CN102277030A - Efficient environment-friendly flame retardant for flame retardance of coating and preparation method thereof - Google Patents
Efficient environment-friendly flame retardant for flame retardance of coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an efficient environment-friendly flame retardant for flame retardance of a coating and a preparation method thereof. The novel flame retardant is prepared by combining tea saponin serving as an air source and an acid source and a carbon source in a certain ratio, and a coupling agent, a dispersing agent and the like are added into alkyd resin vernix serving as a base stock to prepare an efficient flame retardant coating. On the basis of the solid content of the coating, the coating comprises the following components in percentage by weight: 40 to 60 percent of alkyd resin vernix, 25 to 35 percent of ammonium polyphosphate, 12 to 18 percent of pentaerythritol, 2 to 5 percent of tea saponin, 1 to 3 percent of silane coupling agent and 1 to 3 percent of organic bentonite. The preparation method comprises the following steps of: mixing the tea saponin, the ammonium polyphosphate and the pentaerythritol in a ratio, grinding fully to form superfine powder, adding into the alkyd resin vernix in a certain ratio, stirring and mixing fully and uniformly, adding the silane coupling agent, and stirring with the organic bentonite in a high-speed shear stirrer fully and dispersing uniformly to obtain the finished product. The efficient environment-friendly flame retardant does not contain a halogen flame retardant, and has the advantages of low volatility, high flame retardant property, high finishing performance, high efficiency, environment friendliness.
Description
Technical field
The present invention relates to a kind of fire-retardant novel environment-friendly fire retardant of coating that can be used for, specifically be as the trimeric cyanamide in the source of the gas replacement conventional expanded type fire retardant with tea saponin, the novel environment friendly flame retardant that can be used for anti-flaming dope with acid source and the composite preparation in charcoal source can obtain to have good flame retardant effect and eco-friendly anti-flaming dope.
Technical background
Anti-flaming dope be most widely used in the modern project, suitability is the strongest, construction material of construction the most easily, is bringing into play enormous function aspect the building safety ensureing.Along with the raising that people live and sample, people favor more to material of construction such as wooden structures, steel construction.And anti-flaming dope has the covering with paint beauty function on the one hand to above-mentioned materials, and when presence of fire or when being subjected to high temperature action, anti-flaming dope has good protective action to timber, steel construction, is good anti-flaming thermal-insulation material of construction on the other hand.In addition, along with the enhancing of global environmental protection consciousness, the safety requirements cry that coating is used grow to even greater heights, developed country has begun to develop the novel flame-retardant coating that helps environment protection, high-efficiency low-toxicity.Simultaneously, for adapting to the new environment that whole coating industry strides forward to " five E " direction, promptly improve film quality (Excellence of finish), convenient construction (Easy of application), save resource (E-conomics), save the energy (Energy saving) and conform (Ecology), anti-flaming dope develops the environmental compatibility of more and more paying attention to improving anti-flaming dope, the flame retardant properties of improving coating, makes anti-flaming dope reach high-efficiency low-toxicity.
Expansion type flame-retarding coating is to be base-material with the high molecular polymer, and adds flame retardance elements such as whipping agent, carbonifying catalyst, carbonized agent.Its coating is under the high-temperature heating situation, and top coat meeting fusion, foaming, protuberance form fine and close carbonaceous insulated foam coating, and discharge non-flammable gases.The expanded foamed process of expansion coating is the process of a volumetric expansion, heat absorption, consumes a large amount of heat, helps reducing system temperature, so its anti-flaming thermal-insulation effect is remarkable.And traditional anti-flaming dope forms glaze shape protective layer when high-temperature heating, but the glaze shape protective layer thermal conductivity that generates is often bigger, and effect of heat insulation is poor; in order to reach certain flame retardant effect, often need thicker coating, thereby the unit surface consumption is big; the use cost height, decorative effect is poor.And the expansion type flame-retarding paint coatings is generally thinner, helps satisfying the decoration requirement.Therefore, consider from flame retardant effect, decorative effect and Financial cost angle, expansion type flame-retarding application of paints more extensive, its flame retardant effect is better, is the development trend of anti-flaming dope in season.
P-C-N is that product at home and abroad is most widely used in the expansion type flame-retarding coating at present, but such expansion type flame-retarding coating,, mainly there are problems such as water tolerance, humidity resistance problem and flame retardant rating are lower.Anti-flaming dope also may produce the danger of hypertoxic prussic acid in combustion processes in addition.For the consideration to environment protection and Secure Application, the research of fire retardant material mainly concentrates on the aspects such as toxicity that improve flame retarding efficiency, reduce fire retardant.
Tea saponin is a kind of pentacyclic triterpene material that extracts from tea-seed pancake, and the by product as oil tea processing easily is degraded into non-toxic substance, environmentally safe under natural environmental condition.Tea saponin has stronger foaming effect, and the whipping agent as spongy rubber, frothextinguisher can be used for gas concrete production and fiberboard production, can partially or completely replace traditional whipping agent in expansion type flame retardant.Decision in " national camellia oleiferaindustry development program (2009-2020) ": the year two thousand twenty China oil tea cultivated area will reach 6,631 ten thousand mu.China's oil tea area has 4,500 ten thousand mu approximately at present, about 1,000,000 tons of tea seed annual production, and the remaining cake of camellia oleifera seeds in annual oil expression back has 500,000 tons approximately, and wherein the tea saponin amount is up to ten thousand tons of 5-10.
(Shanghai coating such as Xu Qianwei, 2008,46 (1): be flame-retardant system 8-11) with ammonium polyphosphate (APP), trimeric cyanamide (MEL), dipentaerythritol (DPER), self-crosslinking silicopropyl emulsion is that the expansion type flame-retarding coating of matrix resin is research object, the research Cellmic C 121 is to the influence of anti-flaming dope flame retardant properties, the result shows: when the Cellmic C 121 consumption is 1.5%, best to the foaming effect of anti-flaming dope; (coatings industry such as Huo Haifeng, 2008,38 (3): 27-29) adopt ammonium molybdate (AM), expansible black lead (EG) and AM/EG that melamine polyphosphate (MPP)/trimeric cyanamide (MEL)/ultrathin anti-flaming dope of tetramethylolmethane (PER) is carried out modification, the preparation modified paint.The result shows: the carbon residue amount and the fire resistance period of the anti-flaming dope of AM/EG modification all are significantly improved.
Wang Qingwen etc. (CN 101117510A) have invented a kind of modified amino resin expansion type anti-flaming dope, the material anti-flaming dope of its invention is compared with three layers of wooden gummed laminin plate, its anti-burning time has improved 9 times, the total heat burst size has reduced by 42.5%, and the heat release rate peak value has also reduced by 11.5%; Tang Wanxiong etc. (CN 10121280142A) have invented a kind of environment-friendly aqueous nanometer anti-flaming dope, adopt nano-magnesium hydrate fire retardant that phosphorous, nitrogen organic intercalated layered silicate nano-meter flame retardants and polymkeric substance the comprise flame-retardant system as coating respectively, coating has fabulous flame retardant effect.
Summary of the invention
The purpose of this invention is to provide the expansion environmental protection sex flame retardant that is used for anti-flaming dope, the problem that solves is that disclosing a kind of is the novel intumescent fire-retardant coating material and preparation method thereof of source of the gas with the tea saponin, to overcome the danger that may produce hypertoxic prussic acid when traditional trimeric cyanamide burns as expansion type flame-retarding coating source of the gas.Improve the covering with paint and the film forming properties of product simultaneously.
The composition that the present invention is used for the fire retardant of expansion type flame-retarding coating is that the mass ratio of ammonium polyphosphate, tetramethylolmethane, tea saponin is 10-40: 10-20: 1-5.
According to invention, the mass ratio of preferred ammonium polyphosphate, tetramethylolmethane, tea saponin is 25-35: 12-18: 2-5.
Ammonium polyphosphate as acid source, tetramethylolmethane as carbon source, tea saponin as source of the gas.
Among the present invention, tea saponin is the tea saponin class mixture that extracts in the cake of camellia oleifera seeds, and tea saponin content is generally 60%, has finished industrial product to sell.
The content of tea saponin in novel intumescent fire-retardant coating material is too high or too low all can to influence the cooperative flame retardant effect, and when content was too low, charcoal layer expansion effect was bad; When content was too high, the charcoal layer was of low quality, to the barriering effect ability drop of heat and fire.
The flame-retardant system consumption very little, the flame retardant properties of coating does not reach the fire-retardant requirement of anti-flaming dope Application Areas, the flame-retardant system consumption is too high, the stability in storage of coating, covering with paint, lacquer, colour wash, etc. film performance will decline to a great extent; Also influence the flame retardant effect of anti-flaming dope on the other hand.
The novel intumescent fire-retardant coating material that the present invention adopts above-mentioned coating fire retardant formulation to form, wherein to account for the mass percent of solids coatings be 35-55% to expanding fire retardant, preferred 40-41%.The quality percentage composition of paint in expansion type flame-retarding coating is 40-60%, can select alkyd varnish for use, and for example the C-101 alkyd varnish is medium oil alkyd varnish.
Stablizer adopts industrial silane coupling agent commonly used, and the coupling agent addition is the 1-3% of expansion type flame-retarding coating, preferred 1-2%.
Dispersion agent adopts the organobentonite of palmityl trimethyl ammonium chloride modification.The dispersion agent addition is the 1-3% of expansion type flame-retarding coating, preferred 1.5-2.5%.
Described novel intumescent fire-retardant coating material is preparation like this: after tea saponin, ammonium polyphosphate, tetramethylolmethane are mixed according to the above ratio, after fully grinding reaches superfine powder, add in the alkyd varnish by a certain percentage, after fully mixing, add silane coupling agent and organobentonite, evenly obtain finished product in the abundant dispersed with stirring of high speed shear agitator.
Tea saponin and acid source and carbon source are composite, under the situation of being heated, have good expansion character and carbon-forming performance.Tea saponin is substituted the source of the gas trimeric cyanamide of present expansibility flame-proof system, not only can reduce cost, and improving flame-retardant system and Synolac interface compatibility, improve the heat-insulating flame-retardant aspect and have significant effect, the danger that may produce prussic acid when particularly eliminating trimeric cyanamide and being heated.
The present invention adopts economy, workable method, and phosphor nitrogen combustion inhibitor and the composite preparation novel flame-retardant of tea saponin system are used for expansion type flame-retarding coating.The flame-retardant system that is used for novel intumescent fire-retardant coating material that the present invention is prepared, have good cooperative flame retardant effect between phosphor nitrogen combustion inhibitor and tea saponin, compare, have cost and reduce with traditional trimeric cyanamide expansion type flame retardant, good flame retardation effect is covered with paint, lacquer, colour wash, etc. advantages such as film performance is good, high-efficiency environment friendly.
Embodiment
Following mask body is elaborated to novel intumescent fire-retardant coating material provided by the invention and preparation method thereof in conjunction with example.But the present invention never is confined to these embodiment.
Embodiment 1 (Comparative Examples)
With the 100g Synolac, under mechanical stirring, add 1.5g silane coupling agent level 2.0g organic bentonite, under high shear rate, mix, get final product phthalic resin coating.
Embodiment 2 (trimeric cyanamide Comparative Examples)
Ammonium polyphosphate 42g, tetramethylolmethane 25g, trimeric cyanamide 5g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product expansion type flame-retarding coating.
Embodiment 3
Ammonium polyphosphate 27g, tetramethylolmethane 12g, tea saponin 9g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 4
Ammonium polyphosphate 36g, tetramethylolmethane 28g, tea saponin 8g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 5
Ammonium polyphosphate 32g, tetramethylolmethane 36g, tea saponin 4g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 6
Ammonium polyphosphate 43g, tetramethylolmethane 25g, tea saponin 4g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 7
Ammonium polyphosphate 35g, tetramethylolmethane 29g, tea saponin 9g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 8
Ammonium polyphosphate 54g, tetramethylolmethane 14g, tea saponin 4g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 9
Ammonium polyphosphate 43g, tetramethylolmethane 20g, tea saponin 9g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 10
Ammonium polyphosphate 40g, tetramethylolmethane 27g, tea saponin 5g are re-dubbed BACN, through grinding 1-2h, mix, join in the 100g alkyd varnish, stir 0.5-1h, add 2.1g silane coupling agent level 2.8g organic bentonite, under high shear rate, mix, get final product novel intumescent fire-retardant coating material.
Embodiment 11
A kind of phthalic resin coating and the 9 kind intumescent fire-retardant coating materials prepared to the foregoing description carry out flame retardant properties test (oxygen index, smoke density, fire resistance period).The oxygen index test is undertaken by ISO4589-1984, and batten is of a size of 130.0mm * 6.5mm * 3.0mm.Batten size 40.0mm * 40.0mm * 3.0mm is carried out in the smoke density test by ASTME662-95.Fire resistance period is with reference to GB15442.2-1995.Classification of finishing fire retardant paint flame retardant properties and test method one big panel method adopt self-designed vertical combustion method to make brief appraisal.Detailed process is as follows: will place the iron ring that test panel uses and be fixed on the iron stand, the vertical range of iron ring and alcohol blast burner mouth is 7cm, and test panel is put on the iron ring, picks up counting to endpoint detection then.When detecting, carry on the back fiery face charing during the plank burning, the crack appears, be decided to be the anti-combustion time (min).Enforcement 9 and embodiment 1 (contrast) are according to GB/T 6739-1996 test hardness of paint film, according to GB/1731-93 test paint film flexibility, according to GB/T 9286-1998 test paint film adhesion, according to GB/T 1732-93 test paint film shock resistance.
Fire-retardant and the smoke suppressing of table 1 sample
The interpolation expansion type flame retardant can significantly improve the flame retardant properties of coating, replaces the expansion type flame retardant anti-flaming dope flame retardant effect of melamine preparation better with tea saponin, and smoke suppressing improves.Wherein fire-retardant embodiment 8 has the highest oxygen index and long fire resistance period, and flame retardant properties is best.But smoke density grade height, embodiment 9 smoke density grades are minimum, and smoke suppressing is best, has higher oxygen index and long fire resistance period simultaneously.Embodiment 6 has the longest fire resistance period and high oxygen index, and flame retardant properties is good, and the smoke density grade is lower than the smoke density of embodiment 8.Hardness of paint film, sticking power and shock resistance all are better than embodiment 1 among the embodiment 9, and be loss of adhesion, totally covers with paint, lacquer, colour wash, etc. performance and improve.
Claims (7)
1. the expanding fire retardant of a novel intumescent fire-retardant coating material, it is characterized in that ammonium polyphosphate, tetramethylolmethane, tea saponin are by following mass ratio 10-40: 10-20: 1-5 forms.
2. expanding fire retardant according to claim 1, it is characterized in that ammonium polyphosphate, tetramethylolmethane, tea saponin are by following mass ratio 25-35: 12-18: 2-5 forms.
3. expanding fire retardant according to claim 1 and 2 is characterized in that ammonium polyphosphate is the molten ammonium phosphate polymkeric substance of high-polymerization degree, shipwreck, and the polymerization degree is 700-1500.
4. one kind is the expansion type flame-retarding coating of basic coating with the alkyd varnish, the quality percentage composition that it is characterized in that expansion type flame-retarding coating is: alkyd varnish 40-60%, the described expansion type flame retardant 35-55% of one of claim 1-3, stablizer 1-3%; Dispersion agent 1-3%.
5. expansion type flame-retarding coating according to claim 4 is characterized in that stablizer is a silane coupling agent, and massfraction is 1-2%.
6. intumescent fire-retardant coating material according to claim 4 is characterized in that dispersion agent is the organobentonite of palmityl trimethyl ammonium chloride modification, and massfraction is 1.5-2.5%.
7. according to the described expansion type flame-retarding coating of one of claim 4--6, the quality percentage composition that it is characterized in that expanding fire retardant is 40-41%.
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Cited By (6)
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| CN103992440A (en) * | 2014-05-08 | 2014-08-20 | 武汉纺织大学 | Preparation method of novel waste cooking oil based unsaturated polyester resin |
| CN104877174A (en) * | 2015-05-13 | 2015-09-02 | 沈阳化工大学 | Preparation method of environment-friendly flame retardant flame-retardant rubber |
| CN106084665A (en) * | 2016-06-29 | 2016-11-09 | 郭舒洋 | A kind of preparation method of expansion type flame retardant |
| CN107163655A (en) * | 2017-06-26 | 2017-09-15 | 东莞市道尔新材料科技有限公司 | DOPO base expanding fire retardants |
| CN109054121A (en) * | 2018-08-09 | 2018-12-21 | 安徽中宏线缆有限公司 | A kind of power cable oil resistant high fire-retardance native rubber composite material |
| CN114230861A (en) * | 2021-11-19 | 2022-03-25 | 安徽沸点新材料有限公司 | Flame-retardant silane coupling agent and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992440A (en) * | 2014-05-08 | 2014-08-20 | 武汉纺织大学 | Preparation method of novel waste cooking oil based unsaturated polyester resin |
| CN103992440B (en) * | 2014-05-08 | 2017-01-11 | 武汉纺织大学 | Preparation method of waste cooking oil based unsaturated polyester resin |
| CN104877174A (en) * | 2015-05-13 | 2015-09-02 | 沈阳化工大学 | Preparation method of environment-friendly flame retardant flame-retardant rubber |
| CN104877174B (en) * | 2015-05-13 | 2018-01-05 | 沈阳化工大学 | A kind of preparation method of environment friendly flame retardant flame retardant rubber |
| CN106084665A (en) * | 2016-06-29 | 2016-11-09 | 郭舒洋 | A kind of preparation method of expansion type flame retardant |
| CN106084665B (en) * | 2016-06-29 | 2018-05-08 | 绍兴金阳纺织有限公司 | A kind of preparation method of expansion type flame retardant |
| CN107163655A (en) * | 2017-06-26 | 2017-09-15 | 东莞市道尔新材料科技有限公司 | DOPO base expanding fire retardants |
| CN107163655B (en) * | 2017-06-26 | 2019-08-13 | 东莞市道尔新材料科技有限公司 | DOPO base expanding fire retardant |
| CN109054121A (en) * | 2018-08-09 | 2018-12-21 | 安徽中宏线缆有限公司 | A kind of power cable oil resistant high fire-retardance native rubber composite material |
| CN114230861A (en) * | 2021-11-19 | 2022-03-25 | 安徽沸点新材料有限公司 | Flame-retardant silane coupling agent and preparation method thereof |
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Application publication date: 20111214 |