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CN117304441A - High-elasticity biliquid grouting material for plugging and preparation method thereof - Google Patents

High-elasticity biliquid grouting material for plugging and preparation method thereof Download PDF

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Publication number
CN117304441A
CN117304441A CN202311111556.3A CN202311111556A CN117304441A CN 117304441 A CN117304441 A CN 117304441A CN 202311111556 A CN202311111556 A CN 202311111556A CN 117304441 A CN117304441 A CN 117304441A
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China
Prior art keywords
component
grouting material
elasticity
parts
plugging
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CN202311111556.3A
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Inventor
韦代东
李士强
李惠枝
曾娟娟
古伟斌
邓淑玲
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Guangzhou Chemical Grouting Co ltd Cas
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Guangzhou Chemical Grouting Co ltd Cas
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Priority to CN202311111556.3A priority Critical patent/CN117304441A/en
Publication of CN117304441A publication Critical patent/CN117304441A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/302—Water
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/54—Polycondensates of aldehydes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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    • C08K3/20—Oxides; Hydroxides
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
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    • C08K2003/2241—Titanium dioxide

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  • Polymers & Plastics (AREA)
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  • Sealing Material Composition (AREA)

Abstract

The invention discloses a high-elasticity biliquid grouting material for plugging, which comprises the following components in parts by weight: 82-94 parts of active prepolymer, 6-18 parts of alpha-silane modified polymer, 2-3 parts of vinyl trimethoxy silane, 55-65 parts of tackifying resin solution, 5-15 parts of triethylene diamine aqueous solution, 5-15 parts of polyaspartic acid ester resin, 45-55 parts of composite filler, 3-6 parts of titanium dioxide, 0.3-0.6 part of high pigment carbon black, 0.3-0.7 part of antioxidant, 0.3-0.7 part of ultraviolet absorber, 0.3-0.1 part of defoamer, 0.3-0.7 part of anti-settling agent and 1-3 parts of aminosilane coupling agent. The invention also discloses a preparation method of the high-elasticity biliquid grouting material, which leads the material to have the advantage of double solidification by introducing the active prepolymer containing isocyanate groups and the alpha-silane modified polymer, realizes priming-free bonding and is beneficial to improving the wet bonding strength.

Description

High-elasticity biliquid grouting material for plugging and preparation method thereof
Technical Field
The invention relates to the field of waterproof plugging, in particular to a high-elasticity biliquid grouting material for plugging and a preparation method thereof.
Background
In the field of waterproof and leaking stoppage, a certain amount of inorganic or organic materials are prepared into a true solution, and the true solution is poured into a stratum or a gap by power equipment such as a grouting pump to form an effective gel or a solidified body, so that the physical and mechanical properties of a poured body are improved, and the waterproof and leaking stoppage effect is achieved.
In recent years, urban rail transit in China is rapidly developed, and subways become a main line of an urban rail transit transportation system, so that great convenience is provided for urban residents to travel. Along with the increase of the operation years of subways, the main concrete structure generates large-area water leakage diseases and diseases, and the appearance and the service life of the structure are directly and adversely affected. The deformation joint is the place where the subway leakage water most frequently occurs, and is also a difficult problem facing the underground plugging reinforcement for a long time. The leakage water of the reinforced concrete cracks is usually grouted and blocked by adopting polyurethane grouting material, so that the effects of quick blocking and water stopping can be achieved. Polyurethane grouting material, especially oil-soluble polyurethane grouting material, reacts with water in grouting process to rapidly generate a large amount of CO 2 Forming 10-20 times of foam body, expanding and filling cracks, and achieving the purpose of water stop. However, the high expansibility may be secondary failure of the structure, and the existence of communicating pores in the rigid foam-like consolidated body results in poor water-resistant permeability, inelastic, inability to adapt to the swelling and shrinkage deformation of the crack, and severe rethreading. Therefore, the polyurethane grouting material in the prior art is only suitable for being used as a temporary water shutoff material, solves the problem of diseases in a short period of time, and cannot be used as a durable water shutoff material.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the high-elasticity biliquid grouting material for plugging, and solve the problem of poor durability of the existing plugging material.
The invention further aims to provide a preparation method of the high-elasticity biliquid grouting material for plugging.
The aim of the invention is achieved by the following technical scheme:
the high-elasticity biliquid grouting material for plugging comprises an A component and a B component, wherein the A component comprises the following components in parts by weight:
82-94 parts of active prepolymer;
6-18 parts of alpha-silane modified polymer;
2-3 parts of vinyl trimethoxy silane;
the component B comprises the following components in parts by weight:
preferably, the reactive prepolymer has the following structural formula:
wherein R is 1 -NCO is Is->
Preferably, the alpha-silane modified polymer is commercially available as GENIOSIL STP-E10 (watts).
Preferably, the polyaspartic acid ester resin comprises F420, F520, or a combination thereof.
Preferably, the titanium dioxide comprises commercially available rutile titanium dioxide NR9503, NR960 (Nanjing titanium dioxide) or a combination thereof.
Preferably, the high pigment carbon black comprises commercially available MA-100, MA-11 (Mitsubishi Japanese), or combinations thereof.
Preferably, the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (antioxidant 1010).
Preferably, the concentration of the triethylenediamine aqueous solution is 4-7%.
Preferably, the tackifying resin solution comprises the following components in percentage:
preferably, the composite filler comprises calcium hydroxide, talc or a combination thereof.
More preferably, the composite filler is a combination of 800 mesh calcium hydroxide and 1250 mesh talc.
More preferably, the mass ratio of the calcium hydroxide to the talcum powder is 3:2.
preferably, the ultraviolet light absorber comprises 2-hydroxy-4-n-octoxybenzophenone (UV-531), tinuvin B75 (Basoff), or a combination thereof.
More preferably, the ultraviolet absorber is 2-hydroxy-4-n-octoxybenzophenone (UV-531).
Preferably, the defoamer comprises a hydrophobic particle polysiloxane compound, a foam breaking polysiloxane solution, or a combination thereof, wherein the hydrophobic particle polysiloxane compound is commercially available as Defom-6800 (Hammingnsted), and the foam breaking polysiloxane solution is commercially available as BYK-066N (Pick).
More preferably, the antifoaming agent is commercially available Defom-6800 (Hamming court).
Preferably, the anti-settling agent comprises a modified urea solution, a modified polyurea solution, or a combination thereof; the modified urea solution is commercially available BYK-410 (Pick), and the modified urea solution is commercially available BYK-420 (Pick).
More preferably, the anti-settling agent is BYK-410 (Pick).
Preferably, the aminosilane coupling agent comprises N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane (KH-792), 3-aminopropyl trimethoxysilane (KH-540), or a combination thereof.
Preferably, the aminosilane coupling agent is N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane (KH-792).
The preparation method of the high-elasticity biliquid grouting material for plugging comprises the following specific steps:
(1) Respectively vacuumizing and dehydrating polyether glycol and polyether triol at 110-120 ℃; mixing dehydrated polyether triol and acetyl tributyl citrate, heating, dropwise adding toluene diisocyanate, reacting under the condition of nitrogen, adding polyether diol and dibutyl tin dilaurate, continuously heating for reaction, and vacuumizing to obtain an active prepolymer;
(2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane, and then sealing and preserving to obtain a component A;
(3) Adding the tackifying resin solution, the triethylene diamine aqueous solution, the polyaspartic acid ester resin, the defoaming agent and the aminosilane coupling agent into a container, and mechanically stirring to obtain uniform mixed solution; adding composite filler, titanium dioxide, high pigment carbon black, antioxidant and ultraviolet absorbent into the mixed solution, stirring and dispersing uniformly, adding anti-settling agent, continuing stirring, subpackaging the dispersed fluid, and sealing and preserving to obtain component B.
Preferably, the A and B components are injected into the fracture at the time of use.
More preferably, the volume ratio of the A component to the B component is 1:1.
Compared with the prior art, the invention has the following advantages:
(1) According to the high-elasticity biliquid grouting material for plugging, the active prepolymer containing isocyanate groups and the alpha-silane modified polymer are introduced, so that the material has the advantage of dual solidification. The curing of the reactive prepolymer forms a gel with low modulus and high elasticity, and the moisture curing of the alpha-silane modified polymer has good adhesion to a wide range of substrates, can realize primer-free adhesion, and is beneficial to improving the wet adhesion strength.
(2) The invention provides a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following components in percentage by volume: 1, grouting is carried out without weighing and slurry preparation, and the operation is convenient. After the component A and the component B are mixed, the isocyanate groups of the active prepolymer react with the polyaspartic acid ester resin, water and aldehyde ketone resin immediately and rapidly to form a polyurea-polyurethane gel crosslinked network structure with low modulus and high elasticity. The amino group of the aminosilane coupling agent not only participates in the curing of the reactive prepolymer, but also reacts with the alpha-silane modified polymer in a crosslinking manner. In addition, the aminosilane coupling agent and the hydroxyl on the surface of the concrete form covalent bond connection through condensation, so that the grouting material and a poured interface are connected into a whole, and the bonding strength of the grouting material is further improved.
(3) The high-elasticity biliquid grouting material for plugging provided by the invention is not dispersed in water, and can squeeze out and discharge water in cracks. The grouting material is fast in solidification, the solidification speed is not influenced by humidity and thickness of the grouting material, gel can be controlled within 10min, surface drying is controlled within 30min, elongation at break is greater than 1500%, tensile modulus is less than 0.3MPa, elastic recovery rate is 95%, bonding strength of a dry base surface is 1.58MPa, and bonding strength of a wet base surface can reach 1.30MPa. The cured high-elasticity gel with low modulus is not foamed, does not shrink and has compact inside, has good bonding strength to concrete and other substrates, meets the subway plugging requirements of strong vibration and large deformation, and solves the problem of poor durability of the existing polyurethane grouting material.
The principle of the invention is as follows:
the low-modulus high-elasticity active prepolymer is prepared by the polyether with low unsaturation degree and high molecular weight, so that the component A not only has isocyanate groups, but also introduces an alpha-silane modified polymer, and the material has the advantage of dual curing.
One of the curing mechanisms is as follows: the isocyanate groups in the reactive prepolymer react with water in the component B to form a high-elasticity polyurea structure; reacting the isocyanate groups with the polyaspartic acid ester resin to form a high-toughness polyurea structure; reacting the isocyanate group with the hydroxyl group of the aldehyde ketone resin to form a polyurethane structure; furthermore, the isocyanate group also reacts with amino (-NH 2 and-NH) of the aminosilane coupling agent, the alkoxy of the aminosilane coupling agent reacts with the siloxane of the alpha-silane modified polymer in a crosslinking way, the aminosilane coupling agent and the hydroxyl on the surface of the concrete form covalent bond connection through condensation, the grouting material and the interface to be grouting are connected into a whole, and the bonding strength of the grouting material is further improved.
The second curing mechanism is as follows: the alkoxy at the tail end of the alpha-silane modified polymer is hydrolyzed and condensed with moisture to form a stable three-dimensional network structure of siloxane Si-O-Si, the high-activity silane end capped polyether has strong induction effect of carbamate groups because the electron donating group and the alkoxy are separated by only 1 carbon atom, has alpha-effect, greatly accelerates the hydrolysis/condensation reaction activity of siloxane, can be quickly solidified without a catalyst, has good adhesion to a wide range of substrates, can realize primer-free adhesion, and improves the wet adhesion strength.
Calcium hydroxide and CO in the B component 2 Is capable of absorbing CO generated by the reaction of isocyanate groups with water 2 And the gas ensures that the grouting material does not expand and form air holes in the curing process.
Drawings
FIG. 1 is a block diagram of an alpha-silane modified polymer.
FIG. 2 is a diagram of the reaction mechanism for preparing a reactive prepolymer.
FIG. 3 is a graph of the internal topography of the slurry of example 8 after solidification.
Detailed Description
The present invention will be described in further detail with reference to the drawings and specific examples, which are not to be construed as limiting the embodiments of the present invention.
Example 1
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. the preparation of the active prepolymer comprises the following steps:
(a) Respectively vacuumizing and dehydrating polyether glycol DL-1000D and polyether triol EP-3600 at 115 ℃ by using a vacuum pump for 2 hours, and cooling for standby.
(b) 35.82g of the polyether triol EP-3600 treated in the step (a) and 4.81g of acetyl tributyl citrate are put into a three-neck flask, the temperature is raised to 60 ℃, 6.90g of toluene diisocyanate is added dropwise, and the reaction is carried out for 2.5h under the nitrogen condition. Then 13.05g of polyether glycol DL-1000D and 0.02g of dibutyltin dilaurate are added dropwise, the temperature is raised to 80 ℃, the reaction is carried out for 3 hours, the vacuum pumping is carried out for removing bubbles, the active prepolymer is obtained, the isocyanate content is 4.91+/-0.3%, the temperature is reduced to 50 ℃, and the sealing and the storage are carried out for standby;
the structural formula of the active prepolymer is as follows:
wherein R is 1 -NCOFor (I)>Is->
2. The preparation of the component A comprises the following steps:
1) Weighing the component A:
91g of active prepolymer;
9g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
2g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of the component B comprises the following steps:
1) Weighing the component B:
60g of tackifying resin solution;
15g of triethylene diamine aqueous solution;
polyaspartic acid ester resin F420 5g;
defom-6800.5 g of defoamer;
aminosilane coupling agent KH-792 g;
30g of 800-mesh calcium hydroxide and 20g of 1250-mesh talcum powder;
rutile type titanium dioxide NR9503 g;
high pigment carbon black MA-100.3 g;
1010.4 g of antioxidant;
UV absorber UV-531 0.4g;
0.5g of anti-settling agent BYK-410;
2) Adding a tackifying resin solution, a triethylene diamine aqueous solution, polyaspartic acid ester resin, a defoaming agent and an aminosilane coupling agent into a container according to the metering, and mechanically stirring to obtain a uniform mixed solution;
3) Adding composite filler, titanium dioxide, high pigment carbon black, antioxidant and ultraviolet absorber into the mixed solution in the step 2), uniformly stirring and dispersing at a low speed for 15 minutes, dispersing at a high speed for 20 minutes, adding anti-settling agent, and continuously stirring at a high speed for 10 minutes;
4) And (3) subpackaging the fluid obtained in the step (3) into a tin barrel for sealing and preserving to obtain the component B.
4. When the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 2
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. the preparation of the active prepolymer comprises the following steps:
(a) Respectively vacuumizing and dehydrating polyether glycol DL-1000D and polyether triol EP-3600 at 120 ℃ by using a vacuum pump for 2 hours, and cooling for standby.
(b) 35.82g of the polyether triol EP-3600 treated in the step (a) and 4.83g of acetyl tributyl citrate are put into a three-neck flask, the temperature is raised to 60 ℃, 7.15g of toluene diisocyanate is added dropwise, and the reaction is carried out for 2.5h under the nitrogen condition. Then 13.05g of polyether glycol DL-1000D and 0.02g of dibutyltin dilaurate are added dropwise, the temperature is raised to 80 ℃, the reaction is carried out for 3 hours, the vacuum pumping is carried out for removing bubbles, the active prepolymer is obtained, the isocyanate content is 5.16+/-0.3%, the temperature is reduced to 50 ℃, and the sealing and the storage are carried out for standby;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
91g of active prepolymer;
9g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
2g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of component B was carried out in the same manner as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 3
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. the preparation of the active prepolymer comprises the following steps:
(a) Respectively vacuumizing and dehydrating polyether glycol DL-1000D and polyether triol EP-3600 at 110 ℃ by using a vacuum pump for 2 hours, and cooling for standby.
(b) 35.82g of the polyether triol EP-3600 treated in the step (a) and 4.86g of acetyl tributyl citrate are put into a three-neck flask, the temperature is raised to 60 ℃, 7.41g of toluene diisocyanate is added dropwise, and the reaction is carried out for 2.5h under the nitrogen condition. Then 13.05g of polyether glycol DL-1000D and 0.02g of dibutyltin dilaurate are added dropwise, the temperature is raised to 80 ℃, the reaction is carried out for 3 hours, the vacuum pumping is carried out for removing bubbles, the active prepolymer is obtained, the isocyanate content is 5.42+/-0.3%, the temperature is reduced to 50 ℃, and the sealing and the storage are carried out for standby;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
91g of active prepolymer;
9g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
2g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of component B was carried out in the same manner as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 4
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
94g of active prepolymer;
6g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
3g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of component B was carried out in the same manner as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 5
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
88g of active prepolymer;
12g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
3g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of component B was carried out in the same manner as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 6
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
85g of active prepolymer;
15g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
3g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of component B was carried out in the same manner as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 7
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
82g of active prepolymer;
18g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
3g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of component B was carried out in the same manner as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 8
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
85g of active prepolymer;
15g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
3g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of the component B comprises the following steps:
1) Weighing the component B:
65g of tackifying resin solution;
10g of triethylene diamine aqueous solution;
520 g of polyaspartic acid ester resin F;
polyaspartic acid ester resin F420 5g;
0.6g of defoaming agent BYK-066N;
2g of aminosilane coupling agent KH-540;
35g of 800-mesh calcium hydroxide and 20g of 1250-mesh talcum powder;
960 g of rutile titanium dioxide NR;
the high pigment carbon black is MA-11.4 g;
1010.3 g of antioxidant;
75.7 g of ultraviolet absorber Tinuvin B;
0.7g of anti-settling agent BYK-420;
2) Adding a tackifying resin solution, a triethylene diamine aqueous solution, polyaspartic acid ester resin, a defoaming agent and an aminosilane coupling agent into a container according to the metering, and mechanically stirring to obtain a uniform mixed solution;
3) Adding composite filler, titanium dioxide, high pigment carbon black, antioxidant and ultraviolet absorber into the mixed solution in the step 2), uniformly stirring and dispersing at a low speed for 15 minutes, dispersing at a high speed for 20 minutes, adding anti-settling agent, and continuously stirring at a high speed for 10 minutes;
4) And (3) subpackaging the fluid obtained in the step (3) into a tin barrel for sealing and preserving to obtain the component B.
4. When the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Example 9
The embodiment discloses a preparation method of a high-elasticity biliquid grouting material for plugging, which comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
85g of active prepolymer;
15g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
3g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. the preparation of the component B comprises the following steps:
1) Weighing the component B:
55g of tackifying resin solution;
5g of triethylene diamine aqueous solution;
polyaspartic acid ester resin F420 10g;
520 g of polyaspartic acid ester resin F;
BYK-066N defoamer 0.6g;
KH-540 aminosilane coupling agent 1g;
25g of 800-mesh calcium hydroxide and 20g of 1250-mesh talcum powder;
960 g of rutile titanium dioxide NR;
high pigment carbon black MA-11.4 g;
1010.7 g of antioxidant;
0.3g of Tinuvin B75 ultraviolet absorbent;
0.7g of anti-settling agent BYK-420;
2) Adding a tackifying resin solution, a triethylene diamine aqueous solution, polyaspartic acid ester resin, a defoaming agent and an aminosilane coupling agent into a container according to the metering, and mechanically stirring to obtain a uniform mixed solution;
3) Adding composite filler, titanium dioxide, high pigment carbon black, antioxidant and ultraviolet absorber into the mixed solution in the step 2), uniformly stirring and dispersing at a low speed for 15 minutes, dispersing at a high speed for 20 minutes, adding anti-settling agent, and continuously stirring at a high speed for 10 minutes;
4) And (3) subpackaging the fluid obtained in the step (3) into a tin barrel for sealing and preserving to obtain the component B.
4. When the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1, grouting, curing to form low-modulus high-elasticity gel, no foaming, no shrinkage, compact inside, good bonding strength to concrete and other substrates, and meeting the subway plugging requirements of strong vibration and large deformation.
Comparative example 1
The comparative example 1 discloses a preparation method of a high-elasticity biliquid grouting material for plugging, wherein an A component of the grouting material does not contain an alpha-silane modified polymer, and the preparation method comprises the following steps:
1. preparation of reactive prepolymer as in example 2;
2. the preparation of the component A comprises the following steps:
1) Weighing the component A:
100g of active prepolymer;
2g of vinyl trimethoxy silane;
2) Uniformly mixing the active prepolymer and vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
3. preparation of component B as in example 1;
4. when the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1 grouting.
Comparative example 2
The comparative example 1 discloses a preparation method of a high-elasticity biliquid grouting material for plugging, wherein the A component of the grouting material does not contain an active prepolymer, and the preparation method comprises the following steps:
1. the preparation of the component A comprises the following steps:
1) Weighing the component A:
100g of Vak GENIOSIL STP-E10 (alpha-silane modified polymer);
2g of vinyl trimethoxy silane;
2) Uniformly mixing the alpha-silane modified polymer and vinyl trimethoxy silane according to the measurement, and then sub-packaging the mixture into a tin barrel for sealing and preserving to obtain a component A;
2. the preparation of the component B comprises the following steps:
1) Weighing the component B:
55g of tackifying resin solution;
5g of triethylene diamine aqueous solution;
10g of PPG-2000 polyether polyol;
polyaspartic acid ester resin F420 5g;
defom-6800.5 g of defoamer;
aminosilane coupling agent KH-792 g;
aminosilane coupling agent KH-540 2g
30g of 800-mesh calcium hydroxide and 20g of 1250-mesh talcum powder;
rutile type titanium dioxide NR9503 g;
high pigment carbon black MA-100.3 g;
1010.4 g of antioxidant;
UV absorber UV-531 0.4g;
0.5g of anti-settling agent BYK-410;
2) Adding a tackifying resin solution, a triethylene diamine aqueous solution, PPG-2000 polyether polyol, polyaspartic acid ester resin, a defoaming agent and an aminosilane coupling agent into a container according to the metering, and mechanically stirring to obtain a uniform mixed solution;
3) Adding composite filler, titanium dioxide, high pigment carbon black, antioxidant and ultraviolet absorber into the mixed solution in the step 2), uniformly stirring and dispersing at a low speed for 15 minutes, dispersing at a high speed for 20 minutes, adding anti-settling agent, and continuously stirring at a high speed for 10 minutes;
4) And (3) subpackaging the fluid obtained in the step (3) into a tin barrel for sealing and preserving to obtain the component B.
4. When the high-elasticity biliquid grouting material for plugging is used, the volume ratio of the component A to the component B is 1:1 grouting.
The testing method comprises the following steps:
the high-elasticity biliquid grouting materials for plugging prepared in examples 1-9 and comparative examples 1-2 comprise the following components in percentage by volume: 1, carrying out slurry preparation and sample preparation, and carrying out test after the test piece is cured for 7 days under standard curing conditions.
Gel time: under standard experimental conditions, the sample (50+ -0.1) g was weighed into a container and the time t was recorded 0 Stirring uniformly, detecting viscosity change with glass rod, and drawing when the glass rod leaves the liquid surfaceThe sample had gelled and the time t was recorded 1 Gel time t=t 1 -t 0 ；
Surface drying time: the test is carried out according to the method B of 12.2.1 in GB/T16777-2008;
tensile strength and elongation at break: according to GB/T2567-2008, a WDW3020 type micro-control electronic universal testing machine is adopted for testing, the effective stretching length of a dumbbell type stretching spline is 25mm, the width is 4mm, the thickness is 2mm, and the stretching rate is 200mm/min;
tensile modulus: the test was carried out according to the method of GB/T13477.8-2017, expressed as strength at 60% elongation, tensile modulus at 23℃without explanation;
elastic recovery rate: the test was carried out as described in GB/T23457-2017 at 6.10. The distance between the standard lines is stretched from 25mm to 50mm and kept for 24 hours. Taking down the test piece, and placing the test piece on the smooth surface paved with talcum powder for 2 hours for measurement;
dry base adhesion strength: experiments are carried out according to GB/T16777-2008 chapter 7B method;
wet base adhesion strength: the test is carried out according to GB/T16777-2008 chapter 7B method, before preparing a test piece, a mortar test block is soaked in water at 23 ℃ for 24 hours, the water stain is wiped off by a wet towel after the test block is taken out, and after the test block is dried in the air for 5 minutes, the surface of the mortar block is smeared with the test sample. The test results of each example are shown in table 1.
TABLE 1 Performance test results of a high elasticity biliquid grouting material for plugging
As can be seen from the data in Table 1, the high-elasticity biliquid grouting material for plugging disclosed by the invention is high in curing speed, free from the influence of humidity and slurry thickness, capable of forming a gel with low modulus and high elasticity after curing, free from foaming and shrinkage, compact in the gel, good in bonding strength on substrates such as concrete, and the like, and capable of meeting the subway plugging requirements of strong vibration and large deformation, and solves the problems that the existing grouting material is poor in water-resistant permeability, inelastic, incapable of adapting to expansion and shrinkage deformation of cracks and serious in leakage due to the fact that a large number of communicated rigid foams, holes and large numbers of water-resistant holes are formed after curing. The component A in the embodiment 8 is a clear and transparent component, the compatibility of each component is excellent, the component B is a gray viscous fluid, the components A, B are mixed and poured into water, the slurry is not dispersed in water, the grouting material is favorable for forming a continuous gel structure to thoroughly block cracks, and after the gel is solidified, the gel has few internal bubbles and compact structure, so that the grouting material is favorable for long-term waterproof and plugging effects. The adhesive can be controlled to be gel for 10min, surface drying for 30min, elongation at break of more than 1500%, tensile modulus of less than 0.3MPa, elastic recovery rate of 95%, adhesive strength of a dry base surface of 1.58MPa and adhesive strength of a wet base surface of 1.30MPa.
In contrast, comparative example 1 has lower adhesive strength than examples 1 to 8 because no α -silane-modified polymer was added. In comparative example 2, the reactive prepolymer was not added, curing was insufficient, gel having a relatively large elongation at break could not be formed, and the adhesive strength was the worst. Therefore, the high-elasticity biliquid grouting material for plugging provided by the invention has the advantage of dual curing by introducing the active prepolymer containing isocyanate groups and the alpha-silane modified polymer. The curing speed, tensile strength, elongation at break, dry base adhesive strength and elastic recovery rate properties are greatly improved compared with those of comparative examples 1 and 2. The grouting material prepared by the invention has extremely high elongation at break of more than 1500% after solidification, and can meet the subway plugging requirements of strong vibration and larger deformation. The slurry is solidified in water without foaming and expansion, has excellent toughness, good interfacial bonding strength performance and no debonding.
Fig. 3 is an internal morphology diagram of the slurry of example 8 after curing, and as can be seen from fig. 3, the gel has few internal bubbles and compact structure after curing, which is beneficial to long-term waterproof and plugging effects.
The above embodiments are preferred examples of the present invention, and the present invention is not limited thereto, and any other modifications or equivalent substitutions made without departing from the technical aspects of the present invention are included in the scope of the present invention.

Claims (9)

1. The high-elasticity biliquid grouting material for plugging is characterized by comprising an A component and a B component, wherein the A component comprises the following components in parts by weight:
82-94 parts of active prepolymer;
6-18 parts of alpha-silane modified polymer;
2-3 parts of vinyl trimethoxy silane;
the component B comprises the following components in parts by weight:
2. the high elasticity biliquid grouting material for plugging according to claim 1, wherein the reactive prepolymer has the following structural formula:
wherein R is 1 -NCO is Is->
3. The high elasticity biliquid grouting material for plugging according to claim 1, wherein the tackifying resin solution comprises the following components in percentage:
4. a high elasticity biliquid grouting material for plugging according to claim 1, wherein the composite filler comprises calcium hydroxide, talc or a combination thereof.
5. A high elasticity biliquid grouting material for plugging according to claim 1, wherein the antifoaming agent comprises hydrophobic particle silicone compound, foam breaking polysiloxane solution or a combination thereof.
6. The high elasticity biliquid grouting material for plugging according to claim 1, wherein the anti-settling agent comprises a modified urea solution, a modified polyurea solution or a combination thereof.
7. The high elasticity biliquid grouting material for plugging according to claim 1, wherein the aminosilane coupling agent comprises N- (β -aminoethyl) - γ -aminopropyl trimethoxysilane, 3-aminopropyl trimethoxysilane or a combination thereof.
8. The method for preparing the high-elasticity biliquid grouting material for plugging according to claim 1, which is characterized by comprising the following specific steps:
(1) Respectively vacuumizing and dehydrating polyether glycol and polyether triol at 110-120 ℃; mixing dehydrated polyether triol and acetyl tributyl citrate, heating, dropwise adding toluene diisocyanate, reacting under the condition of nitrogen, adding polyether diol and dibutyl tin dilaurate, continuously heating for reaction, and vacuumizing to obtain an active prepolymer;
(2) Uniformly mixing the active prepolymer, the alpha-silane modified polymer and the vinyl trimethoxy silane, and then sealing and preserving to obtain a component A;
(3) Adding the tackifying resin solution, the triethylene diamine aqueous solution, the polyaspartic acid ester resin, the defoaming agent and the aminosilane coupling agent into a container, and mechanically stirring to obtain uniform mixed solution; adding composite filler, titanium dioxide, high pigment carbon black, antioxidant and ultraviolet absorbent into the mixed solution, stirring and dispersing uniformly, adding anti-settling agent, continuing stirring, subpackaging the dispersed fluid, and sealing and preserving to obtain component B.
9. The method for preparing the high-elasticity biliquid grouting material for plugging according to claim 8, wherein the A component and the B component are injected into a crack in use, and the volume ratio of the A component to the B component is 1:1.
CN202311111556.3A 2023-08-31 2023-08-31 High-elasticity biliquid grouting material for plugging and preparation method thereof Pending CN117304441A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118271954A (en) * 2024-04-25 2024-07-02 广东蓝迪高新材料科技有限公司 Polyaspartic acid ester elastic waterproof grouting material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118271954A (en) * 2024-04-25 2024-07-02 广东蓝迪高新材料科技有限公司 Polyaspartic acid ester elastic waterproof grouting material and preparation method thereof

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