本文選題：芳砜綸 + 氫氧化鎂　； 參考：《東華大學(xué)》2017年博士論文

【摘要】：隨著社會的發(fā)展,我國的冶金、消防、軍事等領(lǐng)域?qū)Ω魺崮突鸱雷o(hù)服的需求量越來越大,目前已有防護(hù)服還不具備使穿著者安全出入火場的防護(hù)能力。提高材料的隔熱阻燃性能,對開發(fā)具有高熱隔絕性能、耐明火性能,又具有高度靈活性和舒適性的熱防護(hù)服具有決定性作用。本課題以耐高溫芳砜綸(PSA)織物作為基材,采用晶體生長技術(shù)制備出PSA/SiO_2/Mg(OH)_2隔熱阻燃復(fù)合材料;采用氣凝膠技術(shù)分別制備了PSA/氫氧化鋁氣凝膠隔熱阻燃復(fù)合材料、PSA/二氧化硅-氫氧化鋁氣凝膠隔熱阻燃復(fù)合材料和PSA/氫氧化鎂鋁氣凝膠隔熱阻燃復(fù)合材料。與純PSA相比,其隔熱性能和阻燃性能均有顯著提高。具體研究內(nèi)容如下所述�；诰w生長技術(shù)制備了隔熱芳砜綸織物并對其性能進(jìn)行了研究。在經(jīng)SiO_2整理的芳砜綸上種植Mg(OH)_2晶種后進(jìn)行二次生長,制備出了具有隔熱阻燃性能的負(fù)載Mg(OH)_2和SiO_2的芳砜綸復(fù)合織物(PSA/SiO_2/Mg(OH)_2)。通過控制晶體生長時間、原料濃度、氧化硅粒徑大小及整理液濃度等條件,可在織物表面均勻地包覆不同形貌的Mg(OH)_2層,如倒伏片狀、豎立花瓣狀、蜂窩狀、致密排列的倒三角臺狀以及致密排列的倒三角錐、倒三角臺夾雜有棒狀等。Mg(OH)_2包覆于芳砜綸可使其初始分解溫度和最大熱失重分解溫度有著很大的提高,尤以蜂窩狀結(jié)構(gòu)包覆的芳砜綸的起始分解溫度最高可達(dá)451.6℃、最大熱失重分解溫度最高可達(dá)483.6℃。Mg(OH)_2包覆芳砜綸后可降低其導(dǎo)熱系數(shù)和垂直燃燒損毀長度,增強(qiáng)其隔熱性能和阻燃性能。Mg(OH)_2的形貌對復(fù)合材料的導(dǎo)熱系數(shù)有著極其重要的影響,通過TC-3000熱線法導(dǎo)熱系數(shù)儀于25℃測試導(dǎo)熱系數(shù)得Mg(OH)_2以致密排列的倒三角錐狀、倒三角臺狀并夾雜有棒狀的形貌包覆時導(dǎo)熱系數(shù)最低,僅為0.0553 W/(m·K),蜂窩狀形貌包覆時導(dǎo)熱系數(shù)可低至0.0559 W/(m·K),致密排列的倒三角臺形貌包覆時低至0.0568 W/(m·K),遠(yuǎn)低于芳砜綸原布的0.0975W/(m·K)。PSA/SiO_2/Mg(OH)_2復(fù)合材料具有優(yōu)異的阻燃性能,損毀長度為1.20 cm,屬于難燃材料。多孔結(jié)構(gòu)有利于提高材料的隔熱性能,為了進(jìn)一步提高芳砜綸織物的隔熱性能,采用溶膠-凝膠法和常壓干燥法制得了氫氧化鋁氣凝膠并將其成功地應(yīng)用到芳砜綸上。氫氧化鋁氣凝膠的孔結(jié)構(gòu)和表觀密度對其隔熱性能均有影響,孔容越大、表觀密度越低,復(fù)合材料的導(dǎo)熱系數(shù)越低、隔熱性能越好。通過改變反應(yīng)配比來調(diào)控氣凝膠的孔結(jié)構(gòu)和表觀密度,獲得了表觀密度為0.172~0.645 g/cm3、孔容為0.717~2.325 cm3/g、比表面積為292.703~408.696 m2/g、平均孔徑為10.9~21.8 nm的白色半透明塊狀氫氧化鋁氣凝膠,其為γ-Al OOH勃姆石晶體,空間網(wǎng)絡(luò)結(jié)構(gòu)由納米纖維狀顆粒相互交錯連接而成。采用溶膠-凝膠成型法和常壓干燥法制得了PSA/氫氧化鋁氣凝膠復(fù)合材料,通過TC-3000熱線法導(dǎo)熱系數(shù)儀于25℃測試導(dǎo)熱系數(shù)、垂直燃燒儀測試損毀長度表征了其隔熱阻燃性能,其與芳砜綸原織物相比,導(dǎo)熱系數(shù)從0.0975 W/(m·K)降到0.0599 W/(m·K),損毀長度從4.90 cm減少到1.25 cm,隔熱和阻燃性能得到顯著提高。為進(jìn)一步降低氫氧化鋁氣凝膠的表觀密度、增大其孔容,在其制備過程中加入正硅酸四乙酯(TEOS),獲得了表觀密度為0.140g/cm3,比表面積為366.686 m2/g,孔容為2.798 cm3/g,平均孔徑為28.3 nm的白色半透明塊狀二氧化硅-氫氧化鋁復(fù)合氣凝膠,其為γ-Al OOH勃姆石晶體與非晶態(tài)SiO_2的混合物,空間網(wǎng)絡(luò)結(jié)構(gòu)由納米葉片狀顆粒彼此相互交錯連接而成。采用溶膠-凝膠成型法和常壓干燥法成功地制得了PSA/二氧化硅-氫氧化鋁氣凝膠復(fù)合材料,通過TC-3000熱線法導(dǎo)熱系數(shù)儀于25℃測試導(dǎo)熱系數(shù)和垂直燃燒儀測試損毀長度表征了其隔熱阻燃性能,與芳砜綸原織物相比,其導(dǎo)熱系數(shù)從0.0975 W/(m·K)降到0.0581 W/(m·K),垂直燃燒損毀長度從4.90 cm減少到2.85 cm,隔熱和阻燃性能得到了較大提高。為進(jìn)一步提高氫氧化鋁氣凝膠的隔熱性能,采用溶膠-凝膠法和常壓干燥、真空干燥相結(jié)合的方法制得了白色氫氧化鎂鋁氣凝膠。通過改變反應(yīng)配比來調(diào)控氫氧化鎂鋁氣凝膠的物相組成、表觀密度和孔結(jié)構(gòu),獲得了表觀密度為0.108~0.689 g/cm3,孔容為0.655~2.430 cm3/g,比表面積為177.514~459.376 m2/g,平均孔徑為5.1~32.4 nm的具有不同物相組成的氫氧化鎂鋁氣凝膠。其空間網(wǎng)絡(luò)結(jié)構(gòu)由納米片狀顆粒相互交錯連接而成,或由片狀氫氧化鎂鋁相互交錯疊加構(gòu)成的球形花朵狀顆粒相互連接堆積而成。采用溶膠-凝膠成型法和常壓干燥、真空干燥相結(jié)合的方法成功地制得了PSA/氫氧化鎂鋁氣凝膠復(fù)合材料。通過TC-3000熱線法導(dǎo)熱系數(shù)儀于25℃測試導(dǎo)熱系數(shù)和垂直燃燒儀測試損毀長度表征了其隔熱阻燃性能,與芳砜綸原織物相比,其導(dǎo)熱系數(shù)從0.0975 W/(m·K)降到0.0532W/(m·K),垂直燃燒損毀長度從4.90 cm減少到2.10 cm,隔熱和阻燃性能都得到了顯著提高。對比PSA/SiO_2/Mg(OH)_2復(fù)合材料、PSA/氫氧化鋁氣凝膠復(fù)合材料、PSA/二氧化硅-氫氧化鋁氣凝膠復(fù)合材料、PSA/氫氧化鎂鋁氣凝膠復(fù)合材料的隔熱阻燃性能可知,PSA/氫氧化鎂鋁氣凝膠復(fù)合材料的隔熱性能最好,導(dǎo)熱系數(shù)可低至0.0532 W/(m·K);倒三角臺形貌Mg(OH)_2包覆的PSA/SiO_2/Mg(OH)_2復(fù)合材料的阻燃性能最好,垂直燃燒損毀長度可低至1.20 cm。本文的研究結(jié)果可為具有高隔熱性能和高耐火性能的熱防護(hù)紡織品的開發(fā)提供參考。
[Abstract]:With the development of society, the demand for heat insulation fire-resistant protective clothing is becoming more and more large in our metallurgical, fire, military and other fields. At present, the protective clothing has not been able to protect the wearer from the safety of the fire field. It improves the heat insulation and flame retardancy of the material, and has high thermal insulation and bright fire resistance, and has high flexibility and flexibility. The thermal protective clothing of comfort has a decisive effect. The heat resistant and Flame Retardant Composites of PSA/SiO_2/Mg (OH) _2 are prepared by crystal growth technology with high temperature resistant polysulfone (PSA) fabric as the substrate, and the heat insulation and Flame Retardant Composites of PSA/ hydrogel aerogel are prepared by aerogel technology, and the PSA/ silica - aluminum hydroxide gas condensate is prepared. The thermal insulation and flame retardancy of PSA/ magnesium hydroxide aluminum aerogel have been improved significantly compared with pure PSA. The specific research contents are as follows. The thermal insulation polysulfone fabric is prepared based on the crystal growth technology and its properties are studied. The SiO_2 finishing polysulfone fiber is used. After planting Mg (OH) _2 seeds for two times, the polysulfonamide composite fabric (PSA/SiO_2/Mg (OH) _2) with Mg (OH) _2 and SiO_2 with heat insulation and flame retardancy was prepared. By controlling the growth time of the crystal, the concentration of the raw material, the size of the silicon oxide particle and the concentration of the finishing liquid, the Mg (OH) layer with different morphologies could be coated evenly on the surface of the fabric. Such as lodging flake, petal shaped, honeycomb, dense arranged inverted triangulation and dense arranged inverted triangle cone,.Mg (OH) _2 coated with polysulfonamide in the inverted triangle can make the initial decomposition temperature and maximum thermal weight loss decomposition temperature be greatly improved, especially the initial decomposition temperature of the polysulfone coated by honeycomb structure. The maximum thermal loss decomposition temperature is up to 451.6 degrees C, the maximum thermal weight loss decomposition temperature can be up to 483.6.Mg (OH) _2 coated with polysulfone fiber. The thermal conductivity and the vertical combustion damage length can be reduced, and the thermal insulation and flame retardant properties of.Mg (OH) _2 have been greatly influenced by the thermal conductivity of the composites by the TC-3000 hot wire thermal conductivity meter. The thermal conductivity of Mg (OH) _2 is measured at 25 C, and the thermal conductivity is the lowest when the inverted triangulation and clad is clad with a rod like appearance, only 0.0553 W/ (M. K). The thermal conductivity of the honeycomb shape coating can be as low as 0.0559 W/ (M. K), and the dense arrangement of the inverted triangle is as low as 0.0568 W/ (m K), far below it. The 0.0975W/ (M. K).PSA/SiO_2/Mg (OH) _2 composite has excellent flame retardancy and the damage length is 1.20 cm, which is a refractory material. The porous structure helps to improve the insulation property of the material. In order to further improve the heat insulation property of the polysulfone fabric, the sol-gel method and the atmospheric drying method are used to obtain the aluminum hydroxide gas. The pore structure and apparent density of the aluminum hydroxide aerogels have influence on the thermal insulation properties of the hydrogel. The larger the pore volume, the lower the apparent density, the lower the thermal conductivity of the composite, the better the heat insulation performance. The apparent density is obtained by changing the reaction ratio to regulate the pore structure and apparent density of the aerogels. The degree is 0.172~0.645 g/cm3, Kong Rong is 0.717~2.325 cm3/g, the specific surface area is 292.703~408.696 m2/g, the average pore size is 10.9~21.8 nm, the white semitransparent massive aluminum hydroxide aerogel is the gamma -Al OOH boehmite crystal. The space network structure is interlaced with the nanofibrous particles. The sol-gel forming method and the atmospheric pressure dry method are used. The PSA/ aluminum hydroxide aerogel composite was obtained by dryness. The thermal conductivity was measured by the TC-3000 hot wire thermal conductivity meter at 25 C. The damage length of the vertical combustion instrument was tested for its thermal insulation and flame retardancy. Compared with the aramid fabric, the thermal conductivity decreased from 0.0975 W/ (M. K) to 0.0599 W/ (M. K), and the damage length was reduced from 4.90 cm to 1.25. Cm, in order to further reduce the apparent density of the aluminum hydroxide aerogel and increase its Kong Rong, four ethyl orthosilicate (TEOS) is added to the preparation process. The apparent density is 0.140g/cm3, the surface area is 366.686 m2/g, the Kong Rong is 2.798 cm3/g, and the average pore size is 28.3 nm white semitransparent block. The silica - aluminum hydroxide compound aerogel is a mixture of gamma -Al OOH boehmite crystal and amorphous SiO_2. The spatial network structure is interlaced with each other. The PSA/ two silicon oxide - aluminum hydroxide aerogel composite is successfully prepared by sol-gel method and atmospheric pressure drying method, through TC-3 The thermal conductivity of the 000 hot wire method was measured at 25 degrees centigrade thermal conductivity and the test damage length of the vertical combustion instrument. Compared with the aramid fabric, the thermal conductivity decreased from 0.0975 W/ (m K) to 0.0581 W/ (M. K), and the vertical combustion damage length decreased from 4.90 cm to 2.85 cm, and the heat insulation and flame retardant properties were greatly improved. In order to further improve the insulation performance of aluminum hydroxide aerogels, white magnesium aluminum hydroxide aerogels were prepared by combining sol-gel method with atmospheric pressure drying and vacuum drying. By changing the reaction ratio, the phase composition, apparent density and pore structure of magnesium hydroxide aerogels were controlled, and the apparent density of 0.108~0.689 g/ was obtained. Cm3, Kong Rong is a 0.655~2.430 cm3/g, with a specific surface area of 177.514~459.376 m2/g and an average pore size of 5.1~32.4 nm, with different phases of magnesium aluminum hydroxide. The spatial network structure is interlaced by interlaced nanometallic particles, or the spherical flower particles composed of flake magnesium aluminum phase interlaced and interlaced with each other. PSA/ magnesium aluminium aerogel composite was successfully prepared by combination of sol-gel forming method, atmospheric drying and vacuum drying. The thermal conductivity and damage length of vertical combustion apparatus were tested by TC-3000 hot wire thermal conductivity meter at 25 C. The thermal conductivity decreased from 0.0975 W/ (M. K) to 0.0532W/ (M. K), the vertical combustion damage length decreased from 4.90 cm to 2.10 cm, and the heat insulation and flame retardant properties were greatly improved. The heat insulation and flame retardancy of the magnesium aluminum aerogel composite can be found that the heat insulation performance of PSA/ mg Al aerogel composite material is the best, the thermal conductivity can be as low as 0.0532 W/ (M. K), and the Mg (OH) _2 coated PSA/SiO_2/Mg (OH) _2 composite with Mg (OH) _2 has the best flame retardancy and the vertical combustion damage length can be lower to 1.20 cm.. The results can provide references for the development of thermal protective textiles with high thermal insulation and high fire resistance.

【學(xué)位授予單位】：東華大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：TS106;TS941.731
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本文編號：1870455