CN107312456B - Composition for protecting liquid crystal circuit and preparation method thereof - Google Patents

Composition for protecting liquid crystal circuit and preparation method thereof Download PDF

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CN107312456B
CN107312456B CN201710607997.0A CN201710607997A CN107312456B CN 107312456 B CN107312456 B CN 107312456B CN 201710607997 A CN201710607997 A CN 201710607997A CN 107312456 B CN107312456 B CN 107312456B
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liquid crystal
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葛鑫
庞小燕
葛建芳
辛展
张桂云
蒲侠
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Zhongkai University of Agriculture and Engineering
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    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The invention relates to the field of circuit protection materials, and discloses a composition for protecting a liquid crystal circuit and a preparation method thereof. The composition for protecting the liquid crystal circuit comprises the following components in parts by weight: 10-30 parts of hydrogenated styrene-butadiene block copolymer and petroleum resin, 0.5-3.6 parts of boron nitride, 10-20 parts of naphthenic oil, 60-70 parts of main solvent and auxiliary solvent and 0.3-1 part of fluorine-containing auxiliary agent. The prepared protective composition has the advantages of high film strength, good tensile property, difficult tearing, good barrier property, capability of improving the moisture resistance of the film and wide application prospect.

Description

Composition for protecting liquid crystal circuit and preparation method thereof
Technical Field
The invention relates to the field of circuit protection materials, in particular to a composition for protecting a liquid crystal circuit and a preparation method thereof.
Background
With the development of the world to the information society, the importance of display devices as key components of human-computer interaction is increasing, and various displays such as liquid crystal display, plasma PDP display, organic light emitting OLED display, and the like are being developed vigorously. Anisotropic Conductive Film (ACF) is a material for connecting a display and a driving circuit in a chemical bonding mode, and realizes Z-direction conduction and X-Y-direction insulation through high polymer microspheres coated with metal layers on the surfaces. However, the products of domestic manufacturers have poor strength, coating film property, moisture resistance and humidity resistance, adhesion and strippability, are easy to break and have undesirable effects.
Disclosure of Invention
The invention aims to provide a composition for protecting a liquid crystal circuit.
In order to achieve the purpose, the invention adopts the following technical scheme:
the composition for protecting the liquid crystal circuit comprises the following components in parts by weight: 10-30 parts of hydrogenated styrene-butadiene block copolymer and petroleum resin (SEBS), 0.5-3.6 parts of boron nitride, 10-20 parts of naphthenic oil, 60-70 parts of main solvent and auxiliary solvent and 0.3-1 part of fluorine-containing auxiliary agent.
Preferably, the fluorine-containing auxiliary agent is a fluorine-containing siloxane coupling agent. The film formed by the liquid crystal circuit protection composition is non-wettable, and the total average contact angle can be rapidly increased after the fluorine-containing siloxane coupling agent is added, so that the hydrophobic property of the system is greatly improved, and the strippability of the prepared film is improved.
Preferably, the auxiliary solvent is one or a mixture of two of trimethyl ketone alcohol and hydroxypropyl acrylate, and the main solvent is preferably methyl cyclohexane, cyclohexane or n-hexane. The viscosity of the methylcyclohexane solution of SEBS can be obviously reduced after the trimethyl ketone alcohol and the hydroxypropyl acrylate are added, so that the operation performance is improved.
Preferably, the liquid crystal circuit protecting composition further comprises not more than 0.5 parts by weight of a blue dye. This allows the color of the resulting film to be adjusted.
Another object of the present invention is to disclose the preparation method of the above composition for protecting a liquid crystal circuit, comprising the steps of:
s1: drying the hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours according to the parts by weight;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to the mixed solvent of the auxiliary solvent and the main solvent with stirring;
s3: adding other raw materials into the mixture prepared in the step S2, and stirring the mixture uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
BN is a synthetic non-oxide ceramic material which is an isoelectric substance with C2, so the BN has a similar crystal structure with a carbon simple substance, has a plurality of characteristics, and has excellent physicochemical characteristics of thermal vibration resistance, high temperature resistance, high thermal conductivity, oxidation resistance, high resistivity, high dielectric property, self lubrication, low density, chemical corrosion resistance, good processability, non-infiltration with various metals and the like. The BN is added into the composite material, so that the advantages of the BN ceramic can be fully exerted, the defects of low mechanical property and poor rain erosion resistance of a single-phase BN ceramic material can be overcome, and the antioxidant coating and the heat-conducting heat-resisting composite material with excellent comprehensive properties can be obtained.
Naphthenic oil can be used to improve the light transmission performance of the system and increase the transparency of the system. After the plasticizer is added, the melt viscosity of the SEBS can be reduced, and the coating process is facilitated; the initial viscosity of the SEBS is increased, and the low-temperature flexibility is improved; and reduces the cost.
The petroleum resin plays a role in tackifying. Because the SEBS has no adhesiveness, after the SEBS is added with petroleum resin, the cohesion, the peel strength and the shear strength can be improved, the permanent adhesive strength is increased, the melt viscosity of the mixture is reduced, the wettability of the adhered material is improved, and the operating performance is improved.
The composition for protecting the liquid crystal circuit has the advantages that the raw materials are easy to obtain, heterogeneous materials are added into homogeneous materials to produce an interface, and the interface can absorb the external force impact, so that the strength is improved, the process flow is simple, and the cost performance is high. The used solvent and the auxiliary agent are environment-friendly and nontoxic, the production is efficient and safe, the leftover materials can be recycled without influencing the performance of the product, and the environment-friendly effect is conformed. The prepared protective composition film has the following advantages: 1. good film forming property and moderate flexibility. 2. Excellent mechanical strength and excellent atmospheric resistance. 3. Good barrier property, and the prepared film has excellent moisture resistance.
Detailed Description
In the examples of the present invention, a hydrogenated styrene-butadiene block copolymer (SEBS) was obtained from Takekuan rubber (Shanghai) industries, Ltd., type Kraton G1650; the silane coupling agent is purchased from Jie chemical technology Co., Ltd, Guangzhou city, and has the model of KH-550; the petroleum resin is purchased from Ison chemical Co., Ltd, Qingdao, and the model is LH 100-1; methylcyclohexane was purchased from cantonese chemical ltd; naphthenic oil was purchased from flex chemical, Inc., Guangzhou.
In the embodiment of the invention, the viscosity test is carried out according to the national standard GB 12005.1-89; the determination of the mechanical property is carried out according to the national standard GB/T528-2009; the torque test is carried out by using a torque tester after the sample is pressed and prepared; infrared spectroscopic analysis was performed using a GBT21186-2007 Fourier transform infrared spectrometer.
The present invention will be further described with reference to the following examples.
Example 1
SEBS is dissolved in methylcyclohexane to prepare a solution of 2g/dl, and the outflow time t is measured00.01mL of the solution was taken out for 147.50s, 10 parts of the solution were taken out, 6 different solvents of ethyl acetate, isobutyl acetate, trimethylketol, toluene, hydroxypropyl acrylate and butyl acrylate were added dropwise to each of the solutions, 0.01mL of each solvent was added dropwise to 0.07mL of each solvent, and the average flow-out time of each group of the solutions was measured, and the amount of change in the flow-out time of the solution was determined according to the following equation,
Figure BDA0001358844500000033
to average outflow time, t0147.50s, and r is the amount of change in the outflow time. The results are shown in Table 1.
Figure BDA0001358844500000031
< Table 1>
Figure BDA0001358844500000032
Figure BDA0001358844500000041
It can be shown that the viscosity of the solution is obviously reduced after adding the trimethyl ketol or hydroxypropyl acrylate into the methylcyclohexane solution of SEBS, which indicates that the three liquids are suitable to be used as the solvents of the system; after the ethyl acetate, the isobutyl acetate or the butyl acrylate are added, the viscosity of a mixed system is not changed greatly and the mixed system is not suitable for being used as a solvent of a basic solution; in addition, after toluene is added, the viscosity of a mixed system is increased on the contrary, and the viscosity reduction effect cannot be realized, which further indicates that the solutions are not suitable to be used as solvents of base solutions.
Example 2
Petroleum resin was added to the methylcyclohexane solution of SEBS in different proportions, and the mechanical properties of the resulting solution after film formation were tested, with the results shown in table 2. It can be seen that as the amount of petroleum resin used increases, the total elongation at break of the sample increases, the tensile strength decreases, the modulus of elasticity decreases, and the maximum tensile stress decreases. On one hand, the relative molecular mass of petroleum resin is lower than that of rubber, and petroleum resin molecules are mixed among rubber molecular chains to play a lubricating role, so that the chains are easy to extend and move; on the other hand, the molecular chain of the resin is linear, so that the resin is easy to stretch and orient under external force. SEBS and petroleum resin are blended to become soft and tough, and the mixture has excellent performances of strong flexibility, good scratch resistance, easy integral peeling and the like after being formed into a film.
< Table 2>
Figure BDA0001358844500000042
Example 3
Naphthenic oil was added to methylcyclohexane solutions of SEBS in different proportions, and the mechanical properties of the resulting solutions after film formation were tested, with the results shown in table 3. It can be seen that the modulus of elasticity, maximum tensile stress, tensile strength, and total elongation at break are all reduced with the addition of naphthenic oil. When the addition of the naphthenic oil is increased from 0 to 25 percent, the maximum tensile stress, the tensile strength and the elastic modulus of the SEBS are reduced greatly, and the total elongation at break is reduced slowly; when the addition amount of the naphthenic oil is more than 25 percent, the total elongation at break of the SEBS is suddenly reduced from 9.3 percent to 6.09 percent, and the maximum tensile stress and the elastic modulus and the tensile strength are in a slow reduction trend.
< Table 3>
Figure BDA0001358844500000051
Example 4
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 40g of trimethylketone and 30g of methylcyclohexane with stirring;
s3: adding 16g of petroleum resin, 10g of naphthenic oil, 0.3g of KH-550 type silane coupling agent and 0.5g of boron nitride into the mixture prepared in the step S2, and stirring uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
Example 5
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 30g of hydroxypropyl acrylate and 30g of cyclohexane with stirring;
s3: adding 20g of petroleum resin, 20g of naphthenic oil, 1g of KH-550 type silane coupling agent and 1.7g of boron nitride into the mixture prepared in the step S2, and stirring uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
Example 6
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 35g of trimethylketone and 30g of cyclohexane with stirring;
s3: adding 14g of petroleum resin, 15g of naphthenic oil, 0.6g of KH-550 type silane coupling agent, 2.6g of boron nitride and 0.5g of blue dye into the mixture prepared in the step S2, and stirring uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
Example 7
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 30g of trimethylketone and 35g of n-hexane with stirring;
s3: adding 10g of petroleum resin, 13g of naphthenic oil, 0.7g of KH-550 type silane coupling agent, 1.5g of boron nitride and 0.08g of blue dye into the mixture prepared in the step S2, and stirring uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
Example 8
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 32g of trimethylketone and 35g of n-hexane with stirring;
s3: adding 15g of petroleum resin, 18g of naphthenic oil, 0.9g of KH-550 type silane coupling agent, 3.6g of boron nitride and 0.08g of blue dye into the mixture prepared in the step S2, and stirring uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
Comparative example 1
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 30g of hydroxypropyl acrylate and 30g of cyclohexane with stirring;
s3: adding 20g of petroleum resin, 20g of naphthenic oil and 1g of KH-550 type silane coupling agent into the mixture prepared in the step S2, and stirring the mixture uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
Comparative example 2
The composition for protecting a liquid crystal circuit of the present example was prepared by the following steps:
s1: drying 10g of hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to a mixed solvent of 30g of hydroxypropyl acrylate and 30g of cyclohexane with stirring;
s3: to the mixture obtained in step S2 were added 20g of petroleum resin, 20g of naphthenic oil, 1g of KH-550 type silane coupling agent, 1.7g of aluminum silicate (Al)2SiO5) Stirring to be uniform;
s4: filtering insoluble substances, defoaming, and packaging.
Effects of the embodiment
The compositions of example 5, comparative example 1 and comparative example 2 were formed into films, and then bottles containing the color-changing silica gel were sealed and left to stand for 150 days, and the color change of the color-changing silica gel in the bottles was observed, and the results are shown in Table 4.
TABLE 4 Effect of inorganic Filler on Water vapor Barrier Properties of protective films
Figure BDA0001358844500000071
It can be seen from table 4 that the water vapor barrier property of the non-reinforced SEBS film under natural conditions is poor, within 30 days, a small amount of water vapor enters the bottle through the film, the color of the silica gel changes from dark blue to blue, 90 days later, the water vapor entering the bottle increases, the silica gel changes into light blue, and 150 days later, the original dark blue of the silica gel changes into light purple red, which indicates that the water vapor barrier property of the film is good, and the film is not beneficial to playing the barrier protection role. When the filler is added for reinforcement, the water vapor barrier property of the film is obviously improved, after 90 days of adding the aluminum silicate, the color of the silica gel is changed from dark blue to blue, and is changed into light blue after 150 days, compared with the original color, the color change time of the silica gel is prolonged, which shows that the barrier property of the material is greatly improved; and after the boron nitride is added, the barrier property of the film is improved more remarkably, the silica gel is changed from deep blue to blue, and the effect is better than that of the former two after the long-time span of 150 days. The boron nitride nano sheet structure is mainly benefited from a special nano sheet structure of boron nitride, is added into a system to perform organic-inorganic hybridization with SEBS after surface chemical modification, and greatly reduces the moisture permeability of the material by virtue of the barrier property expressed by the sheet structure. The diameter of the boron nitride is very small and reaches the nanometer level, so that the comprehensive performance of the material can be improved by utilizing the nanometer effect of the boron nitride when the boron nitride is filled into a high polymer material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be encompassed by the present invention.

Claims (3)

1. The composition for protecting the liquid crystal circuit is characterized by comprising the following components in parts by weight: 10-30 parts of hydrogenated styrene-butadiene block copolymer and petroleum resin, 0.5-3.6 parts of boron nitride, 10-20 parts of naphthenic oil, 60-70 parts of main solvent and auxiliary solvent and 0.3-1 part of fluorine-containing auxiliary agent, wherein the fluorine-containing auxiliary agent is fluorine-containing siloxane coupling agent, the main solvent is methylcyclohexane, cyclohexane or normal hexane, and the auxiliary solvent is one or a mixture of two of trimethylketol and hydroxypropyl acrylate.
2. The composition for protecting a liquid crystal circuit according to claim 1, wherein: the liquid crystal circuit protection composition further comprises not more than 0.5 part by weight of a blue dye.
3. The method for producing a composition for liquid crystal circuit protection according to claim 1 or 2, characterized by comprising the steps of:
s1: drying the hydrogenated styrene-butadiene block copolymer at 65-75 ℃ for more than 4 hours;
s2: adding the hydrogenated styrene-butadiene block copolymer treated in step S1 to the mixed solvent of the auxiliary solvent and the main solvent with stirring;
s3: adding other raw materials into the mixture prepared in the step S2, and stirring the mixture uniformly;
s4: filtering insoluble substances, defoaming, and packaging.
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Citations (5)

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Publication number Priority date Publication date Assignee Title
CN102757709A (en) * 2011-04-26 2012-10-31 奇美实业股份有限公司 Moisture-proof insulating paint and application thereof
CN103571125A (en) * 2012-07-31 2014-02-12 中国石油化工股份有限公司 Elastomer nylon coating material as well as preparation method thereof
CN104650687A (en) * 2013-11-21 2015-05-27 奇美实业股份有限公司 Moisture-proof Insulating Paint And Application Thereof
CN105980505A (en) * 2014-01-22 2016-09-28 株式会社钟化 Polyolefin resin composition for hot melt adhesive, hot melt adhesive film, and laminate
CN106318101A (en) * 2015-06-30 2017-01-11 奇美实业股份有限公司 moisture-proof insulating paint and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102757709A (en) * 2011-04-26 2012-10-31 奇美实业股份有限公司 Moisture-proof insulating paint and application thereof
CN103571125A (en) * 2012-07-31 2014-02-12 中国石油化工股份有限公司 Elastomer nylon coating material as well as preparation method thereof
CN104650687A (en) * 2013-11-21 2015-05-27 奇美实业股份有限公司 Moisture-proof Insulating Paint And Application Thereof
CN105980505A (en) * 2014-01-22 2016-09-28 株式会社钟化 Polyolefin resin composition for hot melt adhesive, hot melt adhesive film, and laminate
CN106318101A (en) * 2015-06-30 2017-01-11 奇美实业股份有限公司 moisture-proof insulating paint and application thereof

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