CN111389353A - 一种添加k助剂的ph3防护材料及其制备方法 - Google Patents

一种添加k助剂的ph3防护材料及其制备方法 Download PDF

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CN111389353A
CN111389353A CN202010142860.4A CN202010142860A CN111389353A CN 111389353 A CN111389353 A CN 111389353A CN 202010142860 A CN202010142860 A CN 202010142860A CN 111389353 A CN111389353 A CN 111389353A
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安丽花
裴佩
郭军军
王德周
金彦任
张金凤
宋雯
邢浩洋
温宇慧
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Shanxi Xinhua Chemical Industry Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0218—Compounds of Cr, Mo, W
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0233—Compounds of Cu, Ag, Au
    • B01J20/0237—Compounds of Cu
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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    • B01J20/0244—Compounds of Zn
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/354—After-treatment

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Abstract

本发明公开了一种添加K助剂的PH3防护材料的制备方法：称取椰壳破碎活性炭，采用等量浸渍法，按照该活性炭的水容量的90%量取氨水，剩余10%量取去离子水；称取碳酸氢铵、碱式碳酸铜、钼酸铵、碱式碳酸锌、K化合物；将量好的氨水和去离子水混合均匀加热至40～80℃，依次加入称好的活性组分，搅拌至充分溶解后配置成浸渍液；将配置好的浸渍液均匀倒入活性炭载体上，并不断搅拌，待充分浸渍后，将混合料装入密封袋内，静置1～4h后于120～190℃温度下烘干，烘干时间20～40min。本发明制备的PH3防护材料，经批量制备验证工艺可行，经动力管检测对PH3的防护性能较优。

Description

一种添加K助剂的PH3防护材料及其制备方法
技术领域
本发明涉及防护材料技术领域，具体为一种添加K助剂的PH3防护材料及其制备方法。
背景技术
PH3是一种无色、高毒、易燃的气体，微溶于水，易溶于乙醇。它常用于粮食熏蒸杀虫，主要经呼吸道吸入人体，暴露在空气中能自燃，与空气混合物爆炸的下限为26g/m3，具有强还原性，吸入高浓度的PH3会对人体的神经系统、呼吸系统以及肝脏、心脏造成很大伤害。
对PH3的防护主要是使用负载有Cu、Cr、Ag的ASC惠特莱特炭，该浸渍炭对PH3具有较好的防护效果。装有ASC浸渍炭的P-B-3中型滤毒罐在30L/min的流量，磷化氢浓度1000mg/m3，透过浓度为0.3mg/m3，相对湿度50%的条件下，防护时间达到200min。但由于负载的Cr有致癌作用，会对人体造成很大的伤害。
发明内容
本发明目的是提供一种PH3气体的防护材料及其制备方法，不仅对PH3具有较好的防护作用，而且制备过程中不负载Cr化合物，不会对人体造成伤害。
本发明是采用如下技术方案实现的：
一种添加K助剂的PH3防护材料，以椰壳活性炭作为载体材料，采用等量浸渍法负载1%～7%（重量）的碳酸氢铵、1%～20%（重量）的碱式碳酸铜、1%～10%（重量）的钼酸铵、1%～10%（重量）的碱式碳酸锌，还负载1%～10%（重量）的K化合物作为活性组分助剂，余量为活性炭。
优选的，负载5%～7%（重量）的碳酸氢铵、15%～20%（重量）的碱式碳酸铜、1%～6%（重量）的钼酸铵、1%～2%（重量）的碱式碳酸锌、2%～10%（重量）的K化合物。
优选的，所述K化合物采用碳酸钾或者氯化钾。
上述添加K助剂的PH3防护材料的制备方法：称取椰壳破碎活性炭，采用等量浸渍法，按照该活性炭的水容量的90%量取氨水，剩余10%量取去离子水；称取碳酸氢铵、碱式碳酸铜、钼酸铵、碱式碳酸锌、K化合物；将量好的氨水和去离子水混合均匀加热至40～80℃，依次加入称好的活性组分，搅拌至充分溶解后配置成浸渍液；将配置好的浸渍液均匀倒入活性炭载体上，并不断搅拌，待充分浸渍后，将混合料装入密封袋内，静置1～4h后于120～190℃温度下烘干，烘干时间20～40min。
本发明的磷化氢防护材料选择具有高比表面积、孔隙结构发达的椰壳活性炭作为载体材料，采用等量浸渍法负载Cu、Mo、Zn、K，即通过负载Cu、Mo、Zn为活性组分的基础上负载一定的K化合物作为活性组分助剂，对PH3具有较高的反应活性，且不含有毒的Cr化合物。其中，Cu来源于碱式碳酸铜，Mo来源于钼酸铵，Zn来源于碱式碳酸锌，K来源于碳酸钾。采用流动床活化法使活性组分具有反应活性，制备得到催化剂样品。
本发明制备的PH3防护材料，经批量制备验证工艺可行，经动力管检测对PH3的防护性能较优，并且与B类滤毒罐的滤毒材料相比不含铬。B类滤毒罐的滤毒材料负载的活性组分为Cu、Cr、Ag化合物，该材料对PH3具有一定的防护作用，但负载的活性组分铬有致癌作用。
具体实施方式
下面对本发明的具体实施例进行详细说明。
实施例1
一种添加K助剂的PH3防护材料的制备方法，如下：
取100g 0.6～1.6mm范围的椰壳破碎炭，按照该活性炭水容量的90%量取氨水，剩余10%量取去离子水于烧杯中；称取5g碳酸氢铵、15g碱式碳酸铜、1g钼酸铵、1g碱式碳酸锌、10g碳酸钾，将量好的氨水和去离子水混合均匀加热至40～80℃，依次加入称好的活性组分，搅拌至充分溶解后配置成浸渍液；将配置好的浸渍液均匀倒入活性炭载体上，并不断搅拌，待充分浸渍后，将混合料装入密封袋内，静置1h后，于流动床层烘干，烘干温度为135℃，烘干时间25min。
实施例2
一种添加K助剂的PH3防护材料的制备方法，如下：
取100g 0.6～1.6mm范围的椰壳破碎炭，按照该活性炭水容量的90%量取氨水，剩余10%量取去离子水于烧杯中；称取7g碳酸氢铵、20g碱式碳酸铜、6g钼酸铵、2g碱式碳酸锌、2g碳酸钾，将量好的氨水和去离子水混合均匀加热至40～80℃，依次加入称好的活性组分，搅拌至充分溶解后配置成浸渍液；将配置好的浸渍液均匀倒入活性炭载体上，并不断搅拌，待充分浸渍后，将混合料装入密封袋内，静置1h后，于流动床层烘干，烘干温度为145℃，烘干时间30min。
本发明实施例制备的催化剂对PH3的防护效果见下表1：
表1防护材料对PH3的防护效果
Figure DEST_PATH_IMAGE001
从表1结果来看，在相同测试条件下，按照实施例1、实施例2制备催化剂与含Cr催化剂（对比例）对PH3均有较好的防护效果，并且实施例中不含铬。
本发明的催化剂以优质活性炭为载体，在添加Cu、Mo、Zn活性组分的基础上添加碳酸钾作为活性组分助剂对PH3有良好的防护效果，与ASC炭相比不含有毒的Cr化合物。
本发明中的载体材料可以选择其他种类性质的活性炭材料、多孔隙吸附材料作为替代；K化合物为碳酸钾、氯化钾或其他含钾的化合物，如KCl等作为替代，另外，Mo化合物可以用W盐、V盐、Zr盐等作为替代。
除非特别说明，本发明中所用的技术手段均为本领域技术人员所公知的方法。另外，实施方案应理解为说明性的，而非限制本发明的范围，本发明的实质和范围仅由权利要求书所限定。对于本领域技术人员而言，在不背离本发明实质和范围的前提下，对这些实施方案中的物料成分和用量进行的各种改变或改动也属于本发明的保护范围。

Claims (4)

1.一种添加K助剂的PH3防护材料，其特征在于：以椰壳活性炭作为载体材料，采用等量浸渍法负载1%～7%（重量）的碳酸氢铵、1%～20%（重量）的碱式碳酸铜、1%～10%（重量）的钼酸铵、1%～10%（重量）的碱式碳酸锌，还负载1%～10%（重量）的K化合物作为活性组分助剂，余量为活性炭。
2.根据权利要求1所述的一种添加K助剂的PH3防护材料，其特征在于：负载5%～7%（重量）的碳酸氢铵、15%～20%（重量）的碱式碳酸铜、1%～6%（重量）的钼酸铵、1%～2%（重量）的碱式碳酸锌、2%～10%（重量）的K化合物。
3.根据权利要求1或2所述的一种添加K助剂的PH3防护材料，其特征在于：所述K化合物采用碳酸钾或者氯化钾。
4.一种权利要求1至3任一所述的添加K助剂的PH3防护材料的制备方法，其特征在于：称取椰壳破碎活性炭，采用等量浸渍法，按照该活性炭的水容量的90%量取氨水，剩余10%量取去离子水；称取碳酸氢铵、碱式碳酸铜、钼酸铵、碱式碳酸锌、K化合物；将量好的氨水和去离子水混合均匀加热至40~80℃，依次加入称好的活性组分，搅拌至充分溶解后配置成浸渍液；将配置好的浸渍液均匀倒入活性炭载体上，并不断搅拌，待充分浸渍后，将混合料装入密封袋内，静置1～4h后于120～190℃温度下烘干，烘干时间20～40min。
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Application publication date: 20200710