CN116355377B - 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

Info

Publication number
CN116355377B
CN116355377B CN202310349660.XA CN202310349660A CN116355377B CN 116355377 B CN116355377 B CN 116355377B CN 202310349660 A CN202310349660 A CN 202310349660A CN 116355377 B CN116355377 B CN 116355377B
Authority
CN
China
Prior art keywords
modified polyether
silane
resin material
polyether resin
prepolymer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202310349660.XA
Other languages
Chinese (zh)
Other versions
CN116355377A (en
Inventor
朱炜健
廖剑平
梅志强
谢标
周智
白玮
穆文庆
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Railway Construction South China Construction Co Ltd
CRCC South China Construction Guangzhou High Tech Industry Co Ltd
Original Assignee
China Railway Construction South China Construction Co Ltd
CRCC South China Construction Guangzhou High Tech Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Railway Construction South China Construction Co Ltd, CRCC South China Construction Guangzhou High Tech Industry Co Ltd filed Critical China Railway Construction South China Construction Co Ltd
Priority to CN202310349660.XA priority Critical patent/CN116355377B/en
Publication of CN116355377A publication Critical patent/CN116355377A/en
Application granted granted Critical
Publication of CN116355377B publication Critical patent/CN116355377B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

The silane modified polyether resin material provided by the application enables polyol, diisocyanate and 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 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 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 degradation 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, large elongation at break, large 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.
The application provides a silane modified polyether resin material, which comprises the following raw material components in parts by weight:
in one embodiment, the structural formula of the silane-modified polyether is shown in the formulas (1) to (4):
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,selected from the group consisting ofn 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 to 8 parts of water scavenger and
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 aspect 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 modified polyether can react with the prepolymer and the chain-extended prepolymer rapidly to form polyurea so as to make up for the defect of low curing speed of 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 degradation 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, large elongation at break, large 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 described more fully and clearly below with reference to specific examples. The present 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 the present 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 technical features 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 application, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present application, the numerical ranges are referred to as continuous, and include the minimum and maximum values of the ranges, and each value between the minimum and maximum values, unless otherwise specified. 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 percentage for both solid-liquid mixing and solid-solid mixing and volume percentage for liquid-liquid mixing unless otherwise specified.
The percentage concentrations referred to in the present application refer to the final concentrations unless otherwise specified. 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" means 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 the present 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. The phrase containing the term, for example, "C1-C4 alkyl" refers to an alkyl group containing 1 to 4 carbon atoms, which may be, for each occurrence, independently of one another, C1 alkyl, C2 alkyl, C3 alkyl, C4 alkyl. 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 the present 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 inventor of the present application has found, based on abundant 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 curing speed. In order to solve the problems, the silane modified polyether is taken 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, a certain reinforcing effect of a polyurea chain segment on the silane modified polyether material is realized, 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, large elongation at break, high tensile strength and high curing speed.
The application provides a silane modified polyether resin material, which comprises the following raw material components in parts by weight:
in one example, the silane-modified polyether has a structural formula shown in formulas (1) to (4):
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, and (2)>Selected from-> n and q are each independently integers of 30 to 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 to 8 parts of water scavenger and
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 example, 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 adopted by 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:
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, and can avoid breaking and breaking of cracks in the process of stretching and retracting under vibration, so that the service time is prolonged; (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, and can ensure that grouting materials are tightly bonded with interfaces; (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 beneficial to 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 application is not limited to a method of 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 aspect of the present application.
The silane modified polyether resin material provided by the application can be applied to 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:
wherein m is 3; r is R 1 Selected from C1 alkoxy, R 2 Selected from the group consisting of C1 alkoxy groups,selected from the group consisting ofn is 800-1000.
Example 1
The embodiment 1 of the application provides a silane modified polyether resin material and a preparation method thereof, and the silane modified polyether resin material 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
The embodiment 2 of the application provides a silane modified polyether resin material and a preparation method thereof, and the silane modified polyether resin material 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
The embodiment 3 of the application provides a silane modified polyether resin material and a preparation method thereof, and the silane modified polyether resin material 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 the 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
/>
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 application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. It should be understood that, based on the technical solutions provided by the present application, those skilled in the art may obtain technical solutions through logical analysis, reasoning or limited experiments, which are all within the scope of protection of the appended claims. The scope of the patent of the application should therefore be determined with reference to the appended claims, which are to be construed as in accordance with the doctrines of claim interpretation.

Claims (10)

1. A preparation method of a silane modified polyether resin material is characterized in that,
the silane modified polyether resin material comprises the following raw material components in parts by weight:
wherein the structural formula of the silane modified polyether is shown as a formula (1):
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,selected from the group consisting ofn and q are each independently integers of 30 to 2000;
the polyol includes one or more of a polyester polyol, a polyether polyol, and a polycarbonate polyol;
the catalyst comprises 0.5-1 part of a first catalyst and 2-4 parts of a second catalyst by weight; 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 dibutyl tin dilaurate, dibutyl tin diacetylacetonate and dibutyl tin diacetylacetonate;
the latent curing agent comprises one or more of an imine type latent curing agent and an oxazolidine type latent curing agent;
the preparation method comprises the following steps:
carrying out prepolymerization reaction on the diisocyanate, the polyol and the first 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, the latent curing agent and the second catalyst into the chain-extended prepolymer to prepare the silane modified polyether resin material.
2. The method for producing a 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.
3. The method of preparing a silane-modified polyether resin material according to claim 1, wherein said polyol has one or more of the following characteristics:
(1) The number average molecular weight of the polyol is 500-1000;
(2) The functionality of the polyol is 2 to 4.
4. The method of preparing a silane-modified polyether resin material according to 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.
5. The method for preparing a silane-modified polyether resin material according to claim 1, wherein 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 to 8 parts of water scavenger and
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.
6. The method for preparing a silane-modified polyether resin material according to claim 1, wherein the process parameters of the prepolymerization reaction include: the reaction temperature is 60-90 ℃.
7. The method for producing a silane-modified polyether resin material according to any one of claims 1 to 6, wherein the process parameters for producing a chain-extended prepolymer by adding a plasticizer and a chain extender to said prepolymer include: the reaction temperature is 10-25 ℃.
8. A silane-modified polyether resin material characterized by being prepared by the preparation method according to any one of claims 1 to 7.
9. The silane-modified polyether resin material of claim 8, wherein 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 grouting material comprising the silane-modified polyether resin material according to claim 8 or 9.
CN202310349660.XA 2023-04-04 2023-04-04 Silane modified polyether resin material, preparation method thereof and grouting material Active CN116355377B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310349660.XA CN116355377B (en) 2023-04-04 2023-04-04 Silane modified polyether resin material, preparation method thereof and grouting material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310349660.XA CN116355377B (en) 2023-04-04 2023-04-04 Silane modified polyether resin material, preparation method thereof and grouting material

Publications (2)

Publication Number Publication Date
CN116355377A CN116355377A (en) 2023-06-30
CN116355377B true CN116355377B (en) 2023-11-03

Family

ID=86920691

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310349660.XA Active CN116355377B (en) 2023-04-04 2023-04-04 Silane modified polyether resin material, preparation method thereof and grouting material

Country Status (1)

Country Link
CN (1) CN116355377B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107022333A (en) * 2017-04-19 2017-08-08 常熟市恒信粘胶有限公司 Silane-terminated polyether modified structure fluid sealant
CN107033827A (en) * 2017-03-28 2017-08-11 苏州正硅防水科技有限公司 A kind of single component silane modified polyether seal glue for building and preparation method thereof
CN111574950A (en) * 2020-06-08 2020-08-25 厦门韦尔通科技有限公司 Ultra-soft silane modified polyether adhesive with buffering performance and preparation method thereof
CN113527629A (en) * 2021-06-15 2021-10-22 深圳市百丽春粘胶实业有限公司 High-weather-resistance high-performance modified polyether resin and sealant for building exterior wall
CN114015036A (en) * 2021-11-01 2022-02-08 三棵树(上海)新材料研究有限公司 Low-viscosity silane modified polyether resin and preparation method thereof
CN115725046A (en) * 2022-12-14 2023-03-03 上海东大化学有限公司 Yellowing-resistant silane modified polyurethane resin and preparation method thereof, and MS sealant and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107033827A (en) * 2017-03-28 2017-08-11 苏州正硅防水科技有限公司 A kind of single component silane modified polyether seal glue for building and preparation method thereof
CN107022333A (en) * 2017-04-19 2017-08-08 常熟市恒信粘胶有限公司 Silane-terminated polyether modified structure fluid sealant
CN111574950A (en) * 2020-06-08 2020-08-25 厦门韦尔通科技有限公司 Ultra-soft silane modified polyether adhesive with buffering performance and preparation method thereof
CN113527629A (en) * 2021-06-15 2021-10-22 深圳市百丽春粘胶实业有限公司 High-weather-resistance high-performance modified polyether resin and sealant for building exterior wall
CN114015036A (en) * 2021-11-01 2022-02-08 三棵树(上海)新材料研究有限公司 Low-viscosity silane modified polyether resin and preparation method thereof
CN115725046A (en) * 2022-12-14 2023-03-03 上海东大化学有限公司 Yellowing-resistant silane modified polyurethane resin and preparation method thereof, and MS sealant and preparation method thereof

Also Published As

Publication number Publication date
CN116355377A (en) 2023-06-30

Similar Documents

Publication Publication Date Title
CN106675373B (en) A kind of uncured polyurethane water-proof paint and preparation method thereof
CN101220203B (en) Polyurethane chemical grouting material and production method
CN104974332B (en) It is a kind of to cure high-strength polyurethane plugging watertight grouting material soon without foaming
CN106634547B (en) A kind of one-component exposed conveying appliance acrylic acid modified polyurethane water-repellent paint and preparation method
CN101818045A (en) Two-component polyurethane sealant
CN104292412A (en) Cellulose base polyurethane prepolymer as well as sealing material using cellulose base polyurethane prepolymer, preparation method and application of cellulose base polyurethane prepolymer
CN101987940A (en) Method for preparing high-performance single-component polyurethane waterproof coating
CN103012712B (en) Method for preparing organic and inorganic hybridization modified polyurethane chemical grouting material
CN111690250A (en) Low-viscosity silicate reinforcing material and preparation method and application thereof
CN111518476A (en) Polyurethane modified asphalt-based non-cured waterproof coating and preparation method and application thereof
CN104559137B (en) High resiliency no-solvent polyurethane loss circulation material and preparation method and application
CN111978850A (en) Silane modified waterproof coating and preparation method thereof
CN116355377B (en) Silane modified polyether resin material, preparation method thereof and grouting material
CN111303366A (en) Halogen-free flame-retardant organic polymer grouting reinforcement material and preparation method thereof
CN109385256A (en) Coal mine glass composite polyurethane water reinforcement material and preparation method thereof
CN108715682B (en) Mining organic reinforcing material and preparation method thereof
CN104861143B (en) A kind of room curing and high temperature resistant polyurethane sealing material and preparation method thereof
CN115160914B (en) Single-component polyurethane waterproof coating special for waterproof repairing engineering of back water surface
CN102850506B (en) Preparation method of polyurethane modified asphalt
CN106753045A (en) A kind of polyurethane-modified high temperature resistant pressure sensitive adhesive and preparation method thereof
CN115322724A (en) Environment-friendly high-low temperature impact-resistant weather-resistant bi-component polyurethane potting sealant and preparation method thereof
CN111057461B (en) Preparation method of single-component water-curing polyurethane waterproof coating
CN107298961A (en) A kind of power system insulation water-proof seal glue
CN114015345A (en) Anti-sagging polyurethane waterproof coating of water curing system and preparation method thereof
CN115246919B (en) Polyurethane grouting material and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant