發(fā)布時間：2018-04-21 03:33

  本文選題：嘧菌酯 + 噻蟲嗪　； 參考：《中國農(nóng)業(yè)大學(xué)》2016年博士論文

【摘要】：本論文通過利用x射線光電子能譜分析儀、傅里葉紅外線光譜分析儀、掃描電子顯微鏡、Zeta電位儀、差熱分析儀和流變儀等技術(shù)手段對25%嘧菌酯懸浮劑和21%噻蟲嗪懸浮劑進行了細致綜合的研究,為制備性能優(yōu)良的懸浮劑提供了依據(jù),其結(jié)論如下。對分散劑在嘧菌酯和噻蟲嗪顆粒表面的吸附機理進行了研究。在298K、308K和318K的實驗溫度下,分散劑在嘧菌酯和噻蟲嗪顆粒表面的吸附等溫線模型均符合Lamgmuir模型,吸附動力學(xué)模型均高度符合準二級動力學(xué)模型。分散劑在嘧菌酯和噻蟲嗪顆粒表面的熱力學(xué)參數(shù)結(jié)果顯示吸附均可自發(fā)進行,屬于物理吸附,吸附過程均為熵增過程。鈉離子濃度和pH均能影響分散劑在嘧菌酯和噻蟲嗪顆粒表面的吸附。傅里葉紅外光譜分析結(jié)果表明分散劑D-425,2700和2210與嘧菌酯之間、分散劑2700和2210與噻蟲嗪之間均以范德華力為主結(jié)合在原藥顆粒表面。Zeta電位結(jié)果顯示分散劑D-425、2700和2210在嘧菌酯懸浮液中的最佳含量點分別為2.5%,2.0%和3.0%;分散劑2700和2210在噻蟲嗪懸浮液中的最佳含量點均為3.0%。XPS結(jié)果顯示嘧菌酯和噻蟲嗪的C 1s和O 1s總峰在吸附分散劑后含量明顯提高。分散劑在嘧菌酯和噻蟲嗪顆粒表面的吸附層厚度隨著溫度的變化而變化,與吸附等溫線宏觀結(jié)果一致。在制作配方時,分散劑含量為最佳濃度時,吸附層厚度達到最大。熱重數(shù)據(jù)結(jié)果顯示分散劑/嘧菌酯體系在600℃以下為簡單一步分解,分散劑/噻蟲嗪體系在400℃以下為簡單兩步分解。通過FWO法分別對分散劑/嘧菌酯體系和分散劑/噻蟲嗪體系進行熱分解動力學(xué)研究,兩個體系下的分散劑最佳含量均與Zeta和XPS結(jié)果相符,且在常規(guī)分散劑推薦含量2-3%的范圍內(nèi),同一分散劑含量下不同轉(zhuǎn)化率α的擬合公式平行性良好,表明FWO法能在實際應(yīng)用中更好的指導(dǎo)分散劑在懸浮劑中含量的應(yīng)用。分散劑/嘧菌酯和分散劑/噻蟲嗪懸浮液的流變曲線均符合Hershel-Bulkley模型。在最佳分散劑用量時,體系的屈服值τH和黏度具有極小值,隨著分散劑含量的增加,稠度指數(shù)K逐漸增大,流動特性指數(shù)n逐漸減小。分散劑/嘧菌酯和分散劑/噻蟲嗪懸浮液體系的黏度均隨時間有周期性振蕩行為,在分散劑D-425、2700和2210最佳用量時,體系的振蕩振幅較小,比較集中,穩(wěn)定性較好。2700/噻蟲嗪懸浮劑體系,分散劑含量在0-1.5%之間的流變振蕩曲線剪切3min和10min有振幅,而當分散劑含量大于2%時振蕩幅度逐漸減小,高濃度時幾乎沒有。2210/噻蟲嗪懸浮劑體系振蕩振幅較小。在298K、308K和318K下,隨著溫度的升高,分散劑/嘧菌酯和分散劑/噻蟲嗪懸浮液體系的黏度逐漸降低；Hershel-Bulkley模型的三個代表參數(shù)屈服值τH、稠度指數(shù)k和流動特性指數(shù)n均隨溫度和pH的升高而變化;分散劑/嘧菌酯和分散劑/噻蟲嗪懸浮液體系的流變振蕩曲線的振蕩頻率和振幅均隨著實驗溫度的升高發(fā)生了較大變化,溫度越高振蕩振幅越大,振蕩曲線表現(xiàn)雜亂無序。利用精準量化的結(jié)果結(jié)合常規(guī)手段對懸浮劑的配方進行篩選,確定了在25%嘧菌酯懸浮劑中分散劑D-425、2700和2210的最佳用量分別為2.5%、2.0%和3.0%；在研發(fā)21%噻蟲嗪懸浮劑過程中,發(fā)現(xiàn)僅2210能制備合格的懸浮劑,其最佳用量為3.0%。本論文制備的25%嘧菌酯懸浮劑和21%噻蟲嗪懸浮劑理化性能指標良好,達到行業(yè)標準要求。
[Abstract]:By using X ray photoelectron spectroscopy analyzer, Fourier Infrared Spectroscopy Analyzer, scanning electron microscope, Zeta potentiometer, differential thermal analyzer and rheometer, the 25% thiazide suspension and 21% thiazimine suspension are studied in detail, which provides a basis for the preparation of excellent suspension agents. The adsorption mechanism of dispersant on the surface of azimetide and thiazimine particles was studied. At the temperature of 298K, 308K and 318K, the adsorption isotherm model of the dispersants on the surface of pyrazine and thiazimine particles conformed to the Lamgmuir model, and the average height of the adsorption kinetics model was in accordance with the quasi two stage kinetic model. The thermodynamic parameters of the surface of the ester and thiazimine particles show that the adsorption can be carried out spontaneously, which belongs to the physical adsorption, and the adsorption process is the entropy increase process. The concentration of sodium ion and pH can affect the adsorption of dispersants on the surface of pyrazine and thiazimine particles. The Fourier Infrared spectrum analysis indicates that the dispersant D-4252700 and 2210 are with pyrazine. Among the dispersants 2700 and 2210 and thiimazine, the optimal concentration of dispersant D-4252700 and 2210 in the suspension of azimthiazide was 2.5%, 2% and 3%, respectively, with the.Zeta potential on the surface of the particle on the particle surface of the original powder. The optimum content of dispersant 2700 and 2210 in the thiimazine suspension was 3.0%.XPS results. The total peak of C 1s and O 1s of azimetin and thiamazine increased obviously after the adsorption dispersant. The thickness of the adsorbed layer on the surface of the dispersant on the surface of pyrazine and thiazimine was changed with the temperature, which was in accordance with the macroscopical result of the adsorption isotherm. When the formulation was made, the thickness of the dispersant was the best. The thermal weight of the adsorbed layer was maximum. The data showed that the dispersant / pyrazine system was decomposed in a simple step below 600 C, and the dispersant / thiazine system was decomposed in a simple two step below 400 C. The thermal decomposition kinetics of dispersant / azoxpyrazine system and dispersant / thiazimine system were studied by FWO. The optimum content of dispersants under the two individual system were all with the content of the dispersant. The results of XPS are consistent, and in the range of recommended concentration of 2-3% for conventional dispersants, the fitting formula of different conversion rates under the same dispersant content is good, indicating that the FWO method can better guide the application of dispersant in the suspension agent in practical application. The rheological curves of dispersant / azoxpyrazine and dispersant / thiazine suspension are all in character. When the dosage of the best dispersant, the yield value H and viscosity of the system have minimal value. With the increase of the dispersant content, the consistency index K gradually increases and the flow characteristic index n gradually decreases. The viscosity of the dispersant / azoxpyrazine and the dispersant / thiazimine suspension system are all periodically oscillating with time, and dispersing with time. When the best dosage of agent D-4252700 and 2210, the oscillation amplitude of the system is smaller, more concentrated, the stability is better.2700/ thietazine suspension system, the rheological oscillation curve between 0-1.5% and 3min and 10min have amplitude, but when the dispersant content is more than 2%, the oscillation amplitude decreases gradually, and there is almost no.2210/ thiazine when the concentration is high. The oscillation amplitude of the suspension system is smaller. With the increase of temperature, the viscosity of the dispersant / azimetide / dispersant / thiimazine suspension system gradually decreases with the increase of 298K, 308K and 318K; the yield value H of the three representative parameters of the Hershel-Bulkley model, the consistency index K and the number n of the flow characteristics are all changed with the increase of temperature and pH; dispersant / azoxoxy. The oscillating frequency and amplitude of the rheological oscillation curve of the bacteria ester and the dispersant / thiazimine suspension system changed greatly with the increase of the experimental temperature. The higher the temperature, the greater the amplitude of the oscillation and the disorder of the oscillation curve. The formula of the suspension was screened by the result of precise quantification and the conventional means. The 25% azoxazin was determined. The optimum dosage of dispersant D-4252700 and 2210 was 2.5%, 2% and 3%, respectively. In the process of R & D 21% thiazimine suspension, only 2210 was found to be able to prepare qualified suspension agents. The optimum dosage was 3.0%., 25% azoxazin suspension and 21% thiazimine suspending agent had good physical and chemical properties, and reached the industry standard. Requirement.

【學(xué)位授予單位】：中國農(nóng)業(yè)大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2016
【分類號】：TQ450.1

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