CN111826120B - Preparation method of high-temperature-resistant strippable alcohol-type silica gel - Google Patents
Preparation method of high-temperature-resistant strippable alcohol-type silica gel Download PDFInfo
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- CN111826120B CN111826120B CN202010792173.7A CN202010792173A CN111826120B CN 111826120 B CN111826120 B CN 111826120B CN 202010792173 A CN202010792173 A CN 202010792173A CN 111826120 B CN111826120 B CN 111826120B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a preparation method of high-temperature-resistant strippable alcohol-type silica gel, which comprises the following steps: uniformly mixing a plurality of alpha, omega-hydroxyl terminated 107 silicon resins with different viscosities by a double-planet dispersing machine; adding methyl MQ resin powder, heating and stirring at high speed for melting; reducing the stirring speed, adding alumina, cerium oxide and superfine silicon dioxide, heating and keeping the vacuum degree to be less than-0.09 MPa for dehydration, and cooling to room temperature; adding ethyl orthosilicate and an organic tin catalyst, controlling the stirring speed, keeping the vacuum degree to be less than-0.09 MPa, dispersing the primary vulcanized base rubber in a double-planet dispersing machine, and continuously stirring to completely remove bubbles in the rubber liquid; adding an alkyl silane coupling agent as an adhesion reducing unit, and dispersing at high speed in a double-planet dispersing machine. The shielding adhesive suitable for the electrophoresis processing of the metal frame of the mobile phone is obtained, and has the characteristic of long-time high-temperature resistance and stripping.
Description
Technical Field
The invention belongs to the technical field of mobile phone metal frame electrophoresis processing shielding glue, and particularly relates to a preparation method of high-temperature-resistant peelable alcohol-type silica gel.
Background
The silicon rubber has the prominent performances of temperature resistance, weather resistance, electric insulation, low surface tension, low surface energy and the like. Can be used as a protective film of the material. The silicon rubber can be divided into room temperature vulcanization, high temperature vulcanization and low temperature vulcanization according to the vulcanization mode. The room temperature vulcanized silicone rubber can be deacidified, deoximated, dealcoholized, deaminated, deamidated, deacylamide, ketonized and other varieties. The room temperature vulcanized silicone rubber of deacidified type, deaminated type and ketoxime type has limited application due to the odor and the defect of corrosion to metals. The dealcoholized room temperature vulcanized silicone rubber releases low molecular alcohol during crosslinking, is tasteless, non-corrosive, good in caking property and high in surface drying speed, and has wider application prospect.
The metal frame of the mobile phone comprises stainless steel and aluminum alloy. In order to meet the requirements of appearance and performance, the shell needs to be treated by anode oxidation, micro-arc oxidation, electrophoresis and the like. The parts needing to be exposed can be protected by adopting a masking adhesive tape and a masking adhesive. The masking tape is commonly used, and is economical and practical for large-area masking, but the masking of a tiny part affects the efficiency and the economic cost.
In addition, electrophoresis has the advantages of high coating efficiency, small coating loss, uniform coating thickness, strong adhesion, good coating quality and the like, but requires higher curing temperature and longer curing time. The masking adhesive applied to the field of electrophoresis processing or the similar field needs to meet the requirement of long-time high-temperature resistance and stripping. At present, most of the existing shielding adhesives do not meet the requirement of long-time temperature resistance and stripping.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is to provide a method for preparing a high temperature resistant peelable alcohol-type silica gel, which can be baked at high temperature for more than 30 minutes and still has good peelability.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of high-temperature-resistant peelable alcohol-type silica gel is characterized by comprising the following steps:
s10: uniformly mixing alpha, w hydroxyl-terminated 107 silicon resin with the viscosity of 100000, 5000 and 1000 by using a double-planet dispersing machine to obtain a mixture;
s20: adding methyl MQ resin powder into the mixture, heating to 150 ℃, and melting by high-speed stirring to obtain a melt;
s30: reducing the stirring speed, adding alumina, cerium oxide and superfine silicon dioxide into the melt, heating to 150 ℃, keeping the vacuum degree less than-0.09 MPa, dehydrating for 1-2 hours, and cooling to room temperature to obtain base rubber;
s40: adding ethyl orthosilicate and an organic tin catalyst into the base adhesive, controlling the stirring speed, keeping the vacuum degree to be less than-0.09 MPa, dispersing in a double-planet dispersing machine for 20-40 minutes, and primarily vulcanizing the base adhesive to obtain an adhesive solution;
s50: and adding an alkyl silane coupling agent serving as an adhesion reducing unit into the glue solution, and dispersing for 20-40 minutes at a high speed in a double-planet dispersing machine.
S60: and (6) discharging the glue.
Preferably, in S40, after obtaining the glue solution, stirring is continued for 40-80 minutes to completely remove air bubbles in the glue solution.
Preferably, the proportion of the 100000 viscosity, 5000 viscosity and 1000 viscosity alpha, w hydroxyl-terminated 107 silicone resin, alumina and cerium oxide is 10:20:40:140: 2.8.
Preferably, in S10, the revolution frequency of stirring is 20-30HZ, and the dispersion frequency is 20-30 HZ.
Preferably, in S20, the revolution frequency of stirring is 30-40HZ, and the dispersion frequency is 30-40 HZ.
Preferably, in S30, the revolution frequency of stirring is 20-30HZ, and the dispersion frequency is 20-30 HZ.
Preferably, in S40, the revolution frequency of stirring is 20-30HZ, and the dispersion frequency is 20-30 HZ.
Preferably, in S50, the revolution frequency of stirring is 30-40HZ, and the dispersion frequency is 30-40 HZ.
Preferably, in S50, the alkylsilane coupling agent includes one or a combination of three of hexadecyltrimethoxysilane, dodecyltrimethoxysilane and octadecyltrimethoxysilane.
Preferably, the organic tin catalyst comprises one or a combination of three of stannous octoate, dibutyltin dilaurate and dibutyltin diacetate.
Compared with the prior art, the invention has the beneficial effects that:
the adhesive film is favorable for stripping after long-time high-temperature baking, after the adhesive is solidified, the adhesive film has better stripping performance after being subjected to heat aging in an oven at 180 ℃, 200 ℃, 220 ℃ and 230 ℃ for 30min, and the adhesive film has no fracture condition in the stripping process. The prior art is difficult to implement at 180 ℃, and less ready-made products are available above 200 ℃. The high temperature resistance of the silica gel can well solve the defects in the aspect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a process flow diagram of a method for preparing a high temperature resistant peelable alcohol-type silica gel of the present invention.
The implementation, functional features and advantages of the present invention will be further described with reference to the accompanying drawings.
Detailed Description
The present invention is further illustrated by the following specific examples, but it should be noted that the specific material ratios, process conditions, results, etc. described in the examples of the present invention are only for illustrating the present invention and are not to be construed as limiting the scope of the present invention, and all equivalent changes and modifications according to the spirit of the present invention should be covered by the scope of the present invention.
Example (b):
the preparation method of the high-temperature-resistant strippable alcohol-type silica gel comprises the following steps:
referring to fig. 1, 10g of α, w hydroxyl-terminated 107 silicone resin with 100000 viscosity, 20g of α, w hydroxyl-terminated 107 silicone resin with 5000 viscosity, and 40g of α, w hydroxyl-terminated 107 silicone resin with 1000 viscosity were mixed by a double planetary disperser, the revolution frequency of stirring was 20HZ, the dispersion frequency was 20HZ, and the mixture was obtained by stirring for 10 min;
adding 20g of methyl MQ resin powder into the mixture, heating to 150 ℃, stirring at a high speed for melting, wherein the revolution frequency of stirring is 35HZ, and the dispersion frequency is 35HZ, so as to obtain a melt;
reducing the stirring speed, wherein the revolution frequency of stirring is 20HZ, the dispersion frequency is 20HZ, adding 140g of alumina, 2.8g of cerium oxide and 3g of superfine silicon dioxide into the melt, heating to 150 ℃, keeping the vacuum degree to be less than-0.09 MPa, dehydrating for 2 hours, and cooling to room temperature to obtain base rubber;
adding 3g of ethyl orthosilicate and 0.2g of dibutyltin dilaurate into the base adhesive, controlling the stirring speed, controlling the revolution frequency of stirring to be 20HZ, the dispersion frequency to be 20HZ, keeping the vacuum degree to be less than-0.09 MPa, dispersing for 30 minutes in a double-planet dispersing machine, preliminarily vulcanizing the base adhesive to obtain an adhesive solution, and continuing stirring for 30 minutes after the adhesive solution is obtained so as to completely remove bubbles in the adhesive solution;
adding 10g of hexadecyl trimethoxy silane as an adhesion reducing unit into the glue solution, and dispersing for 30 minutes at a high speed in a double-planet dispersing machine, wherein the revolution frequency of stirring is 35HZ, and the dispersion frequency is 35 HZ; finally obtaining the high-temperature resistant strippable alcohol-type silica gel.
Comparative example:
| silane coupling agent | Room temperature releasability | High temperature strippability |
| Tetraethoxysilane | Can be peeled off | Non-strippable |
| Dodecyl trimethoxy silane | Can be peeled off | Can be peeled off |
| Hexadecyl trimethoxy silane | Can be peeled off | Can be peeled off |
| Gamma-aminopropyltriethoxysilane | Non-strippable | Non-strippable |
| 3- (2, 3-glycidoxy) propyltrimethoxysilane | Non-strippable | Non-strippable |
| Gamma-methacryloxypropyltrimethoxysilane | Non-strippable | Non-strippable |
| N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane | Non-strippable | Non-strippable |
| Vinyl trimethoxy silane | Non-strippable | Non-strippable |
| Bis- [3- (triethoxysilicon) -propyl]-amines | Non-strippable | Non-strippable |
| 3-phenylaminopropyl trimethoxy silane | Non-strippable | Non-strippable |
| N-N-butyl-3-aminopropyltrimethoxysilane | Non-strippable | Non-strippable |
As can be seen from the above examples and comparative examples, when the silane coupling agent is dodecyltrimethoxysilane or hexadecyltrimethoxysilane, the colloid is peelable at both room temperature and high temperature. The silane coupling agent is ortho-silicic acidWith ethyl ester, the gel was peelable at room temperature, but not at high temperatures. The silane coupling agent has the general formula Y-R-Si (OR)3The OR hydrolyzes to form hydroxyl groups that react with the hydroxyl groups on the substrate, and the Y reacts with the colloid. When Y contains functional groups such as benzene ring, alkenyl, amino, hydroxyl, epoxy and the like, the colloid can not be stripped.
Comparing the results of different compounding ratios of alpha and w hydroxyl-terminated 107 silicon resins with different viscosities:
| ratio of | Tensile strength | Elongation at break | Viscosity mPa.s |
| 100000:5000:1000=1:2:4 | 1.5MPa | 400% | 10000 |
| 100000:5000:1000=2:1:2 | 2.0MPa | 500% | 100000 |
| 100000:1000=1:2 | 1.0MPa | 200% | 30000 |
| 5000:1000=1:1 | 1.0MPa | 100% | 10000 |
From the relationship between the compounding ratio of the alpha and w hydroxyl-terminated 107 silicon resins with different viscosities and the tensile strength, the elongation at break and the viscosities, it can be seen that when the two resins are compounded, the tensile strength and the elongation at break are too low. When three resins are used for compounding, the tensile strength and the elongation at break are increased, and the moderate viscosity can be ensured. The high viscosity of the colloid causes construction inconvenience, the amount of the used colloid is increased, and the construction cost is increased. And the viscosity is too thin, so that the strength of the glue is not enough.
Comparison of the results for different ratios of alumina and hydroxyl-terminated 107 silicone:
| ratio of | Tensile strength | Elongation at break | Viscosity mPa.s |
| Alumina: resin =0:1 | 0.5MPa | 50% | 3000 |
| Alumina: resin =1:1 | 1.0MPa | 100% | 5000 |
| Alumina: resin =2:1 | 1.5MPa | 400% | 10000 |
| Alumina: resin =4:1 | 2.0MPa | 200% | 200000 |
From the relationship between the ratio of alumina to hydroxyl-terminated 107 silicone resin and the tensile strength, elongation at break and viscosity, it is clear that an increase in the proportion of alumina added is beneficial to an increase in the tensile strength of the colloid. However, too much alumina will result in too fast a viscosity increase and a decrease in elongation at break. Too high viscosity can lead to the construction inconvenience, and the volume of using glue increases, increases construction cost.
Comparison of the results for different ratios of cerium oxide and hydroxyl-terminated 107 silicone:
| ratio of | Temperature resistant | Tensile strength | Elongation at break |
| Cerium oxide: resin =0:1 | 230 | 1.5MPa | 400% |
| Cerium oxide: resin =0.02:1 | 230 | 1.5MPa | 400% |
| Cerium oxide: resin =0.04:1 | 260 | 1.5MPa | 400% |
| Cerium oxide: resin =0.06:1 | 250 | 1.5MPa | 200% |
| Cerium oxide: resin =0.1:1 | 250 | 1.0 MPa | 50% |
As can be seen from the relationship between the ratio of cerium oxide to hydroxyl-terminated 107 silicone resin and the tensile strength, elongation at break and viscosity, cerium oxide is beneficial to improving the temperature resistance of the glue, but excessive cerium oxide can cause the glue to be fluffy and loose, and the strength of the glue body can be sharply reduced. Although the temperature resistance of the glue is good, the strength of the glue body is damaged, and the glue is not beneficial to stripping.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A preparation method of high-temperature-resistant peelable alcohol-type silica gel is characterized by comprising the following steps:
s10: uniformly mixing alpha, omega-hydroxyl terminated 107 silicon resin with 100000, 5000 and 1000 viscosities by a double-planet dispersing machine to obtain a mixture;
s20: adding methyl MQ resin powder into the mixture, heating to 150 ℃, and melting by high-speed stirring to obtain a melt;
s30: reducing the stirring speed, adding alumina, cerium oxide and superfine silicon dioxide into the melt, heating to 150 ℃, keeping the vacuum degree less than-0.09 MPa, dehydrating for 1-2 hours, and cooling to room temperature to obtain base rubber;
s40: adding ethyl orthosilicate and an organic tin catalyst into the base adhesive, controlling the stirring speed, keeping the vacuum degree to be less than-0.09 MPa, dispersing in a double-planet dispersing machine for 20-40 minutes, and primarily vulcanizing the base adhesive to obtain an adhesive solution;
s50: adding an alkyl silane coupling agent serving as an adhesion reducing unit into the glue solution, and dispersing for 20-40 minutes at a high speed in a double-planet dispersing machine; the alkyl silane coupling agent comprises one or the combination of three of hexadecyl trimethoxy silane, dodecyl trimethoxy silane and octadecyl trimethoxy silane;
s60: and (6) discharging the glue.
2. The method of preparing a high temperature-resistant peelable alcohol-type silica gel according to claim 1, further comprising: and in the S40, after the colloid is obtained, stirring is continued for 40-80 minutes to completely remove air bubbles in the colloid.
3. The method for preparing the high temperature resistant peelable alcohol type silica gel according to claim 1, wherein the mass ratio of the alpha, omega-hydroxyl terminated 107 silicone resin with 100000 viscosity, 5000 viscosity and 1000 viscosity, the alumina and the cerium oxide is 10:20:40:140: 2.8.
4. The method of claim 1, wherein the revolution frequency of stirring in S10 is 20 to 30Hz, and the dispersion frequency is 20 to 30 Hz.
5. The method of claim 1, wherein the revolution frequency of stirring in S20 is 30 to 40Hz, and the dispersion frequency is 30 to 40 Hz.
6. The method of claim 1, wherein the revolution frequency of stirring in S30 is 20 to 30Hz, and the dispersion frequency is 20 to 30 Hz.
7. The method of claim 1, wherein the revolution frequency of stirring in S40 is 20 to 30Hz, and the dispersion frequency is 20 to 30 Hz.
8. The method of claim 1, wherein the revolution frequency of stirring in S50 is 30 to 40Hz, and the dispersion frequency is 30 to 40 Hz.
9. The method of claim 1, wherein the organotin catalyst comprises one or a combination of stannous octoate, dibutyltin dilaurate and dibutyltin diacetate.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101724269A (en) * | 2008-10-22 | 2010-06-09 | 广东恒大新材料科技有限公司 | Easy-stripping type room temperature vulcanizing silicone rubber and preparation method thereof |
| CN102876249A (en) * | 2012-08-31 | 2013-01-16 | 江苏创基新材料有限公司 | Preparation method of peelable type organosilicon pressure-sensitive adhesive |
| CN106833502A (en) * | 2016-12-29 | 2017-06-13 | 深圳市安品有机硅材料有限公司 | Peelable organic pressure-sensitive gel, pressure sensitive adhesive product and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI250190B (en) * | 2001-10-03 | 2006-03-01 | Dow Corning Toray Silicone | Adhesive sheet of cross-linked silicone, method of manufacturing thereof, and device |
| JP4623410B2 (en) * | 2003-06-13 | 2011-02-02 | 東レ・ダウコーニング株式会社 | Silicone pressure sensitive adhesive and adhesive tape |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101724269A (en) * | 2008-10-22 | 2010-06-09 | 广东恒大新材料科技有限公司 | Easy-stripping type room temperature vulcanizing silicone rubber and preparation method thereof |
| CN102876249A (en) * | 2012-08-31 | 2013-01-16 | 江苏创基新材料有限公司 | Preparation method of peelable type organosilicon pressure-sensitive adhesive |
| CN106833502A (en) * | 2016-12-29 | 2017-06-13 | 深圳市安品有机硅材料有限公司 | Peelable organic pressure-sensitive gel, pressure sensitive adhesive product and preparation method thereof |
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