本文選題：濕法磷酸 + 萃取磷酸�。� 參考：《昆明理工大學(xué)》2015年碩士論文

【摘要】：磷酸作為磷化工生產(chǎn)過程中最為關(guān)鍵的中間體,是生產(chǎn)磷酸鹽、磷肥等的主要原料之一。隨著磷化工精細(xì)化的發(fā)展,各種級(jí)別的磷酸市場(chǎng)需求不斷加大,而近年來我國磷化工一直存在產(chǎn)能嚴(yán)重過剩、產(chǎn)品質(zhì)量低、結(jié)構(gòu)單一,精細(xì)化程度不夠,國際市場(chǎng)競(jìng)爭(zhēng)力不強(qiáng)的缺陷。為了實(shí)現(xiàn)磷化工行業(yè)的可持續(xù)發(fā)展,濕法磷酸凈化技術(shù)已成為研究的熱點(diǎn)。云天化國際三環(huán)分公司所生產(chǎn)濕法磷酸同樣存在雜質(zhì)多、P205含量較低的問題。目前三環(huán)分公司已與四川大學(xué)合作,通過預(yù)處理、溶劑萃取(磷酸三丁酯)、洗滌及反萃進(jìn)行凈化精制,精制生產(chǎn)的磷酸除氟外,其他指標(biāo)均能達(dá)到食品級(jí)質(zhì)量標(biāo)準(zhǔn),本文針對(duì)該現(xiàn)狀,以三環(huán)公司現(xiàn)有的濕法磷酸凈化后的萃取磷酸為原料,擬開展?jié)穹姿嵘疃让摲芯?欲使其達(dá)到食品級(jí)磷酸質(zhì)量標(biāo)準(zhǔn),即氟含量降到10mg/L (10ppm)以下。本文以脫氟率及P205收率為主要指標(biāo),應(yīng)用單因素實(shí)驗(yàn)與正交實(shí)驗(yàn)相結(jié)合的方法,分別探索了稀堿液洗滌、真空濃縮、氮?dú)馄崛N方法的脫氟效果。首先采用稀堿液洗滌萃取酸的有機(jī)相進(jìn)行脫氟,單因素實(shí)驗(yàn)得到的較優(yōu)化條件為：稀堿液濃度20%；稀堿液用量1.4%；稀堿液洗滌溫度45℃。隨后進(jìn)行正交實(shí)驗(yàn),得出較優(yōu)化的操作條件為稀堿液濃度20%,用量1.4%,洗滌溫度45℃,此時(shí)脫氟率達(dá)67.75%,有機(jī)相中P205收率達(dá)95.50%,經(jīng)蒸餾水反萃后磷酸中氟含量降至272ppm。說明單一的稀堿液洗滌磷酸脫氟效果還達(dá)不到食品級(jí)磷酸標(biāo)準(zhǔn)。然后對(duì)精制磷酸進(jìn)行真空濃縮脫氟實(shí)驗(yàn)研究。單因素實(shí)驗(yàn)得出的較優(yōu)化條件為：濃縮時(shí)間120min：脫氟劑添加量是磷酸中氟含量理論量的200%：濃縮溫度85℃。隨后進(jìn)行正交實(shí)驗(yàn),實(shí)驗(yàn)結(jié)果為濃縮時(shí)間120min,硅藻土用量是理論量的200%,濃縮溫度為90℃時(shí),脫氟率達(dá)到66.72%,氟含量降到160ppm左右,濃縮酸磷質(zhì)量濃度w(P205)達(dá)67.53%。說明真空濃縮脫氟效果也未達(dá)到食品級(jí)磷酸標(biāo)準(zhǔn)。再者采用氮?dú)馄崦摲鷮?shí)驗(yàn)研究,結(jié)果表明較優(yōu)化的工藝條件為：汽提時(shí)間120min、硅藻土添加量是磷酸中氟含量理論量的200%、汽提溫度900C、氮?dú)馔饬?.5-0.6L/min、攪拌速度300r/min。在較優(yōu)條件下,脫氟率可達(dá)85%以上,氟含量降到110ppm左右,濃縮酸磷質(zhì)量濃度w(P205)達(dá)70%左右。說明氮?dú)馄崦摲Ч晕催_(dá)到食品級(jí)磷酸標(biāo)準(zhǔn)。由以上三種單一方法脫氟,均未達(dá)到食品級(jí)磷酸標(biāo)準(zhǔn),是由于原料酸含有多種雜質(zhì)如鐵、鋁、鎂、硫酸根等離子,影響了氟在磷酸中的存在形式,使其存在形式多樣化,從而難以實(shí)現(xiàn)預(yù)計(jì)的脫氟目標(biāo)。鑒于此,最后設(shè)計(jì)將上述三種方法串聯(lián)集成,初步實(shí)驗(yàn)結(jié)果顯示氟含量可降至10ppm左右,汽提后磷酸中磷質(zhì)量濃度達(dá)到72%左右。該集成技術(shù)能有效脫除萃取磷酸中的氟,為濕法磷酸深度脫氟精制食品級(jí)磷酸提供了新的思路。本研究不僅有利于拓寬云天化生產(chǎn)工業(yè)磷酸的利用途徑,提高企業(yè)自身的經(jīng)濟(jì)效益和市場(chǎng)競(jìng)爭(zhēng)力,充分實(shí)現(xiàn)資源的有效利用,還可以為磷化工產(chǎn)品的精細(xì)化、專業(yè)化發(fā)展提供一定的技術(shù)支撐。
[Abstract]:Phosphoric acid is one of the most important intermediates in the process of phosphorous chemical production. It is one of the main raw materials for the production of phosphate and phosphate. With the development of fine phosphorus chemical industry, the demand of various levels of phosphoric acid is increasing. In recent years, there has been a lot of heavy production capacity, low product quality, single structure and insufficient fine degree in the phosphorus chemical industry in recent years. In order to realize the sustainable development of the phosphorous and chemical industry, the wet process phosphoric acid purification technology has become the hot spot of research. The wet process phosphoric acid produced by the international tricyclic company of Yunnan Tianhua has the same impurity and low P205 content. At present, the three ring branch company has been working with the Sichuan University by preprocessing and dissolving. The other indexes can reach the food grade quality standard. In this paper, the research on deep defluorination of wet process phosphoric acid is intended to be carried out to reach food grade phosphorus. The standard of acid quality, that is, the content of fluorine drops below 10mg/L (10ppm). In this paper, the defluorination effect of three methods, dilute alkaline solution, vacuum concentration and nitrogen stripping, is explored by the combination of single factor experiment and orthogonal experiment with the defluorination rate and the yield of P205 as the main index. The optimum conditions of fluorine were as follows: the concentration of dilute alkali solution was 20%, the dosage of dilute alkaline solution was 1.4%, the washing temperature of dilute alkaline solution was 45. Then orthogonal experiment was carried out. The optimum operating conditions were 20%, 1.4% and 45, the defluorination rate was 67.75%, the P205 yield of the organic phase was 95.50%, and the distilled water was reversed. The content of fluorine in the extracted phosphoric acid decreased to 272ppm., indicating that the defluorination effect of a single dilute lye washing phosphoric acid could not reach the standard of food grade phosphoric acid. Then, the experimental study on the defluorination of refined phosphoric acid was carried out in vacuum concentration. The optimum conditions of the single factor experiment were as follows: concentration time was 120min: the addition of defluorinated agent was 200% of the theoretical amount of fluorine content in phosphoric acid. The concentration temperature was 85. Then the experiment was carried out. The result was the concentration time 120min, the dosage of diatomite was 200% of the theoretical amount, the defluorination rate reached 66.72%, the fluorine content was about 66.72%, the fluorine content was reduced to about 160ppm, the concentration of concentrated acid phosphorus was w (P205) to 67.53%., indicating that the effect of true air concentration and defluorination did not reach the standard of food grade phosphoric acid. The experimental study of nitrogen stripping defluorination shows that the optimum technological conditions are as follows: the extraction time is 120min, the addition of diatomite is 200% of the theoretical amount of fluorine content in phosphoric acid, the stripping temperature is 900C, the nitrogen ventilation is 0.5-0.6L/min, and the rate of defluorination can reach more than 85%, and the content of fluorine drops to about 110ppm under the favorable conditions. The concentration of W (P205) is about 70%. It shows that the defluorination effect of nitrogen stripping has not reached the standard of food grade phosphoric acid. Defluorination by the above three single methods has not reached the standard of food grade phosphoric acid. It is because the raw acid contains a variety of impurities such as iron, aluminum, magnesium and sulfate, which affect the existence form of fluorine in phosphoric acid and make it form. It is difficult to achieve the expected defluorination target. In view of this, the three methods are integrated in series. The preliminary experimental results show that the fluorine content can be reduced to about 10ppm and the phosphorus concentration in the phosphoric acid is about 72% after stripping. The integrated technology can effectively remove fluorine in the extraction of phosphoric acid and refine the defluorination of the wet process phosphoric acid. Food grade phosphoric acid provides a new way of thinking. This study not only helps to widen the utilization of phosphoric acid in the industrial production, improve the economic and market competitiveness of enterprises, fully realize the effective utilization of resources, but also provide some technical support for the refined and specialized development of phosphorus chemical products.
【學(xué)位授予單位】：昆明理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ126.35

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本文編號(hào)：1967422