碱洗氧化工艺中杂质对硫酸钠结晶粒度的影响

doi:10.19964/j.issn.1006-4990.2021-0397

Abstract

Abstract:

Aiming at the evaporative crystallization of sodium sulfate in the desulfurization wastewater from alkaline washing oxidation process,an experimental device was designed and developed to investigate the influence of the impurities on the evaporative crystallization of sodium sulfate,mainly on the particle size of the sodium sulfate crystal,which include sodium carbonate,ferric ion and sodium sulfite in the wastewater.The results showed that 1.0% mass fraction of sodium carbonate in wastewater had no obvious influence on the particle size of sodium sulfate crystal.When iron existed in the form of precipitate,it was easy to cause sodium sulfate crystals to agglomerate and the particle size becomed smaller.When iron was existed in dissolved form,it had little effect on the particle size of sodium sulfate crystal.The existence of sodium sulfite was easy to reduce the particle size of sodium sulfate crystal.After eliminating sodium sulfite in wastewater by H₂O₂ oxidation,the crystal size of sodium sulfite was increased apparently.After the transformation of the industrial device,the average particle size of the anhydrous Na₂SO₄ product was increased from 106.71 μm to 129.99 μm.

Key words: impurity, anhydrous sodium sulfate, vaporation crystallization, rystal size

CLC Number:

TQ131.12

LIU Zhuang,AN Jimin,LI Yongjun,CHEN Xing,ZHAO Yigang,ZHAI Ruiguo. Effect of impurity in alkaline washing oxidation process on crystal size of sodium sulfate[J]. Inorganic Chemicals Industry, 2022, 54(4): 123-127.

Figures/Tables 12

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References 19

[1]	陆操, 程荫东. 无水硫酸钠生产、消费及对策[J]. 无机盐工业, 1992(3):14-17.
[2]	李淑萍. 大颗粒无水硫酸钠结晶工艺及数学模型研究[D]. 太原:华北工学院, 2001.
[3]	廖恩鑫, 陈丽芳, 张泽亚, 等. 硫酸钠与氯化钾制备硫酸钾实验研究[J]. 无机盐工业, 2020, 52(10):106-109.
[4]	谢明胜, 卫锋, 王爱广. 颗粒状无水硫酸钠的生产[J]. 无机盐工业, 2003, 35(6):30-31.
[5]	刘云琴. 元明粉结块原因及防止方法的探讨[J]. 无机盐工业, 2001, 33(2):28-29.
[6]	唐娜, 白丽荣, 沙作良, 等. 添加剂对硫酸钠晶体粒度的影响[J]. 盐业与化工, 2007, 36(6):1-3.
[7]	黄欣, 陈业钢, 苏楠楠, 等. 高盐废水分质结晶及资源化利用研究进展[J]. 化学工业与工程, 2019, 36(1):10-23.
[8]	裴旭东, 陈卫红, 李朝恒. 煤化工废水中硫酸钠-氯化钠-硝酸钠分离工艺研究[J]. 工业水处理, 2020, 40(1):63-66.
[9]	雷少成, 李玉林. DTNF膜对煤化工HERO高盐废水的分盐实验研究[J]. 无机盐工业, 2020, 52(9):84-87.
[10]	BHARMORIA P, GEHLOT P S, GUPTA H, et al. Temperaturedependent solubility transition of Na₂SO₄ in water and the effect of NaCl therein:solution structures and salt water dynamics[J]. Journal of Physical Chemistry B, 2014, 118(44):12734-12742. doi: 10.1021/jp507949h
[11]	张峰榛, 张孝果, 杨虎, 等. 硫酸钠废水真空蒸发结晶脱盐性能研究[J]. 天然气化工:C1化学与化工, 2019, 44(3):49-52.
[12]	许莉, 丁成荣. 铁离子杂质对过硫酸钠结晶过程的影响[J]. 精细化工, 2001, 18(9):547-549.
[13]	ZENG G, LI H, LUO S, et al. Effects of ultrasonic radiation on induction period and nucleation kinetics of sodium sulfate[J]. Korean Journal of Chemical Engineering, 2014, 31(5):807-811. doi: 10.1007/s11814-013-0290-6
[14]	SU N, WANG Y, YAN X, et al. Mechanism of influence of organic impurity on crystallization of sodium sulfate[J]. Industrial & Engineering Chemistry Research, 2018, 57(5):1705-1713. doi: 10.1021/acs.iecr.7b04625
[15]	曾桂生, 李慧, 王贤勇. 无水硫酸钠结晶热力学及介稳区宽度研究[J]. 南昌航空大学学报:自然科学版, 2012, 26(4):66-70.
[16]	丁爱娟. 亚熔盐法粉煤灰提铝清洁工艺硫行为研究[D]. 北京:北京化工大学, 2013.
[17]	侯长军, 霍丹群, 唐晓萍. 结晶添加剂对硫酸钾结晶过程影响研究[J]. 海湖盐与化工, 2002, 31(2):20-24.
[18]	丁绪淮, 谈遒. 工业结晶[M]. 北京: 化学工业出版社, 1985:74-132.
[19]	科尔索夫. 定量化学分析[M]. 南京化工学院分析化学教研组译. 北京: 人民教育出版社, 1981:234-235.

项目			w （Na₂SO₄）/ %	w （水不溶物）/%	w [钙和镁（以Mg计）]/ %	w [氯化物（以Cl 计）]/%	w [铁（Fe）]/%	w （水分）/ %	白度（R457）/ %	pH（50 g/L 水溶液, 25 ℃）	w （Na₂SO₃）/ %	w （Na₂CO₃）/ %
无水Na₂SO₄			86.3	0.08	—	0.03	0.035	0.57	65	8.6	11.5	0.6
指标	Ⅱ类	一等品	≥98.0	≤0.10	≤0.30	≤0.70	≤0.010	≤0.50	82	—
	Ⅱ类	合格品	≥97.0	≤0.20	≤0.40	≤0.90	≤0.040	≤1.0	—	—
	Ⅲ类	一等品	≥95.0	—	≤0.60	≤2.0	—	≤1.5	—	—
	Ⅲ类	合格品	≥92.0	—	—		—	—	—	—

杂质Fe含量/（mg·L^-1）	质量分数/%								平均粒径/ μm
杂质Fe含量/（mg·L^-1）	<75 μm	75~125 μm	125~150 μm	150~212 μm	212~300 μm	300~425 μm	425~600 μm	600~850 μm	平均粒径/ μm
0	2.32	5.98	6.39	13.11	25.11	27.98	19.01	0.10	303.23
11.1,无沉淀	3.78	8.54	7.01	12.76	21.33	29.56	17.02	0.00	291.68
20.0,有沉淀	7.21	11.57	12.05	13.56	18.87	34.43	2.31	0.00	240.34
50.0,有沉淀	8.11	11.72	13.25	12.27	17.89	35.44	1.32	0.00	236.22

杂质Fe含量/ （mg·L^-1）	白度（R457）/%	杂质Fe含量/ （mg·L^-1）	白度（R457）/%
0	90	20.0,有沉淀	74
11.1,无沉淀	82	50.0,有沉淀	68

组成	质量分数/%								平均粒径/ μm
组成	<75 μm	75~125 μm	125~150 μm	150~212 μm	212~300 μm	300~425 μm	425~600 μm	600~850 μm	平均粒径/ μm
Na₂SO₄ 20.0%	2.32	5.98	6.39	13.11	25.11	27.98	19.01	0.10	303.23
Na₂SO₄ 15.0%,Na₂SO₃ 5.0%	11.55	25.34	11.23	8.22	12.86	28.26	2.54	0.00	208.37
Na₂SO₄ 20.0%,Na₂SO₃ 5.0%	10.88	17.95	20.66	9.12	11.65	17.96	11.78	0.00	222.25

组成	晶体组分含量/%
组成	w（Na₂SO₄）	w（Na₂SO₃）
Na₂SO₄ 20%	100.0	0.0
Na₂SO₄ 15%,Na₂SO₃ 5%	76.1	23.9
Na₂SO₄ 20%,Na₂SO₃ 5%	80.3	19.8

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Inorganic Acid-Base-Salt Committee of CIESC

Effect of impurity in alkaline washing oxidation process on crystal size of sodium sulfate

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样品处理方式	质量分数/%								平均粒径/ μm
样品处理方式	<75 μm	75~125 μm	125~150 μm	150~212 μm	212~300 μm	300~425 μm	425~600 μm	600~850 μm	平均粒径/ μm
样品20.0%,无处理	23.65	24.56	26.32	11.89	8.91	4.65	0.02	0.00	130.91
过滤除铁沉淀	18.56	21.83	30.11	12.65	10.40	5.43	1.02	0.00	144.62
氧化Na₂SO₃	8.79	13.99	14.12	13.23	13.22	24.11	12.54	0.00	246.16

样品处理方式	晶体组分含量/%
样品处理方式	w （Na₂SO₄）	w （Na₂SO₃）	w [铁（Fe）]	白度（R457）/%
样品20.0%,无处理	85.2	10.8	0.031	67
过滤除铁沉淀	85.9	11.1	0.005	82
氧化Na₂SO₃	98.6	0.2	0.028	75

项目	w （Na₂SO₄）/%	w（水不溶物）/%	w[钙和镁（以Mg计）]/%	w[氯化物（以Cl计）]/%	w [铁（Fe）]/%	w （水分）/%	白度（R457）/%	pH（50 g/L水溶液,25℃）	w （Na₂SO₃）/%	w （Na₂CO₃） /%
改造前	86.3	0.08	—	0.03	0.035	0.57	65	8.6	11.5	0.6
改造后	98.4	0.09	—	0.03	0.005	0.42	82	7.5	0.5	0.4

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