CN103803584B - 氟化氢铵制备方法 - Google Patents
氟化氢铵制备方法 Download PDFInfo
- Publication number
- CN103803584B CN103803584B CN201210444065.6A CN201210444065A CN103803584B CN 103803584 B CN103803584 B CN 103803584B CN 201210444065 A CN201210444065 A CN 201210444065A CN 103803584 B CN103803584 B CN 103803584B
- Authority
- CN
- China
- Prior art keywords
- ammonium bifluoride
- hydrogen fluoride
- liquefied ammonia
- anhydrous hydrogen
- mother liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound 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[NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 51
- KRHYYFGTRYWZRS-UHFFFAOYSA-N HF Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 45
- 239000012452 mother liquor Substances 0.000 claims abstract description 29
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound 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- 238000003860 storage Methods 0.000 description 2
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- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound 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[Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- -1 aluminum magnesium Chemical compound 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium(0) Chemical compound 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Abstract
本发明提供了一种氟化氢铵的制备方法，具体包括将液氨和无水氟化氢加入到含有母液的反应槽中进行反应，将生成的反应产物进行冷却结晶、离心脱水、破碎烘干后得到氟化氢铵成品，特别是采用了喷淋的方式加入液氨和无水氟化氢，使反应物料均匀混合，充分反应。本发明具有投料速度快、产量高、产品含水量低、不易结块、耐储存、品质高、成本低的优点。
Description
技术领域
[0001] 本发明属于化工生产领域，具体涉及一种氟化氢铵的制备方法。
背景技术
[0002] 氟化氢铵，分子式为NH4HF2，相对分子质量为57. 05,是一种白色或无色透明斜方 晶体，相对密度1. 52(25°C)，熔点125. 6°C，沸点239. 5°C。氟化氢铵可作为玻璃蚀刻剂、 防腐剂、氧化铍制金属铍的溶剂、化学试剂、锅炉给水系统和蒸汽发生系统的清洗剂、发酵 工业消毒剂和硅素钢板表面处理剂、制造陶瓷和铝镁合金的氧化剂、有机合成氟化剂、电镀 液、提取稀有元素的溶剂、硅素钢板的表面处理剂和铝型材表面处理时的腐蚀剂、油田沙石 的酸化处理剂等。
[0003] 根据生产工艺的不同，氟化氢铵制备方法可分为液相法和气相法。气相法对工艺 和设备的要求很严格，投资大，生产成本高；液相法合成工艺的设备简单，投料省，工艺条件 温和，生产操作易于控制。目前，国内大多采用液相法生产氟化氢铵。
[0004] 传统的液相法生产氟化氢铵存在液氨或氨气与无水氟化氢混合不均匀、反应不彻 底、产品含水量高、易结块、不能长期储存等缺点。如申请号为200710069003. 0,申请名称为 "一种湿法生产氟化氢铵工艺及设备的改进方法"的中国专利申请，其具体过程是，先将一 定量的母液打入到塑制带冷却盘管反应釜中，再将氨气和无水氟化氢同时通入反应釜中， 直至反应到达终点，最后经过结晶、脱水、干燥工序得到氟化氢铵产品。此工艺选用氨气为 原料，投料速度慢，产量低，直接通入氨气与无水氟化氢，会导致物料混合不均匀，很难进行 充分反应，而且也没有彻底解决液相法生产的产品含水量较高、易结块、不能长期储存等问 题。
发明内容
[0005] 为了克服上述现有技术的不足，本发明的目的是提供一种氟化氢铵的制备方法， 使液氨和无水氟化氢均匀混合，彻底反应，加快投料速度、增加产量、制备出含水量低、不易 结块、耐储存、品质尚、成本低的氣化氛钱广品。
[0006] 本发明提供的一种氟化氢铵制备方法，具体包括以下步骤：
[0007] 将液氨和无水氟化氢加入到含有母液的反应槽中，使液氨和无水氟化氢进行反 应，生成反应产物；
[0008] 将反应产物放入结晶桶中进行冷却结晶，得到氟化氢铵晶体及杂质的混合物；
[0009] 将氟化氢铵晶体及杂质的混合物放入离心机进行脱水，得到的固体为氟化氢铵；
[0010] 将氟化氢铵破碎成粉末，烘干后得到氟化氢铵成品。
[0011] 其中，所述母液为氟化氢铵结晶残液，包含氟化氢铵和氨水。
[0012] 所述液氨与无水氟化氢的重量比为1. 25-1. 30,在将其加入到含有母液的反应槽 中的过程中，先加入液氨50_60kg，再加入无水氟化氢100-110kg，最后通过喷淋装置同时 加入剩余的液氨和无水氟化氢。优选地，液氨的喷淋速度控制在30-50m3/h，无水氟化氢的 喷淋速度控制在50-80m3/h。
[0013] 所述喷淋装置包括：送入所述剩余的液氨和无水氟化氢的给料管，以及喷洒所述 剩余的液氨和无水氟化氢的喷嘴，其中所述喷嘴的孔径为1. 5-10mm，同时使用2-10组喷淋 装置加入所述剩余的液氨和无水氟化氢。
[0014] 所述反应温度为95. 5-109°C，反应压力为常压，反应终点的pH值控制在2. 1- 2. 9,在投料终点还差50kg时（以液氨计)，检测其pH值，然后根据检测结果做相应的调整。
[0015] 所述结晶桶带有冷却水管，利用流过所述冷却水管中的冷却水降低温度。
[0016] 利用温度为15°C-30°C冷却水进行所述的冷却结晶，结晶时间为24h。
[0017] 所述氟化氢铵晶体及杂质的混合物经由离心机进行脱水处理所分离出的母液被 返回到反应槽中循环利用。
[0018] 将脱水后的氟化氢铵放入破碎盘中，利用铁f产搅拌均匀，然后使氟化氢铵匀速通 过破碎机进行破碎处理。
[0019] 所述氟化氢铵的烘干温度为50-70°C，烘干时间为8-12h。在每个烘干盘中装 入破碎后的氟化氢铵22-28kg，将其送入烘干房后，以20°C/h的速率使烘干房中的温度逐 渐升温至50 - 70 °C。
[0020] 本发明的理论依据如下：
[0021] 1.本发明主要涉及到的反应为：
[0022] NH3+2HF-NH4HF2
[0023] 在制备氟化氢铵的过程中，投料方式对整个工艺的技术效果有很大影响，先在反 应槽中注入母液，可以有效降低无水氟化氢对设备的污染，降低设备的维修周期和维修成 本；其次，加入母液后，应先加入一定量的液氨，再加入一定量的无水氟化氢方式，因为无 水氟化氢密度大，先加入会沉入底部，从而导致反应不彻底。在先后加入液氨和无水氟化 氢后，通过喷淋的方式继续加入剩余的液氨和无水氟化氢，优选液氨的喷淋速度控制在 30-50m3/h，无水氟化氢的喷淋速度控制在50-80m3/h，因为低于此范围会导致氟化氢铵的生 产周期延长，并且容易引起喷嘴的堵塞；而高于此范围，则会使液氨和无水氟化氢不能均匀 混合以及不能充分反应。
[0024] 2.氟化氢铵的溶解度随着温度的降低而减小，所以通过降温析出氟化氢铵晶体。
[0025] 3.离心后破碎，能够使氟化氢铵彻底分散，以便在烘干时受热均匀。
[0026] 有益效果：
[0027] 本发明采用液氨为原料，相比采用氨气为原料的制备方法，加快了投料速度，采用 喷淋装置投料，保证了反应物料的均匀混合及充分反应，具有投料速度快、产量高、产品含 水量低、不易结块、耐储存、品质高、成本低的优点。
附图说明
[0028] 图1为本发明的制备流程图。
具体实施方式
[0029] 下面结合附图1和实施例对本发明进行详细说明。
[0030] 实施例1.
[0031] 将母液打入反应槽中，使反应槽中母液液位在75 - 80cm，按液氨与无水氟化氢的 重量比为1. 25的比例计算出加料量，先向母液中缓慢加入液氨50 - 60kg，再缓慢加入无水 氟化氢100 - 110kg，最后启动喷淋装置以30m3/h和50m3/h的速度分别开始喷淋剩余的液 氨和无水氟化氢，控制反应温度为95. 5°C，反应压力为常压。
[0032] 在离投料终点还差50 kg时（以液氨计)，检测其pH值，然后根据检测结果对液氨和 无水氟化氢的后续加入量进行调整，使反应终点pH值为2. 1。
[0033] 反应结束后，将反应产物放入材质为PP的结晶桶中，在结晶桶桶壁和底部的冷却 水管中通入30°C冷却水，使反应产物冷却结晶24h，得到氟化铵晶体及杂质的混合物，然后 利用离心机对氟化氢铵晶体及杂质的混合物进行脱水处理。
[0034] 将脱水后的氟化氢铵放入破碎盘中，利用铁f产搅拌均匀，然后使氟化氢铵匀速通 过破碎机进行破碎处理。
[0035] 然后在每个烘干盘中装入破碎后的氟化氢铵22 - 28kg，将其送入烘干房后，以 20°C/h的速率使烘干房中得温度逐渐升温至70°C，烘干8h。将离心得到的母液返回到反 应槽中循环利用。
[0036] 此条件下，连续制备，得到的氟化氢铵产品的产量为17. 0吨/天，氟化氢铵含量为 99. 2%，含水量为0. 5%。
[0037] 实施例2.
[0038] 将母液打入反应槽中，使反应槽中母液液位在75 - 80cm，按液氨与无水氟化氢的 重量比为1. 30的比例计算出加料量，先向母液中缓慢加入液氨50 - 60kg，再缓慢加入无水 氟化氢100 - 110kg，最后启动喷淋装置以50m3/h和80m3/h的速度分别开始喷淋剩余的液 氨和无水氟化氢，控制反应温度为109 °C，反应压力为常压。
[0039] 在离投料终点还差50kg时（以液氨计)，检测其pH值，然后根据检测结果对液氨和 无水氟化氢的后续加入量进行调整，使反应终点pH值为2. 9。
[0040] 反应结束后，将反应产物放入材质为PP的结晶桶中，在结晶桶桶壁和底部的冷却 水管中通入30°C冷却水，使反应产物冷却结晶24h，得到氟化铵晶体及杂质的混合物，然后 利用离心机对氟化氢铵晶体及杂质的混合物进行脱水处理。
[0041] 将脱水后的氟化氢铵放入破碎盘中，利用铁f产搅拌均匀，然后使氟化氢铵匀速通 过破碎机进行破碎处理。
[0042] 然后在每个烘干盘中装入破碎后的氟化氢铵22 - 28kg，将其送入烘干房后，以 20°C/h的速率使烘干房中得温度逐渐升温至60°C，烘干10h。将离心得到的母液返回到反 应槽中循环利用。
[0043] 此条件下，连续制备，得到的氟化氢铵产品的产量为18. 1吨/天，氟化氢铵含量为 99. 5%，含水量为0. 3%。
[0044] 实施例3.
[0045] 将母液打入反应槽中，使反应槽中母液液位在75 - 80cm，按液氨与无水氟化氢的 重量比为1. 27的比例计算出加料量，先向母液中缓慢加入液氨50 - 60kg，再缓慢加入无水 氟化氢100 - 110kg，最后启动喷淋装置以40m3/h和60m3/h的速度分别开始喷淋剩余的液 氨和无水氟化氢，控制反应温度为100 °C，反应压力为常压。
[0046] 在离投料终点还差50 kg时（以液氨计)，检测其pH值，然后根据检测结果对液氨和 无水氟化氢的后续加入量进行调整，使反应终点pH值为2. 5。
[0047] 反应结束后，将反应产物放入材质为PP的结晶桶中，在结晶桶桶壁和底部的冷却 水管中通入30°C冷却水，使反应产物冷却结晶24h，得到氟化铵晶体及杂质的混合物，然后 利用离心机对氟化氢铵晶体及杂质的混合物进行脱水处理。
[0048] 将脱水后的氟化氢铵放入破碎盘中，利用铁f产搅拌均匀，然后使氟化氢铵匀速通 过破碎机进行破碎处理。
[0049] 然后在每个烘干盘中装入破碎后的氟化氢铵22 - 28kg，将其送入烘干房后，以 20°C/h的速率使烘干房中得温度逐渐升温至50°C，烘干12h。将离心得到的母液返回到反 应槽中循环利用。
[0050] 此条件下，连续制备，得到的氟化氢铵产品的产量为17. 2吨/天，氟化氢铵含量为 99. 1%，含水量为0.6%。
[0051] 实施例4.
[0052] 按实施例3的操作步骤，控制结晶时冷却水的温度为15°C、20°C、25°C、30°C，其他 条件不变时，所得的氟化氢铵产品的产量和质量情况如表一所示。
[0053] 表一：氟化氢铵产品产量和质量表
[0054]
[0055] 从表一中可以看出，其他条件不变，只改变结晶时冷却水的温度，冷却水温度越 低，氟化氢铵产量越高、品质越好、含水量也越低。
[0056] 以上内容是结合优选技术方案对本发明所做的进一步详细说明，不能认定发明的 具体实施仅限于这些说明。对本发明所属技术领域的普通技术人员来说，在不脱离本发明 的构思的前提下，还可以做出简单的推演及替换，都应当视为本发明的保护范围。
Claims (10)
1. 一种氟化氢铵制备方法，其特征在于，包括以下步骤： 将液氨和无水氟化氢加入到含有母液的反应槽中，使液氨和无水氟化氢进行反应，生 成反应产物，包括： 先将一定量的液氨加入到含有母液的反应槽中； 再将一定量的无水氟化氢加入到含有母液的反应槽中； 最后通过喷淋装置同时将剩余的液氨和无水氟化氢加入到含有母液的反应槽中； 将反应产物放入结晶桶中进行冷却结晶，得到氟化氢铵晶体及杂质的混合物； 将氟化氢铵晶体及杂质的混合物放入离心机进行脱水，得到的固体为氟化氢铵； 将氟化氢铵破碎成粉末，烘干后得到氟化氢铵成品； 其中，所述液氨的喷淋速度控制在30-50m3/h，所述无水氟化氢的喷淋速度控制在 50-80m3/h。
2. 根根据权利要求1所述的方法，其特征在于，所述母液为氟化氢铵结晶残液，包含氟 化氢铵和氨水。
3. 根据权利要求1所述的方法，其特征在于，所述液氨与无水氟化氢的重量比为 1. 25-1. 30,在将其加入到含有母液的反应槽中的过程中，先将50-60kg的液氨加入到含有 母液的反应槽中，再将l〇〇-ll〇kg的无水氟化氢加入到含有母液的反应槽中，最后通过喷 淋装置同时加入剩余的液氨和无水氟化氢。
4. 根据权利要求3所述的方法，其特征在于，所述喷淋装置包括：送入所述剩余的液氨 和无水氟化氢的给料管，以及喷洒所述剩余的液氨和无水氟化氢的喷嘴，其中所述喷嘴的 孔径为1. 5-10mm。
5. 根据权利要求4所述的方法，其特征在于，同时使用2-10组喷淋装置加入所述剩余 的液氨和无水氟化氢。
6. 根据权利要求1所述的方法，其特征在于，所述反应温度为95. 5-109Γ，反应压力为 常压，反应终点的pH值控制在2. 1 - 2. 9。
7. 根据权利要求1所述的方法，其特征在于，所述结晶桶带有冷却水管，利用流过所述 冷却水管中的冷却水降低温度。
8. 根据权利要求7所述的方法，其特征在于，利用温度为15°C- 30°C冷却水进行所述 的冷却结晶，结晶时间为24h。
9. 根据权利要求1所述的方法，其特征在于，所述氟化氢铵晶体及杂质的混合物经由 离心机进行脱水处理所分离出的母液被返回到反应槽中循环利用。
10. 根据权利要求1所述的方法，其特征在于，所述氟化氢铵的烘干温度为50 - 70°C， 烘干时间为8-12h。
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