CN108753021A - A kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating - Google Patents
A kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating Download PDFInfo
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- CN108753021A CN108753021A CN201810530236.4A CN201810530236A CN108753021A CN 108753021 A CN108753021 A CN 108753021A CN 201810530236 A CN201810530236 A CN 201810530236A CN 108753021 A CN108753021 A CN 108753021A
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- polyester resin
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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
- C09D5/24—Electrically-conducting 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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
-
- 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
- C09D5/185—Intumescent 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
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
-
- 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
- C09D7/65—Additives macromolecular
-
- 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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- 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
- C08L2201/04—Antistatic
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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)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention proposes a kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating, it is to gather materials with polyester resin, graphite is to strengthen fire retardant and conductive material, sodium metasilicate is dispersant, dimethyl silicone polymer is film forming agent and modifying agent, prepare novel environment friendly, the fire-retardant composite coating of multifunction of low cost contributes to the functionalization of anti-flaming dope to develop with excellent fire-retardancy and electric conductivity.
Description
Technical field
The invention belongs to chemical building material and technical field of fire safety, more particularly to a kind of polyester resin-based conduction intumescent
The preparation method of fire-retardant composite coating.
Background technology
Intumescent paints (IFR) are the main trends for realizing the non-halogen ecodevelopment of fire proofing, are given birth to when burning
At porous foamed char, there is the mass-and heat-transfers barrier effects such as heat-insulated, oxygen barrier, prevention volatile matter effusion and oxygen diffusion, and
The gaseous free radicals that the free radical that layer of charcoal contains can be formed with mixture thermal degradation react, and terminate the free radical of high polymer thermal cracking
Reaction chain slows down the thermal degradation in condensed phase by layer of charcoal protection high polymer.But intumescent paints but there are still still
The defect that problem to be solved and own material structure are brought, is mainly shown as：(1) flame retardant property needs to be further increased；(2)
Water resistance is relatively low, and film cracking is also easy to produce when curing shrinkage, and hydroscopicity is high；(3) impact resistance is weak, and coating is crisp and nothing
Elasticity, does not adapt to base material breathing variation and the ability etc. closed is opened in crack.Meanwhile realizing the multifunction development of anti-flaming dope
As current important developing direction, such as conductive coating, but the record at present about conductive fire-retardant composite coating is still rare.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of expansions of polyester resin-based conduction
The preparation method of the fire-retardant composite coating of type can improve the flame retardant property and electric conductivity of coating simultaneously.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating, includes the following steps：
Dispersant solution prefabricated first：Nine water sodium metasilicate of dispersant is dissolved in gauge water after carrying out first time stirring and is obtained
It arrives；
Then polyester resin-based intumescent paints are prepared：Successively by polyester resin, pentaerythrite, urea and polyphosphoric acid
Prefabricated dispersant solution is added in ammonium, carries out second and stirs, intumescent paints are made；
Graphite and dimethyl silicone polymer are finally sequentially added into intumescent paints, carry out third time stirring to get
To conductive fire-retardant composite coating.
It is calculated in mass percent, each raw material dosage is as follows in preparation process：
The sum of mass percent of raw material is 100%.
The graphite is flakey, and its average grain diameter is less than 2.6 μm, and the time of addition continues 5min~8min.
The ammonium polyphosphate, pentaerythrite, urea and polyester resin addition continue 3min~5min total time.
The kinematic viscosity of the dimethyl silicone polymer is 300~400cs.
The first time stirring condition is 60 DEG C~70 DEG C, 100r/min~200r/min stirs 10min；Second of stirring
Condition is 60 DEG C~70 DEG C, 400r/min~500r/min stirs 30min；Third time stirring condition be 1000r/min~
1500r/min stirs 10min~15min.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the novelty of the present invention is open with graphite, dimethyl silicone polymer, sodium metasilicate, ammonium polyphosphate, season penta
Tetrol, urea, polyester resin prepare conductive expansibility flame-proof composite coating and improve it while improving its flame retardant property
Electric conductivity.
(2) not only excellent fireproof performance, antistatic effect enhancing, self-extinguishment are stronger for composite coating prepared by the present invention.
(3) cost of raw material used in the present invention is cheap, environmentally friendly, and preparation condition is mild, and technique is simple.
Specific implementation mode
In order to make objects and advantages of the present invention be more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.The specific embodiments described herein are merely illustrative of the present invention, is not intended to limit the present invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of polyester resin-based conduction expansion type flame-retarding composite coating, with quality percentage
Number meter, it is as follows using raw material：
Preparation process is as follows：
Dispersant solution prefabricated first：The nine water sodium metasilicate of dispersant of formula ratio is dissolved in gauge water and stir for the first time
It is obtained after mixing, wherein stirring condition is 70 DEG C, 100r/min stirs 10min；
Then polyester resin-based intumescent paints are prepared：Successively by the polyester resin of formula ratio, pentaerythrite, urine
Prefabricated dispersant solution is added in element, ammonium polyphosphate, and addition continues 5min total time.It carries out second to stir, stirring condition 70
DEG C, 500r/min stir 30min, be made intumescent paints,；
Formula ratio graphite and dimethyl silicone polymer are finally sequentially added into intumescent paints, the time that graphite is added
Continue 5min, carry out third time stirring, stirring condition is that 1500r/min stirs 10min to get to conductive fire-retardant compound painting
Material.
The flame retardant property and electric conductivity that prepared composite coating is measured using glued board as carrier, composite coating is coated in
Glued board (97 × 97 × 4mm3) sample surfaces, it is tested using cone calorimetry with reference to 5660 standards of ISO and calculates its anti-flammability
Can, including highest heat release rate (p-HRR), highest heat release rate time (Tp) burning time (TTI), maximum Total amount of heat release
(THR), fire performance index (FPI, FPI=TTI/p-HRR) and flame spread index (FGI, FGI=p-HRR/Tp), wherein
FPI is higher, FGI is lower, shows that the flame retardant property of material is higher.It measures the resistance between two diagonal lines respectively using multimeter and takes
Average value the results are shown in Table 1.
Comparative example：
This comparative example provides a kind of preparation method of polyester resin-based expansion type flame-retarding composite coating, and raw material composition is the same as implementation
Example 1, different is, wherein not including graphite and dimethyl silicone polymer.With embodiment 1, testing result is shown in Table preparation process
1。
As seen from Table 1 using incorporation graphite and dimethyl silicone polymer, can make by ammonium polyphosphate, pentaerythrite, urea,
The flame retardant property of polyester resin composition coating significantly improves, and shows as Total amount of heat release and is down to 63.59MW/m from 182.892, simultaneously
Its fire performance index FPI increases, and fire spread index FGI is reduced, and shows that the possibility that it is flashed over significantly reduces, resistance
Performance is fired to improve；In addition its resistance value is down to 0.22 Ω/cm2。
The flame retardant property and electric conductivity of 1 embodiment of table and comparative example
Note：FPI=TTI/p-HHR, FGI=p-HHR/Tp
Embodiment 2
The present embodiment is calculated in mass percent, as follows using raw material：
Preparation process is as follows：
Dispersant solution prefabricated first：The nine water sodium metasilicate of dispersant of formula ratio is dissolved in gauge water and stir for the first time
It is obtained after mixing, wherein stirring condition is 60 DEG C, 200r/min stirs 10min；
Then polyester resin-based intumescent paints are prepared：Successively by the polyester resin of formula ratio, pentaerythrite, urine
Prefabricated dispersant solution is added in element, ammonium polyphosphate, and addition continues 3min total time.It carries out second to stir, stirring condition 60
DEG C, 400r/min stir 30min, be made intumescent paints,；
Formula ratio graphite and dimethyl silicone polymer are finally sequentially added into intumescent paints, the time that graphite is added
Continue 8min, carry out third time stirring, stirring condition is that 1000r/min stirs 15min to get to conductive fire-retardant compound painting
Material.
The flame retardant property and electric conductivity that prepared composite coating is measured using glued board as carrier, composite coating is coated in
Glued board (97 × 97 × 4mm3) sample surfaces, it is tested using cone calorimetry with reference to 5660 standards of ISO and calculates its anti-flammability
Can, including highest heat release rate (p-HRR), highest heat release rate time (Tp) burning time (TTI), maximum Total amount of heat release
(THR), fire performance index (FPI, FPI=TTI/p-HRR) and flame spread index (FGI, FGI=p-HRR/Tp), wherein
FPI is higher, FGI is lower, shows that the flame retardant property of material is higher.It measures the resistance between two diagonal lines respectively using multimeter and takes
Average value, it is as a result similar to Example 1.
Embodiment 3
The present embodiment is calculated in mass percent, as follows using raw material：
Preparation process is as follows：
Dispersant solution prefabricated first：The nine water sodium metasilicate of dispersant of formula ratio is dissolved in gauge water and stir for the first time
It is obtained after mixing, wherein stirring condition is 65 DEG C, 150r/min stirs 10min；
Then polyester resin-based intumescent paints are prepared：Successively by the polyester resin of formula ratio, pentaerythrite, urine
Prefabricated dispersant solution is added in element, ammonium polyphosphate, and addition continues 4min total time.It carries out second to stir, stirring condition 65
DEG C, 400r/min stir 30min, be made intumescent paints,；
Formula ratio graphite and dimethyl silicone polymer are finally sequentially added into intumescent paints, the time that graphite is added
Continue 6min, carry out third time stirring, stirring condition is that 1200r/min stirs 15min to get to conductive fire-retardant compound painting
Material.
The flame retardant property and electric conductivity that prepared composite coating is measured using glued board as carrier, composite coating is coated in
Glued board (97 × 97 × 4mm3) sample surfaces, it is tested using cone calorimetry with reference to 5660 standards of ISO and calculates its anti-flammability
Can, including highest heat release rate (p-HRR), highest heat release rate time (Tp) burning time (TTI), maximum Total amount of heat release
(THR), fire performance index (FPI, FPI=TTI/p-HRR) and flame spread index (FGI, FGI=p-HRR/Tp), wherein
FPI is higher, FGI is lower, shows that the flame retardant property of material is higher.It measures the resistance between two diagonal lines respectively using multimeter and takes
Average value, it is as a result similar to Example 1.
To sum up, the present invention is to gather materials with polyester resin, and graphite is to strengthen fire retardant and conductive material, and sodium metasilicate is dispersion
Agent, dimethyl silicone polymer are film forming agent and modifying agent, prepare novel environment friendly, the inexpensive fire-retardant composite coating of multifunction,
With excellent fire-retardancy and electric conductivity, the functionalization of anti-flaming dope is contributed to develop.
Claims (9)
1. a kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating, which is characterized in that include the following steps：
Dispersant solution prefabricated first：Nine water sodium metasilicate of dispersant is dissolved in gauge water after carrying out first time stirring and is obtained；
Then polyester resin-based intumescent paints are prepared：Polyester resin, pentaerythrite, urea and ammonium polyphosphate are added successively
Enter prefabricated dispersant solution, carries out second and stir, intumescent paints are made；
Graphite and dimethyl silicone polymer are finally sequentially added into intumescent paints, carry out third time stirring to get to leading
The composite coating of resistance combustion.
2. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1, which is characterized in that with quality percentage
Number is counted, and each raw material dosage is as follows in preparation process：
The sum of mass percent of raw material is 100%.
3. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that the stone
Ink is flakey, and its average grain diameter is less than 2.6 μm.
4. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that described poly-
The kinematic viscosity of dimethyl siloxane is 300~400cs.
5. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that described
Stirring condition is 60 DEG C~70 DEG C, 100r/min~200r/min stirs 10min.
6. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that the stone
The time that ink is added continues 5min~8min.
7. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that described poly-
Ammonium phosphate, pentaerythrite, urea and polyester resin addition continue 3min~5min total time.
8. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that described
Secondary agitation condition is 60 DEG C~70 DEG C, 400r/min~500r/min stirs 30min.
9. polyester resin-based conduction expansion type flame-retarding composite coating according to claim 1 or claim 2, which is characterized in that described
Triple mixing condition is that 1000r/min~1500r/min stirs 10min~15min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810530236.4A CN108753021A (en) | 2018-05-29 | 2018-05-29 | A kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810530236.4A CN108753021A (en) | 2018-05-29 | 2018-05-29 | A kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating |
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| CN108753021A true CN108753021A (en) | 2018-11-06 |
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| CN201810530236.4A Withdrawn CN108753021A (en) | 2018-05-29 | 2018-05-29 | A kind of preparation method of polyester resin-based conduction expansion type flame-retarding composite coating |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115926342A (en) * | 2022-12-30 | 2023-04-07 | 山东博拓新材料科技股份有限公司 | Combined PVC (polyvinyl chloride) automobile board with fireproof function and production process thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312430A (en) * | 2017-07-13 | 2017-11-03 | 西安建筑科技大学 | A kind of modified expanded type fire retarding wood composite coating of silicon ash |
-
2018
- 2018-05-29 CN CN201810530236.4A patent/CN108753021A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312430A (en) * | 2017-07-13 | 2017-11-03 | 西安建筑科技大学 | A kind of modified expanded type fire retarding wood composite coating of silicon ash |
Non-Patent Citations (2)
| Title |
|---|
| 强涛涛: "《合成革化学品》", 31 July 2016, 中国轻工业出版社 * |
| 边炳鑫等: "《石墨加工与石墨材料》", 31 May 2014, 中国矿业大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115926342A (en) * | 2022-12-30 | 2023-04-07 | 山东博拓新材料科技股份有限公司 | Combined PVC (polyvinyl chloride) automobile board with fireproof function and production process thereof |
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