CN111777913A - Preparation method of electrostatic protection epoxy self-leveling colored sand - Google Patents
Preparation method of electrostatic protection epoxy self-leveling colored sand Download PDFInfo
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Abstract
The invention relates to the field of building material preparation, in particular to a preparation method of electrostatic protection epoxy self-leveling colored sand; the amidated conductive graphite auxiliary agent provided by the invention is a conductive carbon nano tube, is obtained by surface modification after combination and compounding of graphene and graphite micropowder, has good dispersibility and strong conductivity, and can well reduce the resistance of epoxy self-leveling colored sand and eliminate static electricity; compared with the epoxy self-leveling colored sand in the existing market, the amidated conductive graphite auxiliary agent is added, so that the resistance of the epoxy self-leveling colored sand is greatly reduced, the problem of static accumulation of the bottom plate surface is effectively solved, and the phenomenon that the terrace accumulates a large amount of static charges due to frequent friction to interfere the work of a precision instrument and even cause fire and explosion accidents is prevented; the electrostatic protection epoxy self-leveling colored sand adopts steel slag-based artificial colored sand, and has the performances of good wear resistance and scratch resistance, skid resistance, heavy pressure resistance, impact resistance and the like.
Description
Technical Field
The invention relates to the field of preparation of building materials, in particular to a preparation method of electrostatic protection epoxy self-leveling colored sand.
Background
The terrace is an integral surface layer and a construction system thereof which play a role in wear resistance, decoration, cleanness, corrosion resistance and the like on the surface of the building ground, and becomes an indispensable important component of industrial and commercial building infrastructure along with the development of modern industrial technology and the requirements of industrial production and high-quality life. The epoxy self-leveling color sand terrace is a terrace system which protects and decorates the ground surface or can play a certain special function by coating the ground surface such as cement mortar, concrete, stone or steel plates. The special dust-proof and dust-proof floor has the characteristics of special functionality, stratum sealing, dust prevention and economy, is mainly used for industrial floor projects, and is less applied to commercial floor projects.
CN107268946A relates to a color sand epoxy self-leveling construction process, which comprises the steps of treating a base layer, leveling a concrete base surface by mortar or putty, and shoveling or grinding an ultra-high position and a protruding point; performing primary coating treatment, namely brushing two epoxy floor primary coatings on the concrete base surface, wherein the brushing thickness of the first epoxy floor primary coating is 0.1-0.3mm, the curing time is 12-24 hours, the brushing thickness of the second epoxy floor primary coating is 0.1-0.3mm, and the curing time is 12-24 hours, so as to obtain a primary coating base surface; preparing a colored sand resin mixture, mixing an epoxy resin synthetic agent and an epoxy curing agent according to the mass ratio of 3-5: 1, adding colored sand and an auxiliary material additive, and uniformly stirring to obtain a colored sand resin mixture; spreading slurry, pouring the color sand resin mixture on the base surface, scraping, defoaming, and curing at 15-30 deg.C for 20-30 hr. After the epoxy resin base coat is smeared on the concrete base surface, a thick high-strength epoxy floor product can be obtained only by pouring and scraping a layer of color sand resin, so that the overall construction time is greatly shortened, and the construction cost is reduced.
CN106316216A provides an epoxy self-leveling color sand coating, which comprises the following components in parts by weight: the component B is prepared by mixing the components in a ratio of 5-6.5: 1, and the epoxy self-leveling finishing paint has the advantages of beautiful appearance, simple construction and the like, meets the requirement of easy cleaning of offices, and is convenient to adjust colors. But scratches are easy to scrape on the surface of the epoxy self-leveling finish paint, and dirt is easy to store after the scratches appear, so that the epoxy self-leveling finish paint is difficult to clean. The invention has no obvious scratch, is wear-resistant, weak acid-base resistant and can inhibit the breeding of the mould. Compared with common epoxy self-leveling finish paint and traditional color sand, the epoxy self-leveling color sand has the advantages of good wear resistance and scratch resistance, skid resistance, heavy pressure resistance and impact resistance; the color is freely matched, the color is soft, the decorative effect is good, and the most important is high cleanness, no connecting seam and capability of meeting KGMP detection requirements.
CN108948952A discloses a solvent-free color sand self-leveling finish paint which comprises the following components in parts by weight: 50-60 parts of epoxy resin; 3-8 parts of a diluent; 10-15 parts of colored sand; 15-20 parts of talcum powder; 0.5-3 parts of a silane coupling agent; 20-25 parts of a curing agent; 1-2 parts of a leveling agent; 0.1-3 parts of an auxiliary agent. The solvent-free color sand self-leveling finish paint has short curing time, solves the problem of complex sand-pressing process of the traditional color sand finish paint in a self-leveling mode, enables the color sand and the talcum powder to be better dispersed in the epoxy resin due to the use of the silane coupling agent, improves the attractiveness of the product due to the addition of the color sand and the talcum powder, ensures the compression resistance and the wear resistance of the product, ensures the corrosion resistance and the impact resistance of the product due to the selection of the epoxy resin, has good compression resistance, impact resistance, corrosion resistance and wear resistance, and attractive appearance, and has no solvent volatilization, environmental pollution prevention and human health protection.
The epoxy self-leveling color sand products prepared by the invention and the prior patent have very large resistance, are easy to cause static accumulation, have very large potential safety hazard in the electronic industry, use the conductive graphite, have poor compatibility with an epoxy resin system, and have agglomeration, thereby influencing and limiting the application of the epoxy self-leveling color sand to high-end terraces in the field of the electronic industry.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of electrostatic protection epoxy self-leveling colored sand.
A preparation method of electrostatic protection epoxy self-leveling colored sand mainly adopts the following scheme:
according to the mass parts, 55-68 parts of epoxy resin, 5-10 parts of talcum powder and 0.5-3.1 parts of amidated conductive graphite auxiliary agent are put into a high-speed mixer to be stirred at a high speed, the stirring speed is controlled to be 500 plus materials/min, the stirring temperature is controlled to be 40-60 ℃, 42-57 parts of artificial colored sand is put into the high-speed mixer to be uniformly stirred after being stirred for 20-30min, and the stirring is continued for 15-45 min; after the preparation, 3 to 8 parts of diluent, 0.3 to 0.8 part of dispersant, 0.4 to 0.7 part of defoaming agent, 0.3 to 0.7 part of polybutyl acrylate powder solid leveling agent and 0.3 to 5 parts of toughening agent polybutadiene rubber are put into a high-speed mixer, mixed and stirred for 30 to 60min, added with 3 to 8 parts of pigment and stirred uniformly to obtain the electrostatic protection epoxy self-leveling colored sand.
A preparation method of acyl chloride conductive graphite micropowder comprises the following steps;
adding 50-80 parts by mass of conductive graphite micropowder into 800 parts by mass of 30-40% sodium hydroxide solution, uniformly stirring, slowly adding 150 parts by mass of 15-20% hydrogen peroxide into a reaction kettle, controlling the addition for 30-60min, controlling the temperature to be 40-60 ℃ after the addition, reacting for 45-90min, cooling to room temperature, standing for 5-10h, filtering, washing to be neutral, drying, adding 300 parts by mass of 8-12% citric acid aqueous solution, uniformly mixing, controlling the temperature to be 40-60 ℃ for reacting for 1-5h, slowly dropwise adding thionyl chloride, uniformly stirring at 50-70 ℃ for reacting for 4-10h, filtering the solution to remove the solvent, washing the solid product with absolute ethyl alcohol, and fully drying, and preparing the acyl chloride conductive graphite micro powder.
The preparation method of the amidated conductive graphite additive comprises the following steps of;
adding 50-80 parts by mass of acyl chloride conductive graphite micro powder, 0.5-2 parts by mass of N, 1-dimethylpyrrolidine-3-amine, 2.2-4.8 parts by mass of 2-aminothiophene azole, 2-5 parts by mass of sodium hydroxide and 2000 parts by mass of water into a reaction kettle, stirring for 30-90 minutes at the temperature of 60-70 ℃, washing with deionized water, carrying out suction filtration and dehydration, and drying to obtain the amidated conductive graphite auxiliary agent.
The acyl chloride graphene and N, 1-dimethylpyrrolidine-3-amine carry out substitution reaction, and part of reaction mechanism is shown as follows:
and the acyl chloride graphene and the 2-aminothiophene azole are subjected to substitution reaction, and part of the reaction mechanism is shown as
The artificial colored sand is prepared by uniformly mixing 130 parts by mass of steel slag, 10-18 parts by mass of cement, 7-12 parts by mass of fly ash, 0.1-0.5 part by mass of methyl cellulose and 0.7-1.8 part by mass of latex powder, adding 10-20 parts by mass of water, uniformly stirring, maintaining for 5-10 days, molding and drying.
The epoxy resin is 828 epoxy resin or 128 epoxy resin.
The diluent is 1, 4-butanediol diglycidyl ether or polypropylene glycol diglycidyl ether or 1, 6-hexanediol diglycidyl ether.
The dispersant is methyl amyl alcohol or polyacrylamide or fatty acid polyglycol ester.
The defoaming agent is polyoxyethylene polyoxypropylene amine ether or polyoxypropylene glycerol ether or polyoxypropylene polyoxyethylene glycerol ether.
The electrostatic protection epoxy self-leveling color sand is matched with an epoxy self-leveling color sand curing agent for use.
The preparation method of the electrostatic protection epoxy self-leveling colored sand provided by the invention is good in dispersing performance and strong in conductivity, and can well reduce the resistance of the epoxy self-leveling colored sand and eliminate static electricity; compared with the epoxy self-leveling colored sand in the existing market, the amidated conductive graphite auxiliary agent is added, the substitution reaction is carried out on the acyl chloride graphene and N, 1-dimethylpyrrolidine-3-amine, and the substitution reaction is carried out on the acyl chloride graphene and 2-aminothiophene azole, so that the resistance of the epoxy self-leveling colored sand is greatly reduced, the problem of electrostatic accumulation of the bottom plate surface is effectively solved, and the phenomenon that a floor is interfered by precision instruments and even fires and explosions are caused due to the fact that the floor is frequently rubbed and accumulated with a large amount of electrostatic charges is prevented; the electrostatic protection epoxy self-leveling colored sand adopts steel slag-based artificial colored sand, and has the performances of good wear resistance and scratch resistance, skid resistance, heavy pressure resistance, impact resistance and the like.
Drawings
FIG. 1 is a Fourier infrared spectrum of the amidated conductive graphite aid prepared in example 3.
At 1660cm-1The absorption peak of carbonyl exists nearby, which indicates that the acyl chloride conductive graphite micropowder participates in the reaction; at 1300cm-1The absorption peak of the carbon-nitrogen single bond of the amide exists nearby, and is 729cm-1An absorption peak of a carbon-sulfur bond exists nearby, which indicates that the 2-aminothiophenazole participates in the reaction; at 2929cm-1The expansion and contraction absorption peak of the hydrocarbon exists nearby, and is 1056cm-1An absorption peak of a carbon-nitrogen single bond exists nearby, which indicates that N, 1-dimethylpyrrolidin-3-amine participates in the reaction.
Detailed Description
The invention is further illustrated by the following specific examples:
the electrostatic protection epoxy self-leveling color sand prepared in the experiment and the epoxy self-leveling color sand H-302 mixed amine epoxy curing are uniformly mixed according to the mass ratio of 5:1 and then cured, the performance is measured, the wear resistance is measured according to ISO7784-2:1997, and the model of the used rubber sand is CS-17. The surface resistance of the material was measured according to GB/T1410.
The high-speed mixer is an HTSHR-5L high-speed mixer.
Example 1
A preparation method of electrostatic protection epoxy self-leveling colored sand mainly adopts the following scheme:
putting 550g of epoxy resin, 50g of talcum powder and 5g of amidated conductive graphite auxiliary agent into a high-speed mixer, stirring at a high speed of 500r/min and a stirring temperature of 40 ℃ for 20min, putting 420g of artificial colored sand into the high-speed mixer, stirring uniformly, and continuing to stir for 15 min; and after the preparation, putting 30g of diluent, 3g of dispersing agent, 4g of defoaming agent, 3g of polybutyl acrylate powder solid flatting agent and 3g of toughening agent polybutadiene rubber into a high-speed mixer, mixing and stirring for 30min, adding 30g of pigment, and uniformly stirring to obtain the electrostatic protection epoxy self-leveling colored sand.
A preparation method of acyl chloride conductive graphite micropowder comprises the following steps;
adding 50g of conductive graphite micropowder into 500g of 30% sodium hydroxide solution by mass, uniformly stirring, slowly adding 100g of 15% hydrogen peroxide by mass into a reaction kettle, controlling the addition for 30min, controlling the temperature to be 40 ℃ after the addition, reacting for 45min, cooling to room temperature, standing for 5h, filtering, washing to be neutral, drying, adding 200g of 8% citric acid aqueous solution by mass, uniformly mixing, controlling the temperature to be 40 ℃, reacting for 1h, slowly dropwise adding thionyl chloride, stirring at 50 ℃ for reacting for 4h, filtering the solution to remove the solvent, washing the solid product by using absolute ethyl alcohol, fully drying, and preparing the acyl chloride conductive graphite micropowder.
The preparation method of the amidated conductive graphite additive comprises the following steps of;
adding 50g of acyl chloride conductive graphite micro powder, 0.5g of N, 1-dimethylpyrrolidine-3-amine, 2.2g of 2-aminothiophene oxazole, 2g of sodium hydroxide and 1000g of water into a reaction kettle, stirring for 30 minutes at 60 ℃, washing with deionized water, carrying out suction filtration and dehydration, and drying to obtain the amidated conductive graphite auxiliary agent.
The epoxy resin is 828 epoxy resin.
The diluent is 1, 4-butanediol diglycidyl ether.
The dispersant is methyl amyl alcohol.
The defoaming agent is polyoxyethylene polyoxypropylene ether.
The electrostatic protection epoxy self-leveling color sand is matched with an epoxy self-leveling color sand curing agent for use.
The product of the cured electrostatic protection epoxy self-leveling color sand prepared by the experiment has the wear resistance of 18(750 g.500 r)/mg and the surface resistance of 3.4 × 106Ω。
Example 2
A preparation method of electrostatic protection epoxy self-leveling colored sand mainly adopts the following scheme:
putting 620g of epoxy resin, 80g of talcum powder and 23g of amidated conductive graphite auxiliary agent into a high-speed mixer, stirring at a high speed of 600r/min and a stirring temperature of 50 ℃ for 25min, putting 500g of artificial colored sand into the high-speed mixer, stirring uniformly, and continuing to stir for 250 min; and after the electrostatic protection epoxy self-leveling colored sand is finished, putting 60g of diluent, 5g of dispersing agent, 6g of defoaming agent, 4g of polybutyl acrylate powder solid leveling agent and 25g of toughening agent polybutadiene rubber into a high-speed mixer, mixing and stirring for 40min, adding 60g of pigment, and uniformly stirring to obtain the electrostatic protection epoxy self-leveling colored sand.
A preparation method of acyl chloride conductive graphite micropowder comprises the following steps;
adding 60g of conductive graphite micropowder into 700g of 35% sodium hydroxide solution by mass percent, stirring uniformly, slowly adding 120g of 18% hydrogen peroxide by mass percent into a reaction kettle, controlling the addition for 40min, controlling the temperature to 45 ℃ after the addition, reacting for 60min, cooling to room temperature, standing for 8h, filtering, washing to be neutral, drying, adding 260g of 10% citric acid aqueous solution by mass percent, mixing uniformly, controlling the temperature to be 46 ℃, reacting for 3h, slowly dropwise adding thionyl chloride, stirring at 55 ℃ for reacting for 6h, filtering the solution to remove the solvent, washing the solid product by using absolute ethyl alcohol, fully drying, and preparing the acyl chloride conductive graphite micropowder.
The preparation method of the amidated conductive graphite additive comprises the following steps of;
70g of acyl chloride conductive graphite micro powder, 1g of N, 1-dimethylpyrrolidine-3-amine, 3.5g of 2-aminothiophene azole, 3g of sodium hydroxide and 1300g of water are added into a reaction kettle, stirred for 60 minutes at 66 ℃, washed by deionized water, filtered, dehydrated and dried. And obtaining the amidated conductive graphite additive.
The artificial colored sand is prepared by uniformly mixing 120g of steel slag, 14g of cement, 9g of fly ash, 0.3g of methyl cellulose and 1.2g of latex powder, adding 15g of water, uniformly stirring, maintaining for 8 days, forming and drying.
The epoxy resin is 128 epoxy resin.
The diluent is polypropylene glycol diglycidyl ether.
The dispersant is polyacrylamide.
The defoaming agent is polyoxypropylene glycerol ether.
The electrostatic protection epoxy self-leveling color sand is matched with an epoxy self-leveling color sand curing agent for use.
The product of the cured electrostatic protection epoxy self-leveling color sand prepared by the experiment has the wear resistance of 16(750 g.500 r)/mg and the surface resistance of 2.8 × 106Ω。
Example 3
A preparation method of electrostatic protection epoxy self-leveling colored sand mainly adopts the following scheme:
680g of epoxy resin, 100g of talcum powder and 31g of amidated conductive graphite auxiliary agent are put into a high-speed mixer to be stirred at a high speed, the stirring speed is controlled to be 700r/min, the stirring temperature is controlled to be 60 ℃, 570g of artificial colored sand is put into the high-speed mixer to be stirred uniformly after stirring for 30min, and stirring is continued for 45 min; and after the electrostatic protection epoxy self-leveling colored sand is finished, putting 80g of diluent, 8g of dispersing agent, 7g of defoaming agent, 7g of polybutyl acrylate powder solid leveling agent and 50g of toughening agent polybutadiene rubber into a high-speed mixer, mixing and stirring for 60min, adding 80g of pigment, and uniformly stirring to obtain the electrostatic protection epoxy self-leveling colored sand.
A preparation method of acyl chloride conductive graphite micropowder comprises the following steps;
adding 80g of conductive graphite micropowder into 800g of 40% sodium hydroxide solution by mass percent, uniformly stirring, slowly adding 150g of 20% hydrogen peroxide by mass percent into a reaction kettle, controlling the addition for 60min, controlling the temperature to be 60 ℃ after the addition is finished, reacting for 90min, cooling to room temperature, standing for 10h, filtering, washing to be neutral, drying, adding 300g of 12% citric acid aqueous solution by mass percent, uniformly mixing, controlling the temperature to be 60 ℃, reacting for 5h, slowly dropwise adding thionyl chloride, stirring and reacting for 10h at 70 ℃, filtering the solution to remove the solvent, washing the solid product by using absolute ethyl alcohol, fully drying, and preparing the acyl chloride conductive graphite micropowder.
The preparation method of the amidated conductive graphite additive comprises the following steps of;
adding 80g of acyl chloride conductive graphite micro powder, 2g of N, 1-dimethylpyrrolidine-3-amine, 4.8g of 2-aminothiophene oxazole, 5g of sodium hydroxide and 2000g of water into a reaction kettle, stirring for 90 minutes at 0 ℃, then washing with deionized water, carrying out suction filtration and dehydration, and drying to obtain the amidated conductive graphite auxiliary agent.
The artificial colored sand is prepared by uniformly mixing 130g of steel slag, 18g of cement, 12g of fly ash, 0.5g of methyl cellulose and 1.8g of latex powder, adding 20g of water, uniformly stirring, maintaining for 10 days, forming and drying.
The epoxy resin is 28 epoxy resin.
The diluent is 1, 6-hexanediol diglycidyl ether.
The dispersant is fatty acid polyglycol ester.
The defoaming agent is polyoxypropylene polyoxyethylene glycerol ether.
The electrostatic protection epoxy self-leveling color sand is matched with an epoxy self-leveling color sand curing agent for use.
The product of the cured electrostatic protection epoxy self-leveling color sand prepared by the experiment has the wear resistance of 12(750 g.500 r)/mg and the surface resistance of 2.1 × 106Ω。
Comparative example 1
A preparation method of acyl chloride conductive graphite micropowder comprises the following steps;
adding 50g of conductive graphite micropowder into 500g of 30% sodium hydroxide solution by mass, uniformly stirring, slowly adding 100g of 15% hydrogen peroxide by mass into a reaction kettle, controlling the addition for 30min, controlling the temperature to be 40 ℃ after the addition, reacting for 45min, cooling to room temperature, standing for 5h, filtering, washing to be neutral, drying, adding 200g of 8% citric acid aqueous solution by mass, uniformly mixing, controlling the temperature to be 40 ℃, reacting for 1h, slowly dropwise adding thionyl chloride, stirring at 50 ℃ for reacting for 4h, filtering the solution to remove the solvent, washing the solid product by using absolute ethyl alcohol, fully drying, and preparing the acyl chloride conductive graphite micropowder.
The preparation method of the amidated conductive graphite additive comprises the following steps of;
adding 50g of acyl chloride conductive graphite micro powder, 2.2g of 2-aminothiophene azole, 2g of sodium hydroxide and 1000g of water into a reaction kettle, stirring for 30 minutes at 60 ℃, washing with deionized water, carrying out suction filtration and dehydration, and drying to obtain the amidation conductive graphite auxiliary agent.
The rest of the process is the same as that of the embodiment 1,
the product of the cured electrostatic protection epoxy self-leveling color sand prepared by the experiment has the wear resistance of 22(750 g.500 r)/mg and the surface resistance of 4.7 × 106Ω。
Comparative example 2
A preparation method of electrostatic protection epoxy self-leveling colored sand mainly adopts the following scheme:
putting 550g of epoxy resin and 50g of talcum powder into a high-speed mixer, stirring at a high speed of 500r/min and a stirring temperature of 40 ℃ for 20min, putting 420g of artificial colored sand into the high-speed mixer, stirring uniformly, and continuing to stir for 15 min; and after the preparation, putting 30g of diluent, 3g of dispersing agent, 4g of defoaming agent, 3g of polybutyl acrylate powder solid flatting agent and 3g of toughening agent polybutadiene rubber into a high-speed mixer, mixing and stirring for 30min, adding 30g of pigment, and uniformly stirring to obtain the electrostatic protection epoxy self-leveling colored sand.
The artificial colored sand is prepared by uniformly mixing 100g of steel slag, 10g of cement, 7g of fly ash, 0.1g of methyl cellulose and 0.7g of latex powder, adding 10g of water, uniformly stirring, maintaining for 5 days, molding and drying.
The epoxy resin is 828 epoxy resin.
The diluent is 1, 4-butanediol diglycidyl ether.
The dispersant is methyl amyl alcohol.
The defoaming agent is polyoxyethylene polyoxypropylene ether.
The electrostatic protection epoxy self-leveling color sand is matched with an epoxy self-leveling color sand curing agent for use.
The product of the cured electrostatic protection epoxy self-leveling color sand prepared by the experiment has the wear resistance of 31(750 g.500 r)/mg and the surface resistance of 6.7 × 1012Ω。
Comparative example 3
A preparation method of acyl chloride conductive graphite micropowder comprises the following steps;
adding 50g of conductive graphite micropowder into 500g of 30% sodium hydroxide solution by mass, uniformly stirring, slowly adding 100g of 15% hydrogen peroxide by mass into a reaction kettle, controlling the addition for 30min, controlling the temperature to be 40 ℃ after the addition, reacting for 45min, cooling to room temperature, standing for 5h, filtering, washing to be neutral, drying, adding 200g of 8% citric acid aqueous solution by mass, uniformly mixing, controlling the temperature to be 40 ℃, reacting for 1h, slowly dropwise adding thionyl chloride, stirring at 50 ℃ for reacting for 4h, filtering the solution to remove the solvent, washing the solid product by using absolute ethyl alcohol, fully drying, and preparing the acyl chloride conductive graphite micropowder.
The preparation method of the amidated conductive graphite additive comprises the following steps of;
adding 50g of acyl chloride conductive graphite micro powder, 0.5g of N, 1-dimethylpyrrolidine-3-amine, 2g of sodium hydroxide and 1000g of water into a reaction kettle, stirring for 30 minutes at 60 ℃, washing with deionized water, performing suction filtration and dehydration, and drying to obtain the amidation conductive graphite auxiliary agent.
The static protection epoxy self-leveling color sand prepared by the experiment is solidifiedThe abrasion resistance of the resulting product was 19(750 g.500 r)/mg, and the surface resistance thereof was 1.8 × 107Ω。
Claims (9)
1. A preparation method of electrostatic protection epoxy self-leveling colored sand mainly adopts the following scheme:
according to the mass parts, 55-68 parts of epoxy resin, 5-10 parts of talcum powder and 0.5-3.1 parts of amidated conductive graphite auxiliary agent are put into a high-speed mixer to be stirred at a high speed, the stirring speed is controlled to be 500 plus materials/min, the stirring temperature is controlled to be 40-60 ℃, 42-57 parts of artificial colored sand is put into the high-speed mixer to be uniformly stirred after being stirred for 20-30min, and the stirring is continued for 15-45 min; after the preparation, 3 to 8 parts of diluent, 0.3 to 0.8 part of dispersant, 0.4 to 0.7 part of defoamer, 0.3 to 0.7 part of polybutyl acrylate powder solid leveling agent and 0.3 to 5 parts of toughening agent polybutadiene rubber are put into a high-speed mixer, mixed and stirred for 30 to 60min, added with 3 to 8 parts of pigment and uniformly stirred to obtain the electrostatic protection epoxy self-leveling colored sand;
and carrying out substitution reaction on the acyl chloride graphene and N, 1-dimethylpyrrolidine-3-amine to prepare the amidated conductive graphite auxiliary agent.
2. The preparation method of the electrostatic protection epoxy self-leveling colored sand as claimed in claim 1, wherein the amidated conductive graphite additive is prepared by the following steps:
adding 50-80 parts by mass of acyl chloride conductive graphite micro powder, 0.5-2 parts by mass of N, 1-dimethylpyrrolidine-3-amine, 2.2-4.8 parts by mass of 2-aminothiophene azole, 2-5 parts by mass of sodium hydroxide and 2000 parts by mass of water into a reaction kettle, stirring for 30-90 minutes at the temperature of 60-70 ℃, washing with deionized water, carrying out suction filtration and dehydration, and drying to obtain the amidated conductive graphite auxiliary agent.
3. The preparation method of the electrostatic protection epoxy self-leveling colored sand according to claim 1, characterized in that the preparation method of the acyl chlorination conductive graphite micro powder is as follows;
adding 50-80 parts by mass of conductive graphite micropowder into 800 parts by mass of 30-40% sodium hydroxide solution, uniformly stirring, slowly adding 150 parts by mass of 15-20% hydrogen peroxide into a reaction kettle, controlling the addition for 30-60min, controlling the temperature to be 40-60 ℃ after the addition, reacting for 45-90min, cooling to room temperature, standing for 5-10h, filtering, washing to be neutral, drying, adding 300 parts by mass of 8-12% citric acid aqueous solution, uniformly mixing, controlling the temperature to be 40-60 ℃ for reacting for 1-5h, slowly dropwise adding thionyl chloride, uniformly stirring at 50-70 ℃ for reacting for 4-10h, filtering the solution to remove the solvent, washing the solid product with absolute ethyl alcohol, and fully drying, and preparing the acyl chloride conductive graphite micro powder.
4. The method for preparing the electrostatic protection epoxy self-leveling colored sand as claimed in claim 1, wherein the artificial colored sand is prepared by uniformly mixing, by mass, 130 parts of steel slag, 10-18 parts of cement, 7-12 parts of fly ash, 0.1-0.5 part of methyl cellulose and 0.7-1.8 part of latex powder, adding 10-20 parts of water, uniformly stirring, curing for 5-10 days, molding, and drying.
5. The method for preparing the electrostatic protection epoxy self-leveling colored sand according to claim 1, wherein the epoxy resin is 828 epoxy resin or 128 epoxy resin.
6. The method of claim 1, wherein the diluent is 1, 4-butanediol diglycidyl ether, polypropylene glycol diglycidyl ether, or 1, 6-hexanediol diglycidyl ether.
7. The method for preparing electrostatic protection epoxy self-leveling colored sand according to claim 1, wherein the dispersant is methyl amyl alcohol or polyacrylamide or fatty acid polyglycol ester.
8. The method for preparing the electrostatic protection epoxy self-leveling colored sand according to claim 1, wherein the defoaming agent is polyoxyethylene polyoxypropylene amine ether or polyoxypropylene glycerol ether or polyoxypropylene polyoxyethylene glycerol ether.
9. The method for preparing the electrostatic protection epoxy self-leveling colored sand according to claim 1, wherein the electrostatic protection epoxy self-leveling colored sand is used in combination with an epoxy self-leveling colored sand curing agent.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03220295A (en) * | 1989-10-06 | 1991-09-27 | Maruwa Bussan Kk | Lubricant for magnetic recording medium and its manufacture |
| CN104387908A (en) * | 2014-07-28 | 2015-03-04 | 常州光辉化工有限公司 | Graphene anti-static floor coating and preparation method thereof |
| CN105400361A (en) * | 2015-11-14 | 2016-03-16 | 合肥标兵凯基新型材料有限公司 | Special graphene oxide modified epoxy resin coating for pop cans |
| CN107221691A (en) * | 2017-05-26 | 2017-09-29 | 厦门大学 | The preparation method of graphene oxide/imidazoles polyphenylene oxide composite anion exchange membrane |
| CN109651927A (en) * | 2018-12-26 | 2019-04-19 | 中国科学院宁波材料技术与工程研究所 | Poly- (thiazolamine)/graphene-epoxy composite coating and preparation method and application |
| CN111334163A (en) * | 2020-03-16 | 2020-06-26 | 上海博歌建材有限公司 | Solvent-free epoxy self-leveling antistatic finish paint and preparation method thereof |
-
2020
- 2020-07-13 CN CN202010671152.XA patent/CN111777913B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03220295A (en) * | 1989-10-06 | 1991-09-27 | Maruwa Bussan Kk | Lubricant for magnetic recording medium and its manufacture |
| CN104387908A (en) * | 2014-07-28 | 2015-03-04 | 常州光辉化工有限公司 | Graphene anti-static floor coating and preparation method thereof |
| CN105400361A (en) * | 2015-11-14 | 2016-03-16 | 合肥标兵凯基新型材料有限公司 | Special graphene oxide modified epoxy resin coating for pop cans |
| CN107221691A (en) * | 2017-05-26 | 2017-09-29 | 厦门大学 | The preparation method of graphene oxide/imidazoles polyphenylene oxide composite anion exchange membrane |
| CN109651927A (en) * | 2018-12-26 | 2019-04-19 | 中国科学院宁波材料技术与工程研究所 | Poly- (thiazolamine)/graphene-epoxy composite coating and preparation method and application |
| CN111334163A (en) * | 2020-03-16 | 2020-06-26 | 上海博歌建材有限公司 | Solvent-free epoxy self-leveling antistatic finish paint and preparation method thereof |
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