CN106751051A - A kind of automobile preparation method of ageing-resistant fluid sealant - Google Patents
A kind of automobile preparation method of ageing-resistant fluid sealant Download PDFInfo
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- CN106751051A CN106751051A CN201611181089.1A CN201611181089A CN106751051A CN 106751051 A CN106751051 A CN 106751051A CN 201611181089 A CN201611181089 A CN 201611181089A CN 106751051 A CN106751051 A CN 106751051A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of automobile preparation method of ageing-resistant fluid sealant, comprise the following steps：Polyisobutenyl random copolymer is prepared first；Then the Nano filling that nano-titanium oxide wraps up nano silicon oxide core shell structure is obtained；Finally by obtained polyisobutenyl random copolymer, butyl rubber, ethylene propylene diene rubber are mixed to join in banbury, the 60min of banburying 30 at 160 170 DEG C；130 135 DEG C are cooled to, continue to add the Petropols of carbon 5, naphthenic oil, plasticizer, the 30min of banburying 10 toward banbury；100 115 DEG C are cooled to, continue to add Nano filling obtained above toward banbury, calcium carbonate, Di(dioctylpyrophosphato) ethylene titanate, the 70min of banburying 45；Continue to be cooled to room temperature, stirring 1 2h of mixing obtains the ageing-resistant fluid sealant of automobile.The fluid sealant mechanical property is good, and wear-resisting ageing-resistant performance is good.
Description
Technical field：
The present invention relates to field of compound material, a kind of preparation method of automobile with ageing-resistant fluid sealant is specifically related to.
Background technology：
As economic continues to develop, developing rapidly for automobile industry has higher for aspects such as automotive trims
It is required that, fluid sealant is widely used in the sealing and adhesion of automobile due to its excellent performance, gradually can not as one kind
Substituted product, there is unlimited development potentiality.
Fluid sealant also known as hydraulic seal pad, compared with sealed solid (such as steel pad, paper washer), with it is easy to use, sealing
The good advantage of property, therefore it is widely used in auto industry.But although fluid sealant sealing at present on the market is relatively good,
It is that high temperature resistant ageing-resistant performance is poor, service life is shorter.
The content of the invention：
It is an object of the invention to provide a kind of automobile preparation method of ageing-resistant fluid sealant, the preparation method is simple, easily
In operation, obtained fluid sealant stable performance, ageing-resistant performance is good, and flexility is good, and resistance to low temperature is excellent, sealing property
It is good.
To achieve the above object, the present invention uses following technical scheme：
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -60~-100 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, with styrene derived
Thing using main initiator, coinitiator ageing complexing 5-30min, is obtained initiation system as second comonomer, and add alcohols or
Alcamines is third component, and third component is added in reactor in monomer feed with polymerized monomer, by cation slurry
Combined polymerization 40-90 hours, polyisobutenyl random copolymer is obtained；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 20-
After 50min, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 60-80 DEG C, reacts 12-40h, be cooled to
Room temperature, filtering, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 3-6h at 60 DEG C, and grinding is received
Rice titanium oxide wraps up the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 10-25 parts of step (1), 12-18 parts of butyl rubber, 5-11 parts
Ethylene propylene diene rubber is mixed to join in banbury, the banburying 30-60min at 160-170 DEG C；130-135 DEG C is cooled to, is continued
The 3-6 parts of Petropols of carbon 5,2-5 parts of naphthenic oil, 1-2 parts of plasticizer, banburying 10-30min are added toward banbury；It is cooled to
100-115 DEG C, continue to add Nano filling, 0.5-3 parts of calcium carbonate, 0.8- obtained in 1-1.5 parts of step (3) toward banbury
2.2 parts of Di(dioctylpyrophosphato) ethylene titanate, banburying 45-70min；Continue to be cooled to room temperature, stirring mixing 1-
2h, obtains the ageing-resistant fluid sealant of automobile.
As the preferred of above-mentioned technical proposal, in step (1), the alcohols be ethanol, normal propyl alcohol, isopropanol, isobutanol,
One kind in n-butanol, sec-butyl alcohol, the tert-butyl alcohol, n-amyl alcohol, cyclopentanol, the alcamines is monoethanolamine, diethanol amine, three second
Hydramine, N, the one kind in N- dimethylethanolamines.
Used as the preferred of above-mentioned technical proposal, in step (1), the main initiator is water, HCl, the Asia of dicyclohexyl carbon two
One kind in the chloro- 2,4,4- trimethylpentanes of amine, 2-；The coinitiator is in alchlor, alkyl aluminum chloride, titanium tetrachloride
One kind.
Used as the preferred of above-mentioned technical proposal, in step (1), the styrene derivative is p-methylstyrene, a first
Base styrene, o-methyl styrene, p -ethyl-styrene, an ethyl styrene, to a propylstyrene, propylstyrene, different
One kind in propylstyrene, p-tert-butylstyrene.
As the preferred of above-mentioned technical proposal, in step (1) reaction system, the gross mass of isobutene and styrene derivative
Concentration is 10-45wt%, and isobutene, the mass ratio of styrene derivative are (0.5-2.5)：1.
Used as the preferred of above-mentioned technical proposal, in step (1) reaction system, the concentration of alcohols or alcamines is 1 × 10-2~
1×10-6mol/L。
Used as the preferred of above-mentioned technical proposal, in step (1), alcohols or alcamines and the mol ratio of coinitiator are (6-
18)：1, main initiator is 1 with the mol ratio of coinitiator：(3-12).
As the preferred of above-mentioned technical proposal, in step (2), the absolute ethyl alcohol, glacial acetic acid, triethylamine, the fourth of metatitanic acid four
The volume ratio of ester is (10-30)：(10-30)：1：(0.5-1).
Used as the preferred of above-mentioned technical proposal, in step (2), the nano silicon oxide is with the mol ratio of butyl titanate
1：(0.5-1).
Used as the preferred of above-mentioned technical proposal, in step (3), the temperature of the reaction is 80 DEG C, and the time of reaction is
22h。
The invention has the advantages that：
The present invention is obtained polyisobutene random copolymer first, rationally the process conditions in control preparation process, Yi Jisuo
With the proportioning of component so that the number-average molecular weight of obtained polyisobutene random copolymer be 50000-500000 between, its property
Can be stable, synthetic ratio is high；
On the other hand, the present invention adds appropriate nano silicon oxide as nucleation during nano-titanium oxide is prepared
Point, has been obtained the Nano filling with nano silicon oxide as core, with nano-titanium oxide as shell, and it can effectively improve the wear-resisting of material
Ageing-resistant performance, and it has good compatibility with polymer；Obtained fluid sealant anti-ultraviolet property of the invention is good, resistance to old
Change anti-wear performance is excellent, and sealing property is good, and mechanical property is good.
Specific embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -60 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, using p-methylstyrene as
Second comonomer, using HCl, alchlor ageing complexing 30min, is obtained initiation system, and adds normal propyl alcohol or the monoethanolamine to be
Third component, third component is added in reactor in monomer feed with polymerized monomer, by cation slurry copolymerizations 40
Hour, polyisobutenyl random copolymer is obtained；Wherein, in reaction system, the gross mass of isobutene and p-methylstyrene is dense
It is 45wt% to spend, and isobutene, the mass ratio of p-methylstyrene are 2.5：1；The concentration of normal propyl alcohol or monoethanolamine is 1 × 10- 6mol/L；Normal propyl alcohol or monoethanolamine and the mol ratio of alchlor are 18：1, HCl is 1 with the mol ratio of alchlor：12；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 50min
Afterwards, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；Wherein, absolute ethyl alcohol, glacial acetic acid, triethylamine,
The volume ratio of butyl titanate is 10：10：1：0.5；Nano silicon oxide is 1 with the mol ratio of butyl titanate：0.5；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 60 DEG C, reacts 40h, be cooled to room temperature, mistake
Filter, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 3h at 60 DEG C, and grinding obtains nano-titanium oxide bag
Wrap up in the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 10 parts of steps (1), 12 parts of butyl rubbers, 5 parts of ethylene-propylene-diene monomers
Glue is mixed to join in banbury, the banburying 30min at 160-170 DEG C；130-135 DEG C is cooled to, continues to add toward banbury
Enter 3 parts of Petropols of carbon 5,2 parts of naphthenic oils, 1 part of plasticizer, banburying 10min；100-115 DEG C is cooled to, is continued toward banbury
Add Nano filling obtained in 1 part of step (3), 0.5 part of calcium carbonate, 0.8 part of double (two octyloxy pyrophosphoric acid ester groups) ethylene metatitanic acid
Ester, banburying 45min；Continue to be cooled to room temperature, stirring mixing 1h obtains the ageing-resistant fluid sealant of automobile.
Embodiment 2
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -100 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, made with o-methyl styrene
It is second comonomer, using water, alkyl aluminum chloride ageing complexing 5min, initiation system is obtained, and add isobutanol or diethanol amine
It is third component, third component is added in reactor in monomer feed with polymerized monomer, by cation slurry copolymerizations
40 hours, polyisobutenyl random copolymer is obtained；Wherein, in reaction system, the gross mass of isobutene and o-methyl styrene
Concentration is 10wt%, and isobutene, the mass ratio of o-methyl styrene are 0.5：1；The concentration of isobutanol or diethanol amine be 1 ×
10-2mol/L；Isobutanol or diethanol amine and the mol ratio of alkyl aluminum chloride are 6：1, water is 1 with the mol ratio of alkyl aluminum chloride：
3；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 50min
Afterwards, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；Wherein, absolute ethyl alcohol, glacial acetic acid, triethylamine,
The volume ratio of butyl titanate is 30：30：1：1；Nano silicon oxide is 1 with the mol ratio of butyl titanate：1；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 80 DEG C, reacts 12h, be cooled to room temperature, mistake
Filter, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 6h at 60 DEG C, and grinding obtains nano-titanium oxide bag
Wrap up in the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 25 parts of steps (1), 18 parts of butyl rubbers, 11 parts of EPDMs
Rubber mix is added in banbury, the banburying 60min at 160-170 DEG C；130-135 DEG C is cooled to, is continued toward banbury
Add 6 parts of Petropols of carbon 5,5 parts of naphthenic oils, 2 parts of plasticizer, banburying 30min；100-115 DEG C is cooled to, is continued toward banbury
Nano filling obtained in 1.5 parts of steps (3) of middle addition, 3 parts of calcium carbonate, 2.2 parts of double (two octyloxy pyrophosphoric acid ester groups) ethylene titaniums
Acid esters, banburying 70min；Continue to be cooled to room temperature, stirring mixing 2h obtains the ageing-resistant fluid sealant of automobile.
Embodiment 3
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -70 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, using an ethyl styrene as
Second comonomer, using dicyclohexylcarbodiimide, alkyl aluminum chloride ageing complexing 10min, is obtained initiation system, and add isopropyl
Alcohol or diethanol amine are third component, and third component is added in reactor in monomer feed with polymerized monomer, by sun from
Sub- slurry copolymerizations 50 hours, are obtained polyisobutenyl random copolymer；Wherein, in reaction system, isobutene and an ethylo benzene
The total mass concentration of ethene is 15wt%, and isobutene, the mass ratio of an ethyl styrene are 0.9：1；Isopropanol or diethanol amine
Concentration be 1 × 10-3mol/L；Isopropanol or diethanol amine and the mol ratio of alkyl aluminum chloride are 10：1, dicyclohexyl carbon two is sub-
Amine is 1 with the mol ratio of alkyl aluminum chloride：5；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 30min
Afterwards, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；Wherein, absolute ethyl alcohol, glacial acetic acid, triethylamine,
The volume ratio of butyl titanate is 15：15：1：0.6；Nano silicon oxide is 1 with the mol ratio of butyl titanate：0.6；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 65 DEG C, reacts 23h, be cooled to room temperature, mistake
Filter, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 4h at 60 DEG C, and grinding obtains nano-titanium oxide bag
Wrap up in the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 13 parts of steps (1), 14 parts of butyl rubbers, 6 parts of ethylene-propylene-diene monomers
Glue is mixed to join in banbury, the banburying 40min at 160-170 DEG C；130-135 DEG C is cooled to, continues to add toward banbury
Enter 4 parts of Petropols of carbon 5,3 parts of naphthenic oils, 1.2 parts of plasticizer, banburying 15min；100-115 DEG C is cooled to, is continued toward banbury
Nano filling obtained in 1.1 parts of steps (3) of middle addition, 1 part of calcium carbonate, 1.1 parts of double (two octyloxy pyrophosphoric acid ester groups) ethylene titaniums
Acid esters, banburying 55min；Continue to be cooled to room temperature, stirring mixing 1.2h obtains the ageing-resistant fluid sealant of automobile.
Embodiment 4
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -80 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, using a propylstyrene as
Second comonomer, using 2- chloro- 2,4,4- trimethylpentanes, titanium tetrachloride ageing complexing 15min, is obtained initiation system, and add
N-amyl alcohol or N, N- dimethylethanolamine are third component, and third component is added to reaction in monomer feed with polymerized monomer
In device, by cation slurry copolymerizations 60 hours, polyisobutenyl random copolymer is obtained；Wherein, in reaction system, isobutyl
The total mass concentration of alkene and a propylstyrene is 20wt%, and isobutene, the mass ratio of a propylstyrene are 1.3：1；Positive penta
The concentration of alcohol or N, N- dimethylethanolamine is 1 × 10-4mol/L；N-amyl alcohol or N, N- dimethylethanolamine and titanium tetrachloride
Mol ratio is 13：1,2- chloro- 2,4,4- trimethylpentanes are 1 with the mol ratio of titanium tetrachloride：7；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 35min
Afterwards, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；Wherein, absolute ethyl alcohol, glacial acetic acid, triethylamine,
The volume ratio of butyl titanate is 20：20：1：0.7；Nano silicon oxide is 1 with the mol ratio of butyl titanate：0.7；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 70 DEG C, reacts 27h, be cooled to room temperature, mistake
Filter, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 4.5h at 60 DEG C, and grinding obtains nano-titanium oxide
Wrap up the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 16 parts of steps (1), 15 parts of butyl rubbers, 7 parts of ethylene-propylene-diene monomers
Glue is mixed to join in banbury, the banburying 45min at 160-170 DEG C；130-135 DEG C is cooled to, continues to add toward banbury
Enter 4.5 parts of Petropols of carbon 5,3.5 parts of naphthenic oils, 1.4 parts of plasticizer, banburying 20min；100-115 DEG C is cooled to, continues past close
Nano filling obtained in 1.2 parts of steps (3), 1.5 parts of calcium carbonate, 1.4 parts double (two octyloxy pyrophosphoric acid ester groups) are added in mill
Ethylene titanate esters, banburying 60min；Continue to be cooled to room temperature, stirring mixing 1.4h obtains the ageing-resistant fluid sealant of automobile.
Embodiment 5
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -90 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, using o-methyl styrene as
Second comonomer, using water, alkyl aluminum chloride ageing complexing 20min, is obtained initiation system, and add ethanol or N, N- dimethyl second
Hydramine is third component, and third component is added in reactor in monomer feed with polymerized monomer, common by cation slurry
Polymerase 17 0 hour, is obtained polyisobutenyl random copolymer；Wherein, in reaction system, isobutene and o-methyl styrene it is total
Mass concentration is 30wt%, and isobutene, the mass ratio of o-methyl styrene are 1.7：1；Ethanol or N, N- dimethylethanolamine
Concentration is 1 × 10-5mol/L；Ethanol or N, N- dimethylethanolamine and the mol ratio of alkyl aluminum chloride are 15：1, water and alkyl chloride
The mol ratio for changing aluminium is 1：9；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 40min
Afterwards, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；Wherein, absolute ethyl alcohol, glacial acetic acid, triethylamine,
The volume ratio of butyl titanate is 25：25：1：0.8；Nano silicon oxide is 1 with the mol ratio of butyl titanate：0.7；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 70 DEG C, reacts 30h, be cooled to room temperature, mistake
Filter, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 4h at 60 DEG C, and grinding obtains nano-titanium oxide bag
Wrap up in the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 19 parts of steps (1), 15 parts of butyl rubbers, 9 parts of ethylene-propylene-diene monomers
Glue is mixed to join in banbury, the banburying 50min at 160-170 DEG C；130-135 DEG C is cooled to, continues to add toward banbury
Enter 5 parts of Petropols of carbon 5,4 parts of naphthenic oils, 1.6 parts of plasticizer, banburying 20min；100-115 DEG C is cooled to, is continued toward banbury
Nano filling obtained in 1.4 parts of steps (3) of middle addition, 2 parts of calcium carbonate, 1.7 parts of double (two octyloxy pyrophosphoric acid ester groups) ethylene titaniums
Acid esters, banburying 60min；Continue to be cooled to room temperature, stirring mixing 1.6h obtains the ageing-resistant fluid sealant of automobile.
Embodiment 6
A kind of automobile preparation method of ageing-resistant fluid sealant, comprises the following steps：
(1) at -90 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, using isopropyl styrene as
Second comonomer, using 2- chloro- 2,4,4- trimethylpentanes, alchlor ageing complexing 25min, is obtained initiation system, and add
Cyclopentanol or diethanol amine are third component, and third component is added in reactor with polymerized monomer in monomer feed, passes through
Cation slurry copolymerizations 80 hours, are obtained polyisobutenyl random copolymer；Wherein, in reaction system, isobutene and isopropyl
The total mass concentration of base styrene is 10-45wt%, and isobutene, the mass ratio of isopropyl styrene are 2.2：1；Cyclopentanol or two
The concentration of monoethanolamine is 1 × 10-6mol/L；Cyclopentanol or diethanol amine and the mol ratio of alchlor are 17：1,2- chloro- 2,4,
4- trimethylpentanes are 1 with the mol ratio of alchlor：11；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, mix 45min
Afterwards, butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；Wherein, absolute ethyl alcohol, glacial acetic acid, triethylamine,
The volume ratio of butyl titanate is 30：30：1：0.5；Nano silicon oxide is 1 with the mol ratio of butyl titanate：0.8；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 75 DEG C, reacts 37h, be cooled to room temperature, mistake
Filter, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 5.5h at 60 DEG C, and grinding obtains nano-titanium oxide
Wrap up the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 23 parts of steps (1), 17 parts of butyl rubbers, 10 parts of EPDMs
Rubber mix is added in banbury, the banburying 55min at 160-170 DEG C；130-135 DEG C is cooled to, is continued toward banbury
Add 5.5 parts of Petropols of carbon 5,4.5 parts of naphthenic oils, 1.8 parts of plasticizer, banburying 25min；100-115 DEG C is cooled to, continues past
Nano filling obtained in 1.4 parts of steps (3), 2 parts of calcium carbonate, 2.0 parts double (two octyloxy pyrophosphoric acid ester groups) are added in banbury
Ethylene titanate esters, banburying 60min；Continue to be cooled to room temperature, stirring mixing 1.8h obtains the ageing-resistant fluid sealant of automobile.
Performance test is carried out to fluid sealant obtained in the present invention below；Wherein, comparative example is compared with embodiment 1, poly- different
What is added in butene random copolymer is nano silicon oxide；
The main performance index tested by JC/T 914-2003 requirements is as follows：
From the point of view of data above, the obtained Automobile sealant of the present invention, mechanical property is good, and anti-ultraviolet property is excellent,
Resistance to elevated temperatures is good.
Claims (10)
1. a kind of automobile preparation method of ageing-resistant fluid sealant, it is characterised in that comprise the following steps：
(1) at -60~-100 DEG C, using chloromethanes as solvent, using isobutene as the first monomer, made with styrene derivative
It is second comonomer, using main initiator, coinitiator ageing complexing 5-30min, initiation system is obtained, and add alcohols or hydramine
Class is third component, and third component is added in reactor in monomer feed with polymerized monomer, by cation slurry copolymerization
Close 40-90 hours, polyisobutenyl random copolymer is obtained；
(2) nano silicon oxide is scattered in absolute ethyl alcohol, is subsequently adding glacial acetic acid, triethylamine, after mixing 20-50min,
Butyl titanate is added dropwise over, continues to stir 30min, obtain mixed solution；
(3) mixed solution obtained in step (2) is transferred to water heating kettle, at 60-80 DEG C, reacts 12-40h, be cooled to room temperature,
Filtering, precipitation is washed 3-5 times with absolute ethyl alcohol, deionized water successively, freeze-day with constant temperature 3-6h at 60 DEG C, and grinding obtains nano oxidized
Titanium wraps up the Nano filling of nano silicon oxide core shell structure；
(4) by polyisobutenyl random copolymer obtained in 10-25 parts of step (1), 12-18 parts of butyl rubber, 5-11 parts of ternary
EP rubbers is mixed to join in banbury, the banburying 30-60min at 160-170 DEG C；130-135 DEG C is cooled to, continues past close
The 3-6 parts of Petropols of carbon 5,2-5 parts of naphthenic oil, 1-2 parts of plasticizer, banburying 10-30min are added in mill；It is cooled to 100-115
DEG C, continuing to add Nano filling obtained in 1-1.5 parts of step (3) toward banbury, 0.5-3 parts of calcium carbonate, 0.8-2.2 parts is double
(two octyloxy pyrophosphoric acid ester groups) ethylene titanate esters, banburying 45-70min；Continue to be cooled to room temperature, stirring mixing 1-2h is obtained
The ageing-resistant fluid sealant of automobile.
2. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：In step (1),
The alcohols is in ethanol, normal propyl alcohol, isopropanol, isobutanol, n-butanol, sec-butyl alcohol, the tert-butyl alcohol, n-amyl alcohol, cyclopentanol
Kind, the alcamines is monoethanolamine, diethanol amine, triethanolamine, N, the one kind in N- dimethylethanolamines.
3. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：In step (1),
The main initiator is the one kind in water, HCl, dicyclohexylcarbodiimide, the chloro- 2,4,4- trimethylpentanes of 2-；It is described to draw altogether
Hair agent is the one kind in alchlor, alkyl aluminum chloride, titanium tetrachloride.
4. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：In step (1),
The styrene derivative is p-methylstyrene, a methyl styrene, o-methyl styrene, p -ethyl-styrene, an ethyl
Styrene, to the one kind in propylstyrene, a propylstyrene, isopropyl styrene, p-tert-butylstyrene.
5. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：Step (1) is anti-
Answer in system, the total mass concentration of isobutene and styrene derivative is 10-45wt%, isobutene, the matter of styrene derivative
Amount is than being (0.5-2.5)：1.
6. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：Step (1) is anti-
Answer in system, the concentration of alcohols or alcamines is 1 × 10-2~1 × 10-6mol/L。
7. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：In step (1),
Alcohols or alcamines and the mol ratio of coinitiator are (6-18)：1, main initiator is 1 with the mol ratio of coinitiator：(3-
12)。
8. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：In step (2),
The absolute ethyl alcohol, glacial acetic acid, triethylamine, the volume ratio of butyl titanate are (10-30)：(10-30)：1：(0.5-1).
9. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：In step (2),
The nano silicon oxide is 1 with the mol ratio of butyl titanate：(0.5-1).
10. a kind of automobile as claimed in claim 1 preparation method of ageing-resistant fluid sealant, it is characterised in that：Step (3)
In, the temperature of the reaction is 80 DEG C, and the time of reaction is 22h.
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| CN110819268A (en) * | 2019-12-13 | 2020-02-21 | 安徽微威环保科技有限公司 | Wear-resistant sealant and preparation method thereof |
| CN116179004A (en) * | 2023-03-22 | 2023-05-30 | 北京华楚路美交通科技有限公司 | Method for preparing super-hydrophobic anti-fouling paint by self-assembly method and application |
| CN116179004B (en) * | 2023-03-22 | 2024-05-17 | 北京华楚路美交通科技有限公司 | Method for preparing super-hydrophobic anti-fouling paint by self-assembly method and application |
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