發(fā)布時(shí)間：2018-07-26 16:27

【摘要】：木炭因其灰分低,孔隙率高,是工業(yè)硅生產(chǎn)的最佳碳質(zhì)還原劑。隨著森林資源的日益匱乏,人類環(huán)保意識(shí)的提高,導(dǎo)致木炭?jī)r(jià)格升高甚至木炭廠停產(chǎn),對(duì)工業(yè)硅生產(chǎn)造成嚴(yán)重影響。因此,尋找完全替代木炭的碳質(zhì)還原劑已刻不容緩。工業(yè)硅生產(chǎn)用碳質(zhì)還原劑具有以下要求：化學(xué)成分要求固定碳高、水分低、揮發(fā)分適中、灰分低(灰分含量5%,Fe含量0.2%)；具有一定的機(jī)械強(qiáng)度；粒度組成合適；電阻率高和化學(xué)反應(yīng)能力強(qiáng)。本論文以云南周邊地區(qū)的提供的煙煤和生產(chǎn)中由于運(yùn)輸、破碎、洗料等工藝產(chǎn)生的粉料(簡(jiǎn)稱粉料)為原料,兩者顆粒粒度小,制團(tuán)后方能入爐。冷壓成型后除化學(xué)成分外,其他性能通過生球抗壓強(qiáng)度、干球抗壓強(qiáng)度、抗碎率、熱強(qiáng)度和孔隙率來反映。煙煤灰分含量為16.09%,需要進(jìn)行預(yù)處理。粉料化學(xué)組成滿足工業(yè)硅生產(chǎn)的要求,不需進(jìn)行預(yù)處理。本論文首先研究了煙煤的預(yù)處理,并對(duì)工業(yè)硅生產(chǎn)用碳質(zhì)還原劑球團(tuán)的原料進(jìn)行選擇。煙煤預(yù)處理過程分為浮選和酸浸兩個(gè)階段,浮選最佳工藝參數(shù)如下：選用三粗兩精閉路實(shí)驗(yàn)流程,起泡劑松醇油用量為120g/t；捕收劑柴油用量為600g/t；抑制劑玻璃用量為2300g/t。經(jīng)浮選后,灰分含量為4.68%,Fe元素含量為0.32%,不能滿足工業(yè)硅生產(chǎn)對(duì)碳質(zhì)還原劑化學(xué)成分的要求,需對(duì)其進(jìn)一步脫灰除鐵。酸浸脫灰除鐵過程采用4mol/L鹽酸浸出,反應(yīng)溫度為60℃,浸出時(shí)間為60min,液固比為5：1,廢酸循環(huán)使用3次后,酸浸后的精煤灰分含量為3.89%,Fe含量為0.17%,滿足工業(yè)硅生產(chǎn)對(duì)碳質(zhì)還原劑化學(xué)成分的要求。將預(yù)處理后的煙煤或粉料作為球團(tuán)原料進(jìn)行冷壓制團(tuán),比較球團(tuán)性能,選用粉料作為工業(yè)硅生產(chǎn)用碳質(zhì)還原劑球團(tuán)的原料。其次,以R為粘結(jié)劑,研究了冷壓成型過程,最佳工藝參數(shù)如下：成型壓力為25MPa, NaOH溶液濃度為4.8mo1/L、含量取8.0%,微硅粉加入量為8.0%,洗精煤：石油焦：木炭為9.3：8.8：1(質(zhì)量一定),成型顆粒最大粒度范圍為3.3mm～4.75mm、比例占60%；R粘結(jié)劑含量為3.5%。在此條件下,所制備的球團(tuán)性能最佳,生球抗壓強(qiáng)度為698.0N,干球抗壓強(qiáng)度為6985.0N,抗碎率為93.68%,熱強(qiáng)度為55.25%,孔隙率為14.69%。生產(chǎn)結(jié)果表明：此球團(tuán)可以用于工業(yè)硅生產(chǎn),但爐況較差,球團(tuán)性能有待提高。本論文以此球團(tuán)性能為參考。再次,研究了以煤瀝青、NaHA(腐植酸鈉)、木質(zhì)素磺酸鈉、水玻璃以及淀粉類粘結(jié)劑(淀粉A、淀粉B、淀粉C與淀粉D)對(duì)球團(tuán)性能的影響,其中以淀粉D制備的球團(tuán)性能最佳,綜合考慮,其含量選用1.96%,此時(shí),生球抗壓強(qiáng)度為873.2N,干球抗壓強(qiáng)度為8091.4N,抗碎率為99.21%,熱強(qiáng)度為94.44%,孔隙率為5.86%。以上性能除孔隙率外其他性能均滿足生產(chǎn)要求,因此,在此基礎(chǔ)上,進(jìn)一步研究了非生物質(zhì)造孔劑空心微珠、氧化鈣和生物質(zhì)造孔劑稻殼、玉米秸稈、小麥秸稈、水稻秸稈與木屑對(duì)球團(tuán)性能的影響,結(jié)果表明,除空心微珠制備的球團(tuán)不能滿足工業(yè)硅生產(chǎn)要求外,以其他物質(zhì)為造孔劑制備的球團(tuán)性能均較好。當(dāng)選用水稻秸稈為造孔劑時(shí),最佳含量為2.5%時(shí),成型顆粒最大粒度為4.75mm,分布模數(shù)為0.5時(shí)球團(tuán)性能最佳,在此條件下,生球抗壓強(qiáng)度為4700.2N,干球抗壓強(qiáng)度為9536.1N,抗碎率為99.07%,熱強(qiáng)度為96.21%,孔隙率為30.78%,能滿足工業(yè)硅生產(chǎn)的要求。此外,研究了冷壓成型過程中含水率、潤濕介質(zhì)和粘結(jié)劑、造孔劑、成型壓力、物料粒度組成對(duì)球團(tuán)性能影響機(jī)理,得到以下結(jié)論：冷壓成型過程中,以NaOH溶液為潤濕介質(zhì)時(shí),NaOH與淀粉D反應(yīng)產(chǎn)生的新化學(xué)鍵對(duì)顆粒的結(jié)合能力提高。顆粒與粘結(jié)劑之間的結(jié)合力是機(jī)械結(jié)合力和物理化學(xué)結(jié)合力綜合作用的結(jié)果,其中,機(jī)械結(jié)合力的作用大于物理化學(xué)結(jié)合力的作用。水稻秸稈在球團(tuán)中提高孔隙率的主要是由于本身其密度小,外力消失后容易發(fā)生塑性形變等特性決定的；原料粒度組成符合GGS粒度特性方程時(shí),球團(tuán)性能最佳。最后將最佳工藝參數(shù)下制備的球團(tuán)投入25.5MVA半封閉旋轉(zhuǎn)礦熱爐中,通過工業(yè)化生產(chǎn)數(shù)據(jù)分析可知：該球團(tuán)能夠滿足工業(yè)硅生產(chǎn)的要求,最佳替代量為80%。
[Abstract]:Due to its low ash content and high porosity, charcoal is the best carbonaceous reducing agent in industrial silicon production. With the increasing shortage of forest resources and the improvement of human environmental awareness, the price of charcoal increased even in the charcoal plant, which has a serious effect on the industrial silicon production. Therefore, it is urgent to find a carbonaceous reducing agent to replace the charcoal. The carbon reducing agent for production has the following requirements: chemical composition requires high fixed carbon, low moisture, moderate volatilization, low ash content (ash content 5%, Fe content 0.2%), a certain mechanical strength, suitable size composition, high resistivity and chemical reaction ability. This paper is provided in the coal and production of the surrounding area of Yunnan because of the high resistivity and chemical reaction ability. In addition to chemical composition, other properties are reflected by the compressive strength of the raw ball, the compressive strength of the dry ball, the crushing rate, the heat strength and the porosity. The ash content of the bituminous coal is 16.09%, which needs to be pretreated. The chemical composition meets the requirements of industrial silicon production without preprocessing. In this paper, the pretreatment of bituminous coal was first studied, and the raw materials of carbon reduction agent pellets used in industrial silicon production were selected. The pretreatment process of bituminous coal was divided into two stages of flotation and acid leaching. The optimum flotation process parameters were as follows: the three coarse two finish closed circuit experiment process was selected. The amount of the defoaming agent is 120g/t, the amount of the collector diesel oil is 600g/t, the amount of the inhibitor glass is 2300g/t. after flotation, the ash content is 4.68%, the content of the Fe element is 0.32%. It can not meet the requirement of the chemical composition of the carbon reducing agent in the industrial silicon production. It needs further deashing and removing iron. The process of acid soot deashing and removing iron is 4mol/L hydrochloric acid. The leaching time is 60 C, the leaching time is 60min, the liquid and solid ratio is 5:1, the waste acid is recycled 3 times. The ash content of the refined coal after acid leaching is 3.89%, the content of Fe is 0.17%, which meets the requirement of the chemical composition of the carbonaceous reducing agent in the industrial silicon production. The powder is used as the raw material for the production of carbon reducing agent pellets for industrial silicon. Secondly, the cold press molding process is studied with R as a binder. The optimum process parameters are as follows: the molding pressure is 25MPa, the concentration of NaOH solution is 4.8mo1/L, the content is 8%, the micro silicon powder is added to 8%, the washed coal is coke: charcoal is 9.3:8.8:1 (quality certain), The maximum grain size range of the formed particles is 3.3mm to 4.75mm, and the proportion is 60%. Under the R binder content 3.5%., the pellet has the best performance, the ball compression strength is 698.0N, the dry ball compressive strength is 6985.0N, the crushing rate is 93.68%, the heat strength is 55.25%, and the porosity of 14.69%. production shows that this pellet can be used in industrial silicon. Production, but the condition of the furnace is poor, the performance of pellet needs to be improved. This paper takes this ball as a reference. Again, the effects of coal tar pitch, NaHA (humic acid sodium), sodium lignosulfonate, water glass and starch binder (starch A, starch B, starch C and starch D) on pellet performance are studied. The performance of pellets prepared by starch D is the best and comprehensive examination The content is 1.96%. At this time, the compressive strength of the ball is 873.2N, the compressive strength of the dry ball is 8091.4N, the crushing rate is 99.21%, the heat strength is 94.44%, the porosity is above 5.86%., and the other properties except the porosity are all satisfied with the production requirements. Therefore, on this basis, the hollow microspheres, calcium oxide and biological materials of non biomass pore making agents are studied on this basis. The effect of the porous rice husk, corn straw, wheat straw, rice straw and wood chips on the pellet performance was found. The results showed that the Pelletizing Properties of the pellets prepared by other substances except the hollow microspheres could not meet the industrial silicon production requirements. When the water rice straw was selected as the pore making agent, the optimum content was 2.5%. When the maximum particle size is 4.75mm and the distribution modulus is 0.5, the ball has the best performance. Under this condition, the compressive strength of the ball is 4700.2N, the compressive strength of the dry ball is 9536.1N, the crushing rate is 99.07%, the heat strength is 96.21%, the porosity is 30.78%, which can meet the requirements of the industrial silicon production. In addition, the water content, wetting medium and bond during the cold pressing process are studied. The influence mechanism of agent, pore forming agent, molding pressure and material size composition on pellet properties is obtained. The following conclusions are obtained: in the process of cold pressing, when the NaOH solution is the wetting medium, the new chemical bonds produced by the reaction of NaOH and starch D increase the binding capacity of the particles. The binding force between the particles and the binder is the mechanical binding force and the physical and chemical binding force. As a result of the comprehensive effect, the effect of mechanical binding force is greater than that of physical chemical binding force. The main reason for the increase of the porosity of rice straw in the pellet is due to its small density and the characteristics of plastic deformation after the external force is disappearing. When the particle size composition of the raw material is in line with the GGS particle size characteristic equation, the best performance of the pellets is the best. The pellets prepared under the best technological parameters are put into the 25.5MVA semi closed rotary mine hot stove. The analysis of industrial production data shows that the pellet can meet the requirements of industrial silicon production, and the optimum replacement amount is 80%..
【學(xué)位授予單位】：昆明理工大學(xué)
【學(xué)位級(jí)別】：博士
【學(xué)位授予年份】：2016
【分類號(hào)】：TN304.12

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