医药废硫酸钠盐燃烧特性及低温炭化除杂研究

doi:10.19964/j.issn.1006-4990.2020-0604

摘要/Abstract

摘要：

使用低温炭化-高温活化两步工艺处理典型的医药废盐,成功回收了无机盐和活性炭材料。低温炭化阶段将废盐中的有机物转变为不溶性残余炭渣,通过简单的溶解、过滤即可实现无机盐与有机物的分离;残余炭渣作为炭前体经过活化可得到活性炭材料。使用原子荧光光谱法、气相色谱-质谱联用法对废盐成分进行分析,采用Friedman法和Starink法计算废盐焚烧的活化能,通过管式炉模拟试验对废盐低温炭化条件进行优化,最后采用氢氧化钾浸渍法活化残余炭渣以制备活性炭。结果表明,废盐中溶解性有机碳在空气气氛、350 ℃、60 min条件下去除率达到99.98%,得到的无机盐产品符合GB/T 6009—2014《工业无水硫酸钠》Ⅲ类要求。残余炭渣经活化所得活性炭对亚甲基蓝的吸附容量达到762.86 mg/g。

关键词: 医药废盐, 热重分析, 低温炭化, 残余炭渣, 资源化

Abstract:

A two-step process of low temperature carbonization and high temperature activation was used to treat typical medical waste salt,and inorganic salt and activated carbon materials were recovered successfully.The organic matter in the waste salt was converted into insoluble residual carbon slag in low temperature carbonization section,which could be separated from inorganic salts by simple dissolution and filtration.Activated carbon material could be obtained by activating residual carbon residue as carbon precursor.The components of waste salt were analyzed by atomic fluorescence spectrometry and gas chroma-tography mass spectrometry.The activation energy of waste salt incineration was calculated by Friedman method and Starink method.The carbonization conditions of waste salt at low temperature were optimized by pipe furnace simulation test.The carbon residues were KOH impregnation method to prepare activated carbon.The results showed that the removal rate of dissolved organic carbon in the waste salt reached 99.98% under the conditions of air atmosphere,350 ℃ and 60 min,and the obtained inorganic salt products met the requirements of GB/T 6009—2014“Industrial anhydrate Sodium Sulfate” class Ⅲ.The adsorption capacity of activated carbon for methylene blue reached 762.86 mg/g.

Key words: pharmaceutical waste salt, thermal treatment, low-temperature carbonization, carbon residues, recovery

中图分类号:

X787

杨文振,熊萍,孙秀云,韩卫清. 医药废硫酸钠盐燃烧特性及低温炭化除杂研究[J]. 无机盐工业, 2021, 53(9): 76-82.

Yang Wenzhen,Xiong Ping,Sun Xiuyun,Han Weiqing. Study on combustion characteristics of waste pharmaceutical Na₂SO₄ and impurity removal by low-temperature carbonization[J]. Inorganic Chemicals Industry, 2021, 53(9): 76-82.

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工业分析（收到基）				元素分析（冷冻干燥基）
w（灰分）	w（挥发分）	w（固定碳）	w（水分）	w（C）	w（H）	w（O）	w（N）	w（S）
79.11	17.78	0.65	2.46	4.13	1.37	45.39	4.25	14.42

保留时间/min	名称	峰面积分数/%	沸点/℃
6.4	二甲基甲酰胺	10.56	153
10.2	氨基甲酸甲酯	6.01	177
10.4	N-甲基甲酰胺	12.14	199
15.5	甲酰基三甲基脲	8.75	—
18.6	2,6-二甲氧基-4-氟嘧啶	8.00	100
18.9	—^①	8.14	—
19.2	1,1-二甲基脲	8.47	163
21.2	1,2-二甲基咪唑烷-2,4,5-三酮	10.58	—
23.2	1,3-二甲基脲	27.36	270

α	Friedman法		Starink法
α	E/（kJ·mol^-1）	R²	E/（kJ·mol^-1）	R²
0.05	94.88	0.962	97.05	0.937
0.10	91.03	0.959	95.10	0.954
0.15	88.08	0.960	93.01	0.959
0.20	87.39	0.964	91.46	0.961
0.25	89.26	0.971	90.63	0.964
0.30	94.25	0.977	91.05	0.967
0.35	102.98	0.979	92.88	0.970
0.40	113.15	0.977	97.21	0.971
0.45	114.92	0.980	102.41	0.971
0.50	111.98	0.979	105.81	0.973
0.55	111.47	0.982	107.58	0.975
0.60	116.51	0.995	109.21	0.981
0.65	136.50	0.995	116.40	0.987
0.70	178.38	0.992	138.10	0.988
0.75	252.99	0.984	205.57	0.983
0.80	601.08	0.635	794.17	0.527
0.85	161.57	0.973	186.79	0.983
0.90	107.92	0.931	143.39	0.978

处理时间/min	DOC含量/（mg·g^-1）	处理时间/min	DOC含量/（mg·g^-1）
30	1.39	90	0.85
45	1.29	120	0.77
60	0.87

	项目		w（Na₂SO₄）/%	w（水分）/%	w（水不溶物）/%	w（钙镁）/%	w（氯）/%
国标	Ⅰ类	优级品	≥99.6	≤0.05	≤0.005	—	≤0.05
	Ⅰ类	一等品	≥99.0	≤0.50	≤0.05	≤0.15	≤0.35
	Ⅱ类	一等品	≥98.0	≤0.80	≤0.10	≤0.30	≤0.70
	Ⅱ类	合格品	≥97.0	≤3.00	≤0.20	≤0.40	≤0.90
	Ⅲ类	一等品	≥95.0	≤3.50	—	≤0.6	≤2.0
	Ⅲ类	合格品	≥93.3	—	—	—	—
回收无机盐			96.57	0.03	未检出	0.21	3.19

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