CN107434943B - A kind of preparation method of fire resistant coating - Google Patents
A kind of preparation method of fire resistant coating Download PDFInfo
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- CN107434943B CN107434943B CN201710801988.5A CN201710801988A CN107434943B CN 107434943 B CN107434943 B CN 107434943B CN 201710801988 A CN201710801988 A CN 201710801988A CN 107434943 B CN107434943 B CN 107434943B
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- C—CHEMISTRY; METALLURGY
- 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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C09D161/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C09D161/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C—CHEMISTRY; METALLURGY
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of preparation methods of fire resistant coating, melamine resin, epoxy novolac acrylic resin, acrylyl oxy-ethyl-trimethyl salmiac, pentaerythrite, antimony trichloride, talcum powder, TS-1/ kaolinite nano powder, ammonium polyphosphate is raw material, by ammonium polyphosphate to epoxy novolac acrylic resin modification, it reuses auxiliary agent doping TS-1/ kaolinite nano powder and prepares fireproof coating resistant to high temperature, the present invention is by ammonium polyphosphate to epoxy novolac acrylic resin modification, it reuses auxiliary agent doping TS-1/ kaolinite nano powder and prepares fireproof coating resistant to high temperature, material is prepared to be easy to get, cost reduces, high temperature resistant, good flame resistance, long service life.
Description
Technical field
Invention is related to a kind of preparation method of fire resistant coating, belongs to concrete manufacturing field.
Background technique
High-temperature resistant coating is also known as heat-resisting paint, generally refers at 200 DEG C or more, and paint film is non-discolouring, does not fall off, and is still able to maintain
The coating of physical mechanical property appropriate can make protected object that can normally play a role in the high temperature environment special functional
Coating.Therefore, high-temperature resistant coating is widely used in steel chimney, high-temperature pipe, high temperature stove outer covering, petroleum cracking device and smooth
Gram, the high-temperature fields institute such as cannon, delay the heat hydrogenation corrosion of the metal equipments such as steel at high temperature, it is ensured that equipment can be used for a long time.
It is many to the report of heat-resisting paint at present, and the heat resistance of existing high-temperature resistant coating is substantially attained by use and wants
It asks, but all there are some disadvantages.If paint film surface drying time is long, cause in use because the reasons such as dust influence outside paint film
It sees, the common high-temperature resistant coating in market can cause very big harm, corrosion resistance under high temperature mostly using Cr VI as corrosion inhibiter to environment
The disadvantages of poor.
Summary of the invention
The purpose of the present invention is to provide a kind of fire resistant coating preparation method, the coating prepared by this method
With excellent heat resistance and flame retardant property.
A kind of preparation method of fire resistant coating, method includes the following steps:
Step 1, under conditions of 60 DEG C, by 70 parts of melamine resins, 30 modified phenolic epoxy acrylic resins,
20 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.
Wherein, heat stabilizer is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polyoxypropylene glyceryl
Ether.
The melamine resin the preparation method is as follows:
10 parts of melamines, 40 parts of formaldehyde and 15 parts of water are added in beakers and stir by step 1, and with mass concentration 5%
Sodium carbonate liquor adjusts PH=8, pours into reaction vessel and stirs, and is warming up to 70 ~ 80 DEG C, stirring rate 3500r/min, reaction
Pre-polymerization liquid is obtained after 30min；
20 parts of ammonium polyphosphates are added in beaker by step 2, and 15 parts of ethyl alcohol are added, and are dispersed with stirring uniformly, are obtained poly phosphorus
Then pre-polymerization liquid is added in ammonium polyphosphate suspension by sour ammonium suspension, adjust PH=5 with dilute hydrochloric acid, then heat to 80
DEG C, 2h is stirred to react with the rate of 550r/min, is filtered, washed, dried, that is, obtain melamine resin；
The epoxy novolac acrylic resin the preparation method is as follows:
100 parts of novolac epoxy resins are added in four-hole boiling flask, while 20 parts of modifying agent isophorones two are added for step 1
Amine, 5 parts of p methoxy phenols and 5 parts of catalyst triethanolamines, stirring evenly dissolves resin all；
Step 2 is warming up to 80 DEG C, 55 parts of acrylic acid is slowly added dropwise with separatory funnel, heating is added dropwise in control in 3h
It to 90 DEG C and keeps the temperature, strict control reaction temperature maintains reaction, until reaction acid value is less than 15mgKOH/g, stops reaction；
Appropriate 90 DEG C of hot water is added in step 3, stirs 20min, upper solution is gone in stratification hypsokinesis, to remove unreacted
Acrylic acid, modifying agent, p methoxy phenol and catalyst, in triplicate, finally the moisture in removing system i.e. be modified
Epoxy novolac acrylic resin；
The TS-1/ kaolinite process for preparing nm powder is as follows:
20 parts of kaolinites are crushed to 100 mesh, then by smashed kaolinite mountain flour be placed in electric furnace heating device with 10 DEG C/
After the heating rate of min is heated to 1000 DEG C of heat preservation 3h, kaolinite stone powder is made, by 50 parts of TS-1 zeolite molecular sieve powder and obtains
Then the kaolinite stone powder mixing arrived is added 45 parts of glycerine fusion agents and stirs evenly, the oil bath 2h at 300 DEG C, and every therebetween
It is stirred evenly once every 0.5, stands 1h or more at room temperature, discard supernatant, lower layer's substance is cleaned with ultrapure water, then at 110 DEG C
Drying sieves with 100 mesh sieve after grinding to constant weight, obtains TS-1/ kaolinite nano powder.
The utility model has the advantages that fire resistant coating prepared by the present invention, by melamine-formaldehyde resin and modified phenolic epoxy third
Olefin(e) acid resin combines part instead of traditional P-C-N expansible fireproof system with acrylic acid and nanocomposite reaction, overcomes
Fire-proof packing water suction migration and the problem incompatible with film forming matter use modified phenolic epoxy acrylic resin lotion as forming a film
Object improves its adhesive force with steel, while enhancing its anti-corrosion capability and waterproof ability, using TS-1/ kaolinite nano powder
As filler, it is improved fireproof coating by the carbonaceous froth bed intensity of thermosetting, greatly extends fire prevention
The fire endurance time of coating improves the construction of fireproof coating on the other hand but also the adhesion strength of material increases
Performance improves the fire protecting performance of material indirectly, the nano combined fire resistant coating tool of the modified resin being prepared
Have the advantages that lightweight water-tolerant, high temperature resistant, pollution-free, at low cost, the fire endurance time is long, the service life is long, can be used in steel knot
Structure, concrete, functional plastics, wood materials etc. need to do the material surface of fire prevention measure.
Specific embodiment
Embodiment 1
The preparation method of kind fire resistant coating, method includes the following steps:
Step 1, under conditions of 60 DEG C, by 70 parts of melamine resins, 30 modified phenolic epoxy acrylic resins,
20 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.
Wherein, heat stabilizer is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polyoxypropylene glyceryl
Ether.
The melamine resin the preparation method is as follows:
10 parts of melamines, 40 parts of formaldehyde and 15 parts of water are added in beakers and stir by step 1, and with mass concentration 5%
Sodium carbonate liquor adjusts PH=8, pours into reaction vessel and stirs, and is warming up to 70 ~ 80 DEG C, stirring rate 3500r/min, reaction
Pre-polymerization liquid is obtained after 30min；
20 parts of ammonium polyphosphates are added in beaker by step 2, and 15 parts of ethyl alcohol are added, and are dispersed with stirring uniformly, are obtained poly phosphorus
Then pre-polymerization liquid is added in ammonium polyphosphate suspension by sour ammonium suspension, adjust PH=5 with dilute hydrochloric acid, then heat to 80
DEG C, 2h is stirred to react with the rate of 550r/min, is filtered, washed, dried, that is, obtain melamine resin；
The epoxy novolac acrylic resin the preparation method is as follows:
100 parts of novolac epoxy resins are added in four-hole boiling flask, while 20 parts of modifying agent isophorones two are added for step 1
Amine, 5 parts of p methoxy phenols and 5 parts of catalyst triethanolamines, stirring evenly dissolves resin all；
Step 2 is warming up to 80 DEG C, 55 parts of acrylic acid is slowly added dropwise with separatory funnel, heating is added dropwise in control in 3h
It to 90 DEG C and keeps the temperature, strict control reaction temperature maintains reaction, until reaction acid value is less than 15mgKOH/g, stops reaction；
Appropriate 90 DEG C of hot water is added in step 3, stirs 20min, upper solution is gone in stratification hypsokinesis, to remove unreacted
Acrylic acid, modifying agent, p methoxy phenol and catalyst, in triplicate, finally the moisture in removing system i.e. be modified
Epoxy novolac acrylic resin；
The TS-1/ kaolinite process for preparing nm powder is as follows:
20 parts of kaolinites are crushed to 100 mesh, then by smashed kaolinite mountain flour be placed in electric furnace heating device with 10 DEG C/
After the heating rate of min is heated to 1000 DEG C of heat preservation 3h, kaolinite stone powder is made, by 50 parts of TS-1 zeolite molecular sieve powder and obtains
Then the kaolinite stone powder mixing arrived is added 45 parts of glycerine fusion agents and stirs evenly, the oil bath 2h at 300 DEG C, and every therebetween
It is stirred evenly once every 0.5, stands 1h or more at room temperature, discard supernatant, lower layer's substance is cleaned with ultrapure water, then at 110 DEG C
Drying sieves with 100 mesh sieve after grinding to constant weight, obtains TS-1/ kaolinite nano powder.
Embodiment 2
Step 1, under conditions of 60 DEG C, by 40 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 3
Step 1, under conditions of 60 DEG C, by 70 parts of melamine resins, 50 modified phenolic epoxy acrylic resins,
30 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 4
Step 1, under conditions of 60 DEG C, by 80 parts of melamine resins, 10 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 5
Step 1, under conditions of 60 DEG C, by 20 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
5 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 6
Step 1, under conditions of 60 DEG C, by 40 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
10 parts of antimony trichlorides, 30 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 7
Step 1, under conditions of 60 DEG C, by 40 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 30 parts of talcum powder and 20 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 8
Step 1, under conditions of 60 DEG C, by 40 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
5 parts of antimony trichlorides, 10 parts of talcum powder and 20 parts of TS-1/ kaolinite nano powders are added to described first and mix by step 2
It closes in solution, and ultrasonic disperse 30 minutes, obtains the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added to second mixed solution by step 3
In, and stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, thermostabilization
Agent is dibasic lead stearate, and levelling agent is dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 9
Step 1, under conditions of 60 DEG C, by 40 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
1.4 parts of heat stabilizers, 1 part of levelling agent, 0.5 part of defoaming agent are added in second mixed solution by step 3,
And stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, heat stabilizer is
Dibasic lead stearate, levelling agent are dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Embodiment 10
Step 1, under conditions of 60 DEG C, by 40 parts of melamine resins, 20 modified phenolic epoxy acrylic resins,
10 parts of pentaerythrites and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to described first by step 2
In mixed solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
2 parts of heat stabilizers, 0.1 part of levelling agent, 0.6 part of defoaming agent are added in second mixed solution by step 3,
And stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made.Wherein, heat stabilizer is
Dibasic lead stearate, levelling agent are dimethicone, and defoaming agent is polypropylene glycerol aether.
Remaining preparation and embodiment 1 are identical.
Reference examples 1
It is with 1 difference of embodiment: in the step 1 of melamine resin preparation, melamine is removed, is added
50 parts of formaldehyde, remaining step are identical with embodiment 1.
Reference examples 2
It is with 1 difference of embodiment: in the step 1 of melamine resin preparation, solution is adjusted to neutrality i.e.
PH=5, remaining step are identical with embodiment 1.
Reference examples 3
It is with 1 difference of embodiment: in the step 2 of melamine resin preparation, does not add ammonium polyphosphate,
But 20 parts of diallyl dimethyl ammonium ammonium chloride is added, remaining step is identical with embodiment 1.
Reference examples 4
It is with 1 difference of embodiment: in the step 2 of melamine resin preparation, 10 parts of ammonium polyphosphates is added
Enter into beaker, 5 parts of ethyl alcohol be added, remaining step is identical with embodiment 1.
Reference examples 5
It is with 1 difference of embodiment: in the step 1 of modified phenolic epoxy acrylic resin preparation, 50 parts of epoxy novolacs
Resin, while 10 parts of modifying agent isophorone diamine, 5 parts of p methoxy phenols and 5 parts of catalyst triethanolamines are added, remaining step
Suddenly identical with embodiment 1.
Reference examples 6
It is with 1 difference of embodiment: in the step 1 of modified phenolic epoxy acrylic resin preparation, 100 parts of epoxy novolacs
Resin, while 30 parts of modifying agent isophorone diamine, 10 parts of p methoxy phenols and 6 parts of catalyst triethanolamines are added, remaining
Step is identical with embodiment 1.
Reference examples 7
It is with 1 difference of embodiment: in the step 1 of modified phenolic epoxy acrylic resin preparation, does not add modification
Agent isophorone diamine, remaining step are identical with embodiment 1.
Reference examples 8
It is with 1 difference of embodiment: slow with separatory funnel in the step 2 of modified phenolic epoxy acrylic resin preparation
Slowly 25 parts of acrylic acid are added dropwise, remaining step is identical with embodiment 1.
Reference examples 9
Be with 1 difference of embodiment: in the preparation of TS-1/ kaolinite nano powder, kaolinite and TS-1 be respectively 30 parts and
30 parts, remaining step is identical with embodiment 1.
Reference examples 10
Be with 1 difference of embodiment: in the preparation of TS-1/ kaolinite nano powder, kaolinite and TS-1 be respectively 50 parts and
20 parts, remaining step is identical with embodiment 1.
Reference examples 11
It is with 1 difference of embodiment: is added without TS-1/ kaolinite nano powder, remaining step and the complete phase of embodiment 1
Together.
The test that the coating being prepared carries out correlated performance respectively is chosen, coating is pressed in 220 DEG C of fire endurance (min)
Obtain according to the detection of standard GB/T/T15442.2-1995, coating quality loss (g) according to GB/T15442.4-1995 standard into
Performing check.
The experimental results showed that coating provided by the invention has good heat resistance and anti-flammability, fire resistant coating exists
When fc-specific test FC, mass loss is bigger, illustrates that resistance to thermal energy is poorer, and fire resistance period is shorter, and anti-flammability is poorer, conversely, property
It can be better；Embodiment 1 arrives embodiment 10, changes the proportion of each raw material composition in fire resistant coating respectively, to coating
Heat resistance and anti-flammability have different degrees of influence, in melamine resin and modified phenolic epoxy acrylic resin
Proportion is 7:3, and when other ingredient dosages are fixed, the impact of performance is best；Reference examples 1 to reference examples 4 change melamino-formaldehyde
The dosage and ph value of mixture of resin raw material, heat resistance and flame retardant effect are decreased obviously, and illustrate that melamine and solution alkaline are strong
Degree produces bigger effect the synthesising property of melamine resin；Reference examples 5 change modified phenolic epoxy third to reference examples 8
Olefin(e) acid resin raw material proportion, effect is also bad, says that modifying agent isophorone diamine and the dosage of other raw materials have coating property
Great influence；Reference examples 9 and example 10 change kaolinite and the proportion of TS-1, and mass loss rate and fire resistance period significantly improve,
Illustrate the compound very big on the influence of its performance of nano material；Therefore there is good high temperature resistant using coating prepared by the present invention and prevent
Fiery effect.
Claims (1)
1. a kind of preparation method of fire resistant coating, it is characterised in that method includes the following steps:
Step 1, under conditions of 60 DEG C, by 70 parts of melamine resins, 30 parts of modified phenolic epoxy acrylic resins, 20
Part pentaerythrite and the uniform hybrid reaction 1h of 25 parts of water form the first mixed solution；
20 parts of antimony trichlorides, 50 parts of talcum powder and 12 parts of TS-1/ kaolinite nano powders are added to first mixing by step 2
In solution, and ultrasonic disperse 30 minutes, obtain the second mixed solution；
0.4 part of heat stabilizer, 0.5 part of levelling agent, 0.5 part of defoaming agent are added in second mixed solution by step 3, and
It is stirred 6 hours under conditions of 60 DEG C with the revolving speed of 1500r/min, fire resistant coating is made；
The melamine resin the preparation method is as follows:
10 parts of melamines, 40 parts of formaldehyde and 15 parts of water are added in beakers and stir by step 1, and with the carbonic acid of mass concentration 5%
Sodium solution adjusts PH=8, pours into reaction vessel and stirs, and is warming up to 70 ~ 80 DEG C, stirring rate 3500r/min, reacts 30min
After obtain pre-polymerization liquid；
20 parts of ammonium polyphosphates are added in beaker by step 2, and 15 parts of ethyl alcohol are added, and are dispersed with stirring uniformly, are obtained ammonium polyphosphate
Then pre-polymerization liquid is added in ammonium polyphosphate suspension by suspension, adjust PH=5 with dilute hydrochloric acid, then heat to 80 DEG C, with
The rate of 550r/min is stirred to react 2h, is filtered, washed, dried, that is, obtains melamine resin；The phenolic aldehyde
Epoxy acrylic resin the preparation method is as follows:
100 parts of novolac epoxy resins are added in four-hole boiling flask, while 20 parts of modifying agent isophorone diamine, 5 are added for step 1
Part p methoxy phenol and 5 parts of catalyst triethanolamines, stirring evenly dissolves resin all；
Step 2 is warming up to 80 DEG C, 55 parts of acrylic acid is slowly added dropwise with separatory funnel, control is added dropwise in 3h is warming up to 90
DEG C and keep the temperature, strict control reaction temperature maintain reaction, until reaction acid value be less than 15mgKOH/g, stop reaction；
Appropriate 90 DEG C of hot water is added in step 3, stirs 20min, upper solution is gone in stratification hypsokinesis, to remove unreacted third
Olefin(e) acid, modifying agent, p methoxy phenol and catalyst, in triplicate, finally the moisture in removing system obtains modified phenolic
Epoxy acrylic resin；
The TS-1/ kaolinite process for preparing nm powder is as follows:
20 parts of kaolinites are crushed to 100 mesh, then smashed kaolinite mountain flour is placed in electric furnace heating device with 10 DEG C/min
Heating rate be heated to 1000 DEG C of heat preservation 3h after, be made kaolinite stone powder, by 50 parts of TS-1 zeolite molecular sieve powder with obtain
Kaolinite stone powder mixing, then be added 45 parts of glycerine fusion agents stir evenly, the oil bath 2h at 300 DEG C, therebetween at interval of
0.5 stirs evenly once, stands 1h or more at room temperature, discards supernatant, clean lower layer's substance with ultrapure water, then does at 110 DEG C
It is dry to constant weight, sieved with 100 mesh sieve after grinding, obtain TS-1/ kaolinite nano powder.
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| CN112625541A (en) * | 2020-12-08 | 2021-04-09 | 沈阳化工大学 | Hierarchical-pore nano-zeolite modified epoxy flame-retardant coating |
| CN112831235A (en) * | 2021-01-06 | 2021-05-25 | 浙江海悦绿建科技有限公司 | Wood structure flame-retardant coating and preparation method thereof |
| CN117126509A (en) * | 2023-09-12 | 2023-11-28 | 山东省舜天化工集团有限公司 | Fireproof flame-retardant melamine formaldehyde resin and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659823A (en) * | 2009-09-27 | 2010-03-03 | 中国科学技术大学 | Expanded type fireproof coating and preparation method thereof |
| CN102286228A (en) * | 2011-06-20 | 2011-12-21 | 无锡广信感光科技有限公司 | Preparation method of high temperature resistant non-halogen fire resistant ultraviolet curing solder resist ink |
| CN105694627A (en) * | 2016-02-19 | 2016-06-22 | 徐冉 | Waterborne fireproof coating for steel structure and preparation method of waterborne fireproof coating |
| CN106221511A (en) * | 2016-07-25 | 2016-12-14 | 宋晓梅 | A kind of uv-curing type transparent flame-retarding chemical coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101659823A (en) * | 2009-09-27 | 2010-03-03 | 中国科学技术大学 | Expanded type fireproof coating and preparation method thereof |
| CN102286228A (en) * | 2011-06-20 | 2011-12-21 | 无锡广信感光科技有限公司 | Preparation method of high temperature resistant non-halogen fire resistant ultraviolet curing solder resist ink |
| CN105694627A (en) * | 2016-02-19 | 2016-06-22 | 徐冉 | Waterborne fireproof coating for steel structure and preparation method of waterborne fireproof coating |
| CN106221511A (en) * | 2016-07-25 | 2016-12-14 | 宋晓梅 | A kind of uv-curing type transparent flame-retarding chemical coating and preparation method thereof |
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