阅读说明：本技术 一种超薄防火涂层材料及其制备方法 (Ultrathin fireproof coating material and preparation method thereof ) 是由 不公告发明人 于 2020-05-29 设计创作，主要内容包括：本发明涉及防火涂层材料,具体涉及一种超薄膨胀型防火涂层材料,所述涂层材料包括如下重量份数的组成：改性环氧丙烯酸酯乳液35-50份、微胶囊化多聚磷酸铵23-30份、季戊四醇12-18份、三聚氰胺5-16份、颜填料35-50份、无机纤维5-10份、分散剂3-8份、消泡剂0.1-0.5份。所述涂层材料的有益效果在于(1)有机-无机纳米SiO<Sub>2</Sub>/聚环氧丙烯酸酯复合乳液可显著提升其耐温、耐火性能；(2)本发明使用的微胶囊多聚磷酸铵不仅提高了涂层材料的耐水性能,且其膨胀度保持较高水平；(3)通过配方各组分的协同,制备的涂层材料的阻燃性能、耐热性能和力学性能均有显著提高。(The invention relates to a fireproof coating material, in particular to an ultrathin intumescent fireproof coating material, which comprises the following components in parts by weight: 35-50 parts of modified epoxy acrylate emulsion, 23-30 parts of microencapsulated ammonium polyphosphate, 12-18 parts of pentaerythritol, 5-16 parts of melamine, 35-50 parts of pigment and filler, 5-10 parts of inorganic fiber, 3-8 parts of dispersing agent and 0.1-0.5 part of defoaming agent. The coating material has the beneficial effects that (1) the organic-inorganic nano SiO 2 The temperature resistance and the fire resistance of the composite emulsion of the poly epoxy acrylate can be obviously improved; (2) the microcapsule ammonium polyphosphate used in the invention not only improves the water resistance of the coating material, but also keeps the expansion degree at a higher level; (3) through the synergy of all components in the formula, the flame retardant property, the heat resistance and the mechanical property of the prepared coating material are all obviously improved.)

1. An ultrathin fireproof coating material comprises the following components in parts by weight: 35-50 parts of modified epoxy acrylate emulsion, 23-30 parts of microencapsulated ammonium polyphosphate, 12-18 parts of pentaerythritol, 5-16 parts of melamine, 35-50 parts of pigment and filler, 5-10 parts of inorganic fiber, 3-8 parts of dispersing agent and 0.1-0.5 part of defoaming agent;

the modified epoxy acrylate emulsion is organic-inorganic nano SiO₂Polyepoxy acrylate composite emulsion; the preparation method of the modified acrylic emulsion comprises the following steps: (1) adding certain amount of nano silicon dioxide into ethanol solution of gamma- (methacryloyloxy) propyl trimethoxy silane (KH-570), soaking at 50 deg.C for 24 hr, centrifuging, washing, and drying to obtain modified nano SIO₂(ii) a (2) Adding a certain amount of NaHCO into a reaction kettle₃Sodium dodecyl benzene sulfonate and OP-10 emulsifier are stirred at high speed, the PH value is adjusted to 9-10 by NaOH solution, then mixed monomers are added, and pre-emulsification is carried out for 20-30min, thus obtaining pre-emulsion; (3) taking the pre-emulsion 1/3 prepared in the step (2), quickly stirring, and adding the modified nano SiO obtained in the step (1) into the pre-emulsion₂Heating to 70-75 deg.C, adding a certain amount of waterThe rest pre-emulsion is continuously dripped after the reaction is carried out for 1 to 2 hours, aqueous solution of the initiator is dripped in sequence every 20min, the temperature is raised to 80 to 85 ℃ after the dripping is finished, the reaction is carried out for 3 to 4 hours under the condition of heat preservation, the room temperature is cooled, the pH value is adjusted to 7 to 8, and the nano SiO is obtained after the discharging₂Polyepoxy acrylate composite emulsion; the mixed monomer comprises the following monomers in parts by mass: 30-40 parts of methyl methacrylate, 25-32 parts of butyl acrylate, 12-18 parts of styrene and 23-27 parts of E-44 epoxy resin.

2. The ultra-thin fireproof coating material of claim 1, wherein the microencapsulated ammonium polyphosphate is a microencapsulated ammonium polyphosphate prepared by using melamine-formaldehyde as a capsule material and using expandable graphite doped ammonium polyphosphate as a core material; the preparation method of the microencapsulated ammonium polyphosphate comprises the following steps: (1) mixing ammonium polyphosphate and expandable graphite according to a mass ratio, and adding the mixture into a grinding machine to grind for 3-5h to obtain expandable graphite doped ammonium polyphosphate; (2) at 70 ℃, dissolving melamine in formaldehyde according to the mass ratio, continuing stirring for 20-30min after the melamine is completely dissolved to prepare melamine formaldehyde resin, then adding a certain proportion of expandable graphite doped ammonium polyphosphate, violently stirring, adjusting the pH value to 6, continuously stirring, raising the temperature to 85 ℃, reacting for 1-2h, cooling, carrying out suction filtration, and drying to obtain the microencapsulated ammonium polyphosphate.

3. The ultrathin fireproof coating material of claim 1, wherein the pigment and filler are the following composition in parts by weight: 35-50 parts of titanium dioxide, 1-5 parts of needle calcium carbonate, 35-50 parts of zinc borate and 3-8 parts of expandable graphite; the preparation method of the needle-shaped calcium carbonate comprises the following steps: calcining calcium carbonate raw material at 1000 deg.C for 4 hr, adding into 2O times of water, digesting, precipitating for 7 days to obtain Ca (OH)₂Mixing with silica gel according to the molar ratio of Ca to Si of 1.1 to 1, preparing into slurry with 50 times of water, placing into a reaction kettle, adding a certain amount of cetyl trimethyl ammonium bromide, slowly heating to 230 deg.C, keeping the temperature for a certain time, naturally cooling, taking out the slurry from the reaction kettle, filtering the slurry, and dryingSieving with 800 mesh sieve for 8 hr to obtain needle-like calcium silicate.

4. The ultrathin fireproof coating material of claim 1, wherein the dispersant is a composition of polyamide epichlorohydrin resin and N, N-dimethylaminopropylamine at a mass ratio of 1: 0.2-0.5.

5. The ultrathin fireproof coating material of claim 1, wherein the defoaming agent is a silicone defoaming agent comprising at least one of polydimethylsiloxane, fluorosilicone and ethylene glycol siloxane.

6. The ultra-thin fire-retardant coating material of claim 1, wherein said inorganic fiber is at least one of ceramic fiber, high silica fiber, and alumina fiber.

7. The preparation method of the ultrathin fireproof coating material is characterized by comprising the following steps:

(1) adding the modified epoxy acrylate emulsion, pentaerythritol, a dispersing agent and a defoaming agent into a reaction kettle according to the mass ratio, and stirring at a high speed for dispersing for 20-30min to obtain a premixed emulsion;

(2) sequentially adding the microencapsulated ammonium polyphosphate, the melamine, the pigment filler and the inorganic fiber into a grinding machine according to the proportion, and grinding for 3-5 hours to obtain a mixed flame-retardant system;

(3) and (3) adding the mixed flame-retardant system prepared in the step (2) into the premixed emulsion prepared in the step (1) in batches, raising the temperature to 50-60 ℃, stirring vigorously, keeping reacting for 2-3h to obtain uniform emulsion, adding ammonia water to adjust the pH value to 7-8, cooling, and discharging to obtain the ultrathin fireproof coating material.

Technical Field

The invention belongs to the technical field of refractory materials, and particularly relates to an ultrathin fireproof coating material and a preparation method thereof.

Background

The steel structure building has high strength, good shock resistance, flexible design and convenient construction, thereby having wide application. However, some steel structural materials used at present generally have the defect of poor fire resistance. Especially when the temperature of the fire scene is higher than 600 ℃, the strength and hardness of the steel structure are all lost. Because of the heat resistance problem of the steel structure, serious potential safety hazards are brought to the production and life of people, the steel structure needs to be processed before being used, so that the temperature resistance of the steel structure is improved or the tolerance of the steel structure in case of fire and other sudden situations is improved.

Intumescent coatings are widely used in various areas of daily life and industry. Generally, intumescent coatings are applied to the surface of a substrate to alter the fire characteristics of the surface of the substrate material, thereby retarding the rapid spread of fire. In industry, intumescent coatings are applied to, for example, building components to increase the fire endurance of the component. The expansion type fireproof coating can be made into thin and ultrathin fireproof coatings, is convenient to construct, has good bonding performance with a base material, and is more widely applied. Intumescent fire-retardant coatings are generally composed of an organic resin binder, an intumescent agent, a filler and other auxiliary agents, the intumescent agent being a component containing phosphorus (ammonium polyphosphate) -carbon (pentaerythritol) -nitrogen (melamine), which gasifies and carbonizes when heated. Organic resin binders, which serve to bind the various components together and form an integral part of the substrate, are also critical in fire-retardant coatings. The low temperature resistance of organic resin binders and the thermal effects of burning when heated typically impair the fire-retardant effect of the coating, and the burning process often produces toxic fumes. Therefore, the development of an ultrathin fireproof coating material with good temperature resistance and heat resistance is urgently needed.

Disclosure of Invention

In order to solve the defects in the prior art, the invention provides an ultrathin fireproof coating material, which comprises the following components in parts by weight: 35-50 parts of modified epoxy acrylate emulsion, 23-30 parts of microencapsulated ammonium polyphosphate, 12-18 parts of pentaerythritol, 5-16 parts of melamine, 35-50 parts of pigment and filler, 5-10 parts of inorganic fiber, 3-8 parts of dispersing agent and 0.1-0.5 part of defoaming agent;

the modified epoxy acrylate emulsion is organic-inorganic nano SiO₂Polyepoxy acrylate composite emulsion; the emulsion is applied to the affected partover-p-SiO₂The surface modification of the epoxy acrylate resin is realized, so that the epoxy acrylate resin is successfully grafted into the polyepoxy acrylate to form an organic-inorganic composite emulsion, and the temperature resistance and the fire resistance are obviously improved;

the preparation method of the modified acrylic emulsion comprises the following steps: (1) adding certain amount of nano silicon dioxide into ethanol solution of gamma- (methacryloyloxy) propyl trimethoxy silane (KH-570), soaking at 50 deg.C for 24 hr, centrifuging, washing, and drying to obtain modified nano SIO₂(ii) a (2) Adding a certain amount of NaHCO into a reaction kettle₃Sodium dodecyl benzene sulfonate and OP-10 emulsifier are stirred at high speed, the PH value is adjusted to 9-10 by NaOH solution, then mixed monomers are added, and pre-emulsification is carried out for 20-30min, thus obtaining pre-emulsion; (3) taking the pre-emulsion 1/3 prepared in the step (2), quickly stirring, and adding the modified nano SiO obtained in the step (1) into the pre-emulsion₂Heating to 70-75 ℃, adding a certain amount of initiator, reacting for 1-2h, continuously dropwise adding the rest pre-emulsion, dropwise adding aqueous solution of the initiator in sequence every 20min, heating to 80-85 ℃ after dropwise adding, keeping the temperature, reacting for 3-4h, cooling to room temperature, adjusting the pH value to 7-8, and discharging to obtain nano SiO₂Polyepoxy acrylate composite emulsion;

further, the mixed monomer is composed of the following monomers in parts by mass: 30-40 parts of methyl methacrylate, 25-32 parts of butyl acrylate, 12-18 parts of styrene and 23-27 parts of E-44 epoxy resin;

the microencapsulated ammonium polyphosphate is prepared by taking melamine-formaldehyde as a capsule material and taking expandable graphite doped ammonium polyphosphate as a core material; the microencapsulated ammonium polyphosphate improves the water resistance of the microencapsulated ammonium polyphosphate, and solves the problem of reduction of the expansion degree of the ammonium polyphosphate after microencapsulation by doping expandable graphite; the preparation method of the microencapsulated ammonium polyphosphate comprises the following steps: (1) mixing ammonium polyphosphate and expandable graphite according to a mass ratio, and adding the mixture into a grinding machine to grind for 3-5h to obtain expandable graphite doped ammonium polyphosphate; (2) at 70 ℃, dissolving melamine in formaldehyde according to the mass ratio, continuing stirring for 20-30min after the melamine is completely dissolved to prepare melamine formaldehyde resin, then adding a certain proportion of expandable graphite doped ammonium polyphosphate, violently stirring, adjusting the pH value to 6, continuously stirring, raising the temperature to 85 ℃, reacting for 1-2h, cooling, carrying out suction filtration, and drying to obtain the microencapsulated ammonium polyphosphate.

The pigment and filler is a composition with the following parts by weight: 35-50 parts of titanium dioxide, 1-5 parts of needle calcium carbonate, 35-50 parts of zinc borate and 3-8 parts of expandable graphite; the taibai powder mainly plays roles in adjusting color and resisting flame, the zinc borate is a flame-retardant reinforcing agent, a small amount of needle-shaped calcium carbonate is coated on the surface of the filler, so that the heat insulation effect of the filler can be obviously improved, and the expansion multiple of the coating material is further improved by filling expandable graphite;

the preparation method of the needle-shaped calcium carbonate comprises the following steps: calcining calcium carbonate raw material at 1000 deg.C for 4 hr, adding into 2O times of water, digesting, precipitating for 7 days to obtain Ca (OH)₂Mixing the calcium silicate with silica gel according to the molar ratio of Ca to Si of 1.1 to 1, preparing slurry by using water with the mass of 50 times, putting the slurry into a reaction kettle, adding a certain amount of hexadecyl trimethyl ammonium bromide, slowly heating to 230 ℃, preserving the temperature for a certain time, naturally cooling, taking the slurry out of the reaction kettle, filtering the slurry, drying for 8 hours, and screening by using a 800-mesh screen to obtain the needle-shaped calcium silicate.

The dispersant is a composition of polyamide epichlorohydrin resin and N, N-dimethylaminopropylamine, and the mass ratio of the polyamide epichlorohydrin resin to the N, N-dimethylaminopropylamine is 1: 0.2-0.5; the composition can effectively improve the wetting effect of the surface of the pigment and filler, reduce agglomeration and improve the dispersion efficiency of the pigment and filler;

the defoaming agent is an organic silicon defoaming agent and comprises at least one of polydimethylsiloxane, fluorosilicone and ethylene glycol siloxane.

The inorganic fiber is at least one of ceramic fiber, high silica fiber and alumina fiber;

the preparation method of the ultrathin fireproof coating material specifically comprises the following steps:

(1) adding the modified epoxy acrylate emulsion, pentaerythritol, a dispersing agent and a defoaming agent into a reaction kettle according to the mass ratio, and stirring at a high speed for dispersing for 20-30min to obtain a premixed emulsion;

(2) sequentially adding the microencapsulated ammonium polyphosphate, the melamine, the pigment filler and the inorganic fiber into a grinding machine according to the proportion, and grinding for 3-5 hours to obtain a mixed flame-retardant system;

(3) and (3) adding the mixed flame-retardant system prepared in the step (2) into the premixed emulsion prepared in the step (1) in batches, raising the temperature to 50-60 ℃, stirring vigorously, keeping reacting for 2-3h to obtain uniform emulsion, adding ammonia water to adjust the pH value to 7-8, cooling, and discharging to obtain the ultrathin fireproof coating material.

The invention has the beneficial effects that: (1) organic-inorganic nano SiO₂The temperature resistance and the fire resistance of the composite emulsion of the poly epoxy acrylate can be obviously improved; (2) the microcapsule ammonium polyphosphate used in the invention not only improves the water resistance of the coating material, but also keeps the expansion degree at a higher level; (3) through the synergy of all components in the formula, the flame retardant property, the heat resistance and the mechanical property of the prepared coating material are all obviously improved.

Detailed Description

The present invention will now be described in detail by way of examples, which are provided solely for the purpose of illustrating the principles and features of the present invention, and are not intended to limit the scope of the invention.