CN113717608B - Waterproof plugging agent and preparation method thereof - Google Patents

Waterproof plugging agent and preparation method thereof Download PDF

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Publication number
CN113717608B
CN113717608B CN202111080978.XA CN202111080978A CN113717608B CN 113717608 B CN113717608 B CN 113717608B CN 202111080978 A CN202111080978 A CN 202111080978A CN 113717608 B CN113717608 B CN 113717608B
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waterproof
parts
powder
plugging agent
waterproof plugging
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CN113717608A (en
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赵福涛
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Shandong Saigao New Materials Co ltd
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Shandong Saigao New Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D157/00Coating compositions based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09D157/02Copolymers of mineral oil hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • 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
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • 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
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16Fibres; Fibrils

Abstract

The embodiment of the invention relates to the technical field of waterproof construction, and particularly discloses a waterproof plugging agent and a preparation method thereof, wherein the raw materials of the waterproof plugging agent comprise a dispersion medium and a base material; wherein, the base material at least comprises the following raw materials: hydrocarbon resin, SBS rubber, modified fiber material, powder and inorganic aluminum salt waterproof agent; compared with the existing waterproof plugging agent products, the waterproof plugging agent provided by the embodiment of the invention can ensure the waterproof plugging effect and simultaneously improve the compressive strength, effectively improves the application range of the waterproof plugging agent, solves the problem that the existing waterproof plugging agent cannot ensure the waterproof plugging effect and simultaneously improve the compressive strength, and has wide market prospect.

Description

Waterproof plugging agent and preparation method thereof
Technical Field
The embodiment of the invention relates to the technical field of waterproof construction, in particular to a waterproof plugging agent and a preparation method thereof.
Background
In the fields of building construction, well drilling exploitation and the like, the waterproof plugging material is indispensable, for example, in sewer construction, the waterproof plugging material can reduce the problem of water leakage caused by the formation of gaps at the joint of a pipeline and the ground, and well leakage is easy to occur during the development of well drilling oil gas, so that the pressure-bearing plugging agent is needed for plugging.
At present, most of common waterproof plugging agents are organic plugging agents and inorganic plugging agents, wherein most of the inorganic plugging agents adopt calcium carbonate, portland cement and the like as basic materials, and although the compressive strength is high, the inorganic plugging agents are easily corroded by leaked liquid to reduce the waterproof effect; although the resin in the organic plugging agent can play a good waterproof effect, the general compressive strength is not high, and the strength requirement in well drilling and exploitation cannot be met. Some common waterproof plugging agents only have simple filling effect, are poor in plugging effect when used alone, and need to be matched with various materials, so that the construction difficulty is increased.
Therefore, the waterproof plugging agent in the prior art has the following defects: the compressive strength can not be effectively improved while the waterproof and leakage-stopping effects are ensured.
Disclosure of Invention
The embodiment of the invention aims to provide a waterproof plugging agent, which is used for solving the problem that the compressive strength cannot be improved while the waterproof plugging effect cannot be ensured in the conventional waterproof plugging agent in the background art.
In order to achieve the above purpose, the embodiments of the present invention provide the following technical solutions:
the waterproof plugging agent provided by the embodiment of the invention at least comprises a dispersion medium and a base material which is dispersed in the dispersion medium and forms a uniform material;
wherein the base material at least comprises the following raw materials: hydrocarbon resin, SBS rubber (thermoplastic Styrene-Butadiene rubber, namely Styrene-Butadiene-Styrene triblock copolymer, SBS for short), modified fiber material, powder and inorganic aluminum salt waterproof agent; the modified fiber material is prepared by taking corn straw fiber, cellulose acetate and acrylic fiber as raw materials and injecting silica sol under the vacuum heating condition.
As another preferred embodiment of the invention, the preparation method of the modified fiber material comprises the steps of putting the corn straw fiber, the cellulose acetate and the acrylic fiber in a sealed container according to the mass ratio of 1-3:1-5:2-4, vacuumizing to be not more than 0.03MPa, then stirring and injecting excessive silica sol for uniform mixing, then keeping the temperature at 50-80 ℃ for more than 4 hours, and standing to obtain the modified fiber material. The silica sol is an organic solvent silica sol, and is favorable for mixing in a dispersion medium.
According to the embodiment of the invention, the corn stalk fiber, the cellulose acetate and the acrylic fiber are used as raw materials, the fiber expansion state of the corn stalk fiber is further expanded under the vacuum heating condition, and the injected silica sol forms a net structure together with the cellulose acetate and the acrylic fiber in the stirring process, so that the toughness and the strength of the fiber material can be ensured, and the waterproof performance is improved. It should be noted that the corn stalk fiber is a plant fiber material formed by alkalizing corn stalks with alkaline materials such as sodium hydroxide and potassium hydroxide to generate a fiber swelling state, and the specific preparation method may refer to the prior art and is not described herein in detail, and the preparation parameters are selected according to requirements and are not limited herein.
The embodiment of the invention takes hydrocarbon resin and SBS rubber as crosslinking matrix materials, the crosslinking network is formed by dissolving the crosslinking matrix materials in a dispersion medium, and the waterproof and strength enhancing effects of the modified fiber material are matched, so that the waterproof plugging agent with high elasticity, strong adhesive force and high viscosity of a paint film can be formed.
Among them, the hydrocarbon resin is generally selected from any one of four products, such as aliphatic petroleum resin (C5), alicyclic petroleum resin (DCPD, dicyclopentadiene), aromatic petroleum resin (C9), and monomeric petroleum resin such as AMS (alpha methyl styrene).
As another preferred embodiment of the invention, the waterproof plugging agent further comprises a proper amount of propellant, and specifically, the addition amount of the propellant is 1-1.8 times of the mass of the hydrocarbon resin.
In another preferred embodiment of the present invention, the propellant is selected from any one of isobutane, propane, butane, trichlorofluoromethane, difluoromethane, trichlorotetrafluoroethane, pentafluoroethane, chlorodifluoroethane, etc., and in consideration of environmental requirements, environmentally friendly products such as pentafluoroethane are preferred, and it is more preferred to use compressed gas such as nitrogen, carbon dioxide, nitrous oxide, etc. as the propellant, and the compressed gas may be mixed with the above fluorocarbon products to prepare the composite propellant.
As another preferred embodiment of the present invention, the dispersion medium is any one or more of toluene, xylene, and ethyl acetate.
As another preferred embodiment of the invention, the waterproof plugging agent comprises the following raw materials in parts by weight: 48-75 parts of dispersion medium, 22-40 parts of hydrocarbon resin, 0.8-1.8 parts of SBS rubber, 16-28 parts of modified fiber material, 10-18 parts of powder material and 0.01-0.05 part of inorganic aluminum salt waterproof agent.
As another preferred embodiment of the invention, the waterproof plugging agent comprises the following raw materials in parts by weight: 50-70 parts of dispersion medium, 26-36 parts of hydrocarbon resin, 1-1.5 parts of SBS rubber, 20-24 parts of modified fiber material, 12-16 parts of powder material and 0.02-0.04 part of inorganic aluminum salt waterproof agent.
Preferably, the waterproof plugging agent comprises the following raw materials in parts by weight: 60 parts of dispersion medium, 30 parts of hydrocarbon resin, 1.3 parts of SBS rubber, 22 parts of modified fiber material, 15 parts of powder material and 0.03 part of inorganic aluminum salt waterproof agent (solution and powder prepared by taking inorganic aluminum salt as a main raw material and adding a plurality of chemical raw materials for chemical combination).
As another preferred embodiment of the invention, the powder material at least comprises 15-25 parts of modified slag powder, 8-12 parts of calcite powder, 40-60 parts of heavy calcium powder, 30-48 parts of titanium dioxide and 15-25 parts of calcined kaolin according to parts by weight. The modified slag powder, the calcite powder, the triple superphosphate powder, the titanium dioxide powder and the calcined kaolin are mixed and ground to prepare powder, the calcium hydroxide powder, the triple superphosphate powder and the like are used as bonding materials, the titanium dioxide powder, the calcined kaolin and the like are used as water-absorbing waterproof materials, and the bonding framework structure of the modified slag powder is matched.
Preferably, the powder material comprises, by weight, 20 parts of modified slag powder, 10 parts of calcite powder, 50 parts of heavy calcium powder, 40 parts of titanium dioxide and 20 parts of calcined kaolin.
As another preferred embodiment of the present invention, the modified slag powder is prepared by adding water to slag powder, mixing uniformly, adding sulfuric acid, performing ultrasonic dispersion to acidify the slag powder, adding cetyltrimethylammonium bromide and urea, mixing uniformly, heating, and drying to obtain the modified slag powder.
As another preferred embodiment of the invention, the preparation method of the modified slag powder comprises the steps of adding water with the weight not less than 10 times of the weight of the slag powder into the slag powder, uniformly mixing, adding (dropwise adding) sulfuric acid (the adding amount is 0.01-0.1 time of the weight of the slag powder) for ultrasonic dispersion (the ultrasonic output power is 400-800W, and the ultrasonic time is 40-200min), adding hexadecyl trimethyl ammonium bromide and urea (the adding amount is 0.01-0.04 time of the weight of the slag powder, wherein the mass ratio of the hexadecyl trimethyl ammonium bromide to the urea is 1:1-50), uniformly mixing, heating to 40-80 ℃, taking out, drying, obtaining the modified slag powder, and sealing in a shade dry place for storage. By adopting the slag powder as the raw material, the waste of the slag powder is reduced, the environmental pollution is avoided, and meanwhile, the waste can be recycled as the material for improving the compressive strength.
As another preferred embodiment of the present invention, the slag powder is specifically a melt floating on the surface of a liquid material such as metal generated in a pyrometallurgical process, and the composition of the slag powder mainly comprises oxides (silica, alumina, calcium oxide, magnesium oxide), and often contains sulfides and carries a small amount of metal. The slag may be any of a smelting slag, a refining slag, a synthetic slag, and the like, and is selected according to the need, and is not limited herein.
The embodiment of the invention also provides a preparation method of the waterproof plugging agent, which comprises the following steps:
1) adding hydrocarbon resin and SBS rubber into the dispersion medium, and mixing uniformly to obtain a mixture;
2) and adding the modified fiber material and the powder material into the mixture according to the proportion, pulping and mixing (specifically, adjusting the rotating speed to about 1000-2000 r/min by a dispersion machine), and adding the inorganic aluminum salt waterproof agent for uniformly mixing to obtain the waterproof plugging agent.
Preferably, the preparation method of the waterproof plugging agent comprises the steps of putting toluene into a batching cylinder, then putting raw materials of hydrocarbon resin and SBS rubber, stirring for 30 minutes through a powder machine, dispersing for 30 minutes at the rotating speed of 80 rpm, then adding modified fiber material and powder, adjusting the rotating speed to about 1200 rpm through a dispersing machine, stirring for 40 minutes, then putting an inorganic aluminum salt waterproof agent, stirring uniformly to form a product, and filling the product into a fogging bottle for use.
As another preferred embodiment of the present invention, in the preparation method of the waterproof and leak-stopping agent, when the waterproof and leak-stopping agent further includes a propellant, the preparation method of the waterproof and leak-stopping agent further includes a step of injecting the propellant into a fogging bottle.
The embodiment of the invention also aims to provide the waterproof plugging agent prepared by the preparation method of the waterproof plugging agent.
Compared with the prior art, the embodiment of the invention has the beneficial effects that:
the raw materials of the waterproof plugging agent provided by the embodiment of the invention comprise a dispersion medium and a base material; wherein, the base material at least comprises the following raw materials: hydrocarbon resin, SBS rubber, modified fiber material, powder and inorganic aluminum salt waterproof agent; compared with the existing waterproof plugging agent products, the waterproof plugging agent provided by the embodiment of the invention can ensure the waterproof plugging effect and simultaneously improve the compressive strength, effectively improves the application range of the waterproof plugging agent, solves the problem that the existing waterproof plugging agent cannot ensure the waterproof plugging effect and simultaneously improve the compressive strength, and has wide market prospect.
Detailed Description
The present invention will be described in further detail by way of examples. The present embodiment is implemented on the premise of the technology of the embodiment of the present invention, and a detailed implementation manner and a specific operation procedure are given to illustrate the inventive embodiment of the present invention, but the scope of the embodiment of the present invention is not limited to the following embodiments. It is to be understood that all numbers expressing quantities, percentages, and other numerical values used in the application are to be understood as being modified in all instances by the term "about". Accordingly, unless expressly indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained.
The waterproof plugging agent provided by the embodiment of the invention at least comprises a dispersion medium and a base material which is dispersed in the dispersion medium and forms a uniform material;
wherein the base material at least comprises the following raw materials: hydrocarbon resin, SBS rubber, modified fiber material, powder material and inorganic aluminium salt waterproof agent; the modified fiber material is prepared by taking corn straw fiber, cellulose acetate and acrylic fiber as raw materials and injecting silica sol under the vacuum heating condition.
The embodiment of the invention takes hydrocarbon resin and SBS rubber as crosslinking matrix materials, the crosslinking network is formed by dissolving the crosslinking matrix materials in a dispersion medium, and the waterproof and strength enhancing effects of the modified fiber material are matched, so that the waterproof plugging agent with high elasticity, strong adhesive force and high viscosity of a paint film can be formed. In addition, the embodiment of the invention takes the corn stalk fiber, the cellulose acetate and the acrylic fiber as raw materials, the fiber expansion state of the corn stalk fiber is further expanded under the vacuum heating condition, and the injected silica sol forms a net structure together with the cellulose acetate and the acrylic fiber in the stirring process, so that the toughness and the strength of the fiber material can be ensured, and meanwhile, the waterproof performance is improved.
The technical effects of the waterproof plugging agent of the embodiment of the present invention will be further described below by referring to specific examples.
Example 1
In this embodiment, a specific preparation method of the waterproof plugging agent includes the following steps:
respectively weighing 48kg of dispersion medium, 22kg of hydrocarbon resin, 0.8kg of SBS rubber, 16kg of modified fiber material, 10kg of powder material and 0.01kg of inorganic aluminum salt waterproof agent for later use;
the weighed dispersion medium (specifically toluene) is put into a proportioning cylinder, then raw materials of hydrocarbon resin and SBS rubber are put into the proportioning cylinder and stirred for 30 minutes through a powder machine, the mixture is dispersed for 30 minutes at the rotating speed of 80 r/min, then modified fiber material and powder are added, the rotating speed is adjusted to about 1000 r/min through the powder machine and stirred for 40 minutes, then inorganic aluminum salt waterproof agent is added and stirred uniformly to form a product, and the product is filled into a fogging bottle for use.
In the present embodiment, the hydrocarbon resin is a C9 aromatic petroleum resin. The preparation method of the modified fiber material comprises the steps of placing corn straw fiber, cellulose acetate and acrylic fiber in a sealed container according to the mass ratio of 1:1:2, vacuumizing to be not more than 0.03MPa, stirring while injecting excessive silica sol, uniformly mixing, preserving heat at 50 ℃ for 5 hours, and standing to obtain the modified fiber material. The preparation method of the powder material comprises the steps of weighing 15kg of modified slag powder, 8kg of calcite powder, 40kg of heavy calcium powder, 30kg of titanium dioxide and 15kg of calcined kaolin, mixing the modified slag powder, the calcite powder, the heavy calcium powder, the titanium dioxide and the calcined kaolin, and grinding the mixture to obtain the powder material.
In this embodiment, the preparation method of the modified slag powder includes adding water, which is 10 times the weight of the slag powder, into the slag powder, mixing uniformly, adding sulfuric acid (which is 0.01 times the weight of the slag powder) dropwise to perform ultrasonic dispersion (the ultrasonic output power is 400W, and the ultrasonic time is 40min), adding cetyl trimethyl ammonium bromide and urea (the total amount of the added sulfuric acid is 0.01 times the weight of the slag powder, wherein the mass ratio of the cetyl trimethyl ammonium bromide to the urea is 1:1), mixing uniformly, heating to 40 ℃, taking out, and drying to obtain the modified slag powder.
Example 2
In this embodiment, a specific preparation method of the waterproof plugging agent includes the following steps:
respectively weighing 75kg of dispersion medium, 40kg of hydrocarbon resin, 1.8kg of SBS rubber, 28kg of modified fiber material, 18kg of powder material and 0.05kg of inorganic aluminum salt waterproof agent for later use;
the weighed dispersion medium (specifically toluene) is put into a proportioning cylinder, then raw materials of hydrocarbon resin and SBS rubber are put into the proportioning cylinder and stirred for 40 minutes through a powder machine, the raw materials are dispersed for 40 minutes at the rotating speed of 100 r/min, then modified fiber material and powder are added, the rotating speed is adjusted to about 2000 r/min through a dispersion machine, the mixture is stirred for 20 minutes, then inorganic aluminum salt waterproof agent is added, the mixture is uniformly stirred to form a product, and the product is placed into a fog bottle for use.
In the present embodiment, the hydrocarbon resin is a C9 aromatic petroleum resin. The preparation method of the modified fiber material comprises the steps of placing corn straw fiber, cellulose acetate and acrylic fiber in a sealed container according to the mass ratio of 3:5:4, vacuumizing to be not more than 0.03MPa, stirring while injecting excessive silica sol, uniformly mixing, preserving heat at 80 ℃ for 8 hours, and standing to obtain the modified fiber material. The preparation method of the powder material comprises the steps of weighing 25kg of modified slag powder, 12kg of calcite powder, 60kg of heavy calcium powder, 48kg of titanium dioxide and 25kg of calcined kaolin, mixing the modified slag powder, the calcite powder, the heavy calcium powder, the titanium dioxide and the calcined kaolin, and grinding the mixture to obtain the powder material.
In this embodiment, the preparation method of the modified slag powder includes adding water in an amount which is 12 times the weight of the slag powder into the slag powder, uniformly mixing, dropwise adding sulfuric acid (the addition amount is 0.1 time of the weight of the slag powder) to perform ultrasonic dispersion (the ultrasonic output power is 800W, the ultrasonic time is 200min), then adding cetyl trimethyl ammonium bromide and urea (the addition amount is 0.04 time of the weight of the slag powder, wherein the mass ratio of the cetyl trimethyl ammonium bromide to the urea is 1:50), uniformly mixing, heating to 80 ℃, taking out, and drying to obtain the modified slag powder.
Example 3
In this embodiment, a specific preparation method of the waterproof plugging agent includes the following steps:
respectively weighing 50kg of dispersion medium, 26kg of hydrocarbon resin, 1kg of SBS rubber, 20kg of modified fiber material, 12kg of powder material and 0.02kg of inorganic aluminum salt waterproof agent for later use;
the weighed dispersion medium (specifically dimethylbenzene) is put into a proportioning cylinder, then raw materials of hydrocarbon resin and SBS rubber are put into the proportioning cylinder and stirred for 30 minutes through a powder machine, the mixture is dispersed for 30 minutes at the rotating speed of 80 r/min, then modified fiber material and powder are added, the rotating speed is adjusted to about 1200 r/min through the powder machine and stirred for 40 minutes, then an inorganic aluminum salt waterproof agent is added and stirred uniformly to form a product, and the product is filled into a fogging bottle for use.
In the present embodiment, the hydrocarbon resin is a C5 aliphatic petroleum resin. The preparation method of the modified fiber material comprises the steps of placing corn straw fibers, cellulose acetate and acrylic fibers in a sealed container according to the mass ratio of 3:2:2.5, vacuumizing to 0.01MPa, stirring while injecting excessive silica sol, uniformly mixing, preserving heat at 65 ℃ for more than 4 hours, and standing to obtain the modified fiber material. The preparation method of the powder material comprises the steps of weighing 20kg of modified slag powder, 10kg of calcite powder, 50kg of heavy calcium powder, 40kg of titanium dioxide and 20kg of calcined kaolin, mixing the modified slag powder, the calcite powder, the heavy calcium powder, the titanium dioxide and the calcined kaolin, and grinding the mixture to obtain the powder material.
In this embodiment, the preparation method of the modified slag powder includes adding water, which is not less than 10 times of the weight of the slag powder, into the slag powder, uniformly mixing, then dropwise adding sulfuric acid (the addition amount is 0.03 times of the weight of the slag powder) to perform ultrasonic dispersion (the ultrasonic output power is 600W, the ultrasonic time is 100min), then adding cetyl trimethyl ammonium bromide and urea (the addition amount is 0.02 times of the weight of the slag powder, wherein the mass ratio of the cetyl trimethyl ammonium bromide to the urea is 1:15), uniformly mixing, heating to 65 ℃, taking out, and drying to obtain the modified slag powder.
Example 4
The test piece was the same as example 3 except that the waterproof plugging agent was prepared from 70kg of a dispersion medium, 36kg of hydrocarbon resin, 1.5kg of SBS rubber, 24kg of modified fiber material, 16kg of powder material and 0.04kg of an inorganic aluminum salt water repellent as the raw materials in example 3.
Example 5
The test piece was the same as example 3 except that the waterproof plugging agent used in example 3 was prepared from 60kg of a dispersion medium, 30kg of a hydrocarbon resin, 1.3kg of SBS rubber, 22kg of a modified fiber material, 15kg of a powdery material, and 0.03kg of an inorganic aluminum salt water repellent.
Example 6
In this embodiment, a specific preparation method of the waterproof plugging agent includes the following steps:
respectively weighing 62kg of dispersion medium, 32kg of hydrocarbon resin, 1.3kg of SBS rubber, 19kg of modified fiber material, 14kg of powder material and 0.01kg of inorganic aluminum salt waterproof agent for later use;
the weighed dispersion medium (specifically dimethylbenzene) is put into a proportioning cylinder, then raw materials of hydrocarbon resin and SBS rubber are put into the proportioning cylinder and stirred for 30 minutes through a powder machine, the mixture is dispersed for 30 minutes at the rotating speed of 80 r/min, then modified fiber material and powder are added, the rotating speed is adjusted to about 1200 r/min through the powder machine and stirred for 40 minutes, then an inorganic aluminum salt waterproof agent is added and stirred uniformly to form a product, and the product is filled into a fogging bottle for use.
In the present embodiment, the hydrocarbon resin is a C5 aliphatic petroleum resin. The preparation method of the modified fiber material comprises the steps of placing corn straw fibers, cellulose acetate and acrylic fibers in a sealed container according to the mass ratio of 3:1:2.5, vacuumizing to 0.01MPa, stirring while injecting excessive silica sol, uniformly mixing, preserving heat at 65 ℃ for more than 4 hours, and standing to obtain the modified fiber material. The preparation method of the powder material comprises the steps of weighing 20kg of modified slag powder, 10kg of calcite powder, 50kg of heavy calcium powder, 40kg of titanium dioxide and 20kg of calcined kaolin, mixing the modified slag powder, the calcite powder, the heavy calcium powder, the titanium dioxide and the calcined kaolin, and grinding the mixture to obtain the powder material.
In this embodiment, the preparation method of the modified slag powder includes adding water, which is not less than 10 times of the weight of the slag powder, into the slag powder, uniformly mixing, then dropwise adding sulfuric acid (the addition amount is 0.03 times of the weight of the slag powder) to perform ultrasonic dispersion (the ultrasonic output power is 600W, the ultrasonic time is 100min), then adding cetyl trimethyl ammonium bromide and urea (the addition amount is 0.02 times of the weight of the slag powder, wherein the mass ratio of the cetyl trimethyl ammonium bromide to the urea is 1:25), uniformly mixing, heating to 65 ℃, taking out, and drying to obtain the modified slag powder.
Example 7
The test piece was the same as example 6 except that the waterproof plugging agent was prepared from 72kg of a dispersion medium, 38kg of hydrocarbon resin, 1.7kg of SBS rubber, 26kg of modified fiber material, 17kg of powder material and 0.04kg of an inorganic aluminum salt water repellent as the raw materials of example 6.
Example 8
The same as example 7 except that xylene was replaced with toluene, as compared with example 7.
Example 9
The same procedure as in example 7 was repeated, except that the xylene was replaced with ethyl acetate, as compared with example 7.
Example 10
The procedure was repeated as in example 7 except that xylene was replaced with toluene, xylene and ethyl acetate to prepare a mixed solution, which was mixed in an equal amount by weight as compared with example 7.
Example 11
The process was performed in the same manner as in example 7 except that the aliphatic petroleum resin C5 was replaced with an alicyclic petroleum resin, as compared with example 7.
Example 12
The same as in example 7, except that the aliphatic petroleum resin C5 was replaced with an α -methylstyrene resin, as compared with example 7.
Example 13
The same as example 7 was conducted except that pentafluoroethane as a propellant was further included in the waterproof plugging agent in an amount of 1 time the mass of the hydrocarbon resin as compared with example 7.
Example 14
The same as example 7 except that pentafluoroethane of 1.4 times the mass of the hydrocarbon resin was further included as a propellant in the waterproof plugging agent as compared with example 7.
Example 15
The same as example 7 except that pentafluoroethane of 1.8 times the mass of the hydrocarbon resin was further included as a propellant in the waterproof plugging agent as compared with example 7.
Example 16
Compared with the example 6, the preparation method of the modified slag powder is the same as that of the example 6 except that the modified slag powder is prepared by adding water 15 times the weight of the slag powder into the slag powder, uniformly mixing, dropwise adding sulfuric acid (the addition is 0.04 times of the weight of the slag powder) to perform ultrasonic dispersion (the ultrasonic output power is 600W, the ultrasonic time is 100min), then adding cetyl trimethyl ammonium bromide and urea (the addition is 0.015 time of the total weight of the slag powder, wherein the mass ratio of the cetyl trimethyl ammonium bromide to the urea is 1:5), uniformly mixing, heating to 70 ℃, taking out and drying, thus obtaining the modified slag powder, and the other steps are the same as those of the example 6.
Comparative example 1
The procedure of example 3 was repeated except that the waterproof plugging agent used in example 3 was prepared from 60kg of a dispersion medium, 30kg of a hydrocarbon resin, 1.3kg of SBS rubber, 15kg of a powdery material, and 0.03kg of an inorganic aluminum salt water repellent. That is, the sample of example 5 containing no modified fiber material was used as comparative example 1.
Comparative example 2
The test piece was the same as example 3 except that the waterproof plugging agent used in example 3 was composed of 60kg of a dispersion medium, 30kg of hydrocarbon resin, 22kg of modified fiber material, 15kg of powder, and 0.03kg of an inorganic aluminum salt water repellent. That is, the sample of example 5 containing no SBS rubber was taken as comparative example 2.
Comparative example 3
The same as example 5 except that SBS rubber and the modified fiber material were not contained, as compared with example 5.
Comparative example 4
The same procedure as in example 5 was repeated except that the powder was a heavy calcium powder alone, as compared with example 5.
Comparative example 5
The procedure of example 5 was repeated, except that calcined kaolin was used alone as the powder in comparison with example 5.
Comparative example 6
The same as example 5 was repeated, except that the modified slag powder in the raw material of the powdery material was replaced with the ordinary slag powder, as compared with example 5.
Performance detection
In order to observe whether the curing of the waterproof plugging agent prepared in the embodiment of the present invention is rapid, the waterproof plugging agents prepared in the embodiments 1 to 5 were subjected to curing detection. Specifically, the waterproof plugging agents prepared in examples 1 to 5 were respectively put into a fogging bottle, pentafluoroethane of the same weight as that of the hydrocarbon resin in the waterproof plugging agent was injected into the fogging bottle as a propellant, and then sprayed onto a wall surface and placed at room temperature to calculate the time for forming a uniform cured film, which was counted in table 1 as a surface drying time.
TABLE 1 film formation time results Table
Group of Temperature of Open time
Example 1 25℃ <10h
Example 2 26℃ <10h
Example 3 25℃ <10h
Example 4 24℃ <10h
Example 5 26℃ <10h
According to the data provided in the table 1, the surface drying time of the waterproof plugging agent provided by the embodiment of the invention is short, and the waterproof plugging agent has good construction performance.
Next, in order to investigate the influence of different raw materials on the product performance, the waterproof performance and compressive strength of the waterproof plugging agent prepared in example 5 and the samples prepared in comparative examples 1 to 3 were respectively tested by referring to the method in the national standard GB 23440-. The impervious pressure of the coating test piece is that the coating test piece which is prepared according to 6.5.1 and cured to the age of 7d is taken out, washed clean, air-dried on the surface and subjected to impervious test according to the method of 6.5.1.2. If the pressure is increased to 1.5MPa, the pressure is kept constant for 1 hour, and the pressure is increased after stopping. The anti-seepage pressure of the coating test piece is the maximum water pressure when no water seepage occurs in four of six test pieces in each group. Specific results are shown in table 2.
TABLE 2 waterproof Property test results Table
Group of Coating resistance to pressure (MPa)
Example 5 2.9
Comparative example 1 2.2
Comparative example 2 1.8
Comparative example 3 1.2
As can be seen from the data in Table 2, in the embodiment of the invention, the hydrocarbon resin and the SBS rubber are used as crosslinking matrix materials, the crosslinking network is formed by dissolving in the dispersion medium, and the waterproof reinforcing effect of the modified fiber material is matched, so that the waterproof plugging agent with high paint film elasticity, strong adhesive force and high viscosity can be formed, and the compressive strength is improved while the waterproof performance is ensured.
The compression strength is measured by pressing the waterproof plugging agent prepared in the example 5 and the samples prepared in the comparative examples 4 to 6 into test pieces of 40mm × 40mm × 160mm, and measuring the compression strength according to GB/T17671. Specific results are shown in table 3.
TABLE 3 compressive strength test results table
Group of Compressive strength (MPa)
Example 5 18
Comparative example 4 8
Comparative example 5 9
Comparative example 6 14
As can be seen from the data in table 3, in the embodiment of the present invention, the modified slag powder, the calcite powder, the triple superphosphate powder, the titanium dioxide powder, and the calcined kaolin are mixed and ground to form the powder, compared with a method in which one of the triple superphosphate powder, the titanium dioxide powder, the calcined kaolin, and the like is singly used, the compressive strength of the waterproof plugging agent can be effectively improved, and meanwhile, the hydraulic gelation property of the modified slag powder can play a good role in a framework, so as to further improve the compressive strength.
While the preferred embodiments of the present invention have been described in detail, the embodiments of the present invention are not limited to the above embodiments, and various changes can be made without departing from the spirit of the embodiments of the present invention within the knowledge of those skilled in the art. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the embodiments of the present invention are still within the scope of the embodiments of the present invention as thus claimed.

Claims (6)

1. The waterproof plugging agent is characterized in that raw materials of the waterproof plugging agent at least comprise a dispersion medium and a base material which is dispersed in the dispersion medium and forms a uniform material;
wherein the base material at least comprises the following raw materials: hydrocarbon resin, SBS rubber, modified fiber material, powder and inorganic aluminum salt waterproof agent; the modified fiber material is prepared by taking corn straw fiber, cellulose acetate and acrylic fiber as raw materials and injecting silica sol under the vacuum heating condition;
the waterproof plugging agent comprises the following raw materials in parts by weight: 48-75 parts of dispersion medium, 22-40 parts of hydrocarbon resin, 0.8-1.8 parts of SBS rubber, 16-28 parts of modified fiber material, 10-18 parts of powder material and 0.01-0.05 part of inorganic aluminum salt waterproof agent;
the specific preparation method of the modified fiber material comprises the steps of putting corn straw fiber, cellulose acetate and acrylic fiber in a sealed container according to the mass ratio of 1-3:1-5:2-4, vacuumizing until the vacuum degree is not more than 0.03MPa, then injecting silica sol, mixing uniformly, and then preserving heat at 50-80 ℃ to obtain the modified fiber material;
the powder material at least comprises 15-25 parts of modified slag powder, 8-12 parts of calcite powder, 40-60 parts of heavy calcium powder, 30-48 parts of titanium dioxide and 15-25 parts of calcined kaolin according to parts by weight;
the preparation method of the modified slag powder comprises the steps of adding water into the slag powder, uniformly mixing, adding sulfuric acid, performing ultrasonic dispersion to acidify the slag powder, adding cetyl trimethyl ammonium bromide and urea, uniformly mixing, heating and drying to obtain the modified slag powder.
2. The waterproof plugging agent as claimed in claim 1, wherein the waterproof plugging agent comprises the following raw materials in parts by weight: 50-70 parts of dispersion medium, 26-36 parts of hydrocarbon resin, 1-1.5 parts of SBS rubber, 20-24 parts of modified fiber material, 12-16 parts of powder material and 0.02-0.04 part of inorganic aluminum salt waterproof agent.
3. The waterproof plugging agent as claimed in claim 1, wherein the waterproof plugging agent further comprises a proper amount of propellant.
4. The waterproof plugging agent according to claim 1, wherein the dispersion medium is any one or more of toluene, xylene and ethyl acetate.
5. A preparation method of the waterproof plugging agent as described in any one of claims 1 to 4, characterized by comprising the following steps:
1) adding hydrocarbon resin and SBS rubber into the dispersion medium, and mixing uniformly to obtain a mixture;
2) and adding the modified fiber material and the powder material into the mixture according to a ratio, pulping and mixing, and adding the inorganic aluminum salt waterproof agent for uniformly mixing to obtain the waterproof plugging agent.
6. The waterproof plugging agent prepared by the preparation method of the waterproof plugging agent according to claim 5.
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CN106753684A (en) * 2016-12-25 2017-05-31 常州创索新材料科技有限公司 A kind of method that utilization blast furnace slag prepares the burning chemistry chains carrier of oxygen

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