WO2007140676A1 - Fireproofing powder coating for steel structures and the preparing method thereof - Google Patents

Fireproofing powder coating for steel structures and the preparing method thereof Download PDF

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Publication number
WO2007140676A1
WO2007140676A1 PCT/CN2007/000704 CN2007000704W WO2007140676A1 WO 2007140676 A1 WO2007140676 A1 WO 2007140676A1 CN 2007000704 W CN2007000704 W CN 2007000704W WO 2007140676 A1 WO2007140676 A1 WO 2007140676A1
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Prior art keywords
agent
powder coating
steel structure
coating
structure fireproof
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PCT/CN2007/000704
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French (fr)
Chinese (zh)
Inventor
Dongfang Lu
Cuncai Lu
Bing Zhao
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Xuzhou Zenith Coating Co., Ltd
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Publication of WO2007140676A1 publication Critical patent/WO2007140676A1/en

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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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03—Powdery paints
    • C09D5/032—Powdery paints characterised by a special effect of the produced film, e.g. wrinkle, pearlescence, matt finish
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins

Definitions

  • the invention relates to a steel structure fireproof powder coating and a preparation method thereof, and belongs to the technical field of fireproof coatings. Background technique
  • fire-retardant coatings for steel structures. According to the state of materials, they can be divided into solvent-based, water-soluble and powder-based. According to the fire-proof mechanism, they can be divided into two types: expanded and non-expanded. , thin and ultra-thin.
  • Steel structure fireproof coating is a fireproof coating applied to the surface of steel structures of buildings and structures, which can form a fireproof and heat insulation layer to improve the fire resistance of steel structures. It is the main type of fireproof coatings. In recent years, with the development of the economy and the continuous improvement of coating technology, steel structure fireproof coating products are developing in the direction of ultra-thin, decorative and weather resistance.
  • Powder coatings contain no solvent, have nearly 100% utilization rate, high efficiency, environmental protection, energy saving and economy. It is one of the main directions of future coating development. At present, most research and application products of powder coatings focus on decorative, anti-corrosion, etc. In terms of the literature, there are few literature reports and related patent applications for steel fire retardant coatings.
  • CN1380370A discloses a fireproof powder coating and a production process thereof, and discusses the fireproof powder coating and the preparation method thereof, first pre-dispersing various fireproofing assistants into the resin and then mixing other materials with the processing of the powder coating. The method provides a fireproof coating product. Since many fireproofing agents have low melting point and high activity, these all affect their use in fireproof powder coatings, and also increase the difficulty in research and development of fireproof powder coatings. So far we have not seen successful reports in this regard. Summary of the invention
  • the object of the present invention is to provide a steel structure fireproof powder coating which has ultra-thin coating, excellent fire resistance and thickened expansion foam layer and a preparation method thereof.
  • the invention is realized by the following technical scheme: a steel structure fireproof powder coating, which is characterized in that it is composed of a polyester resin, an epoxy resin, a curing agent, a catalyst, a carbonizing agent, a foaming agent, an expansion aid, and a supplement. Strong agent, smoke suppressant, toughening agent, leveling agent, deaerator, flow agent, pigment and filler are prepared by multiple melt extrusion and extrusion, tableting and milling process.
  • the specific formula of each raw material is as follows (parts by weight) :
  • the epoxy resin is a bisphenol A epoxy resin having an epoxy value of 0.01 to 0.12
  • the polyester resin is a polyester resin for powder coating having an acid value of 68 to 82 mgKOH/g;
  • the curing agent is epoxy low temperature curing.
  • the leveling agent is a leveling agent for epoxy-polyester powder coatings PV88, GLP588, GLP503;
  • the deaerator is a degassing wax for benzoin or powder coating
  • ammonium polyphosphate is n>1000, type II high molecular weight ammonium polyphosphate
  • the smoke suppressing agent is zinc oxide or molybdenum oxide
  • the reinforcing agent is kaolin, attapulgite, rutile titanium dioxide;
  • the toughening agent is polyvinyl butyral, dioctyl ester
  • the flow agent is A1 2 0 3 -C, gas phase SiO 2 .
  • the fireproof coating is prepared by first mixing and dispersing ammonium polyphosphate, pentaerythritol, melamine, melamine pyrophosphate through a 200 mesh sieve and a formula amount of a polyester resin, an epoxy resin, and a leveling agent according to a formula amount. After being added to a screw extruder for extrusion, tableting, and crushing, the crushed material is again melt-extruded, pressed, and crushed, and thus the melt-extrusion, tableting, and crushing operations are repeated several times to prepare a pre-dispersed mixture.
  • the front temperature of the extruder is 85-95 °C
  • the rear temperature is 110-120 °C
  • the repeated operations of material melt extrusion, tableting and crushing are accumulated 2-3 times, and the material mixing time is accumulated. 60 - 200s. Then, it is uniformly mixed with other components, and then sent to an extruder for extrusion, tableting, and crushing; finally, the ultra-thin expanded steel structure fireproof powder coating is obtained by grinding with an ACM mill, and then sieving and packaging.
  • the epoxy resin and polyester resin in the formulation are film-forming materials which impart good decorative, bonding strength and mechanical properties to the coating.
  • the curing agent is an epoxy low temperature curing agent such as AB68, M68, dimethylimidazole, etc., and the amount thereof is determined according to the amount of the epoxy resin and the polyester resin.
  • Leveling agent and deaerator are additives to improve the surface decoration properties of powder coatings.
  • Pentaerythritol is a carbon forming agent
  • melamine is a foaming agent
  • ammonium polyphosphate is used as a catalyst
  • high molecular weight polyphosphoric acid with thermal stability greater than 270 ° C is selected. Ammonium ( ⁇ >1000, type II).
  • Melamine pyrophosphate is a swelling agent used to enhance the expansion of the coating.
  • ammonium polyphosphate is thermally decomposed to form phosphoric acid, and then further dehydrated to form polyphosphoric acid or polymetaphosphoric acid; polyphosphoric acid or polymetalactic acid reacts with the polyhydroxy compound pentaerythritol to form a carbonized layer; meanwhile, the foaming agent is trimeric
  • the heat of cyanamide liberates the incombustible gas, and the carbonized layer is bubbled and expanded to form a porous, dense and uniform honeycomb insulation layer.
  • the melamine pyrophosphate decomposes into phosphoric acid and emits a non-combustible gas, which enhances the foam expansion of the coating.
  • the smoke suppressant is zinc oxide or molybdenum oxide, which is used to reduce the amount of smoke when the coating is burned.
  • the reinforcing agent kaolin and rutile titanium dioxide are used to increase the mechanical strength of the carbonized layer after expansion.
  • the toughening agent polyvinyl butyral or dioctyl ester is used to increase the flexibility of the coating.
  • the pigment filler is used for the decorativeness of the coating and to improve the physical and mechanical properties of the coating.
  • the flow aid A1 2 0 3 -C or the vapor phase SiO 2 is used to improve the fluidity and powder rate of the powder coating.
  • the present invention has the following advantages and effects:
  • the coating contains no solvents, avoids environmental pollution caused by organic solvents, fire hazard, waste of organic solvents and human health hazards.
  • the coating also does not contain water and can also prevent water pollution like water-based coatings.
  • the coating has nearly 100% utilization and high coating efficiency, and can be applied in several coats or even dozens of coatings in a single coat.
  • the coating is applied without the influence of temperature and season, and the construction is simple.
  • the fire-retardant coating of the coating is better than the solvent-based and water-based coatings in terms of physical and mechanical properties and chemical resistance. detailed description
  • Epoxy resin E-12, Zhejiang Nanhai Pharmaceutical Group; Polyester Resin: P5127, DSM Coating Resin Company; Melamine Pyrophosphate MPP: Shandong Shi'an Chemical Co., Ltd.; Ammonium Polyphosphate APP ( ⁇ ), n ⁇ 1000 : Shandong Shi'an Chemical Co., Ltd.; Others are commercially available products.
  • Zinc oxide 3 3 2. 5 2 2 2 kaolin 3 3 3 3 3
  • ammonium polyphosphate, pentaerythritol, melamine, melamine pyrophosphate are passed through a 200 mesh sieve according to the formula amount, and the formulated amount of polyester resin, epoxy resin, and leveling agent are mixed and dispersed, and added to a screw extruder for extrusion.
  • the crushed material is melted and extruded again, pressed, and crushed, and the melt-extrusion, tableting, and crushing operations are repeated three times to prepare a pre-dispersed mixture, and the temperature of the extruder is 85-95 Torr. After the temperature is 110-120 °C, the material mixing time is 60-200s. Then, it is uniformly mixed with other components, and then sent to an extruder for extrusion, tableting and crushing; finally, the ultra-thin expanded steel structure fireproof powder coating is obtained by grinding with an A C M mill, and then sieving and packaging.
  • the fireproof coating was applied to the steel structural substrate and tested according to GB14907-2002.
  • the physical and mechanical properties and fire resistance of the fireproof coating greatly exceeded the requirements of the national standard.
  • the main properties of the corresponding fire retardant coatings are shown in Table 2.
  • Example 1 Example 2
  • Example 3 Example 4
  • the appearance of the powder coating is loose, no agglomerate, loose, no agglomerated, loose, no agglomerate, loose, no agglomerate, loose, no agglomeration, flat, no crack, flat, no crack, flat, no crack Smooth without cracks and no cracks
  • Adhesion grade 3 3 3 3 3 Impact strength ⁇ 30kg.cm ⁇ 30kg.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paints Or Removers (AREA)

Abstract

A fireproofing powder coating for steel structures and the preparing method thereof, which belong to the coating technique field, are disclosed. The raw materials for preparing the fireproofing powder coating comprise polyester resin, epoxy resin, hardening agent, catalyst, charring agent, foaming agent, expansion auxiliary agent, reinforcing agent, fume inhibitor, flexibilizer, levelling agent, degassing agent, flowing agent, pigments and fillers. The fireproofing powder coating can be prepared by melting polyester resin, epoxy resin, catalyst, carbon-forming agent, foaming agent, expansion auxiliary agent and levelling agent together and extruding, then mixing with other components and melt extruding, tabletting and crushing, followed by pulverizing with ACM mill, sieving and packing to give the resultant product. The coating can be used as fireproofing coating for various steel structures.

Description

说明书 一种钢结构防火粉末涂料及其制备方法 技术领域  Steel structure fireproof powder coating and preparation method thereof
本发明涉及一种钢结构防火粉末涂料及该涂料的制备方法， 属于防火涂料技术领 域。 背景技术  The invention relates to a steel structure fireproof powder coating and a preparation method thereof, and belongs to the technical field of fireproof coatings. Background technique
现在的钢结构防火涂料种类较多， 按材料状态可分为溶剂型、 水溶型和粉末型， 按 防火机理可分为膨胀型和非膨胀型两大类， 按涂层厚度可分为厚型、 薄型和超薄型。  There are many types of fire-retardant coatings for steel structures. According to the state of materials, they can be divided into solvent-based, water-soluble and powder-based. According to the fire-proof mechanism, they can be divided into two types: expanded and non-expanded. , thin and ultra-thin.
钢结构防火涂料是施涂于建筑物及构筑物钢结构表面， 能形成耐火隔热保护层， 以 提高钢结构耐火极限的防火涂料， 是防火涂料的主要品种。 近年来， 随着经济的发展和 涂料技术的不断提高，钢结构防火涂料产品正朝着超薄型、装饰性、耐候性的方向发展。  Steel structure fireproof coating is a fireproof coating applied to the surface of steel structures of buildings and structures, which can form a fireproof and heat insulation layer to improve the fire resistance of steel structures. It is the main type of fireproof coatings. In recent years, with the development of the economy and the continuous improvement of coating technology, steel structure fireproof coating products are developing in the direction of ultra-thin, decorative and weather resistance.
目前研究的技术和应用的产品大多是溶剂型和水溶型防火涂料。随着人们环保意识 的逐渐提高， 环保法规的逐渐健全， 溶剂型涂料越来越不能适应社会的发展， 最终将被 淘汰； 水溶型防火涂料在防火性能、 理化性能、 耐候性等方面不如溶剂型。 目前钢结构 防火涂料随着整个涂料工业正在向 "五 E"方向迈进， 即提高涂膜质量 （Excellence of finish)、方便施工 (Easy of application)、节省资源 (Economics)、节省能源 (Energy- saving) 和适应环境 (Ecology) 。  Most of the technologies and applications currently under study are solvent-based and water-soluble fire retardant coatings. With the gradual improvement of people's awareness of environmental protection and the gradual improvement of environmental protection regulations, solvent-based coatings are increasingly unable to adapt to the development of society and will eventually be eliminated. Water-soluble fire-retardant coatings are not as good as solvent-based in terms of fire resistance, physical and chemical properties, and weather resistance. . At present, steel structure fireproof coatings are moving towards the "five E" direction, that is, improving the finish of finish, ease of application, economics, and energy-saving. ) and adapt to the environment (Ecology).
粉末涂料不含溶剂， 具有近 100%的利用率， 高效、 环保、 节能、 经济， 是未来涂 料发展的主要方向之一， 目前粉末涂料的研究技术和应用产品大多集中于装饰性、 防腐 性等方面， 很少有钢结构防火涂料方面的文献报道和相关的申请专利。 CN1380370A公 幵了一种防火粉末涂料及其生产工艺， 对防火粉末涂料及其制备方法进行了一定的探 讨，先将各种防火助剂预分散到树脂中然后再混合其他材料采用粉末涂料的加工方法制 备出防火涂料产品， 由于许多防火助剂不仅熔点低， 而且活性高， 这些都影响了他们在 防火粉末涂料中的使用， 也增加了防火粉末涂料的研发难度。所以至今我们也没有见到 这方面成功的报道。 发明内容  Powder coatings contain no solvent, have nearly 100% utilization rate, high efficiency, environmental protection, energy saving and economy. It is one of the main directions of future coating development. At present, most research and application products of powder coatings focus on decorative, anti-corrosion, etc. In terms of the literature, there are few literature reports and related patent applications for steel fire retardant coatings. CN1380370A discloses a fireproof powder coating and a production process thereof, and discusses the fireproof powder coating and the preparation method thereof, first pre-dispersing various fireproofing assistants into the resin and then mixing other materials with the processing of the powder coating. The method provides a fireproof coating product. Since many fireproofing agents have low melting point and high activity, these all affect their use in fireproof powder coatings, and also increase the difficulty in research and development of fireproof powder coatings. So far we have not seen successful reports in this regard. Summary of the invention
本发明的目的在于提供一种具有涂层超薄、 耐火性能优异、 膨胀发泡层均勾致密的 钢结构防火粉末涂料及其制备方法。 本发明是以如下技术方案实现： 一种钢结构防火粉末涂料， 其特征是， 它是由聚酯 树脂、 环氧树脂、 固化剂、 催化剂、 成碳剂、 发泡剂、 膨胀助剂、 补强剂、 抑烟剂、 增 韧剂、 流平剂、 脱气剂、 流动剂、 颜填料经多次熔融挤出混合、 压片、 磨粉工艺制成， 各原料具体配方如下 （重量份）： The object of the present invention is to provide a steel structure fireproof powder coating which has ultra-thin coating, excellent fire resistance and thickened expansion foam layer and a preparation method thereof. The invention is realized by the following technical scheme: a steel structure fireproof powder coating, which is characterized in that it is composed of a polyester resin, an epoxy resin, a curing agent, a catalyst, a carbonizing agent, a foaming agent, an expansion aid, and a supplement. Strong agent, smoke suppressant, toughening agent, leveling agent, deaerator, flow agent, pigment and filler are prepared by multiple melt extrusion and extrusion, tableting and milling process. The specific formula of each raw material is as follows (parts by weight) :
环氧树脂 30-47.5  Epoxy resin 30-47.5
聚酯树脂 13.5-30  Polyester resin 13.5-30
固化剂 0〜5  Curing agent 0~5
流平剂 0.8-4  Leveling agent 0.8-4
脱气剂 0.1-1  Deaerator 0.1-1
聚磷酸铵 15-20  Ammonium polyphosphate 15-20
三聚氰胺 5-12  Melamine 5-12
季戊四醇 7-15  Pentaerythritol 7-15
三聚氰胺焦磷酸盐 4-9  Melamine pyrophosphate 4-9
抑烟剂 0-5  Smoke suppressant 0-5
补强剂 5-10  Reinforcing agent 5-10
增韧剂 0-5  Toughener 0-5
颜填料 0-10  Pigment filling 0-10
流动剂 0.1-0.5  Flow agent 0.1-0.5
所述的环氧树脂为环氧值 0.01~0.12的双酚 A型环氧树脂， 聚酯树脂为酸值 68〜82 mgKOH/g的粉末涂料专用聚酯树脂； 固化剂为环氧类低温固化剂；  The epoxy resin is a bisphenol A epoxy resin having an epoxy value of 0.01 to 0.12, and the polyester resin is a polyester resin for powder coating having an acid value of 68 to 82 mgKOH/g; the curing agent is epoxy low temperature curing. Agent
所述的流平剂为环氧 -聚酯型粉末涂料用流平剂 PV88、 GLP588, GLP503 ;  The leveling agent is a leveling agent for epoxy-polyester powder coatings PV88, GLP588, GLP503;
所述的脱气剂为安息香或粉末涂料用脱气蜡；  The deaerator is a degassing wax for benzoin or powder coating;
所述的聚磷酸铵为 n〉1000, II型的高分子量多聚磷酸铵；  The ammonium polyphosphate is n>1000, type II high molecular weight ammonium polyphosphate;
所述的抑烟剂为氧化锌、 氧化钼；  The smoke suppressing agent is zinc oxide or molybdenum oxide;
所述的补强剂为高嶺土、 凹凸棒土、 金红石型钛白粉；  The reinforcing agent is kaolin, attapulgite, rutile titanium dioxide;
所述的增韧剂为聚乙烯醇缩丁醛、 二辛酯；  The toughening agent is polyvinyl butyral, dioctyl ester;
所述的流动剂为 A1203-C、 气相 Si02。 The flow agent is A1 2 0 3 -C, gas phase SiO 2 .
所述的该防火涂料的制备方法是，首先按配方量将聚磷酸铵、季戊四醇、三聚氰胺、 三聚氰胺焦磷酸盐过 200目筛后和配方量的聚酯树脂、 环氧树脂、 流平剂混合分散， 加 到螺杆挤出机中挤出、 压片、 破碎后， 将破碎物再次熔融挤出、 压片、 破碎， 如此重复 熔融挤出、 压片、 破碎的操作多次而制成预分散混合物， 挤出机前温 85-95 °C， 后温 110-120°C , 物料熔融挤出、 压片、 破碎的重复操作累计 2-3 次， 物料混合时间累积 60 - 200s。 然后与其它各组分混合均匀， 再送至挤出机挤出、 压片、 破碎； 最后， 用 A C M磨机磨粉， 再过筛、 包装即可得到该超薄膨胀型钢结构防火粉末涂料。 The fireproof coating is prepared by first mixing and dispersing ammonium polyphosphate, pentaerythritol, melamine, melamine pyrophosphate through a 200 mesh sieve and a formula amount of a polyester resin, an epoxy resin, and a leveling agent according to a formula amount. After being added to a screw extruder for extrusion, tableting, and crushing, the crushed material is again melt-extruded, pressed, and crushed, and thus the melt-extrusion, tableting, and crushing operations are repeated several times to prepare a pre-dispersed mixture. , the front temperature of the extruder is 85-95 °C, the rear temperature is 110-120 °C, and the repeated operations of material melt extrusion, tableting and crushing are accumulated 2-3 times, and the material mixing time is accumulated. 60 - 200s. Then, it is uniformly mixed with other components, and then sent to an extruder for extrusion, tableting, and crushing; finally, the ultra-thin expanded steel structure fireproof powder coating is obtained by grinding with an ACM mill, and then sieving and packaging.
所述配方中环氧树脂和聚酯树脂是成膜物质， 它能使涂层具有良好的装饰性、 粘接 强度、 机械性能。 固化剂为环氧类低温固化剂， 如 AB68、 M68、 二甲基咪唑等， 其用 量根据环氧树脂和聚酯树脂的用量而定。流平剂和脱气剂是改善粉末涂料表面装饰性能 的助剂， 季戊四醇为成炭剂， 三聚氰胺为发泡剂， 聚磷酸铵为催化剂， 选用热稳定性大 于 270°C的高分子量多聚磷酸铵 （η>1000， II型）。 三聚氰胺焦磷酸盐为一种膨胀剂， 用以加强涂层的膨胀效果。 当涂层受热软化后， 聚磷酸铵受热分解生成磷酸， 然后，进 一步脱水生成聚磷酸或聚偏磷酸；聚磷酸或聚偏酸与多羟基化合物季戊四醇反应形成炭 化层； 同时， 发泡剂三聚氰铵热分解放出不燃性气体， 使炭化层鼓泡膨胀， 形成多孔致 密均匀的蜂窝状隔热层。 三聚氰胺焦磷酸盐在涂层软化后分解成磷酸并放出不燃性气 体， 加强涂层发泡膨胀。 抑烟剂是氧化锌或氧化钼， 用于降低涂层燃烧时的烟雾量。 补 强剂高嶺土、 金红石型钛白粉是提高炭化层膨胀后的机械强度。增韧剂聚乙烯醇缩丁醛 或二辛酯为了提高涂层的柔韧性。 颜填料用于涂层的装饰性和改善涂层的物理机械性 能。 流动助剂 A1203-C或气相 Si02用于改善粉末涂料的流动性、 上粉率。 The epoxy resin and polyester resin in the formulation are film-forming materials which impart good decorative, bonding strength and mechanical properties to the coating. The curing agent is an epoxy low temperature curing agent such as AB68, M68, dimethylimidazole, etc., and the amount thereof is determined according to the amount of the epoxy resin and the polyester resin. Leveling agent and deaerator are additives to improve the surface decoration properties of powder coatings. Pentaerythritol is a carbon forming agent, melamine is a foaming agent, ammonium polyphosphate is used as a catalyst, and high molecular weight polyphosphoric acid with thermal stability greater than 270 ° C is selected. Ammonium (η>1000, type II). Melamine pyrophosphate is a swelling agent used to enhance the expansion of the coating. When the coating is softened by heat, ammonium polyphosphate is thermally decomposed to form phosphoric acid, and then further dehydrated to form polyphosphoric acid or polymetaphosphoric acid; polyphosphoric acid or polymetalactic acid reacts with the polyhydroxy compound pentaerythritol to form a carbonized layer; meanwhile, the foaming agent is trimeric The heat of cyanamide liberates the incombustible gas, and the carbonized layer is bubbled and expanded to form a porous, dense and uniform honeycomb insulation layer. After the coating softens, the melamine pyrophosphate decomposes into phosphoric acid and emits a non-combustible gas, which enhances the foam expansion of the coating. The smoke suppressant is zinc oxide or molybdenum oxide, which is used to reduce the amount of smoke when the coating is burned. The reinforcing agent kaolin and rutile titanium dioxide are used to increase the mechanical strength of the carbonized layer after expansion. The toughening agent polyvinyl butyral or dioctyl ester is used to increase the flexibility of the coating. The pigment filler is used for the decorativeness of the coating and to improve the physical and mechanical properties of the coating. The flow aid A1 2 0 3 -C or the vapor phase SiO 2 is used to improve the fluidity and powder rate of the powder coating.
本发明与现有技术相比较， 具有如下优点和效果：  Compared with the prior art, the present invention has the following advantages and effects:
该涂料不含溶剂， 可避免有机溶剂带来的环境污染、 火灾危险、 浪费有机溶剂和危 害人体健康等问题； 该涂料亦不含水， 也可避免像水基涂料那样， 对水质造成污染。 该 涂料有近 100%的利用率且涂装效率高，一次涂装即可达到溶剂型或水性涂料几道甚至几 十道涂装的厚度。 该涂料的涂装不受气温和季节的影响， 施工简便。 该涂料的防火涂层 物理力学性能和耐化学介质等性能比溶剂型和水基型涂料好。 具体实施方式  The coating contains no solvents, avoids environmental pollution caused by organic solvents, fire hazard, waste of organic solvents and human health hazards. The coating also does not contain water and can also prevent water pollution like water-based coatings. The coating has nearly 100% utilization and high coating efficiency, and can be applied in several coats or even dozens of coatings in a single coat. The coating is applied without the influence of temperature and season, and the construction is simple. The fire-retardant coating of the coating is better than the solvent-based and water-based coatings in terms of physical and mechanical properties and chemical resistance. detailed description
下面结合实施例进一步阐明本发明的方案及效果。一种钢结构防火粉末涂料及该涂 料的制备方法  The aspects and effects of the present invention will be further clarified below with reference to the embodiments. Steel structure fireproof powder coating and preparation method of the same
本发明的超薄膨胀型钢结构防火粉末涂料共列举五个实施例， 各实施例的原料用 量按重量份如表 1。  Five examples of the ultra-thin expanded steel structure fireproof powder coating of the present invention are listed, and the raw materials used in the respective examples are shown in Table 1 by weight.
实施例中使用的原料名称和生产厂家如下：  The names of the raw materials used in the examples and the manufacturers are as follows:
环氧树)旨： E— 12， 浙江省南海药化集团； 聚酯树脂： P5127, DSM涂料树脂公司； 三聚氰胺焦磷酸盐 MPP: 山东世安化工有限公司； 聚磷酸铵 APP ( Π )，n〉1000: 山东 世安化工有限公司； 其它均为市售商品。 Epoxy resin): E-12, Zhejiang Nanhai Pharmaceutical Group; Polyester Resin: P5127, DSM Coating Resin Company; Melamine Pyrophosphate MPP: Shandong Shi'an Chemical Co., Ltd.; Ammonium Polyphosphate APP ( Π ), n〉 1000 : Shandong Shi'an Chemical Co., Ltd.; Others are commercially available products.
表 1 本发明的超薄膨胀型防火涂料实施例配方 实施例 1 实施例 2 实施例 3 实施例 4 实施例 5 环氧树脂 E— 12 30 47 47 47 47 聚酯树脂 30 14 14 14 13. 5 固化剂 M68 0 5 5 5 5 流平剂 GLP588 2 2 2 2 2 安息香 0. 4 0. 5 0. 4 0. 4 0. 4. Table 1 Formulation of the ultra-thin intumescent fireproof coating embodiment of the present invention Example 1 Example 2 Example 3 Example 4 Example 5 Epoxy Resin E-12 30 47 47 47 47 Polyester Resin 30 14 14 14 13. 5 Curing Agent M68 0 5 5 5 5 Leveling Agent GLP588 2 2 2 2 2 benzoin 0. 4 0. 5 0. 4 0. 4 0. 4.
聚磷酸铵 APP 15 15 20 18 20 ( II ) n^2000 Ammonium polyphosphate APP 15 15 20 18 20 ( II ) n^2000
三聚氰胺 8 8 10 8 10 季戊四醇 9 9 10 12 15 三聚氰胺焦磷酸 5 5 8 8 8 Melamine 8 8 10 8 10 pentaerythritol 9 9 10 12 15 melamine pyrophosphate 5 5 8 8 8
盐 MPP  Salt MPP
氧化锌 3 3 2. 5 2 2 高岭土 3 3 3 3 3 Zinc oxide 3 3 2. 5 2 2 kaolin 3 3 3 3 3
增韧剂 PVB 3 3 3 3 3 金红石型钛白粉 7 7 7 7 7 气相 Si02 0. 2 0. 2 0. 1 0. 1 0. 1 各实施例的制造方法相同， 其方法如下: Toughener PVB 3 3 3 3 3 Rutile Titanium Dioxide 7 7 7 7 7 Gas phase Si0 2 0. 2 0. 2 0. 1 0. 1 0. 1 The manufacturing method of each example is the same, and the method is as follows:
首先按配方量将聚磷酸铵、 季戊四醇、 三聚氰胺、 三聚氰胺焦磷酸盐过 200目筛后 和配方量的聚酯树脂、 环氧树脂、 流平剂混合分散， 加到螺杆挤出机中挤出、 压片、 破 碎后， 将破碎物再次熔融挤出、 压片、 破碎， 如此重复熔融挤出、 压片、 破碎的操作 3 次而制成预分散混合物， 挤出机前温 85-95 Ό , 后温 110-120 °C， 物料混合时间累积 60 - 200s。 然后与其它各组分混合均匀， 再送至挤出机挤出、 压片、 破碎； 最后， 用 A C M磨机磨粉， 再过筛、 包装即可得到该超薄膨胀型钢结构防火粉末涂料。  First, ammonium polyphosphate, pentaerythritol, melamine, melamine pyrophosphate are passed through a 200 mesh sieve according to the formula amount, and the formulated amount of polyester resin, epoxy resin, and leveling agent are mixed and dispersed, and added to a screw extruder for extrusion. After tableting and crushing, the crushed material is melted and extruded again, pressed, and crushed, and the melt-extrusion, tableting, and crushing operations are repeated three times to prepare a pre-dispersed mixture, and the temperature of the extruder is 85-95 Torr. After the temperature is 110-120 °C, the material mixing time is 60-200s. Then, it is uniformly mixed with other components, and then sent to an extruder for extrusion, tableting and crushing; finally, the ultra-thin expanded steel structure fireproof powder coating is obtained by grinding with an A C M mill, and then sieving and packaging.
将该防火涂料用于钢结构底材， 按照 GB14907— 2002进行性能测试， 其物理机械 性能和耐火性能均大大超过国标中要求的指标。 其相应防火涂料的主要性能如表 2。  The fireproof coating was applied to the steel structural substrate and tested according to GB14907-2002. The physical and mechanical properties and fire resistance of the fireproof coating greatly exceeded the requirements of the national standard. The main properties of the corresponding fire retardant coatings are shown in Table 2.
表 2本发明防火涂料的主要性能  Table 2 Main performance of the fire retardant coating of the present invention
性能项目 实施例 1 实施例 2 实施例 3 实施例 4 实施例 5 粉末涂料外观 疏松无结块 疏松无结块 疏松无结块 疏松无结块 疏松无结块 外观 平整无裂纹 平整无裂纹 平整无裂紋 平整无裂纹 平整无裂纹 附着力，级 3 3 3 3 3 冲击强度 ^30kg.cm ^30kg. cm ^30kg.cm ^30kg.cm ^30kg.cm 耐水性 (h) 168,涂层 168,涂层 168,涂层 168,涂层 168,涂层 无起层、 发 无起层、 发 无起层、 发 无起层、 发 无起层、 发 泡、 脱落现 泡、 脱落现 泡、 脱落现 泡、 脱落现 泡、 脱落现 涂 象 象 象 象 象 层 耐湿热性 ^720,涂层 ^720,涂层 720，涂层 720，涂层 ^720,涂层 性 (h) 无起泡、 脱 无起泡、 脱 无起泡、 脱 无起泡、 脱 无起泡、 脱 能 落现象 落现象 落现象 落现象 · 落现象 耐冷热循 ^20, 涂层 20， 涂层 ^20 , 涂层 20， 涂层 ^20 , 涂层 环性，次 无开裂、 剥 无开裂、 剥 无开裂、 剥 无开裂、 剥 无开裂、 剥 落、 起泡现 落、 起泡现 落、 起泡现 落、 起泡现 落、 起泡现 象 象 象 象 象 耐 涂层厚度 1.8 1.8 1.8 1.8 1.8 火 mm Performance Item Example 1 Example 2 Example 3 Example 4 Example 5 The appearance of the powder coating is loose, no agglomerate, loose, no agglomerated, loose, no agglomerate, loose, no agglomerate, loose, no agglomeration, flat, no crack, flat, no crack, flat, no crack Smooth without cracks and no cracks Adhesion, grade 3 3 3 3 3 Impact strength ^30kg.cm ^30kg. cm ^30kg.cm ^30kg.cm ^30kg.cm Water resistance (h) 168, coating 168, coating 168, coating 168, Coating 168, coating without layer, no layer, no layer, no layer, no layer, foaming, shedding, shedding, shedding, shedding, shedding, shedding Now painted like elephant image layer heat and humidity resistance 720, coating ^ 720, coating 720, coating 720, coating ^ 720, coating properties (h) no blistering, no blistering, no detachment Bubble, no blistering, no blistering, dissociation, falling phenomenon, falling phenomenon, falling phenomenon, cold and hot resistance, 20, coating 20, coating 20, coating 20, coating ^20, Coating ringing, no cracking, no cracking, no cracking, no cracking, no cracking, no cracking, peeling, foaming, foaming, foaming, foaming, foaming, foaming Image-like coating thickness 1.8 1.8 1.8 1.8 1.8 fire mm
时 耐火极限 67 70 75 73 80 间 min Time Fire endurance 67 70 75 73 80 minutes min

Claims

权利要求书 Claim
1、 一种钢结构防火粉末涂料， 其特征是， 它是由聚酯树脂、 环氧树脂、 固化剂、 催化剂、 成碳剂、 发泡剂、 膨胀助剂、 补强剂、 抑烟剂、 增韧剂、 流平剂、 脱气剂、 流 动剂、 颜填料经多次熔融挤出混合、 压片、 磨粉工艺制成， 各原料具体配方如下 （重量 份)： 1. A steel structure fireproof powder coating, characterized in that it is composed of a polyester resin, an epoxy resin, a curing agent, a catalyst, a carbon-forming agent, a foaming agent, an expansion aid, a reinforcing agent, a smoke suppressing agent, Toughener, leveling agent, deaerator, flow agent, pigment and filler are prepared by multiple melt extrusion and extrusion, tableting and milling processes. The specific formula of each raw material is as follows (parts by weight):
环氧树脂 30-47.5  Epoxy resin 30-47.5
聚酯树脂 13.5-30  Polyester resin 13.5-30
固化剂 0〜5  Curing agent 0~5
流平剂 0.8-4  Leveling agent 0.8-4
脱气剂 0.1-1  Deaerator 0.1-1
聚磯酸铵 15-20  Ammonium polyamic acid 15-20
三聚氰胺 5-12  Melamine 5-12
季戊四醇 7-15  Pentaerythritol 7-15
三聚氰胺焦磷酸盐 4-9  Melamine pyrophosphate 4-9
抑烟剂 0-5  Smoke suppressant 0-5
补强剂 5-10  Reinforcing agent 5-10
增韧剂 0〜5  Toughener 0~5
颜填料 0-10  Pigment filling 0-10
流动剂 0.1-0.5 。  Flow agent 0.1-0.5.
2、 根据权利要求 1 所述的一种钢结构防火粉末涂料， 其特征是环氧树脂为环氧值 0.01-0.12的双酚 A型环氧树脂，聚酯树脂为酸值 68~82 mgKOH/g的粉末涂料专用聚酯 树脂； 固化剂为环氧类低温固化剂。  2. A steel structure fireproof powder coating according to claim 1, wherein the epoxy resin is a bisphenol A type epoxy resin having an epoxy value of 0.01 to 0.12, and the polyester resin has an acid value of 68 to 82 mgKOH/ g special polyester resin for powder coating; curing agent is epoxy low temperature curing agent.
3、 根据权利要求 1所述的一种钢结构防火粉末涂料， 其特征是流平剂为环氧 -聚酯 型粉末涂料用流平剂 PV88、 GLP588、 GLP503。  3. A steel structure fireproof powder coating according to claim 1, wherein the leveling agent is a leveling agent for epoxy-polyester powder coatings, PV88, GLP588, GLP503.
4、 根据权利要求 1 所述的一种钢结构防火粉末涂料， 其特征是脱气剂为安息香或, 粉末涂料用脱气蜡。  4. A steel structure fireproof powder coating according to claim 1, wherein the deaerator is benzoin or a degassing wax for powder coating.
5、根据权利要求 1所述的一种钢结构防火粉末涂料，其特征是聚磷酸铵为 n〉1000， II型的高分子量多聚磷酸铵。  A steel structure fireproof powder coating according to claim 1, wherein the ammonium polyphosphate is a high molecular weight ammonium polyphosphate of n>1000, type II.
6、 根据权利要求 1 所述的一种钢结构防火粉末涂料， 其特征是抑烟剂为氧化锌、 氧化钼。 6. A steel structure fireproof powder coating according to claim 1, wherein the smoke suppressant is zinc oxide or molybdenum oxide.
7、 根据权利要求 1所述的一种钢结构防火粉末涂料， 其特征是补强剂为高嶺土、 凹凸棒土、 金红石型钛白粉。 7. A steel structure fireproof powder coating according to claim 1, wherein the reinforcing agent is kaolin, attapulgite, rutile type titanium dioxide.
8、 根据权利要求 1所述的一种钢结构防火粉末涂料， 其特征是增韧剂为聚乙烯醇 缩丁醛 PVB、 二辛酯。  8. A steel structure fireproof powder coating according to claim 1, wherein the toughening agent is polyvinyl butyral PVB or dioctyl ester.
9、 根据权利要求 1所述的一种钢结构防火粉末涂料， 其特征是流动剂为 A1203-C、 气相 Si02。 9. A steel structure fireproof powder coating according to claim 1, wherein the flow agent is A1 2 0 3 -C, gas phase SiO 2 .
10、 一种权利要求 1所述的一种钢结构防火粉末涂料制备方法， 其特征是， 首先按 配方量将聚磷酸铵、 季戊四醇、 三聚氰胺、 三聚氰胺焦磷酸盐过 200目筛后和配方量的 聚酯树脂、 环氧树脂、 流平剂混合分散， 将混合分散后的料加到螺杆挤出机中挤出、 压 片、 破碎后， 将破碎物再次熔融挤出、 压片、 破碎， 如此重复熔融'挤出、 压片、 破碎 的操作 2-3次而制成预分散混合物， 挤出机前温 85- 95°C， 后温 110-120Ό， 物料混合时 间累积 60- 200s; 然后与其它各组分混合均匀， 再送至挤出机挤出、 压片、破碎； 最后， 用 A C M磨机磨粉， 再过筛、 包装即可得到该钢结构防火粉末涂料。  10. A method for preparing a fire-retardant powder coating for a steel structure according to claim 1, characterized in that first, ammonium polyphosphate, pentaerythritol, melamine, melamine pyrophosphate are sieved through a 200 mesh sieve and a formula amount according to a formula amount. The polyester resin, the epoxy resin and the leveling agent are mixed and dispersed, and the mixed and dispersed materials are added to a screw extruder for extrusion, tableting, and crushing, and the crushed material is melted and extruded again, pressed, and broken. Repeat the melting 'extrusion, tableting, and crushing operations 2-3 times to prepare a pre-dispersed mixture. The pre-extrusion temperature is 85-95 ° C, the post-temperature is 110-120 Ό, and the material mixing time is 60-200 s. The other components are uniformly mixed and sent to the extruder for extrusion, tableting and crushing; finally, the steel structure fireproof powder coating is obtained by grinding with an ACM mill, and then sieving and packaging.
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