-cylohexanediol diglycidyl ether, the resorcinol diglycidyl ether.
Adopt the beneficial effect of above-mentioned further scheme to be: thinner can have enough low viscosity by guarantee system, reduces cost and optimizes matt effect thereby can add more filler.
Further, described filler is mineral filler;
Further, described mineral filler is any one in hydrophobic type silicon powder, calcium carbonate, silicate, diatomite, kaolin, the ball-shaped silicon micro powder;
Adopt the beneficial effect of above-mentioned further scheme to be: the adding of mineral filler can produce the effect of delustring to a certain extent.
Further, described dyestuff is carbon black 101;
Further, described defoamer is silane coupling agent;
Adopt the beneficial effect of above-mentioned further scheme to be: coupling agent can guarantee to solidify organic phase and inorganic abundant combination mutually in the system of back, can fully eliminate the bubble that system produces in the technological process, guarantees the quality of glue.
Further, described solidifying agent is latent epoxy resin curing agent;
Further, described latent epoxy resin curing agent is any one among aginomoto PN series, Chkawai MC120D, Fuqing 8000K, the common calla 101s;
Further, described stablizer is Resorcinol;
Further, described CALCIUM ACRYLATE is a kind of or several mixing arbitrarily in methyl methacrylate, Jia Jibingxisuanyizhi, hydroxy methyl methacrylate, the hydroxyethyl methylacrylate;
Adopt the beneficial effect of above-mentioned further scheme to be: to adopt CALCIUM ACRYLATE, can after curing, have the high strength of Resins, epoxy gluing agent in its structure, high-modulus, weather resisteant etc.;
Another technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of inferior light sizing agent comprises the preparation process of A component and the preparation process of B component; Wherein,
The preparation process of described A component is as follows: in the percentage composition of A component gross weight, take by weighing 30～60% Resins, epoxy, 2～15% thinner, 25～40% filler, 0～1% the active coupling agent of silane, 0～1% dyestuff, 0～1% defoamer, 5～20% solidifying agent, successively above-mentioned materials is added in the stirrer, vacuumize, stir, naturally hang to room temperature, pack, namely get described A component;
The preparation process of described B component is as follows: in the percentage composition of B component gross weight, take by weighing 20～70% CALCIUM ACRYLATE, 25～78% filler, 0.1～1% BPO initiator, 0～0.9% stablizer, successively above-mentioned materials is added in the stirrer, vacuumize, stir, naturally hang to room temperature, pack, namely get described B component.
During use, be that 1: 10～10: 1 proportioning mixes by weight with described A component, B component, can carry out bonding.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in the preparation process of described A component and in the preparation process of described B component, the described vacuum tightness that vacuumizes is-0.08～-0.05MPa.
Further, in the preparation process of described A component and in the preparation process of described B component, the processing condition of described stirring are: mixing speed is 500～1000 rev/mins, and churning time is 0.5～2 hour.
Embodiment
Following institute gives an actual example and only is used for explaining the present invention, is not for limiting scope of the present invention.
Embodiment 1
The preparation of A component: take by weighing SST-2390 no-solvent type polyurethane modified epoxy resin 34g, ethylene glycol bisthioglycolate contracting glyceryl ether 5g, hydrophobic type silicon powder 39.5g, KH560 coupling agent 1g, carbon black 101 dyestuff 0.5g, PN40 solidifying agent 20g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 0.5 hour in 500 rev/mins, stir, naturally hang to room temperature, pack and get final product.
The preparation of B component: take by weighing methymethacrylate 38.1g, 600 order silicon powder 60g, BPO initiator 1g, stablizer Resorcinol 0.9g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 0.5 hour in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
A component and B component mix by weight 1: 10 proportioning.
Embodiment 2
The preparation of A component: take by weighing DOW Chemical straight chain type aliphatics snappiness epoxy DER-732 resin 27g, the toughness reinforcing MX125 Resins, epoxy of Japanese core shell rubbers 20g, butanediol diglycidyl ether 2g, calcium carbonate 35g, KH560 coupling agent 0.5g, carbon black 101 dyestuff 0.5g, 101S solidifying agent 15g, add in the stirrer successively, being evacuated to vacuum tightness is-0.05MPa, stirred 2 hours in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
The preparation of B component: take by weighing methacrylic acid second fat 69g, calcium carbonate 30g, BPO initiator 1g, add successively in the stirrer, be evacuated to vacuum tightness and be-0.07MPa, stirred 1.5 hours in 500 rev/mins, stir, hang naturally to room temperature, pack and get final product.
A component and B component mix by weight 10: 1 proportionings.
Embodiment 3
A component preparation: take by weighing shell 828 Resins, epoxy 51g, 1,2-cylohexanediol diglycidyl ether 2g, diatomite 25g, KH560 coupling agent 1g, carbon black 101 dyestuff 1g, PN23 solidifying agent 20g, add in the stirrer successively, being evacuated to vacuum tightness is-0.06MPa, stirred 1 hour in 800 rev/mins, stir, hang naturally to room temperature, pack and get final product.
B component preparation: take by weighing hydroxyethyl methacrylate formicester 21g, silicate 78g, BPO initiator 0.5g, stablizer Resorcinol 0.5g, add in the stirrer successively, being evacuated to vacuum tightness is-0.06MPa, stirred 1 hour in 600 rev/mins, stir, naturally hang to room temperature, pack and get final product.
A component and B component mix by weight 1: 1 proportioning.
Embodiment 4
The preparation of A component: take by weighing DOW Chemical straight chain type aliphatics snappiness epoxy DER-755 resin 26.5g, the aliphatic diol Resins, epoxy XZ02466.00 compound 18.5g of aromatic epoxies end-blocking, resorcinol diglycidyl ether 3g, kaolin 40g, KH560 coupling agent 1g, carbon black 101 dyestuff 0.5g, MC120D solidifying agent 10.5g, add in the stirrer successively, being evacuated to vacuum tightness is-0.07MPa, stirred 1.5 hours in 600 rev/mins, stir, naturally hang to room temperature, pack and get final product.
The preparation of B component: take by weighing hydroxyethyl methacrylate second fat 45g, diatomite 54.5g, BPO initiator 0.3g, stablizer Resorcinol 0.2g, add in the stirrer successively, being evacuated to vacuum tightness is-0.05MPa, stirred 2 hours in 600 rev/mins, stir, naturally hang to room temperature, pack and get final product.
A component and B component are that 3: 7 proportionings mix by weight.
Embodiment 5
The preparation of A component: take by weighing epoxy terminated aliphatic diol flexible chain epoxy XZ92465.00 resin 46g, N10 thinner 5g, ball-shaped silicon micro powder 40g, KH560 coupling agent 0.5g, carbon black 101 dyestuff 0.5g, 8000K solidifying agent 8g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 2 hours in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
The preparation of B component: take by weighing hydroxyethyl methacrylate formicester 35g, hydroxyethyl methacrylate formicester 25g, kaolin 39g, BPO initiator 0.5g, stablizer Resorcinol 0.5g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 0.5 hour in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
A component and B component mix by weight 7: 3 proportionings.
Embodiment 6
The preparation of A component: take by weighing epoxy terminated aliphatic diol flexible chain epoxy XZ92465.00 resin 30g, N10 thinner 15g, ball-shaped silicon micro powder 40g, KH560 coupling agent 0.5g, carbon black 101 dyestuff 0.5g, 8000K solidifying agent 14g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 2 hours in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
The preparation of B component: take by weighing hydroxyethyl methacrylate formicester 20g, kaolin 78g, BPO initiator 0.1g, stablizer Resorcinol 0.9g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 0.5 hour in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
A component and B component mix by weight 2: 3 proportionings.
Embodiment 7
The preparation of A component: take by weighing SST-2390 no-solvent type polyurethane modified epoxy resin 60g, ethylene glycol bisthioglycolate contracting glyceryl ether 5g, hydrophobic type silicon powder 28g, KH560 coupling agent 1g, carbon black 101 dyestuff 1g, PN40 solidifying agent 5g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 0.5 hour in 500 rev/mins, stir, naturally hang to room temperature, pack and get final product.
The preparation of B component: take by weighing methymethacrylate 74.8g, 600 order silicon powder 25g, BPO initiator 0.1g, stablizer Resorcinol 0.1g, add in the stirrer successively, being evacuated to vacuum tightness is-0.08MPa, stirred 0.5 hour in 1000 rev/mins, stir, naturally hang to room temperature, pack and get final product.
A component and B component mix by weight 3: 2 proportionings.
Performance by following experimental test inferior light sizing agent of the present invention.
At first by the matt effect behind the outward appearance judgement products solidifying, pass through hardness then respectively, tensile strength, performances such as shearing resistance and modulus characterize, and sample and the existing common double component epoxy sizing agent with embodiment 1-5 carries out property comparison at last.
Test example 1 outward appearance contrast test
Outward appearance contrast test scheme is carried out by the following method: behind the sample and existing common inferior light sizing agent curing with embodiment 1-5, judge final matt effect by observing, the result is as shown in table 1.
Table 1 embodiment 1-5 and common inferior light sizing agent outward appearance contrast test result
| Sample | Outward appearance |
| The sample of embodiment 1 | Quan Yaguang |
| The sample of embodiment 2 | Quan Yaguang |
| The sample of embodiment 3 | Quan Yaguang |
| The sample of embodiment 4 | Quan Yaguang |
| The sample of embodiment 5 | Quan Yaguang |
| Comparative example's sample | Half inferior light |
Shore hardness test under test example 2 differing tempss
Hardness test: test according to GB/T 531-1999
The hardness test embodiment is carried out by the following method: after the sample of embodiment 1-5 and existing common inferior light sizing agent are solidified, tests respectively at 0 ℃ according to GB/T 531-1999, and 25 ℃, the hardness under 65 ℃ of conditions.Concrete data see Table 2.
Table 2 embodiment 1-5 and common inferior light sizing agent Shore hardness contrast test result
The test of test example 3 tensile strengths
Tensile strength test: test according to GB/T528-1998;
Tensile strength test implementation scheme is carried out by the following method: behind the sample and existing common inferior light sizing agent curing with embodiment 1-5, according to the GB/T528-1998 test tensile strength.Concrete data see Table 3.
Table 3 embodiment 1-5 and common inferior light sizing agent tensile strength contrast test result
The test of test example 4 shearing resistances
Shearing resistance test: test according to GB/T7124-1986.
Shearing resistance test implementation scheme is carried out by the following method: behind the sample and existing common inferior light sizing agent curing with embodiment 1-5, according to GB/T7124-1986 test shearing resistance.Data see Table 4.
Table 4 embodiment 1-5 and common inferior light sizing agent shearing resistance test result
| Sample | Shearing resistance performance test (Mpa) |
| The sample of embodiment 1 | 13.3 |
| The sample of embodiment 2 | 12.9 |
| The sample of embodiment 3 | 12.8 |
| The sample of embodiment 4 | 13.5 |
| The sample of embodiment 5 | 13.2 |
| Comparative example's sample | 11.4 |
The test of test example 5 modulus
Modulus strength test embodiment is carried out by the following method: behind the sample and existing common inferior light sizing agent curing with embodiment 1-5, the preparation standard batten uses DMA test modulus, 25 ℃ and 65 ℃ two temperature spots of value then.Concrete data see Table 5.
Table 5 embodiment 1-5 and common inferior light sizing agent modulus contrast test result
From above data analysis, the embodiment sample after having obtained completely matt effect, shore hardness, tensile strength, shearing resistance, performances such as modulus contrast with comparative example result, every performance all is better than the comparative example, and inferior light sizing agent of the present invention is described, is the novel sizing agent of a class.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. an inferior optical cement sizing agent is characterized in that, is that A component and the B component of 1:10～10:1 formed by weight proportion,
Described A component is made up of following each raw material in the percentage composition of A component gross weight: Resins, epoxy accounts for 30～60%, thinner accounts for 2～15%, filler accounts for 25～40%, silane coupling agent accounts for 0～1%, dyestuff carbon black 101 accounts for 0～1%, defoamer accounts for 0～1%, solidifying agent accounts for 5～20%; Get silane coupled agent content and be 0 and antifoam content be not 0 technical scheme;
Described latent epoxy resin curing agent is any one among aginomoto PN series, the Chkawai MC120D; Described defoamer is the KH560 coupling agent; Described thinner is ethylene glycol bisthioglycolate contracting glyceryl ether, butanediol diglycidyl ether, 1, a kind of or several mixing arbitrarily in 2-cylohexanediol diglycidyl ether, the resorcinol diglycidyl ether;
Described B component is made up of following each raw material in the percentage composition of B component gross weight: acrylate accounts for 20～75%, filler accounts for 25～78%, the BPO initiator accounts for 0.1～1%, the stablizer Resorcinol accounts for 0～0.9%, and each raw material sum of described B component is 100%;
Described acrylate is a kind of or several mixing arbitrarily in methyl methacrylate, Jia Jibingxisuanyizhi, hydroxy methyl methacrylate, the hydroxyethyl methylacrylate;
Filler in described A component and the B component is any one in hydrophobic type silicon powder, calcium carbonate, silicate, diatomite, kaolin, the ball-shaped silicon micro powder.
2. a kind of inferior light sizing agent according to claim 1 is characterized in that described Resins, epoxy is the organic compound that contains two above epoxide groups.
3. a kind of inferior light sizing agent according to claim 2 is characterized in that, described Resins, epoxy is a kind of or several mixing arbitrarily in bisphenol A epoxide resin, bisphenol F epoxy resin, the multi-functional epoxy's basic ring epoxy resins.
4. the preparation method as the arbitrary described inferior light sizing agent of claim 1-3 is characterized in that, comprises the preparation process of A component and the preparation process of B component; Wherein,
The preparation process of described A component is as follows: in the percentage composition of A component gross weight, take by weighing 30～60% Resins, epoxy, 2～15% thinner, 25～40% filler, 0～1% silane coupling agent, 0～1% dyestuff carbon black 101,0～1% defoamer, 5～20% solidifying agent, get silane coupled agent content and be 0 and antifoam content be not 0 technical scheme, successively above-mentioned materials is added in the stirrer, vacuumize, stir, naturally hang to room temperature, pack, namely get described A component;
The preparation process of described B component is as follows: in the percentage composition of B component gross weight, take by weighing 20～75% acrylate, 25～78% filler, 0.1～1% BPO initiator, 0～0.9% stablizer Resorcinol, each raw material sum of described B component is 100%, successively above-mentioned materials is added in the stirrer, vacuumize, stir, hang naturally to room temperature, pack, namely get described B component;
During use, described A component and described B component are mixed for the proportioning of 1:10～10:1 by weight.
5. the preparation method of a kind of inferior light sizing agent according to claim 4 is characterized in that, in the preparation process of described A component and in the preparation process of described B component, the described vacuum tightness that vacuumizes is-0.08～-0.05MPa.
6. the preparation method of a kind of inferior light sizing agent according to claim 4, it is characterized in that, in the preparation process of described A component and in the preparation process of described B component, the processing condition of described stirring are: mixing speed is 500～1000 rev/mins, and churning time is 0.5～2 hour.
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| CN104057653A (en) * | 2014-06-13 | 2014-09-24 | 江苏悦达新材料科技有限公司 | Graphite membrane/metal composite cooling fin and preparation method thereof |
| CN104327780A (en) * | 2014-10-23 | 2015-02-04 | 招远鸿瑞印染有限公司 | Double-component epoxy bonding material |
| CN106318227A (en) * | 2016-08-23 | 2017-01-11 | 武汉科技大学 | Organic-inorganic compound adhesive with elasticity and oxidization resistance and use method of organic-inorganic compound adhesive |
| CN107983603A (en) * | 2018-01-30 | 2018-05-04 | 成都正恒动力股份有限公司 | Engine cylinder body micropore sealing technology |
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| WO2005073763A1 (en) * | 2004-01-29 | 2005-08-11 | Nippon Paint Co., Ltd. | Antidazzle coating composition, antidazzle film and process for producing the same |
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