CN115612050B - Water shutoff grouting material and preparation method thereof - Google Patents
Water shutoff grouting material and preparation method thereof Download PDFInfo
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- CN115612050B CN115612050B CN202211629075.7A CN202211629075A CN115612050B CN 115612050 B CN115612050 B CN 115612050B CN 202211629075 A CN202211629075 A CN 202211629075A CN 115612050 B CN115612050 B CN 115612050B
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
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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
- C08K3/34—Silicon-containing compounds
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Consolidation Of Soil By Introduction Of Solidifying Substances Into Soil (AREA)
Abstract
The water shutoff grouting material consists of black material 30-50 weight portions and white material 50-70 weight portions, wherein the raw material black material is silane modified silica 1.6-3.2 weight portions; 0.4-0.8 part of silane modified calcium sulfate whisker; 4-5 parts of sodium carboxymethylcellulose; 10-15 parts of water glass; 360-28 parts of polyether polyol; 0.2-1 part of triethylene diamine; the balance of water. In addition, the preparation method of the water shutoff grouting material is also disclosed.
Description
Technical Field
The invention belongs to the technical field of civil engineering grouting; relates to a water shutoff grouting material and a preparation method thereof.
Background
The fine sand is a loose deposit formed during the fourth period, mainly referring to sand with a particle size of less than 0.25mm in an amount of more than 50% of the total weight, and particles with a particle size of more than 0.075mm also in an amount of more than 50% of the total mass. The fine sand in the natural state has poor cementing property, loose structure and lower bearing capacity, can be compacted under the action of dead weight, and the density of the fine sand layer becomes larger along with the increase of the embedded depth.
Construction of underground engineering is carried out in the fine sand stratum, and as the fine sand stratum is loose in structure and the stress state of the original surrounding rock of the stratum after excavation is changed, the stress of the surrounding rock is released, and if no pre-supporting measures are adopted, engineering accidents such as collapse, roof fall and the like are easy to occur.
However, the particle size of each fine particle of the common fine sand is smaller, the distribution is uniform, and the non-uniformity coefficient is generally smaller than 5; at the same time, the fine particles mutually fill the pores in the structure, so that the permeability coefficient is generally reduced. When grouting is performed by adopting a cement and other particle grouting materials, the situation that the slurry is difficult to inject or even cannot enter can occur due to the large particle size of the slurry particles. Even if a part of the slurry is injected into the fine sand, a poor reinforcing effect results.
Chinese patent application CN114196191a discloses a water-plugging grouting composite material for fine sand stratum, which consists of black material and white material, the raw materials in parts by weight are, white material 50-70: 2-4 parts of silane modified silicon dioxide; 4-5 parts of sodium carboxymethylcellulose; 10-15 parts of water glass; 20-28 parts of polyether polyol; 0.2-1 part of triethylene diamine; the balance of water; 30-50 parts of black material: 20-28 parts of polyisocyanate; the balance of water. The fine sand soil sample reinforced by the water shutoff grouting composite material has higher compressive strength and higher tensile strength.
However, there is still a need for further improvement in the compressive and tensile strength of the fine sand soil sample according to the actual needs of the fine sand formation.
Disclosure of Invention
The invention aims to provide a water shutoff grouting material with better compressive strength and tensile strength and a preparation method thereof.
In order to achieve the above object, on the one hand, the technical scheme adopted by the invention is as follows: the water shutoff grouting material consists of black material 30-50 weight portions and white material 50-70 weight portions, and features that the material includes the following materials in weight portion,
black material:
20-28 parts of diphenylmethane diisocyanate;
the balance of water;
white material:
1.6-3.2 parts of silane modified silicon dioxide;
0.4-0.8 part of silane modified calcium sulfate whisker;
4-5 parts of sodium carboxymethylcellulose;
10-15 parts of water glass;
360-28 parts of polyether polyol;
0.2-1 part of triethylene diamine;
the balance of water.
The invention relates to a water shutoff grouting material, wherein the preparation of silane modified calcium sulfate whisker is as follows: uniformly mixing absolute ethyl alcohol and gamma-aminopropyl triethoxysilane, and regulating the pH value to be 3-4 to obtain a modified solution; heating to 30-50 ℃, and adding calcium sulfate whisker into the modified solution, wherein the weight-volume ratio of the calcium sulfate whisker to the gamma-aminopropyl triethoxysilane is 1g:0.08mL, and reacting for 0.5-2h at a constant temperature; washing with absolute ethyl alcohol and vacuum drying.
The water shutoff grouting material provided by the invention, wherein the melting point of the calcium sulfate whisker is 1540 ℃; density of 2.69g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Bulk density of 0.2-0.4g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Tensile strength of 20.53GPa; the diameter is 2-4 mu m; the length is 20-80 μm.
The water shutoff grouting material disclosed by the invention is prepared by the following steps of: reacting absolute ethyl alcohol, ammonia water, deionized water and tetraethoxysilane at 40-60 ℃ for 6-72h in a heat preservation way; the volume ratio of the four is 55:3:1:2; then adding 0.2-0.3mL of gamma-aminopropyl triethoxysilane into the mixture, and continuing to react for 0.5-24h under heat preservation; washing with absolute ethyl alcohol and vacuum drying.
The water shutoff grouting material provided by the invention, wherein the average particle size of the silane modified silicon dioxide is 50-100nm.
The water-plugging grouting material according to the invention, wherein the average molecular weight M of the sodium carboxymethylcellulose w =22-28 kilodaltons.
The water shutoff grouting material provided by the invention, wherein the substitution degree DS=0.7-1.1 of sodium carboxymethyl cellulose.
The water shutoff grouting material provided by the invention, wherein the Baume degree of the water glass is 50-55, and the modulus is 2.6-3.0.
The water-plugging grouting material according to the invention, wherein the polyether polyol has a functionality of 3; average molecular weight M w =4800 daltons.
On the other hand, the invention provides a preparation method of the water shutoff grouting material, which is characterized in that black materials and white materials are respectively prepared and mixed before use.
Compared with the prior art, the water shutoff grouting material disclosed by the invention has better compressive strength and tensile strength, and has higher use value under specific engineering requirements.
Detailed Description
It must be noted that, as used in this specification and the appended claims, the singular forms "a," "an," and "the" include both a reference and a plurality of references (i.e., more than two, including two) unless the context clearly dictates otherwise.
Unless otherwise indicated, the numerical ranges in the present invention are approximate, and thus values outside the ranges may be included. The numerical ranges may be expressed herein as from "about" one particular value, and/or to "about" another particular value. When such a range is expressed, another aspect includes from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent "about," it will be understood that the particular value forms another aspect. It will also be understood that the endpoints of each of the numerical ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
References in the specification and the claims to parts by weight of a particular element or component in a composition or article refer to the relationship by weight between that element or component and any other element or component in the composition or article.
In the present invention, unless specifically indicated to the contrary, or implied by the context of the context or conventional means in the art, the solutions referred to in the present invention are aqueous solutions; when the solute of the aqueous solution is a liquid, all fractions and percentages are by volume, and the volume percent of the component is based on the total volume of the composition or product comprising the component; when the solute of the aqueous solution is a solid, all fractions and percentages are by weight, and the weight percentages of the components are based on the total weight of the composition or product comprising the components.
References to "comprising," "including," "having," and similar terms in this invention are not intended to exclude the presence of any optional components, steps or procedures, whether or not any optional components, steps or procedures are specifically disclosed. For the avoidance of any doubt, unless stated to the contrary, all methods claimed through use of the term "comprising" may include one or more additional steps, apparatus parts or components and/or materials. In contrast, the term "consisting of … …" excludes any component, step or procedure not specifically recited or enumerated. The term "or" refers to members recited individually as well as in any combination unless otherwise specified.
Furthermore, the contents of any of the referenced patent documents or non-patent documents in the present invention are incorporated by reference in their entirety, especially with respect to the definitions and general knowledge disclosed in the art (in case of not inconsistent with any definitions specifically provided by the present invention).
In the present invention, parts are parts by weight unless otherwise indicated, temperatures are expressed in degrees celsius or at ambient temperature, and pressures are at or near atmospheric. Room temperature represents 20-30 ℃. There are numerous variations and combinations of reaction conditions (e.g., component concentrations, solvents needed, solvent mixtures, temperatures, pressures, and other reaction ranges) and conditions that can be used to optimize the purity and yield of the product obtained by the process. Only reasonable routine experimentation will be required to optimize such process conditions.
Example 1
Adding absolute ethyl alcohol, ammonia water and deionized water into a reaction device, wherein the volumes of the absolute ethyl alcohol, the ammonia water and the deionized water are 550mL, 30mL and 10mL respectively, and heating to 50 ℃; 20mL of tetraethoxysilane is added dropwise, and the reaction is carried out for 24 hours after the completion of the dropwise addition. 2.5mL of gamma-aminopropyl triethoxysilane was then added thereto and the reaction was allowed to stand for 6h. And (3) centrifugally washing the silicon dioxide with absolute ethyl alcohol for 3 times, and carrying out vacuum drying to obtain the silane modified silicon dioxide. The average particle size of the silane-modified silica was 72nm.
100mL of absolute ethanol and 5mL of gamma-aminopropyl triethoxysilane were mixed uniformly, and pH=3.5 was adjusted with acetic acid to obtain a modified solution. Heating to 40deg.C, and mixing with calcium sulfate whisker (melting point 1540deg.C; density 2.69 g/cm) 3 The method comprises the steps of carrying out a first treatment on the surface of the Bulk density of 0.2-0.4g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Tensile strength of 20.53GPa; the diameter is 2-4 mu m; length 20-80 μm) is added into the modified solution, and the weight volume ratio of the calcium sulfate whisker to the gamma-aminopropyl triethoxysilane is 1g:0.08mL, and the reaction was incubated for 1h. And (3) centrifugally washing the mixture with absolute ethyl alcohol for 3 times, and carrying out vacuum drying to obtain the silane modified calcium sulfate whisker. IR spectrum shows that silane modified calcium sulfate whisker is 2925cm in length -1 、1564cm -1 、1438cm -1 、1108cm -1 And 1076cm -1 The allele exhibits a characteristic absorption peak.
2.4 parts by weight of silane-modified silica, 0.6 part by weight of silane-modified calcium sulfate whisker, 4.5 parts by weight of sodium carboxymethylcellulose (M w =25 kilodaltons; degree of substitution ds=0.9), 12 parts by weight of water glass (baume degree 53.1, modulus 2.8), 0.5 part by weight of triethylenediamine was added to 24 parts by weight of polyether polyol 360 (functionality 3, average molecular weight M w =4800 daltons) and 16 parts by weight of water, stirring for 30minStanding to obtain white material; 24 parts by weight of diphenylmethane diisocyanate MDI and 16 parts by weight of water were mixed homogeneously as a black material.
And mixing the black material and the white material before use to obtain the grouting material. According to the mixing ratio of 30%, adding the grouting material into a locally collected fine sand soil sample, placing the fine sand soil sample into a mould with the thickness of 30mm multiplied by 120mm, naturally curing for 1 day, removing the mould, and cutting the mould into samples with the thickness of 30mm multiplied by 30 mm. The samples were dry-cultured under natural conditions for 14 days.
And (3) uniformly mixing the soil sample before the test, air-drying, sieving with a 2mm sieve, carrying out particle analysis by using a laser particle size distribution instrument, and analyzing the soil texture by using an international standard. Cumulative percentage of soil sample particle diameter (D) 10 、D 30 And D 60 ) The curvature coefficient, non-uniformity coefficient, density and void ratio are specifically shown in table 1 below.
The unconfined compressive strength of the test specimens was measured using a universal tester. The test method adopts a displacement control method, and the displacement change rate is 5mm/min. The compressive strength of the test piece was 5.72MPa.
The tensile strength of the test specimen was measured using a strain-controlled unconfined pressure gauge. The test method adopts Brazilian split method, and the strain applying speed is 5mm/min. The tensile strength of the test specimen in the dry condition was 535kPa.
Comparative example 1
Example 1 of chinese patent application CN114196191 a.
Comparative example 2
100mL of absolute ethanol and 5mL of gamma-aminopropyl triethoxysilane were mixed uniformly, and pH=3.5 was adjusted with acetic acid to obtain a modified solution. Heating to 40 ℃, adding calcium sulfate whisker (melting point is 1540 ℃, density is 2.69g/cm3, loose density is 0.2-0.4g/cm3, tensile strength is 20.53GPa, diameter is 2-4 mu m, length is 20-80 mu m) into the modified solution, wherein the weight-volume ratio of the calcium sulfate whisker to gamma-aminopropyl triethoxysilane is 1g:0.08mL, and the reaction was incubated for 1h. And (3) centrifugally washing the mixture with absolute ethyl alcohol for 3 times, and carrying out vacuum drying to obtain the silane modified calcium sulfate whisker.
3 parts by weight of silane-modified calcium sulfate whisker, 4.5 parts by weight of sodium carboxymethylcellulose (mw=25 kilodaltons; degree of substitution ds=0.9), 12 parts by weight of water glass (baume degree 53.1, modulus 2.8), 0.5 part by weight of triethylenediamine were added to 24 parts by weight of polyether polyol 360 (functionality 3, average molecular weight mw=4800 daltons) and 16 parts by weight of water, stirred for 30 minutes and left to stand as a white material; 24 parts by weight of diphenylmethane diisocyanate MDI and 16 parts by weight of water were mixed homogeneously as a black material.
The other conditions were the same as in example 1. The compressive strength of the sample is 4.17MPa; the tensile strength of the test specimen was 380kPa.
Further, it should be understood that various changes, substitutions, omissions, modifications, or adaptations to the present invention may be made by those skilled in the art after having read the present disclosure, and such equivalent embodiments are within the scope of the present invention as defined in the appended claims.
Claims (8)
1. The water shutoff grouting material consists of black material 30-50 weight portions and white material 50-70 weight portions, and features that the material includes the following materials in weight portion,
black material:
20-28 parts of diphenylmethane diisocyanate;
the balance of water;
white material:
1.6-3.2 parts of silane modified silicon dioxide;
0.4-0.8 part of silane modified calcium sulfate whisker;
4-5 parts of sodium carboxymethylcellulose;
10-15 parts of water glass;
360-28 parts of polyether polyol;
0.2-1 part of triethylene diamine;
the balance of water;
wherein, the liquid crystal display device comprises a liquid crystal display device,
the preparation method of the silane modified calcium sulfate whisker comprises the following steps: uniformly mixing absolute ethyl alcohol and gamma-aminopropyl triethoxysilane, and regulating the pH value to be 3-4 to obtain a modified solution; heating to 30-50 ℃, and adding calcium sulfate whisker into the modified solution, wherein the weight-volume ratio of the calcium sulfate whisker to the gamma-aminopropyl triethoxysilane is 1g:0.08mL, and reacting for 0.5-2h at a constant temperature; washing with absolute ethyl alcohol and drying in vacuum;
the melting point of the calcium sulfate whisker is 1540 ℃; density of 2.69g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Bulk density of 0.2-0.4g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Tensile strength of 20.53GPa; the diameter is 2-4 mu m; the length is 20-80 μm.
2. The water shutoff grouting material of claim 1, wherein the silane modified silica is prepared by: reacting absolute ethyl alcohol, ammonia water, deionized water and tetraethoxysilane at 40-60 ℃ for 6-72h in a heat preservation way; the volume ratio of the four is 55:3:1:2; then adding 0.2-0.3mL of gamma-aminopropyl triethoxysilane into the mixture, and continuing to react for 0.5-24h under heat preservation; washing with absolute ethyl alcohol and vacuum drying.
3. The water-plugging grouting material of claim 2, wherein the silane-modified silica has an average particle size of 50-100nm.
4. The water-plugging grouting material of claim 1, wherein the sodium carboxymethylcellulose has an average molecular weight M w =22-28 kilodaltons.
5. The water-plugging grouting material of claim 4, wherein the substitution degree ds=0.7-1.1 of sodium carboxymethyl cellulose.
6. The water-plugging grouting material of claim 1, wherein the water glass has a baume of 50-55 and a modulus of 2.6-3.0.
7. The water-plugging grouting material of claim 1, wherein the polyether polyol has a functionality of 3; average molecular weight M w =4800 daltons.
8. A method of preparing a water-plugging, grouting material according to any one of claims 1-7, wherein black and white materials are prepared separately and mixed prior to use.
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| CN115612050A (en) | 2023-01-17 |
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