CN109652007A - Impervious oily bi-component silicone sealant of one kind and preparation method thereof - Google Patents
Impervious oily bi-component silicone sealant of one kind and preparation method thereof Download PDFInfo
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- CN109652007A CN109652007A CN201811489695.9A CN201811489695A CN109652007A CN 109652007 A CN109652007 A CN 109652007A CN 201811489695 A CN201811489695 A CN 201811489695A CN 109652007 A CN109652007 A CN 109652007A
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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
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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
- 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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a kind of impervious oily bi-component silicone sealants, are made of following mass parts raw material: component A: α, alpha, omega-dihydroxy polydimethyl siloxane: 100 parts；Methyl-silicone oil: 5~15 parts；Active nano-calcium carbonate: 80~150 parts；B component: carbon black color paste: 100 parts；Crosslinking and curing agent: 60~80 parts；Silane coupling agent: 8~20 parts；Impervious oil assistant: 0.2~1 part；Organotin catalysts: 0.1~1 part.The present invention also provides the preparation methods of impervious oily bi-component silicone sealant.Bi-component silicone sealant prepared by the present invention solves the problems, such as permeability after common bi-component glue B component through a long time placement, preparation method simple possible.With quick solidifying, bonding is wide, VOC is low, good weatherability characteristic, can be used for the numerous areas such as car light adhering and sealing, solar energy backboard bonding.
Description
Technical field
The invention belongs to silicone sealant technical fields, and in particular to the impervious oily bi-component silicone sealant of one kind and its system
Preparation Method.
Background technique
Dealcoholized type room temperature vulcanized silicone rubber has many advantages, such as that smell is small, does not corrode glued substrate.But one pack system glue is solid
Change is from outward appearance to inner essence, to be fully cured and need the long period.The dealcoholized type room temperature vulcanized silicone sealant of bi-component and one pack system are de-
Alcohol type room temperature vulcanized silicone rubber compared to have many advantages, such as volume contraction it is small, can deep layer vulcanization and be widely used in building curtain wall, vehicle
The fields such as lamp sealing, industrial antisepsis, electronics, new energy.
In order to increase the workability of bi-component silicone sealant, B component is generally done by methyl-silicone oil or end hydroxyl silicone oil
Plasticizer is added a certain amount of carbon black or white carbon black, crosslinking agent, coupling agent, catalyst etc. and is uniformly mixed preparation under vacuum conditions
At consistency and extrudability suitable mixture.Since methyl-silicone oil is apolar substance, the suction of carbon black or white carbon black powder to it
Attached effect is weaker, and with the extension of B component period of storage, suction-operated gradually weakens, and methyl-silicone oil can be leaked out gradually,
Surface forms oil reservoir, influences the stability and workability of product.
Summary of the invention
In order to after overcoming existing bi-component silicone sealant B component to place for a long time the shortcomings that easy permeability, the present invention provides
Impervious oily bi-component silicone sealant of one kind and preparation method thereof.
The present invention is realized using following technology:
A kind of impervious oily bi-component silicone sealant, it is characterised in that be made of following mass parts raw material:
Component A
α, alpha, omega-dihydroxy polydimethyl siloxane: 100 parts
Methyl-silicone oil: 5~15 parts
Active nano-calcium carbonate: 80~150 parts
B component
Carbon black color paste: 100 parts
Crosslinking and curing agent: 60~80 parts
Silane coupling agent: 8~20 parts
Impervious oil assistant: 0.2~1 part
Organotin catalysts: 0.1~1 part
The present invention uses following impervious oil assistant mainly to improve the impervious oily ability of B component:
The impervious oil assistant is a kind of Lauryl Alcohol ester type compound or several Lauryl Alcohol esters such as flowering structure
Close the mixture of object.This kind of compound can form lotion with crosslinking and curing agent, be adsorbed on carbon black particle surface enhanced crosslinking curing
And the interaction with silicone oil in carbon black color paste, to achieve the purpose that impervious oil.The Lauryl Alcohol ester type compound has
Such as flowering structure:
Further scheme is:
The α, alpha, omega-dihydroxy polydimethyl siloxane viscosity are 10000mPas~200000mPas, preferably
20000mPas~80000mPas.
The α of different viscositys can be used, alpha, omega-dihydroxy polydimethyl siloxane compounds.As 20000mPas,
50000mPas or 10000mPas and 80000mPas are re-dubbed 50000mPas.
Further scheme is:
The methyl-silicone oil viscosity is 50-1000mPas.
Further scheme is:
The carbon black color paste is prepared via a method which to obtain: will be by acid system surface treatment or alkaline process surface treatment
25~40 mass parts of carbon black powder obtained afterwards, 30~50 mass parts of methyl-silicone oil and viscosity that viscosity is 100~500mPas are
The α of 700~1500mPas, 20~40 mass parts of alpha, omega-dihydroxy polydimethyl siloxane, 120 DEG C of vacuum are de- in kneader
Water is mediated 3 hours and is made.
Further scheme is:
It is preferred that oil factor is the carbon black powder of 50~60cc/100g, preferably 30~35 mass parts of carbon black loading, preferably methyl is poly-
40~45 mass parts of dimethyl siloxane dosage, preferably α, ω -- 25~30 mass parts of dialkyl polydimethylsiloxane dosage.
Further scheme is:
The crosslinking and curing agent is selected from ethyl orthosilicate, positive silicic acid propyl ester, ethyl polysilicate, poly- methyl triethoxy
One or more of silane, methyltrimethoxysilane, vinyltrimethoxysilane.
Further scheme is:
The silane coupling agent is selected from γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-shrink
Glycerin ether oxygroup trimethoxy silane, N-(β-aminoethyl)-gamma-aminopropyl-triethoxy-silane and N-(β-aminoethyl)-γ-ammonia
One or more of propyl trimethoxy silicane.
Further scheme is:
The organotin catalysts are selected from dibutyl tin dilaurate, dioctyl tin cinnamic acid tin, the new last of the ten Heavenly stems of dioctyl two
In sour tin, dibutyl tin acetate, the one or more of bis- (acetopyruvic acid) dibutyl tins.It is preferred that two neodecanoic acid of dioctyl
One of tin, bis- (acetopyruvic acid) dibutyl tins.
The present invention also provides the preparation methods of the impervious oily bi-component silicone sealant, comprising the following steps:
(1) preparation of component A
By α, ω -- 100 mass parts of dialkyl polydimethylsiloxane, 5~15 mass parts of methyl-silicone oil, active nano carbon
Component A is uniformly made in dispersion mixing to the raw material of sour 80~150 mass parts of calcium under vacuum conditions；
(2) preparation of B component
By 100 mass parts of B component carbon black color paste, crosslinking and curing agent 60-80 mass parts, impervious oil assistant (K1) 0.2-1 matter
Part is measured, is stirred 30 minutes in the condition of≤- 0.08MPa, is uniformly mixed rear shovel side, silane coupling agent 8-20 mass parts are added, have
0.1~1 mass parts of machine tin catalyst stir 30 minutes obtained B components that are uniformly dispersed in the condition of≤- 0.08MPa；
(3) A, B component mixing
A, B component is used by the mass ratio of A:B=8~15:1 after mixing at room temperature.
The silicone sealant has the substrates such as glass, anodised aluminium, PP (plasma treatment), PC, PMMA, PBT, ASA
There is good cementability.
Compared with prior art, the beneficial effects of the present invention are:
The a small amount of impervious oil assistant of addition is able to achieve B component and places for a long time in B component, and it is existing not occur layering, permeability
As having better stability and workability.Bi-component silicone sealant prepared by the present invention has most of substrates good
Good cementability.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1
By the α of 100 parts of 20000mPas, ω -- dialkyl polydimethylsiloxane, 100 parts of active nano-calcium carbonates, 10
The methyl-silicone oil of part 100mPas is blended dispersion under vacuum condition, component A is made；By 100 mass parts of B component carbon black color paste,
30 parts of ethyl orthosilicates (Si-28), 30 parts of methyltrimethoxysilane, 5 parts of vinyltrimethoxysilanes, 0.5 part of impervious oil
Auxiliary agent (K1), 10 parts of gamma-aminopropyl-triethoxy-silanes, 1 part of two neodecanoic acid tin of dioctyl, under≤- 0.8MPa vacuum condition
Dispersion is blended, component B is made；By component A: component B=10:1~12:1 be blended, respectively gluing in glass, anodised aluminium,
On PP, PP (plasma treatment), PC, PMMA, PBT, ASA, gluing thickness about 3~4mm.By B component loaded on quiet in 300mL glue bottle
It sets.
Embodiment 2
By the α of 100 parts of 50000mPas, ω -- dialkyl polydimethylsiloxane, 100 parts of active nano-calcium carbonates, 10
The methyl-silicone oil of part 100mPas is blended dispersion under vacuum condition, component A is made；By 100 mass parts of B component carbon black color paste,
30 parts of ethyl polysilicates (Si-40), 30 parts of methyltrimethoxysilane, 5 parts of vinyltrimethoxysilanes, 0.5 part of impervious oil
Auxiliary agent (K2), 12 parts of N-(β-aminoethyl)-gamma-aminopropyl-triethoxy-silanes, 1 part of two neodecanoic acid tin of dioctyl ,≤-
Dispersion is blended under 0.8MPa vacuum condition, component B is made；Component A: component B=10:1~12:1 is blended, gluing is in glass respectively
Glass, anodised aluminium, PP, PP (plasma treatment), on PC, PMMA, PBT, ASA, gluing thickness about 3~4mm.B component is filled
It is stood in 300mL glue bottle.
Embodiment 3
By the α of 100 parts of 50000mPas, ω -- dialkyl polydimethylsiloxane, 100 parts of active nano-calcium carbonates, 10
The methyl-silicone oil of part 100mPas is blended dispersion under vacuum condition, component A is made；By 100 mass parts of B component carbon black color paste,
30 parts of ethyl polysilicates (Si-40), 30 parts of methyltrimethoxysilane, 5 parts of vinyltrimethoxysilanes, 0.2 part of impervious oil
Auxiliary agent (K1), 0.2 part of impervious oil assistant (K2), 12 parts of γ-glycidol ether oxygroup trimethoxy silane, 1 part of bis- (acetylacetone,2,4-pentanedione
Acid) dibutyl tin, dispersion is blended under≤- 0.8MPa vacuum condition, component B is made；By component A: component B=10:1~12:1
It is blended, gluing is on glass, anodised aluminium, PP, PP (plasma treatment), PC, PMMA, PBT, ASA respectively, and gluing thickness is about
3~4mm.B component is loaded in 300mL glue bottle and is stood.
Comparative example 1
Compared with Example 1, in addition to not adding impervious oil assistant, remaining formula and technique and embodiment 1 it is completely the same.I.e.
By the α of 100 parts of 20000mPas, ω -- dialkyl polydimethylsiloxane, 100 parts of active nano-calcium carbonates, 10 parts
Dispersion is blended under vacuum condition, component A is made for the methyl-silicone oil of 100mPas；By 100 mass parts of B component carbon black color paste, 30
Part ethyl orthosilicate (Si-28), 30 parts of methyltrimethoxysilane, 5 parts of vinyltrimethoxysilanes, 0.5 part of impervious oil help
Agent, 10 parts of gamma-aminopropyl-triethoxy-silanes, 1 part of two neodecanoic acid tin of dioctyl are blended point under≤- 0.8MPa vacuum condition
It dissipates, component B is made；Component A: component B=10:1~12:1 is blended, gluing is in glass, anodised aluminium, PP, PP (etc. respectively
Ion processing), on PC, PMMA, PBT, ASA, gluing thickness about 3~4mm.B component is loaded in 300mL glue bottle and is stood.
Comparative example 2
Compared with Example 2, in addition to not adding impervious oil assistant, remaining formula and technique and embodiment 2 it is completely the same.I.e.
By the α of 100 parts of 50000mPas, ω -- dialkyl polydimethylsiloxane, 100 parts of active nano-calcium carbonates, 10 parts
Dispersion is blended under vacuum condition, component A is made for the methyl-silicone oil of 100mPas；By 100 mass parts of B component carbon black color paste, 30
Part ethyl polysilicate (Si-40), 30 parts of methyltrimethoxysilane, 5 parts of vinyltrimethoxysilanes, 0.5 part of impervious oil help
Agent, 12 parts of N-(β-aminoethyl)-gamma-aminopropyl-triethoxy-silanes, 1 part of two neodecanoic acid tin of dioctyl, in≤- 0.8MPa vacuum
Under the conditions of be blended dispersion, component B is made；Component A: component B=10:1~12:1 is blended, gluing is in glass, anodic oxygen respectively
Change aluminium, PP, PP (plasma treatment), on PC, PMMA, PBT, ASA, gluing thickness about 3~4mm.B component is loaded on 300mL glue
It is stood in bottle.
Comparative example 3
Compared with Example 3, in addition to not adding impervious oil assistant, remaining formula and technique and embodiment 3 it is completely the same.I.e.
By the α of 100 parts of 50000mPas, ω -- dialkyl polydimethylsiloxane, 100 parts of active nano-calcium carbonates, 10 parts
Dispersion is blended under vacuum condition, component A is made for the methyl-silicone oil of 100mPas；By 100 mass parts of B component carbon black color paste, 30
Part ethyl polysilicate (Si-40), 30 parts of methyltrimethoxysilane, 5 parts of vinyltrimethoxysilanes, 0.5 part of impervious oil help
Agent, 12 parts of γ-glycidol ether oxygroup trimethoxy silane, 1 part of bis- (acetopyruvic acid) dibutyl tin are true in≤- 0.8MPa
Dispersion is blended under empty condition, component B is made；Component A: component B=10:1~12:1 is blended, gluing is in glass, anode respectively
Aluminium oxide, PP, PP (plasma treatment), on PC, PMMA, PBT, ASA, gluing thickness about 3~4mm.B component is loaded on 300mL
It is stood in glue bottle.
Permeability test
| Sample number into spectrum | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Permeability amount1) | 0g | 0g | 0g | 5g | 8g | 12g |
1) after normality is placed 6 months, the 300mL glue bottle bottleneck for filling B component is cut, the liquid matter that can be squeezed out from bottleneck
Amount.
Cementability test
Illustrate: +++ represent bonding very well, --- representative is not glued.
As can be seen from the above table, it is added after impervious oil assistant on bonding without influence.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (10)
1. a kind of impervious oily bi-component silicone sealant, it is characterised in that be made of following mass parts raw material:
Component A
α, alpha, omega-dihydroxy polydimethyl siloxane: 100 parts
Methyl-silicone oil: 5~15 parts
Active nano-calcium carbonate: 80~150 parts
B component
Carbon black color paste: 100 parts
Crosslinking and curing agent: 60~80 parts
Silane coupling agent: 8~20 parts
Impervious oil assistant: 0.2~1 part
Organotin catalysts: 0.1~1 part.
2. impervious oily bi-component silicone sealant according to claim 1, it is characterised in that:
The impervious oil assistant is a kind of Lauryl Alcohol ester type compound or several Lauryl Alcohol ester type compounds such as flowering structure
Mixture；
3. impervious oily bi-component silicone sealant according to claim 1, it is characterised in that:
The α, alpha, omega-dihydroxy polydimethyl siloxane viscosity are 10000mPas~200000mPas.
4. impervious oily bi-component silicone sealant according to claim 3, it is characterised in that:
The α, alpha, omega-dihydroxy polydimethyl siloxane viscosity are 20000mPas~80000mPas.
5. impervious oily bi-component silicone sealant according to claim 1, it is characterised in that:
The methyl-silicone oil viscosity is 50~1000mPas.
6. impervious oily bi-component silicone sealant according to claim 1, it is characterised in that:
The carbon black color paste is prepared via a method which to obtain: will obtain after acid system is surface-treated or alkaline process is surface-treated
25~40 mass parts of carbon black powder arrived, 30~50 mass parts of methyl-silicone oil, α, 20~40 matter of alpha, omega-dihydroxy polydimethyl siloxane
Part is measured, 120 DEG C of vacuum dehydrations are mediated 3 hours and are made in kneader.
7. impervious oily bi-component silicone sealant according to claim 6, it is characterised in that:
The carbon black powder is the carbon black powder that oil factor is 50~60cc/100g.
8. impervious oil bi-component silicone sealant described according to claim 6 or 7, it is characterised in that:
30~35 mass parts of carbon black loading, 40~45 mass parts of methyl dimethyl silicone polymer dosage, α, alpha, omega-dihydroxy are poly-
25~30 mass parts of dimethyl siloxane dosage.
9. impervious oily bi-component silicone sealant according to claim 1, it is characterised in that:
The crosslinking and curing agent is selected from ethyl orthosilicate, positive silicic acid propyl ester, ethyl polysilicate, poly- methyltriethoxy silane
One or more of alkane, methyltrimethoxysilane, vinyltrimethoxysilane；
The silane coupling agent is selected from γ-aminopropyltrimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-glycidol
Ether oxygen base trimethoxy silane, N-(β-aminoethyl)-gamma-aminopropyl-triethoxy-silane and N-(β-aminoethyl)-γ-ammonia third
One or more of base trimethoxy silane；
The organotin catalysts be selected from dibutyl tin dilaurate, dioctyl tin cinnamic acid tin, two neodecanoic acid tin of dioctyl,
One or more of dibutyl tin acetate, bis- (acetopyruvic acid) dibutyl tins.
10. the preparation method of impervious oil bi-component silicone sealant, feature described in claim 1 to 9 any claim exist
In the following steps are included:
(1) preparation of component A
By α, 100 mass parts of alpha, omega-dihydroxy polydimethyl siloxane, 5~15 mass parts of methyl-silicone oil, active nano-calcium carbonate 80
Component A is uniformly made in dispersion mixing to the raw material of~150 mass parts under vacuum conditions；
(2) preparation of B component
By 100 mass parts of B component carbon black color paste, crosslinking and curing agent 60-80 mass parts, impervious oil assistant 0.2-1 mass parts,
The condition of≤- 0.08MPa stirs 30 minutes, and silane coupling agent 8-20 mass parts, organotin catalysts are added after mixing
0.1-1 mass parts stir 30 minutes obtained B components that are uniformly dispersed in the condition of≤- 0.08MPa；
(3) A, B component mixing
A, B component is used by the mass ratio of A:B=8~15:1 after mixing at room temperature.
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| CN201811489695.9A CN109652007B (en) | 2018-12-06 | 2018-12-06 | Oil-seepage-resistant bi-component silicone sealant and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114085641A (en) * | 2021-10-25 | 2022-02-25 | 广州集泰化工股份有限公司 | Silicone sealant and preparation method thereof |
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