水性超薄型钢结构防火涂料的制备及防火作用机理研究
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摘要
溶剂型超薄钢结构防火涂料含有大量的挥发性有机物(VOC)，其应用越来越受到限制，甚至被发达国家禁用。水性超薄型钢结构防火涂料以水性聚合物作为成膜物质，减少了VOC的排放量，降低了涂料在生产、施工、应用等环节中对人体的危害和对环境的污染，符合节能减排、绿色环保的发展趋势，是防火涂料研究的重点。本论文针对水性超薄型钢结构防火涂料的防火性能差、膨胀倍率低、膨胀层结构强度低、耐水性差等问题进行了深入研究，并对成膜物质(醋叔聚合物)的热分解过程和成炭机理、聚磷酸铵对醋叔聚合物热分解过程的影响进行了讨论；探索性地研究了纳米二氧化锆及水性含磷聚合物在防火涂料中地应用。主要研究工作如下：
(1)从热分解特性、动态流变性能和复合黏度的角度研究了成膜物质对防火涂料膨胀防火性能的影响。研究结果表明：纯丙和苯丙聚合物熔体的储存模量(G＇)大于损耗模量(G＂)，以弹性流动为主，复合黏度高(>1000Pa·s)；醋叔聚合物熔体的G＂大于G＇，以粘性流动为主，复合黏度低(33Pa·s)。具有热稳定性好、成炭能力强、复合黏度低、粘性流体特性的聚合物适合作为防火涂料的成膜物质，有利于涂层的膨胀和防火性能的提高。
(2)以醋叔聚合物(VAc-VeoVa)作为成膜物质，聚磷酸铵/季戊四醇/三聚氰胺/可膨胀石墨(APP/PER/MEL/EG)作为膨胀阻燃体系(IFR)，研究了IFR及其与VAc-VeoVa的配比对防火涂料性能的影响。正交实验直观分析结果表明，IFR中各组分对防火涂料性能的影响顺序依次为：APP＞EG＞PER＞MEL，最佳配比为APP:PER:MEL:EG=22:8:8:4.5。当VAc-VeoVa用量为30%，IFR用量为40%时，防火涂层的防火性能最佳(燃烧30min后钢板背温为262℃)。
(3)研究了无机填料的组成、颗粒大小及形态等因素对防火涂料的影响。TG、毛细管流变测试、防火性能测试等研究结果表明：以TiO_2/SAp/HNTs (8/1/1)作为无机填料时，防火涂料的防火性能优异(3327s)，膨胀倍率较高(28.14)，膨胀层结构好、强度高。无机填料通过限制成膜聚合物分子链的松弛和旋转，以及降低APP对PER和VAc-VeoVa的催化脱水效率来影响防火涂料的膨胀倍率与防火性能。同时在黏度较高时，无机填料难以迁移到膨胀层表面聚集形成无机隔热层，导致防火涂料的防火性能下降。通过配方优化，自制水性防火涂料的性能已超过国外知名品牌。
(4)研究了纳米二氧化锆(nano-ZrO_2)在防火涂料中的作用。研究结果表明：硅烷偶联剂γ-甲基丙烯酰氧基丙基三甲氧基硅烷(Z-6030)改性后的nano-ZrO_2在VAc-VeoVa乳液中具有良好的分散性。在不含EG的无卤防火涂料中，加入nano-ZrO_2后膨胀层不再具有连续致密的结构，且结构强度降低，防火性能随着nano-ZrO_2用量地增加反而下降。在含有EG的有卤防火涂料中，EG穿插在膨胀层中，起到结构支撑的作用；ZrO_2在膨胀层中起到隔热和防止热氧化分解的作用，防火时间达到3837s。XRD结果表明膨胀层中生成了焦磷酸钛(TiP2O7)、焦磷酸锆(ZrP2O7)和焦磷酸锆钛固溶体(Ti0.8Zr0.2P2O7)。
(5)研究了Vac-VeoVa的热分解过程及APP对VAc-VeoVa热分解过程的影响。研究结果表明：在空气氛围中VAc-VeoVa的热氧化分解过程分为三个阶段：(1)脱除醋酸和叔碳酸基团，生成不饱和碳链；(2)不饱和碳链的氧化脱氢、环化、芳构化，生成六方晶系碳；(3)六方晶系碳的热氧化。在氮气氛围中VAc-VeoVa热分解过程分为两个阶段：(1)脱除醋酸和叔碳酸基团，生成不饱和碳链；(2)不饱和碳链的断链或者环化、芳构化，生成六方晶系碳。密度泛函理论(DFT)计算结果表明VAc-VeoVa分子中叔碳酸与醋酸基团的脱除为竞争断裂的关系。TG和FTIR结果表明，APP降低了VAc-VeoVa的热分解温度，加快了VAc-VeoVa侧链基团的脱除速度。此外，APP热分解生成的聚磷酸与VAc-VeoVa分子脱除乙烯酮后生成的侧链羟基反应生成P-O-C键。P-O-C键将不饱和烯烃芳构化后生成的产物连接成为交联网络状结构，使炭残余物具有更好的热稳定性。
(6)合成了水性含磷苯丙聚合物P(MMA/St/BA/MAA/PAM100)，并以此作为成膜物质，研究了其在防火涂料中的应用。研究结果表明，乙烯基烷氧基磷酸酯(PAM100)提高了聚合物的热稳定性，属于凝聚相作用机理。防火性能测试结果表明，以StA-P1.5作为成膜物质制备的防火涂料的防火性能最佳。Flymn-Wall-Ozawa(FWO)方法与Kissinger-Akahira-Sunose(KAS)方法计算结果表明，PAM100显著地增大了聚合物的热分解活化能，但活化能随PAM100用量地增加而减小。聚合物热分解的机理函数分别为g(α)=-ln(1-α)，f(α)=1-α，反应级数n=1，热分解速率表达式为d
dt A exp E/RT1。
Solventborne ultra-thin fire retardant coatings for steel structure has been limited, evenforbidden in many developed countries owing to its high content of volatile organiccompounds (VOC). In reverse, waterborne ultra-thin fire retardant coatings for steel structurewith polymer latex as binder have become the emphasis of modern research works, as it cutsdown the emissions of VOC, reduces the health hazards and environmental pollution duringthe production, construction and application, being in accordance with the trend of energyconservation and environmental protection. In order to improve the fire retardant property ofcoatings, the intumescent ratio and the structural strength of char layer, and the water-resistantof the coating film, etc., in this dissertation, studies about the preparation and performance ofwaterborne ultra-thin steel structure fire retardant coatings are carried out, and the thermaldegradation and char formation mechanism of vinyl acetate-vinyl ester of versatic acid(VAc-VeoVa) polymer, the influences of ammonium polyphosphate (APP) on the thermaldegradation of VAc-VeoVa are investigated. Moreover, the application of nanosized zirconiaand waterborne phosphorus-containing polymer in fire retardant coatings are also exploratorystudied. The main research works are as follows:
In part one, the effects of binder on the intumescent and fire retardant performance offire retardant coatings were intensively studied in terms of thermal degradation characteristic,dynamic rheology and composite viscosity. The results revealed that, for acrylic,styrene-acrylic molten polymers, the elastic modulus (G＇) were larger than the viscousmodulus (G＂), which meant the elastic behavior was predominant in these melts, and thecomplex viscosity was high up to1000Pa·s. While for VAc-VeoVa molten polymer, G＂waslarger than G＇, which meant the viscous behavior was predominant in this melt, and thecomplex viscosity was low as33Pa·s. Polymer with good thermal stability, strongcarbonization capacity, low complex viscosity, and significant viscous flow behavior, wassuitable as the binder for improving the fire retardancy of coatings.
In part two, when VAc-VeoVa latexes was used as the binder, and ammoniumpolyphosphate/pentaerythritol/melamine/expandable graphite (APP/PER/MEL/EG) were usedas the intumescent flame retardant (IFR) system, the effects of IFR and its proportion with VAc-VeoVa latexes on fire retardant performance, intumescent ratio, structure and strength ofswollen layers were studied. The orthogonal direct analysis showed that the effect order ofIFR on fire retardant coatings was APP＞EG＞PER＞MEL, and the optimal ratio wasAPP:PER:MEL:EG=22:8:8:4.5. When the weight content of VAc-VeoVa latexes and the IFRsystem was30%and40%, respectively, the coatings films presented excellent fire retardantproperty (the temperature of steel backside was262℃after exposing to fire for30min).
In part three, the effects of the component, size and morphology of inorganic fillers onthe fire retardant coatings were investigated. The results of thermogravimetry (TG), capillaryrheometer, fire retardant test, etc., demonstrated that, the coatings using TiO_2/SAp/HNTs(8/1/1) as multiple fillers presented outstanding fire retardant performance (3327s), and highintumescent ratio (28.14). The structure and strength of the intumescent layer was alsoexcellent. The inorganic fillers immobilized the relaxation and rotation of polymer chain, andreduced the catalytic dehydration efficiency of APP with PER and VAc-VeoVa, which, as aresult, affected the intumescent ratio and fire retardant performance of coatings. Moreover,under high melt viscosity, it was not easy for the filler to transfer to the surface to form aninorganic layer, which reduced the fire retardant performance of the coatings. Theperformance of home-made waterborne fire retardant coatings with optimized recipe wasbetter than that of the world famous brand one.
In part four, the effects of nano-ZrO_2on the performance of fire retardant coatings wereinvestigated. The results demonstrated that, nano-ZrO_2had excellent dispersion property inVAc-VeoVa polymer emulsion after surface modified by silicate coupling agent γ-methacryl-oxypropyltrimethoxysilane (Z-6030). In halogen-free fire retardant coatings and withoutexpandable graphite (EG), the addition of nano-ZrO_2resulted in the formed intumescent layerwas not compact, and the structural strength was decreased, so the fire retardant performancewas decreased as the content of nano-ZrO_2increased. But in the halogen fire retardantcoatings containing EG, EG penetrated in the intumescent char layer and supported itsstructural strength, nano-ZrO_2stayed in the intumescent char layer, prevented itsthermal-oxidative degradation and insulated heat, and the fire retardant time of the coatingswas3837s. XRD results demonstrated that titanium pyrophosphate (TiP2O7), zirconiumpyrophosphate (ZrP2O7), zirconate titanate pyrophosphate solid solution (Ti0.8Zr0.2P2O7) were formed in high temperature during fire.
In part five, the thermal degradation and the effect of APP on the thermal degradation ofVAc-VeoVa polymer were studied. The results revealed that, at air atmosphere, thethermal-oxidative degradation of VAc-VeoVa had three steps,(1) elimination of acetic acidand versatic acid to form unsaturated olefin carbon chain;(2) oxidative dehydrogenation,cyclization and aromatization of unsaturated olefin carbon chain to form hexagonal systemcarbon;(3) thermal oxidative of hexagonal system carbon. At nitrogen atmosphere, its thermaldegradation contained two steps,(1) elimination of acetic acid and versatic acid to formunsaturated olefin carbon chain;(2) scission or cyclization and aromatization of unsaturatedolefin carbon chain to form hexagonal system carbon. The results of density functional theory(DFT) revealed that the elimination of versatic acid was competing with acetate acid. Theresults of thermogravimetry-fourier transform infrared (TG-FTIR) analysis of VAc-VeoVa/APP at nitrogen atmosphere indicated that APP has reduced the thermal degradationtemperature and accelerated the side group elimination rate of VAc-VeoVa polymer. Moreover,the polyphosphate acid, formed by APP thermal degradation, reacted with the sidechainhydroxyl of VAc-VeoVa which was formed by eliminating ketene, to form P-O-C bond. ThisP-O-C bond could connect the aromatic product, formed by unsaturated olefin aromatizationreaction, into a crosslinked network structure, therefore improving the thermal stability ofcarbonate redidue.
In part six, waterborne phosphorus-containing styrene-acrylic polymer P(MMA/BA/MAA/PAM100), which was synthesized by free radical emulsion polymerization, was used asbinder in fire retardant coatings and the performance was evaluated. It was found that thethermal stability of the polymer was improved by phosphate esters of polyethylene glycolmonomethacrylate (PAM100), through condensed phase mechanism. The results of fireretardant test showed that the fire retardant coatings with StA-P1.5as binder processed the bestfire retardant performance. The calculation results from Kissinger-Akahira-Sunose (KAS)method and Flynm-Wall-Ozawa (FWO) method revealed that the thermal degradationactivation energy (Ea) of polymer was remarkably improved by PAM100, but Eawasdecreased as the weight content of PAM100increased. The thermal degradation mechanismfunctions of polymer were g(α)=-ln(1-α)，f(α)=1-α, respectively, the order of reaction was n=1, the thermal degradation rate expression wasdt|da=A·exp(-E/RT).(1-a).
(1)从热分解特性、动态流变性能和复合黏度的角度研究了成膜物质对防火涂料膨胀防火性能的影响。研究结果表明：纯丙和苯丙聚合物熔体的储存模量(G＇)大于损耗模量(G＂)，以弹性流动为主，复合黏度高(>1000Pa·s)；醋叔聚合物熔体的G＂大于G＇，以粘性流动为主，复合黏度低(33Pa·s)。具有热稳定性好、成炭能力强、复合黏度低、粘性流体特性的聚合物适合作为防火涂料的成膜物质，有利于涂层的膨胀和防火性能的提高。
(2)以醋叔聚合物(VAc-VeoVa)作为成膜物质，聚磷酸铵/季戊四醇/三聚氰胺/可膨胀石墨(APP/PER/MEL/EG)作为膨胀阻燃体系(IFR)，研究了IFR及其与VAc-VeoVa的配比对防火涂料性能的影响。正交实验直观分析结果表明，IFR中各组分对防火涂料性能的影响顺序依次为：APP＞EG＞PER＞MEL，最佳配比为APP:PER:MEL:EG=22:8:8:4.5。当VAc-VeoVa用量为30%，IFR用量为40%时，防火涂层的防火性能最佳(燃烧30min后钢板背温为262℃)。
(3)研究了无机填料的组成、颗粒大小及形态等因素对防火涂料的影响。TG、毛细管流变测试、防火性能测试等研究结果表明：以TiO_2/SAp/HNTs (8/1/1)作为无机填料时，防火涂料的防火性能优异(3327s)，膨胀倍率较高(28.14)，膨胀层结构好、强度高。无机填料通过限制成膜聚合物分子链的松弛和旋转，以及降低APP对PER和VAc-VeoVa的催化脱水效率来影响防火涂料的膨胀倍率与防火性能。同时在黏度较高时，无机填料难以迁移到膨胀层表面聚集形成无机隔热层，导致防火涂料的防火性能下降。通过配方优化，自制水性防火涂料的性能已超过国外知名品牌。
(4)研究了纳米二氧化锆(nano-ZrO_2)在防火涂料中的作用。研究结果表明：硅烷偶联剂γ-甲基丙烯酰氧基丙基三甲氧基硅烷(Z-6030)改性后的nano-ZrO_2在VAc-VeoVa乳液中具有良好的分散性。在不含EG的无卤防火涂料中，加入nano-ZrO_2后膨胀层不再具有连续致密的结构，且结构强度降低，防火性能随着nano-ZrO_2用量地增加反而下降。在含有EG的有卤防火涂料中，EG穿插在膨胀层中，起到结构支撑的作用；ZrO_2在膨胀层中起到隔热和防止热氧化分解的作用，防火时间达到3837s。XRD结果表明膨胀层中生成了焦磷酸钛(TiP2O7)、焦磷酸锆(ZrP2O7)和焦磷酸锆钛固溶体(Ti0.8Zr0.2P2O7)。
(5)研究了Vac-VeoVa的热分解过程及APP对VAc-VeoVa热分解过程的影响。研究结果表明：在空气氛围中VAc-VeoVa的热氧化分解过程分为三个阶段：(1)脱除醋酸和叔碳酸基团，生成不饱和碳链；(2)不饱和碳链的氧化脱氢、环化、芳构化，生成六方晶系碳；(3)六方晶系碳的热氧化。在氮气氛围中VAc-VeoVa热分解过程分为两个阶段：(1)脱除醋酸和叔碳酸基团，生成不饱和碳链；(2)不饱和碳链的断链或者环化、芳构化，生成六方晶系碳。密度泛函理论(DFT)计算结果表明VAc-VeoVa分子中叔碳酸与醋酸基团的脱除为竞争断裂的关系。TG和FTIR结果表明，APP降低了VAc-VeoVa的热分解温度，加快了VAc-VeoVa侧链基团的脱除速度。此外，APP热分解生成的聚磷酸与VAc-VeoVa分子脱除乙烯酮后生成的侧链羟基反应生成P-O-C键。P-O-C键将不饱和烯烃芳构化后生成的产物连接成为交联网络状结构，使炭残余物具有更好的热稳定性。
(6)合成了水性含磷苯丙聚合物P(MMA/St/BA/MAA/PAM100)，并以此作为成膜物质，研究了其在防火涂料中的应用。研究结果表明，乙烯基烷氧基磷酸酯(PAM100)提高了聚合物的热稳定性，属于凝聚相作用机理。防火性能测试结果表明，以StA-P1.5作为成膜物质制备的防火涂料的防火性能最佳。Flymn-Wall-Ozawa(FWO)方法与Kissinger-Akahira-Sunose(KAS)方法计算结果表明，PAM100显著地增大了聚合物的热分解活化能，但活化能随PAM100用量地增加而减小。聚合物热分解的机理函数分别为g(α)=-ln(1-α)，f(α)=1-α，反应级数n=1，热分解速率表达式为d
dt A exp E/RT1。
Solventborne ultra-thin fire retardant coatings for steel structure has been limited, evenforbidden in many developed countries owing to its high content of volatile organiccompounds (VOC). In reverse, waterborne ultra-thin fire retardant coatings for steel structurewith polymer latex as binder have become the emphasis of modern research works, as it cutsdown the emissions of VOC, reduces the health hazards and environmental pollution duringthe production, construction and application, being in accordance with the trend of energyconservation and environmental protection. In order to improve the fire retardant property ofcoatings, the intumescent ratio and the structural strength of char layer, and the water-resistantof the coating film, etc., in this dissertation, studies about the preparation and performance ofwaterborne ultra-thin steel structure fire retardant coatings are carried out, and the thermaldegradation and char formation mechanism of vinyl acetate-vinyl ester of versatic acid(VAc-VeoVa) polymer, the influences of ammonium polyphosphate (APP) on the thermaldegradation of VAc-VeoVa are investigated. Moreover, the application of nanosized zirconiaand waterborne phosphorus-containing polymer in fire retardant coatings are also exploratorystudied. The main research works are as follows:
In part one, the effects of binder on the intumescent and fire retardant performance offire retardant coatings were intensively studied in terms of thermal degradation characteristic,dynamic rheology and composite viscosity. The results revealed that, for acrylic,styrene-acrylic molten polymers, the elastic modulus (G＇) were larger than the viscousmodulus (G＂), which meant the elastic behavior was predominant in these melts, and thecomplex viscosity was high up to1000Pa·s. While for VAc-VeoVa molten polymer, G＂waslarger than G＇, which meant the viscous behavior was predominant in this melt, and thecomplex viscosity was low as33Pa·s. Polymer with good thermal stability, strongcarbonization capacity, low complex viscosity, and significant viscous flow behavior, wassuitable as the binder for improving the fire retardancy of coatings.
In part two, when VAc-VeoVa latexes was used as the binder, and ammoniumpolyphosphate/pentaerythritol/melamine/expandable graphite (APP/PER/MEL/EG) were usedas the intumescent flame retardant (IFR) system, the effects of IFR and its proportion with VAc-VeoVa latexes on fire retardant performance, intumescent ratio, structure and strength ofswollen layers were studied. The orthogonal direct analysis showed that the effect order ofIFR on fire retardant coatings was APP＞EG＞PER＞MEL, and the optimal ratio wasAPP:PER:MEL:EG=22:8:8:4.5. When the weight content of VAc-VeoVa latexes and the IFRsystem was30%and40%, respectively, the coatings films presented excellent fire retardantproperty (the temperature of steel backside was262℃after exposing to fire for30min).
In part three, the effects of the component, size and morphology of inorganic fillers onthe fire retardant coatings were investigated. The results of thermogravimetry (TG), capillaryrheometer, fire retardant test, etc., demonstrated that, the coatings using TiO_2/SAp/HNTs(8/1/1) as multiple fillers presented outstanding fire retardant performance (3327s), and highintumescent ratio (28.14). The structure and strength of the intumescent layer was alsoexcellent. The inorganic fillers immobilized the relaxation and rotation of polymer chain, andreduced the catalytic dehydration efficiency of APP with PER and VAc-VeoVa, which, as aresult, affected the intumescent ratio and fire retardant performance of coatings. Moreover,under high melt viscosity, it was not easy for the filler to transfer to the surface to form aninorganic layer, which reduced the fire retardant performance of the coatings. Theperformance of home-made waterborne fire retardant coatings with optimized recipe wasbetter than that of the world famous brand one.
In part four, the effects of nano-ZrO_2on the performance of fire retardant coatings wereinvestigated. The results demonstrated that, nano-ZrO_2had excellent dispersion property inVAc-VeoVa polymer emulsion after surface modified by silicate coupling agent γ-methacryl-oxypropyltrimethoxysilane (Z-6030). In halogen-free fire retardant coatings and withoutexpandable graphite (EG), the addition of nano-ZrO_2resulted in the formed intumescent layerwas not compact, and the structural strength was decreased, so the fire retardant performancewas decreased as the content of nano-ZrO_2increased. But in the halogen fire retardantcoatings containing EG, EG penetrated in the intumescent char layer and supported itsstructural strength, nano-ZrO_2stayed in the intumescent char layer, prevented itsthermal-oxidative degradation and insulated heat, and the fire retardant time of the coatingswas3837s. XRD results demonstrated that titanium pyrophosphate (TiP2O7), zirconiumpyrophosphate (ZrP2O7), zirconate titanate pyrophosphate solid solution (Ti0.8Zr0.2P2O7) were formed in high temperature during fire.
In part five, the thermal degradation and the effect of APP on the thermal degradation ofVAc-VeoVa polymer were studied. The results revealed that, at air atmosphere, thethermal-oxidative degradation of VAc-VeoVa had three steps,(1) elimination of acetic acidand versatic acid to form unsaturated olefin carbon chain;(2) oxidative dehydrogenation,cyclization and aromatization of unsaturated olefin carbon chain to form hexagonal systemcarbon;(3) thermal oxidative of hexagonal system carbon. At nitrogen atmosphere, its thermaldegradation contained two steps,(1) elimination of acetic acid and versatic acid to formunsaturated olefin carbon chain;(2) scission or cyclization and aromatization of unsaturatedolefin carbon chain to form hexagonal system carbon. The results of density functional theory(DFT) revealed that the elimination of versatic acid was competing with acetate acid. Theresults of thermogravimetry-fourier transform infrared (TG-FTIR) analysis of VAc-VeoVa/APP at nitrogen atmosphere indicated that APP has reduced the thermal degradationtemperature and accelerated the side group elimination rate of VAc-VeoVa polymer. Moreover,the polyphosphate acid, formed by APP thermal degradation, reacted with the sidechainhydroxyl of VAc-VeoVa which was formed by eliminating ketene, to form P-O-C bond. ThisP-O-C bond could connect the aromatic product, formed by unsaturated olefin aromatizationreaction, into a crosslinked network structure, therefore improving the thermal stability ofcarbonate redidue.
In part six, waterborne phosphorus-containing styrene-acrylic polymer P(MMA/BA/MAA/PAM100), which was synthesized by free radical emulsion polymerization, was used asbinder in fire retardant coatings and the performance was evaluated. It was found that thethermal stability of the polymer was improved by phosphate esters of polyethylene glycolmonomethacrylate (PAM100), through condensed phase mechanism. The results of fireretardant test showed that the fire retardant coatings with StA-P1.5as binder processed the bestfire retardant performance. The calculation results from Kissinger-Akahira-Sunose (KAS)method and Flynm-Wall-Ozawa (FWO) method revealed that the thermal degradationactivation energy (Ea) of polymer was remarkably improved by PAM100, but Eawasdecreased as the weight content of PAM100increased. The thermal degradation mechanismfunctions of polymer were g(α)=-ln(1-α)，f(α)=1-α, respectively, the order of reaction was n=1, the thermal degradation rate expression wasdt|da=A·exp(-E/RT).(1-a).
引文
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