CN113861697A - Liquid silica gel with excellent dispersibility and preparation method thereof - Google Patents
Liquid silica gel with excellent dispersibility and preparation method thereof Download PDFInfo
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- CN113861697A CN113861697A CN202111207095.0A CN202111207095A CN113861697A CN 113861697 A CN113861697 A CN 113861697A CN 202111207095 A CN202111207095 A CN 202111207095A CN 113861697 A CN113861697 A CN 113861697A
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- silicone oil
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 239000007788 liquid Substances 0.000 title claims abstract description 88
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 72
- 239000000741 silica gel Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 43
- 229920002545 silicone oil Polymers 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- XISWSMPYOFEMKE-AATRIKPKSA-N [(e)-pent-1-enyl] acetate Chemical compound CCC\C=C\OC(C)=O XISWSMPYOFEMKE-AATRIKPKSA-N 0.000 claims abstract description 16
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000003112 inhibitor Substances 0.000 claims abstract description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 10
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229920002379 silicone rubber Polymers 0.000 claims description 30
- 239000004944 Liquid Silicone Rubber Substances 0.000 claims description 20
- 239000002202 Polyethylene glycol Substances 0.000 claims description 19
- 229920001223 polyethylene glycol Polymers 0.000 claims description 19
- 239000004417 polycarbonate Substances 0.000 claims description 18
- 229920000515 polycarbonate Polymers 0.000 claims description 18
- 150000002009 diols Chemical class 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 239000011812 mixed powder Substances 0.000 claims description 10
- -1 diester diol Chemical class 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 4
- 238000003860 storage Methods 0.000 abstract description 9
- 230000002035 prolonged effect Effects 0.000 abstract description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 229940072049 amyl acetate Drugs 0.000 abstract description 2
- PGMYKACGEOXYJE-UHFFFAOYSA-N anhydrous amyl acetate Natural products CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 abstract description 2
- MNWFXJYAOYHMED-UHFFFAOYSA-M heptanoate Chemical compound CCCCCCC([O-])=O MNWFXJYAOYHMED-UHFFFAOYSA-M 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 19
- 229910021485 fumed silica Inorganic materials 0.000 description 16
- 239000000377 silicon dioxide Substances 0.000 description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 239000004945 silicone rubber Substances 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 8
- 230000002776 aggregation Effects 0.000 description 7
- 230000003014 reinforcing effect Effects 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/095—Oxygen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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Abstract
The application relates to the technical field of liquid silica gel, in particular to liquid silica gel with excellent dispersibility and a preparation method thereof. The liquid silica gel is prepared by mixing a mixture, and comprises the following raw materials in parts by weight: vinyl silicone oil, hydroxyl silicone oil, modified fumed silica, a silane treating agent, a catalyst, ceramic powder, amyl acetate, diethylene glycol dimethyl ether, polyacrylate, hydrogen-containing silicone oil and an inhibitor; the preparation method comprises the following steps: uniformly stirring vinyl silicone oil, hydroxyl silicone oil, pentenyl acetate and a catalyst, heating, vacuumizing, and dividing into a first base material and a second base material, adding modified fumed silica and ceramic powder into the first base material to obtain a component A, adding a component B of diethylene glycol dimethyl ether, hydrogen-containing silicone oil, acrylate and an inhibitor into the second base material, and mixing the component A and the component B. Through the synergistic effect of the reagents, the modified fumed silica can be uniformly dispersed in the liquid silica gel for a long time, and the storage time of the liquid silica gel is prolonged.
Description
Technical Field
The application relates to the technical field of liquid silica gel, in particular to liquid silica gel with excellent dispersibility and a preparation method thereof.
Background
Liquid silicone rubber, also known as two-component addition silicone rubber, has excellent transparency, tear strength, thermal stability, yellowing resistance, viscosity and fluidity, and is therefore used in various fields, such as infant products, medical products, electronic products (keys), and the like.
At present, the fumed silica is added into liquid silica gel to achieve a reinforcing effect, silicon hydroxyl (Si-OH) on the surface of fumed silica can form physical or chemical combination with silicone rubber macromolecules, a silicone rubber molecule adsorption layer is formed on the surface of the silica to form a three-dimensional network structure integrating silica particles and silicone rubber molecules, deformation of silicone rubber molecular chains is effectively limited, and the reinforcing effect is achieved. The smaller the particle size of the fumed silica, the larger the specific surface area, the larger the contact surface between the particles and the rubber material, the more the binding points, the better the reinforcing performance on the liquid silicone rubber, and the high tensile strength, tearing strength, wear resistance and hardness of the vulcanized rubber.
However, fumed silica itself is in the order of nanometers, has a small particle size, a large specific surface area, and a high free energy, and generally exists in an agglomerated state, and is easily agglomerated and hardly dispersed in silicone oil, so that fumed silica is hardly uniformly dispersed in a system, and the dispersion effect is poor, resulting in a reduction in the reinforcing effect, and thus the inventors considered that improvement is required.
Disclosure of Invention
In order to solve the problem that a reinforcing machine in the existing silicone rubber is not uniformly dispersed, the liquid silicone rubber with excellent dispersibility and the preparation method thereof are provided.
The liquid silica gel with excellent dispersibility and the preparation method thereof adopt the following technical scheme:
in a first aspect, the present application provides a liquid silica gel having excellent dispersibility, the liquid silica gel comprising a mixture of the following raw materials in parts by weight:
70-90 parts of vinyl silicone oil
20-30 parts of hydroxyl silicone oil
10-15 parts of modified fumed silica
5-10 parts of silane treating agent
0.006-0.06 part of catalyst
15-20 parts of ceramic powder
5-10 parts of pentenyl acetate
10-15 parts of diethylene glycol dimethyl ether
5-10 parts of polyacrylate
0.5-10 parts of hydrogen-containing silicone oil
0.002-0.04 parts of inhibitor.
By adopting the technical scheme, the liquid silica gel with excellent dispersibility is obtained; the ceramic powder, the pentenyl acetate and the modified fumed silica are uniformly mixed, so that agglomeration of the modified fumed silica can be reduced, the modified fumed silica can be uniformly dispersed in a system, the reinforcing effect of the modified fumed silica is improved, and the tensile strength, tear strength, hardness and light transmittance of the liquid silica are improved; under the combined action of the amyl acetate, the diethylene glycol dimethyl ether and the polyacrylate, the modified fumed silica has good compatibility in a liquid silica gel system, and can be uniformly dispersed in the liquid silica gel system for a long time, so that the storage time of the liquid silica gel is prolonged.
Preferably, the particle size of the ceramic powder is 10-15 nm.
By adopting the technical scheme, the particle size of the ceramic powder is smaller than that of the modified fumed silica, so that the ceramic powder and the modified fumed silica can be favorably attached to the surface of the modified fumed silica, and agglomeration among particles of the modified fumed silica is reduced, so that the particles can be uniformly dispersed in a liquid silica system.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.5-0.7%, and the viscosity of the hydrogen-containing silicone oil is 10-1000mpa · s.
By adopting the technical scheme, under the action of the catalyst, the hydrogen-containing silicone oil and the vinyl silicone oil form Si-C bonds, and the crosslinking degree of the liquid silicone rubber can be adjusted by matching with other reagents, so that the tensile strength of a vulcanized rubber product is improved, and the liquid silicone rubber with moderate hardness and stable product quality and long storage time is obtained by matching with the modified fumed silica.
Preferably, the liquid silica gel further comprises polycarbonate diester diol and polyethylene glycol; the mixing weight ratio of the mixture to the polycarbonate diester diol is 5-16: 1-3: 1.
By adopting the technical scheme, the polycarbonate diol and the polyethylene glycol promote the modified fumed silica to be uniformly dispersed in the liquid silica system for a long time, so that the liquid silica has excellent dispersibility, the stability of the liquid silica system is enhanced, the storage time of the liquid silica is prolonged, the storage time of the liquid silica can exceed 8 months, and meanwhile, the tensile strength, the tear strength, the hardness and the light transmittance of the liquid silica are also improved.
Preferably, the mass ratio of the liquid silica gel to the polycarbonate diol is (4:1) to (8: 1).
The polyethylene glycol plays a role in maintaining uniform dispersion of the gas phase method black-white carbon and a liquid silica gel system, precipitation and aggregation of the gas phase method black-white carbon are reduced, and when the mass ratio of the liquid silica gel to the polycarbonate diol is more than 5:1, the content of the liquid silica gel is relatively reduced, so that the phenomenon that the liquid silica gel is difficult to cure is possibly caused, and the use is influenced; when the mass ratio of the liquid silica gel to the polycarbonate diol is less than 10:1, the liquid silica gel may not be sufficient to maintain good dispersibility for a long time, and the storage time of the liquid silica gel is shortened; within this range, the liquid silica gel can be stably stored for a long period of time while exhibiting excellent dispersibility.
Preferably, the mass ratio of the polyethylene glycol to the liquid silica gel is (5:1) - (10: 1).
The polyethylene glycol plays a role in maintaining the uniform dispersion of the fumed silica and the liquid silica gel system, and the precipitation and aggregation of the fumed silica are reduced; when the mass ratio of the liquid silica gel to the polyethylene glycol is more than 5:1, the liquid silica gel is difficult to solidify or is in a semi-solidified state in the subsequent use process, so that the use is influenced; when the mass ratio of the liquid silica gel to the polyethylene glycol is less than 10:1, the liquid silica gel may not be sufficient to maintain good dispersibility for a long time, and the storage time of the liquid silica gel is shortened; within this range, the liquid silica gel can be stably stored for a long period of time while exhibiting excellent dispersibility.
In a second aspect, the present application provides a method for preparing a liquid silica gel having excellent dispersibility, which adopts the following technical scheme:
a preparation method of liquid silica gel with excellent dispersibility comprises the following steps:
1) weighing vinyl silicone oil and hydroxyl silicone oil according to the weight, uniformly stirring, heating to 120-150 ℃, slowly adding a silane treating agent, uniformly stirring, stirring for 1-1.5 h under the condition that the vacuum degree is-0.09-0.1 MPa, cooling to 40 ℃ to prepare a base material, and uniformly dividing the base material into a first base material and a second base material;
2) uniformly mixing the modified fumed silica and the ceramic powder according to the parts by weight, adding the pentenyl acetate to obtain mixed powder, adding the mixed powder into the first base material by 3-5 times, uniformly stirring, adding the catalyst, and uniformly stirring under the condition that the vacuum degree is-0.09 to-0.1 MPa to obtain a component A;
3) weighing diethylene glycol dimethyl ether, hydrogen-containing silicone oil, acrylate and an inhibitor according to the weight parts, adding the diethylene glycol dimethyl ether, the hydrogen-containing silicone oil, the acrylate and the inhibitor into the second base material, uniformly stirring, adding a catalyst, and uniformly stirring under the condition that the vacuum degree is-0.09 to-0.1 MPa to obtain a component B;
4) and uniformly mixing the composition A and the composition B to obtain the liquid silicone rubber.
By adopting the technical scheme, the first base material and the second base material are prepared in the step 1), the high-molecular elastomer is obtained, and the high-molecular elastomer has good physical and mechanical properties, so that other reagents are added subsequently, the fumed silica is uniformly dispersed in the liquid silica gel, the tear resistance, resilience and stability of the liquid silica gel are also improved, the component A and the component B are mixed, the fumed silica in a mixed system can be uniformly dispersed, and the tensile strength, tear strength and hardness of the liquid silica gel are improved.
Preferably, 10-15 parts of polycarbonate diol and 5-15 parts of polyethylene glycol are weighed according to parts by weight, added into the liquid silicone rubber prepared in the step 4), and uniformly stirred under the condition that the vacuum degree is-0.09 to-0.1 MPa.
By adopting the technical scheme, the polycarbonate diol and the polyethylene glycol added in the step 4) can keep the fumed silica uniformly dispersed in the liquid silicone colloid system for a long time, and the storage time of the fumed silica is prolonged.
Preferably, the dosage of the pentenyl acetate is not more than 3-15% of the total mass of the component A.
By adopting the technical scheme, the pentenyl acetate can reduce the friction force between the fumed silica and reduce the agglomeration of the fumed silica, so that the modified fumed silica can be uniformly dispersed in a liquid silica system. If the content of the pentenyl acetate is less than 3%, the agglomeration of the white carbon black by a gas phase method is increased, and the tensile strength of the vulcanized rubber product is weakened; if the content of the pentenyl acetate exceeds 15%, the lubricating effect of the pentenyl acetate is increased, so that the adhesion of substances in the liquid silica gel system is weakened, and the physical properties of the liquid silica gel system are deteriorated.
Preferably, the polyacrylate constitutes no more than 6% of the total mass of component B.
By adopting the technical scheme, the polyacrylate has good aging resistance, the tensile strength of vulcanization of the liquid silica gel can be enhanced by adding the polyacrylate into the component B, if the usage amount of the polyacrylate exceeds 6% of the total mass of the component B, the polyacrylate can firstly react with the silicone oil, and the excessive polyacrylate reacts with the silicone oil copolymer, so that the copolymer is broken, the physical property of the liquid silica gel is changed, the physical property of the liquid silica gel is weakened, and the dispersibility of the liquid silica gel is influenced.
Preferably, the mass ratio of the component A to the component B is (0.9:1) to (1.1: 1).
By adopting the technical scheme, when the mass ratio of the component A to the component B is less than 0.9:1, the liquid silica gel can not be completely cured; when the mass ratio of the component A to the component B is more than 1.1: 1, it may result in incomplete curing of the liquid silicone gel.
In summary, the present application has the following beneficial effects:
the ceramic powder is attached to the surface of the modified fumed silica, so that the agglomeration of the modified fumed silica is reduced, and the modified fumed silica can be uniformly dispersed in a system, so that the liquid silica has better fluidity; under the combined action of the pentenyl acetate, the diethylene glycol dimethyl ether and the polyacrylate, the modified fumed silica has good compatibility in a pentenyl acetate system, the fumed silica can be uniformly dispersed in a liquid silica gel system and can be stored for a long time, and the storage time can reach more than 8 months.
Detailed Description
The following comparative examples and examples further illustrate the present application in detail.
The raw materials used in the preparation examples, examples and comparative examples of the present application are all commercially available as shown in table 1.
TABLE 1 sources of raw materials
Preparation example of liquid silica gel
Example 1
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1) weighing 1 kg of vinyl silicone oil, 0.28 kg of hydroxyl silicone oil and 0.07 kg of amylene acetate according to the weight, uniformly stirring, heating to 120 ℃, slowly adding 0.07 kg of silane treating agent (KH550), uniformly stirring, stirring for 1h under the condition that the vacuum degree is-0.09 MPa, cooling to 40 ℃, preparing a base material, and uniformly dividing the base material into a first base material and a second base material;
2) uniformly mixing 0.14 kg of modified fumed silica and 0.21 kg of ceramic powder (the particle size of the ceramic powder is 10nm) according to the parts by weight to obtain mixed powder, adding the mixed powder into a first base material in batches, uniformly stirring, adding 0.00009 kg of catalyst (di-n-butyltin dilaurate), and stirring under the condition that the vacuum degree is-0.09 MPa to obtain a component A;
3) weighing 0.14 kg of diethylene glycol dimethyl ether, 0.007 kg of hydrogen-containing silicone oil, 0.07 kg of polyacrylate and 0.00003 kg of inhibitor (1-ethynylcyclohexanol) according to the weight parts, adding the materials into a second base material, and uniformly stirring the materials under the condition that the vacuum degree is-0.09 MPa to obtain a component B;
4) and uniformly mixing the composition A and the composition B to obtain the liquid silicone rubber.
Example 2
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1) weighing 1 kg of vinyl silicone oil, 0.31 kg of hydroxyl silicone oil and 0.09 kg of amylene acetate according to the weight, uniformly stirring, heating to 135 ℃, slowly adding 0.09 kg of silane treating agent (KH550), uniformly stirring, stirring for 1.25h under the condition that the vacuum degree is-0.09 MPa, cooling to 40 ℃, preparing a base material, and uniformly dividing the base material into a first base material and a second base material;
2) uniformly mixing 0.16 kg of modified fumed silica and 0.22 kg of ceramic powder (the particle size of the ceramic powder is 12nm) according to the parts by weight to obtain mixed powder, adding the mixed powder into a first base material in batches, uniformly stirring, adding 0.0004 kg of catalyst (di-n-butyltin dilaurate), and uniformly stirring under the condition that the vacuum degree is-0.09 MPa to obtain a component A;
3) weighing 0.17 kg of diethylene glycol dimethyl ether, 0.06 kg of hydrogen-containing silicone oil, 0.093 kg of polyacrylate and 0.00025 kg of inhibitor (1-ethynylcyclohexanol) according to the weight parts, adding the materials into a second base material, and uniformly stirring the materials under the condition that the vacuum degree is-0.09 MPa to obtain a component B;
4) and uniformly mixing the composition A and the composition B to obtain the liquid silicone rubber.
Example 3
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1) weighing 1 kg of vinyl silicone oil, 0.33 kg of hydroxyl silicone oil and 0.11 kg of amylene acetate according to the weight, uniformly stirring, heating to 150 ℃, slowly adding 0.11 kg of silane treating agent (KH550), uniformly stirring, stirring for 1.5h under the condition that the vacuum degree is 0.1MPa, cooling to 40 ℃, preparing a base material, and uniformly dividing the base material into a first base material and a second base material;
2) uniformly mixing 0.167 kg of modified fumed silica and 0.22 kg of ceramic powder (the particle size of the ceramic powder is 15nm) according to the parts by weight to obtain mixed powder, adding the mixed powder into the first base material in batches, uniformly stirring, adding 0.00067 kg of catalyst (di-n-butyltin dilaurate), and uniformly stirring under the condition that the vacuum degree is 0.1MPa to obtain a component A;
3) weighing 0.167 kg of diethylene glycol dimethyl ether, 0.11 kg of hydrogen-containing silicone oil, 0.11 kg of polyacrylate and 0.00044 kg of inhibitor (1-ethynyl cyclohexanol) according to the weight parts, adding the materials into a second base material, and uniformly stirring the materials under the condition that the vacuum degree is 0.1MPa to obtain a component B;
4) and uniformly mixing the composition A and the composition B to obtain the liquid silicone rubber.
Example 4
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1 kg of the liquid silicone rubber obtained in example 1 was charged with 0.2 kg of polycarbonate diol and 0.2 kg of polyethylene glycol in parts by weight, and the mixture was stirred uniformly under a vacuum of 0.1MPa to obtain a liquid silicone rubber having excellent dispersibility.
Example 5
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1 kg of the liquid silicone rubber obtained in example 2 was taken, 0.25 kg of polycarbonate diol and 0.125 kg of polyethylene glycol were added in parts by weight, and the mixture was stirred uniformly under a vacuum of 0.1MPa to obtain a liquid silicone rubber having excellent dispersibility.
Example 6
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1 kg of the liquid silicone rubber obtained in example 3 was charged with 0.188 kg of polycarbonate diol and 0.063 kg of polyethylene glycol in parts by weight, and the mixture was stirred uniformly under a vacuum of 0.1MPa to obtain a liquid silicone rubber having excellent dispersibility.
Example 7
A liquid silica gel with excellent dispersibility is prepared by the following steps:
1 kg of the liquid silicone rubber obtained in example 3 was charged with 0.2 kg of polycarbonate diol and 0.1 kg of polyethylene glycol in parts by weight, and the mixture was stirred uniformly under a vacuum of 0.1MPa to obtain a liquid silicone rubber having excellent dispersibility.
Comparative example
Comparative example 1
Comparative example 1 differs from example 3 in that: in comparative example 1, the same amount of titanium dioxide was used instead of ceramic powder, pentenyl acetate, diethylene glycol dimethyl ether and polyacrylate.
Comparative example 2
Comparative example 2 differs from example 3 in that: in comparative example 1, the same amount of titanium dioxide was used instead of the ceramic powder.
Comparative example 3
Comparative example 3 differs from example 3 in that: in comparative example 3, the same amount of titanium dioxide was used instead of pentenyl acetate.
Comparative example 4
Comparative example 4 differs from example 3 in that: in comparative example 4, the same amount of titanium dioxide was used instead of diethylene glycol dimethyl ether.
Comparative example 5
Comparative example 5 differs from example 3 in that: in comparative example 5, the same amount of titanium dioxide was used instead of polyacrylate.
Performance test
1. The tensile strength of the silicone rubber was determined in accordance with GB/T528-2009.
2. The tear strength of the silicone rubber was determined in accordance with GB/T529 and 2008.
3. The Shore A hardness of the silicone rubber is determined according to GB/T531-2008.
4. The light transmittance of the silicone rubber was measured using a spectrophotometer.
Detection method/test method
TABLE 1 mechanical Properties and light transmittance of liquid silica gels having Excellent dispersibility
As can be seen by combining examples 1-7 with Table 1, the tensile strength, tear strength, Shore hardness and light transmittance were all higher in examples 1-7 than in comparative examples 1-5. Therefore, under the combined action of the ceramic powder, the pentenyl acetate, the diethylene glycol dimethyl ether and the polyacrylate, the fumed silica can be uniformly dispersed in a liquid silica gel system to obtain the liquid silica gel with excellent dispersibility, so that the tensile strength, the tearing strength, the Shore hardness and the light transmittance of the liquid silica gel are improved.
Combining examples 1-3 and examples 4-7 with table 1, it can be seen that tensile strength, tear strength, shore hardness and light transmittance in examples 1-3 are all less than in examples 4-7, and thus it can be seen that after component a and component B are mixed, polycarbonate diol and polyethylene glycol are added, so that fumed silica can be uniformly dispersed in a liquid silica system, and a liquid silica with excellent dispersibility is obtained, thereby improving tensile strength, tear strength, shore hardness and light transmittance of the liquid silica.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (11)
1. A liquid silica gel excellent in dispersibility, characterized in that: the liquid silica gel comprises a mixture, wherein the mixture comprises the following raw materials in parts by weight:
70-90 parts of vinyl silicone oil and 20-30 parts of hydroxyl silicone oil
10-15 parts of modified fumed silica
5-10 parts of silane treating agent
0.006-0.06 part of catalyst
15-20 parts of ceramic powder
5-10 parts of pentenyl acetate
10-15 parts of diethylene glycol dimethyl ether
5-10 parts of polyacrylate
0.5-10 parts of hydrogen-containing silicone oil
0.002-0.04 parts of inhibitor.
2. The liquid silica gel excellent in dispersibility according to claim 1, characterized in that: the particle size of the ceramic powder is 10-15 nm.
3. The liquid silica gel excellent in dispersibility according to claim 1, characterized in that: the hydrogen content of the hydrogen-containing silicone oil is 0.5-0.7%, and the viscosity of the hydrogen-containing silicone oil is 10-1000mpa & s.
4. The liquid silica gel excellent in dispersibility according to claim 1, characterized in that: the liquid silica gel also comprises polycarbonate diester diol and polyethylene glycol; the mixing weight ratio of the mixture to the polycarbonate diester diol to the polyethylene glycol is 5-16: 1-3: 1.
5. The liquid silica gel excellent in dispersibility according to claim 4, characterized in that: the mass ratio of the mixture to the polycarbonate diol is (4:1) - (8: 1).
6. The liquid silica gel excellent in dispersibility according to claim 4, characterized in that: the mass ratio of the polyethylene glycol to the mixture is (5:1) - (10: 1).
7. A method for preparing the liquid silica gel having excellent dispersibility according to any one of claims 1 to 3, characterized in that: the method comprises the following steps:
1) weighing vinyl silicone oil, hydroxyl silicone oil and amylene acetate according to the weight parts, uniformly stirring, heating to 120-150 ℃, slowly adding a silane treating agent, uniformly stirring, stirring for 1-1.5 hours under the condition that the vacuum degree is-0.09 to-0.1 MPa, cooling to 40 ℃ to prepare a base material, and uniformly dividing the base material into a first base material and a second base material;
2) uniformly mixing the modified fumed silica and the ceramic powder according to the parts by weight to obtain mixed powder, adding the mixed powder into the first base material in batches, uniformly stirring, adding a catalyst, and uniformly stirring under the condition that the vacuum degree is-0.09 to-0.1 MPa to obtain a component A;
3) weighing diethylene glycol dimethyl ether, hydrogen-containing silicone oil, polyacrylate and an inhibitor according to the weight parts, adding the diethylene glycol dimethyl ether, the hydrogen-containing silicone oil, the polyacrylate and the inhibitor into the second base material, uniformly stirring the mixture, and uniformly stirring the mixture under the condition that the vacuum degree is-0.09 to-0.1 MPa to obtain a component B;
4) and uniformly mixing the composition A and the composition B to obtain the liquid silicone rubber.
8. The method for producing a liquid silica gel excellent in dispersibility according to claim 7, characterized in that: weighing 10-15 parts of polycarbonate diol and 5-15 parts of polyethylene glycol according to parts by weight, adding the polycarbonate diol and the polyethylene glycol into the liquid silicone rubber prepared in the step 4), and uniformly stirring under the condition that the vacuum degree is-0.09 to-0.1 MPa.
9. The method for producing a liquid silica gel excellent in dispersibility according to claim 7, characterized in that: the dosage of the pentenyl acetate is not more than 5 percent of the total mass of the component A.
10. The method for producing a liquid silica gel excellent in dispersibility according to claim 7, characterized in that: the amount of the polyacrylate is not more than 6% of the total mass of the component B.
11. The method for producing a liquid silica gel excellent in dispersibility according to claim 7, characterized in that: the mass ratio of the component A to the component B is (0.9:1) - (1.1: 1).
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