CN113529417B - Water-based organic silicon permeable anti-corrosion impregnant and preparation method thereof - Google Patents

Water-based organic silicon permeable anti-corrosion impregnant and preparation method thereof Download PDF

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CN113529417B
CN113529417B CN202110814976.2A CN202110814976A CN113529417B CN 113529417 B CN113529417 B CN 113529417B CN 202110814976 A CN202110814976 A CN 202110814976A CN 113529417 B CN113529417 B CN 113529417B
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impregnant
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silane
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CN113529417A (en
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方子善
王成启
聂亚楠
梁远博
张晓乐
郭玉林
万超群
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CCCC Third Harbor Engineering Co Ltd
CCCC Shanghai Third Harbor Engineering Science and Technology Research Institute Co Ltd
CCCC Shanghai Harbour Engineering Design and Research Institute Co Ltd
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CCCC Third Harbor Engineering Co Ltd
CCCC Shanghai Third Harbor Engineering Science and Technology Research Institute Co Ltd
CCCC Shanghai Harbour Engineering Design and Research Institute Co Ltd
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Abstract

The application discloses a water-based organic silicon permeable anti-corrosion impregnant and a preparation method thereof, wherein the impregnant consists of an alkyl silanol solution, a quaternized silane alcohol solution, ethyl silicate, water, an active component and a curing agent; the molar ratio of alkyl silanol, quaternized silane, ethyl silicate and water is 1: (0.2-1): (0-1.5): (0-2), the ratio of the mass of the active component to the total mass of the solution of alkyl silanol, the alcohol solution of quaternized silane, ethyl silicate and water is 0:1 to 1:1, the ratio of the mass of the curing agent to the mass of the active component is 0: 100-2: 100. the method comprises the following steps: uniformly stirring and aging an alkyl silanol solution, a quaternized silane alcohol solution, ethyl silicate and water; adding active components, and uniformly stirring to obtain a mixed solution; and weighing and uniformly mixing the curing agent to obtain the aqueous organosilicon permeable anti-corrosion impregnant. The application is stored in a stable high-solid-content liquid form, water is added for dilution during use, the concentration can be freely adjusted, and the diluent still has good stability.

Description

Water-based organic silicon permeable anti-corrosion impregnant and preparation method thereof
Technical Field
The application belongs to the technical field of organic silicon materials, and particularly relates to a water-based organic silicon permeable anti-corrosion impregnant and a preparation method thereof.
Background
The organosilicon permeable anticorrosive impregnant is one of the most effective surface hydrophobic anticorrosive modified materials of porous materials with surface hydrophilicity, powder materials, materials with surface micro-nano structure and other high specific surface area materials, and can be divided into pure organosilicon type, paste type, solvent type and water emulsion type according to physical state, wherein the research and application of the organosilicon permeable anticorrosive impregnant of pure organosilicon type are most extensive, and the organosilicon permeable anticorrosive impregnant has the advantages of high solid content, low viscosity, high permeability, convenient treatment and the like, but also has the problems of serious volatilization waste, slow coupling reaction with the surface of the impregnated substrate and the like, and is gradually replaced by the organosilicon permeable impregnant of paste type, solvent type and water emulsion type; the paste organic silicon permeation type anti-corrosion impregnant has extremely low volatility, large surface liquid holdup of the base material and more efficient operation, but has the defect of poor permeability; the solvent type organic silicon permeation type anti-corrosion impregnant has poor permeability, but the solvent volatilizes to cause material waste, pollute the environment and have potential safety hazards; the aqueous emulsion type organic silicon penetrating type anti-corrosion impregnant is a relatively novel organic silicon penetrating type anti-corrosion impregnant, and the ideal organic silicon penetrating type anti-corrosion impregnant has the advantages of convenient treatment of the pure organic silicon penetrating type anti-corrosion impregnant, low volatility of the paste type organic silicon penetrating type anti-corrosion impregnant, high permeability of the solvent type organic silicon penetrating type anti-corrosion impregnant and the like, has optimal comprehensive performance and has good application prospect.
The current water emulsion type organic silicon penetrating type anti-corrosion impregnant mainly has the following problems: the emulsion is unstable in state, is easy to delaminate, has short effective period and is not durable to store; the use of the emulsifier leads to the existence of residual emulsifier on the impregnated surface, which causes the defects of unsatisfactory hydrophobic modification effect, oil stain or whitening, unsatisfactory hydrolysis resistance and the like; the solid content is low, the transportation cost is high, the number of dipping times is large, and the operation process is complex; concentration regulation is difficult and universality is poor. Therefore, aiming at the defects and shortcomings in the prior art, the development of an aqueous organosilicon permeable anti-corrosion impregnant and a preparation method thereof are technical problems which are needed to be solved urgently.
Disclosure of Invention
Aiming at the defects or shortcomings of the prior art, the technical problem to be solved by the application is to provide the aqueous organosilicon permeable anticorrosive impregnant and the preparation method, wherein the aqueous organosilicon permeable anticorrosive impregnant is stored in a stable liquid form with high solid content, and can be diluted by adding water when in use, the concentration can be freely adjusted according to the requirement, and the diluent still has good stability and long operation time.
In order to solve the technical problems, the application is realized by the following technical scheme:
in one aspect, the application provides an aqueous organosilicon permeable anticorrosive impregnant which consists of an alkyl silanol solution, a quaternized silane alcohol solution, ethyl silicate, water, an active component and a curing agent;
the molar ratio of the alkyl silanol, the quaternized silane, the ethyl silicate and the water is 1: (0.2-1): (0-1.5): (0-2),
the ratio of the mass of the active component to the total mass of the solution of alkyl silanol, the alcoholic solution of quaternized silane, the ethyl silicate and the water is 0:1 to 1:1,
the ratio of the mass of the curing agent to the mass of the active component is 0: 100-2: 100.
preferably, the aqueous organosilicon penetrating type antiseptic impregnant, wherein the structural formula of the alkyl silanol is R m Si(OH) 4-m Or (HO) 3 Si(CH 2 ) n Si(OH) 3 And a low molecular weight polycondensate thereof, wherein R represents a hydrocarbon group having 1 to 22 carbon atoms and a derivative thereof which is stable in a weakly acidic alcohol-water system and has neutral acid-base property to weakly acidic property and has hydrophobicity, m is 1 to 3, n is 1 to 22;
the solution of the alkyl silanol is clear and transparent homogeneous liquid, the pH value is 2-8, the mass fraction of the alkyl silanol is 40-100%, the alkyl alkoxysilane corresponding to the alkyl silanol is prepared by acid hydrolysis, and is freshly prepared, the hydrolysis system contains a solvent, if the hydrolysis adopts a solvent-free method, the solvent in the hydrolysis system is alcohol generated by alkoxy of the alkyl alkoxysilane corresponding to the alkyl silanol when the alkyl alkoxysilane is hydrolyzed, and if the hydrolysis adopts a method with a reaction solvent, the solvent in the hydrolysis system comprises: the alcohol generated by alkoxy and reaction solvent during the hydrolysis of alkyl alkoxy silane corresponding to alkyl silanol, and the reaction solvent can be low-toxicity water-miscible small-molecule volatile alcohol, ester, ether and ketone solvents, wherein the relation between the water used for the hydrolysis and the alkyl alkoxy silane corresponding to the alkyl silanol is that the mole number of the alkyl alkoxy silane corresponding to the alkyl silanol is less than or equal to the mole number of the water used for the hydrolysis and less than or equal to the total mole number of alkoxy in the alkyl alkoxy silane corresponding to the alkyl silanol, and a hydrolysis system after the hydrolysis is used as a solution of the alkyl silanol, or a solution of the alkyl silanol after partial solvent is removed by reduced pressure distillation;
further, the alkylsilanol includes: any ratio of one or more of dimethylsilanol, butylsilanol, cyclohexylsilanol, octylsilanol, decylsilanol, dodecylsilanol, octadecyl silanol, butylmethylsilanol, cyclohexylmethylsilanol, octylmethylsilanol, dodecylmethylsilanol, octadecylmethylsilanol, dibutylsilanol, dicyclohexylsilanol, dioctyl silanol, 3- (methacryloyloxy) propylsilanol, 1, 2-bis (trihydroxysilane) ethane or 1, 6-bis (trihydroxysilane) hexane;
and/or, the reaction solvent comprises: any mixture of one or more of methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, tert-butanol or ethylene glycol dimethyl ether.
Preferably, the aqueous organosilicon permeable preservative impregnant is a silane coupling agent or oligomer thereof with a functionality of 2-3 and containing quaternary ammonium salt groups in the molecule, and the structural formula is [ R ] 1 x (R 2 O) 3-x Si-(CH 2 ) y -N + (R 3 ) 2 -R 4 ]X - Wherein R is 1 And R is 4 All represent hydrocarbon groups of 1 to 22 carbon atoms and derivatives which are stable in a weakly acidic alcohol-water system, neutral in acid-base nature to weakly acidic and hydrophobic in nature, R 2 Represents an alkyl group having 1 to 3 carbon atoms, R 3 Represents a hydrocarbon group having 1 to 7 carbon atoms, x is 1 to 2, y is 1 to 8, and X is 1 to 8 - Represents F - 、Cl - 、Br - 、NO 3 - 、ClO 4 - 、(SO 4 C n H 2n+1 ) - (1≤n≤4)、(SO 3 C n H 2n-m+1 Y m ) - (n is not less than 1 and not more than 4, m is not less than 0 and not more than 2n+1, Y is F - Or Cl - 、(SO 3 C 6 H 5 ) - 、(SO 3 C 7 H 7 ) - 、H 2 PO 4 - 、H 2 PO 3 - 、[PO 2 (OC n H 2n+1 ) 2 ] - (1≤n≤3)、BF 4 - 、PF 6 - 、HPO 3 F - 、
Figure BDA0003169695790000041
Figure BDA0003169695790000042
C n H 2n-m+ 1 Y m COO - (n is more than or equal to 0 and less than or equal to 4, m is more than or equal to 0 and less than or equal to 2n+1, Y is F) - Or Cl - 、NH 2 C n H 2n COO - (1.ltoreq.n.ltoreq.2) or HOC n H 2n COO - (1 is more than or equal to n is more than or equal to 2) and the like-1 valence anions;
the alcohol adopted in the alcohol solution of the quaternized silane is methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol or tertiary butanol, and the mass fraction of the quaternized silane in the alcohol solution of the quaternized silane is 40-100%;
further, the quaternized silane includes: any mixture of one or more of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, decyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, didecylmethyl [3- (trimethoxysilyl) propyl ] ammonium chloride (deciduous ammonium chloride), dodecyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, tetradecyldimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, hexadecyldimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, and octadecyldimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride.
Preferably, the aqueous organosilicon penetrating type antiseptic impregnant is prepared from tetraethyl orthosilicate and low molecular weight polycondensate thereof, siO 2 The mass fraction is 28-50%.
Preferably, the aqueous organosilicon penetrating type preservative impregnant, wherein the active components comprise: hydrogen-containing silicone oil, alkyl alkoxy silane, drying oil, unsaturated monomer, prepolymer thereof or alcohol-soluble unsaturated resin;
further, the hydrogen-containing silicone oil includes: any mixture of one or more of methyl hydrogen silicone oil, ethyl hydrogen silicone oil or phenyl hydrogen silicone oil;
and/or, the structural formula of the alkyl alkoxy silane is R 1 m Si(OR 2 ) 4-m Or (R) 2 O) 3 Si(CH 2 ) n Si(OR 2 ) 3 And low molecular weight polycondensates thereof, wherein R 1 Represents a hydrocarbon group having 1 to 22 carbon atoms and a derivative which is stable in a weakly acidic alcohol-water system, has neutral acid-base properties to weakly acidic properties and has hydrophobicity, R 2 Represents alkyl with 1-3 carbon atoms, m is more than or equal to 1 and less than or equal to 3, and n is more than or equal to 1 and less than or equal to 22;
and/or, the drying oil comprises: any ratio mixture of one or more of tung oil, catalpa oil or flax oil and the like;
and/or, the unsaturated monomer comprises: any ratio mixture of one or more of styrene, vinyl ester, vinyl ether, acrylic ester or methacrylic ester and the like;
and/or, the alcohol-soluble unsaturated resin comprises: a mixture of one or more of unsaturated polyester resin, vinyl ester resin, polybutadiene resin, modified terpene resin and the like in any proportion;
still further, the alkylalkoxysilane includes: any mixture of one or more of methyltrimethoxysilane, methyltriethoxysilane, methyltripropoxysilane, methyltrisopropoxysilane, chloromethyltrimethoxysilane, (dichloromethyl) trimethoxysilane, (trifluoromethyl) trimethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane, ethylmethyldimethoxysilane, cyanoethylmethyldimethoxysilane, vinyltrimethoxysilane, phenyltrimethoxysilane, cyclopentyltrimethoxysilane, mercaptopropyltrimethoxysilane, acetoxypropyltrimethoxysilane, 3- (2, 3-epoxypropoxy) propyltriethoxysilane, 2- (3, 4-epoxycyclohexane) ethyltriethoxysilane, 3-methacryloxypropyltriethoxysilane, butyltriethoxysilane, octyltriethoxysilane, decyltriethoxysilane, dodecyltrimethoxysilane, octadecyltrimethoxysilane, trideoxyoctyltrimethoxysilane, ethylenebis (trimethoxysilane), bis- [3- (trimethoxy) propyl ] disulfide or bis- [3- (triethoxysilyl) propyl ] tetrasulfide.
Preferably, the aqueous organosilicon penetrating type preservative impregnant, wherein the curing agent comprises: a polymerization initiator and a promoter, a catalyst or a drier which are matched with the active components;
further, the curing agent includes: any ratio of one or more substances selected from dioctyltin laurate, dibutyl tin oxide, isopropyl tri (dioctyl oxy pyrophosphoryl) titanate, bis (dioctyl oxy pyrophosphoryl) ethylene titanate, tetraisopropyl di (dioctyl phosphyloxy) titanate, 2-di (allyloxymethyl) -1-butoxytri (dioctyl oxy pyrophosphoryl) titanate or titanate coupling agent TC-27, which are suitable for catalyzing crosslinking and curing of alkylalkoxysilane;
further comprises: the catalyst is a mixture of one or more of iron naphthenate, copper naphthenate, cobalt isooctanoate, zirconium isooctanoate or manganese isooctanoate which are suitable for catalyzing oxidative crosslinking and curing of drying oil in any proportion;
further comprises: the catalyst is suitable for initiating or catalyzing the free radical polymerization and curing of unsaturated monomers and prepolymers thereof or alcohol-soluble unsaturated resins, namely, any ratio mixture of one or more of tert-butyl hydroperoxide, di-tert-butyl hydroperoxide, methyl ethyl ketone peroxide, methyl ethyl ketone-cobalt isooctanoate, benzoyl peroxide-N, N-dimethylaniline, ammonium persulfate or azodiisobutyronitrile.
The application also provides a preparation method of the aqueous organosilicon permeable antiseptic impregnant,
weighing 1mol of solution containing alkyl silanol, 0.2-1 mol of alcohol solution containing quaternized silane, 0-1.5 mol of ethyl silicate and 0-2 mol of water, uniformly stirring and aging;
adding an active component into the mixture, and uniformly stirring the mixture to obtain a mixed solution, wherein the ratio of the mass of the active component to the total mass of the alkyl silanol solution, the quaternized silane alcohol solution, the ethyl silicate and the water is 0:1-1:1; wherein, optionally, stirring uniformly at a rotating speed of 300-1000 r/min, and aging for 1-10 d;
weighing a curing agent, wherein the mass ratio of the curing agent to the active components is 0:100-2:100, adding the water-insoluble curing agent into the mixed solution and stirring uniformly, and adding the water-insoluble curing agent immediately after adding the active components and stirring uniformly, or adding the water-insoluble curing agent before use to obtain the water-based organic silicon permeable anti-corrosion impregnant, wherein the water-based organic silicon permeable anti-corrosion impregnant can be used by adding the water according to a certain proportion and stirring uniformly, and the stirring speed is 500-1000 r/min;
the water-soluble curing agent is not required to be added into the mixed solution, and is respectively stored in different containers with the mixed solution to be used as a matched combination, namely the water-based organic silicon permeation type anti-corrosion impregnant.
If the water-insoluble curing agent is selected from the curing agents such as peroxides and azo compounds which have catalytic activity or are not known whether or not they can be stabilized in the mixed solution, the curing agents can be added into the mixed solution only before use; if the curing agent which does not have catalytic activity and can be stabilized in the mixed solution is selected, such as zirconium isooctanoate, manganese isooctanoate and the like which can catalyze the crosslinking and curing of the drying oil by oxygen and light, the active components can be added into the mixed solution immediately after being uniformly stirred, but the mixed solution added with the curing agent needs to be stored in a shade, dry and light-proof place in a sealing way.
Compared with the prior art, the application has the following technical effects:
(1) The application introduces emulsifying quaternary ammonium salt groups into organosilicon molecules through condensation of organosilicon quaternary ammonium salt and alkyl silanol, so that the organosilicon molecules have self-emulsifying property; through condensation of ethyl silicate and alkyl silanol, the functionality of the organosilicon molecules is improved, and the activity of coupling reaction between the organosilicon molecules and the surface of the substrate is improved, so that the organosilicon molecules are compactly arranged on the surface of the substrate and are compactly combined with the surface of the substrate, and the effect of hydrophobic modification is improved; in addition, the condensation polymerization reaction is used up to consume water and silicon hydroxyl in the system, namely the system is converted into an oligomeric alkyl silicate solution without water and alkyl silanol after aging, the oligomeric alkyl silicate solution is free of reactivity when not contacted with water, is very stable and has a longer effective period, the dilute oligomeric alkyl silicate is contacted with water and is partially hydrolyzed, the dilute oligomeric alkyl silicate solution has stronger reactivity, and meanwhile, the oligomeric alkyl silicate solution is formed into emulsion under the effect of emulsifying quaternary ammonium salt groups in molecules, the oligomeric alkyl silicate molecules are consistent on the interface and are arranged in a way that alkyl groups point to an oil phase, silicate groups and silanol groups generated by hydrolysis of the oligomeric alkyl silicate molecules point to an aqueous phase, compared with the conventional alkyl trialkoxysilane, the organic silicon is difficult to generate side reactions such as forming cage polysilsesquioxane, all active groups are combined with the surface of a substrate, and the effective utilization rate of the active groups is higher.
(2) The aqueous organosilicon permeable anti-corrosion impregnant has self-emulsifying property, and can be dispersed in water to form stable emulsion without adding any emulsifying agent; in addition, the aqueous organic silicon penetrating type anti-corrosion impregnant and the preparation method thereof are characterized in that active components such as hydrogen-containing silicone oil, alkyl alkoxy silane, drying oil, unsaturated monomer and prepolymer thereof or alcohol-soluble unsaturated resin are added into the aqueous organic silicon penetrating type anti-corrosion impregnant, and the active components are emulsified to form stable emulsion in the dilution process by utilizing the emulsifying property of the aqueous organic silicon penetrating type anti-corrosion impregnant, so that the active components have better film forming property and sealing property, the hydrophobic modification effect on a base material is further improved, the dosage of the organic silicon components is reduced to a certain extent, the cost is reduced, and the aqueous organic silicon penetrating type anti-corrosion impregnant has good economy.
(3) The aqueous organosilicon permeation type antiseptic impregnant is stable pale yellow to light brown clear transparent organosilicon solution with high solid content, has self-emulsifying property, needs to be diluted by adding water when in use, can be freely adjusted according to the needs, can be dispersed in water to form stable colorless transparent to white emulsion without high-speed shearing and emulsification when in dilution and only needs stirring at a rotating speed of 500-1000 r/min, and has the advantages of low transportation cost, convenience in operation, long operable time and the like.
(4) The water-based organic silicon permeable type anti-corrosion impregnant has excellent waterproof performance, high reactivity and high permeability, can be used for impregnating stone, concrete, fabrics, paper, hydrophilic fibers, wood and other base materials, can also be used as an inorganic solid particle oleophilic modifier, an inorganic solid surface waterproof agent and other interface hydrophobic oleophilic modifier, has the functions of waterproof ventilation, antifouling self-cleaning, antibacterial mildew prevention, anti-permeability and anti-corrosion and the like, does not influence the appearance of the base material, does not change the surface color of the base material, does not generate oil spots and bright spots, and has good application prospect.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The raw materials used in the examples below were commercial industrial grade chemical raw materials unless specifically indicated, except that the alkyl silanol was freshly prepared.
Example 1
The aqueous organosilicon penetrating type anti-corrosive impregnant of the embodiment is prepared according to the following method:
136.222g (1.0 mol) of butyl silanol and 90.840g (0.2 mol) of dodecyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride solution (40% isopropyl alcohol solution) are respectively weighed, namely, the mol ratio of alkyl silanol to quaternized silane is 1:0.2, uniformly stirred at the rotating speed of 300r/min, and aged for 10d, so as to obtain the aqueous organosilicon permeable anti-corrosive impregnant. In this example, the amounts of ethyl silicate, water, active ingredient and curing agent added were all 0.
When in use, the emulsion is added into water and stirred uniformly, the stirring speed is 1000r/min, and when the mass ratio of the aqueous organosilicon permeable anti-corrosion impregnant to the water is 1:4, the milky emulsion with self-emulsifying property and coupling activity is obtained.
Example 2
The aqueous organosilicon penetrating type anti-corrosive impregnant of the embodiment is prepared according to the following method:
the method comprises the steps of weighing 192.329g (1.0 mol) of solution of octyl silanol (69.561% ethanol solution), 496.282g (1.0 mol) of solution of octadecyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride (60% isopropanol solution), 312.491g (1.5 mol) of ethyl orthosilicate and 36.030 (2.0 mol) of water, namely alkyl silanol, quaternized silane, ethyl silicate and water, stirring uniformly at a rotating speed of 1000r/min, ageing for 1d, adding 1452.126g of tung oil, namely the total mass ratio of the active component mass to the alkyl silanol solution, the quaternized silanol solution, the ethyl silicate and the water is 1:1, adding 29.043g of cobalt isooctanoate, namely the mass ratio of a curing agent to the active component is 2:100, and stirring uniformly to obtain the aqueous organic silicon penetrating impregnant.
When in use, the aqueous organosilicon permeable anti-corrosive impregnant is added into water and stirred uniformly, the stirring speed is 1000r/min, and when the mass ratio of the aqueous organosilicon permeable anti-corrosive impregnant to the water is 1:4, the white emulsion is obtained.
Example 3
The aqueous organosilicon penetrating type anti-corrosive impregnant of the embodiment is prepared according to the following method:
the solution containing 192.329g (1.0 mol) of octyl silanol (69.561% ethanol solution), the solution containing 248.141g (0.5 mol) of octadecyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride (60% isopropanol solution), 145.829g (0.7 mol) of ethyl orthosilicate, namely alkyl silanol, quaternized silane and ethyl silicate, were weighed respectively, the molar ratio of 1:0.5:0.7, stirred uniformly at a speed of 1000r/min, aged for 10d, 208.971g of octyl triethoxysilane, namely the ratio of the mass of the active component to the total mass of the alkyl silanol solution, the quaternized silane alcohol solution and the ethyl silicate was 0.25:1, and stirred uniformly to obtain the aqueous organosilicon penetrating type anti-corrosive impregnant.
When in use, the water-based organic silicon penetrating type anti-corrosion impregnant is added into water and stirred uniformly, the stirring speed is 500r/min, and when the mass ratio of the water-based organic silicon penetrating type anti-corrosion impregnant to the water is 1:4, the near-transparent blue-light emulsion is obtained.
The aqueous organosilicon penetrating type antiseptic impregnant obtained in this example can impregnate stone, concrete, fabric, paper, hydrophilic fiber, wood and other substrates, and the above examples 1,2 and 3 are 3 different impregnants developed for different substrates.
Wherein the aqueous organosilicon penetrating type anti-corrosive impregnant prepared in the embodiment 3 can be used for impregnating concrete, the concrete is taken as an example, the near-transparent blue-light emulsion prepared in the embodiment 3 is adopted, and C40 concrete is subjected to silane impregnation according to the current industry standard of anti-corrosive construction Specification of Water transportation engineering construction (JTS/T209-2020), 3 times of impregnation are carried out, and the usage amount of each time is 300mL/m 2 Through test, the penetration depth is 2.5mm, and the water is absorbedThe rate is less than or equal to 0.008mm/min 0.5 The other performance indexes also meet the standard requirements.
In summary, the application introduces the quaternary ammonium salt group with emulsifying property into the organic silicon molecule through condensation of the organic silicon quaternary ammonium salt and the alkyl silanol, so that the organic silicon molecule has self-emulsifying property, can be dispersed in water to form stable emulsion without adding any emulsifying agent, the concentration can be freely adjusted according to the requirement, and the organic silicon quaternary ammonium salt can be dispersed in water to form stable colorless transparent to white emulsion without high-speed shearing and emulsifying during dilution and only with stirring at the rotating speed of 500-1000 r/min, and has the advantages of low transportation cost, convenience in operation, long operation time and the like; through condensation of ethyl silicate and alkyl silanol, the functionality of the organosilicon molecules is improved, and the activity of coupling reaction between the organosilicon molecules and the surface of the substrate is improved, so that the organosilicon molecules are compactly arranged on the surface of the substrate and are compactly combined with the surface of the substrate, and the effect of hydrophobic modification is improved; through the synergistic effect of the condensation reaction, the stability of the aqueous organosilicon permeation type anti-corrosion impregnant and the water diluent thereof is improved, the reactivity is improved, the utilization rate of active groups is improved, and in addition, active components such as hydrogen-containing silicone oil, alkylalkoxysilane, drying oil, unsaturated monomers, prepolymers thereof or alcohol-soluble unsaturated resins and the like are added, and the components are emulsified together by means of the self-emulsifying property of organosilicon, so that the hydrophobic modification effect of the base material is further improved, the consumption of organosilicon components is reduced, the cost is reduced, and the method has good economical efficiency. The water-based organic silicon permeable type anti-corrosion impregnant has excellent waterproof performance, high reactivity and high permeability, can be used for impregnating stone, concrete, fabrics, paper, hydrophilic fibers, wood and other base materials, can also be used as an inorganic solid particle oleophilic modifier, an inorganic solid surface waterproof agent and other interface hydrophobic oleophilic modifier, has the functions of waterproof ventilation, antifouling self-cleaning, antibacterial mildew prevention, anti-permeability and anti-corrosion and the like, does not influence the appearance of the base material, does not change the surface color of the base material, does not generate oil spots and bright spots, and has good application prospect.
The above embodiments are only for illustrating the technical solution of the present application, not for limiting, and the present application is described in detail with reference to the preferred embodiments. It will be understood by those skilled in the art that various modifications and equivalent substitutions may be made to the technical solution of the present application without departing from the spirit and scope of the technical solution of the present application, and it is intended to cover within the scope of the claims of the present application.

Claims (12)

1. The aqueous organosilicon permeable anticorrosive impregnant is characterized by comprising an alkyl silanol solution, a quaternized silane alcohol solution, ethyl silicate, water, an active component and a curing agent;
the molar ratio of the alkyl silanol, the quaternized silane, the ethyl silicate and the water is 1: (0.2-1): (0-1.5): (0-2),
the ratio of the mass of the active component to the total mass of the solution of alkyl silanol, the alcoholic solution of quaternized silane, the ethyl silicate and the water is 0:1 to 1:1,
the ratio of the mass of the curing agent to the mass of the active component is 0: 100-2: 100;
the structural formula of the alkyl silanol is R m Si(OH) 4-m Or (HO) 3 Si(CH 2 ) n Si(OH) 3 And low molecular weight polycondensates thereof, wherein R represents a hydrocarbon group having 1 to 22 carbon atoms and a derivative thereof which is stable in a weakly acidic alcohol-water system and has neutral acid-base property to weakly acidic property and has hydrophobicity, m is 1 to 3, n is 1 to 22;
the quaternized silane is a silane coupling agent or oligomer thereof containing quaternary ammonium salt groups in the molecule and having the functionality of 2-3, and the structural formula is [ R ] 1 x (R 2 O) 3-x Si-(CH 2 ) y -N + (R 3 ) 2 -R 4 ]X - Wherein R is 1 And R is 4 All represent hydrocarbon groups of 1 to 22 carbon atoms and derivatives which are stable in a weakly acidic alcohol-water system, neutral in acid-base nature to weakly acidic and hydrophobic in nature, R 2 Represents an alkyl group having 1 to 3 carbon atoms, R 3 Represents a hydrocarbon group having 1 to 7 carbon atoms, x is 1 to 2, y is 1 to 8, and X is 1 to 8 - Represents a-1 valent anion;
the active components comprise: hydrogen-containing silicone oil, alkyl alkoxy silane, drying oil, unsaturated monomer, prepolymer thereof or alcohol-soluble unsaturated resin.
2. The aqueous organosilicon permeable corrosion protection impregnant according to claim 1, wherein the solution of the alkyl silanol is a clear and transparent homogeneous liquid, the pH value is 2-8, the mass fraction of the alkyl silanol is 40-100%, the aqueous organosilicon permeable corrosion protection impregnant is prepared by acid hydrolysis of alkyl alkoxy silane corresponding to the alkyl silanol, the hydrolysis system contains a solvent, if the hydrolysis adopts a solvent-free method, the solvent in the hydrolysis system is alcohol generated by alkoxy of the alkyl alkoxy silane corresponding to the alkyl silanol when the hydrolysis adopts a method with a reaction solvent, and the solvent in the hydrolysis system comprises: the alcohol generated by alkoxy and reaction solvent during the hydrolysis of alkyl alkoxy silane corresponding to alkyl silanol, and the reaction solvent can be low-toxicity water-miscible small-molecule volatile alcohol, ester, ether and ketone solvents, wherein the relation between the water used for the hydrolysis and the alkyl alkoxy silane corresponding to the alkyl silanol is that the mole number of the alkyl alkoxy silane corresponding to the alkyl silanol is less than or equal to the mole number of the water used for the hydrolysis and the mole number of alkoxy in the alkyl alkoxy silane corresponding to the alkyl silanol, and a hydrolysis system after the hydrolysis is used as a solution of the alkyl silanol or a solution of the alkyl silanol after partial solvent is removed by reduced pressure distillation.
3. The aqueous silicone-penetrating preservative impregnant according to claim 2, wherein the alkyl silanol comprises: any ratio mixture of one or more of dimethylsilanol, butylsilanol, cyclohexylsilanol, octylsilanol, decylsilanol, dodecylsilanol, octadecyl silanol, butylmethylsilanol, cyclohexylmethylsilanol, octylmethylsilanol, dodecylmethylsilanol, octadecylmethylsilanol, dibutylsilanol, dicyclohexylsilanol, dioctyl silanol, 3- (methacryloyloxy) propylsilanol, 1, 2-bis (trihydroxysilane) ethane or 1, 6-bis (trihydroxysilane) hexane;
and/or, the reaction solvent comprises: any ratio of one or more of methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, tert-butanol or ethylene glycol dimethyl ether.
4. The aqueous silicone-penetrating preservative impregnant according to claim 1, characterized in that X - Represents F - 、Cl - 、Br - 、NO 3 - 、ClO 4 - 、(SO 3 C 6 H 5 ) - 、(SO 3 C 7 H 7 ) - 、H 2 PO 4 - 、H 2 PO 3 - 、BF 4 - 、PF 6 - 、HPO 3 F - 、
Figure FDA0004230103540000021
(SO 4 C n H 2n+1 ) - 、(SO 3 C n H 2n-m+ 1 Y m ) - 、[PO 2 (OC n H 2n+1 ) 2 ] - 、/>
Figure FDA0004230103540000022
C n H 2n-m+1 Y m COO - 、NH 2 C n H 2n COO - Or HOC n H 2n COO - The method comprises the steps of carrying out a first treatment on the surface of the When said X - Representation (SO) 4 C n H 2n+1 ) - When the number n is more than or equal to 1 and less than or equal to 4; when said X - Representation (SO) 3 C n H 2n-m+1 Y m ) - N is more than or equal to 1 and less than or equal to 4, m is more than or equal to 0 and less than or equal to 2n+1, and Y is F or Cl; when said X - Representation [ PO ] 2 (OC n H 2n+1 ) 2 ] - When n is more than or equal to 1 and less than or equal to 3; when said X - Representation->
Figure FDA0004230103540000031
When n is more than or equal to 0 and less than or equal to 2; when said X - Is C n H 2n-m+1 Y m COO - When n is more than or equal to 0 and less than or equal to 4, m is more than or equal to 0 and less than or equal to 2n+1, and Y is F or Cl; when said X - Is NH 2 C n H 2n COO - Or HOC n H 2n COO - When the number n is more than or equal to 1 and less than or equal to 2.
5. The aqueous silicone-penetrating type antiseptic impregnant according to claim 4, wherein the alcohol used in the alcohol solution of quaternized silane is methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, tert-butanol, and the mass fraction of quaternized silane in the alcohol solution of quaternized silane is 40-100%.
6. The aqueous silicone-penetrating corrosion protection impregnant according to claim 3, wherein the quaternized silane comprises: any mixture of one or more of trimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, decyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, didecylmethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, dodecyl dimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, tetradecyldimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, hexadecyldimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride, or octadecyldimethyl [3- (trimethoxysilyl) propyl ] ammonium chloride.
7. The aqueous silicone penetrating type antiseptic impregnant according to claim 1, wherein the ethyl silicate is tetraethyl orthosilicate and low molecular weight polycondensate thereof, siO 2 The mass fraction is 28-50%.
8. The aqueous silicone-penetrating anticorrosive impregnant according to claim 1, characterized in that the hydrogen-containing silicone oil comprises: any ratio mixture of one or more of methyl hydrogen silicone oil, ethyl hydrogen silicone oil or phenyl hydrogen silicone oil;
and/or, the structural formula of the alkyl alkoxy silane is R 1 m Si(OR 2 ) 4-m Or (b)
(R 2 O) 3 Si(CH 2 ) n Si(OR 2 ) 3 And low molecular weight polycondensates thereof, wherein R 1 Represents a hydrocarbon group having 1 to 22 carbon atoms and a derivative which is stable in a weakly acidic alcohol-water system, has neutral acid-base properties to weakly acidic properties and has hydrophobicity, R 2 Represents alkyl with 1-3 carbon atoms, m is more than or equal to 1 and less than or equal to 3, and n is more than or equal to 1 and less than or equal to 22;
and/or, the drying oil comprises: any ratio of one or more of tung oil, catalpa oil and linseed oil;
and/or, the unsaturated monomer comprises: any ratio mixture of one or more of styrene, vinyl ester, vinyl ether, acrylate or methacrylate;
and/or, the alcohol-soluble unsaturated resin comprises: any ratio of one or more of unsaturated polyester resin, vinyl ester resin, polybutadiene resin or modified terpene resin.
9. The aqueous silicone-penetrating anticorrosive impregnant according to claim 7 or 8, characterized in that the alkylalkoxysilane comprises: methyl trimethoxysilane, methyl triethoxysilane, methyl tripropoxysilane, methyl triisopropoxysilane, chloromethyltrimethoxysilane, (dichloromethyl) trimethoxysilane, (trifluoromethyl) trimethoxysilane, dimethyl dimethoxy silane, trimethyl methoxy silane, ethyl methyl dimethoxy silane, cyanoethyl methyl dimethoxy silane, vinyl trimethoxysilane, phenyl trimethoxysilane, cyclopentyl trimethoxysilane, mercaptopropyl trimethoxysilane, acetoxypropyl trimethoxysilane, 3- (2, 3-epoxypropoxy) propyl triethoxysilane, 2- (3, 4-epoxycyclohexane) ethyl triethoxysilane, 3-methacryloxypropyl triethoxysilane, butyl triethoxysilane, octyl triethoxysilane, decyl triethoxysilane, dodecyl trimethoxysilane, octadecyl trimethoxysilane, tridecyl octyl trimethoxysilane, ethylene bis (trimethoxysilane), bis- [3- (trimethoxy) propyl ] disulfide, or bis- [3- (triethoxysilane) propyl ] tetrasulfide.
10. The aqueous silicone-penetrating anticorrosive impregnant according to claim 1, characterized in that the curing agent comprises: and a polymerization initiator and a promoter, a catalyst or a drier matched with the active component.
11. The aqueous silicone-penetrating anticorrosive impregnant according to claim 10, characterized in that the curing agent comprises: any ratio of mixtures of one or more of dioctyltin laurate, dibutyltin oxide, isopropyl tris (dioctyloxypyrophosphoyloxy) titanate, bis (dioctyloxypyrophosphato) ethylene titanate, tetraisopropyl bis (dioctylphosphoyloxy) titanate, 2-bis (allyloxymethyl) -1-butoxytris (dioctyloxypyrophosphoyloxy) titanate, or titanate coupling agent TC-27 suitable for catalyzing the crosslinking cure of alkylalkoxysilanes;
further comprises: any ratio of mixture of one or more of iron naphthenate, copper naphthenate, cobalt isooctanoate, zirconium isooctanoate or manganese isooctanoate suitable for catalyzing oxidative crosslinking and curing of drying oil;
further comprises: any ratio of the mixture of one or more of t-butyl hydroperoxide, di-t-butyl hydroperoxide, methyl ethyl ketone peroxide, methyl ethyl ketone-iso-octoate, benzoyl peroxide-N, N-dimethylaniline, ammonium persulfate or azobisisobutyronitrile suitable for initiating or catalyzing the free radical polymerization cure of unsaturated monomers and prepolymers or alcohol soluble unsaturated resins.
12. A process for the preparation of an aqueous organosilicon permeation type antiseptic impregnant according to claim 1 to 11,
weighing an alkyl silanol solution containing 1mol of alkyl silanol, a quaternized silane alcohol solution containing 0.2-1 mol of quaternized silane, 0-1.5 mol of ethyl silicate and 0-2 mol of water, uniformly stirring and aging;
adding an active component into the mixture, and uniformly stirring the mixture to obtain a mixed solution, wherein the ratio of the mass of the active component to the total mass of the alkyl silanol solution, the quaternized silane alcohol solution, the ethyl silicate and the water is 0:1-1:1;
weighing a curing agent, wherein the mass ratio of the curing agent to the active components is 0:100-2:100, adding the water-insoluble curing agent into the mixed solution and stirring uniformly, and adding the water-insoluble curing agent immediately after adding the active components and stirring uniformly, or adding the water-insoluble curing agent before use to obtain the water-based organic silicon permeable anti-corrosion impregnant, wherein the water-based organic silicon permeable anti-corrosion impregnant can be used by adding the water according to a certain proportion and stirring uniformly, and the stirring speed is 500-1000 r/min;
the water-soluble curing agent is not required to be added into the mixed solution, and is respectively stored in different containers with the mixed solution to be used as a matched combination, namely the water-based organic silicon permeation type anti-corrosion impregnant.
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