CN107513366A - A kind of oil resistant fluid sealant and preparation method thereof - Google Patents

A kind of oil resistant fluid sealant and preparation method thereof Download PDF

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Publication number
CN107513366A
CN107513366A CN201710810107.6A CN201710810107A CN107513366A CN 107513366 A CN107513366 A CN 107513366A CN 201710810107 A CN201710810107 A CN 201710810107A CN 107513366 A CN107513366 A CN 107513366A
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China
Prior art keywords
parts
fluid sealant
oil
oil resistant
rtv
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CN201710810107.6A
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Inventor
郭澄
宋顺刚
阚新宇
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JIANGSU TIANCHEN NEW MATERIALS Co Ltd
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JIANGSU TIANCHEN NEW MATERIALS Co Ltd
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Priority to CN201710810107.6A priority Critical patent/CN107513366A/en
Publication of CN107513366A publication Critical patent/CN107513366A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • C09J183/06Polysiloxanes containing silicon bound to oxygen-containing groups
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/14Gas barrier composition

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention discloses a kind of single-component room temperature vulcanized organosilicon sealant technology, specifically a kind of dealcoholized type oil resistant fluid sealant and preparation method thereof.Its recipe ingredient is measured by following parts by weight:50 100 parts of the dimethyl silicone polymer of terminal methyl group dimethoxy silica, 50 100 parts of calcium carbonate, 5 15 parts of gas-phase silica, 5 10 parts of silicone oil plasticizer, 5 15 parts of crosslinking agent, 0.5 7.5 parts of coupling agent, 0.1 5 parts of catalyst.The advantage of the invention is that:Due to selecting rational component formula, not only so that obtained fluid sealant smell is very low, to metal protection very little, and on the basis of fluid sealant properties are not changed, make its oil resistivity very high, in addition, its methodological science is reasonable, so that preparation process is simple, manufactured product cementability is strong, and storage period is stable.

Description

A kind of oil resistant fluid sealant and preparation method thereof
Technical field
The present invention relates to a kind of single-component room temperature vulcanized organosilicon sealant technology, specifically a kind of dealcoholized type oil resistant Fluid sealant and preparation method thereof.
Background technology
Fluid sealant has excellent anti-weathering aging, UV stable, high-low temperature resistant, in harsh climate environment The features such as elasticity can be kept, do not tear and be not cracked, it is widely used in every field, it is especially close in automotive field, fuel tank etc. Envelope requires that oil resistivity is high, and traditional silicon rubber is made that very big improvement in oil resistivity, but smell is big, and cementability is not Enough, the reason such as be corrosive to metal limits application of the silicon rubber in fields such as automobiles, therefore, is improving silicon rubber oil resistivity On the basis of, improve some of the above shortcoming tool and be of great significance.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of smell is low, cementability is strong, small to metal protection and can Ensure oil resistant fluid sealant of fluid sealant properties and preparation method thereof.
In order to solve the above-mentioned technical problem, oil resistant fluid sealant of the invention, it is characterised in that:Its recipe ingredient is by following heavy Measure number metering:Dimethyl silicone polymer 50-100 parts of terminal methyl group dimethoxy silica, calcium carbonate 50-100 parts, gas phase are white Carbon black 5-15 parts, silicone oil plasticizer 5-10 parts, crosslinking agent 5-15 parts, coupling agent 0.5-7.5 parts, catalyst 0.1-5 parts.
The dimethyl silicone polymer of the terminal methyl group dimethoxy silica, structural formula (viscosity is 0.5-200Pas at n=750-2000,25 DEG C).
The calcium carbonate is the precipitated calcium carbonate crossed through fatty acid treatment.
The gas-phase silica that the gas-phase silica is handled for surface through HMDS, specific surface area 100- 300m2/g。
The silicone oil plasticizer is the dimethyl silicone polymer of terminal methyl group, and viscosity is 0.5-20Pas at 25 DEG C.
The crosslinking agent is in MTMS, vinyltrimethoxy silane or phenyltrimethoxysila,e It is at least one.
The coupling agent is gamma-aminopropyl-triethoxy-silane, β-aminoethyl-γ-aminopropyltrimethoxysilane, double At least one of (γ-trimethoxysilylpropyl) amine, glycidol ether propyl trimethoxy silicane.
The catalyst is the tert-butyl ester compound of metatitanic acid four.
A kind of preparation method of above-mentioned oil resistant fluid sealant, comprises the following steps:
A) by dimethyl silicone polymer 50-100 parts, calcium carbonate 50-100 parts, gas phase of terminal methyl group dimethoxy silica White carbon 5-15 parts, dimethyl silicone polymer 5-10 parts, which are added to be stirred under vacuum in kneader, is made rubber master batch;
B) crosslinking agent 5-15 parts, coupling agent 0.5-7.5 parts, catalyst 0.1-5 parts are added in rubber master batch again, in planet stirring It is stirred under vacuum in machine, vacuum 0.06-0.09MPa, 50 revs/min of mixing speed, stirs 2.5-3h, it is close that RTV-1 oil resistants are made Sealing.
The advantage of the invention is that:Due to selecting rational component formula, not only cause obtained fluid sealant smell very It is low, to metal protection very little, and on the basis of fluid sealant properties are not changed, make its oil resistivity very high, in addition, Its methodological science is reasonable so that preparation process is simple, and manufactured product cementability is strong, and storage period is stable.
Embodiment
Oil resistant fluid sealant of the present invention and preparation method thereof is further elaborated with reference to embodiment.
Embodiment one:
The oil resistant fluid sealant of the present embodiment, is prepared using formula as below and preparation method thereof, by terminal methyl group diformazan 5 parts of 5 parts of 50 parts of 50 parts of dimethyl silicone polymer, calcium carbonate, gas-phase silica, the dimethyl silicone polymer of epoxide silica is being mediated It is stirred under vacuum in machine and rubber master batch is made, then by 5 parts of MTMS, 0.5 part of gamma-aminopropyl-triethoxy-silane, metatitanic acid Four 0.1 part of tert-butyl ester compounds are added in rubber master batch, are stirred in planetary mixer, vacuum 0.06-0.09MPa, stirring speed 50 revs/min of degree, 2.5-3h is stirred, RTV-1 oil resistant fluid sealants are made.Properties of product test result sees attached list 1.Oil resistant test knot Fruit is shown in Table 2.
Embodiment two:
The oil resistant fluid sealant of the present embodiment, is prepared using formula as below and preparation method thereof, by terminal methyl group diformazan 5 parts of 10 parts of 70 parts of 70 parts of dimethyl silicone polymer, calcium carbonate, gas-phase silica, the dimethyl silicone polymer of epoxide silica is being pinched It is stirred under vacuum in conjunction machine and rubber master batch is made, then by 5 parts of MTMS, 2 parts of gamma-aminopropyl-triethoxy-silane, metatitanic acid Four 0.5 part of tert-butyl ester compounds are added in rubber master batch, are stirred in planetary mixer, vacuum 0.06-0.09MPa, stirring speed 50 revs/min of degree, 2.5-3h is stirred, RTV-1 oil resistant fluid sealants are made.Properties of product test result sees attached list 1.Oil resistant test knot Fruit is shown in Table 2.
Embodiment three:
The oil resistant fluid sealant of the present embodiment, is prepared using formula as below and preparation method thereof, by terminal methyl group diformazan 10 parts of 10 parts of 85 parts of 85 parts of dimethyl silicone polymer, calcium carbonate, gas-phase silica, the dimethyl silicone polymer of epoxide silica is being pinched It is stirred under vacuum in conjunction machine and rubber master batch is made, then by 5 parts of MTMS, 5 parts of gamma-aminopropyl-triethoxy-silane, metatitanic acid Four 3 parts of tert-butyl ester compounds are added in rubber master batch, are stirred in planetary mixer, vacuum 0.06-0.09MPa, mixing speed 50 revs/min, 2.5-3h is stirred, RTV-1 oil resistant fluid sealants are made.Properties of product test result sees attached list 1.Oil resistant test result It is shown in Table 2.
Example IV:
The oil resistant fluid sealant of the present embodiment, is prepared using formula as below and preparation method thereof, by terminal methyl group diformazan 10 parts of 15 parts of 100 parts of 100 parts of dimethyl silicone polymer, calcium carbonate, gas-phase silica, the dimethyl silicone polymer of epoxide silica exist In kneader be stirred under vacuum be made rubber master batch, then by 15 parts of MTMS, 7.5 parts of gamma-aminopropyl-triethoxy-silane, 5 parts of four tert-butyl ester compound of metatitanic acid is added in rubber master batch, is stirred in planetary mixer, vacuum 0.06-0.09MPa, stirring 50 revs/min of speed, 2.5-3h is stirred, RTV-1 oil resistant fluid sealants are made.Properties of product test result sees attached list 1.Oil resistant is tested It the results are shown in Table 2.
The test result of table 1
Test event Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Surface drying time (min) 8 7 6 4
Tensile strength (MPa) 2.14 2.21 2.31 2.44
Elongation at break (%) 540 530 555 565
Hardness (Shore A) 27 29 24 31
Shear strength (MPa) 2.45 2.47 2.39 2.51
The test result of table 2

Claims (9)

  1. A kind of 1. oil resistant fluid sealant, it is characterised in that:Its recipe ingredient is measured by following parts by weight:Terminal methyl group dimethoxy Dimethyl silicone polymer 50-100 parts of silica, calcium carbonate 50-100 parts, gas-phase silica 5-15 parts, silicone oil plasticizer 5-10 Part, crosslinking agent 5-15 parts, coupling agent 0.5-7.5 parts, catalyst 0.1-5 parts.
  2. 2. oil resistant fluid sealant according to claim 1, it is characterised in that:Poly- the two of the terminal methyl group dimethoxy silica Methylsiloxane, structural formula(viscosity is 0.5- at n=750-2000,25 DEG C 200Pa·s)。
  3. 3. oil resistant fluid sealant according to claim 1, it is characterised in that:The calcium carbonate is light to be crossed through fatty acid treatment Matter calcium carbonate.
  4. 4. RTV-1 oil resistants fluid sealant according to claim 1, it is characterised in that:The gas-phase silica is surface six The gas-phase silica of methyl disilazane processing, specific surface area 100-300m2/g。
  5. 5. RTV-1 oil resistants fluid sealant according to claim 1, it is characterised in that:The silicone oil plasticizer is terminal methyl group Dimethyl silicone polymer, viscosity is 0.5-20Pas at 25 DEG C.
  6. 6. RTV-1 oil resistants fluid sealant according to claim 1, it is characterised in that:The crosslinking agent is methyl trimethoxy epoxide At least one of silane, vinyltrimethoxy silane or phenyltrimethoxysila,e.
  7. 7. RTV-1 oil resistants fluid sealant according to claim 1, it is characterised in that:The coupling agent is the second of γ-aminopropyl three TMOS, β-aminoethyl-γ-aminopropyltrimethoxysilane, double (γ-trimethoxysilylpropyl) amine, glycidol At least one of ether propyl trimethoxy silicane.
  8. 8. RTV-1 oil resistants fluid sealant according to claim 1, it is characterised in that:The catalyst is the tert-butyl ester of metatitanic acid four Compound.
  9. 9. a kind of preparation method of the oil resistant fluid sealant as described in one of claim 1-8, it is characterised in that comprise the following steps:
    A) by dimethyl silicone polymer 50-100 parts, calcium carbonate 50-100 parts, gas phase hard charcoal of terminal methyl group dimethoxy silica Black 5-15 parts, dimethyl silicone polymer 5-10 parts, which are added to be stirred under vacuum in kneader, is made rubber master batch;
    B) crosslinking agent 5-15 parts, coupling agent 0.5-7.5 parts, catalyst 0.1-5 parts are added in rubber master batch again, in planetary mixer It is stirred under vacuum, vacuum 0.06-0.09MPa, 50 revs/min of mixing speed, stirs 2.5-3h, RTV-1 oil resistant fluid sealants are made.
CN201710810107.6A 2017-09-11 2017-09-11 A kind of oil resistant fluid sealant and preparation method thereof Pending CN107513366A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109161204A (en) * 2018-08-20 2019-01-08 镇江创达新材料科技有限公司 A kind of preparation method of oil resistant dealcoholized type one-component RTV silicon rubber
CN112210340A (en) * 2020-11-06 2021-01-12 福建省昌德胶业科技有限公司 Oil-resistant organosilicon sealant and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101012364A (en) * 2007-01-29 2007-08-08 成都硅宝科技实业有限责任公司 Single-component room-temperature fast sulfidization dealcoholization type sealing rubber with silicone structure and preparing method thereof
CN103436217A (en) * 2013-09-06 2013-12-11 江苏天辰硅材料有限公司 Single-component dealcoholized oil-resistant silicone sealant and preparation method thereof
CN103602306A (en) * 2013-09-06 2014-02-26 江苏天辰硅材料有限公司 Single-component room-temperature sulfuration transparent dealcoholization-type mildew-resistant silicone sealant and preparation method thereof
CN107189753A (en) * 2017-07-12 2017-09-22 山东大学 A kind of de-oxime type oil resistant fluorine silicone sealant and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101012364A (en) * 2007-01-29 2007-08-08 成都硅宝科技实业有限责任公司 Single-component room-temperature fast sulfidization dealcoholization type sealing rubber with silicone structure and preparing method thereof
CN103436217A (en) * 2013-09-06 2013-12-11 江苏天辰硅材料有限公司 Single-component dealcoholized oil-resistant silicone sealant and preparation method thereof
CN103602306A (en) * 2013-09-06 2014-02-26 江苏天辰硅材料有限公司 Single-component room-temperature sulfuration transparent dealcoholization-type mildew-resistant silicone sealant and preparation method thereof
CN107189753A (en) * 2017-07-12 2017-09-22 山东大学 A kind of de-oxime type oil resistant fluorine silicone sealant and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109161204A (en) * 2018-08-20 2019-01-08 镇江创达新材料科技有限公司 A kind of preparation method of oil resistant dealcoholized type one-component RTV silicon rubber
CN112210340A (en) * 2020-11-06 2021-01-12 福建省昌德胶业科技有限公司 Oil-resistant organosilicon sealant and preparation method thereof

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