CN117887112A - Preparation method of low-outgassing low-volatility silica gel - Google Patents
Preparation method of low-outgassing low-volatility silica gel Download PDFInfo
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- CN117887112A CN117887112A CN202311866878.9A CN202311866878A CN117887112A CN 117887112 A CN117887112 A CN 117887112A CN 202311866878 A CN202311866878 A CN 202311866878A CN 117887112 A CN117887112 A CN 117887112A
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- silica gel
- volatility
- outgassing
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- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 76
- 239000000741 silica gel Substances 0.000 title claims abstract description 76
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000010943 off-gassing Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 25
- -1 methyl vinyl siloxane Chemical class 0.000 claims abstract description 20
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 10
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 238000004898 kneading Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 15
- 229920006267 polyester film Polymers 0.000 claims description 15
- 239000000839 emulsion Substances 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 238000003490 calendering Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000004595 color masterbatch Substances 0.000 claims description 5
- 229910021485 fumed silica Inorganic materials 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 239000007789 gas Substances 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000004132 cross linking Methods 0.000 abstract description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 description 7
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
In the preparation process of the low-outgassing low-volatility silica gel, methyl vinyl siloxane and hydroxyl silicone oil are used for enabling a silica gel molecular chain to carry out a crosslinking reaction, a certain amount of the banburying low-outgassing low-volatility silica gel and a silica gel vulcanizing agent are mixed in an open mill, friction and adhesion between materials and the surface of a roller are achieved, and the volatilization of original material gases of the silica gel is reduced. The method can treat siloxane, moisture and gas in the raw material cleanly, so that the low-volatility bubble-free low-moisture silica gel material is prepared; the low outgassing and low volatility silica gel has greatly improved mechanical properties, no viscosity, no breakage and no dissolution in organic solvents. The preparation method of the low-outgassing low-volatility silica gel has scientific and reasonable process design, simple and easy operation and is suitable for popularization and use.
Description
Technical Field
The invention relates to the technical field of silica gel preparation, in particular to a preparation method of low-outgassing and low-volatility silica gel.
Background
The silica gel has excellent heat resistance, cold resistance, dielectric property, ozone resistance, atmospheric aging resistance and other performances, has outstanding temperature resistance and wide range, and can be used for a long time at-60 ℃ to +250 ℃. It has excellent physiological inertia, no toxicity, no smell, no corrosion, anticoagulation, good compatibility with organism and can withstand harsh disinfection conditions.
The low-volatility silica gel is mainly used for bonding and sealing air conditioners and lamps, such as bonding and sealing products of LED energy-saving lamps, automobile LED daytime running lamps and the like, bonding and sealing of precise instruments and meters, bonding and sealing of medical appliances, protective reinforcement and sealing protection of important parts on high-end electronic appliances, bonding and sealing of structures of various glass, aluminum materials, stone materials and metal structural engineering, and bonding or sealing in other industries.
Disclosure of Invention
In order to solve the technical problems, the preparation method of the low-outgassing low-volatility silica gel provided by the invention is characterized by comprising the following steps: the preparation method comprises the following steps of taking the following components in parts by weight, namely, firstly, uniformly mixing 60-70 parts of methyl vinyl siloxane, 1-3 parts of cross-linking agent and 0.05-1.5 parts of hydroxyl silicone oil to obtain emulsion;
b. Then, mixing 25-35 parts of fumed silica and the emulsion uniformly;
c. Mixing, putting into a kneader for mixing, putting into the kneader for mixing, heating the kneader to 100 ℃, kneading at a mixing speed of 1500 rpm, and performing heat treatment for 240 minutes; then heating to 160 ℃, kneading and mixing at 500 rpm, vacuumizing for 240 minutes in the kneading and mixing process, turning off a kneading and mixing machine, vacuumizing for 120 minutes at rest, keeping the vacuum degree at not lower than-0.07 MP in the rest process, and placing silica gel for more than 48 hours under normal pressure to enable the silica gel to be crosslinked and formed completely;
d. adding 0.5-1.5 parts of platinum catalyst and 2-3 parts of silica gel color masterbatch into a kneading mixer, and uniformly mixing on an opener;
e. Selecting a polyester film, and calendaring the low outgassing low volatility silica gel prepared in the step d on the polyester film to form a silica gel compound;
f. The silica gel compound is subjected to high-temperature baking treatment, a calender for high-temperature baking is provided with nine baking ovens, the temperature of each baking oven is set to be 55 ℃ in the first section, 65 ℃ in the second section, 75 ℃ in the third section, 85 ℃ in the fourth section, 95 ℃ in the fifth section, 105 ℃ in the sixth section, 125 ℃ in the seventh section, 135 ℃ in the eighth section, 155 ℃ in the ninth section, and the baking time of each baking oven is 2-5 minutes;
g. removing the polyester film to obtain the low outgassing and low volatility silica gel;
h. And finally, covering, cutting, packaging and warehousing by using a die cutting machine to finish the preparation of the low-outgassing low-volatility silica gel.
Preferably, the methyl vinyl siloxane in the step a is 65 parts.
Preferably, the crosslinking agent in the step a is 2 parts.
Preferably, the hydroxyl silicone oil in the step a is 1 part.
Preferably, in the step f, each section of oven drying time is 3 minutes.
In the preparation process of the low-outgassing low-volatility silica gel, methyl vinyl siloxane and hydroxyl silicone oil are used for enabling a silica gel molecular chain to carry out a crosslinking reaction, a certain amount of the banburying low-outgassing low-volatility silica gel and a silica gel vulcanizing agent are mixed in an open mill, friction and adhesion between materials and the surface of a roller are achieved, and the volatilization of original material gases of the silica gel is reduced. The method can treat siloxane, moisture and gas in the raw material cleanly, so that the low-volatility bubble-free low-moisture silica gel material is prepared; the low outgassing and low volatility silica gel has greatly improved mechanical properties, no viscosity, no breakage and no dissolution in organic solvents. The preparation method of the low-outgassing low-volatility silica gel has scientific and reasonable process design, simple and easy operation and is suitable for popularization and use.
Detailed Description
Example 1: a preparation method of low-outgassing low-volatility silica gel comprises the following steps: the components are taken as the weight portions,
A. Firstly, 60 parts of methyl vinyl siloxane, 1 part of cross-linking agent and 0.05 part of hydroxyl silicone oil are uniformly mixed to obtain emulsion;
b. then, mixing 25 parts of fumed silica and the emulsion uniformly;
c. Mixing, putting into a kneader for mixing, putting into the kneader for mixing, heating the kneader to 100 ℃, kneading at a mixing speed of 1500 rpm, and performing heat treatment for 240 minutes; then heating to 160 ℃, kneading and mixing at 500 rpm, vacuumizing for 240 minutes in the kneading and mixing process, turning off a kneading and mixing machine, vacuumizing for 120 minutes at rest, keeping the vacuum degree at not lower than-0.07 MP in the rest process, and standing for 50 hours under normal pressure to ensure that the silica gel is completely crosslinked and formed;
d. Adding 0.5 part of platinum catalyst and 2 parts of silica gel color master batch into a kneading mixer, and uniformly mixing on a developing machine;
e. Selecting a polyester film, and calendaring the low outgassing low volatility silica gel prepared in the step d on the polyester film to form a silica gel compound;
f. The silica gel compound is subjected to high-temperature baking treatment, a calender for high-temperature baking is provided with nine baking ovens, the temperature of each baking oven is set to be 55 ℃ in the first section, 65 ℃ in the second section, 75 ℃ in the third section, 85 ℃ in the fourth section, 95 ℃ in the fifth section, 105 ℃ in the sixth section, 125 ℃ in the seventh section, 135 ℃ in the eighth section, 155 ℃ in the ninth section, and the baking time of each baking oven is set to be 2 minutes;
g. removing the polyester film to obtain the low outgassing and low volatility silica gel;
h. And finally, covering, cutting, packaging and warehousing by using a die cutting machine to finish the preparation of the low-outgassing low-volatility silica gel.
Example 2: a preparation method of low-outgassing low-volatility silica gel is characterized by comprising the following steps: the components are taken as the weight portions,
A. firstly, uniformly mixing 65 parts of methyl vinyl siloxane, 2 parts of cross-linking agent and 1 part of hydroxyl silicone oil to obtain emulsion;
b. then, mixing 30 parts of fumed silica and the emulsion uniformly;
c. Mixing, putting into a kneader for mixing, putting into the kneader for mixing, heating the kneader to 100 ℃, kneading at a mixing speed of 1500 rpm, and performing heat treatment for 240 minutes; then heating to 160 ℃, kneading and mixing at 500 rpm, vacuumizing for 240 minutes in the kneading and mixing process, turning off a kneading and mixing machine, vacuumizing for 120 minutes at rest, keeping the vacuum degree at not lower than-0.07 MP in the rest process, and standing for 50 hours under normal pressure to ensure that the silica gel is completely crosslinked and formed;
d. adding 1 part of platinum catalyst and 2.5 parts of silica gel color masterbatch into a kneading mixer, and uniformly mixing on a developing machine;
e. Selecting a polyester film, and calendaring the low outgassing low volatility silica gel prepared in the step d on the polyester film to form a silica gel compound;
f. The silica gel compound is subjected to high-temperature baking treatment, a calender for high-temperature baking is provided with nine baking ovens, the temperature of each baking oven is set to be 55 ℃ in the first section, 65 ℃ in the second section, 75 ℃ in the third section, 85 ℃ in the fourth section, 95 ℃ in the fifth section, 105 ℃ in the sixth section, 125 ℃ in the seventh section, 135 ℃ in the eighth section, 155 ℃ in the ninth section, and the baking time of each baking oven is set to be 3 minutes;
g. removing the polyester film to obtain the low outgassing and low volatility silica gel;
h. And finally, covering, cutting, packaging and warehousing by using a die cutting machine to finish the preparation of the low-outgassing low-volatility silica gel.
Example 3: a preparation method of low-outgassing low-volatility silica gel is characterized by comprising the following steps: the components are taken as the weight portions,
A. Firstly, uniformly mixing 70 parts of methyl vinyl siloxane, 3 parts of cross-linking agent and 1.5 parts of hydroxyl silicone oil to obtain emulsion;
b. Then, uniformly mixing 35 parts of fumed silica and the emulsion;
c. Mixing, putting into a kneader for mixing, putting into the kneader for mixing, heating the kneader to 100 ℃, kneading at a mixing speed of 1500 rpm, and performing heat treatment for 240 minutes; then heating to 160 ℃, kneading and mixing at 500 rpm, vacuumizing for 240 minutes in the kneading and mixing process, turning off a kneading and mixing machine, vacuumizing for 120 minutes at rest, keeping the vacuum degree at not lower than-0.07 MP in the rest process, and standing for 50 hours under normal pressure to ensure that the silica gel is completely crosslinked and formed;
d. adding 1.5 parts of platinum catalyst and 3 parts of silica gel color master batch into a kneading mixer, and uniformly mixing on a developing machine;
e. Selecting a polyester film, and calendaring the low outgassing low volatility silica gel prepared in the step d on the polyester film to form a silica gel compound;
f. The silica gel compound is subjected to high-temperature baking treatment, a calender for high-temperature baking is provided with nine baking ovens, the temperature of each baking oven is set to be 55 ℃ in the first section, 65 ℃ in the second section, 75 ℃ in the third section, 85 ℃ in the fourth section, 95 ℃ in the fifth section, 105 ℃ in the sixth section, 125 ℃ in the seventh section, 135 ℃ in the eighth section, 155 ℃ in the ninth section, and the baking time of each baking oven is set to be 5 minutes;
g. removing the polyester film to obtain the low outgassing and low volatility silica gel;
h. And finally, covering, cutting, packaging and warehousing by using a die cutting machine to finish the preparation of the low-outgassing low-volatility silica gel.
In the preparation process of the low-outgassing low-volatility silica gel, methyl vinyl siloxane and hydroxyl silicone oil are used for enabling a silica gel molecular chain to carry out a crosslinking reaction, a certain amount of the banburying low-outgassing low-volatility silica gel and a silica gel vulcanizing agent are mixed in an open mill, friction and adhesion between materials and the surface of a roller are achieved, and the volatilization of original material gases of the silica gel is reduced. The method can treat siloxane, moisture and gas in the raw material cleanly, so that the low-volatility bubble-free low-moisture silica gel material is prepared; the low outgassing and low volatility silica gel has greatly improved mechanical properties, no viscosity, no breakage and no dissolution in organic solvents. The preparation method of the low-outgassing low-volatility silica gel has scientific and reasonable process design, simple and easy operation and is suitable for popularization and use.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts are included in the scope of the present invention.
Claims (5)
1. A preparation method of low-outgassing low-volatility silica gel is characterized by comprising the following steps: the components are taken as the weight portions,
A. Firstly, 60-70 parts of methyl vinyl siloxane, 1-3 parts of cross-linking agent and 0.05-1.5 parts of hydroxyl silicone oil are uniformly mixed to obtain emulsion;
b. Then, mixing 25-35 parts of fumed silica and the emulsion uniformly;
c. Mixing, putting into a kneader for mixing, putting into the kneader for mixing, heating the kneader to 100 ℃, kneading at a mixing speed of 1500 rpm, and performing heat treatment for 240 minutes; then heating to 160 ℃, kneading and mixing at 500 rpm, vacuumizing for 240 minutes in the kneading and mixing process, turning off a kneading and mixing machine, vacuumizing for 120 minutes at rest, keeping the vacuum degree at not lower than-0.07 MP in the rest process, and placing silica gel for more than 48 hours under normal pressure to enable the silica gel to be crosslinked and formed completely;
d. adding 0.5-1.5 parts of platinum catalyst and 2-3 parts of silica gel color masterbatch into a kneading mixer, and uniformly mixing on an opener;
e. Selecting a polyester film, and calendaring the low outgassing low volatility silica gel prepared in the step d on the polyester film to form a silica gel compound;
f. The silica gel compound is subjected to high-temperature baking treatment, a calender for high-temperature baking is provided with nine baking ovens, the temperature of each baking oven is set to be 55 ℃ in the first section, 65 ℃ in the second section, 75 ℃ in the third section, 85 ℃ in the fourth section, 95 ℃ in the fifth section, 105 ℃ in the sixth section, 125 ℃ in the seventh section, 135 ℃ in the eighth section, 155 ℃ in the ninth section, and the baking time of each baking oven is 2-5 minutes;
g. removing the polyester film to obtain the low outgassing and low volatility silica gel;
h. And finally, covering, cutting, packaging and warehousing by using a die cutting machine to finish the preparation of the low-outgassing low-volatility silica gel.
2. The method for preparing the low outgassing and low volatility silica gel as claimed in claim 1, wherein the method comprises the steps of: the methyl vinyl siloxane in the step a is 65 parts.
3. The method for preparing the low outgassing and low volatility silica gel as claimed in claim 1, wherein the method comprises the steps of: the cross-linking agent in the step a is 2 parts.
4. The method for preparing the low outgassing and low volatility silica gel as claimed in claim 1, wherein the method comprises the steps of: the hydroxyl silicone oil in the step a is 1 part.
5. The method for preparing the low outgassing and low volatility silica gel as claimed in claim 1, wherein the method comprises the steps of: and f, drying time of each section of oven in the step is 3 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311866878.9A CN117887112A (en) | 2023-12-31 | 2023-12-31 | Preparation method of low-outgassing low-volatility silica gel |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311866878.9A CN117887112A (en) | 2023-12-31 | 2023-12-31 | Preparation method of low-outgassing low-volatility silica gel |
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| Publication Number | Publication Date |
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| CN117887112A true CN117887112A (en) | 2024-04-16 |
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| CN202311866878.9A Pending CN117887112A (en) | 2023-12-31 | 2023-12-31 | Preparation method of low-outgassing low-volatility silica gel |
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| CN (1) | CN117887112A (en) |
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- 2023-12-31 CN CN202311866878.9A patent/CN117887112A/en active Pending
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