CN116715964A - Liquid silica gel with high cold resistance and preparation process thereof - Google Patents
Liquid silica gel with high cold resistance and preparation process thereof Download PDFInfo
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- CN116715964A CN116715964A CN202310789375.XA CN202310789375A CN116715964A CN 116715964 A CN116715964 A CN 116715964A CN 202310789375 A CN202310789375 A CN 202310789375A CN 116715964 A CN116715964 A CN 116715964A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000007788 liquid Substances 0.000 title claims abstract description 68
- 239000000741 silica gel Substances 0.000 title claims abstract description 65
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 43
- 229920000642 polymer Polymers 0.000 claims abstract description 33
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 21
- 229920001971 elastomer Polymers 0.000 claims abstract description 19
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 16
- 239000004945 silicone rubber Substances 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 10
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 239000013530 defoamer Substances 0.000 claims abstract description 7
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920002545 silicone oil Polymers 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002518 antifoaming agent Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 3
- 239000012964 benzotriazole Substances 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 125000005375 organosiloxane group Chemical group 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- -1 vinyl siloxane Chemical class 0.000 claims description 3
- 229910052882 wollastonite Inorganic materials 0.000 claims description 3
- 239000010456 wollastonite Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 7
- 238000005336 cracking Methods 0.000 abstract description 3
- 239000012783 reinforcing fiber Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 22
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 12
- 238000004073 vulcanization Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 230000009477 glass transition Effects 0.000 description 4
- 238000001746 injection moulding Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- 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
-
- 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
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
-
- 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
-
- 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
-
- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses high-cold-resistance liquid silica gel and a preparation process thereof, and relates to the technical field of liquid silica gel preparation. The invention is prepared from a component A, a component B and a fiber polymer, wherein the content ratio of the component A to the component B to the fiber polymer is 12:8:1-18:7:1, and the component A comprises methoxy-terminated silicone oil and a catalyst; the component B comprises methyl vinyl silicone rubber raw rubber, an inhibitor, a porcelain powder defoamer and a filler. According to the invention, by changing the formula of the liquid silica gel and adding the reinforcing fiber for matching during the production of the liquid silica gel, the state data of the liquid silica gel product in an extremely cold state is improved, so that the liquid silica gel product still maintains better elasticity and tensile strength in the extremely cold state, the failure caused by embrittlement, hardening and cracking in a low-temperature state for a long time is prevented, and meanwhile, the prepared liquid silica gel product also has excellent stretch-break elongation and tear resistance, and the use effect is ensured.
Description
Technical Field
The invention relates to the technical field of liquid silica gel preparation, in particular to high-cold-resistance liquid silica gel and a preparation process thereof.
Background
Liquid silicone rubber, i.e. injection molded Liquid Silicone Rubber (LSR): the whole name is injection molding liquid silicone rubber, and the vulcanizing device is an injection molding machine. The injection molding process is very simple, the product accuracy is high, the yield is high (the A/B glue is mixed and molded for a few seconds at a certain temperature), the injection molding process has the advantages of saving labor, energy, materials and the like, can produce all products produced by high-temperature glue, and is a main stream of the development of silicone rubber materials in the future.
The liquid silica gel is organic silica gel which is relative to mixed semi-solid silicone rubber and common room temperature vulcanized single-component silica gel, has good fluidity and quick vulcanization, and can be cast and injection molded. Currently, liquid silica gel has been used in a variety of products including infant products, medical products, automotive products, and the like.
The liquid silicone rubber is applied to the field of automobiles, and generally relates to production of products such as automobile sealing rings, tires or cable wrapping layers, for example, chinese patent No. CN100503223C discloses a manufacturing method of the silicone rubber sealing rings, which comprises the steps of extruding silicone rubber strips by an extruder, baking, cutting into round shapes, coating liquid silicone rubber on the joints, vulcanizing and baking to form the silicone rubber sealing rings by the silicone rubber strips, wherein the silicone rubber sealing rings are connected by the same material; the silicon rubber sealing ring produced by the manufacturing process has larger tensile strength, and the strength of the joint is larger than that of other positions; the invention has the advantages of lower cost, better product quality, higher production efficiency and the like.
The working temperature of the liquid silicone rubber material is generally between 50 ℃ below zero and 200 ℃, and the low temperature resistance of part of the material can reach 60 ℃ below zero, so that most working environments can be covered, but the liquid silicone rubber material has defects for application in certain extreme environments. For example, when the rubber is applied to a scientific research vehicle in a south pole area, the lowest temperature can reach minus 89 ℃ because the south pole area is in a low-temperature state throughout the year, products such as tires, sealing rings and the like made of common liquid silicone rubber materials cannot adapt to extremely cold working states at all, and the products become hard, brittle and crack and lose effectiveness due to the excessively low temperature, so that the products are damaged and bring danger.
Disclosure of Invention
Aiming at the technical problems, the invention overcomes the defects of the prior art and provides high-cold-resistance liquid silica gel and a preparation process thereof.
In order to solve the technical problems, the invention provides the high-cold-resistance liquid silica gel and the preparation process thereof.
The technical effects are as follows: through changing the formula of the liquid silica gel, adding reinforcing fibers for cooperation during the production of the liquid silica gel, the state data of the liquid silica gel product in an extremely cold state is improved, the liquid silica gel product still keeps better elasticity and tensile strength in the extremely cold state, the failure caused by embrittlement, hardening and cracking in a low-temperature state for a long time is prevented, and meanwhile, the prepared liquid silica gel product also has excellent stretch-break elongation and tear resistance, and the use effect is ensured.
The technical scheme of the invention is as follows: a high-cold-resistance liquid silica gel is prepared from a component A, a component B and a fiber polymer, wherein the content ratio of the component A to the component B to the fiber polymer is 12:8:1-18:7:1;
the component A comprises 80-100 parts of methoxy-terminated silicone oil and 2-5 parts of catalyst by weight;
the component B comprises 50 to 60 parts of methyl vinyl silicone rubber raw rubber, 2 to 6 parts of inhibitor, 4 to 8 parts of porcelain powder, 1 to 3 parts of defoamer and 12 to 18 parts of filler according to the weight component.
Further, the preferred content ratio of component A, component B and the fibrous polymer is 14:8:1.
The fiber polymer of the high-cold-resistance liquid silica gel is one or more of PPS fiber, PI fiber, PAN fiber and PA6 fiber.
The catalyst is a metal nickel catalyst, and the ceramic powder is powder prepared from at least one of aluminum hydroxide, wollastonite, zirconia and lithium porcelain stone, and the granularity is 50-120 microns.
The high-cold-resistance liquid silica gel is characterized in that the defoaming agent is one or more of an organosiloxane defoaming agent, a polyether defoaming agent, a silicon and ether grafting defoaming agent, and the filler is white carbon black.
The high cold resistance liquid silica gel is prepared from one or more of vinyl siloxane, alkynol, alkynate, 2-vinyl isopropyl ketone and benzotriazole.
A preparation process of high-cold-resistance liquid silica gel comprises the following steps:
s1, preparing a component A, namely adding methoxy-terminated silicone oil into a stirrer, adding 30 parts of deionized water, mixing and stirring for 20min at normal temperature, dropwise adding 15-20 parts of ethyl orthosilicate, heating to 85 ℃ for reaction for 2h, cooling to normal temperature, performing vacuum reduced pressure distillation to obtain an intermediate product, adding a quantitative catalyst into the intermediate product, stirring for 15min, heating to 90-100 ℃, and reacting for 3h to obtain the component A;
s2, preparing a component B, namely placing quantitative methyl vinyl silicone rubber raw rubber into a kneader, adding quantitative porcelain powder and 10-20 parts of deionized water, carrying out vacuum stirring treatment for 3 hours at 170-190 ℃, passing through three rollers to obtain a base rubber, cooling to normal temperature, and adding quantitative defoamer and filler to obtain the component B;
s3, preparing a mixture, namely adding the component A into the component B, adding quantitative fiber polymer, mixing and stirring for 30min, adding inhibitor, uniformly stirring, performing heat treatment to obtain colloid, performing grinding treatment on the colloid, and performing filter pressing and packaging to obtain a high-cold-resistance liquid silica gel finished product.
In the preparation process of the high-cold-resistance liquid silica gel, in the step S1, the preferable addition amount of the tetraethoxysilane is 18 parts, and the preferable temperature is 98 ℃ during the heating reaction.
In the preparation process of the high-cold-resistance liquid silica gel, in the step S2, the preferable adding amount of deionized water is 14 parts, and the preferable temperature of the vacuum stirring treatment is 185 ℃.
In the preparation process of the high-cold-resistance liquid silica gel, in the step S3, the temperature of heat treatment is maintained at 158-162 ℃, and the mixture is mixed for 200min under the vacuum condition.
The beneficial effects of the invention are as follows:
(1) According to the invention, after a proper amount of fiber polymer is added, the flexibility of rubber molecules can be increased, the acting force among molecules is reduced, so that a molecular chain segment is easy to move, and after a proper amount of fiber polymer is added, the vulcanization speed of liquid silica gel can be increased, the hysteresis loss after vulcanization is reduced, and the creep rate is increased, so that the acting force among molecules in the liquid rubber can be reduced, and the cold resistance is improved;
(2) According to the invention, after the fiber polymer is added, the mechanical property of the liquid silica gel in the high and cold state can be improved, and the viscosity of some liquid silica gel can be reduced, but the tensile strength and the stretch-break elongation of the material in the high and cold state can be greatly improved, the hardness of the material is optimized, and the service life and the state of the liquid silica gel product in the high and cold state are improved;
(3) In the invention, the elasticity and pressure resistance of the liquid silicone rubber material added with the fiber polymer at the conventional use temperature are greatly enhanced, the liquid silicone rubber material can be applied to more occasions, and meanwhile, the production cost is low, and the consumption of manpower and material resources is reduced;
(4) According to the invention, by changing the formula of the liquid silica gel and adding the reinforcing fiber for cooperation during the production of the liquid silica gel, the state data of the liquid silica gel product in an extremely cold state is improved, so that the liquid silica gel product still maintains better elasticity and tensile strength in the extremely cold state, the failure caused by embrittlement, hardening and cracking in a low-temperature state for a long time is prevented, and meanwhile, the prepared liquid silica gel product also has excellent stretch-break elongation and tear resistance, and the use effect is ensured.
Detailed Description
The high-cold-resistance liquid silica gel is mainly prepared from a component A, a component B and a fiber polymer, wherein the content ratio of the component A to the component B to the fiber polymer is 12:8:1-18:7:1. In the present invention, the preferred content ratio of component A, component B and the fibrous polymer is 14:8:1.
Wherein the component A comprises 80-100 parts of methoxy-terminated silicone oil and 2-5 parts of catalyst by weight;
the component B comprises 50 to 60 parts of methyl vinyl silicone rubber raw rubber, 2 to 6 parts of inhibitor, 4 to 8 parts of porcelain powder, 1 to 3 parts of defoamer and 12 to 18 parts of filler according to the weight component.
In the existing liquid silica gel material, factors influencing the cold resistance of the material mainly comprise the glass transition temperature, crystallization condition, flexibility among molecular chains, type of cross-linking bonds and selection of a vulcanization system, and the influence of the filling material on the cold resistance. In general, plasticizers may be added to reduce the glass transition temperature in order to improve the cold resistance of the rubber.
In the invention, the glass transition temperature is reduced by increasing the fiber polymer, so that the cold resistance of the liquid silica gel is improved. The invention discovers that after a proper amount of fiber polymer is added, the flexibility of rubber molecules can be increased, the acting force among molecules can be reduced, the molecular chain segments are easy to move, and after a proper amount of fiber polymer is added, the vulcanization speed of liquid silica gel can be increased, the hysteresis loss after vulcanization is reduced, and the creep rate is increased, so that the acting force among molecules in the liquid rubber can be reduced, and the cold resistance is improved.
In addition, the porcelain powder is also added in the invention. The ceramic powder is generally added into the silicone rubber, and the synergistic flame retardant effect of the ceramic powder and the flame retardant are mainly utilized to synergistically improve the flame retardant effect of the silicone rubber. However, the porcelain powder is added in the invention, so that on one hand, the flame retardant effect is improved, and on the other hand, the crosslinking density in the liquid rubber is improved, and the crosslinking bond is improved during vulcanization, so that the tensile strength of the liquid rubber is increased. In addition, after the fiber polymer is added, the fiber polymer is free at the edge of the fiber polymer, so that the flexibility of the liquid silica gel is improved, the influence of temperature on material crystallization is reduced, the fiber polymer and the liquid silica gel have synergistic effect, and the glass transition temperature of the material is reduced.
The fiber polymer adopted in the invention is one or more of PPS fiber, PI fiber, PAN fiber and PA6 fiber. The catalyst is a metal nickel catalyst, and the porcelain powder is powder prepared from at least one of aluminum hydroxide, wollastonite, zirconia and lithium porcelain stone, and the granularity is 50-120 microns.
In the component B, the defoaming agent is one or more of an organosiloxane defoaming agent, a polyether defoaming agent, a silicon and ether grafting defoaming agent, and the filler is white carbon black. The inhibitor is one or more of vinyl siloxane, alkynol, alkynate, 2-vinyl isopropyl ketone and benzotriazole.
After the fiber polymer is added, the mechanical property of the liquid silica gel in the high and cold state can be improved, the viscosity of some liquid silica gel can be reduced, but the tensile strength and the tensile elongation of the material in the high and cold state can be greatly improved, the hardness of the material is optimized, and the service life and the state of the liquid silica gel product in the high and cold state are improved. The pressure resistance and elasticity of the liquid silica gel material product can be enhanced.
The invention also provides a preparation process of the high-cold-resistance liquid silica gel, which comprises the following steps:
s1, preparing a component A, namely adding methoxy-terminated silicone oil into a stirrer, adding 30 parts of deionized water, mixing and stirring for 20min at normal temperature, dropwise adding 15-20 parts of ethyl orthosilicate, heating to 85 ℃ for reaction for 2h, cooling to normal temperature, performing vacuum reduced pressure distillation to obtain an intermediate product, adding a quantitative catalyst into the intermediate product, stirring for 15min, heating to 90-100 ℃, and reacting for 3h to obtain the component A.
In this step, the preferable addition amount of ethyl orthosilicate is 18 parts, and the preferable temperature at the time of the temperature-raising reaction is 98 ℃.
S2, preparing a component B, namely placing quantitative methyl vinyl silicone rubber raw rubber into a kneader, adding quantitative porcelain powder and 10-20 parts of deionized water, carrying out vacuum stirring treatment for 3 hours at 170-190 ℃, passing through three rollers to obtain a base rubber, cooling to normal temperature, and adding quantitative defoamer and filler to obtain the component B;
in this step, the preferable addition amount of deionized water is 14 parts, and the preferable temperature of the vacuum stirring treatment is 185 ℃.
S3, preparing a mixture, namely adding the component A into the component B, adding quantitative fiber polymer, mixing and stirring for 30min, adding inhibitor, uniformly stirring, performing heat treatment to obtain colloid, maintaining the heat treatment temperature at 158-162 ℃, and mixing for 200min under vacuum condition. Grinding the colloid, and press-filtering and packaging to obtain a high-cold-resistance liquid silica gel finished product.
The invention also verifies the mechanical properties of different liquid silicone rubber products in the high and cold state after adding fiber polymer and porcelain powder and changing various components through a plurality of groups of examples, and is also provided with comparative example reference results.
TABLE 1 base component content Table in different examples
The content ratio of the component A, the component B and the fiber polymer in the above examples was 14:8:1.
Table 2 table of the content ratios of the components in the examples
The properties of the materials in each example and comparative example were tested under different temperature conditions.
Table 3 performance test table for different articles in each example
As shown in Table 3, the liquid silica gel prepared in example 7 exhibited the best performance at normal temperature and low temperature, and it was confirmed that the optimum ratio was 14:8:1, and the optimum content of the porcelain powder was 6 parts. As can be seen from Table 3, the liquid rubber product prepared by the invention has reduced performance but smaller reduction range after the temperature is reduced to-90 ℃, while in the comparative example, the hardness is sharply increased, the tensile strength is obviously increased, the elongation at break and the tearing strength are obviously reduced after the temperature is reduced to-90 ℃, which means that the material is hardened in a high-cold state, the elasticity is reduced, and the mechanical property is sharply reduced. In addition, as can be seen from table 3, the addition of the ceramic powder and the fiber polymer has obvious influence on the performance of the liquid silica gel in the severe cold state, and the two have a synergistic effect when added together, and the influence of the fiber polymer on the ceramic powder is larger when the two are added independently.
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (10)
1. The high-cold-resistance liquid silica gel is characterized by being prepared from a component A, a component B and a fiber polymer, wherein the content ratio of the component A to the component B to the fiber polymer is 12:8:1-18:7:1;
the component A comprises 80-100 parts of methoxy-terminated silicone oil and 2-5 parts of catalyst by weight;
the component B comprises 50 to 60 parts of methyl vinyl silicone rubber raw rubber, 2 to 6 parts of inhibitor, 4 to 8 parts of porcelain powder, 1 to 3 parts of defoamer and 12 to 18 parts of filler according to the weight component.
2. The high cold resistant liquid silica gel according to claim 1, wherein: the preferred content ratio of the component A, the component B and the fiber polymer is 14:8:1.
3. The high cold resistant liquid silica gel according to claim 1, wherein: the fiber polymer is one or more of PPS fiber, PI fiber, PAN fiber and PA6 fiber.
4. The high cold resistant liquid silica gel according to claim 1, wherein: the catalyst is a metal nickel catalyst, and the porcelain powder is powder prepared from at least one of aluminum hydroxide, wollastonite, zirconia and lithium porcelain stone, and the granularity is 50-120 microns.
5. The high cold resistant liquid silica gel according to claim 1, wherein: the defoaming agent is one or more of an organosiloxane defoaming agent, a polyether defoaming agent, a silicon and ether grafting defoaming agent, and the filler is white carbon black.
6. The high cold resistant liquid silica gel according to claim 1, wherein: the inhibitor is one or more combinations of vinyl siloxane, alkynol, alkynoate, 2-vinyl isopropyl ketone and benzotriazole.
7. The preparation process of the high-cold-resistance liquid silica gel is characterized by comprising the following steps of:
s1, preparing a component A, namely adding methoxy-terminated silicone oil into a stirrer, adding 30 parts of deionized water, mixing and stirring for 20min at normal temperature, dropwise adding 15-20 parts of ethyl orthosilicate, heating to 85 ℃ for reaction for 2h, cooling to normal temperature, performing vacuum reduced pressure distillation to obtain an intermediate product, adding a quantitative catalyst into the intermediate product, stirring for 15min, heating to 90-100 ℃, and reacting for 3h to obtain the component A;
s2, preparing a component B, namely placing quantitative methyl vinyl silicone rubber raw rubber into a kneader, adding quantitative porcelain powder and 10-20 parts of deionized water, carrying out vacuum stirring treatment for 3 hours at 170-190 ℃, passing through three rollers to obtain a base rubber, cooling to normal temperature, and adding quantitative defoamer and filler to obtain the component B;
s3, preparing a mixture, namely adding the component A into the component B, adding quantitative fiber polymer, mixing and stirring for 30min, adding inhibitor, uniformly stirring, performing heat treatment to obtain colloid, performing grinding treatment on the colloid, and performing filter pressing and packaging to obtain a high-cold-resistance liquid silica gel finished product.
8. The process for preparing the high-cold-resistance liquid silica gel according to claim 7, wherein the process comprises the following steps: in the step S1, the preferable addition amount of the tetraethoxysilane is 18 parts, and the preferable temperature in the heating reaction is 98 ℃.
9. The process for preparing the high-cold-resistance liquid silica gel according to claim 7, wherein the process comprises the following steps: in the step S2, the preferable addition amount of deionized water is 14 parts, and the preferable temperature of the vacuum stirring treatment is 185 ℃.
10. The process for preparing the high-cold-resistance liquid silica gel according to claim 7, wherein the process comprises the following steps: in the step S3, the temperature of the heat treatment is maintained at 158-162 ℃, and the mixture is mixed for 200min under the vacuum condition.
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| CN202310789375.XA CN116715964A (en) | 2023-06-30 | 2023-06-30 | Liquid silica gel with high cold resistance and preparation process thereof |
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