本文關(guān)鍵詞：二氧化鈦納米材料的制備及其對農(nóng)藥樂果的光催化性能研究　出處：《北京化工大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 鈦鐵礦 液相法 納米TiO_2 TiO_2/SBA-15 改性 光催化氧化 樂果

【摘要】：當(dāng)前水污染問題是一項非常復(fù)雜的系統(tǒng)工程,其中,農(nóng)藥廢水是水污染治理的具有挑戰(zhàn)性的課題之一,用于水處理的新材料和新技術(shù)的開發(fā)成為研究者們關(guān)注的焦點(diǎn)。光催化氧化技術(shù)作為一種新型的環(huán)境友好的技術(shù),在農(nóng)藥廢水處理領(lǐng)域具有良好的發(fā)展前景。光催化氧化技術(shù)降解農(nóng)藥的關(guān)鍵在于光催化劑的選擇以及催化劑的結(jié)構(gòu)和性能。Ti02納米材料因其氧化能力強(qiáng)、化學(xué)穩(wěn)定性和熱穩(wěn)定性良好、且不會造成二次污染,從而成為該領(lǐng)域的金牌催化材料。為此,本文以廉價且資源豐富的鈦鐵礦為原料,通過一系列單因素實驗制得Ti02催化劑,得到了優(yōu)化的制備條件。為了改善純Ti02催化劑分散性差和比表面積小等不足,將其負(fù)載到SBA-15分子篩上,從而提高催化劑比表面積。同時以農(nóng)藥樂果為目標(biāo)降解物,考察這兩種催化劑的光催化性能,研究其相互關(guān)系和影響規(guī)律。1.以四川攀枝花鈦鐵礦為原料,采用液相法硫酸酸解鈦鐵礦制得TiOSO4溶液,然后TiOSO4經(jīng)過水解制得不同晶型、不同形貌和不同顆粒大小的納米TiO2。深入考察了酸解過程中硫酸摩爾體積、反應(yīng)時間、反應(yīng)溫度和硫酸濃度對鈦鐵礦酸解率的影響和還原劑鐵粉的用量,并探討了水解過程中不同水解條件對產(chǎn)物結(jié)晶度、形貌、產(chǎn)率的影響以及不同煅燒溫度對Ti02晶型和粒徑的影響。結(jié)果表明,當(dāng)硫酸濃度為13.5 mol·L-1,硫酸摩爾體積為0.32 mol,反應(yīng)時間為120 min,反應(yīng)溫度為160℃時,鈦鐵礦酸解率高達(dá)95.21%,所得的鈦液中Ti4+濃度為121 g.L-1,鈦液穩(wěn)定性良好。在不同水解條件下制得不同形貌的TiO2產(chǎn)物,最高產(chǎn)率達(dá)到92.18%。在600℃-950℃溫度范圍下煅燒得到不同晶型(銳鈦礦型、金紅石型、銳鈦礦-金紅石混晶型)和不同顆粒大小的納米TiO2(40 nm-60 nm),TiO2產(chǎn)物純度高于99%。2.用前期制得的TiOSO4溶液作為前驅(qū)體和自制的SBA-15介孔分子篩作為載體,通過后合成水解法制備了含有不同TiO2負(fù)載量的TiO2/SBA-15催化劑。在模擬太陽光下,考察了催化劑煅燒溫度、溶液初始pH值、催化劑用量、不同TiO2負(fù)載量和不同反應(yīng)溫度對樂果降解的光催化活性的影響,并對所制得的TiO2/SBA-15催化劑的穩(wěn)定性進(jìn)行研究。此外,對光催化過程中產(chǎn)生的中間產(chǎn)物和光催化動力學(xué)規(guī)律也進(jìn)行了分析。研究結(jié)果表明,負(fù)載后的催化劑仍能保持SBA-15介孔分子篩穩(wěn)定有序的二維六方孔結(jié)構(gòu),且比表面積大,克服了常用光催化劑因比表面積小而導(dǎo)致光催化效率低的缺點(diǎn)。26%TiO2/SBA-15催化劑的比表面積為386m2·g-1,它對農(nóng)藥樂果的光催化活性最高,在7小時內(nèi)樂果可完全降解,該催化劑比純TiO2催化性能高約62%,且其穩(wěn)定性良好,使用4個循環(huán)后催化性能沒有明顯降低。分析結(jié)果表明,光催化降解農(nóng)藥樂果的反應(yīng)是一級反應(yīng)。
[Abstract]:At present, water pollution is a very complex systematic project. Pesticide wastewater is one of the challenging problems in water pollution control. The development of new materials and technologies for water treatment has become the focus of researchers. As a new and environmentally friendly technology, photocatalytic oxidation technology has a good prospect in the field of pesticide wastewater treatment. The key of photocatalytic oxidation technology to degrade pesticides is the selection of photocatalyst and the structure and performance of the catalyst. Ti02 nanomaterials, due to their strong oxidizing ability, good chemical stability and thermal stability, will not cause two pollution, thus becoming the gold catalytic material in this field. Therefore, in this paper, the Ti02 catalyst was prepared by a series of single factor experiments with the cheap and rich ilmenite as raw material, and the optimum preparation conditions were obtained. In order to improve the poor dispersivity and small specific surface area of the pure Ti02 catalyst, the catalyst was loaded onto the SBA-15 molecular sieve to improve the specific surface area of the catalyst. At the same time, the photocatalytic properties of the two catalysts were investigated with the pesticide dimethoate as the target, and the relationship and influence law of these catalysts were studied. 1. the TiOSO4 solution was prepared from sulfuric acid and Ilmenite from Sichuan Panzhihua ilmenite by liquid phase method. Then TiOSO4 was hydrolyzed to prepare nano TiO2 with different crystal forms, different morphologies and different particle sizes. An in-depth study of the acid hydrolysis process of sulfuric acid molar volume, reaction time, reaction temperature and concentration of sulfuric acid hydrolysis rate of ilmenite and iron reducing agent dosage, and discusses the different hydrolysis conditions during the hydrolysis effect of crystallinity, morphology and yield of product and the effect of different calcination temperature on Ti02 crystal type and particle size. The results show that when the concentration of sulfuric acid is 13.5 mol? L-1, the molar volume of sulfuric acid is 0.32 mol, the reaction time is 120 min, and the reaction temperature is 160 degrees, the dissolution rate of ilmenite is as high as 95.21%. The Ti4+ concentration in the titanium solution is 121 g.L-1, and the stability of titanium liquid is good. TiO2 products with different morphologies were prepared under different hydrolysis conditions, with the highest yield of 92.18%. Different crystalline forms (anatase, Jin Hongshi type, anatase, Jin Hongshi mixed crystal type) and nano TiO2 (40 nm-60 nm) with different particle sizes were obtained at calcination temperature of 600 -950, and the purity of TiO2 product was higher than 99%. 2., using TiOSO4 solution as precursor and homemade SBA-15 mesoporous molecular sieve as carrier, TiO2/SBA-15 catalyst containing different TiO2 loading was prepared by post synthesis hydrolysis method. Under the simulated sunlight, the effects of calcination temperature, initial pH value, amount of catalyst, TiO2 loading and reaction temperature on photocatalytic activity of dimethoate degradation were investigated, and the stability of the TiO2/SBA-15 catalyst was studied. In addition, the intermediate products and the regularities of photocatalytic kinetics produced during the photocatalytic process are also analyzed. The results show that the immobilized catalyst can keep SBA-15 mesoporous molecular sieve stable six dimensional pore structure and large specific surface area, to overcome the common photocatalyst surface area than the resulting photocatalytic efficiency low. The specific surface area of 26%TiO2/SBA-15 catalyst is 386m2. G-1. It has the highest photocatalytic activity for pesticide dimethoate. In 7 hours, dimethoate can be completely degraded. The catalytic performance of the catalyst is about 62% higher than that of pure TiO2, and its stability is good. After 4 cycles, the catalytic performance is not significantly reduced. The results show that the reaction of photocatalytic degradation of pesticide dimethoate is a first-order reaction.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X592;TQ426

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本文編號：1339144