CN116355377A - Silane modified polyether resin material, preparation method thereof and grouting material - Google Patents

Silane modified polyether resin material, preparation method thereof and grouting material Download PDF

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Publication number
CN116355377A
CN116355377A CN202310349660.XA CN202310349660A CN116355377A CN 116355377 A CN116355377 A CN 116355377A CN 202310349660 A CN202310349660 A CN 202310349660A CN 116355377 A CN116355377 A CN 116355377A
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modified polyether
silane
resin material
polyether resin
prepolymer
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CN116355377B (en
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朱炜健
廖剑平
梅志强
谢标
周智
白玮
穆文庆
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China Railway Construction South China Construction Co Ltd
CRCC South China Construction Guangzhou High Tech Industry Co Ltd
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China Railway Construction South China Construction Co Ltd
CRCC South China Construction Guangzhou High Tech Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/02Polyalkylene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045Sulfates

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

The silane modified polyether resin material provided by the application enables the polyol, the diisocyanate and the catalyst to form a prepolymer on the basis of reasonable proportion of each component and each component in parts by weight, and meanwhile, the synergistic chain extender can ensure the diffusion extension of a molecular chain; under the cooperation of the latent curing agent, the silane modified polyether resin material can react with the prepolymer and the chain-extended prepolymer rapidly to form polyurea so as to make up the defect of low curing speed of the silane modified polyether, improve the curing speed of the silane modified polyether, and the polyurea chain segment has a certain reinforcing effect on the silane modified polyether material, so that the product performance reduction caused by the addition of the plasticizer can be avoided, and further the silane modified polyether resin material provided by the application has the advantages of high solid content, high elongation at break, high tensile strength and high curing speed.

Description

Silane modified polyether resin material, preparation method thereof and grouting material
Technical Field
The application relates to the field of building materials, in particular to a silane modified polyether resin material, a preparation method thereof and a grouting material.
Background
In various concrete construction projects, various cracks are commonly existed, and the existence of the cracks leads to the long-term existence of water leakage, thereby leading to the reduction of the service life of the concrete project. At present, the water hazard treatment in the construction engineering mainly adopts a mode of injecting chemical slurry.
The common plugging grouting material in the current market mainly comprises epoxy resin, polyurethane and acrylate. The epoxy resin grouting material has high strength after solidification, but has low elongation at break, and is easy to break and fracture in the process of stretching and expanding the crack along with the vibration of the subway rail. The polyurethane grouting material mainly comprises foaming polyurethane, and can react and expand rapidly after meeting water, and can stop water rapidly, but the polyurethane grouting material has exothermic reaction in the application process, and has the advantages of severe reaction, high speed, and large amount of heat generation, so that local cell ablation collapse is caused, the strength is influenced, and even safety accidents occur. The acrylate grouting material can be injected into the micro cracks, but the solid content of the acrylate grouting material is lower due to the adopted acrylate aqueous solution in the use process; and further, the grouting material is contracted to different degrees after being cured, and the contraction stress can cause the bonding damage of the grouting material and the concrete or the damage from the inside of the grouting material, so that the risk of re-leakage occurs.
Disclosure of Invention
Based on the above, the application provides a silane modified polyether resin material, a preparation method thereof and a grouting material. The silane modified polyether resin material has high solid content and larger elongation at break. Meanwhile, the adhesive has the advantages of high tensile strength and high curing speed.
In a first aspect of the present application, there is provided a silane modified polyether resin material, comprising the following raw material components in parts by weight:
Figure BDA0004161019630000021
in one embodiment, the structural formula of the silane-modified polyether is shown in the formulas (1) to (4):
Figure BDA0004161019630000022
Figure BDA0004161019630000031
wherein each m is independently an integer between 3 and 5; r is R 1 Selected from C1-C4 alkoxy or C1-C4 alkyl, R 2 Selected from C1-C4 alkoxy or C1-C4 alkyl,
Figure BDA0004161019630000032
selected from->
Figure BDA0004161019630000033
n and q are each independently integers of 30 to 2000.
In one embodiment, the diisocyanate comprises one or more of hexamethylene diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, and isophorone diisocyanate.
In one embodiment, the polyol has one or more of the following characteristics:
(1) The polyol includes one or more of a polyester polyol, a polyether polyol, and a polycarbonate polyol;
(2) The number average molecular weight of the polyol is 500-1000;
(3) The functionality of the polyol is 2 to 4.
In one embodiment, the catalyst comprises a first catalyst and a second catalyst;
the first catalyst comprises one or more of stannous octoate, bismuth laurate, bismuth isooctanoate and zinc neodecanoate;
the second catalyst comprises one or more of dibutyltin dilaurate, dibutyltin diacetylacetonate, and dibutyltin diacetylacetonate.
In one embodiment, the latent curing agent includes one or more of an imine-type latent curing agent and an oxazolidine-type latent curing agent.
In one embodiment, the silane modified polyether resin material has one or more of the following characteristics:
(1) The plasticizer comprises one or more of diisodecyl phthalate, diisononyl phthalate, dioctyl phthalate and dibutyl phthalate;
(2) The chain extender comprises one or more of ethylene glycol, ethylenediamine, butanediol or hexanediol.
In one embodiment, the silane modified polyether resin material further comprises the following raw material components in parts by weight:
4 to 8 parts of silane coupling agent,
4-8 parts of water scavenger
30-50 parts of filler;
optionally, the silane coupling agent comprises one or more of gamma-aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane;
optionally, the water scavenger comprises one or more of 3-butyl-2- (1-ethylpentyl) oxazolidine and vinyltrimethoxysilane;
optionally, the filler comprises one or more of calcium carbonate, magnesium carbonate, barium sulfate, and talc.
In one embodiment, the silane modified polyether resin material has one or more of the following characteristics:
(1) The tensile strength of the silane modified polyether resin material is more than or equal to 2.8MPa;
(2) The elongation at break of the silane modified polyether resin material is more than or equal to 450%;
(3) The solid content of the silane modified polyether resin material is more than or equal to 90%;
(4) The real-drying time of the silane modified polyether resin material is less than or equal to 2 hours.
In a second aspect of the present application, there is provided a method for preparing the silane-modified polyether resin material according to any one of the above embodiments, comprising the steps of:
carrying out prepolymerization reaction on the diisocyanate, the polyol and the catalyst to prepare a prepolymer;
adding the plasticizer and the chain extender into the prepolymer to prepare a chain-extended prepolymer;
and adding the silane modified polyether and the latent curing agent into the chain-extended prepolymer to prepare the silane modified polyether resin material.
In one embodiment, the process parameters of the prepolymerization reaction include: the reaction temperature is 60-90 ℃.
In one embodiment, the process parameters for preparing the chain extended prepolymer by adding a plasticizer and a chain extender to the prepolymer include: the reaction temperature is 10-25 ℃.
In a third aspect of the present application, there is provided a grouting material comprising the silane-modified polyether resin material according to any one of the first aspects of the present application.
The silane modified polyether resin material provided by the application can form a prepolymer by the polyol, the diisocyanate and the catalyst on the basis of reasonable proportion of each component in parts by weight, and meanwhile, the synergistic chain extender can ensure the diffusion extension of a molecular chain; under the coordination of the latent curing agent, the silane modified polyether resin material can react with the prepolymer and the chain-extended prepolymer rapidly to form polyurea so as to make up the defect of low curing speed of the silane modified polyether, improve the curing speed, and the polyurea chain segment has a certain reinforcing effect on the silane modified polyether material, so that the product performance reduction caused by the addition of the plasticizer can be avoided, and further the silane modified polyether resin material provided by the application has the advantages of high solid content, high elongation at break, high tensile strength and high curing speed.
Detailed Description
The silane-modified polyether resin material, the preparation method of the silane-modified polyether resin material, and the grouting material of the present application are further fully and clearly described below with reference to specific examples. This application may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
Herein, "one or more" refers to any one, any two, or any two or more of the listed items.
In this application, "first aspect," "second aspect," "third aspect," "fourth aspect," "fifth aspect," etc. are for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity, nor as implying an importance or quantity of a technical feature being indicated. Also, "first," "second," "third," "fourth," "fifth," etc. are for non-exhaustive list of descriptive purposes only and are not to be construed as limiting the number of closed forms.
In the present application, the technical features described in an open manner include a closed technical scheme composed of the listed features, and also include an open technical scheme including the listed features.
In the present application, reference is made to numerical intervals, where the numerical intervals are considered to be continuous unless specifically stated, and include the minimum and maximum values of the range, and each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
The percentage content referred to in the present application refers to mass percent for both solid-liquid and solid-solid phase mixing and volume percent for liquid-liquid phase mixing unless otherwise specified.
The percentage concentrations referred to in this application, unless otherwise indicated, refer to the final concentrations. The final concentration refers to the ratio of the additive component in the system after the component is added.
The temperature parameter in the present application is not particularly limited, and may be a constant temperature treatment or a treatment within a predetermined temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control.
In the present application, unless otherwise specified, "silane-modified polyether" refers to an organic compound in which the main chain of the structure is macromolecular polyether and the terminal group is a silane group containing a hydrolyzable group.
In this application, the term "alkyl" refers to a saturated hydrocarbon group containing a primary (positive) carbon atom, or a secondary carbon atom, or a tertiary carbon atom, or a quaternary carbon atom, or a combination thereof. Phrases containing this term, e.g., "C1-C4 alkyl "means an alkyl group containing 1 to 4 carbon atoms, and may be, independently of one another, C1 alkyl, C2 alkyl, C3 alkyl, C4 alkyl at each occurrence. Suitable examples include, but are not limited to: methyl (Me, -CH) 3 ) Ethyl (Et, -CH) 2 CH 3 ) 1-propyl (n-propyl, n-Pr, n-propyl, -CH 2 CH 2 CH 3 ) 2-propyl (i-Pr, i-propyl, -CH (CH) 3 ) 2 ) 1-butyl (n-butyl, n-Bu, n-butyl, -CH) 2 CH 2 CH 2 CH 3 ) 2-methyl-1-propyl (i-Bu, i-butyl, -CH) 2 CH(CH 3 ) 2 ) 2-butyl (s-Bu, s-butyl, -CH (CH) 3 )CH 2 CH 3 ) Tert-butyl (1, 1-dimethylethyl, t-Bu, t-butyl, -C (CH) 3 ) 3 )。
In this application, the term "alkoxy" refers to a group having an-O-alkyl group, i.e. an alkyl group as defined above, attached to the parent core structure via an oxygen atom. The phrase containing the term, for example, "C1-C4 alkoxy" means that the alkyl moiety contains from 1 to 4 carbon atoms, and each occurrence may be, independently of the other, C1 alkoxy, C2 alkoxy, C3 alkoxy, C4 alkoxy. Suitable examples include, but are not limited to: methoxy (-O-CH) 3 or-OMe), ethoxy (-O-CH 2 CH 3 or-OEt) and t-butoxy (-O-C (CH) 3 ) 3 or-OtBu).
The common grouting materials in the current market have various defects or shortages in comprehensive plugging performance, and cannot meet the target requirements. Meanwhile, the current silane modified polyether material is mainly applied to the field of home decoration, and the viscosity of the current silane modified polyether material in the use process is too high to be suitable for the field of grouting. The inventors of the present application have found, based on extensive experience and through extensive research, that the addition of a plasticizer is required to reduce the viscosity of the silane-modified polyether material, but the plasticizer tends to degrade the properties of the silane-modified polyether material, resulting in a slower cure rate. In order to solve the problems, the silane modified polyether is used as a main raw material, the raw materials such as the polyol, the diisocyanate, the chain extender and the latent curing agent are added, the polyol, the diisocyanate and the catalyst form a prepolymer in the production process, the molecular weight of the prepolymer is further prolonged in the presence of the chain extender, the latent curing agent is added, the prepolymer and the chain-extended prepolymer can be rapidly reacted to form polyurea, so that the defect of low curing speed of the silane modified polyether is overcome, the curing speed is improved, the polyurea chain segment has a certain reinforcing effect on the silane modified polyether material, the product performance reduction caused by the addition of the plasticizer can be avoided, and the silane modified polyether resin material provided by the application has the advantages of high solid content, high elongation at break, high tensile strength and high curing speed.
In a first aspect of the present application, there is provided a silane modified polyether resin material, comprising the following raw material components in parts by weight:
Figure BDA0004161019630000081
in one example, the silane-modified polyether has a structural formula shown in formulas (1) to (4):
Figure BDA0004161019630000082
Figure BDA0004161019630000091
wherein each m is independently an integer between 3 and 5; r is R 1 Selected from C1-C4 alkoxy or C1-C4 alkyl, R 2 Selected from C1-C4 alkoxy or C1-C4 alkyl,
Figure BDA0004161019630000092
selected from->
Figure BDA0004161019630000093
Figure BDA0004161019630000094
n and q are each independentlyAn integer between 30 and 2000. The curing speed of the silane modified polyether is slower, the main chain of the silane modified polyether is macromolecular polyether, the end group of the silane modified polyether is silane group or siloxane group containing a hydrolyzable group, the curing speed of the system can be regulated and controlled by regulating and controlling the hydrolysis rate of the terminal alkoxy of the silane modified polyether, meanwhile, the curing speed of the silane modified polyether can be synergistically improved by adding the latent curing agent, and in some specific examples, the curing time of the silane modified polyether is less than or equal to 2 hours.
In one example, the diisocyanate includes one or more of hexamethylene diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, and isophorone diisocyanate. The diisocyanate selected by the application basically does not generate side reaction with the polyol, can reduce the viscosity of the prepolymer, has stable property, and basically does not react with moisture, so that the prepared prepolymer has excellent adhesiveness.
In one example, the polyol includes one or more of a polyester polyol, a polyether polyol, and a polycarbonate polyol.
In one example, the number average molecular weight of the polyol is 500 to 1000.
In one example, the polyol has a functionality of 2 to 4. By limiting the functionality of the polyol, the speed of the prepolymerization can be controlled.
In one example, the catalyst includes a first catalyst and a second catalyst.
In one example, the first catalyst includes one or more of stannous octoate, bismuth laurate, bismuth isooctanoate, and zinc neodecanoate.
In one example, the second catalyst includes one or more of dibutyltin dilaurate, dibutyltin diacetylacetonate, and dibutyltin diacetylacetonate.
In one example, the latent curing agent includes one or more of an imine-type latent curing agent and an oxazolidine-type latent curing agent.
The imine-type latent curing agent used in the present application may be exemplified by an aromatic imine-type latent curing agent or an aliphatic amine-type latent curing agent.
The oxazolidine latent curing agent used in the present application may be exemplified by 3-hydroxyethyl-1, 3-oxazolidine, 2-isopropyl-3-hydroxyethyl-1, 3-oxazolidine or 2-phenyl-3-hydroxyethyl-1, 3-oxazolidine.
The latent curing agent can promote the rapid curing of the prepolymer and the chain-extended prepolymer, and can reduce foaming in the curing process; meanwhile, the addition of the latent curing agent is beneficial to improving the solid content of the silane modified polyether resin material and increasing the compatibility of each component in the silane modified polyether resin material.
In one example, the plasticizer includes one or more of diisodecyl phthalate, diisononyl phthalate, dioctyl phthalate, and dibutyl phthalate.
In one example, the chain extender includes one or more of ethylene glycol, ethylene diamine, butylene glycol, or hexylene glycol.
In one example, the silane modified polyether resin material further comprises the following raw material components in parts by weight:
4 to 8 parts of silane coupling agent,
4-8 parts of water scavenger
30-50 parts of filler.
In one example, the silane coupling agent includes one or more of gamma-aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane, and gamma- (methacryloyloxy) propyl trimethoxysilane.
In one example, the water scavenger includes one or more of 3-butyl-2- (1-ethylpentyl) oxazolidine and vinyltrimethoxysilane.
In one example, the filler includes one or more of calcium carbonate, magnesium carbonate, barium sulfate, and talc.
In one specific exampleWherein the filler comprises light calcium carbonate. The most obvious difference between heavy calcium carbonate and light calcium carbonate is the difference of bulk density of the products, the bulk density of the heavy calcium carbonate products is larger, and is generally 0.8-1.3 g/cm 3 The bulk density of the light calcium carbonate used in the application is less than 0.8g/cm 3
In one specific example, the silane modified polyether resin material comprises the following components in parts by weight:
Figure BDA0004161019630000111
Figure BDA0004161019630000121
in one example, the silane modified polyether resin material has a tensile strength of 2.8MPa or more.
In one example, the elongation at break of the silane modified polyether resin material is greater than or equal to 450%.
In one example, the solids content of the silane modified polyether resin material is greater than or equal to 90%.
In one example, the silane-modified polyether resin material has a dry time of 2h or less.
In one example, the silane-modified polyether resin material has a viscosity of 12000 mPa.s or less.
The silane modified polyether resin material provided by the application has the following excellent properties: (1) The solid content is more than or equal to 90%, and the silane modified polyether resin material provided by the application has high solid content, can ensure that the material does not shrink to different degrees after being solidified, and further has good waterproof performance; (2) The tensile strength is more than or equal to 2.8MPa, the elongation at break is more than or equal to 450%, and the silane modified polyether resin material provided by the application has excellent tensile strength and elongation at break, can avoid breaking and breaking of cracks in the process of stretching and retracting under vibration, and further prolongs the service time; (3) The viscosity is less than or equal to 12000 mPa.s, and the silane modified polyether resin material provided by the application has low viscosity and long working time, and can ensure full gap filling; (4) The bonding strength is more than or equal to 1.8MPa, and the silane modified polyether resin material provided by the application has high bonding strength, so that the grouting material and an interface can be tightly bonded; (5) the surface drying time is less than or equal to 60min, and the actual drying time is less than or equal to 120min; the silane modified polyether resin material provided by the application has short surface drying time and real drying time, and is favorable for construction.
In a second aspect of the present application, there is provided a method for preparing the silane-modified polyether resin material according to any one of the above embodiments, comprising the steps of:
carrying out prepolymerization reaction on the diisocyanate, the polyol and the catalyst to prepare a prepolymer;
adding the plasticizer and the chain extender into the prepolymer to prepare a chain-extended prepolymer;
and adding the silane modified polyether and the latent curing agent into the chain-extended prepolymer to prepare the silane modified polyether resin material.
In one example, the process of preparing the prepolymer by mixing the diisocyanate, the polyol and the catalyst includes the step of determining the mass fraction of NCO in the prepolymer.
In one example, the NCO mass fraction in the prepolymer is 10% to 15%.
It will be appreciated that the present application is not limited to a method for determining the NCO mass fraction. The method for determining the NCO mass fraction can be exemplified by titration.
In one example, the process parameters in the preparation of the prepolymer by mixing the diisocyanate, the polyol and the catalyst include: the reaction temperature is 60-90 ℃ and the reaction time is 2-4 h. In the process, the mass fraction of-NCO in the prepolymer can be sampled and measured, if the test value is higher than 15%, the reaction is continued until the mass fraction of NCO in the prepolymer is 10% -15%, namely the reaction end point; a plasticizer and a chain extender may be added to the prepolymer for the next step.
In one example, the process parameters of the prepolymerization reaction include: the reaction temperature is 60-90 ℃ and the reaction time is 2-4 h.
In one example, the process parameters for preparing the chain extended prepolymer by adding a plasticizer, a chain extender to the prepolymer include: the reaction temperature is 10-25 ℃; the reaction time is 0.5 h-2 h.
In one example, the step of adding the silane-modified polyether and the latent curing agent to prepare the silane-modified polyether resin material requires vacuum conditions.
In one specific example, the preparation method of the silane modified polyether resin material comprises the following steps:
s1, prepolymerization: taking polyol and diisocyanate in a three-neck flask, stirring uniformly, then heating slowly to 60-90 ℃ for reacting for 2-4 hours by using a first catalyst, and measuring the NCO mass fraction to prepare a prepolymer;
s2, chain extension: cooling the prepolymer to 10-25 ℃ by using ice water bath, adding a plasticizer and a chain extender, and reacting for 0.5-2 h to prepare a chain-extended prepolymer;
s3, mixing: heating the chain-extended prepolymer to 60 ℃, adding silane modified polyether and filler, and stirring for 0.5-1 h under vacuum condition; adding a silane coupling agent and a water scavenger, and stirring for 0.5-1 h under vacuum condition; and adding a latent curing agent, stirring for 0.5-1 h under vacuum condition, adding a second catalyst, stirring for 0.5-1 h under vacuum condition, and discharging under the protection of nitrogen gas to prepare the silane modified polyether resin material.
In a third aspect of the present application, there is provided a grouting material comprising the silane-modified polyether resin material according to any one of the first aspects of the present application.
The application of the silane modified polyether resin material provided by the application can be exemplified as the application in repairing road and tunnel pavement diseases; the method is applied to water conservancy and electric power facilities, mining resource exploitation, underground and underwater construction engineering waterproof treatment, maintenance, reinforcement or/and water leakage and water permeability fault emergency repair treatment.
The following are specific examples, and all materials used in the examples are commercially available products unless otherwise specified.
In the following examples:
polyether polyol: functionality is 2, number average molecular weight is 1000;
silane modified polyether resin:
Figure BDA0004161019630000141
wherein m is 3; r is R 1 Selected from C1 alkoxy, R 2 Selected from the group consisting of C1 alkoxy groups,
Figure BDA0004161019630000142
selected from the group consisting of
Figure BDA0004161019630000143
n is 800-1000.
Example 1
Embodiment 1 of the present application provides a silane modified polyether resin material and a preparation method thereof, which mainly comprises the following steps:
(1) 120 parts of polyether polyol and 30 parts of hexamethylene diisocyanate are taken in a three-neck flask, 1 part of bismuth laurate is added after stirring uniformly, the temperature is slowly raised to 80 ℃ for reaction for 3 hours, a prepolymer is prepared, the mass fraction of-NCO in the prepolymer is measured by sampling, the reaction is continued until the mass fraction of NCO in the prepolymer is 10% -15%, and the reaction is stopped.
(2) And (3) cooling the prepolymer prepared in the step (1) to 15 ℃ in an ice water bath, adding 50 parts of diisodecyl phthalate, adding 6 parts of ethylene glycol, and reacting for 1h to prepare the chain-extended prepolymer.
(3) Heating the chain-extended prepolymer prepared in the step (2) to 60 ℃, adding 300 parts of silane modified polyether resin and 50 parts of light calcium carbonate, and stirring for 1h under vacuum; adding 8 parts of gamma-aminopropyl triethoxysilane and 8 parts of vinyl trimethoxysilane, and stirring for 0.5h under vacuum; then adding 8 parts of imine latent curing agent and stirring for 0.5h under vacuum; and finally, adding 4 parts of dibutyltin dilaurate, stirring for 0.5h under the vacuum condition, discharging under the protection of nitrogen, sealing and packaging to prepare the silane modified polyether resin material.
Example 2
Embodiment 2 of the present application provides a silane modified polyether resin material and a preparation method thereof, which mainly comprises the following steps:
(1) Taking 80 parts of polyether polyol and 20 parts of hexamethylene diisocyanate in a three-neck flask, uniformly stirring, adding 1 part of bismuth laurate, slowly heating to 80 ℃ for reaction for 3 hours to prepare a prepolymer, sampling and measuring the mass fraction of-NCO in the prepolymer, and continuing the reaction until the mass fraction of NCO in the prepolymer is 10% -15%, and stopping the reaction.
(2) And (3) cooling the prepolymer prepared in the step (1) to 15 ℃ in an ice water bath, adding 30 parts of diisodecyl phthalate, adding 2 parts of ethylene glycol, and reacting for 1h to prepare the chain-extended prepolymer.
(3) Heating the chain-extended prepolymer prepared in the step (2) to 60 ℃, adding 200 parts of silane modified polyether and 50 parts of light calcium carbonate, and stirring for 1h under vacuum; adding 8 parts of gamma-aminopropyl triethoxysilane and 8 parts of vinyl trimethoxysilane, and stirring for 0.5h under vacuum; then adding 8 parts of imine latent curing agent and stirring for 0.5h under vacuum; and finally, adding 4 parts of dibutyltin dilaurate, stirring for 0.5h under the vacuum condition, discharging under the protection of nitrogen, sealing and packaging to prepare the silane modified polyether resin material.
Example 3
Embodiment 3 of the present application provides a silane modified polyether resin material and a preparation method thereof, which mainly comprises the following steps:
(1) Taking 80 parts of polyether polyol and 20 parts of toluene diisocyanate in a three-neck flask, uniformly stirring, adding 1 part of stannous octoate, slowly heating to 80 ℃ for reaction for 3 hours, preparing a prepolymer, sampling, measuring the mass fraction of-NCO in the prepolymer, and continuing the reaction until the mass fraction of NCO in the prepolymer is 10% -15%, and stopping the reaction.
(2) And (3) cooling the prepolymer prepared in the step (1) to 15 ℃ in an ice water bath, adding 30 parts of dibutyl phthalate, and then adding 2 parts of ethylenediamine, and reacting for 1h to prepare the chain-extended prepolymer.
(3) Heating the chain-extended prepolymer prepared in the step (2) to 60 ℃, adding 200 parts of silane modified polyether and 50 parts of barium sulfate, and stirring for 1h under vacuum; 8 parts of gamma-glycidoxypropyl trimethoxysilane and 8 parts of 3-butyl-2- (1-ethylpentyl) oxazolidine are added and stirred under vacuum for 0.5h; then adding 8 parts of oxazolidine latent curing agent and stirring for 0.5h under vacuum; and finally adding 4 parts of dibutyltin diacetylacetonate, stirring for 0.5h under the vacuum condition, discharging under the protection of nitrogen, sealing and packaging to prepare the silane modified polyether resin material.
Comparative example 1
(1) 120 parts of polyether polyol and 30 parts of hexamethylene diisocyanate are taken in a three-neck flask, 1 part of bismuth laurate is added after stirring uniformly, the temperature is slowly raised to 80 ℃ for reaction for 3 hours, a prepolymer is prepared, the mass fraction of-NCO in the prepolymer is measured by sampling, the reaction is continued until the mass fraction of NCO in the prepolymer is 10% -15%, and the reaction is stopped.
(2) And (3) cooling the prepolymer prepared in the step (1) to 15 ℃ in an ice water bath, adding 50 parts of diisodecyl phthalate, adding 6 parts of ethylene glycol, and reacting for 1h to prepare the chain-extended prepolymer.
(3) Heating the chain-extended prepolymer prepared in the step (2) to 60 ℃, adding 300 parts of amino-terminated polyether and 50 parts of light calcium carbonate, and stirring for 1h under vacuum; adding 8 parts of gamma-aminopropyl triethoxysilane and 8 parts of vinyl trimethoxysilane, and stirring for 0.5h under vacuum; then adding 8 parts of imine latent curing agent and stirring for 0.5h under vacuum; finally, 4 parts of dibutyltin dilaurate is added, stirred for 0.5h under the vacuum condition, discharged under the protection of nitrogen, sealed and packaged.
Comparative example 2
(1) 220 parts of polyether polyol and 80 parts of hexamethylene diisocyanate are taken in a three-neck flask, 1 part of bismuth laurate is added after stirring uniformly, the temperature is slowly raised to 80 ℃ for reaction for 3 hours, a prepolymer is prepared, the mass fraction of-NCO in the prepolymer is measured by sampling, the reaction is continued until the mass fraction of NCO in the prepolymer is 10% -15%, and the reaction is stopped.
(2) And (3) cooling the prepolymer prepared in the step (1) to 15 ℃ in an ice water bath, adding 50 parts of diisodecyl phthalate, adding 6 parts of ethylene glycol, and reacting for 1h to prepare the chain-extended prepolymer.
(3) Heating the chain-extended prepolymer prepared in the step (2) to 60 ℃, adding 150 parts of silane modified polyether and 50 parts of light calcium carbonate, and stirring for 1h under vacuum; adding 8 parts of gamma-aminopropyl triethoxysilane and 8 parts of vinyl trimethoxysilane, and stirring for 0.5h under vacuum; then adding 8 parts of imine latent curing agent and stirring for 0.5h under vacuum; finally, 4 parts of dibutyltin dilaurate is added, stirred for 0.5h under the vacuum condition, discharged under the protection of nitrogen, sealed and packaged.
The silane-modified polyether resin materials provided in examples and comparative examples of the present application were subjected to performance tests according to national standards. The test results are shown in table 1:
TABLE 1
Figure BDA0004161019630000171
Figure BDA0004161019630000181
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which facilitate a specific and detailed understanding of the technical solutions of the present application, but are not to be construed as limiting the scope of the invention. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. It should be understood that those skilled in the art, based on the technical solutions provided in the present application, can obtain technical solutions through logical analysis, reasoning or limited experiments, all fall within the protection scope of the claims attached in the present application. The scope of the patent application is therefore intended to be indicated by the appended claims, and the description may be used to interpret the contents of the claims.

Claims (13)

1. The silane modified polyether resin material is characterized by comprising the following raw material components in parts by weight:
Figure FDA0004161019620000011
2. the silane-modified polyether resin material according to claim 1, wherein the structural formula of the silane-modified polyether is represented by the formulae (1) to (4):
Figure FDA0004161019620000012
Figure FDA0004161019620000021
wherein each m is independently an integer between 3 and 5; r is R 1 Selected from C1-C4 alkoxy or C1-C4 alkyl, R 2 Selected from C1-C4 alkoxy or C1-C4 alkyl,
Figure FDA0004161019620000022
selected from->
Figure FDA0004161019620000023
n and q are each independently integers of 30 to 2000.
3. The silane-modified polyether resin material according to claim 1, wherein said diisocyanate comprises one or more of hexamethylene diisocyanate, toluene diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate and isophorone diisocyanate.
4. The silane-modified polyether resin material of claim 1, wherein said polyol has one or more of the following characteristics:
(1) The polyol includes one or more of a polyester polyol, a polyether polyol, and a polycarbonate polyol;
(2) The number average molecular weight of the polyol is 500-1000;
(3) The functionality of the polyol is 2 to 4.
5. The silane-modified polyether resin material of claim 1, wherein said catalyst comprises a first catalyst and a second catalyst;
the first catalyst comprises one or more of stannous octoate, bismuth laurate, bismuth isooctanoate and zinc neodecanoate;
the second catalyst comprises one or more of dibutyltin dilaurate, dibutyltin diacetylacetonate, and dibutyltin diacetylacetonate.
6. The silane-modified polyether resin material according to claim 1, wherein said latent curing agent comprises one or more of an imine-type latent curing agent and an oxazolidine-type latent curing agent.
7. The silane-modified polyether resin material of claim 1, wherein said silane-modified polyether resin material has one or more of the following characteristics:
(1) The plasticizer comprises one or more of diisodecyl phthalate, diisononyl phthalate, dioctyl phthalate and dibutyl phthalate;
(2) The chain extender comprises one or more of ethylene glycol, ethylenediamine, butanediol or hexanediol.
8. The silane-modified polyether resin material according to claim 1, further comprising the following raw material components in parts by weight:
4 to 8 parts of silane coupling agent,
4-8 parts of water scavenger
30-50 parts of filler;
optionally, the silane coupling agent comprises one or more of gamma-aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane;
optionally, the water scavenger comprises one or more of 3-butyl-2- (1-ethylpentyl) oxazolidine and vinyltrimethoxysilane;
optionally, the filler comprises one or more of calcium carbonate, magnesium carbonate, barium sulfate, and talc.
9. The silane-modified polyether resin material according to any one of claims 1 to 8, characterized in that said silane-modified polyether resin material has one or more of the following characteristics:
(1) The tensile strength of the silane modified polyether resin material is more than or equal to 2.8MPa;
(2) The elongation at break of the silane modified polyether resin material is more than or equal to 450%;
(3) The solid content of the silane modified polyether resin material is more than or equal to 90%;
(4) The real-drying time of the silane modified polyether resin material is less than or equal to 2 hours.
10. A method for producing the silane-modified polyether resin material according to any one of claims 1 to 9, comprising the steps of:
carrying out prepolymerization reaction on the diisocyanate, the polyol and the catalyst to prepare a prepolymer;
adding the plasticizer and the chain extender into the prepolymer to prepare a chain-extended prepolymer;
and adding the silane modified polyether and the latent curing agent into the chain-extended prepolymer to prepare the silane modified polyether resin material.
11. The method for preparing a silane-modified polyether resin material according to claim 10, wherein the process parameters of the prepolymerization reaction include: the reaction temperature is 60-90 ℃.
12. The method for producing a silane-modified polyether resin material according to claim 10 or 11, wherein the process parameters for producing a chain-extended prepolymer by adding a plasticizer and a chain extender to the prepolymer include: the reaction temperature is 10-25 ℃.
13. A grouting material comprising the silane-modified polyether resin material according to any one of claims 1 to 9.
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