CN108587378A - A kind of impregnating with silane agent and preparation method thereof - Google Patents
A kind of impregnating with silane agent and preparation method thereof Download PDFInfo
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D143/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5035—Silica
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/65—Coating or impregnation with inorganic materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F130/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F130/04—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F130/08—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The invention discloses a kind of impregnating with silane agent and preparation method thereof, belong to chemical field.The present invention is using ethyl orthosilicate as raw material, using tartaric acid as catalyst, condensation product is obtained through hydrolysis, hydrolysis generates positive silicic acid, then condensation forms silica dioxide gel in situ in substrate pores, filling pore, improve the compactness of handled base material, and then achieve the purpose that protect concrete stone material, small-molecular-weight end hydroxyl silicone oil is added, it can form hydrophobic film layer on test specimen surface layer, prevent the entrance of moisture, and colloidal sol penetrates into inside concrete, gel is formed after condensation reaction, it is filled with hole, microcrack, increase the compactness of Surface layer's concrete, the raising of compactness makes extraneous CO2 gases be more difficult to enter inside concrete, achieve the purpose that anti-carbonation, improve the durability of concrete.The present invention solves current impregnating with silane agent poor performance, and the long-term waterproof requirement of concrete structure is not achieved, and silane emulsion content is low, volume is big, the problem of increasing cost of manufacture.
Description
Technical field
The invention belongs to chemical fields, and in particular to a kind of impregnating with silane agent and preparation method thereof.
Background technology
Impregnating with silane agent, one of Concrete Surface Durability anti-corrosion protection product.Concrete material is since the appearance, experience
Low-intensity, the development course of moderate strength, high intensity or even superhigh intensity.But the thing of a large amount of concrete structure premature failures
Show that high intensity is not meant to high-durability in fact.Concrete structure is during military service, inevitably by ambient enviroment
Physics, chemistry and biological effect, and the porosity of concrete itself provides channel for the intrusion of extraneous harmful ion, makes to mix
Solidifying soil material performance deterioration and decline, and then endanger the performance of concrete structure.Due to concrete durability deficiency, cause structure
Premature failure is so that the event for destroying avalanche is seen everywhere, and regulation effect seems not very significantly.
Newly-built reinforced concrete structures take necessary safeguard procedures to improving the durable of concrete structure
Property and extends its service life and have a very important significance.Numerous studies and engineering practice show the endurance quality of concrete
Deterioration is mostly related with water, and therefore, waterproof becomes the important means for improving concrete structure durability.
Silane is widely used in respectively because of its excellent waterproof durability and gas permeability in architectural waterproof material
In kind architectural engineering.Silane is a kind of Thief zone type waterproof material, and concrete table is sprayed in the form of solution, lotion or lotion
The waterproof anti-corrosion performance of concrete can be improved in face.
The agent of type of latex type impregnating with silane and lotion one type of silane impregnating agent are the most two one type of silane protection of application currently on the market
Agent, but current impregnating with silane agent poor performance, are not achieved the long-term waterproof requirement of concrete structure, silane emulsion content is low, mixes
The problem of measuring greatly, increasing cost of manufacture.
Invention content
The technical problems to be solved by the invention：For current impregnating with silane agent poor performance, it is long that concrete structure is not achieved
Phase waterproof requirement, silane emulsion content is low, volume is big, the problem of increasing cost of manufacture, provide a kind of impregnating with silane agent and its
Preparation method.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of impregnating with silane agent, which is characterized in that meter includes following component, 100 ~ 150 parts of impregnating with silane agent bases in parts by weight
Body object, 50 ~ 60 parts of aged substances, 70 ~ 80 parts of impregnating with silane agent spikes；
The preparation method of the aged substance, includes the following steps：According to the mass fraction, 30 ~ 40 parts of ethyl orthosilicates, 80 ~ 100 are taken
Part absolute ethyl alcohol, 100 ~ 150 parts of deionized waters, 10 ~ 15 parts of end hydroxyl silicone oils are stirred 20 ~ 30min in 25 ~ 30 DEG C, then add
The tartaric acid for entering ethyl orthosilicate quality 3 ~ 6%, is stirred, still aging to get aged substance；
The preparation method of the impregnating with silane agent matrix object, includes the following steps：Take vinyltrimethoxysilane in mass ratio
80~90：1 is added cumyl peroxide, is passed through nitrogen protection, is stirred in 100 ~ 120 DEG C, obtains mixture, take mixture
In mass ratio 3：5 are added Arlacel-80, are stirred, obtain mixture A, take mixture A in mass ratio 10：3：3 addition paregal Os,
Distilled water mixes, and is stirred in 30 ~ 40 DEG C to get impregnating with silane agent matrix object；
The preparation method of the impregnating with silane agent spike, includes the following steps：According to the mass fraction, take 5 ~ 8 parts of sodium hydroxides,
100 ~ 150 parts of deionized waters, 2 ~ 6 parts of sodium metaaluminates, 20 ~ 30 parts of Ludox, are stirred in 50 ~ 70 DEG C, obtain stirring mixture,
Take stirring mixture in mass ratio 10：1 is added 4-propyl bromide, adjusts pH to 10 ~ 10.5, is stirred, obtains mixed liquor A,
Mixed liquor A is added in the reaction kettle of polytetrafluoroethyllining lining, is warming up to 170 ~ 180 DEG C of reactions, is cooled to room temperature, filtered, take
Filter residue and drying, grinding crushed 200 mesh sieve, collect sieving particle, take sieving particulate matter in 500 ~ 550 DEG C of roastings to get silane
Impregnating agent spike.
The preparation method includes the following steps：According to the mass fraction, 100 ~ 150 parts of impregnating with silane agent matrix objects, 30 ~ 40 are taken
Part polyethylene glycol 2000,50 ~ 60 parts of aged substances, are stirred 2 ~ 3h in 50 ~ 70 DEG C, obtain impregnating agent base-material, take impregnating with silane agent
Spike in mass ratio 5：3 are added the ammonium nitrate solution of a concentration of 2mol/L, and 10 ~ 12h is stirred in 70 ~ 80 DEG C, centrifuge, it is heavy to take
It forms sediment through distilling water washing, takes washings to roast 3 ~ 4h in 530 ~ 540 DEG C, obtain calcining matter, take calcining matter in mass ratio 3：10 incorporations
Impregnating agent base-material is stirred 40 ~ 50min in 50 ~ 60 DEG C, and homogeneous is to get impregnating with silane agent.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention is using ethyl orthosilicate as raw material, using tartaric acid as catalyst, obtains condensation product through hydrolysis, hydrolysis generates
Positive silicic acid, then condensation forms silica dioxide gel in situ in substrate pores, and filling pore improves the closely knit of handled base material
Degree, and then achieve the purpose that protect concrete stone material, small-molecular-weight end hydroxyl silicone oil is added, and surface tension is relatively low and with thin
Water base methyl, with gel have good intersolubility, can test specimen surface layer formed hydrophobic film layer, prevent moisture into
Enter, and colloidal sol penetrates into inside concrete, forms gel after condensation reaction, is filled with hole, microcrack, it is mixed to increase surface layer
The compactness of soil is coagulated, the raising of compactness makes extraneous CO2 gases be more difficult to enter inside concrete, achievees the purpose that anti-carbonation, carry
The high durability of concrete；
（2）Initiator is added using vinyltrimethoxysilane as raw material in the present invention, forms silane polymer, adds sapn-
80, the compound emulsions such as paregal O disperse, and obtain silane emulsion, under lipophilic emulsifier and hydrophilic emulsifier collective effect,
Water can be preferably wrapped in silane monomer surface, improve emulsion intercalation method, connected Si polar group and concrete
Condensation reaction occurs for the hydroxyl on surface, and nonpolar hydrophobic group flexes outward to form water-repellent layer, makes connecing for concrete surface and water
Feeler increase, the Si-O-Si long-chains being formed simultaneously surface formed reticulated film structure, can effectively prevent moisture content infiltration and
Transfer, significantly reduces the water imbibition of coagulation, and prevents using water as the intrusion of the harmful ion of conveying medium, can be long-term, have
Effect achievees the effect that waterproofing protection, and is compounded with above-mentioned hydrophobic silica hybrid gel, is small molecule silane, mixes
Enter in impregnating with silane agent base-material, on the one hand promotes the permeance property of impregnating with silane agent, on the other hand can solve silane in lotion
The low problem of content, while liquid reduces the cost of manufacture of silane；
（3）The present invention, as silicon source, prepares the filler of impregnating with silane agent using Ludox as silicon source, sodium metaaluminate, has three-dimensional
Intersect straight passage structures, containing unique five-membered ring structure, there is thermal stability, high oleophilic drainage, preferable corrosion resisting property, silicon
Bonding reaction can occur for alcoxyl silicon group and the hydroxyl on filler surface in alkane impregnating agent, and silane breast is doped to using it as filler
The mechanical performance that lotion can be not only improved in liquid base material, being coated to concrete substrate surface can also eliminate in fragile material
The hidden danger such as portion's micro-crack extension.
Specific implementation mode
Aged substance：According to the mass fraction, take 30 ~ 40 parts of ethyl orthosilicates, 80 ~ 100 parts of absolute ethyl alcohols, 100 ~ 150 parts go
Ionized water, 10 ~ 15 parts of end hydroxyl silicone oils, are stirred 20 ~ 30min in 25 ~ 30 DEG C, add ethyl orthosilicate quality 3 ~ 6%
Tartaric acid is stirred 1 ~ 2h, and still aging 10 ~ 12h is to get aged substance.
Impregnating with silane agent matrix object：Take vinyltrimethoxysilane in mass ratio 80 ~ 90：1 is added peroxidating diisopropyl
Benzene is passed through nitrogen protection, is stirred 6 ~ 9h in 100 ~ 120 DEG C, obtains mixture, takes mixture in mass ratio 3：5 are added sapn-
80, it is stirred 30 ~ 40min, obtains mixture A, takes mixture A in mass ratio 10：3：3 are added paregal O, distilled water mixing,
1 ~ 2h is stirred to get mixed liquor in 30 ~ 40 DEG C.
Impregnating with silane agent spike：According to the mass fraction, take 5 ~ 8 parts of sodium hydroxides, 100 ~ 150 parts of deionized waters, 2 ~ 6 parts partially
Sodium aluminate, 20 ~ 30 parts of Ludox, are stirred 2 ~ 3h in 50 ~ 70 DEG C, obtain stirring mixture, take stirring mixture in mass ratio
10：1 is added 4-propyl bromide, adjusts pH to 10 ~ 10.5, is stirred 2 ~ 5h, obtains mixed mixed liquor A, mixed liquor A is added poly-
In the reaction kettle of tetrafluoroethene liner, 170 ~ 180 DEG C of 2 ~ 4h of reaction are warming up to, is cooled to room temperature, is filtered, take filter residue and drying, grind
Mill crushed 200 mesh sieve, collects sieving particle, takes sieving particulate matter to roast 2 ~ 3h in 500 ~ 550 DEG C, obtain impregnating with silane agent and mix
Material.
A kind of preparation method of impregnating with silane agent, includes the following steps：According to the mass fraction, 100 ~ 150 parts of silane leachings are taken
Stain agent matrix object, 30 ~ 40 parts of polyethylene glycol 2000s, 50 ~ 60 parts of aged substances, are stirred 2 ~ 3h in 50 ~ 70 DEG C, obtain impregnating agent base
Material, takes impregnating with silane agent spike in mass ratio 5：3 are added the ammonium nitrate solution of a concentration of 2mol/L, are stirred in 70 ~ 80 DEG C
10 ~ 12h, centrifugation take precipitation through distilling water washing, take washings to roast 3 ~ 4h in 530 ~ 540 DEG C, obtain calcining matter, take calcining matter
In mass ratio 3：10 incorporation impregnating agent base-materials, 40 ~ 50min are stirred in 50 ~ 60 DEG C, homogeneous is to get impregnating with silane agent.
Embodiment 1
Aged substance：According to the mass fraction, 30 parts of ethyl orthosilicates, 80 parts of absolute ethyl alcohols, 100 parts of deionized waters, 10 parts of end hydroxyls are taken
Base silicone oil is stirred 20min in 25 DEG C, adds the tartaric acid of ethyl orthosilicate quality %, is stirred 1h, still aging
10h is to get aged substance.
Impregnating with silane agent matrix object：Take vinyltrimethoxysilane in mass ratio 80：1 is added cumyl peroxide,
It is passed through nitrogen protection, 6h is stirred in 100 DEG C, obtains mixture, takes mixture in mass ratio 3：5 are added Arlacel-80, and stirring is mixed
30min is closed, mixture A is obtained, takes mixture A in mass ratio 10：3：3 are added paregal O, distilled water mixing, mixed in 30 DEG C of stirrings
1h is closed to get mixed liquor.
Impregnating with silane agent spike：According to the mass fraction, take 5 parts of sodium hydroxides, 100 parts of deionized waters, 2 parts of sodium metaaluminates,
20 parts of Ludox are stirred 2h in 50 DEG C, obtain stirring mixture, take stirring mixture in mass ratio 10：1 is added tetrapropyl bromine
Change ammonium, adjust pH to 10, be stirred 2h, obtain mixed mixed liquor A, mixed liquor A is added in the reaction kettle of polytetrafluoroethyllining lining,
170 DEG C of reaction 2h are warming up to, is cooled to room temperature, filters, take filter residue and drying, grind, crushed 200 mesh sieve, collect sieving particle,
It takes sieving particulate matter to roast 2h in 500 DEG C, obtains impregnating with silane agent spike.
A kind of preparation method of impregnating with silane agent, includes the following steps：According to the mass fraction, 100 parts of impregnating with silane agent are taken
Matrix object, 30 parts of polyethylene glycol 2000s, 50 parts of aged substances, are stirred 2h in 50 DEG C, obtain impregnating agent base-material, take impregnating with silane agent
Spike in mass ratio 5：3 are added the ammonium nitrate solution of a concentration of 2mol/L, and 10h is stirred in 70 DEG C, centrifuge, and take precipitation through steaming
Distilled water is washed, and is taken washings to roast 3h in 530 DEG C, is obtained calcining matter, take calcining matter in mass ratio 3：10 incorporation impregnating agent base-materials, in
50 DEG C are stirred 40min, and homogeneous is to get impregnating with silane agent.
Embodiment 2
Aged substance：According to the mass fraction, 40 parts of ethyl orthosilicates, 100 parts of absolute ethyl alcohols, 150 parts of deionized waters, 15 parts of end hydroxyls are taken
Base silicone oil is stirred 30min in 30 DEG C, adds the tartaric acid of ethyl orthosilicate quality 6%, is stirred 2h, still aging
12h is to get aged substance.
Impregnating with silane agent matrix object：Take vinyltrimethoxysilane in mass ratio 90：1 is added cumyl peroxide,
It is passed through nitrogen protection, 9h is stirred in 120 DEG C, obtains mixture, takes mixture in mass ratio 3：5 are added Arlacel-80, and stirring is mixed
40min is closed, mixture A is obtained, takes mixture A in mass ratio 10：3：3 are added paregal O, distilled water mixing, mixed in 40 DEG C of stirrings
2h is closed to get mixed liquor.
Impregnating with silane agent spike：According to the mass fraction, take 8 parts of sodium hydroxides, 150 parts of deionized waters, 6 parts of sodium metaaluminates,
30 parts of Ludox are stirred 3h in 70 DEG C, obtain stirring mixture, take stirring mixture in mass ratio 10：1 is added tetrapropyl bromine
Change ammonium, adjust pH to 10.5, be stirred 5h, obtain mixed mixed liquor A, mixed liquor A is added to the reaction kettle of polytetrafluoroethyllining lining
In, 180 DEG C of reaction 4h are warming up to, is cooled to room temperature, filters, take filter residue and drying, grind, 200 mesh sieve is crushed, collects sieving
Grain takes sieving particulate matter to roast 3h in 550 DEG C, obtains impregnating with silane agent spike.
A kind of preparation method of impregnating with silane agent, includes the following steps：According to the mass fraction, 150 parts of impregnating with silane agent are taken
Matrix object, 40 parts of polyethylene glycol 2000s, 60 parts of aged substances, are stirred 3h in 70 DEG C, obtain impregnating agent base-material, take impregnating with silane agent
Spike in mass ratio 5：3 are added the ammonium nitrate solution of a concentration of 2mol/L, and 12h is stirred in 80 DEG C, centrifuge, and take precipitation through steaming
Distilled water is washed, and is taken washings to roast 4h in 540 DEG C, is obtained calcining matter, take calcining matter in mass ratio 3：10 incorporation impregnating agent base-materials, in
60 DEG C are stirred 50min, and homogeneous is to get impregnating with silane agent.
Embodiment 3
Aged substance：According to the mass fraction, 35 parts of ethyl orthosilicates, 90 parts of absolute ethyl alcohols, 125 parts of deionized waters, 12.5 parts of ends are taken
Hydroxy silicon oil is stirred 25min in 27.5 DEG C, adds the tartaric acid of ethyl orthosilicate quality 4.5%, be stirred 1.5h,
Still aging 11h is to get aged substance.
Impregnating with silane agent matrix object：Take vinyltrimethoxysilane in mass ratio 85：1 is added cumyl peroxide,
It is passed through nitrogen protection, 7.5h is stirred in 110 DEG C, obtains mixture, takes mixture in mass ratio 3：5 are added Arlacel-80, stirring
35min is mixed, mixture A is obtained, takes mixture A in mass ratio 10：3：3 are added paregal O, distilled water mixing, in 35 DEG C of stirrings
1.5h is mixed to get mixed liquor.
Impregnating with silane agent spike：According to the mass fraction, 7.5 parts of sodium hydroxides, 125 parts of deionized waters, 4 parts of meta-aluminic acids are taken
Sodium, 25 parts of Ludox, are stirred 2.5h in 60 DEG C, obtain stirring mixture, take stirring mixture in mass ratio 10：1 is added four
Propyl ammonium bromide adjusts pH to 10.25, is stirred 3.5h, obtains mixed mixed liquor A, polytetrafluoroethyllining lining is added in mixed liquor A
Reaction kettle in, be warming up to 175 DEG C reaction 3h, be cooled to room temperature, filter, take filter residue and drying, grind, crushed 200 mesh sieve, receive
Collection sieving particle, takes sieving particulate matter to roast 2 ~ 3h in 525 DEG C, obtains impregnating with silane agent spike.
A kind of preparation method of impregnating with silane agent, includes the following steps：According to the mass fraction, 125 parts of impregnating with silane agent are taken
Matrix object, 35 parts of polyethylene glycol 2000s, 55 parts of aged substances, are stirred 2.5h in 60 DEG C, obtain impregnating agent base-material, take impregnating with silane
Agent spike in mass ratio 5：3 are added the ammonium nitrate solution of a concentration of 2mol/L, in
75 DEG C are stirred 11h, centrifugation, take precipitation through distillation water washing, take washings to roast 3.5h in 535 DEG C, obtain calcining matter,
Take calcining matter in mass ratio 3：10 incorporation impregnating agent base-materials, 45min are stirred in 55 DEG C, homogeneous is to get impregnating with silane agent.
Comparative example 1
It is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking aged substance.
Comparative example 2
It is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking aged substance and impregnating with silane agent matrix object.
Comparative example 3
It is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking aged substance, impregnating with silane agent matrix object and silane
Impregnating agent spike.
Comparative example 4：A kind of impregnating with silane agent of company of Chongqing City production
The impregnating with silane agent sample of the present invention and the impregnating with silane agent sample of comparative example prepared by embodiment 1 ~ 3 are pressed into 300g/m2
Dosage is coated on the concrete surface that intensity is C40, and room temperature maintenance is surveyed by the method in specification JTJ275-2000 after a week
Examination, test result is as follows table 1：
Table 1
Impregnating with silane agent weatherability contrast test：The impregnating with silane agent prepared for the qualitative embodiment of the present invention 1 ~ 3 and comparative example
Impregnating with silane agent weather resistance, carried out impregnating with silane agent weatherability contrast test.Test result such as table 2：
Table 2
The concrete surface hydrophobicity performance for having brushed impregnating with silane agent product of the present invention is excellent, and the water absorption rate of concrete test block is average
Value is less than 0.01mm/min1/2, and penetration depth reaches 3 ~ 4mm or more, and the reducing effect average value of chloride uptake is more than
90%, meet JTJ275-2000《Concrete for marine works structural anticorrosion loses technical specification》It is required that and there is good weatherability
Energy.In conclusion the application effect of impregnating with silane agent prepared in the present invention complies fully with requirement, it is worth promoting and makes
With.
Claims (2)
1. a kind of impregnating with silane agent, which is characterized in that meter includes following component, 100 ~ 150 parts of impregnating with silane agent in parts by weight
Matrix object, 50 ~ 60 parts of aged substances, 70 ~ 80 parts of impregnating with silane agent spikes；
The preparation method of the aged substance, includes the following steps：According to the mass fraction, 30 ~ 40 parts of ethyl orthosilicates, 80 ~ 100 are taken
Part absolute ethyl alcohol, 100 ~ 150 parts of deionized waters, 10 ~ 15 parts of end hydroxyl silicone oils are stirred 20 ~ 30min in 25 ~ 30 DEG C, then add
The tartaric acid for entering ethyl orthosilicate quality 3 ~ 6%, is stirred, still aging to get aged substance；
The preparation method of the impregnating with silane agent matrix object, includes the following steps：Take vinyltrimethoxysilane in mass ratio
80~90：1 is added cumyl peroxide, is passed through nitrogen protection, is stirred in 100 ~ 120 DEG C, obtains mixture, take mixture
In mass ratio 3：5 are added Arlacel-80, are stirred, obtain mixture A, take mixture A in mass ratio 10：3：3 addition paregal Os,
Distilled water mixes, and is stirred in 30 ~ 40 DEG C to get impregnating with silane agent matrix object；
The preparation method of the impregnating with silane agent spike, includes the following steps：According to the mass fraction, take 5 ~ 8 parts of sodium hydroxides,
100 ~ 150 parts of deionized waters, 2 ~ 6 parts of sodium metaaluminates, 20 ~ 30 parts of Ludox, are stirred in 50 ~ 70 DEG C, obtain stirring mixture,
Take stirring mixture in mass ratio 10：1 is added 4-propyl bromide, adjusts pH to 10 ~ 10.5, is stirred, obtains mixed liquor A,
Mixed liquor A is added in the reaction kettle of polytetrafluoroethyllining lining, is warming up to 170 ~ 180 DEG C of reactions, is cooled to room temperature, filtered, take
Filter residue and drying, grinding crushed 200 mesh sieve, collect sieving particle, take sieving particulate matter in 500 ~ 550 DEG C of roastings to get silane
Impregnating agent spike.
2. a kind of preparation method of impregnating with silane agent as described in claim 1, which is characterized in that the preparation method includes as follows
Step：According to the mass fraction, 100 ~ 150 parts of impregnating with silane agent matrix objects, 30 ~ 40 parts of polyethylene glycol 2000s, 50 ~ 60 parts of ageings are taken
Object is stirred 2 ~ 3h in 50 ~ 70 DEG C, obtains impregnating agent base-material, takes impregnating with silane agent spike in mass ratio 5：3 additions are a concentration of
The ammonium nitrate solution of 2mol/L is stirred 10 ~ 12h in 70 ~ 80 DEG C, centrifugation, take precipitation through distill water washing, take washings in
530 ~ 540 DEG C of 3 ~ 4h of roasting, obtain calcining matter, take calcining matter in mass ratio 3：10 incorporation impregnating agent base-materials, it is mixed in 50 ~ 60 DEG C of stirrings
40 ~ 50min is closed, homogeneous is to get impregnating with silane agent.
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Application publication date: 20180928 |