CN103396758A - Anti-static dealcoholization-type silicone sealant and preparation method thereof - Google Patents
Anti-static dealcoholization-type silicone sealant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an anti-static dealcoholization-type silicone sealant and a preparation method thereof. The preparation method is characterized in that 30-55 parts of alpha, omega-dyhydroxyl dimethyl silicone polymer, 40-60 parts of calcium carbonate and 1-10 parts of methyl dimethyl silicone polymer are added to a kneading machine, are blended and dehydrated for 2 to 3 hours at 100-120 DEG C in a vacuum of 0.08 to 0.09MPa so as to obtain a base stock; 100 parts of base stock, 0.24-6 parts of ionic-type anti-static liquid with concentration of 15-25wt%f, 2-5 parts of crosslinking agent, 3-7 parts of catalyst and 0.1-4 parts of coupling agent are added to a planetary mixer and are dispersed for 35 to 45 minutes in a vacuum, thus the anti-static dealcoholization-type silicone sealant is obtained. After being cured, the anti-static dealcoholization-type silicone sealant is anti-static and insulated, has good dielectric property, is used in the field of adhesives of laboratory floors with high anti-static requirements, door and window sealants and combination bonding of anti-static operation console devices as well as electronic sealant industries with high dielectric constant requirements and avoids the dust pollution caused by static electricity.
Description
Technical field
The present invention relates to a kind of anti-electrostatic dealcoholizing-type silicone sealant and preparation method thereof, belong to the manufacturing field of functional high molecule material.
Background technology
Along with development and the growth in the living standard of high-grade, precision and advanced science and technology, silicone sealant, as a kind of bonding and sealing material commonly used, is had higher requirement to its static electricity resistance in many workplaces.Prepare the anti-electrostatic silicone sealant, addible antistatic agent has two classes, and a class adopts conduction powder or polyethers filler to make antistatic agent, but too much filler is not good to material mechanical performance and anti-static electrification net effect.Another kind of is the ionic antistatic agent, and it is a kind of tensio-active agent with amphipathic structure, can be adsorbed on phase interface, reduces phase and phase interfacial surface tension and resistivity of material; Perhaps permeating at material surface, its molecule water-wet side forms thin water layer and anti-electrostatic on top layer.A series of Ionic conductivity static inhibitor have been announced in Chinese patent CN101338075A, be used for silicone rubber mold-making material, obtained the add-on type anti-electrostatic silicon rubber of high volume specific resistance, high-antistatic effect, in Chinese patent CN101421104A, this type of antistatic agent is used for organosilicon ionic coat film afterwards, be used for preventing that the static of electronic installation from polluting and the product defects problem of generation, above product is add-on type silica gel, moulded product, but in quick bonding field there are no technical literature and amateur bibliographical information.
Summary of the invention:
The objective of the invention is provides a kind of anti-electrostatic dealcoholizing-type silicone sealant and preparation method thereof for the deficiencies in the prior art, be characterized in α, alpha, omega-dihydroxy polydimethyl siloxane, calcium carbonate, the at high temperature vacuum hydro-extraction of methyl polydimethylsiloxane, make base-material; , with base-material and linking agent, catalyzer, coupling agent and ionic anti-electrostatic liquid, add in planetary mixer after vacuum is disperseed and obtain dealcoholizing-type anti-electrostatic silicone sealant again.This silicone sealant is used for the bonding field of combination of floor, the demanding laboratory of anti-electrostatic, doors and windows sealing and anti-electrostatic operator's console device.
Purpose of the present invention realizes by following technical measures, and wherein said raw material umber except specified otherwise, is parts by weight.
The starting raw material of anti-electrostatic dealcoholizing-type silicone sealant is composed of the following components is:
Described α, the viscosity of alpha, omega-dihydroxy polydimethyl siloxane is 500～200000 mPas.
Described calcium carbonate is 0.1～10 μ m activated Calcium carbonate of processing through tensio-active agent.
The viscosity of described anti-electrostatic dealcoholizing-type silicone sealant methyl polydimethylsiloxane is the methyl polydimethylsiloxane of 50～500 mPas.
Described linking agent is methyltrimethoxy silane. Union carbide A-162. and vinyltrimethoxy silane. vinyltriethoxysilane. at least a in phenyltrimethoxysila,e and phenyl triethoxysilane.
Described titanate ester catalyzer is two (methyl aceto acetate base) inner complexs of diisopropoxy titanium or metatitanic acid binary alcohol esters beta-diketon inner complex.
Described coupling agent is γ-aminopropyl triethoxysilane. γ-aminopropyltrimethoxysilane. and γ-glycidyl ether oxygen propyl trimethoxy silicane. at least a in γ-(methacryloxypropyl) propyl trimethoxy silicane and N-(β-aminoethyl)-γ-aminopropyl triethoxysilane.
Described ionic antistatic agent is the trifluoromethanesulfonic acid lithium. any of two (trifluoromethane sulphonyl) imine lithiums or LiBF4.
The manufacture method of anti-electrostatic dealcoholizing-type silicone sealant comprises the following steps:
Step 1: be the α of 500～200000 mPas with viscosity, 30～55 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 40～60 parts of 0.1～10 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 1～10 part of the methyl polydimethylsiloxane of 50～500 mPas adds in kneader, in 100～120 ℃ of temperature, vacuum tightness 0.08～0.09MPa blend dehydration 2-3h, obtain base-material;
Step 2: with 15～25 portions of ionic antistatic agents, be dissolved in the Octyl adipate of 75-85 part, add in there-necked flask, under nitrogen protection, mix 10～20 min in temperature 70-80 ℃, at vacuum tightness 0.07～0.08MPa dehydration 1.5～2.5h, obtaining concentration is the ionic anti-electrostatic liquid of 15～25wt%, and sealing is preserved;
Step 3: with 100 parts of resulting base-materials of step 1,3～7 parts of 2～5 parts of 0.24～6 part of ionic anti-electrostatic liquid, linking agents, catalyzer, 0.1～4 part of the coupling agent with step 2 gained, add in planetary mixer, keep vacuum tightness 0.08～0.09MPa to stir 35～45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
Structural characterization and performance test:
, with the anti-electrostatic dealcoholizing-type silicone sealant that makes, according to GB/T 13477 tests, refer to touch surface drying time; According to GB/T 582-209 test mechanical property, according to GB/T 1693 and GB/T 1695 test dielectric properties and volume specific resistances, decline the phase according to SJ/T 10694-2006 testing high voltage electrostatic half-life and 1/10, this testing method is to be written into high static voltage at material surface, by detector detect its surface electrostatic press decline to half/1/10th o'clock time used.Test result is as shown in Table 1 below
The present invention has the following advantages:
1, add a small amount of ionic anti-electrostatic liquid, the anti-electrostatic silicone sealant high-voltage transformation period, by greater than 100s, drops in 1s, and anti-static effect is good;
2, with the increase of ionic anti-electrostatic liquid measure, anti-electrostatic silicone sealant volume specific resistance descends, if add 0.4 ‰ to, volume specific resistance is still 10
-13More than Ω m, kept the advantage that silicon rubber uses as insulating material;
3, add and do not add ionic anti-electrostatic liquid, little on the impact of silicone sealant dielectric loss.
Embodiment
Below by embodiment, the present invention is specifically described; be necessary to be pointed out that at this present embodiment only is used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1:
Step 1: be the α of 500 mPas with viscosity, 30 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 60 parts of the 0.1 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 10 parts of the methyl polydimethylsiloxanes of 50 mPas add in kneader, in 120 ℃ of temperature,, at vacuum tightness 0.09MPa blend dehydration 3h, obtain base-material;
Step 2: with 15 portions of antistatic agents, 85 parts of Octyl adipate solvents, add in there-necked flask, under nitrogen, is warming up to 70 ℃, mixes 10 min, and at the vacuum tightness 0.08 MPa 2h that dewaters, obtaining concentration is the ionic anti-electrostatic liquid of 15wt%, and sealing is preserved;
Step 3: 0.1 part of 3 parts of two (methyl aceto acetate base) inner complex of 100 parts of the resulting base-materials of step 1,0.24 part of the ionic anti-electrostatic liquid of step 2 gained, 1.5 parts of methyltrimethoxy silanes, 0.5 part of Union carbide A-162, diisopropoxy titanium, γ-aminopropyl triethoxysilane are added in planetary mixer, keep vacuum tightness 0.09MPa to stir 45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
Embodiment 2:
Step 1: be the α of 200000 mPas with viscosity, 55 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 40 parts of the 10 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 5 parts of the methyl polydimethylsiloxanes of 500 mPas add in kneader, in 100 ℃ of temperature,, at vacuum tightness 0.08MPa blend dehydration 2h, obtain base-material;
Step 2: with 25 portions of antistatic agents, 75 parts of Octyl adipate solvents, add in there-necked flask, under nitrogen, is warming up to 80 ℃, mixes 20 min, and at the vacuum tightness 0.09 MPa 3h that dewaters, obtaining concentration is the ionic anti-electrostatic liquid of 25wt%, and sealing is preserved;
Step 3: 1 part of 7 parts of two (methyl aceto acetate base) inner complex of 100 parts of the resulting base-materials of step 1,6 parts of the ionic anti-electrostatic liquid of step 2 gained, 4 parts of vinyltrimethoxy silanes, 1 part of vinyltriethoxysilane, diisopropoxy titanium, 3 parts of γ-aminopropyltrimethoxysilanes, γ-aminopropyl triethoxysilane are added in planetary mixer, keep vacuum tightness 0.09MPa to stir 45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
Embodiment 3:
Step 1: be the α of 10000 mPas with viscosity, 50 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 40 parts of the 0.4 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 10 parts of the methyl polydimethylsiloxanes of 200 mPas add in kneader, in 110 ℃ of temperature,, at vacuum tightness 0.085MPa blend dehydration 1.8h, obtain base-material;
Step 2: with 22 portions of antistatic agents, 78 parts of Octyl adipate solvents, add in there-necked flask, under nitrogen, is warming up to 80 ℃, mixes 20 min, and at the vacuum tightness 0.09 MPa 2.5h that dewaters, obtaining concentration is the ionic anti-electrostatic liquid of 22wt%, and sealing is preserved;
Step 3: 1 part of 3.5 parts of two (methyl aceto acetate base) inner complex of 100 parts of the resulting base-materials of step 1,1 part of the ionic anti-electrostatic liquid of step 2 gained, 2 parts of phenyltrimethoxysila,e, 3 parts of methyltrimethoxy silanes, diisopropoxy titanium, γ-aminopropyl triethoxysilane are added in planetary mixer with 1 part of γ-aminopropyltrimethoxysilane, keep vacuum tightness 0.09MPa to stir 45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
Embodiment 4
Step 1: be the α of 50000 mPas with viscosity, 45 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 54 parts of the 0.8 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 1 part of the methyl polydimethylsiloxane of 300 mPas adds in kneader, in 110 ℃ of temperature,, at vacuum tightness 0.085MPa blend dehydration 2.5h, obtain base-material;
Step 2: with 20 portions of antistatic agents, 80 parts of Octyl adipate solvents, add in there-necked flask, under nitrogen, is warming up to 80 ℃, mixes 20 min, and at the vacuum tightness 0.09 MPa 2h that dewaters, obtaining concentration is the ionic anti-electrostatic liquid of 20wt%, and sealing is preserved;
Step 3: with 100 parts of the resulting base-materials of step 1,2 parts of the ionic anti-electrostatic liquid of step 2 gained, 1 part of vinyltrimethoxy silane, 2.5 parts of phenyltrimethoxysila,e, 3 parts of metatitanic acid binary alcohol esters beta-diketon inner complexs, 1.5 parts of γ-aminopropyltrimethoxysilanes, 1 part of γ-aminopropyl triethoxysilane, add in planetary mixer, keep vacuum tightness 0.09MPa to stir 45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
Embodiment 5
Step 1: be the α of 80000 mPas with viscosity, 45 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 50 parts of the 5 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 5 parts of the methyl polydimethylsiloxanes of 400 mPas add in kneader, in 105 ℃ of temperature,, at vacuum tightness 0.085MPa blend dehydration 2.1h, obtain base-material;
Step 2: with 20 portions of antistatic agents, 80 parts of Octyl adipate solvents, add in there-necked flask, under nitrogen, is warming up to 80 ℃, mixes 20 min, and at the vacuum tightness 0.09 MPa 2.5h that dewaters, obtaining concentration is the ionic anti-electrostatic liquid of 20wt%, and sealing is preserved;
Step 3: 2 parts of 2 parts of 100 parts of the resulting base-materials of step 1,3.5 parts of the ionic anti-electrostatic liquid of step 2 gained, Union carbide A-162 and 2 parts of vinyltrimethoxy silanes, 3 parts of metatitanic acid binary alcohol esters beta-diketon inner complexs, γ-aminopropyl triethoxysilanes are added in planetary mixer with 0.5 part of γ-aminopropyltrimethoxysilane, keep vacuum tightness 0.09MPa to stir 45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
Application Example 1
Step 1: be the α of 60000 mPas with viscosity, 35 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 55 parts of the 10 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 10 parts of the methyl polydimethylsiloxanes of 200 mPas add in kneader, in 120 ℃ of temperature,, at vacuum tightness 0.09MPa blend dehydration 3h, obtain base-material;
Step 2: with 22 portions of antistatic agents, the blend of 78 parts of Octyl adipate solvents, add in there-necked flask, under nitrogen, is warming up to 70-80 ℃, mixes 15min, and at the vacuum tightness 0.09 MPa 2h that dewaters, obtaining concentration is the ionic anti-electrostatic liquid of 22wt%, and sealing is preserved;
Step 3: 1 part of 100 parts of the resulting base-material of step 1,0.5 part of the ionic anti-electrostatic liquid of step 2 gained, 3 parts of phenyltrimethoxysila,e, 2 parts of vinyltrimethoxy silanes, 3 parts of metatitanic acid binary alcohol esters beta-diketon inner complexs, γ-aminopropyl triethoxysilane is added in planetary mixer with 2.5 parts of γ-glycidyl ether oxygen propyl trimethoxy silicanes, keep vacuum tightness 0.09MPa to stir 45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
This dealcoholizing-type anti-electrostatic silicone sealant is used for the bonding of antifouling door and window, thixotropy is good, does not hang stream, and cementability is strong,, cruelly in the more place of dust, does not hang dirt in one month.
The performance test results of table 1 anti-electrostatic dealcoholizing-type silicone sealant
Claims (9)
1. an anti-electrostatic dealcoholizing-type silicone sealant, is characterized in that the starting raw material of this silicone sealant is composed of the following components, is by weight:
2. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, is characterized in that α, and the viscosity of alpha, omega-dihydroxy polydimethyl siloxane is 500～200000 mPas.
3. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, is characterized in that calcium carbonate is 0.1～10 μ m activated Calcium carbonate of processing through tensio-active agent.
4. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, the viscosity that it is characterized in that the methyl polydimethylsiloxane is the methyl polydimethylsiloxane of 50～500 mPas.
5. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, is characterized in that linking agent is methyltrimethoxy silane. Union carbide A-162. and vinyltrimethoxy silane. vinyltriethoxysilane. at least a in phenyltrimethoxysila,e and phenyl triethoxysilane.
6. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, is characterized in that the titanate ester catalyzer is two (methyl aceto acetate base) inner complexs of diisopropoxy titanium or metatitanic acid binary alcohol esters beta-diketon inner complex.
7. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, is characterized in that coupling agent is γ-aminopropyl triethoxysilane. γ-aminopropyltrimethoxysilane. and γ-glycidyl ether oxygen propyl trimethoxy silicane. at least a in γ-(methacryloxypropyl) propyl trimethoxy silicane and N-(β-aminoethyl)-γ-aminopropyl triethoxysilane.
8. anti-electrostatic dealcoholizing-type silicone sealant according to claim 1, is characterized in that the ionic antistatic agent is the trifluoromethanesulfonic acid lithium. any of two (trifluoromethane sulphonyl) imine lithiums or LiBF4.
9. the manufacture method of one of according to claim 1～9 described anti-electrostatic dealcoholizing-type silicone sealants is characterized in that the method comprises the following steps:
Step 1: be the α of 500～200000 mPas with viscosity, 30～55 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 40～60 parts of 0.1～10 μ m activated Calcium carbonates of processing through tensio-active agent, viscosity is that 1～10 part of the methyl polydimethylsiloxane of 50～500 mPas adds in kneader, in 100～120 ℃ of temperature,, at vacuum tightness 0.08～0.09MPa blend dehydration 2-3h, obtain base-material;
Step 2: with 15～25 portions of ionic antistatic agents, be dissolved in the Octyl adipate of 75-85 part, add in there-necked flask, under nitrogen protection, mix 10～20 min in temperature 70-80 ℃, at vacuum tightness 0.07～0.08MPa dehydration 1.5～2.5h, obtaining concentration is the ionic anti-electrostatic liquid of 15～25wt%, and sealing is preserved;
Step 3: 0.1～4 part of 3～7 parts of 2～5 parts of 0.24～6 part of ionic anti-electrostatic liquid, linking agents, catalyzer, the coupling agent of 100 parts of resulting base-materials of step 1 and step 2 gained is added in planetary mixer, keep vacuum tightness 0.08～0.09MPa to stir 35～45min, obtain dealcoholizing-type anti-electrostatic silicone sealant, by platen, the sealing mucilage binding is entered sealing in plastic rubber bottle and preserve.
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| CN104059597B (en) * | 2014-06-26 | 2015-12-09 | 河北硅谷化工有限公司 | The production method of step down side busbar sheath bonded adhesives |
| CN105754536A (en) * | 2016-03-10 | 2016-07-13 | 张家港锐码新材料有限公司 | Transparent antistatic pressure-sensitive adhesive |
| CN105925200A (en) * | 2016-05-06 | 2016-09-07 | 烟台图文马克化工科技有限公司 | Silicone sealant for automotive chassis |
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