CN108485500A - A kind of preparation method of anti-oxidation anti-flaming dope - Google Patents
A kind of preparation method of anti-oxidation anti-flaming dope Download PDFInfo
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- CN108485500A CN108485500A CN201810365835.5A CN201810365835A CN108485500A CN 108485500 A CN108485500 A CN 108485500A CN 201810365835 A CN201810365835 A CN 201810365835A CN 108485500 A CN108485500 A CN 108485500A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
-
- 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
- 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
- C09D7/63—Additives non-macromolecular organic
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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
- C08L2201/02—Flame or fire retardant/resistant
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention provides a kind of preparation method of anti-oxidation anti-flaming dope, phenolic resin and nitrile rubber are uniformly mixed, it is stirred after continuously adding dibenzoyl peroxide, pentaerythrite and salicylic acid, temperature is risen to 100 120 DEG C with the heating rate of 36 DEG C/min in whipping process, 1 2h postcoolings to room temperature of heat preservation obtains phenol-formaldehyde resin modified；Phenol-formaldehyde resin modified, ethyl cellulose, dibutyl tin laurate and butyl glycol ether are ultrasonically treated 20 40min, obtain mixed liquor A；Aqueous polyurethane emulsion, pure-acrylic emulsion, N isopropylhydroxylas and 2 naphthols, 6 sulfonic acid are stirred, mixed liquor A is added, be added dropwise the sodium bicarbonate solution of 0.2 0.5mol/L to pH be 79, temperature is risen to 130 150 DEG C with 48 DEG C/min speed, 30 60min of insulation reaction, 20 40min of subsequent high speed dispersion, can be obtained the anti-oxidation anti-flaming dope after cooling.
Description
Technical field
The present invention relates to the preparing technical fields of coating, and in particular to a kind of preparation method of anti-oxidation anti-flaming dope.
Background technology
With the development of construction industry, the demand of coating is growing day by day.Coating is a kind of material, and this material can be used not
Same construction technology is formed and is adhered to securely, with some strength, continuous solid film, in this way formation coated in object surface
Film be generally called film, also known as paint film or coating.Object is exposed among air, by the erosion of oxygen, moisture etc., is be easy to cause
The breakoff phenomenons such as corrosion of metal, foxiness, cement weathering are coated with coating in object surface, form layer protecting film, can hinder
Only or postpone the occurrence and development of these breakoff phenomenons, the service life of a variety of materials can be made to extend the service life and extended.
Polyurethane coating has good dicoration, and because of its good flexibility, impact resistance because of its appearance of film grace
Property, corrosion resistance, chemical-resistant and excellent lower temperature resistance and the features such as wearability, hardness is big, high resiliency, widely answer
In decoration and protection for fields such as car and boat, aviation, electronics, building, bridge, lathe, woodenware and indoor decorations, at the same it is also big
Anti-corrosion protection and decoration of the amount for the industry such as petrochemical equipment, pipeline, marine facility, heavy-duty machinery.However, polyurethane coating
Flame retardant property it is also very poor, when fire occurs, good fire retardation cannot be played, the sprawling of the intensity of a fire cannot be inhibited, and
Polyurethanes also has combustion-supporting effect.Therefore, there are prodigious defects in terms of fire preventing for polyurethane coating.
Invention content
The purpose of the present invention is the deficiency for polyurethane coating in the prior art, a kind of anti-oxidation anti-flaming dope is provided
Preparation method is aided with the ingredients such as ethyl cellulose, lotion, improves the fire-retardant and oxygen of coating with phenol-formaldehyde resin modified for main matrix
Change performance, extends its service life and safety.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
A kind of preparation method of anti-oxidation anti-flaming dope, includes the following steps：
S1：20-40 parts of phenolic resin and 8-12 parts of nitrile rubbers are uniformly mixed, 1-3 parts of diphenyl peroxides are continuously added
It is stirred with the mixing speed of 300-400rpm/min after formyl, 0.5-2 part pentaerythrite and 3-10 parts of salicylic acids, in whipping process
In with the heating rate of 3-6 DEG C/min temperature is risen to 100-120 DEG C, heat preservation 1-2h postcoolings to room temperature obtains modified phenolic resin
Fat；
S2：By 8-10 parts of phenol-formaldehyde resin modifieds, 4-8 parts of ethyl celluloses, 3-6 parts of dibutyl tin laurates and 10-15
Part butyl glycol ether is ultrasonically treated 20-40min, and the frequency of supersound process is 20-30KHz, and the power of supersound process is 1000-
The burst length of 1400W, supersound process are 8-12s, obtain mixed liquor A；
S3：By 40-50 parts of aqueous polyurethane emulsions, 20-30 parts of pure-acrylic emulsions, 3-6 parts of N- isopropylhydroxylas and 5-7 parts of 2-
Naphthols -6- sulfonic acid is stirred, and mixed liquor A in step S2 is added, and the sodium bicarbonate solution of 0.2-0.5mol/L is added dropwise to pH
For 7-9, temperature is risen to 130-150 DEG C with 4-8 DEG C/min speed, insulation reaction 30-60min, subsequent high speed dispersion 20-
40min can be obtained the anti-oxidation anti-flaming dope after cooling.
Preferably, 30 parts of phenolic resin and 10 parts of nitrile rubbers are uniformly mixed in step S1, continuously add 2 parts of peroxidating
Dibenzoyl, 1.5 parts of pentaerythrites and 7 parts of salicylic acids.
Preferably, mixing speed is 300-400rpm/min in step S1, and temperature is risen to 116 DEG C with 4 DEG C/min of rate,
Keep the temperature 1.5h.
Preferably, in step S2 by 9 parts of phenol-formaldehyde resin modifieds, 7 parts of ethyl celluloses, 5 parts of dibutyl tin laurates and
13 parts of butyl glycol ether mixing.
Preferably, the frequency being ultrasonically treated in step S2 is 25KHz, and the power of supersound process is 1200W, supersound process
Burst length is 10s, time 35min.
Preferably, by 45 parts of aqueous polyurethane emulsions, 25 parts of pure-acrylic emulsions, 5 parts of N- isopropylhydroxylas and 6 parts in step S3
Beta naphthal -6- sulfonic acid.
Preferably, in step S3 be added dropwise 0.35mol/L sodium bicarbonate solution to pH be 8.5, will be warm with 6 DEG C/min speed
Degree rises to 140 DEG C, insulation reaction 35min, subsequent high speed dispersion 25min.
Advantageous effect：
The preparation method of a kind of anti-oxidation anti-flaming dope of the present invention, with nitrile rubber, dibenzoyl peroxide, season penta
Tetrol and salicylic acid etc. obtain phenol-formaldehyde resin modified, and the substances such as ethyl cellulose is coordinated to obtain mixed liquor A, to improve coating
Flame retardant effect；By the way that the ingredients such as N- isopropylhydroxylas, beta naphthal -6- sulfonic acid are added, the oxidation proof propertiess of coating are improved；In second two
In the presence of alcohol butyl ether, aqueous polyurethane emulsion, pure-acrylic emulsion etc., dispersed more preferable, coating property is evenly.
Specific implementation mode
It being further illustrated the present invention below in conjunction with following embodiments, following embodiments are merely to illustrate the present invention, and
The unrestricted present invention.
Embodiment 1
S1：20 parts of phenolic resin and 8 parts of nitrile rubbers are uniformly mixed, 1 part of dibenzoyl peroxide, 0.5 are continuously added
It is stirred with the mixing speed of 300rpm/min after part pentaerythrite and 3 parts of salicylic acids, with the heating of 3 DEG C/min in whipping process
Temperature is risen to 100 DEG C by speed, and heat preservation 1h postcoolings to room temperature obtains phenol-formaldehyde resin modified；
S2：By 8 parts of phenol-formaldehyde resin modifieds, 4 parts of ethyl celluloses, 3 parts of dibutyl tin laurates and 10 parts of ethylene glycol fourths
Ether is ultrasonically treated 20min, and the frequency of supersound process is 20KHz, and the power of supersound process is 1000W, when the pulse of supersound process
Between be 8s, obtain mixed liquor A；
S3：By 40 parts of aqueous polyurethane emulsions, 20 parts of pure-acrylic emulsions, 3 parts of N- isopropylhydroxylas and 5 parts of beta naphthal -6- sulphurs
Acid is stirred, and mixed liquor A in step S2 is added, be added dropwise the sodium bicarbonate solution of 0.2mol/L to pH be 7, with 4 DEG C/min
Temperature is risen to 130 DEG C by speed, and insulation reaction 30min, subsequent high speed dispersion 20min can be obtained the oxygen after cooling
Change anti-flaming dope.
After testing, the flame retardant rating of above-mentioned anti-oxidation anti-flaming dope is UL94V-0, and antioxygenic property is good, and coating uses
Service life extends 420%.
Embodiment 2
S1：40 parts of phenolic resin and 12 parts of nitrile rubbers are uniformly mixed, continuously add 3 parts of dibenzoyl peroxides, 2 parts
It is stirred with the mixing speed of 400rpm/min after pentaerythrite and 10 parts of salicylic acids, with the heating of 6 DEG C/min in whipping process
Temperature is risen to 120 DEG C by speed, and heat preservation 2h postcoolings to room temperature obtains phenol-formaldehyde resin modified；
S2：By 10 parts of phenol-formaldehyde resin modifieds, 8 parts of ethyl celluloses, 6 parts of dibutyl tin laurates and 15 parts of ethylene glycol fourths
Ether is ultrasonically treated 40min, and the frequency of supersound process is 30KHz, and the power of supersound process is 1400W, when the pulse of supersound process
Between be 12s, obtain mixed liquor A；
S3：By 50 parts of aqueous polyurethane emulsions, 30 parts of pure-acrylic emulsions, 6 parts of N- isopropylhydroxylas and 7 parts of beta naphthal -6- sulphurs
Acid is stirred, and mixed liquor A in step S2 is added, be added dropwise the sodium bicarbonate solution of 0.5mol/L to pH be 9, with 8 DEG C/min
Temperature is risen to 150 DEG C by speed, and insulation reaction 60min, subsequent high speed dispersion 40min can be obtained the oxygen after cooling
Change anti-flaming dope.
After testing, the flame retardant rating of above-mentioned anti-oxidation anti-flaming dope is UL94V-0, and antioxygenic property is good, and coating uses
Service life extends 45%.
Embodiment 3
S1：25 parts of phenolic resin and 10 parts of nitrile rubbers are uniformly mixed, 1 part of dibenzoyl peroxide, 0.8 are continuously added
It is stirred with the mixing speed of 340rpm/min after part pentaerythrite and 5 parts of salicylic acids, with the heating of 4 DEG C/min in whipping process
Temperature is risen to 105 DEG C by speed, and heat preservation 1.5h postcoolings to room temperature obtains phenol-formaldehyde resin modified；
S2：By 8 parts of phenol-formaldehyde resin modifieds, 5 parts of ethyl celluloses, 4 parts of dibutyl tin laurates and 12 parts of ethylene glycol fourths
Ether is ultrasonically treated 25min, and the frequency of supersound process is 22KHz, and the power of supersound process is 1200W, when the pulse of supersound process
Between be 10s, obtain mixed liquor A；
S3：By 42 parts of aqueous polyurethane emulsions, 23 parts of pure-acrylic emulsions, 4 parts of N- isopropylhydroxylas and 5 parts of beta naphthal -6- sulphurs
Acid is stirred, and mixed liquor A in step S2 is added, be added dropwise the sodium bicarbonate solution of 0.25mol/L to pH be 7.5, with 5 DEG C/
Temperature is risen to 135 DEG C, insulation reaction 35min, subsequent high speed dispersion 23min by min speed, can be obtained after cooling described anti-
Aoxidize anti-flaming dope.
After testing, the flame retardant rating of above-mentioned anti-oxidation anti-flaming dope is UL94V-0, and antioxygenic property is good, and coating uses
Service life extends 43%.
Embodiment 4
S1：35 parts of phenolic resin and 12 parts of nitrile rubbers are uniformly mixed, 3 parts of dibenzoyl peroxides, 1.5 are continuously added
It is stirred with the mixing speed of 380rpm/min after part pentaerythrite and 8 parts of salicylic acids, with the heating of 6 DEG C/min in whipping process
Temperature is risen to 115 DEG C by speed, and heat preservation 2h postcoolings to room temperature obtains phenol-formaldehyde resin modified；
S2：By 10 parts of phenol-formaldehyde resin modifieds, 7 parts of ethyl celluloses, 6 parts of dibutyl tin laurates and 14 parts of ethylene glycol fourths
Ether is ultrasonically treated 35min, and the frequency of supersound process is 28KHz, and the power of supersound process is 1300W, when the pulse of supersound process
Between be 12s, obtain mixed liquor A；
S3：By 48 parts of aqueous polyurethane emulsions, 27 parts of pure-acrylic emulsions, 5 parts of N- isopropylhydroxylas and 6 parts of beta naphthal -6- sulphurs
Acid is stirred, and mixed liquor A in step S2 is added, be added dropwise the sodium bicarbonate solution of 0.35mol/L to pH be 8.5, with 7 DEG C/
Temperature is risen to 145 DEG C, insulation reaction 45min, subsequent high speed dispersion 36min by min speed, can be obtained after cooling described anti-
Aoxidize anti-flaming dope.
After testing, the flame retardant rating of above-mentioned anti-oxidation anti-flaming dope is UL94V-0, and antioxygenic property is good, and coating uses
Service life extends 48%.
Embodiment 5
S1：30 parts of phenolic resin and 10 parts of nitrile rubbers are uniformly mixed, 2 parts of dibenzoyl peroxides, 1.5 are continuously added
It is stirred with the mixing speed of 350rpm/min after part pentaerythrite and 7 parts of salicylic acids, with the heating of 4 DEG C/min in whipping process
Temperature is risen to 116 DEG C by speed, and heat preservation 1.5h postcoolings to room temperature obtains phenol-formaldehyde resin modified；
S2：By 9 parts of phenol-formaldehyde resin modifieds, 7 parts of ethyl celluloses, 5 parts of dibutyl tin laurates and 13 parts of ethylene glycol fourths
Ether is ultrasonically treated 35min, and the frequency of supersound process is 25KHz, and the power of supersound process is 1200W, when the pulse of supersound process
Between be 10s, obtain mixed liquor A；
S3：By 45 parts of aqueous polyurethane emulsions, 25 parts of pure-acrylic emulsions, 5 parts of N- isopropylhydroxylas and 6 parts of beta naphthal -6- sulphurs
Acid is stirred, and mixed liquor A in step S2 is added, be added dropwise the sodium bicarbonate solution of 0.35mol/L to pH be 8.5, with 6 DEG C/
Temperature is risen to 140 DEG C, insulation reaction 35min, subsequent high speed dispersion 25min by min speed, can be obtained after cooling described anti-
Aoxidize anti-flaming dope.
After testing, the flame retardant rating of above-mentioned anti-oxidation anti-flaming dope is UL94V-0, and antioxygenic property is good, and coating uses
Service life extends 50%.
The foregoing is merely the better embodiment of the present invention, protection scope of the present invention is not with the above embodiment
Limit, as long as those of ordinary skill in the art should all be included in power according to equivalent modification or variation made by disclosed content
In protection domain described in sharp claim.
Claims (8)
1. a kind of preparation method of anti-oxidation anti-flaming dope, which is characterized in that include the following steps：
S1：20-40 parts of phenolic resin and 8-12 parts of nitrile rubbers are uniformly mixed, continuously add 1-3 parts of dibenzoyl peroxides,
After 0.5-2 parts of pentaerythrites and 3-10 parts of salicylic acids with the mixing speed of 300-400rpm/min stir, in whipping process with
Temperature is risen to 100-120 DEG C by the heating rate of 3-6 DEG C/min, and heat preservation 1-2h postcoolings to room temperature obtains phenol-formaldehyde resin modified；
S2：By 8-10 parts of phenol-formaldehyde resin modifieds, 4-8 parts of ethyl celluloses, 3-6 parts of dibutyl tin laurates and 10-15 parts of second
Glycol butyl ether is ultrasonically treated 20-40min, and the frequency of supersound process is 20-30KHz, and the power of supersound process is 1000-1400W,
The burst length of supersound process is 8-12s, obtains mixed liquor A；
S3：By 40-50 parts of aqueous polyurethane emulsions, 20-30 parts of pure-acrylic emulsions, 3-6 parts of N- isopropylhydroxylas and 5-7 parts of 2- naphthalenes
Phenol -6- sulfonic acid is stirred, and mixed liquor A in step S2 is added, and the sodium bicarbonate solution of 0.2-0.5mol/L is added dropwise to pH and is
Temperature is risen to 130-150 DEG C, insulation reaction 30-60min, subsequent high speed dispersion 20-40min by 7-9 with 4-8 DEG C/min speed,
It can be obtained the anti-oxidation anti-flaming dope after cooling.
2. a kind of preparation method of anti-oxidation anti-flaming dope according to claim 1, which is characterized in that by 30 in step S1
Part phenolic resin and 10 parts of nitrile rubbers are uniformly mixed, and continuously add 2 parts of dibenzoyl peroxides, 1.5 parts of pentaerythrites and 7 parts
Salicylic acid.
3. a kind of preparation method of anti-oxidation anti-flaming dope according to claim 1, which is characterized in that stirred in step S1
Speed is 300-400rpm/min, and temperature is risen to 116 DEG C with 4 DEG C/min of rate, keeps the temperature 1.5h.
4. a kind of preparation method of anti-oxidation anti-flaming dope according to claim 1, which is characterized in that by 9 in step S2
Part phenol-formaldehyde resin modified, 7 parts of ethyl celluloses, 5 parts of dibutyl tin laurates and 13 parts of butyl glycol ethers mixing.
5. a kind of preparation method of anti-oxidation anti-flaming dope according to claim 1, which is characterized in that ultrasonic in step S2
The frequency of processing is 25KHz, and the power of supersound process is 1200W, and the burst length of supersound process is 10s, time 35min.
6. a kind of preparation method of anti-oxidation anti-flaming dope according to claim 1, which is characterized in that by 45 in step S3
Part aqueous polyurethane emulsion, 25 parts of pure-acrylic emulsions, 5 parts of N- isopropylhydroxylas and 6 parts of beta naphthal -6- sulfonic acid.
7. a kind of preparation method of anti-oxidation anti-flaming dope according to claim 1, which is characterized in that be added dropwise in step S3
The sodium bicarbonate solution of 0.35mol/L is 8.5 to pH, and temperature is risen to 140 DEG C, insulation reaction 35min with 6 DEG C/min speed,
Subsequent high speed dispersion 25min.
8. the anti-oxidation anti-flaming dope obtained according to any one preparation method of claim 1-7.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810365835.5A CN108485500A (en) | 2018-04-23 | 2018-04-23 | A kind of preparation method of anti-oxidation anti-flaming dope |
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| CN201810365835.5A CN108485500A (en) | 2018-04-23 | 2018-04-23 | A kind of preparation method of anti-oxidation anti-flaming dope |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194572A (en) * | 2014-09-25 | 2014-12-10 | 芜湖县双宝建材有限公司 | Anti-corrosion and flame retardant coating |
| CN104293071A (en) * | 2014-09-28 | 2015-01-21 | 芜湖县双宝建材有限公司 | Degradable corrosion-resistant paint |
| CN105315820A (en) * | 2015-12-09 | 2016-02-10 | 郑州仁宏医药科技有限公司 | Waterproofing acid-proofing anti-collision insulating coating |
-
2018
- 2018-04-23 CN CN201810365835.5A patent/CN108485500A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194572A (en) * | 2014-09-25 | 2014-12-10 | 芜湖县双宝建材有限公司 | Anti-corrosion and flame retardant coating |
| CN104293071A (en) * | 2014-09-28 | 2015-01-21 | 芜湖县双宝建材有限公司 | Degradable corrosion-resistant paint |
| CN105315820A (en) * | 2015-12-09 | 2016-02-10 | 郑州仁宏医药科技有限公司 | Waterproofing acid-proofing anti-collision insulating coating |
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Application publication date: 20180904 |