CN103275605A - Phosphorous alkyd resin overcoating fire retardant coating and preparation method thereof - Google Patents
Phosphorous alkyd resin overcoating fire retardant coating and preparation method thereof Download PDFInfo
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- CN103275605A CN103275605A CN2013102590437A CN201310259043A CN103275605A CN 103275605 A CN103275605 A CN 103275605A CN 2013102590437 A CN2013102590437 A CN 2013102590437A CN 201310259043 A CN201310259043 A CN 201310259043A CN 103275605 A CN103275605 A CN 103275605A
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- 0 *=C(CC1P2(Oc3ccccc3-c3c2cccc3)=O)OC1=O Chemical compound *=C(CC1P2(Oc3ccccc3-c3c2cccc3)=O)OC1=O 0.000 description 1
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Abstract
The invention provides a phosphorous alkyd resin overcoating fire retardant coating and a preparation method thereof. A formula of the phosphorous alkyd resin overcoating fire retardant coating comprises the following components in percentage by weight: 30%-36% of phosphorous alkyd resin, 11.5%-15.8% of ammonium polyphosphate, 9.5%-10.8% of melamine, 4.2%-4.8% of pentaerythritol, 2.7%-3.6% of zinc borate, 4.1%-4.8% of titanium dioxide, 1%-1.2% of molybdenum sesquioxide, 0.1%-0.12% of simethicone, 0.9%-1.08% of drier, and 30%-36% of solvent. The preparation method comprises the steps of sequentially adding the solvent, ammonium polyphosphate, melamine, pentaerythritol, zinc borate, titanium dioxide and molybdenum sesquioxide at the formula ratio to a multipurpose dispersion and grinding machine, dispersing at a high speed for 30-60min, reducing a stirring speed, adding the phosphorated alkyd resin, dispersing for 20-40min, adding simethicone, grinding to the required fineness with a cone mill, dispersing in the multipurpose dispersion and grinding machine for 10-20min, adding the drier, dispersing uniformly, and obtaining the phosphorous alkyd resin overcoating fire retardant coating.
Description
Technical field
The present invention relates to the technology of preparing of finishing fire retardant paint.
Background technology
Finishing fire retardant paint is to decorate and fire prevention is the new coating kind of one a kind of the collection.When it is coated on flammable substrate surface, can play certain decoration function at ordinary times, in case fire takes place, then have the prevention fire spreading, the purpose that reach the protection base material, makes people have time enough to leave the scene of a fire and organize the rescue work.
Patent CN102746774A discloses bromine carbon Synolac finishing fire retardant paint and preparation method thereof, be grouped into by following one-tenth by massfraction: bromine carbon Synolac finishing fire retardant paint prescription is: bromine carbon Synolac 30 ~ 36%, ammonium polyphosphate 14 ~ 16.8%, trimeric cyanamide 9 ~ 10.8%, tetramethylolmethane 4 ~ 4.8%, antimonous oxide 4 ~ 4.8%, zinc borate 3 ~ 3.6%, titanium dioxide 4 ~ 4.8%, molybdenum sesquioxide 1 ~ 1.2%, dimethyl silicone oil 0.1 ~ 0.12%, siccative 0.9 ~ 1.08%, solvent 30 ~ 36%; Total mass based on preparation bromine carbon Synolac, by mass percentage, bromine carbon alkyd resin formulation is: behenic acid 44.70 ~ 67.00%, tetramethylolmethane 8.20 ~ 12.20%, Tetra hydro Phthalic anhydride 8.90 ~ 13.40%, catalyzer 0.02 ~ 0.03%, brominated epoxy resin 14.40 ~ 21.50%, dimethylbenzene 3.90 ~ 5.80%; Based on the total mass of each component of preparation siccative, by mass percentage, prepare consisting of of each component of siccative: cobalt iso-octoate 3.70%, manganese iso-octoate 14.81%, zirconium iso-octoate 14.81%, 200# solvent oil 66.67%.The flame retardant properties of this technology is bad.
Summary of the invention
The purpose of this invention is to provide a kind ofPhosphorous Synolac finishing fire retardant paint and preparation method thereof.
The present invention is phosphorous Synolac finishing fire retardant paint and preparation method thereof, phosphorous Synolac finishing fire retardant paint, based on the total mass of phosphorous Synolac finishing fire retardant paint, by mass percentage, phosphorous Synolac finishing fire retardant paint prescription is:
Phosphorous Synolac 30% ~ 36%, ammonium polyphosphate 11.5% ~ 15.8%, trimeric cyanamide 9.5% ~ 10.8%, tetramethylolmethane 4.2% ~ 4.8%, zinc borate 2.7% ~ 3.6%, titanium dioxide 4.1% ~ 4.8%, molybdenum sesquioxide 1% ~ 1.2%, dimethyl silicone oil 0.1% ~ 0.12%, siccative 0.9% ~ 1.08%, solvent 30% ~ 36%;
Based on the total mass of the phosphorous Synolac of preparation, by mass percentage, phosphorous alkyd resin formulation is:
Behenic acid 50.8% ~ 60.5%, tetramethylolmethane 11.6% ~ 17.8%, Tetra hydro Phthalic anhydride 0% ~ 15.5%, DOPOMA9.5% ~ 20.9%, band aqua 5.1% ~ 7%;
Based on the total mass of each component of preparation siccative, by mass percentage, prepare consisting of of each component of siccative:
Cobalt iso-octoate 3.60%, manganese iso-octoate 14.83%, zirconium iso-octoate 14.71%, 200# solvent oil 66.57%.
The preparation method of phosphorous Synolac finishing fire retardant paint prepares burden by the above component and proportioning thereof, the steps include:
(1) preparation process of DOPOMA is:
Agitator is being housed, thermometer, in the there-necked flask of reflux condensing tube, the tetrahydrofuran (THF) of quality such as adding and toluene mixing solutions, DOPO and MALEIC ANHYDRIDE drop into the amount of substance ratio of 1:1.05, stirring heating, temperature begins when being 84 ℃ to occur refluxing, color deepens to become green gradually behind the system stopping reaction 9h, the system color is blackish green behind the continuation reaction 24h, stopped reaction and be cooled to room temperature behind the insulation reaction 24h, in solution, add an amount of dimethylbenzene and constantly stirring, system layering, lower floor is blackish green thick liquid, and the upper strata is faint yellow clarified liq, separates to obtain lower floor's thick liquid, repeatedly wash the back with dimethylbenzene and place dry 48h in 120 ℃ the baking oven, take out and be cooled to the faint yellow crystalline solid of room temperature;
(2) preparation process of phosphorous Synolac is:
In the four-hole boiling flask of 100ml, add behenic acid, tetramethylolmethane, Tetra hydro Phthalic anhydride and dimethylbenzene; Logical nitrogen is opened stirring, slowly heats up; At 30-40min internal heating to 180 ℃; Begin the sound that has oil to spatter in the time of 160 ℃, and backflow phenomenon occurs; System is turbid solution; 170 ℃ of temperature become little glistening yellow clear liquid with afterreaction 20min system; When arriving 180 ℃, system temperature begins to be incubated 40min; The DOPOMA that in batches adds in the 10min after insulation finishes; Slowly be warming up to 200 ℃ of insulation reaction 30min behind reinforced the finishing, slowly be warming up to 210 ℃ again, final insulation reaction temperature is 210-220 ℃; Along with the carrying out of reaction, the system color is deepened gradually, finally becomes orange red; Insulation reaction was measured acid value every half an hour after 2 hours, stops heating, cooling, discharging and can obtain phosphorous Synolac when acid value is the 10mgKOH/g left and right sides;
(3) preparation process of siccative is:
In the 200# solvent oil, add cobalt iso-octoate, manganese iso-octoate, zirconium iso-octoate, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative under the 3500r/mim condition;
(4) preparation process of phosphorous Synolac finishing fire retardant paint is:
Formula ratio solvent, ammonium polyphosphate, trimeric cyanamide, tetramethylolmethane, zinc borate, titanium dioxide, molybdenum sesquioxide are added successively many with carrying out high speed dispersion 30～60min in the dispersion mill, reduce stirring velocity and add phosphorous Synolac redispersion 20～40min, add dimethyl silicone oil, be ground to required fineness with conoidal mill, then many disperse 10～20min in dispersion mill after the adding siccative be uniformly dispersed and namely get product.
Usefulness of the present invention is, at first adopt 9 by molecular designing, 10-dihydro one 9-oxa--10-phospho hetero phenanthrene-10-oxide compound (DOPO) and maleic anhydride (MA) obtain DOPOMA with the molar ratio reaction of 1:1, and come synthetic alkyd resin as raw material, it has introduced the element phosphor with flame retardant properties in macromolecular chain, synthesized the Synolac with flame retardant properties.Be the coating matrix resin with synthetic phosphorous Synolac, be aided with expandable flame retardant system and other auxiliary agent, success is developed and is obtained phosphorous Synolac finishing fire retardant paint, be applied to the application of flammable substrate surfaces such as timber, fiberboard or cardboard, can effectively improve the fire resistance that applies object, win safe escape and the fire extinguishing disaster relief time of disaster affected people under the fire condition, reduce the human, financial, and material resources loss.
Embodiment
The present invention is finished by following technical scheme, DOPO and MA are with the mole synthesis material DOPOMA recently of 1:1, tetramethylolmethane obtains the dibasic alcohol of two functionality through the behenic acid end-blocking, carry out the esterification synthetic alkyd resin with Tetra hydro Phthalic anhydride then, add the DOPOMA polycondensation at last and obtain the phosphor-containing flame-proof Synolac, be matrix resin with synthetic phosphorous Synolac, be aided with the expandable flame retardant system, disperse to obtain phosphorous Synolac finishing fire retardant paint through grinding.
Phosphorous Synolac synthesis route is as follows:
Wherein
R is fatty carbon chain,
Based on the total mass of phosphorous Synolac finishing fire retardant paint, by mass percentage, phosphorous Synolac finishing fire retardant paint prescription is:
Phosphorous Synolac 30% ~ 36%, ammonium polyphosphate 11.5% ~ 15.8%, trimeric cyanamide 9.5% ~ 10.8%, tetramethylolmethane 4.2% ~ 4.8%, zinc borate 2.7% ~ 3.6%, titanium dioxide 4.1% ~ 4.8%, molybdenum sesquioxide 1% ~ 1.2%, dimethyl silicone oil 0.1% ~ 0.12%, siccative 0.9% ~ 1.08%, solvent 30% ~ 36%;
Wherein solvent is made up of 200# solvent oil and pimelinketone, and its weight ratio is 1:1, and the ammonium polyphosphate polymerization degree is 1000.
Based on the total mass of the phosphorous Synolac of preparation, by mass percentage, phosphorous alkyd resin formulation is:
Behenic acid 50.8% ~ 60.5%, tetramethylolmethane 11.6% ~ 17.8%, Tetra hydro Phthalic anhydride 0% ~ 15.5%, DOPOMA9.5% ~ 20.9%, band aqua 5.1% ~ 7%.
Wherein being with aqua is dimethylbenzene.
Based on the total mass of each component of preparation siccative, by mass percentage, prepare consisting of of each component of siccative:
Cobalt iso-octoate 3.60%, manganese iso-octoate 14.83%, zirconium iso-octoate 14.71%, 200# solvent oil 66.57%.
The preparation process of DOPOMA is:
Agitator is being housed, thermometer, in the there-necked flask of reflux condensing tube, the tetrahydrofuran (THF) of quality such as adding and toluene mixing solutions, DOPO and MALEIC ANHYDRIDE drop into the amount of substance ratio of 1:1.05, stirring heating, temperature begins when being 84 ℃ to occur refluxing, color deepens to become green gradually behind the system stopping reaction 9h, the system color is blackish green behind the continuation reaction 24h, stopped reaction and be cooled to room temperature behind the insulation reaction 24h, in solution, add an amount of dimethylbenzene and constantly stirring, system layering, lower floor is blackish green thick liquid, and the upper strata is faint yellow clarified liq, separates to obtain lower floor's thick liquid, repeatedly wash the back with dimethylbenzene and place dry 48h in 120 ℃ the baking oven, take out and be cooled to the faint yellow crystalline solid of room temperature;
The preparation process of phosphorous Synolac is:
In the four-hole boiling flask of 100ml, add behenic acid, tetramethylolmethane, Tetra hydro Phthalic anhydride and dimethylbenzene.Logical nitrogen is opened stirring, slowly heats up.(at 30-40min internal heating to 180 ℃).Begin the sound that has oil to spatter in the time of 160 ℃, and backflow phenomenon occurs.System is turbid solution.170 ℃ of temperature become little glistening yellow clear liquid with afterreaction 20min system.When arriving 180 ℃, system temperature begins to be incubated 40min.The DOPOMA that in batches adds in the 10min after insulation finishes.Slowly be warming up to 200 ℃ of insulation reaction 30min behind reinforced the finishing, slowly be warming up to 210 ℃ again, final insulation reaction temperature is 210-220 ℃ (can not be rapidly heated to 220 ℃, to avoid boiling explosion phenomenon).Along with the carrying out of reaction, the system color is deepened gradually, finally becomes orange red.Insulation reaction was measured acid value every half an hour after 2 hours, stops heating, cooling, discharging and can obtain phosphorous Synolac when acid value is the 10mgKOH/g left and right sides.
The preparation process of siccative is:
In the 200# solvent oil, add cobalt iso-octoate, manganese iso-octoate, zirconium iso-octoate, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative under the 3500r/min condition;
The preparation process of phosphorous Synolac finishing fire retardant paint is:
Formula ratio solvent, ammonium polyphosphate, trimeric cyanamide, tetramethylolmethane, zinc borate, titanium dioxide, molybdenum sesquioxide are added successively many with carrying out high speed dispersion 30～60min in the dispersion mill, reduce stirring velocity and add phosphorous Synolac redispersion 20～40min, add dimethyl silicone oil, be ground to required fineness with conoidal mill, then many disperse 10～20min in dispersion mill after the adding siccative be uniformly dispersed and namely get product.
Below be embodiments of the invention, but the present invention is not limited in the following example.
The preparation of embodiment 1. phosphorous Synolac
In the four-hole boiling flask of 100ml, add 28 parts of behenic acids, 7.6 parts of tetramethylolmethanes, 4.8 parts and 3 parts dimethylbenzene of Tetra hydro Phthalic anhydride.Logical nitrogen is opened stirring, slowly heats up.(at 30-40min internal heating to 180 ℃).Begin the sound that has oil to spatter in the time of 160 ℃, and backflow phenomenon occurs.System is turbid solution.170 ℃ of temperature become little glistening yellow clear liquid with afterreaction 20min system.When arriving 180 ℃, system temperature begins to be incubated 40min.The DOPOMA that in batches adds 4.9 parts after insulation finishes in the 10min.Slowly be warming up to 200 ℃ of insulation reaction 30min behind reinforced the finishing, slowly be warming up to 210 ℃ again, final insulation reaction temperature is 210-220 ℃ (can not be rapidly heated to 220 ℃, to avoid boiling explosion phenomenon).Along with the carrying out of reaction, the system color is deepened gradually, finally becomes orange red.Insulation reaction was measured acid value every half an hour after 2 hours, stops heating, cooling, discharging and get the phosphor-containing flame-proof Synolac when acid value is the 10mgKOH/g left and right sides.
The preparation of embodiment 2. siccative
In the 50g200# solvent oil, add 3 parts of cobalt iso-octoates, 11 parts of manganese iso-octoates, 11 parts of zirconium iso-octoates, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative under the 3500r/min condition.
The preparation of embodiment 3. phosphorous Synolac finishing fire retardant paints
14g200# solvent oil, 14g200# pimelinketone, 13g ammonium polyphosphate, 8g trimeric cyanamide, 3g tetramethylolmethane, 2.5g zinc borate, 3.5g titanium dioxide, 1g molybdenum sesquioxide are added successively many with carrying out high speed dispersion 30～60min in the dispersion mill, reduce stirring velocity and add the phosphorous Synolac redispersion of 30g 20～40min, add the 0.1g dimethyl silicone oil, be ground to fineness with conoidal mill and reach below the 90 μ m, then many disperse 10～20min in dispersion mill after adding 0.9g siccative be uniformly dispersed and namely get product.
Warp is to prepared phosphorous Synolac finishing fire retardant paint performance test results such as table 1.
Table 1: phosphorous Synolac finishing fire retardant paint performance index
Claims (6)
1. phosphorous Synolac finishing fire retardant paint, it is characterized in that: based on the total mass of phosphorous Synolac finishing fire retardant paint, by mass percentage, phosphorous Synolac finishing fire retardant paint prescription is:
Phosphorous Synolac 30% ~ 36%, ammonium polyphosphate 11.5% ~ 15.8%, trimeric cyanamide 9.5% ~ 10.8%, tetramethylolmethane 4.2% ~ 4.8%, zinc borate 2.7% ~ 3.6%, titanium dioxide 4.1% ~ 4.8%, molybdenum sesquioxide 1% ~ 1.2%, dimethyl silicone oil 0.1% ~ 0.12%, siccative 0.9% ~ 1.08%, solvent 30% ~ 36%;
Based on the total mass of the phosphorous Synolac of preparation, by mass percentage, phosphorous alkyd resin formulation is:
Behenic acid 50.8% ~ 60.5%, tetramethylolmethane 11.6% ~ 17.8%, Tetra hydro Phthalic anhydride 0% ~ 15.5%, DOPOMA9.5% ~ 20.9%, band aqua 5.1% ~ 7%;
Based on the total mass of each component of preparation siccative, by mass percentage, prepare consisting of of each component of siccative:
Cobalt iso-octoate 3.60%, manganese iso-octoate 14.83%, zirconium iso-octoate 14.71%, 200# solvent oil 66.57%.
2. phosphorous Synolac finishing fire retardant paint according to claim 1 is characterized in that solvent is made up of 200# solvent oil and pimelinketone, and its weight ratio is 1:1, and the ammonium polyphosphate polymerization degree is 1000.
3. phosphorous Synolac finishing fire retardant paint according to claim 1 is characterized in that described DOPOMA is obtained by 9,10 one dihydros, one 9 one oxa-one 10 one phospho hetero phenanthrenes, one 10 monoxide (DOPO) and the maleic anhydride molar ratio reaction with 1:1.
4. phosphorous Synolac finishing fire retardant paint according to claim 1, it is characterized in that being with aqua is dimethylbenzene.
5. phosphorous Synolac finishing fire retardant paint according to claim 1, the content that it is characterized in that tetramethylolmethane is 93.6%.
6. the preparation method of phosphorous Synolac finishing fire retardant paint prepares burden by the described component of claim 1 and proportioning thereof, the steps include:
(1) preparation process of DOPOMA is:
Agitator is being housed, thermometer, in the there-necked flask of reflux condensing tube, the tetrahydrofuran (THF) of quality such as adding and toluene mixing solutions, DOPO and MALEIC ANHYDRIDE drop into the amount of substance ratio of 1:1.05, stirring heating, temperature begins when being 84 ℃ to occur refluxing, color deepens to become green gradually behind the system stopping reaction 9h, the system color is blackish green behind the continuation reaction 24h, stopped reaction and be cooled to room temperature behind the insulation reaction 24h, in solution, add an amount of dimethylbenzene and constantly stirring, system layering, lower floor is blackish green thick liquid, and the upper strata is faint yellow clarified liq, separates to obtain lower floor's thick liquid, repeatedly wash the back with dimethylbenzene and place dry 48h in 120 ℃ the baking oven, take out and be cooled to the faint yellow crystalline solid of room temperature;
(2) preparation process of phosphorous Synolac is:
In the four-hole boiling flask of 100ml, add behenic acid, tetramethylolmethane, Tetra hydro Phthalic anhydride and dimethylbenzene; Logical nitrogen is opened stirring, slowly heats up; At 30-40min internal heating to 180 ℃; Begin the sound that has oil to spatter in the time of 160 ℃, and backflow phenomenon occurs; System is turbid solution; 170 ℃ of temperature become little glistening yellow clear liquid with afterreaction 20min system; When arriving 180 ℃, system temperature begins to be incubated 40min; The DOPOMA that in batches adds in the 10min after insulation finishes; Slowly be warming up to 200 ℃ of insulation reaction 30min behind reinforced the finishing, slowly be warming up to 210 ℃ again, final insulation reaction temperature is 210-220 ℃; Along with the carrying out of reaction, the system color is deepened gradually, finally becomes orange red; Insulation reaction was measured acid value every half an hour after 2 hours, stops heating, cooling, discharging and can obtain phosphorous Synolac when acid value is the 10mgKOH/g left and right sides;
(3) preparation process of siccative is:
In the 200# solvent oil, add cobalt iso-octoate, manganese iso-octoate, zirconium iso-octoate, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative under the 3500r/mim condition;
(4) preparation process of phosphorous Synolac finishing fire retardant paint is:
Formula ratio solvent, ammonium polyphosphate, trimeric cyanamide, tetramethylolmethane, zinc borate, titanium dioxide, molybdenum sesquioxide are added successively many with carrying out high speed dispersion 30～60min in the dispersion mill, reduce stirring velocity and add phosphorous Synolac redispersion 20～40min, add dimethyl silicone oil, be ground to required fineness with conoidal mill, then many disperse 10～20min in dispersion mill after the adding siccative be uniformly dispersed and namely get product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104312394A (en) * | 2014-11-11 | 2015-01-28 | 山东五洲检测有限公司 | Fire-retardant alkyd resin coating and preparation method thereof |
| CN107805447A (en) * | 2017-10-25 | 2018-03-16 | 成都纽兰晶茂商贸有限公司 | The preparation method that a kind of wood furniture is painted with flame-proof antibiotic |
| CN111484802A (en) * | 2020-05-25 | 2020-08-04 | 郑州中岳高新材料有限公司 | Preparation method of low-cost efficient drier |
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| CN102746774A (en) * | 2012-06-28 | 2012-10-24 | 兰州理工大学 | Bromine carbon alkyd resin finishing fireproof paint and its preparation method |
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| US20100181696A1 (en) * | 2008-03-06 | 2010-07-22 | Udo Glauner | Halogen-free flame retardants |
| CN101307171A (en) * | 2008-07-10 | 2008-11-19 | 天津市凯华绝缘材料有限公司 | Phosphorus-containing polyester fire retardant epoxy resin composition |
| CN101386669A (en) * | 2008-10-29 | 2009-03-18 | 华南理工大学 | Reaction-type transparent halogen-free flameproof unsaturated polyester and preparation method thereof |
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| CN104312394A (en) * | 2014-11-11 | 2015-01-28 | 山东五洲检测有限公司 | Fire-retardant alkyd resin coating and preparation method thereof |
| CN107805447A (en) * | 2017-10-25 | 2018-03-16 | 成都纽兰晶茂商贸有限公司 | The preparation method that a kind of wood furniture is painted with flame-proof antibiotic |
| CN111484802A (en) * | 2020-05-25 | 2020-08-04 | 郑州中岳高新材料有限公司 | Preparation method of low-cost efficient drier |
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