CN111253830A - Preparation method of water-based epoxy floor paint - Google Patents
Preparation method of water-based epoxy floor paint Download PDFInfo
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- CN111253830A CN111253830A CN202010048259.9A CN202010048259A CN111253830A CN 111253830 A CN111253830 A CN 111253830A CN 202010048259 A CN202010048259 A CN 202010048259A CN 111253830 A CN111253830 A CN 111253830A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a preparation method of water-based epoxy floor paint, belonging to the technical field of floor paint processing and preparation, and comprising the following steps: s1, preparing a modified inorganic filler; s2, weighing raw materials; s3, preparing a finished product. The invention provides a preparation method of a water-based epoxy floor paint, which is characterized in that a specially-made modified inorganic filler is added in the preparation of the water-based epoxy floor paint, the compatibility of the modified inorganic filler and matrix components is excellent, and the acid-base resistance, oil resistance, water resistance and wear resistance of the finally-prepared water-based epoxy floor paint are effectively improved, so that a paint film can be corroded by an acid-base medium with a certain concentration, the acid-base resistance time is prolonged, the performance stability is good, the defect of over-low hardness of the paint film is overcome, the hardness can reach 4H, and the comprehensive performance is excellent.
Description
Technical Field
The invention belongs to the technical field of floor paint processing and preparation, and particularly relates to a preparation method of a water-based epoxy floor paint.
Background
Epoxy resin floor paint (or epoxy paint) coating is a ground and wall coating mode which rises rapidly along with the progress of industrial technology and the improvement of living standard of people, and the epoxy floor paint becomes one of the strongest development paints in the coating industry at present. The epoxy floor paint is well known for its advantages in many aspects, such as smooth and clean coating surface and matte state of diffuse reflection; the integrity is good, and the gaps are few or complete and seamless, so that dust and bacteria are not easy to accumulate and the cleaning is easy; the surface hardness is high, and the wear resistance and the compressive strength are certain; the color is rich, gorgeous and strong in decoration; the waterproof and permeability-proof performance is good, and the pollution of underground water and soil caused by the polluted substances along with the water permeating into the ground can be avoided; corrosion resistance, can protect the matrix from being corroded by chemicals, and the surface can be kept in a new state. The advantages enable the epoxy floor paint to be widely applied to coating of the ground and the wall of dust-free and corrosion-resistant factory buildings and warehouses in various industries such as food, chemical industry, electronics, electrical appliances, textile, plastic, electroplating, medicine and the like, also to coating of the ground and the wall of large supermarkets, exhibition halls and stadiums, and even to coating of airport runways and parking aprons with epoxy resin. With the continuous expansion of the application range, the hardness, acid and alkali resistance, water resistance and other qualities of the existing water-based epoxy floor paint cannot meet high requirements.
Graphene is a two-dimensional lamellar carbon material, the Young modulus of the hexabasic ring rigid structure can reach 1.0TPa, the breaking strength can reach 310GPa, and the graphene has excellent barrier property because the electron density of the hexabasic aromatic ring in the plane of the graphene is high enough to repel any atom and gas molecule. In view of the excellent performance of the graphene, the graphene is added into the aqueous epoxy resin coating, so that the hardness, impact resistance, chemical corrosion resistance and the like of the aqueous epoxy resin coating can be remarkably improved, particularly the acid resistance of the chemically modified aqueous epoxy resin is improved, and the graphene has extremely important application value. However, the problem of agglomeration cannot be overcome when graphene is applied to epoxy resin in the prior art, and if a graphene component is directly added in the preparation of the aqueous epoxy resin, an obvious interface exists between the graphene and an aqueous epoxy resin matrix component, which means that a plurality of cavities exist in the matrix, so that the improvement effect of the graphene on the aqueous epoxy floor paint is weakened. Although the phenomenon is improved, the stability is poor, namely, the phenomenon of unstable performance is generated in the process of long-time storage or long-time use. For example, application No. CN201810394115.1 discloses an acid-resistant graphene water-based epoxy floor paint and a preparation method thereof. Adding graphene into a water-based epoxy curing agent, and uniformly dispersing the graphene in the water-based epoxy curing agent by using a high-speed dispersion machine; carrying out ultrasonic treatment on the uniformly dispersed graphene waterborne epoxy curing agent in an ultrasonic cleaner with the frequency of 50-100 KHz, and dispersing partially aggregated or overlapped graphene into single-layer graphene in the ultrasonic cleaner; then adding a filler, a dispersing agent, a defoaming agent, a flatting agent and a uniformly dispersed graphene water-based epoxy curing agent into the water-based epoxy resin, and stirring to obtain acid-resistant water-based epoxy floor paint containing graphene; the invention obviously improves the acid resistance of the water-based epoxy resin, so that the water-based epoxy resin can be used in factory workshops, parking lots, offices and other occasions, in particular pharmaceutical factories, chemical plants and the like which have high requirements on the acid resistance of terrace coatings. Although the aqueous epoxy floor paint prepared by the method overcomes the agglomeration phenomenon of graphene, so that a paint film can withstand the corrosion of acid and alkali media with certain concentration, the stability is poor in long-time use due to the fact that the interfacial property between the graphene and the aqueous epoxy floor paint is not considered, and the paint film cannot withstand the corrosion of acid and alkali for a long time.
Disclosure of Invention
The invention aims to provide a preparation method of water-based epoxy floor paint aiming at the existing problems.
The invention is realized by the following technical scheme:
the preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, preparation of modified inorganic filler:
a. placing natural cellulose in a reaction kettle, raising the temperature in the reaction kettle to 120-140 ℃, raising the pressure in the reaction kettle to 2-3 MPa, controlling the relative humidity of air in the reaction kettle to 88-98%, performing high-temperature and high-pressure treatment for 2-3 min, quickly relieving pressure to normal pressure, and taking out the treated natural cellulose for later use;
b. firstly, immersing natural cellulose and graphene powder treated in the operation a into a treatment liquid together according to the weight ratio of 80-90: 1, keeping the temperature in the treatment liquid at 80-90 ℃, stirring for 30-40 min, performing suction filtration, then putting a solid mixture obtained by suction filtration into a cryogenic crusher, performing crushing treatment in a liquid nitrogen environment, and taking out a mixed powder A for later use after the crushing treatment is performed for 5-7 min;
c. placing the mixed powder A obtained in the operation B on a GJ-1.5 type high-frequency high-voltage high-power electron accelerator for electron beam irradiation treatment, and taking out the mixed powder B for later use after the irradiation treatment is carried out for 10-12 min;
d. adding the mixed powder B obtained in the operation c and deionized water into a flask according to the weight-volume ratio of 0.1g: 90-100 mL, performing ultrasonic dispersion treatment for 50-60 min, heating to 60-70 ℃, then diluting epoxy resin with absolute ethyl alcohol, adding the diluted epoxy resin into the flask through a constant-pressure dropping funnel, performing heat preservation and stirring treatment for 2-3 h, stopping heating, performing suction filtration, washing with butyl acetate for 3-5 times, and performing vacuum drying to obtain a modified inorganic filler for later use;
s2, weighing the following raw materials:
weighing 70-80 parts of epoxy resin by weight, 6-8 parts of modified inorganic filler obtained in the step S1, 1-3 parts of paraffin, 2-3 parts of calcium stearate, 0.4-0.5 part of dibutyltin dilaurate, 0.45-0.49 part of diisodecyl phthalate, 0.08-0.09 part of polydimethylsiloxane, 0.06-0.08 part of polyoxyethylene fatty alcohol ether, 1-3 parts of glycerol, 0.24-0.32 part of phenyl salicylate, 0.05-0.07 part of p-hydroxybenzene sulfonic acid and 40-50 parts of deionized water for later use;
s3, preparation of a finished product:
a. putting the epoxy resin weighed in the S2, the modified inorganic filler obtained in the step S1, paraffin, calcium stearate and deionized water into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 600-900 rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 300-500 rpm for 1-2 hours.
Further, in operation a of step S1, the natural fiber is any one of ramie, flax, hemp, jute, sisal, and abaca.
Further, in the step S1, the treating solution in the operation b includes the following components in percentage by weight: 4-5% of liquid ammonia, 5-6% of titanate coupling agent, 0.6-0.8% of propylene glycol, 1-3% of sodium dodecyl benzene sulfonate and the balance of deionized water.
Further, the rotation speed of the pulverizer in the pulverizing treatment in the operation b of the step S1 is 500 to 800rpm, and the temperature in the pulverizer is controlled to-15 to-7 ℃.
Further, the irradiation dose in the electron beam irradiation treatment in operation c of step S1 is 3.9 to 4.7 kGy.
Further, the frequency of the ultrasonic wave during the ultrasonic dispersion in operation d of step S1 is 20-40 kHz.
The invention comprehensively considers the service performance of the prior water-based epoxy floor paint and the problems of the prior art, develops and researches a preparation method of the water-based epoxy floor paint, adds a specially-made modified inorganic filler in the preparation of the water-based epoxy floor paint, and the modified inorganic filler has excellent compatibility with the matrix component, so that the acid and alkali resistance, oil resistance, water resistance and wear resistance of the finally prepared water-based epoxy floor paint are effectively improved, a paint film can be corroded by acid and alkali mediums with certain concentration, the acid and alkali resistance time is prolonged, the performance stability is good, the defect of over-low hardness of the paint film is overcome, the hardness can reach 4H, and the comprehensive performance is excellent. Specifically, in the preparation of the modified inorganic filler, natural cellulose is firstly placed under the conditions of high temperature and high pressure, high-temperature water vapor permeates into micro fiber bundles, the water vapor rapidly expands in the permeation process and is then violently discharged into the atmosphere, so that the supermolecular structure of the cellulose is damaged, the activity is enhanced, partial hydrogen bonds are exposed, the natural cellulose and graphene are uniformly mixed and then are immersed into a treatment solution, under the action of effective components in the treatment solution, the graphene is attached to the fracture part of the natural cellulose molecules, the agglomeration phenomenon of the graphene can be effectively prevented, a certain weakening effect on the interfacial effect is achieved, then the inorganic filler powder is crushed in a liquid nitrogen environment, the inorganic filler powder is refined, the surface activity of the inorganic filler is reduced, the agglomeration phenomenon is further prevented, in order to further improve the performance of the inorganic filler, the obtained mixed powder is subjected to electron beam irradiation treatment with a specific dose, under the action of electron beams, excited atoms form a certain amount of active free radicals on a molecular chain framework, molecular chains of a crystalline region and an amorphous region of cellulose are uniformly degraded, so that the dispersity of the inorganic modified filler is improved, the durability, the light resistance and the chemical stability of the inorganic modified filler are improved, and finally the epoxy resin is used for forming the coated inorganic filler, so that the agglomeration phenomenon of the inorganic filler is further prevented, the stability of the inorganic modified filler in the water-based epoxy floor paint is enhanced, and the stability of the performance in the using process can be ensured while the performance of the water-based epoxy floor paint is improved.
Compared with the prior art, the invention has the following advantages:
the invention provides a preparation method of a water-based epoxy floor paint, which is characterized in that a specially-made modified inorganic filler is added in the preparation of the water-based epoxy floor paint, the compatibility of the modified inorganic filler and matrix components is excellent, and the acid-base resistance, oil resistance, water resistance and wear resistance of the finally-prepared water-based epoxy floor paint are effectively improved, so that a paint film can be corroded by an acid-base medium with a certain concentration, the acid-base resistance time is prolonged, the performance stability is good, the defect of over-low hardness of the paint film is overcome, the hardness can reach 4H, and the comprehensive performance is excellent.
Drawings
FIG. 1 is a graph of comparative data for tests of acid and alkali resistance according to the present invention.
Detailed Description
The preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, preparation of modified inorganic filler:
a. placing natural cellulose in a reaction kettle, raising the temperature in the reaction kettle to 120-140 ℃, raising the pressure in the reaction kettle to 2-3 MPa, controlling the relative humidity of air in the reaction kettle to 88-98%, performing high-temperature and high-pressure treatment for 2-3 min, quickly relieving pressure to normal pressure, and taking out the treated natural cellulose for later use;
b. firstly, immersing natural cellulose and graphene powder treated in the operation a into a treatment liquid together according to the weight ratio of 80-90: 1, keeping the temperature in the treatment liquid at 80-90 ℃, stirring for 30-40 min, performing suction filtration, then putting a solid mixture obtained by suction filtration into a cryogenic crusher, performing crushing treatment in a liquid nitrogen environment, and taking out a mixed powder A for later use after the crushing treatment is performed for 5-7 min;
c. placing the mixed powder A obtained in the operation B on a GJ-1.5 type high-frequency high-voltage high-power electron accelerator for electron beam irradiation treatment, and taking out the mixed powder B for later use after the irradiation treatment is carried out for 10-12 min;
d. adding the mixed powder B obtained in the operation c and deionized water into a flask according to the weight-volume ratio of 0.1g: 90-100 mL, performing ultrasonic dispersion treatment for 50-60 min, heating to 60-70 ℃, then diluting epoxy resin with absolute ethyl alcohol, adding the diluted epoxy resin into the flask through a constant-pressure dropping funnel, performing heat preservation and stirring treatment for 2-3 h, stopping heating, performing suction filtration, washing with butyl acetate for 3-5 times, and performing vacuum drying to obtain a modified inorganic filler for later use;
s2, weighing the following raw materials:
weighing 70-80 parts of epoxy resin by weight, 6-8 parts of modified inorganic filler obtained in the step S1, 1-3 parts of paraffin, 2-3 parts of calcium stearate, 0.4-0.5 part of dibutyltin dilaurate, 0.45-0.49 part of diisodecyl phthalate, 0.08-0.09 part of polydimethylsiloxane, 0.06-0.08 part of polyoxyethylene fatty alcohol ether, 1-3 parts of glycerol, 0.24-0.32 part of phenyl salicylate, 0.05-0.07 part of p-hydroxybenzene sulfonic acid and 40-50 parts of deionized water for later use;
s3, preparation of a finished product:
a. putting the epoxy resin weighed in the S2, the modified inorganic filler obtained in the step S1, paraffin, calcium stearate and deionized water into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 600-900 rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 300-500 rpm for 1-2 hours.
Further, in operation a of step S1, the natural fiber is any one of ramie, flax, hemp, jute, sisal, and abaca.
Further, in the step S1, the treating solution in the operation b includes the following components in percentage by weight: 4-5% of liquid ammonia, 5-6% of titanate coupling agent, 0.6-0.8% of propylene glycol, 1-3% of sodium dodecyl benzene sulfonate and the balance of deionized water.
Further, the rotation speed of the pulverizer in the pulverizing treatment in the operation b of the step S1 is 500 to 800rpm, and the temperature in the pulverizer is controlled to-15 to-7 ℃.
Further, the irradiation dose in the electron beam irradiation treatment in operation c of step S1 is 3.9 to 4.7 kGy.
Further, the frequency of the ultrasonic wave during the ultrasonic dispersion in operation d of step S1 is 20-40 kHz.
For further explanation of the present invention, reference will now be made to the following specific examples.
Example 1
The preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, preparation of modified inorganic filler:
a. placing natural cellulose in a reaction kettle, then raising the temperature in the reaction kettle to 120 ℃, raising the pressure in the reaction kettle to 2MPa, controlling the relative humidity of air in the reaction kettle to be 88-98%, carrying out high-temperature high-pressure treatment for 2min, then rapidly releasing pressure to normal pressure, and taking out the treated natural cellulose for later use;
b. firstly, immersing natural cellulose and graphene powder treated in the operation a into a treatment fluid together according to the weight ratio of 80:1, keeping the temperature in the treatment fluid at 80 ℃, stirring for 30min, performing suction filtration, then putting a solid mixture obtained by suction filtration into a cryogenic pulverizer, performing pulverization treatment in a liquid nitrogen environment, controlling the rotation speed of the pulverizer at 500rpm, controlling the temperature in the pulverizer at-15 ℃, and taking out mixed powder A for later use after 5min of pulverization treatment;
c. placing the mixed powder A obtained in the operation B on a GJ-1.5 type high-frequency high-voltage high-power electron accelerator for electron beam irradiation treatment, wherein the irradiation dose in the electron beam irradiation treatment is 3.9kGy, and taking out the mixed powder B for later use after the irradiation treatment is carried out for 10 min;
d. adding the mixed powder B obtained in the operation c and deionized water into a flask according to the weight-volume ratio of 0.1g:90mL, performing ultrasonic dispersion treatment at 20kHz for 50min, heating to 60 ℃, then diluting epoxy resin with absolute ethyl alcohol, adding the diluted epoxy resin into the flask through a constant-pressure dropping funnel, performing heat preservation and stirring treatment for 2h, stopping heating, performing suction filtration, washing butyl acetate for 3 times, and performing vacuum drying to obtain a modified inorganic filler for later use;
s2, weighing the following raw materials:
weighing 70 parts of epoxy resin, 6 parts of the modified inorganic filler obtained in the step S1, 1 part of paraffin, 2 parts of calcium stearate, 0.4 part of dibutyltin dilaurate, 0.45 part of diisodecyl phthalate, 0.08 part of polydimethylsiloxane, 0.06 part of polyoxyethylene fatty alcohol ether, 1 part of glycerol, 0.24 part of phenyl salicylate, 0.05 part of p-hydroxybenzene sulfonic acid and 40 parts of deionized water in corresponding parts by weight for later use;
s3, preparation of a finished product:
a. putting the epoxy resin weighed in the S2, the modified inorganic filler obtained in the step S1, paraffin, calcium stearate and deionized water into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 600rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 300rpm for 1 h.
In operation a of step S1, the natural fiber is any one of ramie, flax, hemp, jute, sisal, and abaca.
The treating fluid in the operation b of the step S1 comprises the following components in percentage by weight: 4% of liquid ammonia, 5% of titanate coupling agent, 0.6% of propylene glycol, 1% of sodium dodecyl benzene sulfonate and the balance of deionized water.
Example 2
The preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, preparation of modified inorganic filler:
a. placing natural cellulose in a reaction kettle, then raising the temperature in the reaction kettle to 130 ℃, raising the pressure in the reaction kettle to 2.5MPa, controlling the relative humidity of air in the reaction kettle to 93%, performing high-temperature high-pressure treatment for 2.5min, then quickly releasing pressure to normal pressure, and taking out the treated natural cellulose for later use;
b. firstly, immersing natural cellulose and graphene powder treated in the operation a into a treatment fluid together according to the weight ratio of 85:1, keeping the temperature in the treatment fluid at 85 ℃, stirring for 35min, performing suction filtration, then putting a solid mixture obtained by suction filtration into a cryogenic pulverizer, performing pulverization treatment in a liquid nitrogen environment, controlling the rotation speed of the pulverizer at 650rpm, controlling the temperature in the pulverizer at-11 ℃, and taking out mixed powder A for later use after 6min of pulverization treatment;
c. placing the mixed powder A obtained in the operation B on a GJ-1.5 type high-frequency high-voltage high-power electron accelerator for electron beam irradiation treatment, wherein the irradiation dose in the electron beam irradiation treatment is 4.3kGy, and taking out the mixed powder B for later use after the irradiation treatment is carried out for 11 min;
d. adding the mixed powder B obtained in the operation c and deionized water into a flask according to the weight-volume ratio of 0.1g:95mL, performing ultrasonic dispersion treatment at 30kHz for 55min, heating to 65 ℃, then diluting epoxy resin with absolute ethyl alcohol, adding the diluted epoxy resin into the flask through a constant-pressure dropping funnel, performing heat preservation and stirring treatment for 2.5h, stopping heating, performing suction filtration, washing with butyl acetate for 4 times, and performing vacuum drying to obtain a modified inorganic filler for later use;
s2, weighing the following raw materials:
weighing 75 parts of epoxy resin, 7 parts of the modified inorganic filler obtained in the step S1, 2 parts of paraffin, 2.5 parts of calcium stearate, 0.45 part of dibutyltin dilaurate, 0.47 part of diisodecyl phthalate, 0.085 part of polydimethylsiloxane, 0.07 part of polyoxyethylene fatty alcohol ether, 2 parts of glycerol, 0.28 part of phenyl salicylate, 0.06 part of p-hydroxybenzene sulfonic acid and 45 parts of deionized water in corresponding parts by weight for later use;
s3, preparation of a finished product:
a. putting the epoxy resin weighed in the S2, the modified inorganic filler obtained in the step S1, paraffin, calcium stearate and deionized water into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 750rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 400rpm for 1.5 hours.
In operation a of step S1, the natural fiber is any one of ramie, flax, hemp, jute, sisal, and abaca.
The treating fluid in the operation b of the step S1 comprises the following components in percentage by weight: 4.5% of liquid ammonia, 5.5% of titanate coupling agent, 0.7% of propylene glycol, 2% of sodium dodecyl benzene sulfonate and the balance of deionized water.
Example 3
The preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, preparation of modified inorganic filler:
a. placing natural cellulose in a reaction kettle, then raising the temperature in the reaction kettle to 140 ℃, raising the pressure in the reaction kettle to 3MPa, controlling the relative humidity of air in the reaction kettle to be 98%, carrying out high-temperature high-pressure treatment for 3min, then rapidly releasing pressure to normal pressure, and taking out the treated natural cellulose for later use;
b. firstly, immersing natural cellulose and graphene powder treated in the operation a into a treatment fluid together according to the weight ratio of 90:1, keeping the temperature in the treatment fluid at 90 ℃, stirring for 40min, performing suction filtration, then putting a solid mixture obtained by suction filtration into a cryogenic pulverizer, performing pulverization treatment in a liquid nitrogen environment, controlling the rotation speed of the pulverizer at 800rpm, controlling the temperature in the pulverizer at-7 ℃, and taking out mixed powder A for later use after 7min of pulverization treatment;
c. placing the mixed powder A obtained in the operation B on a GJ-1.5 type high-frequency high-voltage high-power electron accelerator for electron beam irradiation treatment, wherein the irradiation dose in the electron beam irradiation treatment is 4.7kGy, and taking out the mixed powder B for later use after 12min of irradiation treatment;
d. adding the mixed powder B obtained in the operation c and deionized water into a flask according to the weight-volume ratio of 0.1g:100mL, carrying out ultrasonic dispersion treatment at 40kHz for 60min, heating to 70 ℃, diluting epoxy resin with absolute ethyl alcohol, adding the diluted epoxy resin into the flask through a constant-pressure dropping funnel, carrying out heat preservation and stirring treatment for 3h, stopping heating, carrying out suction filtration, washing butyl acetate for 5 times, and carrying out vacuum drying to obtain a modified inorganic filler for later use;
s2, weighing the following raw materials:
weighing 80 parts of epoxy resin, 8 parts of the modified inorganic filler obtained in the step S1, 3 parts of paraffin, 3 parts of calcium stearate, 0.5 part of dibutyltin dilaurate, 0.49 part of diisodecyl phthalate, 0.09 part of polydimethylsiloxane, 0.08 part of polyoxyethylene fatty alcohol ether, 3 parts of glycerol, 0.32 part of phenyl salicylate, 0.07 part of p-hydroxybenzene sulfonic acid and 50 parts of deionized water in corresponding parts by weight for later use;
s3, preparation of a finished product:
a. putting the epoxy resin weighed in the S2, the modified inorganic filler obtained in the step S1, paraffin, calcium stearate and deionized water into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 900rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 500rpm for 1-2 hours.
In operation a of step S1, the natural fiber is any one of ramie, flax, hemp, jute, sisal, and abaca.
The treating fluid in the operation b of the step S1 comprises the following components in percentage by weight: 5% of liquid ammonia, 6% of titanate coupling agent, 0.8% of propylene glycol, 3% of sodium dodecyl benzene sulfonate and the balance of deionized water.
Example 4
The preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, weighing the following raw materials:
weighing 75 parts of epoxy resin, 2 parts of paraffin, 2.5 parts of calcium stearate, 0.45 part of dibutyltin dilaurate, 0.47 part of diisodecyl phthalate, 0.085 part of polydimethylsiloxane, 0.07 part of polyoxyethylene fatty alcohol ether, 2 parts of glycerol, 0.28 part of phenyl salicylate, 0.06 part of p-hydroxybenzene sulfonic acid and 45 parts of deionized water in corresponding parts by weight for later use;
s2, preparation of a finished product:
a. putting the epoxy resin, the paraffin, the calcium stearate and the deionized water weighed in the S2 into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 750rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 400rpm for 1.5 hours.
Example 5
The application numbers are: CN201810394115.1 discloses an acid-resistant graphene water-based epoxy floor paint and a preparation method thereof.
In order to compare the effects of the invention, the preparation methods corresponding to the embodiments 1-5 are respectively used for preparing the water-based epoxy floor paint, then the performances of the water-based floor paints of each group are respectively measured, and the hardness is measured according to GB/T6739-1996; abrasion resistance is measured according to GB/T1768-1979 (1989); the water resistance is tested according to a method for testing the chemical reagent resistance of a paint film (soaking method) of GB/T9274-1988; the acid and alkali resistance and lubricating oil performance were tested according to GB/T9274-1988 paint film resistance to chemical reagents (drop method), wherein the resistance to acid was determined as 10% HCl at 25 ℃ and the resistance to alkali was determined as 10% NaOH solution at 25 ℃. Each group of indexes is subjected to 5 parallel tests at any time during measurement, and the average value is taken as a final test result. The test comparison data of hardness, wear resistance, water resistance and wear resistance are shown in the following table 1, and the test comparison data of acid and alkali resistance are shown in fig. 1.
TABLE 1
As can be seen from table 1 above, by adding a specially-made modified inorganic filler in the preparation of the water-based epoxy floor paint, the oil resistance, water resistance and wear resistance of the finally-prepared water-based epoxy floor paint are effectively improved compared with those of a control group, the defect of too low hardness of the paint film is overcome, the hardness can reach 4H, and the comprehensive performance is excellent.
As can be seen from figure 1, the modified inorganic filler can be uniformly dispersed in the matrix component of the waterborne epoxy floor paint, so that the phenomena of agglomeration and difficult compatibility of the inorganic filler are effectively solved, the acid and alkali resistance of the waterborne epoxy floor paint is improved, a paint film can be corroded by an acid and alkali medium with a certain concentration, the acid and alkali resistance time is prolonged, and the performance stability is good.
Claims (6)
1. The preparation method of the water-based epoxy floor paint is characterized by comprising the following steps:
s1, preparation of modified inorganic filler:
a. placing natural cellulose in a reaction kettle, raising the temperature in the reaction kettle to 120-140 ℃, raising the pressure in the reaction kettle to 2-3 MPa, controlling the relative humidity of air in the reaction kettle to 88-98%, performing high-temperature and high-pressure treatment for 2-3 min, quickly relieving pressure to normal pressure, and taking out the treated natural cellulose for later use;
b. firstly, immersing natural cellulose and graphene powder treated in the operation a into a treatment liquid together according to the weight ratio of 80-90: 1, keeping the temperature in the treatment liquid at 80-90 ℃, stirring for 30-40 min, performing suction filtration, then putting a solid mixture obtained by suction filtration into a cryogenic crusher, performing crushing treatment in a liquid nitrogen environment, and taking out a mixed powder A for later use after the crushing treatment is performed for 5-7 min;
c. placing the mixed powder A obtained in the operation B on a GJ-1.5 type high-frequency high-voltage high-power electron accelerator for electron beam irradiation treatment, and taking out the mixed powder B for later use after the irradiation treatment is carried out for 10-12 min;
d. adding the mixed powder B obtained in the operation c and deionized water into a flask according to the weight-volume ratio of 0.1g: 90-100 mL, performing ultrasonic dispersion treatment for 50-60 min, heating to 60-70 ℃, then diluting epoxy resin with absolute ethyl alcohol, adding the diluted epoxy resin into the flask through a constant-pressure dropping funnel, performing heat preservation and stirring treatment for 2-3 h, stopping heating, performing suction filtration, washing with butyl acetate for 3-5 times, and performing vacuum drying to obtain a modified inorganic filler for later use;
s2, weighing the following raw materials:
weighing 70-80 parts of epoxy resin by weight, 6-8 parts of the modified inorganic filler obtained in the step S1, 1-3 parts of paraffin, 2-3 parts of calcium stearate, 0.4-0.5 part of dibutyltin dilaurate, 0.45-0.49 part of diisodecyl phthalate, 0.08-0.09 part of polydimethylsiloxane, 0.06-0.08 part of polyoxyethylene fatty alcohol ether, 1-3 parts of glycerol, 0.24-0.32 part of phenyl salicylate, 0.05-0.07 part of p-hydroxyphenylsulfonic acid and 40-50 parts of deionized water for later use;
s3, preparation of a finished product:
a. putting the epoxy resin weighed in the S2, the modified inorganic filler obtained in the step S1, paraffin, calcium stearate and deionized water into a dispersion cylinder together, and stirring and uniformly mixing at the rotating speed of 600-900 rpm to obtain a dispersion A;
b. and (4) uniformly mixing dibutyltin dilaurate, diisodecyl phthalate, polydimethylsiloxane, polyoxyethylene fatty alcohol ether, glycerol, phenyl salicylate and p-hydroxyphenylsulfonic acid weighed in the step (S2), putting into the dispersion A in the operation (a), and stirring at the rotating speed of 300-500 rpm for 1-2 hours.
2. The method for preparing an aqueous epoxy floor paint according to claim 1, wherein the natural fiber in operation a of step S1 is any one of ramie, flax, hemp, jute, sisal and abaca.
3. The preparation method of the water-based epoxy floor paint as claimed in claim 1, wherein the treating liquid in the step S1, operation b, comprises the following components in percentage by weight: 4-5% of liquid ammonia, 5-6% of titanate coupling agent, 0.6-0.8% of propylene glycol, 1-3% of sodium dodecyl benzene sulfonate and the balance of deionized water.
4. The method for preparing a water-based epoxy floor paint as claimed in claim 1, wherein the rotation speed of the pulverizer in the pulverizing process in operation b of step S1 is 500-800 rpm, and the temperature in the pulverizer is controlled to-15-7 ℃.
5. The method for preparing the water-based epoxy floor paint according to the claim 1, wherein the irradiation dose during the electron beam irradiation treatment in the operation c of the step S1 is 3.9-4.7 kGy.
6. The preparation method of the water-based epoxy floor paint as claimed in claim 1, wherein the ultrasonic frequency during the ultrasonic dispersion in the operation d of step S1 is 20-40 kHz.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111635648A (en) * | 2020-06-10 | 2020-09-08 | 广东省生物工程研究所（广州甘蔗糖业研究所） | Degradation promoter prepared by layer-by-layer coating method and preparation and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554696A (en) * | 2015-09-25 | 2017-04-05 | 青岛瑞利特新材料科技有限公司 | A kind of Graphene antistatic aqueous epoxy floor paint |
| CN110183757A (en) * | 2019-05-23 | 2019-08-30 | 肥西县创玺建材科技有限公司 | A method of sewage pipe plastic is prepared based on biomass fiber |
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2020
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554696A (en) * | 2015-09-25 | 2017-04-05 | 青岛瑞利特新材料科技有限公司 | A kind of Graphene antistatic aqueous epoxy floor paint |
| CN110183757A (en) * | 2019-05-23 | 2019-08-30 | 肥西县创玺建材科技有限公司 | A method of sewage pipe plastic is prepared based on biomass fiber |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111635648A (en) * | 2020-06-10 | 2020-09-08 | 广东省生物工程研究所（广州甘蔗糖业研究所） | Degradation promoter prepared by layer-by-layer coating method and preparation and application thereof |
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