CN108753123A - A kind of composite graphite alkene prepares the preparation method of electrically conductive intumescent paints - Google Patents
A kind of composite graphite alkene prepares the preparation method of electrically conductive intumescent paints Download PDFInfo
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- CN108753123A CN108753123A CN201810531707.3A CN201810531707A CN108753123A CN 108753123 A CN108753123 A CN 108753123A CN 201810531707 A CN201810531707 A CN 201810531707A CN 108753123 A CN108753123 A CN 108753123A
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- preparation
- electrically conductive
- prepares
- intumescent paints
- graphite alkene
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Classifications
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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
- 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
- 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
- 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
- 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
Abstract
The present invention is to gather materials with polyester resin, spherical graphite/graphene composite powder 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 inexpensive fire-retardant composite coating of multifunction, with excellent fire-retardancy and electric conductivity, the functionalization of anti-flaming dope is contributed to develop.
Description
Technical field
The invention belongs to chemical building material and technical field of fire safety, more particularly to a kind of composite graphite alkene prepares electrically conductive
The preparation method of intumescent paints.
Background technology
Intumescent paints (IFR) are the current main trend for realizing the non-halogen ecodevelopment of fire proofing, burning
The porous foamed chars of Shi Shengcheng have the mass-and heat-transfers barrier effects such as heat-insulated, oxygen barrier, prevention volatile matter escapes and oxygen is spread
It answers, and the gaseous free radicals that the free radical that contains of layer of charcoal can be formed with mixture thermal degradation react, terminates high polymer thermal cracking
Radical reaction chain slows down the thermal degradation in condensed phase by layer of charcoal protection high polymer.But the multifunction of anti-flaming dope develops
Current important developing direction is had become, such as anti-flaming dope also needs have antistatic and electro-magnetic screen function under special operation condition；
Additionally by process such as organic modifiers doping, the flame retardant property and water resistance of IFR are further increased.But utilize graphite
Modified expanded type anti-flaming dope is aided with organic modifiers and dispersant etc., prepares the research of the conductive fire-retardant composite coating of functionalization
It has not been reported.
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 preparations of composite graphite alkene to lead
The preparation method of electric expansion type anti-flaming dope.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of composite graphite alkene prepares the preparation method of electrically conductive intumescent paints, 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；
Spherical graphite/graphene composite powder and dimethyl silicone polymer are finally sequentially added into intumescent paints, into
The stirring of row third time is 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 microcosmic spherical graphite is in elliposoidal, and its average grain diameter is less than 8 μm.
The graphene film layer thickness is less than 2nm, and piece diameter is 5-10 μm.
The time that the graphite composite powder is added continues 5min~8min.
The kinematic viscosity of the dimethyl silicone polymer is 300~400cs.
The polyester resin, pentaerythrite, urea and ammonium polyphosphate addition continue 3min~5min total time.
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.
Graphene is one kind with sp2The single layer of carbon atom that hybridized orbit is formed is in cellular two dimensional crystal, is not only had excellent
Different conduction, high-termal conductivity and mechanical property also has stronger water resistance, can be used as Nano filling and set applied to fire proofing
In meter.Spheroidal graphite materials have excellent electric conductivity and chemical stability, environmentally protective, and the present invention uses spherical graphite/stone
The black modified expanded type anti-flaming dope of alkene, is theoretically scientific and operability.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) the novelty of the present invention is open with spherical graphite/graphene composite powder, dimethyl silicone polymer, silicon
Sour sodium, ammonium polyphosphate, pentaerythrite, urea, polyester resin prepare conductive expansibility flame-proof composite coating, and it is fire-retardant to improve its
While performance, its electric conductivity is improved.
(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 the preparation methods that a kind of composite graphite alkene prepares electrically conductive intumescent paints, with quality hundred
Score 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, 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 5min total times, carries out second and stirs, stirring condition 60
DEG C, 500r/min stir 30min, be made intumescent paints；
Formula ratio spherical graphite/graphene composite powder and dimethyl silicone polymer are finally sequentially added expansion type flame-retarding to apply
Material, the time that composite powder is added continue 5min, carry out third time stirring, stirring condition be 1000r/min stirring 15min to get
To conductive fire-retardant composite coating.
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 heat release
It measures (THR), fire performance index (FPI, FPI=TTI/p-HRR) and flame spread index (FGI, FGI=p-HRR/Tp),
Middle FPI is higher, FGI is lower, shows that the flame retardant property of material is higher.Measure resistance between two diagonal lines respectively using multimeter simultaneously
It is averaged, the results are shown in Table 1.
Comparative example：
This comparative example provides the preparation method that a kind of composite graphite alkene prepares electrically conductive intumescent paints, raw material composition
Same embodiment, different is, wherein not including spherical graphite/graphene composite powder and dimethyl silicone polymer.Preparation process
Same embodiment, testing result are shown in Table 1.
As seen from Table 1 using incorporation spherical graphite/graphene composite powder, can make by ammonium polyphosphate, pentaerythrite, urine
The flame retardant property of element, polyester resin composition coating significantly improves, and shows as Total amount of heat release and is down to 63.37MW/m from 182.892,
Its fire performance index FPI increases simultaneously, and fire spread index FGI is reduced, and shows that the possibility that it occurs with a loud crash significantly drops
Low, flame retardant property improves；In addition its resistance value is down to 0.18 Ω/cm2。
The flame retardant property and electric conductivity of 1 embodiment of table and comparative example
Embodiment 2：
The present embodiment provides the preparation methods that a kind of composite graphite alkene prepares electrically conductive intumescent paints, with quality hundred
Score 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, 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 3min total times, carries out second and stirs, stirring condition 70
DEG C, 400r/min stir 30min, be made intumescent paints；
Formula ratio spherical graphite/graphene composite powder and dimethyl silicone polymer are finally sequentially added expansion type flame-retarding to apply
Material, the time that composite powder is added continue 8min, carry out third time stirring, stirring condition be 1500r/min stirring 10min to get
To conductive fire-retardant composite coating.
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 heat release
It measures (THR), fire performance index (FPI, FPI=TTI/p-HRR) and flame spread index (FGI, FGI=p-HRR/Tp),
Middle FPI is higher, FGI is lower, shows that the flame retardant property of material is higher.Measure resistance between two diagonal lines respectively using multimeter simultaneously
It is averaged, it is as a result similar to Example 1.
Embodiment 3：
The present embodiment provides the preparation methods that a kind of composite graphite alkene prepares electrically conductive intumescent paints, with quality hundred
Score 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, 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 times, carries out second and stirs, stirring condition 65
DEG C, 450r/min stir 30min, be made intumescent paints；
Formula ratio spherical graphite/graphene composite powder and dimethyl silicone polymer are finally sequentially added expansion type flame-retarding to apply
Material, the time that composite powder is added continue 6min, carry out third time stirring, stirring condition be 1200r/min stirring 20min to get
To conductive fire-retardant composite coating.
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 heat release
It measures (THR), fire performance index (FPI, FPI=TTI/p-HRR) and flame spread index (FGI, FGI=p-HRR/Tp),
Middle FPI is higher, FGI is lower, shows that the flame retardant property of material is higher.Measure resistance between two diagonal lines respectively using multimeter simultaneously
It is averaged, it is as a result similar to Example 1.
To sum up, the present invention is to gather materials with polyester resin, and spherical graphite/graphene composite powder is to strengthen fire retardant and conduction material
Material, sodium metasilicate are dispersant, and dimethyl silicone polymer is film forming agent and modifying agent, prepare novel environment friendly, low cost it is multi-functional
Change fire-retardant composite coating, there is excellent fire-retardancy and electric conductivity, the functionalization of anti-flaming dope is contributed to develop.
Claims (10)
1. a kind of composite graphite alkene prepares the preparation method of electrically conductive intumescent paints, which is characterized in that including walking as follows
Suddenly：
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；
Spherical graphite/graphene composite powder and dimethyl silicone polymer are finally sequentially added into intumescent paints, carry out the
Triple mixing is to get to conductive fire-retardant composite coating.
2. composite graphite alkene prepares the preparation method of electrically conductive intumescent paints according to claim 1, feature exists
In being calculated in mass percent, each raw material dosage is as follows in preparation process：
The sum of mass percent of raw material is 100%.
3. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, the microcosmic spherical graphite is in elliposoidal, and its average grain diameter is less than 8 μm.
4. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, the graphene film layer thickness is less than 2nm, and piece diameter is 5~10 μm.
5. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, the time that the graphite composite powder is added continues 5min~8min.
6. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, the kinematic viscosity of the dimethyl silicone polymer is 300~400cs.
7. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, the polyester resin, pentaerythrite, urea and ammonium polyphosphate addition continue 3min~5min total time.
8. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, the first time stirring condition is 60 DEG C~70 DEG C, 100r/min~200r/min stirs 10min.
9. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, feature
It is, second of stirring condition is 60 DEG C~70 DEG C, 400r/min~500r/min stirs 30min.
10. composite graphite alkene according to claim 1 or claim 2 prepares the preparation method of electrically conductive intumescent paints, special
Sign is that the third time stirring condition is that 1000r/min~1500r/min stirs 10min~15min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810531707.3A CN108753123A (en) | 2018-05-29 | 2018-05-29 | A kind of composite graphite alkene prepares the preparation method of electrically conductive intumescent paints |
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| CN201810531707.3A CN108753123A (en) | 2018-05-29 | 2018-05-29 | A kind of composite graphite alkene prepares the preparation method of electrically conductive intumescent paints |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002080729A (en) * | 2000-09-11 | 2002-03-19 | Daicel Chem Ind Ltd | Flame-retarded resin composition |
| CN106810875A (en) * | 2015-12-02 | 2017-06-09 | 中国科学院金属研究所 | A kind of thermal conductivity composite of graphene-containing and its preparation method and application |
| CN107216743A (en) * | 2017-07-07 | 2017-09-29 | 北京化工大学 | A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof |
| 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 CN201810531707.3A patent/CN108753123A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002080729A (en) * | 2000-09-11 | 2002-03-19 | Daicel Chem Ind Ltd | Flame-retarded resin composition |
| CN106810875A (en) * | 2015-12-02 | 2017-06-09 | 中国科学院金属研究所 | A kind of thermal conductivity composite of graphene-containing and its preparation method and application |
| CN107216743A (en) * | 2017-07-07 | 2017-09-29 | 北京化工大学 | A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof |
| 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 (3)
| Title |
|---|
| 尹洪峰等: "阻燃剂与阻燃机理", 《功能复合材料》 * |
| 朱万强: "有机硅类", 《涂料基础教程》 * |
| 王文广: "添加无机阻燃剂", 《聚合物改性原理》 * |
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Application publication date: 20181106 |
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