CN102585745A - Frame sealing adhesive, and preparation method and application thereof - Google Patents

Frame sealing adhesive, and preparation method and application thereof Download PDF

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Publication number
CN102585745A
CN102585745A CN2012100397055A CN201210039705A CN102585745A CN 102585745 A CN102585745 A CN 102585745A CN 2012100397055 A CN2012100397055 A CN 2012100397055A CN 201210039705 A CN201210039705 A CN 201210039705A CN 102585745 A CN102585745 A CN 102585745A
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frame glue
envelope frame
epoxy resin
silane
powder
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冯卫文
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MIANYANG EXAX ELECTRONIC MATERIALS CO Ltd
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MIANYANG EXAX ELECTRONIC MATERIALS CO Ltd
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Abstract

The invention discloses a frame sealing adhesive and a preparation method and application thereof. The frame sealing adhesive comprises the following component: epoxy resin, a curing agent, a rubber powder, an organic filler, a thixotropic agent, a silane coupling agent and a solvent. The frame sealing adhesive has excellent storage performance and an adhesive applying manner suitable for screen printing and is used for sealing a side frame of a TN (twisted nematic) (STN-super twisted nematic) liquid crystal box; in addition, the solidified frame sealing adhesive has the advantages of low hydroscopic property, long-lasting and excellent sealing performance, excellent heat resistance and electric insulation performance, no pollution to liquid crystal, high rigidity, high toughness and high size stability, and important application value.

Description

Envelope frame glue and preparation method thereof and application
Technical field
The present invention relates to a kind of envelope frame glue and preparation method thereof and application.
Background technology
The present invention relates to a kind of envelope frame sealing material that is used for liquid crystal cell.Liquid crystal cell is one of critical material in the liquid crystal display manufacturing processed with envelope frame glue.In the liquid crystal cell manufacturing processed, common technology is, through the screen printing mode applying glue in liquid crystal cell with sheet glass on, carry out 80 ℃/30 minutes predrying desolventizing, hot repressing glass is not higher than curing in 150 ℃/1 hour.The cured article of this sealer, low water absorbable, persistent excellent sealing performance, excellent thermotolerance and electrical insulation capability do not pollute liquid crystal property, high rigidity, H.T. and dimensional stability.It seals to liquid crystal display device, guarantees the normal use of this device under usual conditions, requires this product (1) to have superior being bonded and sealed property; (2) high-low temperature resistant changes performance; (3) electrical insulation capability and do not pollute the performance of liquid crystal; (4) to be fit to the glue-applying technique that the extensive technology of making of liquid crystal display promptly is fit to silk screen printing simultaneously; (5) make things convenient for storge quality as what commodity had.Related prods in the market mainly is the tackiness agent of epoxy group(ing) thermofixation single-component, although still there are some significant disadvantages in commercialization; Can not satisfy 5 above-mentioned Practical Performances fully; The product that for example uses at present, there is certain shortcoming adhesiveproperties aspect at low temperatures, aspect storage; To under lower temperature, deposit, bring very big trouble for the storage and the transportation of product.
Summary of the invention
The purpose of this invention is to provide a kind of envelope frame glue and preparation method thereof and application.
Envelope frame glue provided by the invention comprises epoxy resin, solidifying agent, rubber powder, mineral filler, thixotropic agent, silane coupling agent and solvent.
Said envelope frame glue also can only be made up of said components.Wherein, the hydrolyzable chloride content of said epoxy resin is less than 600 * 10 -6Mg/kg, the selective hydrolysis cl content is less than 300 * 10 -6Mg/kg; The resin hydrolyzing cl content is greater than 600 * 10 -6Mg/kg can cause the pollution of liquid crystal cell frame sealing material to liquid crystal.The hydrolysis chlorine dose can be measured with reference to ASTM D1726-2003.This epoxy resin also can like washing-SX, hyperfiltration process and distillation process for purification, be made with extra care or purifying, to reach above-mentioned requirement through known minimizing hydrolysis chlorine method.
The functionality of said epoxy resin is 2-4.
Said epoxy resin specifically can be selected from least a in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, novolac epoxy, cycloaliphatic epoxy resin, glycidyl amine epoxy resin, difunctionality phenols diglycidyl ether epoxy resin and the difunctionality alcohols diglycidylether resin;
Wherein, said bisphenol A type epoxy resin is that the dihydroxyphenyl propane glycidyl ether can be selected from least a among commercial goods NPEL-128E, NPEL-134 (Nanya of South Asia, Taiwan resin company), CYD128, the CYD134 (the good marble of Yueyang Ba Ling ltd); Said bisphenol f type epoxy resin is that the Bisphenol F glycidyl ether can be selected from least a among commercial goods Epalloy 8220 (U.S. Emerald company) and the NPEF-170 (Nanya of South Asia, Taiwan resin company); Bisphenol-s epoxy resin is that the bisphenol S glycidyl ether can be selected from commercial goods 185S (Jiangsu Aolunda Science and Technology Industry Co.,Ltd); Novolac epoxy is that novolac glycidyl ethers can be selected from least a among commercial goods CYDBN-240, the CYDPN-048 (the good marble of Yueyang Ba Ling ltd); Cycloaliphatic epoxy resin is that alicyclic ring divalent alcohol glycidyl ether can be selected from AL-3040 (the wide Hue chemicals in Yantai ltd); Glycidyl amine epoxy resin can be selected from least a among commercial goods AG-80, AFG-90 (Shanghai resin institute), YH-434 and the 434L (Japanese Dongdu changes into); Difunctionality phenols diglycidyl ether epoxy resin can be selected from commercial goods 694 (the huge rainbow Fine Chemical Works of Yueyang cloud small stream); Difunctionality alcohols diglycidylether resin can be selected from least a among commercial goods 622,669 (Mount Huang new far away chemical company), ED-503, the ED-523T (Nanya of South Asia, Taiwan resin company);
Said solidifying agent is two hydrazides class solidifying agent; Can not dissociate and separate out the pollution liquid crystal, at least a in preferred O-phthalic acid dihydrazide, isophthalic dihydrazide, terephthaldehyde's acid dihydrazide, succinic acid hydrazide ii, adipic dihydrazide, Regulox, adipic dihydrazide, sebacic dihydrazide and the 3-nitro Phthalocyclohydrazide; The median size of said solidifying agent is not more than 3 microns, and the largest particle particle diameter is less than 5 microns;
Said rubber powder is full vulcanized rubber powder, at least a in preferred full sulfuration styrene-butadiene rubber(SBR) powder, carboxylic styrene-butadiene rubber powder, acrylic elastomer powder, paracril powder, carboxyl acrylonitrile-butadiene rubber powder end and the silicone rubber powder; The particle diameter of said rubber powder is 50nm~200nm, preferred 50-150nm;
Said mineral filler be selected from silicon-dioxide, silit, silicon nitride, lime carbonate, magnesiumcarbonate, permanent white, calcium sulfate, aluminum oxide, Natural manganese dioxide, white lake, Marinco H, Calucium Silicate powder, pure aluminium silicate, talcum powder, lithium aluminosilicate, at least a, at least a in preferred silicon-dioxide, aluminum oxide, silicon nitride and the talcum powder; The median size of said mineral filler is the 0.2-3 micron, and the largest particle particle diameter is less than 5 μ m; Preferred median size is 1 μ m, largest particle particle diameter less than the consolidation abrasive silica of 5 μ m or median size is 1 μ m, the largest particle particle diameter precipitated silica less than 5 μ m.Above-mentioned mineral filler all can be bought from open commercial sources and obtain.
Said thixotropic agent is selected from least a in aerosil, THIXCIN, polyethylene wax, polyamide modified THIXCIN, the polyamide wax; As can be at least a in the aerosil of Degussa A200 type or U.S. Cabot M-5 model; Various commercially available THIXCINs all are applicable to this method, like the commercial goods THIXCIN of the emerging combination worker in Tongliao City ltd; Polyethylene wax is specially OPE, and various commercial goods all are suitable for, like commercial goods Clariant polyethylene wax PE520 (Clariant chemical industry (China) ltd); Polyamide modified THIXCIN such as commercial goods France Cray Willie (CRAY VALLEY) MT, SF product, the U.S. special Xiang MT PLUS of Science and Technology Ltd., MT 6650, MT 6900-20X, MT 6900-30X, MT 6900-20H etc.; Polyamide wax such as commercial goods RC-620, RC-820 (Changxing consonance macromolecular material ltd) etc.; CRAY VALLEYsuper (French Cray Willie (CRAYVALLEY)) etc.
Said silane coupling agent is selected from 3-glycidoxy-propyl group-Trimethoxy silane, 3-glycidoxy-propyl group-methyl-dimethoxy silane, 3-glycidoxy-propyl group-methyl-dimethoxy silane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, N-phenyl-gamma-amino propyl group-Trimethoxy silane, N-(2-amino-ethyl) 3-aminopropyl-methyl-dimethoxy silane, N-(2-amino-ethyl) 3-aminopropyl-Trimethoxy silane, 3-aminopropyl-triethoxyl silane, 3-sulfydryl propyl group-Trimethoxy silane, vinyl-Trimethoxy silane, N-(at least a in 2-(vinyl benzyl is amino) ethyl 3-aminopropyl-Trimethoxy silane, 3-methacryloxy-propyl group-trimethoxy-silane, 3-chloropropyl-methyl-dimethoxy silane and the 3-chloropropyl-Trimethoxy silane; This silane coupling agent can obtain by open commercial sources is convenient, as can be available from the KH560 of NanJing Shuguang Chemical Group Co., Ltd. or the silane coupling agent of KH550 model.
Said solvent is selected from least a in glycol ether, diethylene glycol ether, propylene glycol and the dipropylene glycol.
Said epoxy resin accounts for 50~70% of said envelope frame glue total mass, is specially 50%, 70% or 68%, and said solidifying agent accounts for 5~10% of said envelope frame glue total mass; Be specially 8% or 10%, said rubber powder accounts for the 2-6% of said envelope frame glue total mass, is specially 6%; Said mineral filler accounts for 5~8% of said envelope frame glue total mass, is specially 7% or 8%, and said thixotropic agent accounts for 0.5~3.0% of said envelope frame glue total mass; Be specially 1% or 3%; Said silane coupling agent accounts for 0.5~3% of said envelope frame glue total mass, is specially 1% or 0.5%, and surplus is said solvent.
The method of the above-mentioned envelope frame of preparation provided by the invention glue comprises the steps: aforementioned each component mixing is obtained said envelope frame glue.
This mixing step specifically can be: utilize planetary whipping device tentatively to mix earlier, utilize three roller ground and mixed and kneadings again, and then utilize that planetary whipping device stirs, froth breaking and filtration.
Application and this envelope frame glue the application in silk screen printing of the envelope frame glue for preparing according to the method described above in the preparation sealing material also belongs to protection scope of the present invention.Wherein, said sealing material is preferably the sealing material of TN liquid crystal cell or stn liquid crystal box.Said silk screen printing step comprises: aforementioned envelope frame glue provided by the invention is carried out applying glue, predrying and curing.Wherein, said applying glue step is a routine operation; In the said predrying step, temperature is 80 ℃, and the time is 30 minutes; In the said curing schedule, temperature is 120-150 ℃, and preferred 120-130 ℃, the time is 60 minutes.
Envelope frame glue provided by the invention is one of critical material of a kind of TN/STN of being used for liquid crystal display manufacturing processed.This envelope frame glue has good memory property, is fit to the applying glue mode of silk screen printing, and its cured article has low water absorbable; Lasting excellent sealing ability, excellent thermotolerance and electrical insulation capability do not pollute liquid crystal property; High rigidity, H.T. and dimensional stability have important use and are worth.
Embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration, but the present invention is not limited to following examples.Said method is ordinary method if no special instructions.Said raw material all can get from open commercial sources if no special instructions.
Embodiment 1
Utilize planetary whipping device with following each component: bisphenol A type epoxy resin NPEL-134 is (available from South Asia epoxy resin (Kunshan) ltd, hydrolyzable chloride content less than 300 * 10 -6Mg/kg) 68 weight parts; Solidifying agent adipic dihydrazide (available from Wuxi City Liang Xi Fine Chemical Co., Ltd) 8 weight parts (utilize the ultra-fine smooth grinding device processes of micronizer mill; Handle back median size 3 μ m; 5 microns of maximum particle diameters), (particle diameter is 50~200nm to ultra-fine fully vulcanized powder rubber with the VP501 carboxy nitrile rubber; Available from the Beijing Chemical Research Institute) 5 weight parts, filler-silicon dioxide CL-2008-III are (available from the prosperous vast and boundless sodium rice in Hebei Materials Co., Ltd; Median size is that 1 μ m, largest particle particle diameter are less than 5 μ m) after 7 weight parts, thixotropic agent aerosil Degussa A200 model 1 weight part, silane coupling agent KH560 (available from NanJing Shuguang Chemical Group Co., Ltd.) 1 weight part and solvent ethylene glycol butyl ether 10 weight parts tentatively mix earlier; With three roller ground and mixed and kneadings, again in planetary whipping device stir, froth breaking and filtration, obtain envelope frame glue provided by the invention.
This embodiment prepares that the largest particle diameter has good memory property less than 5 microns in the gained envelope frame glue, is fit to the applying glue mode of silk screen printing; Be used for the frame sealing of TN (STN) liquid crystal cell after curable (keeping 30 minutes predrying backs that desolventize to accomplish curing after 60 minutes) in 120 ℃ of maintenances in 80 ℃; Cured article has low water absorbable, lasting excellent sealing ability, excellent thermotolerance and electrical insulation capability; Do not pollute liquid crystal property, high rigidity, H.T. and dimensional stability.
Embodiment 2
According to embodiment 1 identical method, only solidifying agent is replaced with m-phthalic acid two hydrazides (available from the happy strange chemical industry in Jinan ltd), obtain sealing frame glue.
This embodiment prepares in the gained envelope frame glue largest particle diameter less than 5 microns; Has good memory property; The applying glue mode of suitable silk screen printing is used for the frame sealing of TN (STN) liquid crystal cell after curable (keeping 30 minutes predrying backs that desolventize to accomplish curing after 60 minutes in 130 ℃ of maintenances in 80 ℃).
Embodiment 3
According to embodiment 1 identical method, only rubber powder is replaced with VP301 acrylic elastomer (particle diameter is 50~200nm, the Beijing Chemical Research Institute), obtain sealing frame glue.
This embodiment prepares in the gained envelope frame glue largest particle diameter less than 5 microns; Has good memory property; The applying glue mode of suitable silk screen printing is used for the frame sealing of TN (STN) liquid crystal cell after curable (keeping 30 minutes predrying backs that desolventize to accomplish curing after 60 minutes in 120 ℃ of maintenances in 80 ℃).
Embodiment 4
Utilize planetary whipping device with following each component: bisphenol A type epoxy resin NPEL-128 is (available from South Asia epoxy resin (Kunshan) ltd, hydrolyzable chloride content less than 300 * 10 -6Mg/kg) 70 weight parts; Solidifying agent isophthalic dihydrazide (available from Wuxi City Liang Xi Fine Chemical Co., Ltd) 10 weight parts (utilize the ultra-fine smooth grinding device processes of micronizer mill; Handle back median size 2 μ m; 5 microns of maximum particle diameters), (particle diameter is 50~200nm to ultra-fine fully vulcanized powder rubber with the VP501 carboxy nitrile rubber; Available from the Beijing Chemical Research Institute) 5 weight parts, filler spherical silicon dioxide are (available from Suzhou Nano Dispersions Co., Ltd.; Median size is that 1 μ m, largest particle particle diameter are less than 5 μ m) after 8 weight parts, thixotropic agent aerosil Degussa R202 model 1 weight part, coupling agent KH560 (available from NanJing Shuguang Chemical Group Co., Ltd.) 1 weight part and solvent ethylene glycol butyl ether 5 weight parts tentatively mix earlier; With three roller ground and mixed and kneadings, again in planetary whipping device stir, froth breaking and filtration, obtain envelope frame glue provided by the invention.
This embodiment prepares in the gained envelope frame glue largest particle diameter less than 5 microns; Has good memory property; The applying glue mode of suitable silk screen printing is used for the frame sealing of TN (STN) liquid crystal cell after curable (keeping 30 minutes predrying backs that desolventize to accomplish curing after 60 minutes in 120 ℃ of maintenances in 80 ℃).
Embodiment 5
Utilize planetary whipping device with following each component: bisphenol A type epoxy resin NPEL-114 is (available from South Asia epoxy resin (Kunshan) ltd, hydrolyzable chloride content less than 300 * 10 -6Mg/kg) 50 weight parts; Solidifying agent isophthalic dihydrazide (available from the happy strange chemical industry in Jinan ltd) 8 weight parts (utilize the ultra-fine smooth grinding device processes of micronizer mill; Handle back median size 2 μ m; 5 microns of maximum particle diameters), (particle diameter is 50~200nm to ultra-fine fully vulcanized powder rubber with the VP501 carboxy nitrile rubber; Available from the Beijing Chemical Research Institute) 6 weight parts, filler spherical silicon dioxide are (available from Suzhou Nano Dispersions Co., Ltd.; Median size is that 1 μ m, largest particle particle diameter are less than 5 μ m) after 8 weight parts, thixotropic agent tentatively mix earlier with U.S. Cabot M-5 aerosil 1 weight part, coupling agent KH550 (available from NanJing Shuguang Chemical Group Co., Ltd.) 1 weight part and solvent ethylene glycol butyl ether 26 weight parts; With three roller ground and mixed and kneadings, again in planetary whipping device stir, froth breaking and filtration, obtain envelope frame glue provided by the invention.
This embodiment prepares in the gained envelope frame glue largest particle diameter less than 5 microns; Has good memory property; The applying glue mode of suitable silk screen printing is used for the frame sealing of TN (STN) liquid crystal cell after curable (keeping 30 minutes predrying backs that desolventize to accomplish curing after 60 minutes in 130 ℃ of maintenances in 80 ℃).
Embodiment 6
Utilize planetary whipping device with following each component: bisphenol A type epoxy resin E39D is (available from the good marble of Yueyang Ba Ling ltd, hydrolyzable chloride content less than 300 * 10 -6Mg/kg) 65 weight parts; Solidifying agent isophthalic dihydrazide (available from the happy strange chemical industry in Jinan ltd) 9 weight parts (utilize the ultra-fine smooth grinding device processes of micronizer mill; Handle back median size 2 μ m; 5 microns of maximum particle diameters), (particle diameter is 50~200nm to ultra-fine fully vulcanized powder rubber with the VP301 carboxy nitrile rubber; Available from the Beijing Chemical Research Institute) 6 weight parts, filler spherical silicon dioxide are (available from Suzhou Nano Dispersions Co., Ltd.; Median size is that 1 μ m, largest particle particle diameter are less than 5 μ m) after 8 weight parts, thixotropic agent aerosil (available from U.S.'s Cabot, model is M-5) 3 weight parts, coupling agent KH550 (available from NanJing Shuguang Chemical Group Co., Ltd.) 0.5 weight part and solvent ethylene glycol butyl ether 14.5 weight parts tentatively mix earlier, with three roller ground and mixed and kneadings; Again in planetary whipping device stir, froth breaking and filtration, obtain envelope frame glue provided by the invention.
This embodiment prepares in the gained envelope frame glue largest particle diameter less than 5 microns; Has good memory property; The applying glue mode of suitable silk screen printing is used for the frame sealing of TN (STN) liquid crystal cell after curable (keeping 30 minutes predrying backs that desolventize to accomplish curing after 60 minutes in 130 ℃ of maintenances in 80 ℃).
According to following method the correlated performance of embodiment 1~6 preparation gained envelope frame glue and commercially available prod is estimated.
The evaluation method of the suitability of silk screen printing applying glue mode is following:
The envelope frame glue of embodiment or comparative example is transferred to 25 ℃ of following storages 2 hours of room temperature from storage condition; Utilize the viscosity of rotary viscosity design determining in the time of 25 ℃; The suitability of this silk screen printing applying glue mode is characterized by the viscosity velocity of variation that it left standstill under 25 ℃ 12 hours: velocity of variation was less than 10% o'clock, and the suitability of its silk screen printing applying glue mode is " excellent "; Velocity of variation 10.1~50% o'clock, the suitability of its silk screen printing applying glue mode is " generally "; Velocity of variation surpasses at 50% o'clock, and the suitability of its silk screen printing applying glue mode is " bad ".
Envelope frame glue is following to the contamination evaluation method of liquid crystal:
Envelope frame glue with embodiment or comparative example is coated on the slick stripping film (like polytetrafluoroethylene film) with 100~150 micron thickness, and handles 30 minutes down with except that desolvating at 80 ℃, subsequently it is further obtained cured film in 90 minutes 150 ℃ of following thermofixations.Take by weighing 0.5 the gram cured film and place it in the sealed glass container, also add therein in addition 5 the gram liquid crystal material SLC-6614B (available from Shijiazhuang Chengzhi Yonghua Display Materials Co., Ltd.).Under the nitrogen atmosphere protection, heated 1 hour down with this container sealing and at 100 ℃.Material in the container is taken a sample to liquid crystal through the syringe sucking-off, and in used syringe, place undersized ceramic filter made device.Adopt the resistivity of resistivity measurement instrumentation amount liquid crystal, and shown with respect to velocity of variation through the above-mentioned only resistivity value (being initial liquid crystal resistivity) that test obtains to liquid crystal.Based on the resistivity skill of initial liquid crystal, velocity of variation promptly is evaluated as " nothing " less than 50 times; Based on the resistivity skill of initial liquid crystal, velocity of variation promptly is evaluated as " nothing " less than 50 times; Based on the resistivity skill of initial liquid crystal, velocity of variation is 50~200 times, promptly is evaluated as " generally "; Based on the resistivity skill of initial liquid crystal, velocity of variation promptly is evaluated as " greatly " greater than 200 times.
The evaluation method of envelope frame glue sealing property is following:
With the envelope frame glue of embodiment or comparative example, make liquid crystal cell according to deciding glue-applying technique and curing process, place and amplify under 50 times the reading lens and detect by an unaided eye to measure because the potted line turbulent that the generation sealing leak occurs exists and relatively poor point.If the potted line turbulent not occurring exists and relatively poor point, i.e. sealing property " excellent "; Otherwise be " bad ".
Envelope frame glue is following to the adhesiveproperties evaluation method of liquid crystal cell sheet glass:
The experiment that destroys liquid crystal cell through the design chock is to weigh the adhesiveproperties of envelope frame glue to vial.With the envelope frame glue of each embodiment or comparative example, make liquid crystal cell according to deciding glue-applying technique and curing process.The set ambient temperature for a wedge into the liquid crystal cell Xie, to destroy experiments, and based on its failure state to measure its adhesive properties.If substrate destroys, i.e. adhesiveproperties " excellent "; Part is observed the cohesive failure of envelope frame glue, i.e. adhesiveproperties " generally "; Observed the interface stripping damage, i.e. adhesiveproperties " relatively poor ".
The gained result is shown in table 1 and table 2.
Table 1, embodiment prepare the performance tabulation of gained envelope frame glue and commercially available prod
Table 2, embodiment prepare the performance tabulation of gained envelope frame glue and commercially available prod
Figure BDA0000137137680000072
Figure BDA0000137137680000081
Wherein, the adhesiveproperties of alloy aluminum is measured and is got according to the method for GB/T 7124-2008; Viscosity variation between the shelf lives is got by rotary viscosity design determining.
Can know by table 1 and table 2, the embodiment of the invention 1~6 products obtained therefrom, in the suitability of silk screen printing applying glue mode, sealing property, electrical insulation capability with to aspect the pollutant performance of liquid crystal, with comparative example (actual commercial goods of using) quite; Being fit to the TN/STN liquid crystal cell fully is to make to use.Can find out from table 1 that simultaneously embodiments of the invention 1~6 have greater advantage than comparative example aspect adhesiveproperties, the advantage of adhesiveproperties is more obvious especially at low temperatures.Aspect storge quality, the embodiment of the invention 1~6 products obtained therefrom can have 6 months shelf lives under 23 ℃ of environment of normal temperature, compares with comparative example (requiring storage under-20~-10 ℃ of environment), has the accessibility of storage, transportation.Aspect curing process, to compare with comparative example, embodiments of the invention 1~6 products obtained therefrom is in identical set time, and solidification value lower (at 120~130 ℃) has reduced the solidified condition, reaches the purpose that reduces production energy consumption.

Claims (10)

1. an envelope frame glue comprises epoxy resin, solidifying agent, rubber powder, mineral filler, thixotropic agent, silane coupling agent and solvent.
2. envelope frame glue according to claim 1 is characterized in that: said envelope frame glue is by said epoxy resin, solidifying agent, rubber powder, mineral filler, thixotropic agent, silane coupling agent and solvent composition.
3. envelope frame glue according to claim 1, it is characterized in that: the hydrolyzable chloride content of said epoxy resin is less than 600 * 10 -6Mg/kg, the selective hydrolysis cl content is less than 300 * 10 -6Mg/kg, the functionality of said epoxy resin is 2-4; Said epoxy resin specifically is selected from least a in bisphenol A type epoxy resin, bisphenol f type epoxy resin, bisphenol-s epoxy resin, novolac epoxy, cycloaliphatic epoxy resin, glycidyl amine epoxy resin, difunctionality phenols diglycidyl ether epoxy resin and the difunctionality alcohols diglycidylether resin;
Said solidifying agent is two hydrazides class solidifying agent, at least a in preferred O-phthalic acid dihydrazide, isophthalic dihydrazide, terephthaldehyde's acid dihydrazide, succinic acid hydrazide ii, adipic dihydrazide, Regulox, adipic dihydrazide, sebacic dihydrazide and the 3-nitro Phthalocyclohydrazide; The median size of said solidifying agent is not more than 3 microns, and the largest particle particle diameter is less than 5 microns;
Said rubber powder is full vulcanized rubber powder, at least a in preferred full sulfuration styrene-butadiene rubber(SBR) powder, carboxylic styrene-butadiene rubber powder, acrylic elastomer powder, paracril powder, carboxyl acrylonitrile-butadiene rubber powder end and the silicone rubber powder; The particle diameter of said rubber powder is 50nm~200nm, preferred 50-150nm;
Said mineral filler be selected from silicon-dioxide, silit, silicon nitride, lime carbonate, magnesiumcarbonate, permanent white, calcium sulfate, aluminum oxide, Natural manganese dioxide, white lake, Marinco H, Calucium Silicate powder, pure aluminium silicate, talcum powder, lithium aluminosilicate, at least a, at least a in preferred silicon-dioxide, aluminum oxide, silicon nitride and the talcum powder; The median size of said mineral filler is the 0.2-3 micron, and the largest particle particle diameter is less than 5 μ m;
Said thixotropic agent is selected from least a in aerosil, THIXCIN, polyethylene wax, polyamide modified THIXCIN and the polyamide wax;
Said silane coupling agent is selected from 3-glycidoxy-propyl group-Trimethoxy silane, 3-glycidoxy-propyl group-methyl-dimethoxy silane, 3-glycidoxy-propyl group-methyl-dimethoxy silane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, N-phenyl-gamma-amino propyl group-Trimethoxy silane, N-(2-amino-ethyl) 3-aminopropyl-methyl-dimethoxy silane, N-(2-amino-ethyl) 3-aminopropyl-Trimethoxy silane, 3-aminopropyl-triethoxyl silane, 3-sulfydryl propyl group-Trimethoxy silane, vinyl-Trimethoxy silane, N-(at least a in 2-(vinyl benzyl is amino) ethyl 3-aminopropyl-Trimethoxy silane, 3-methacryloxy-propyl group-trimethoxy-silane, 3-chloropropyl-methyl-dimethoxy silane and the 3-chloropropyl-Trimethoxy silane;
Said solvent is selected from least a in butyl glycol ether, diethylene glycol ether, propylene glycol and the dipropylene glycol.
4. according to the arbitrary described envelope frame glue of claim 1-3; It is characterized in that: said epoxy resin accounts for 50~70% of said envelope frame glue total mass; Said solidifying agent accounts for 5~10% of said envelope frame glue total mass; Said rubber powder accounts for 2~6% of said envelope frame glue total mass, and said mineral filler accounts for 5~8% of said envelope frame glue total mass, and said thixotropic agent accounts for 0.5~3.0% of said envelope frame glue total mass; Said silane coupling agent accounts for 0.5~3% of said envelope frame glue total mass, and surplus is said solvent.
5. a method for preparing the arbitrary said envelope frame glue of claim 1-4 comprises the steps: each the component mixing with the arbitrary said envelope frame glue of claim 1-4, obtains said envelope frame glue.
6. the application of the arbitrary said envelope frame glue of claim 1-4 in the preparation sealing material.
7. application according to claim 6 is characterized in that: said sealing material is the sealing material of TN liquid crystal cell or stn liquid crystal box.
8. the application of the arbitrary said envelope frame glue of claim 1-4 in silk screen printing.
9. application according to claim 8 is characterized in that: said silk screen printing step comprises: the arbitrary said envelope frame glue of claim 1-4 is carried out applying glue, predrying and curing.
10. application according to claim 9 is characterized in that: in the said predrying step, temperature is 80 ℃, and the time is 30 minutes; In the said curing schedule, temperature is 120~150 ℃, and preferred 120-130 ℃, the time is 60 minutes.
CN2012100397055A 2012-02-21 2012-02-21 Frame sealing adhesive, and preparation method and application thereof Pending CN102585745A (en)

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CN102888199A (en) * 2012-09-17 2013-01-23 北京京东方光电科技有限公司 Frame sealing glue and preparation method and application thereof
CN102925066A (en) * 2012-11-14 2013-02-13 杭州师范大学 Epoxy resin adhesive film and preparation method thereof
CN102925092A (en) * 2012-11-14 2013-02-13 杭州师范大学 Epoxy resin nano composite adhesive film and preparation method thereof
CN103173175A (en) * 2013-03-23 2013-06-26 广东新展化工新材料有限公司 Organic silicone modified epoxy resin sealant and preparation method thereof
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CN107573885A (en) * 2017-10-17 2018-01-12 王天石 One kind building special seal gum and preparation method thereof
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1346375A (en) * 1999-12-14 2002-04-24 三井化学株式会社 Sealing agent for liquid-crystal display, cell, composition for sealing agent for liquid-crystal display cell, and liquid-crystal display element
CN101608105A (en) * 2008-06-17 2009-12-23 上海得荣电子材料有限公司 Adhesive for packaging smart card module
WO2011043119A1 (en) * 2009-10-07 2011-04-14 ソニーケミカル&インフォメーションデバイス株式会社 Thermosetting adhesive composition, thermosetting adhesive sheet, method for producing same, and reinforced flexible printed wiring board

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1346375A (en) * 1999-12-14 2002-04-24 三井化学株式会社 Sealing agent for liquid-crystal display, cell, composition for sealing agent for liquid-crystal display cell, and liquid-crystal display element
CN101608105A (en) * 2008-06-17 2009-12-23 上海得荣电子材料有限公司 Adhesive for packaging smart card module
WO2011043119A1 (en) * 2009-10-07 2011-04-14 ソニーケミカル&インフォメーションデバイス株式会社 Thermosetting adhesive composition, thermosetting adhesive sheet, method for producing same, and reinforced flexible printed wiring board

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《热固性树脂》 19971115 钱祖荣 "降低双酚A型环氧树脂可水解氯含量方法的探讨" "2可水解氯对环氧树脂性能的影响"部分 1-10 , 第4期 *
钱祖荣: ""降低双酚A型环氧树脂可水解氯含量方法的探讨"", 《热固性树脂》, no. 4, 15 November 1997 (1997-11-15), pages 2 *

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Application publication date: 20120718