CN103275605B - 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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- CN103275605B CN103275605B CN201310259043.7A CN201310259043A CN103275605B CN 103275605 B CN103275605 B CN 103275605B CN 201310259043 A CN201310259043 A CN 201310259043A CN 103275605 B CN103275605 B CN 103275605B
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N O=C(C=C1)OC1=O Chemical compound O=C(C=C1)OC1=O FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- RHVODNOOIKYOGT-UHFFFAOYSA-N O=C(CC1P2(Oc3ccccc3-c3c2cccc3)=O)OC1=O Chemical compound O=C(CC1P2(Oc3ccccc3-c3c2cccc3)=O)OC1=O RHVODNOOIKYOGT-UHFFFAOYSA-N 0.000 description 1
- VBQRUYIOTHNGOP-UHFFFAOYSA-N O=P1Oc(cccc2)c2-c2c1cccc2 Chemical compound O=P1Oc(cccc2)c2-c2c1cccc2 VBQRUYIOTHNGOP-UHFFFAOYSA-N 0.000 description 1
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- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Paints Or Removers (AREA)
- Fireproofing Substances (AREA)
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 a kind of new coating kind integrating decoration and fire prevention.When it is coated on flammable substrate surface, certain decoration function can be played at ordinary times, once fire occurs, then there is prevention fire spreading, the object reach protection base material, making 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, consist of the following composition by massfraction: bromine carbon Synolac finishing fire retardant paint formula 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%; Based on the total mass preparing 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 preparing each component of 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 object of this invention is to provide onephosphorous 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 formula 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%, water entrainer 5.1% ~ 7%;
Based on the total mass preparing each component of siccative, by mass percentage, consisting of of each component of siccative is prepared:
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, tetrahydrofuran (THF) and the toluene mixed solution of quality such as to add, DOPO and MALEIC ANHYDRIDE drop into the amount of substance of 1:1.05 ratio, stirring heating, temperature starts when being 84 DEG C to occur backflow, after stable system reaction 9h, color deepens to become green gradually, after continuation reaction 24h, system color is blackish green, stopped reaction after insulation reaction 24h is also cooled to room temperature, in solution, add appropriate dimethylbenzene and constantly stir, system layering, lower floor is blackish green thick liquid, upper strata is faint yellow clarified liq, separation obtains lower floor's thick liquid, dry 48h in the baking oven of rear placement 120 DEG C is repeatedly washed with dimethylbenzene, taking-up is cooled to room temperature pale yellow crystals solid,
(2) preparation process of phosphorous Synolac is:
Behenic acid is added, tetramethylolmethane, Tetra hydro Phthalic anhydride and dimethylbenzene in the four-hole boiling flask of 100ml; Logical nitrogen, opens stirring, slowly heats up; 180 DEG C are heated in 30-40min; Start the sound having oil to spatter when 160 DEG C, and occur backflow phenomenon; System is turbid solution; Temperature 170 DEG C later reaction 20min system becomes micro-glistening yellow clear liquid; Start to be incubated 40min when system temperature arrives 180 DEG C; Insulation terminates the DOPOMA in batches added in rear 10min; Slowly be warming up to 200 DEG C of insulation reaction 30min after reinforced, be more slowly warming up to 210 DEG C, final insulation reaction temperature is 210-220 DEG C; Along with the carrying out of reaction, system color is deepened gradually, finally becomes orange red; Insulation reaction carried out measurement acid value every half an hour after 2 hours, stopped heating, cooling, discharging can obtain phosphorous Synolac when acid value is about 10mgKOH/g;
(3) preparation process of siccative is:
In 200# solvent oil, add cobalt iso-octoate, manganese iso-octoate, zirconium iso-octoate, under 3500r/min condition, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative;
(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 in multiplex dispersion mill successively and carries out high speed dispersion 30 ~ 60min, reduce stirring velocity and add phosphorous Synolac redispersion 20 ~ 40min, add dimethyl silicone oil, be ground to required fineness with conoidal mill, add siccative after then disperseing 10 ~ 20min in multiplex dispersion mill and be uniformly dispersed and obtain product.
Usefulness of the present invention is, first 9 are adopted 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 carry out synthetic alkyd resin as raw material, it introduces the element phosphor with flame retardant properties in macromolecular chain, has synthesized the Synolac with flame retardant properties.With the phosphorous Synolac of synthesis for coating matrix resin, be aided with Intumescent Retardant System and other auxiliary agent, success is developed and is obtained phosphorous Synolac finishing fire retardant paint, be applied to the application of the flammable substrate surfaces such as timber, fiberboard or cardboard, effectively can improve the fire resistance of coating of objects, win safe escape and the fire extinguishing disaster relief time of disaster affected people under Fire Conditions, reduce human, financial, and material resources loss.
Embodiment
The present invention is completed by following technical scheme, DOPO and MA carrys out synthesis material DOPOMA with the mol ratio of 1:1, tetramethylolmethane obtains the dibasic alcohol of two functionality through behenic acid end-blocking, then esterification synthetic alkyd resin is carried out with Tetra hydro Phthalic anhydride, finally add DOPOMA polycondensation and obtain phosphor-containing flame-proof Synolac, to synthesize phosphorous Synolac for matrix resin, be aided with Intumescent Retardant System, phosphorous Synolac finishing fire retardant paint can be obtained through grinding distribution.
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 formula 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%, water entrainer 5.1% ~ 7%.
Wherein water entrainer is dimethylbenzene.
Based on the total mass preparing each component of siccative, by mass percentage, consisting of of each component of siccative is prepared:
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, tetrahydrofuran (THF) and the toluene mixed solution of quality such as to add, DOPO and MALEIC ANHYDRIDE drop into the amount of substance of 1:1.05 ratio, stirring heating, temperature starts when being 84 DEG C to occur backflow, after stable system reaction 9h, color deepens to become green gradually, after continuation reaction 24h, system color is blackish green, stopped reaction after insulation reaction 24h is also cooled to room temperature, in solution, add appropriate dimethylbenzene and constantly stir, system layering, lower floor is blackish green thick liquid, upper strata is faint yellow clarified liq, separation obtains lower floor's thick liquid, dry 48h in the baking oven of rear placement 120 DEG C is repeatedly washed with dimethylbenzene, taking-up is cooled to room temperature pale yellow crystals solid,
The preparation process of phosphorous Synolac is:
Behenic acid is added, tetramethylolmethane, Tetra hydro Phthalic anhydride and dimethylbenzene in the four-hole boiling flask of 100ml.Logical nitrogen, opens stirring, slowly heats up.(in 30-40min, being heated to 180 DEG C).Start the sound having oil to spatter when 160 DEG C, and occur backflow phenomenon.System is turbid solution.Temperature 170 DEG C later reaction 20min system becomes micro-glistening yellow clear liquid.Start to be incubated 40min when system temperature arrives 180 DEG C.Insulation terminates the DOPOMA in batches added in rear 10min.Slowly be warming up to 200 DEG C of insulation reaction 30min after reinforced, be more slowly warming up to 210 DEG C, final insulation reaction temperature is 210-220 DEG C (can not be rapidly heated to 220 DEG C, to avoid boiling explosion phenomenon).Along with the carrying out of reaction, system color is deepened gradually, finally becomes orange red.Insulation reaction carried out measurement acid value every half an hour after 2 hours, stopped heating, cooling, discharging can obtain phosphorous Synolac when acid value is about 10mgKOH/g.
The preparation process of siccative is:
In 200# solvent oil, add cobalt iso-octoate, manganese iso-octoate, zirconium iso-octoate, under 3500r/min condition, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative;
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 in multiplex dispersion mill successively and carries out high speed dispersion 30 ~ 60min, reduce stirring velocity and add phosphorous Synolac redispersion 20 ~ 40min, add dimethyl silicone oil, be ground to required fineness with conoidal mill, add siccative after then disperseing 10 ~ 20min in multiplex dispersion mill and be uniformly dispersed and obtain product.
Be below embodiments of the invention, but the present invention is not limited in the following example.
The preparation of the phosphorous Synolac of embodiment 1.
Behenic acid 28 parts is added, tetramethylolmethane 7.6 parts, Tetra hydro Phthalic anhydride 4.8 parts and 3 parts of dimethylbenzene in the four-hole boiling flask of 100ml.Logical nitrogen, opens stirring, slowly heats up.(in 30-40min, being heated to 180 DEG C).Start the sound having oil to spatter when 160 DEG C, and occur backflow phenomenon.System is turbid solution.Temperature 170 DEG C later reaction 20min system becomes micro-glistening yellow clear liquid.Start to be incubated 40min when system temperature arrives 180 DEG C.Insulation terminates the DOPOMA in batches adding 4.9 parts in rear 10min.Slowly be warming up to 200 DEG C of insulation reaction 30min after reinforced, be more slowly warming up to 210 DEG C, final insulation reaction temperature is 210-220 DEG C (can not be rapidly heated to 220 DEG C, to avoid boiling explosion phenomenon).Along with the carrying out of reaction, system color is deepened gradually, finally becomes orange red.Insulation reaction carried out measurement acid value every half an hour after 2 hours, stopped heating, cooling, discharging to obtain phosphor-containing flame-proof Synolac when acid value is about 10mgKOH/g.
The preparation of embodiment 2. siccative
In 50g200# solvent oil, add 3 parts of cobalt iso-octoates, 11 parts of manganese iso-octoates, 11 parts of zirconium iso-octoates, under 3500r/min condition, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative.
The preparation of the phosphorous Synolac finishing fire retardant paint of embodiment 3.
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 in multiplex dispersion mill successively and carries out high speed dispersion 30 ~ 60min, reduce stirring velocity and add the phosphorous Synolac redispersion of 30g 20 ~ 40min, add 0.1g dimethyl silicone oil, be ground to fineness with conoidal mill and reach less than 90 μm, add 0.9g siccative after then disperseing 10 ~ 20min in multiplex dispersion mill and be uniformly dispersed and obtain product.
Through to prepared phosphorous Synolac finishing fire retardant paint performance test results as table 1.
table 1: phosphorous Synolac finishing fire retardant paint performance index
Claims (4)
1. phosphorous Synolac finishing fire retardant paint, is characterized in that: based on the total mass of phosphorous Synolac finishing fire retardant paint, by mass percentage, and phosphorous Synolac finishing fire retardant paint formula 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%, water entrainer 5.1% ~ 7%;
Based on the total mass preparing each component of siccative, by mass percentage, consisting of of each component of siccative is prepared:
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 said components 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, tetrahydrofuran (THF) and the toluene mixed solution of quality such as to add, DOPO and MALEIC ANHYDRIDE drop into the amount of substance of 1:1.05 ratio, stirring heating, temperature starts when being 84 DEG C to occur backflow, after stable system reaction 9h, color deepens to become green gradually, after continuation reaction 24h, system color is blackish green, stopped reaction after insulation reaction 24h is also cooled to room temperature, in solution, add appropriate dimethylbenzene and constantly stir, system layering, lower floor is blackish green thick liquid, upper strata is faint yellow clarified liq, separation obtains lower floor's thick liquid, dry 48h in the baking oven of rear placement 120 DEG C is repeatedly washed with dimethylbenzene, taking-up is cooled to room temperature pale yellow crystals solid,
(2) preparation process of phosphorous Synolac is:
Behenic acid is added, tetramethylolmethane, Tetra hydro Phthalic anhydride and dimethylbenzene in the four-hole boiling flask of 100ml; Logical nitrogen, opens stirring, slowly heats up; 180 DEG C are heated in 30-40min; Start the sound having oil to spatter when 160 DEG C, and occur backflow phenomenon; System is turbid solution; Temperature 170 DEG C later reaction 20min system becomes micro-glistening yellow clear liquid; Start to be incubated 40min when system temperature arrives 180 DEG C; Insulation terminates the DOPOMA in batches added in rear 10min; Slowly be warming up to 200 DEG C of insulation reaction 30min after reinforced, be more slowly warming up to 210 DEG C, final insulation reaction temperature is 210-220 DEG C; Along with the carrying out of reaction, system color is deepened gradually, finally becomes orange red; Insulation reaction carried out measurement acid value every half an hour after 2 hours, stopped heating, cooling, discharging can obtain phosphorous Synolac when acid value is about 10mgKOH/g;
(3) preparation process of siccative is:
In 200# solvent oil, add cobalt iso-octoate, manganese iso-octoate, zirconium iso-octoate, under 3500r/min condition, high speed dispersion 2h can obtain phosphorous Synolac finishing fire retardant paint siccative;
(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 in multiplex dispersion mill successively and carries out high speed dispersion 30 ~ 60min, reduce stirring velocity and add phosphorous Synolac redispersion 20 ~ 40min, add dimethyl silicone oil, be ground to required fineness with conoidal mill, add siccative after then disperseing 10 ~ 20min in multiplex dispersion mill and be uniformly dispersed and obtain product.
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, it is characterized in that described DOPOMA is by 9,10 1 dihydro 1 oxa-s 1 phospho hetero phenanthrene 1 monoxide (DOPO) and maleic anhydride obtain with the molar ratio reaction of 1:1.
4. phosphorous Synolac finishing fire retardant paint according to claim 1, is characterized in that water entrainer is dimethylbenzene.
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| CN104312394B (en) * | 2014-11-11 | 2017-02-01 | 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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| CN101386669B (en) * | 2008-10-29 | 2011-05-18 | 华南理工大学 | Reaction-type transparent halogen-free flameproof unsaturated polyester and preparation method thereof |
| TWI598357B (en) * | 2009-05-19 | 2017-09-11 | 亞比馬利股份有限公司 | Dopo derivative flame retardants |
| CN102746774B (en) * | 2012-06-28 | 2014-07-09 | 兰州理工大学 | Bromine carbon alkyd resin finishing fireproof paint and its preparation method |
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