CN116042174A - Oil-resistant silicone sealant and preparation method and application thereof - Google Patents
Oil-resistant silicone sealant and preparation method and application thereof Download PDFInfo
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- CN116042174A CN116042174A CN202310165824.3A CN202310165824A CN116042174A CN 116042174 A CN116042174 A CN 116042174A CN 202310165824 A CN202310165824 A CN 202310165824A CN 116042174 A CN116042174 A CN 116042174A
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- resistant silicone
- silicone sealant
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 169
- 239000003921 oil Substances 0.000 claims abstract description 125
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 83
- 229960000892 attapulgite Drugs 0.000 claims abstract description 48
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 48
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229920005989 resin Polymers 0.000 claims abstract description 40
- 239000011347 resin Substances 0.000 claims abstract description 40
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 40
- 239000010703 silicon Substances 0.000 claims abstract description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000006229 carbon black Substances 0.000 claims abstract description 24
- 238000007789 sealing Methods 0.000 claims abstract description 21
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 54
- 208000005156 Dehydration Diseases 0.000 claims description 40
- 230000018044 dehydration Effects 0.000 claims description 40
- 238000006297 dehydration reaction Methods 0.000 claims description 40
- 238000000227 grinding Methods 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 10
- 239000001038 titanium pigment Substances 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 6
- 230000008569 process Effects 0.000 abstract description 17
- 235000010215 titanium dioxide Nutrition 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 230000003014 reinforcing effect Effects 0.000 description 9
- 230000032683 aging Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 2
- 239000010687 lubricating oil Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000008782 xin-kang Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The application discloses an oil-resistant silicone sealant, a preparation method and application thereof, wherein the oil-resistant silicone sealant comprises the following components in parts by weight: 60-90 parts of organic silicon resin, 120-150 parts of light calcium carbonate, 1-5 parts of white carbon black, 5-10 parts of titanium dioxide, 8-15 parts of attapulgite, 1-3 parts of a binder and 10-20 parts of a coupling agent. The preparation method of the oil-resistant silicone sealant comprises the following steps: the oil-resistant silicone sealant prepared by the preparation method can be applied to the fields of building sealing, electrical appliance sealing, electronic sealing and automobile part sealing. The oil-resistant silicone sealant has the advantages that the oil-resistant silicone sealant is excellent in oil resistance, good in hardness, leveling property and tensile strength, and is difficult to generate bubbles in the curing process.
Description
Technical Field
The application relates to the technical field of high polymer materials, in particular to an oil-resistant silicone sealant and a preparation method and application thereof.
Background
The oil-resistant silicone sealant is a general sealing material and is mainly applied to sealing of various joints. In the prior art, only calcium carbonate is adopted in a part of oil-resistant silicone sealant for reinforcement to enhance the tensile resistance of the oil-resistant silicone sealant, but the silicone sealant is easy to generate bubbles in the surface drying process, and is easy to generate uneven surface after the surface drying, so that the leveling property and the oil resistance are poor; in addition, a large amount of modified substances are adopted in some oil-resistant silicone sealants, so that the problems of poor leveling property and oil resistance still exist, and the oil-resistant silicone sealants cannot be used in environments with more oil media.
In view of the foregoing, there is a need for an oil-resistant silicone sealant that can avoid air bubbles during curing and effectively improve the performance thereof, so as to solve the problems in the prior art.
Disclosure of Invention
In order to solve at least one technical problem, an oil-resistant silicone sealant which can avoid generating bubbles in the curing process and has effectively improved performance is developed.
On the one hand, the oil-resistant silicone sealant provided by the application comprises the following components in parts by weight: 60-90 parts of organic silicon resin, 120-150 parts of light calcium carbonate, 1-5 parts of white carbon black, 5-10 parts of titanium dioxide, 8-15 parts of attapulgite, 1-3 parts of binder and 10-20 parts of coupling agent.
By adopting the technical scheme, the light calcium carbonate, the white carbon black and the titanium pigment are introduced into the organic silicon resin on the basis of the formula of the conventional oil-resistant silicone sealant, so that the oil-resistant silicone sealant is enhanced, the tensile strength and the hardness of the oil-resistant silicone sealant can be effectively improved, and meanwhile, the oil resistance of the oil-resistant silicone sealant can be improved. The mechanism of the light calcium carbonate is that the surface of the light calcium carbonate can form stronger interaction force with structural molecules of the organic silicon resin, so that the light calcium carbonate can further strengthen the oil-resistant silicone sealant, and further effectively improve the tensile strength and hardness of the oil-resistant silicone sealant.
In addition, the attapulgite is introduced between the organic silicon resin and the light calcium carbonate, the characteristic of the attapulgite is utilized, and the mode that the attapulgite is attached to the surface of the light calcium carbonate part and then the organic silicon resin is introduced is adopted, so that the leveling property, the temperature resistance and the ageing resistance of the oil-resistant silicone sealant can be effectively improved, and meanwhile, a series of chemical reactions caused by excessive exposure of the light calcium carbonate to the environment can be avoided, so that bubbles are prevented from being generated in the curing process of the oil-resistant silicone sealant.
Optionally, the particle size of the light calcium carbonate is 50-80 nm.
By adopting the technical scheme, the light calcium carbonate with a specific particle size range can influence the reinforcing effect on the oil-resistant silicone sealant, and the smaller the particle size is, the more obvious the reinforcing effect is; however, when the particle size of the light calcium carbonate is smaller than a certain level, the introduced attapulgite is easily excessively attached to the surface of the light calcium carbonate, so that the reinforcing effect on the oil-resistant silicone sealant is reduced, and therefore, the particle size of the light calcium carbonate needs to be effectively selected and controlled.
Optionally, the mass ratio between the light calcium carbonate and the attapulgite is 10-15: 1.
by adopting the technical scheme, the proportion between the light calcium carbonate and the attapulgite can be adjusted to effectively control the adhesion of the attapulgite on part of the surface of the light calcium carbonate, so that the light calcium carbonate surface is prevented from being completely adhered by the attapulgite, and the reinforcing effect of the light calcium carbonate on the oil-resistant silicone sealant is affected.
Optionally, the binder is aluminosilicate, and the coupling agent is a silane coupling agent.
In a second aspect, the present application provides a method for preparing the oil-resistant silicone sealant, including the following steps:
s1, preparing a mixed material: mixing light calcium carbonate, attapulgite and a binder according to parts by weight to obtain a premix; mixing organic silicon resin, white carbon black and titanium pigment according to parts by weight, and adding premix according to parts by weight to obtain a mixed material;
s2, grinding treatment: grinding the mixed materials, and cooling after grinding;
s3, dehydration: carrying out dehydration treatment on the mixed material subjected to the grinding treatment in the step S2;
s4, glue preparation operation: and (3) mixing the coupling agent with the mixture subjected to the dehydration treatment in the step (S3) according to parts by weight to obtain the oil-resistant silicone sealant.
By adopting the technical scheme, when the light calcium carbonate, the attapulgite and the binder are mixed according to parts by weight, so that the attapulgite is attached to part of the surface of the light calcium carbonate to obtain the premix; and then mixing the organic silicon resin, the white carbon black and the titanium pigment according to the parts by weight, and then mixing the premix according to the parts by weight, so that the aim of introducing the attapulgite between the organic silicon resin and the light calcium carbonate is fulfilled, and a series of chemical reactions caused by excessive exposure of the light calcium carbonate mixed in the oil-resistant silicone sealant in the environment can be effectively avoided when the oil-resistant silicone sealant is used, so that bubbles are prevented from being generated in the curing process of the oil-resistant silicone sealant.
Optionally, the step S2, the grinding process includes: grinding the mixed material for 1-2 h; cooling until the temperature of the mixed materials is 25-35 ℃.
Through adopting above-mentioned technical scheme, can lead to the temperature of compounding to rise at the in-process of grinding treatment, adopt the refrigerated mode to cool off the compounding.
Optionally, the operations of the step S3 and the dehydration process are as follows: and (3) heating the mixed material subjected to the grinding treatment in the step (S2) to 80-100 ℃, heating and dehydrating under vacuum condition, and cooling.
By adopting the technical scheme, the dehydration process comprises two stages: the first stage is to raise the temperature to 80-100 deg.c for eliminating water in the material, mainly light calcium carbonate; the second stage is to carry out temperature rising dehydration under vacuum condition, which is used for removing residual moisture in raw materials and removing monomers of the organic silicon resin in a free state, and the dehydration effect is optimal by adopting the mode.
Optionally, in the step S3, in the dehydration treatment, the conditions for heating and dehydrating under the vacuum condition are as follows: the temperature rising and dehydration time is 5-8 h, the temperature rising and dehydration temperature is 100-130 ℃, and the vacuum degree is 0.05-0.10 MPa.
By adopting the technical scheme, the temperature rising and dehydration are carried out under the vacuum condition and then the cooling is carried out, so that part of water and part of monomers of the organic silicon resin in a free state are pumped out in vacuum, and the other part of water and the other part of monomers of the organic silicon resin in the free state can be cooled and then discharged.
In a third aspect, the application provides application of the oil-resistant silicone sealant in the fields of building sealing, electrical appliance sealing, electronic sealing and automobile part sealing.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the oil-resistant silicone sealant provided by the application introduces light calcium carbonate, white carbon black and titanium pigment into the organic silicon resin on the basis of the existing formula, so that the oil-resistant silicone sealant is enhanced, the tensile strength and hardness of the oil-resistant silicone sealant can be effectively improved, and meanwhile, the oil resistance of the oil-resistant silicone sealant can be improved.
2. The oil-resistant silicone sealant provided by the application introduces attapulgite between the organic silicon resin and the light calcium carbonate on the basis of the existing formula, utilizes the characteristic of the attapulgite, adopts a mode of introducing the organic silicon resin after the attapulgite is attached to the surface of the light calcium carbonate part, can effectively improve the leveling property, the temperature resistance and the ageing resistance of the oil-resistant silicone sealant, and can avoid a series of chemical reactions caused by excessive exposure of the light calcium carbonate in the environment, so that bubbles are prevented from being generated in the curing process of the oil-resistant silicone sealant.
3. In the preparation method of the oil-resistant silicone sealant, when a mixed material is prepared, firstly, light calcium carbonate, attapulgite and a binder are mixed according to parts by weight, so that the attapulgite is attached to part of the surface of the light calcium carbonate to obtain a premix; and then mixing the organic silicon resin, the white carbon black and the titanium pigment according to the parts by weight, and then mixing the premix according to the parts by weight, so that the aim of introducing the attapulgite between the organic silicon resin and the light calcium carbonate is fulfilled, and a series of chemical reactions caused by excessive exposure of the light calcium carbonate mixed in the oil-resistant silicone sealant in the environment can be effectively avoided when the oil-resistant silicone sealant is used, so that bubbles are prevented from being generated in the curing process of the oil-resistant silicone sealant.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of the oil-resistant silicone sealant provided in embodiment 1 of the present application.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples.
The application designs an oil-resistant silicone sealant which comprises the following components in parts by weight: 60-90 parts of organic silicon resin, 120-150 parts of light calcium carbonate, 1-5 parts of white carbon black, 5-10 parts of titanium dioxide, 8-15 parts of attapulgite, 1-3 parts of binder and 10-20 parts of coupling agent.
The applicant found that when the formulation of the oil-resistant silicone sealant is improved, if only light calcium carbonate is used to enhance the tensile strength and hardness of the oil-resistant silicone sealant, the oil-resistant performance is poor, and bubbles are easily generated when the oil-resistant silicone sealant is cured. Therefore, the attapulgite is introduced between the organic silicon resin and the light calcium carbonate, the characteristic of the attapulgite is utilized, and the mode that the attapulgite is attached to the surface of the light calcium carbonate part and then the organic silicon resin is introduced is adopted, so that the leveling property, the temperature resistance and the ageing resistance of the oil-resistant silicone sealant can be effectively improved, and meanwhile, a series of chemical reactions caused by excessive exposure of the light calcium carbonate to the environment can be avoided, so that bubbles are prevented from being generated when the oil-resistant silicone sealant is cured.
In the above technical scheme, optionally, the particle size of the light calcium carbonate is 50-80 nm.
The applicant finds that the light calcium carbonate can effectively enhance the performance of the oil-resistant silicone sealant when improving the formula of the oil-resistant silicone sealant. In addition, the applicant finds that the particle size of the light calcium carbonate can influence the reinforcing effect on the oil-resistant silicone sealant when the particle size of the light calcium carbonate is selected, and the smaller the particle size is, the more obvious the reinforcing effect is; however, when the particle size of the light calcium carbonate is smaller than a certain level, the introduced attapulgite is easily excessively attached to the surface of the light calcium carbonate, so that the reinforcing effect on the oil-resistant silicone sealant is reduced, and therefore, the particle size of the light calcium carbonate needs to be effectively selected and controlled.
The oil-resistant silicone sealant is prepared by the following method and comprises the following steps:
s1, preparing a mixed material: mixing light calcium carbonate, attapulgite and a binder according to parts by weight to obtain a premix; mixing organic silicon resin, white carbon black and titanium pigment according to parts by weight, and adding premix according to parts by weight to obtain a mixed material;
s2, grinding treatment: grinding the mixed materials, and cooling after grinding;
s3, dehydration: carrying out dehydration treatment on the mixed material subjected to the grinding treatment in the step S2;
s4, glue preparation operation: and (3) mixing the coupling agent with the mixture subjected to the dehydration treatment in the step (S3) according to parts by weight to obtain the oil-resistant silicone sealant.
The applicant finds that when the preparation method of the oil-resistant silicone sealant is improved, a mode of directly introducing light calcium carbonate into the organic silicon resin is not adopted when the oil-resistant silicone sealant is prepared, but a mode of attaching attapulgite to part of the surface of the light calcium carbonate and then introducing the light calcium carbonate into the organic silicon resin is adopted, so that a series of chemical reactions caused by excessive exposure of the mixed light calcium carbonate in the oil-resistant silicone sealant can be effectively avoided, and bubbles generated in the curing process of the oil-resistant silicone sealant can be prevented.
In the above technical solution, optionally, the operations of step S3 and the dehydration process are: and (3) heating the mixed material subjected to the grinding treatment in the step (S2) to 80-100 ℃, heating and dehydrating under vacuum condition, and cooling.
The applicant found that when the preparation method of the oil-resistant silicone sealant is improved, if only a direct heating mode or only a mode of heating and dehydrating under vacuum condition is adopted, the dehydrating effect is poor. In this application, the applicant has found that dividing the dehydration stage into two stages, namely a first stage of elevated temperature, is used to remove the moisture from the feedstock; the second stage is heating dehydration under vacuum condition, which is used for removing residual moisture in raw materials and removing monomers of the organic silicon resin in a free state, and can effectively remove moisture in raw materials and monomers of the organic silicon resin in a free state.
The oil-resistant silicone sealant can be applied to the fields of building sealing, electric appliance sealing, electronic sealing and automobile part sealing.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following are examples 1-10 and comparative examples 1-5 of the present application, examples 1-10 and comparative examples 1-5 respectively providing an oil resistant silicone sealant; wherein, the raw materials selected in examples 1 to 10 and comparative examples 1 to 5 are all commercial products unless otherwise specified, and are specifically as follows:
silicone resin: the manufacturer is Nanjing Baimuda biotechnology limited company;
light calcium carbonate: the manufacturer is Shanghai Yuan Ye biotechnology Co., ltd, and the model is S24297;
white carbon black: the manufacturer is Hubei guangdong biotechnology limited company, and the model is GA2689;
titanium white powder: the manufacturer is Shandong Jin Yueyuan new material Co., ltd, and the model is 80204;
attapulgite: the manufacturer is Nanjing Baimuda biotechnology limited company;
and (2) a binder: is selected from aluminosilicate, and the manufacturer is Jiangxi Xin Tao technology Co., ltd;
coupling agent: is selected from silane coupling agent, and the manufacturer is Hubei Xinkang pharmaceutical chemical industry Co., ltd, and the model is KH-550.
Example 1
The embodiment provides an oil-resistant silicone sealant, and a flow chart of a preparation method of the oil-resistant silicone sealant is shown in fig. 1, and the method comprises the following steps:
s1, preparing a mixed material: mixing 24kg of light calcium carbonate, 1.6kg of attapulgite and 0.26kg of aluminosilicate to obtain a premix; 15kg of organic silicon resin, 0.46kg of white carbon black and 1.52kg of titanium dioxide are mixed, and 25.86kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 65nm;
s2, grinding treatment: grinding the mixed materials for 1.5 hours; cooling until the temperature of the mixed materials is 30 ℃;
s3, dehydration: heating the mixed material subjected to the grinding treatment in the step S2 to 90 ℃, heating and dehydrating under vacuum condition, and cooling; wherein, the conditions for heating and dehydrating under the vacuum condition are as follows: the time of heating and dehydration is 6 hours, the temperature of heating and dehydration is 120 ℃, and the vacuum degree is 0.08Mpa;
s4, glue preparation operation: and (3) mixing 2.32kg of silane coupling agent into the mixture subjected to the dehydration treatment in the step (S3) to obtain the oil-resistant silicone sealant.
Example 2
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: mixing 25kg of light calcium carbonate, 2.4kg of attapulgite and 0.36kg of aluminosilicate to obtain a premix; 13kg of organic silicon resin, 0.2kg of white carbon black and 1.2kg of titanium dioxide are mixed, and 27.76kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 50nm;
s4, glue preparation operation: mixing 2kg of silane coupling agent into the mixture subjected to the dehydration treatment in the step S3 to obtain oil-resistant silicone sealant;
other steps, parameters and conditions were the same as in example 1.
Example 3
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: 26kg of light calcium carbonate, 2kg of attapulgite and 0.54kg of aluminosilicate are mixed to obtain a premix; 12kg of organic silicon resin, 0.86kg of white carbon black and 1.68kg of titanium dioxide are mixed, and 28.54kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 55nm;
s4, glue preparation operation: mixing 2.64kg of silane coupling agent into the mixture subjected to the dehydration treatment in the step S3 to obtain oil-resistant silicone sealant;
other steps, parameters and conditions were the same as in example 1.
Example 4
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: 27kg of light calcium carbonate, 2.6kg of attapulgite and 0.2kg of aluminosilicate are mixed to obtain premix; 18kg of organic silicon resin, 0.34kg of white carbon black and 1.4kg of titanium dioxide are mixed, and 29.8kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 60nm;
s4, glue preparation operation: 3.28kg of silane coupling agent is mixed into the mixture subjected to the dehydration treatment in the step S3, so that the oil-resistant silicone sealant is obtained;
other steps, parameters and conditions were the same as in example 1.
Example 5
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: 28kg of light calcium carbonate, 2.2kg of attapulgite and 0.6kg of aluminosilicate are mixed to obtain premix; mixing 14kg of organic silicon resin, 0.72kg of white carbon black and 1kg of titanium dioxide, and adding 30.8kg of premix into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 70nm;
s4, glue preparation operation: mixing 2.96kg of silane coupling agent into the mixture subjected to the dehydration treatment in the step S3 to obtain oil-resistant silicone sealant;
other steps, parameters and conditions were the same as in example 1.
Example 6
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: 29kg of light calcium carbonate, 2.8kg of attapulgite and 0.42kg of aluminosilicate are mixed to obtain premix; 17kg of organic silicon resin, 1kg of white carbon black and 1.84kg of titanium dioxide are mixed, and 32.22kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 75nm;
s4, glue preparation operation: 3.6kg of silane coupling agent is mixed into the mixture subjected to the dehydration treatment in the step S3, so that the oil-resistant silicone sealant is obtained;
other steps, parameters and conditions were the same as in example 1.
Example 7
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: 30kg of light calcium carbonate, 3kg of attapulgite and 0.48kg of aluminosilicate are mixed to obtain a premix; 16kg of organic silicon resin, 0.58kg of white carbon black and 2kg of titanium dioxide are mixed, and 33.48kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 80nm;
s4, glue preparation operation: mixing 4kg of silane coupling agent into the mixture subjected to the dehydration treatment in the step S3 to obtain oil-resistant silicone sealant;
other steps, parameters and conditions were the same as in example 1.
Example 8
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s2, grinding treatment: grinding the mixed materials for 1h; cooling until the temperature of the mixed materials is 25 ℃;
s3, dehydration: heating the mixed material subjected to the grinding treatment in the step S2 to 80 ℃, heating and dehydrating under vacuum condition, and cooling; wherein, the conditions for heating and dehydrating under the vacuum condition are as follows: the temperature rise and dehydration time is 5 hours, the temperature of the temperature rise and dehydration is 100 ℃, and the vacuum degree is 0.05Mpa;
other steps, parameters and conditions were the same as in example 1.
Example 9
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s2, grinding treatment: grinding the mixed materials for 2 hours; cooling until the temperature of the mixed materials is 35 ℃;
s3, dehydration: heating the mixed material subjected to the grinding treatment in the step S2 to 100 ℃, heating and dehydrating under vacuum condition, and cooling; wherein, the conditions for heating and dehydrating under the vacuum condition are as follows: the temperature rise and dehydration time is 8 hours, the temperature of the temperature rise and dehydration is 130 ℃, and the vacuum degree is 0.10Mpa;
other steps, parameters and conditions were the same as in example 1.
Comparative example 1
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: mixing 24kg of light calcium carbonate and 0.26kg of aluminosilicate to obtain a premix; 15kg of organic silicon resin, 0.46kg of white carbon black and 1.52kg of titanium dioxide are mixed, and 24.26kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 65nm;
other steps, parameters and conditions were the same as in example 1.
Comparative example 2
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: 15kg of organic silicon resin, 24kg of light calcium carbonate, 1.6kg of attapulgite, 0.26kg of aluminosilicate, 0.46kg of white carbon black and 1.52kg of titanium dioxide are mixed to obtain a mixed material; wherein the particle size of the light calcium carbonate is 65nm;
other steps, parameters and conditions were the same as in example 1.
Comparative example 3
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: mixing 24kg of light calcium carbonate, 6kg of attapulgite and 0.26kg of aluminosilicate to obtain a premix; 15kg of organic silicon resin, 0.46kg of white carbon black and 1.52kg of titanium dioxide are mixed, and 30.26kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 65nm;
other steps, parameters and conditions were the same as in example 1.
Comparative example 4
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: mixing 24kg of light calcium carbonate, 1.6kg of attapulgite and 0.26kg of aluminosilicate to obtain a premix; 15kg of organic silicon resin, 0.46kg of white carbon black and 1.52kg of titanium dioxide are mixed, and 25.86kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 45nm;
other steps, parameters and conditions were the same as in example 1.
Comparative example 5
Based on embodiment 1, this embodiment differs from embodiment 1 in that:
s1, preparing a mixed material: mixing 24kg of light calcium carbonate, 1.6kg of attapulgite and 0.26kg of aluminosilicate to obtain a premix; 15kg of organic silicon resin, 0.46kg of white carbon black and 1.52kg of titanium dioxide are mixed, and 25.86kg of premix is added into the mixture to obtain a mixed material; wherein the particle size of the light calcium carbonate is 85nm;
other steps, parameters and conditions were the same as in example 1.
Experimental detection
The oil-resistant silicone sealants provided in examples 1 to 9 and comparative examples 1 to 5 were tested for cure time, and were specifically as follows:
1. and (3) detecting a curing process: detecting the curing degree of the oil-resistant silicone sealant, and simultaneously observing whether bubbles are generated in the curing process of the oil-resistant silicone sealant and whether a bulge phenomenon occurs after the curing is finished; the detection results and the observation results are recorded in table 1.
TABLE 1 summary of curing process test results
Referring to table 1, the oil-resistant silicone sealants provided in examples 1 to 9 of the present application reached surface drying at 0.25h, and completely cured from the start of curing at 0.5h to 12h, and substantially no air bubbles were generated during the curing process of the oil-resistant silicone sealant, and no bulging phenomenon was generated after the curing was completed. Therefore, compared with the oil-resistant silicone sealants provided in comparative examples 1 to 5, the oil-resistant silicone sealants provided in examples 1 to 9 of the present application have higher superiority in the curing process, and the mechanism thereof is that: the oil-resistant silicone sealants provided in examples 1 to 9 are prepared by adopting a mode that attapulgite is attached to part of the surface of light calcium carbonate and then introduced into organic silicon resin, so that the characteristic of the attapulgite is introduced while the reinforcing effect of the light calcium carbonate on the oil-resistant silicone sealant is ensured, the leveling property of the oil-resistant silicone sealant is good, the curing time is short, and meanwhile, bubbles generated in the curing process of the oil-resistant silicone sealant and the phenomenon of bulging after the curing of the oil-resistant silicone sealant is completed can be avoided.
The oil-resistant silicone sealants provided in examples 1 to 9 and the oil-resistant silicone sealants provided in comparative examples 1 to 5 were tested for their related properties, specifically as follows:
2. oil resistance: referring to GB/T1690-2010, the oil-resistant silicone sealant is respectively soaked in gasoline and lubricating oil at room temperature, and is taken out after 7 days, and the volume change rate of the oil-resistant silicone sealant is detected; recording the detection results in table 2;
3. sealing performance: taking 14 standard barrels corresponding to examples 1-9 and comparative examples 1-5 respectively, drilling holes with the same size and specification at the same position of the standard barrels by using a puncher, repairing and sealing the holes by using the oil-resistant silicone sealant, and observing whether the repaired and sealed standard barrels have water leakage; the observation results are recorded in table 2;
4. temperature resistance: carrying out a high-temperature oxidation experiment on the oil-resistant silicone sealant, and observing whether the oil-resistant silicone sealant can generate cracking phenomenon or not; the observation results are recorded in table 2;
5. ageing resistance: performing an accelerated aging test on the oil-resistant silicone sealant, and observing whether the oil-resistant silicone sealant can generate cracking phenomenon or not; the observation results are recorded in table 2;
6. tensile properties: detecting the tensile strength (MPa) of the oil-resistant silicone sealant according to GB/T13477.8-2002; recording the detection results in table 2;
7. hardness: detecting the hardness (Shore A) of the oil-resistant silicone sealant after complete curing by a Shore durometer; the detection results are recorded in table 2.
TABLE 2 summary of correlation Performance test results
Referring to table 2, the volume change rate of the oil-resistant silicone sealants provided in examples 1 to 9 of the present application in a gasoline environment is not higher than 6.7%, and the volume change rate in a lubricating oil environment is not higher than 8.6%; the oil-resistant silicone sealant provided in embodiments 1 to 9 of the present application does not have a water leakage phenomenon after curing, and does not have a cracking phenomenon after high-temperature oxidation experiments and accelerated aging experiments; the oil-resistant silicone sealants provided in examples 1-9 herein all had tensile strengths higher than 1.79MPa and hardness above 50Shore a. Therefore, compared with the oil-resistant silicone sealants provided in comparative examples 1 to 5, the oil-resistant silicone sealants provided in examples 1 to 9 have higher superiority in oil resistance, sealing performance, temperature resistance, ageing resistance, tensile resistance and hardness, and the mechanism is that: the oil-resistant silicone sealants provided in examples 1 to 9 were prepared by attaching attapulgite to a part of the surface of light calcium carbonate and then introducing the attapulgite into silicone resin; meanwhile, in the preparation process, the particle size of the light calcium carbonate and the proportion between the light calcium carbonate and the attapulgite are relatively limited, so that the characteristic of the attapulgite is introduced while the reinforcing effect of the light calcium carbonate on the oil-resistant silicone sealant is ensured, and the oil-resistant silicone sealant has excellent oil resistance, sealing performance, temperature resistance, ageing resistance, tensile resistance and higher hardness.
In conclusion, the oil-resistant silicone sealant provided by the application has higher superiority.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (9)
1. The oil-resistant silicone sealant is characterized by comprising the following components in parts by weight: 60-90 parts of organic silicon resin, 120-150 parts of light calcium carbonate, 1-5 parts of white carbon black, 5-10 parts of titanium dioxide, 8-15 parts of attapulgite, 1-3 parts of a binder and 10-20 parts of a coupling agent.
2. The oil-resistant silicone sealant according to claim 1, wherein the particle size of the light calcium carbonate is 50-80 nm.
3. The oil-resistant silicone sealant according to claim 1, wherein the mass ratio between the light calcium carbonate and the attapulgite is 10-15: 1.
4. the oil resistant silicone sealant according to claim 1, wherein the binder is aluminosilicate and the coupling agent is a silane coupling agent.
5. The method for preparing the oil-resistant silicone sealant according to claim 1, which is characterized by comprising the following steps:
s1, preparing a mixed material: mixing light calcium carbonate, attapulgite and a binder according to parts by weight to obtain a premix; mixing organic silicon resin, white carbon black and titanium pigment according to parts by weight, and adding premix according to parts by weight to obtain a mixed material;
s2, grinding treatment: grinding the mixed materials, and cooling after grinding;
s3, dehydration: carrying out dehydration treatment on the mixed material subjected to the grinding treatment in the step S2;
s4, glue preparation operation: and (3) mixing the coupling agent with the mixture subjected to the dehydration treatment in the step (S3) according to parts by weight to obtain the oil-resistant silicone sealant.
6. The method for preparing an oil-resistant silicone sealant according to claim 5, wherein the step S2 of grinding is performed by: grinding the mixed materials for 1-2 hours; and cooling until the temperature of the mixed materials is 25-35 ℃.
7. The method for preparing an oil-resistant silicone sealant according to claim 5, wherein the operations of step S3 and the dehydration treatment are as follows: and (3) heating the mixed material subjected to the grinding treatment in the step (S2) to 80-100 ℃, heating, dehydrating and cooling under vacuum conditions.
8. The method for preparing an oil-resistant silicone sealant according to claim 7, wherein in the step S3, the dehydration treatment is performed under vacuum conditions under which the temperature is raised: the temperature rising and dehydration time is 5-8 h, the temperature rising and dehydration temperature is 100-130 ℃, and the vacuum degree is 0.05-0.10 MPa.
9. An application of the oil-resistant silicone sealant according to claim 1 in the fields of building sealing, electrical sealing, electronic sealing and automobile part sealing.
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| CN104610903A (en) * | 2015-01-23 | 2015-05-13 | 朱小英 | Moisture-proof seal gum for electronic device |
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