Microwave-assisted removal of chlorine from mercaptan methyl tin waste stock

doi:10.16085/j.issn.1000-6613.2018-2421

Abstract

Abstract:

The mercaptan methyl tin waste stock was used as research object. Based on the element composition, XRD analysis and the feature of physical properties of the waste base, the study designed a basic idea that microwave-assisted dry distillation recovery of low-boiling substances from the waste stock was adopted and dechlorinated residue was taken as the tin smelting concentrate. The experimental results showed that dry distillation can recycle about 15.86% of low boiling matter and remove about 31.06% of chlorine. We systematically studied the effect of liquid-solid ratio of residue to hydrogen peroxide, oxidation standing time of hydrogen peroxide,liquid-solid ratio of residue to concentrated sulfuric acid and microwave hardening time on the removal ratios of chlorine. With liquid-solid ratio of hydrogen peroxide being 1∶5, oxidation standing time of hydrogen peroxide being 30min, liquid-solid ratio of residue to concentrated sulfuric being 1∶3 and microwave hardening time being 80min, the chlorine content in the residue was 0.59% and the chlorine removal rate could reach 97.48%, which meet the requirements of the enterprise tin smelting concentrate chlorine content less than 0.8%. Meanwhile, the mechanism of microwave leaching and characterization of residue by XRD and SEM were discussed, after which the dechlorination process of dry distillation residue was analyzed. This provided the theoretical basis for industrial removal of chlorine from mercaptan methyl tin waste stock. In addition, the research results had better application prospect.

Key words: mercaptan methyl tin waste stock, microwave assisted, dry distillation, dechlorination

摘要：

以硫醇甲基锡废底料为研究对象，通过元素组成和XRD分析，结合废底料物性特征，设计了微波辅助干馏回收低沸点物质，残渣脱氯后用作锡冶炼精料的基本构思。实验研究表明：干馏可回收质量分数约15.86%的低沸点物质，同时可脱除约31.06%的氯。以残渣中氯含量为考察指标，系统研究了残渣与过氧化氢液固比、氧化静置时间、残渣与浓硫酸液固比、微波强化时间对氯脱除率的影响，结果表明：过氧化氢与残渣液固比为1∶5、氧化静置时间为30min、浓硫酸与残渣液固比为1∶3、微波强化时间为80min时，残渣中氯质量分数为0.59%，氯的脱除率可达到97.48%，满足企业锡冶炼精料氯质量分数＜0.8%要求。通过对微波浸取机制讨论以及残渣XRD、SEM的表征，初步对干馏残渣脱氯过程进行了机理分析，为硫醇甲基锡废底料中氯的脱除提供了理论依据，研究成果具有较好的应用前景。

关键词: 硫醇甲基锡废底料, 微波辅助, 干馏, 脱氯

CLC Number:

X756

Guangya ZHENG, Jupei XIA, Yin LI, Zhengjie CHEN, Chenglong LIU. Microwave-assisted removal of chlorine from mercaptan methyl tin waste stock[J]. Chemical Industry and Engineering Progress, 2019, 38(07): 3443-3449.

郑光亚, 夏举佩, 李银, 陈正杰, 刘成龙. 基于微波辅助脱除硫醇甲基锡废底料中的氯[J]. 化工进展, 2019, 38(07): 3443-3449.

Figures/Tables 12

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组成元素	质量分数/%
Sn	58.36
Cl	28.78
S	6.32
O	3.02
C	1.21
H	0.75
N	0.68

组成元素	质量分数/%
Sn	58.36
Cl	28.78
S	6.32
O	3.02
C	1.21
H	0.75
N	0.68

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