非木材自苛化堿回收及黑液燃燒法除硅機(jī)理的研究
發(fā)布時(shí)間：2018-07-27 20:01
【摘要】：本論文針對(duì)非木材纖維原料制漿廠廣泛存在的“硅干擾”和白泥回收綜合利用問題,提出一種新的黑液燃燒法除硅技術(shù),并將其與黑液自苛化相結(jié)合,在黑液燃燒過程中完成黑液自苛化的同時(shí)降低黑液硅含量。從而為解決“硅干擾”問題、降低白泥產(chǎn)量提供理論依據(jù)。文章從以下幾個(gè)方面展開了研究:(1)竹漿黑液VIE值測(cè)定方法的研究通過響應(yīng)面優(yōu)化設(shè)計(jì),對(duì)竹漿黑液的固含量、加熱時(shí)間、加熱溫度和黑液添加量四個(gè)因素進(jìn)行優(yōu)化,獲得竹漿黑液VIE值測(cè)定最佳工藝條件,為堿回收黑液的燃燒提供合理的數(shù)據(jù)支撐。研究表明:通過響應(yīng)面設(shè)計(jì)得到黑液VIE值與黑液固含量(A)、加熱時(shí)間(B)、加熱溫度(C)、和黑液質(zhì)量(D)之間關(guān)系的二次回歸方程模型,且其合理性比較高。各因素對(duì)黑液VIE值顯著性影響的大小順序依次為:加熱溫度(C)加熱時(shí)間(B)固形物含量(A)黑液質(zhì)量(D)。進(jìn)而得出竹漿黑液VIE值測(cè)定的最佳參數(shù)為:固形物含量55wt.%,加熱時(shí)間40min,加熱溫度360℃,黑液添加量5g。(2)竹漿黑液流變性能的研究降低竹漿黑液黏度,改善其流變特性可以為優(yōu)化竹漿黑液堿回收系統(tǒng)各單元設(shè)計(jì)提供有效幫助。采用AR2000ex旋轉(zhuǎn)流變儀對(duì)不同濃度(50~78wt.%)的硫酸鹽竹漿黑液在不同溫度下的流變性能進(jìn)行分析。結(jié)果表明:硫酸鹽竹漿中高濃黑液在0.1~100s-1的剪切速率范圍內(nèi)近似于非牛頓流體,并產(chǎn)生剪切-稀化現(xiàn)象。在高溫、高固形物含量條件下,剪切-稀化的特性更加明顯。在較低溫度下,黑液體系所表現(xiàn)出的彈性模量和黏性模量相當(dāng)。當(dāng)固形物含量比較高時(shí),黑液體系的彈性固體特性比較明顯,此時(shí)當(dāng)外界受力不足以完全破壞其結(jié)構(gòu)時(shí),其回復(fù)的能力比較大,從而會(huì)產(chǎn)生增稠現(xiàn)象。此外,黑液在低剪切速率下黏度與剪切速率的關(guān)系呈現(xiàn)不規(guī)則變化,但在一定的剪切速率范圍內(nèi),黏彈性特征符合冪律區(qū)規(guī)律。(3)ICP法分析黑液無機(jī)元素含量文章提出一種采用ICP分析黑液中無機(jī)元素含量(Si、Mg、Al、Ca、B)的方法。該方法采用硝酸/過氧化氫(測(cè)硅時(shí)添加氫氟酸)消解體系對(duì)黑液樣品進(jìn)行預(yù)處理。黑液樣品的消解量為1g,硝酸和過氧化氫的添加量為:10:4,消解后所得樣品為無色透明試樣,滿足ICP測(cè)樣要求。且ICP法測(cè)定黑液體系中的硅、鋁、鈣、鎂等元素具有較好的準(zhǔn)確度和精度,實(shí)驗(yàn)所得相對(duì)標(biāo)準(zhǔn)偏差低于0.8%,回收率在98%~103%之間。(4)鎂鹽除硅劑除硅效果的研究分別采用氧化鎂和硫酸鎂作為燃燒法除硅劑添加到黑液當(dāng)中。實(shí)驗(yàn)所得氧化鎂的最大除硅率為33%。硫酸鎂除硅劑的添加量為2.0%時(shí),除硅率可以達(dá)到82%,反應(yīng)生成類似Mg2Al4Si5O18的沉淀物,該物質(zhì)的粒徑大約為21.20μm,比表面積為47.30 m2/g。黑液樣品的TG-FT-IR分析結(jié)果顯示,黑液樣品在210℃和840℃左右出現(xiàn)最大失重,最大失重處產(chǎn)生的主要熱解產(chǎn)物有CO2、CH4、H2O、醛酮類化合物和醇酚類化合物等。(5)自苛化協(xié)同黑液燃燒法除硅的研究分別對(duì)添加硼酸鈉苛化劑和同時(shí)添加硫酸鎂除硅劑和硼酸鈉苛化劑的黑液進(jìn)行了研究。結(jié)果發(fā)現(xiàn):硼酸鈉具有較好的自苛化效果,當(dāng)硼酸鈉添加量為15%,即B/Na比為0.2時(shí),自苛化率達(dá)到65%。硫酸鎂和硼酸鈉在黑液燃燒過程中具有協(xié)同效應(yīng),反應(yīng)所得綠液不溶物主要含有O、Mg、Al、Si、B、Ca等元素,其可能的化學(xué)組成有:Ca(Si2O5)、CaB2(SiO4)、Ca2B2O5等。
[Abstract]:Aiming at the problem of "Silicon Interference" and the comprehensive utilization of white mud recovery in the non wood fiber raw material pulping plant, a new black liquid combustion method is put forward to remove silicon from the black liquor and reduce the silicon content at the same time in the process of black liquor combustion. The theoretical basis of reducing the production of white mud is provided. The article has been studied in the following aspects: (1) the study on the VIE value determination method of the black liquor of bamboo pulp is optimized by the response surface optimization. The optimization of four factors, the solid content of the black liquor, the heating time, the heating temperature and the amount of the black liquor, is optimized, and the best process bar for the determination of the VIE value of the black liquor of bamboo pulp is obtained. It provides reasonable data support for the combustion of alkali recovery black liquor. The study shows that the two regression equation model of the relationship between black liquid VIE value and black liquid solid content (A), heating time (B), heating temperature (C) and black liquor mass (D) is designed by the response surface, and its rationality is higher. The size of the influence of each factor to the VIE value of black liquor is smooth. The order of the order is: heating time (C) heating time (B) solid content (A) black liquid mass (D). Then the optimum parameters for determining VIE value of black liquor of bamboo pulp are as follows: solid content 55wt.%, heating time 40min, heating temperature 360, 5G. (2) black liquor of black liquor, the viscosity of bamboo pulp black liquor can be reduced and its rheological properties can be improved. The AR2000ex rotating rheometer is used to analyze the rheological properties of the black liquor of different concentrations (50~78wt.%) at different temperatures. The results show that the high concentration black liquor in the sulphate bamboo pulp is similar to the non Newtonian fluid within the range of the shear rate of 0.1~ 100s-1. Under the conditions of high temperature and high solid content, the characteristics of shear thinning are more obvious. At lower temperatures, the elastic modulus and the viscosity modulus of the black liquor system are equal. When the solid content is high, the elastic solid characteristics of the black liquor system are more obvious, when the external stress is not enough to completely break. In addition, the relationship between viscosity and shear rate is irregular in the low shear rate, but in a certain range of shear rate, the viscoelastic characteristics conform to the law of power law. (3) a ICP method is used to analyze the content of inorganic elements in black liquid, and a kind of ICP is proposed. The method of analyzing the content of inorganic elements in black liquor (Si, Mg, Al, Ca, B). The method is pretreated with nitric acid / hydrogen peroxide (adding hydrofluoric acid) digestion system for black liquor samples. The elimination amount of black liquor samples is 1g, the amount of nitric acid and hydrogen peroxide is added as 10:4, and the samples are colorless transparent samples, which meet the requirements of ICP testing. The ICP method for the determination of silicon, aluminum, calcium and magnesium in the black liquor system has good accuracy and precision. The relative standard deviation of the experiment is less than 0.8% and the recovery rate is between 98%~103%. (4) the study on the effect of silicon removal by magnesium salt desilication agent is added to the black liquor by Magnesium Oxide and Magnesium Sulfate as the burning process desilication agent. The experimental Magnesium Oxide When the maximum removal rate of silicon removal is 2%, the addition of 33%. Magnesium Sulfate desilicon is 2%, the silicon removal rate can reach 82%, and the precipitate similar to Mg2Al4Si5O18 is generated. The particle size of the substance is about 21.20 mu m, and the TG-FT-IR analysis results of the specific surface area of 47.30 m2/g. black liquor show that the maximum weight loss of the black liquor samples around 210 and 840 centigrade, the maximum The main pyrolysis products produced by the weightlessness are CO2, CH4, H2O, aldehydes and ketones and alcohols and other compounds. (5) the study on the addition of sodium borate caustic and the addition of the Magnesium Sulfate and sodium borate caustic agent by the self caustic synergistic black liquor combustion method has been studied. The results show that sodium borate has good self causation. When the addition amount of sodium borate is 15%, that is, when the B/Na ratio is 0.2, the self caustic rate reaches 65%. Magnesium Sulfate and sodium borate in the black liquor combustion process, and the green liquid insoluble compounds mainly contain O, Mg, Al, Si, B, Ca and so on. The possible chemical compositions are Ca (Si2O5), CaB2 (SiO4), etc.
【學(xué)位授予單位】：陜西科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X793
本文編號(hào)：2148973
[Abstract]:Aiming at the problem of "Silicon Interference" and the comprehensive utilization of white mud recovery in the non wood fiber raw material pulping plant, a new black liquid combustion method is put forward to remove silicon from the black liquor and reduce the silicon content at the same time in the process of black liquor combustion. The theoretical basis of reducing the production of white mud is provided. The article has been studied in the following aspects: (1) the study on the VIE value determination method of the black liquor of bamboo pulp is optimized by the response surface optimization. The optimization of four factors, the solid content of the black liquor, the heating time, the heating temperature and the amount of the black liquor, is optimized, and the best process bar for the determination of the VIE value of the black liquor of bamboo pulp is obtained. It provides reasonable data support for the combustion of alkali recovery black liquor. The study shows that the two regression equation model of the relationship between black liquid VIE value and black liquid solid content (A), heating time (B), heating temperature (C) and black liquor mass (D) is designed by the response surface, and its rationality is higher. The size of the influence of each factor to the VIE value of black liquor is smooth. The order of the order is: heating time (C) heating time (B) solid content (A) black liquid mass (D). Then the optimum parameters for determining VIE value of black liquor of bamboo pulp are as follows: solid content 55wt.%, heating time 40min, heating temperature 360, 5G. (2) black liquor of black liquor, the viscosity of bamboo pulp black liquor can be reduced and its rheological properties can be improved. The AR2000ex rotating rheometer is used to analyze the rheological properties of the black liquor of different concentrations (50~78wt.%) at different temperatures. The results show that the high concentration black liquor in the sulphate bamboo pulp is similar to the non Newtonian fluid within the range of the shear rate of 0.1~ 100s-1. Under the conditions of high temperature and high solid content, the characteristics of shear thinning are more obvious. At lower temperatures, the elastic modulus and the viscosity modulus of the black liquor system are equal. When the solid content is high, the elastic solid characteristics of the black liquor system are more obvious, when the external stress is not enough to completely break. In addition, the relationship between viscosity and shear rate is irregular in the low shear rate, but in a certain range of shear rate, the viscoelastic characteristics conform to the law of power law. (3) a ICP method is used to analyze the content of inorganic elements in black liquid, and a kind of ICP is proposed. The method of analyzing the content of inorganic elements in black liquor (Si, Mg, Al, Ca, B). The method is pretreated with nitric acid / hydrogen peroxide (adding hydrofluoric acid) digestion system for black liquor samples. The elimination amount of black liquor samples is 1g, the amount of nitric acid and hydrogen peroxide is added as 10:4, and the samples are colorless transparent samples, which meet the requirements of ICP testing. The ICP method for the determination of silicon, aluminum, calcium and magnesium in the black liquor system has good accuracy and precision. The relative standard deviation of the experiment is less than 0.8% and the recovery rate is between 98%~103%. (4) the study on the effect of silicon removal by magnesium salt desilication agent is added to the black liquor by Magnesium Oxide and Magnesium Sulfate as the burning process desilication agent. The experimental Magnesium Oxide When the maximum removal rate of silicon removal is 2%, the addition of 33%. Magnesium Sulfate desilicon is 2%, the silicon removal rate can reach 82%, and the precipitate similar to Mg2Al4Si5O18 is generated. The particle size of the substance is about 21.20 mu m, and the TG-FT-IR analysis results of the specific surface area of 47.30 m2/g. black liquor show that the maximum weight loss of the black liquor samples around 210 and 840 centigrade, the maximum The main pyrolysis products produced by the weightlessness are CO2, CH4, H2O, aldehydes and ketones and alcohols and other compounds. (5) the study on the addition of sodium borate caustic and the addition of the Magnesium Sulfate and sodium borate caustic agent by the self caustic synergistic black liquor combustion method has been studied. The results show that sodium borate has good self causation. When the addition amount of sodium borate is 15%, that is, when the B/Na ratio is 0.2, the self caustic rate reaches 65%. Magnesium Sulfate and sodium borate in the black liquor combustion process, and the green liquid insoluble compounds mainly contain O, Mg, Al, Si, B, Ca and so on. The possible chemical compositions are Ca (Si2O5), CaB2 (SiO4), etc.
【學(xué)位授予單位】：陜西科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：X793
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