本文選題：團粒法 + 固相��； 參考：《山西師范大學》2017年碩士論文

【摘要】：本文介紹了一種固相生長晶體的方法,包括直接固相法和間接固相法。該方法建立在化肥造粒的基礎上。主要使用團粒法造粒工藝,以腐植酸、蘑菇渣為原料,以石膏作粘結(jié)劑,加入其它所需的原料,在溶劑輔助的作用下,研磨并成粒。經(jīng)過一段時間的放置,晶體在顆粒表面長出。其中,腐植酸、蘑菇渣為晶體生長提供環(huán)境,石膏作為粘結(jié)劑將物料緊密團聚在一起,溶劑的揮發(fā)促進了晶體在固相中的生長,研磨過程輔助了固相中的物料之間發(fā)生物理或化學反應。首先,以腐植酸、蘑菇渣、磷酸二氫鈉、尿素、石膏為原料制得的化肥顆粒中,經(jīng)過放置生長出了無色針狀的尿素晶體,晶胞參數(shù)為a=5.6427?;b=5.6427?,c=4.7168?,α=90°,β=90°,γ=90°,分析了晶體在其中形成的原因,同時討論了水量和顆粒大小對晶體生長情況的影響。發(fā)現(xiàn)腐植酸、蘑菇渣作為生長環(huán)境,疏松多孔,為晶體生長提供了通道,而溶劑的揮發(fā)為晶體生長提供了牽引力,這些因素共同促進了晶體的生長。此外,當水量適當時,化肥顆粒的硬度較大,形狀較規(guī)則,生長出的晶體也較長。顆粒直徑在4-5 mm左右時,晶體生長的較好。其次,通過間接固相生長方法,以腐植酸、石膏、氟化銨、尿素為原料,在化肥造�；A上生長得到了硫酸銨晶體,其晶胞參數(shù)為a=7.7814?;b=5.9936?,c=10.6484?,α=90°,β=90°,γ=90°,并分析了硫酸銨晶體在固相中生成的原因及晶體的生長情況。發(fā)現(xiàn)硫酸銨晶體的形成是由于原料中的硫酸鈣和氟化銨發(fā)生了化學反應,生成了氟化鈣和硫酸銨。腐植酸的疏松結(jié)構(gòu)和硫酸鈣的堅固的棒狀結(jié)構(gòu)共同組成了蜂窩狀的通道結(jié)構(gòu),供晶體在其中生長。造粒的過程中,物料之間互相擠壓產(chǎn)生的機械壓力,成為晶體生長的驅(qū)動力。此外,在樣品袋中下層的固相環(huán)境較為穩(wěn)定,水分蒸發(fā)緩慢,因而得到的晶體的質(zhì)量較上層固相中的好。最后,在不直接提供尿素和氯化銨的情況下,以腐植酸、硫氰酸銨、硫酸銨、尿素、氯化鉀、磷酸一銨、石膏為原料,通過間接法固相生長,得到了針狀的尿素氯化銨晶體,其晶胞參數(shù)為a=7.9177?;b=17.1305?,c=8.0557?,α=90°,β=90°,γ=90°,并對其性質(zhì)進行了測定。由硫酸銨、硫氰酸銨等提供銨根離子,氯化鉀提供氯離子,與尿素分子作用共同形成了尿素氯化銨分子。發(fā)現(xiàn)當原料中硫氰酸銨與尿素的物質(zhì)的量比為1:5時,可以生長出尿素氯化銨單晶。總之,在團粒法造粒工藝的基礎上通過直接及間接固相生長得到了尿素晶體、硫酸銨晶體和尿素氯化銨晶體。分別探討了加入不同原料后晶體在其中形成的原因、過程以及部分條件對晶體生長情況的影響,分析了腐植酸、硫酸鈣在晶體生長中的重要性。通過對固相生長機理的探討,有利于進一步結(jié)合固相晶體生長技術(shù)生長其它晶體,同時完善該方法的理論體系。
[Abstract]:In this paper, a method of solid phase growth is introduced, including direct solid phase method and indirect solid phase method. The method is based on chemical fertilizer granulation. The granulation process was mainly used, with humic acid and mushroom dregs as raw materials, gypsum as binder, and other necessary raw materials added, which were ground and granulated with the help of solvent. After a period of time, the crystal grows on the surface of the particle. Among them, humic acid and mushroom dregs provide the environment for crystal growth, gypsum acts as binder to agglomerate materials closely, and the volatilization of solvent promotes the growth of crystals in solid phase. The grinding process assists in the physical or chemical reaction between the materials in the solid phase. Firstly, a colorless needle-like urea crystal was grown from fertilizer granules made from humic acid, mushroom dregs, sodium dihydrogen phosphate, urea and gypsum. The cell parameters of the crystal were as follows: a ~ (5.6427) B ~ (5. 6427) C ~ (4) 7168 ~ (8), 偽 ~ (90 擄), 尾 ~ (90) 擄, 緯 ~ (90) 擄. The reason of crystal formation was analyzed. The effects of water content and particle size on crystal growth were also discussed. It is found that humic acid and mushroom dregs as growth environment are porous and provide a channel for crystal growth, while volatilization of solvent provides tractive force for crystal growth. These factors promote crystal growth together. In addition, when the amount of water is appropriate, the hardness and shape of chemical fertilizer particles are larger, and the crystal is longer. When the particle diameter is about 4-5 mm, the crystal grows well. Secondly, ammonium sulfate crystals were obtained from humic acid, gypsum, ammonium fluoride and urea by indirect solid-phase growth on the basis of chemical fertilizer granulation. The cell parameters of the crystal are as follows: a 7.7814 ~ 5.9936 ~ (6) C ~ (10) ~ (6484), 偽 ~ (90 擄), 尾 ~ (90 擄) and 緯 ~ (90) 擄. The reasons for the formation of ammonium sulfate crystal in solid phase and the growth of the crystal are analyzed. It was found that the formation of ammonium sulfate crystal was due to the chemical reaction between calcium sulfate and ammonium fluoride, which resulted in the formation of calcium fluoride and ammonium sulfate. The loose structure of humic acid and the firm rod-like structure of calcium sulfate form honeycomb channel structure for crystal growth. In the process of granulation, the mechanical pressure produced by extrusion between materials becomes the driving force of crystal growth. In addition, the solid environment in the lower layer of the sample bag is stable and the evaporation of water is slow, so the quality of the crystals obtained is better than that in the upper solid phase. Finally, using humic acid, ammonium thiocyanate, ammonium sulfate, urea, potassium chloride, monoammonium phosphate and gypsum as raw materials, the needle-shaped urea ammonium chloride crystal was obtained by indirect solid-phase growth without directly supplying urea and ammonium chloride. The unit cell parameters are 7.9177B ~ (17. 1305) ~ 8.0557H, 偽 ~ (90 擄), 尾 ~ (90 擄) and 緯 ~ (90 擄), and its properties are determined. Ammonium sulfate, ammonium thiocyanate and potassium chloride provide ammonium radical ions, and potassium chloride provides chloride ions, which interact with urea molecules to form urea ammonium chloride molecules. It is found that when the ratio of ammonium thiocyanate to urea is 1:5, the urea ammonium chloride single crystal can be grown. In conclusion, urea crystal, ammonium sulfate crystal and urea ammonium chloride crystal were obtained by direct and indirect solid phase growth on the basis of granulation process. The reason and process of crystal formation and the influence of some conditions on crystal growth after adding different raw materials were discussed. The importance of humic acid and calcium sulfate in crystal growth was analyzed. By discussing the mechanism of solid phase growth, it is advantageous to further combine solid state crystal growth technology to grow other crystals, and to perfect the theoretical system of this method at the same time.
【學位授予單位】：山西師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O78

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