CN105819469B - 一种利用高温催化氧化处理双甘膦废盐的方法 - Google Patents

一种利用高温催化氧化处理双甘膦废盐的方法 Download PDF

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CN105819469B
CN105819469B CN201610146553.7A CN201610146553A CN105819469B CN 105819469 B CN105819469 B CN 105819469B CN 201610146553 A CN201610146553 A CN 201610146553A CN 105819469 B CN105819469 B CN 105819469B
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金奎�
刘兴武
徐飞
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Anhui Huaxing Chemical Co Ltd
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Abstract

本发明公开了一种利用高温催化氧化处理双甘膦废盐的方法，涉及废盐处理技术领域，包括如下步骤：(1)除渣，(2)高温催化氧化，(3)除磷，(4)纯化。本发明利用双甘膦在230℃时开始熔融并分解，将盐渣置于热分解炉内，在高温条件下，双甘膦等有机物氧化分解，氮以气体形势挥发出去，达到与盐渣分离的目的；有机磷则在高温条件下转化成无机磷存在于固体盐中，将热分解后的盐用水溶解，然后用除磷剂其中的磷沉淀下来，经过滤和纯化得到符合要求的工业原料盐。

Description

一种利用高温催化氧化处理双甘膦废盐的方法
技术领域：
本发明涉及废盐处理技术领域，具体涉及一种利用高温催化氧化处理双甘膦废盐的方法。
背景技术：
生产农药时，通常会通过加入盐酸进行中和，中和后会产生大量的副产品废盐，其中氯化钠含量达到70％以上，同时含有大量的有机或无机杂质。双甘膦盐渣中除了含有大量氯化钠外，还含有少量的亚磷酸钠、双甘膦、甲醛等有害杂质，不能直接用作工业原料盐。为了降低对环境的污染，实现资源的合理回收利用，本公司开发出一种利用高温催化氧化处理双甘膦废盐的方法，通过高温催化氧化除去废盐中的有害物质，最终处理后得到的产物可直接用作工业原料盐。
发明内容：
本发明所要解决的技术问题在于提供一种处理效率高、成本低的利用高温催化氧化处理双甘膦废盐的方法。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种利用高温催化氧化处理双甘膦废盐的方法，包括如下步骤：
(1)除渣：将双甘膦废盐加入水中，浸泡24h后机械搅拌，待固体基本溶解完全后加入固体吸附剂，搅拌混合12h，过滤，滤液经浓缩成膏体后送入冷冻干燥机，所得固体再经粉碎机制成粗盐，然后将粗盐置于干燥环境下堆放24-48h，保持空气流通；
(2)高温催化氧化：向上述所得粗盐中加入催化剂，充分混合后置于分解炉中，先加热至100-110℃保温10-15min，再加热至230-240℃保温15-30min，然后继续加热至320-330℃保温30-45min；
(3)除磷：将上述经高温催化氧化后的粗盐加入水中，完全溶解后过滤，向滤液中加入除磷剂，搅拌3-5h后静置过夜，再次过滤，收集滤液；
(4)纯化：将上述所得滤液蒸发浓缩至含水量低于30％，然后置于0-5℃下自然析晶，最后离心过滤，即得工业原料盐。
所述固体吸附剂由如下重量百分比的原料组成：凹凸棒土30％、聚合氯化铁15％、明矾12％、聚合硅酸铝12％、活性炭10％、氢氧化镁8％、木质素磺酸钠8％、焦亚硫酸钠5％。
所述催化剂由重量百分比为80％主催化剂和20％助催化剂组成，主催化剂是以氧化铝为载体、五氧化二钒为活性组分在惰性环境中于120-130℃下研磨1h制成的，助催化剂选自硫酸钾和硫酸钠中的一种或混合物。
所述除磷剂由如下重量百分比的原料组成：石膏粉45％、聚合硫酸铝15％、聚丙烯酰胺12％、聚丙烯酸钠10％、柠檬酸钙8％、偏硅酸钙5％、尿素4％、硼砂1％。
本发明的有益效果是：本发明利用双甘膦在230℃时开始熔融并分解，将盐渣置于热分解炉内，在高温条件下，双甘膦等有机物氧化分解，氮以气体形势挥发出去，达到与盐渣分离的目的；有机磷则在高温条件下转化成无机磷存在于固体盐中，将热分解后的盐用水溶解，然后用除磷剂其中的磷沉淀下来，经过滤和纯化得到符合要求的工业原料盐。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
一种利用高温催化氧化处理双甘膦废盐的方法，包括如下步骤：
(1)除渣：将双甘膦废盐加入水中，浸泡24h后机械搅拌，待固体基本溶解完全后加入固体吸附剂，搅拌混合12h，过滤，滤液经浓缩成膏体后送入冷冻干燥机，所得固体再经粉碎机制成粗盐，然后将粗盐置于干燥环境下堆放24h，保持空气流通；
(2)高温催化氧化：向上述所得粗盐中加入催化剂，充分混合后置于分解炉中，先加热至100-110℃保温10min，再加热至230-240℃保温25min，然后继续加热至320-330℃保温30min；
(3)除磷：将上述经高温催化氧化后的粗盐加入水中，完全溶解后过滤，向滤液中加入除磷剂，搅拌3h后静置过夜，再次过滤，收集滤液；
(4)纯化：将上述所得滤液蒸发浓缩至含水量低于30％，然后置于0-5℃下自然析晶，最后离心过滤，即得工业原料盐。
固体吸附剂由如下重量百分比的原料组成：凹凸棒土30％、聚合氯化铁15％、明矾12％、聚合硅酸铝12％、活性炭10％、氢氧化镁8％、木质素磺酸钠8％、焦亚硫酸钠5％。
催化剂由重量百分比为80％主催化剂和20％助催化剂组成，主催化剂是以氧化铝为载体、五氧化二钒为活性组分在惰性环境中于120-130℃下研磨1h制成的，助催化剂选自硫酸钾和硫酸钠中的一种或混合物。
除磷剂由如下重量百分比的原料组成：石膏粉45％、聚合硫酸铝15％、聚丙烯酰胺12％、聚丙烯酸钠10％、柠檬酸钙8％、偏硅酸钙5％、尿素4％、硼砂1％。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (1)

1.一种利用高温催化氧化处理双甘膦废盐的方法，其特征在于，包括如下步骤：
(1) 除渣：将双甘膦废盐加入水中，浸泡24 h后机械搅拌，待固体溶解完全后加入固体吸附剂，搅拌混合12 h，过滤，滤液经浓缩成膏体后送入冷冻干燥机，所得固体再经粉碎机制成粗盐，然后将粗盐置于干燥环境下堆放24-48 h，保持空气流通；
(2) 高温催化氧化：向上述所得粗盐中加入催化剂，充分混合后置于分解炉中，先加热至100-110℃保温10-15 min，再加热至230-240℃保温15-30 min，然后继续加热至320-330℃保温30-45 min；
(3) 除磷：将上述经高温催化氧化后的粗盐加入水中，完全溶解后过滤，向滤液中加入除磷剂，搅拌3-5 h后静置过夜，再次过滤，收集滤液；
(4) 纯化：将上述所得滤液蒸发浓缩至含水量低于30%，然后置于0-5℃下自然析晶，最后离心过滤，即得工业原料盐；
所述固体吸附剂由如下重量百分比的原料组成：凹凸棒土 30%、聚合氯化铁 15%、明矾12%、聚合硅酸铝12%、活性炭 10%、氢氧化镁 8%、木质素磺酸钠 8%、焦亚硫酸钠 5%；
所述催化剂由重量百分比为80%主催化剂和 20%助催化剂组成，主催化剂是以氧化铝为载体、五氧化二钒为活性组分在惰性环境中于120-130℃下研磨1 h制成的，助催化剂选自硫酸钾和硫酸钠中的一种或其混合物；
所述除磷剂由如下重量百分比的原料组成：石膏粉 45%、聚合硫酸铝 15%、聚丙烯酰胺12%、聚丙烯酸钠 10%、柠檬酸钙 8%、偏硅酸钙 5%、尿素 4%、硼砂 1%。
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