CN111661828B - 一种高纯试剂硝酸的制备方法 - Google Patents
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Abstract
本发明提出了一种高纯试剂硝酸的制备方法，所述制备方法包括以下步骤：将工业级浓硝酸泵入蒸馏釜，进行减压蒸馏，接收冷凝液，吹白，混匀，尾气处理等工艺处理，并最终得到高纯试剂硝酸。本发明淘汰了以化学纯试剂硝酸做原料的制造方式，使高纯试剂硝酸的原料成本大大降低，同时避免了化学纯试剂硝酸二次精馏的成本、且降低了传统试剂生产方法的废气处理难度，省去了其他辅助离子交换设施投资成本，操作简单，含量控制稳定。
Description
技术领域
本发明属于高纯试剂硝酸生产工艺领域，具体涉及一种高纯试剂硝酸的制备方法。
背景技术
硝酸是一种具有强氧化性、腐蚀性的强酸，属于一元无机强酸，是六大无机强酸之一，也是一种重要的化工原料。在工业上可用于制化肥、农药、炸药、染料、盐类等；在有机化学中，浓硝酸与浓硫酸的混合液是重要的硝化试剂，其水溶液俗称硝镪水或氨氮水。
高纯试剂硝酸是集成电路和超大规模集成电路制作过程中的关键性基础材料之一，主要应用于半导体和太阳能光伏行业及精密电路组件制作。
目前高纯试剂硝酸的提纯方法有较多，如亚沸蒸馏、精馏法等，其方法主要采用化学纯试剂硝酸做原料，成本高，二次精馏投资成本高、能耗大，废气处理难度大，其他辅助离子交换设施投资成本高，操作复杂，含量控制不稳定等。
发明内容
本发明提出一种高纯试剂硝酸的制备方法，本方法是将工业级浓硝酸泵入蒸馏釜，进行减压蒸馏，接收冷凝液，吹白，混匀，尾气处理等工艺处理后，得到高纯试剂硝酸。
本发明的技术方案是这样实现的：
S1、将工业级浓硝酸泵入蒸馏釜，进行减压蒸馏，接收冷凝液，
S2、将冷凝液经高精度聚四氟乙烯过滤器过滤后，接收入已经提前加入定量高纯水的内衬四氟碳钢吹白罐，
S3、待接收液位达到规定硝酸含量液位时，切换接收吹白罐，对已经接收好的吹白罐进行鼓吹高纯压缩空气吹白，经特制鼓泡器鼓泡带走接收液中溶解的NO2和NO，并顺带混合均匀，
S4、吹白的尾气用三级碱洗喷淋塔进行尾气吸收，最后尾气经液封吸收后排空，达到净化生产尾气作用，实现清洁生产。
优选地，所述S1步骤中工业级浓硝酸其含量浓度为98％。
优选地，所述S2步骤中高纯水通过反渗透膜过滤系统生产制得，达到实验室三级用水标准。
优选地，所述S3步骤中四氟碳钢吹白罐采用卧式罐体，总高度180CM，纯水高度40CM，接收完毕液位120CM，占比约0.8。
优选地，所述S4步骤中三级碱洗喷淋塔用尾气吸收液为10％含量的氢氧化钠溶液。
优选地，所述S1～S4各步骤中，需保持无尘作业，确保成品的纯度。
优选地，所述S2步骤中聚四氟乙烯为具有良好防腐固体材料。
本发明的有益效果：
本发明方法淘汰了以化学纯试剂硝酸做原料的制造方式，使高纯试剂硝酸的原料成本大大降低，同时避免了化学纯试剂硝酸二次精馏的成本、且降低了相对于化学纯试剂硝酸为原料制备方法的废气处理难度，省去了其他辅助离子交换设施投资成本，操作简单，含量控制稳定。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明工艺流程图
具体实施方式
实施例1
①将工业级98％浓硝酸经0.2μm聚四氟乙烯过滤器过滤后打入蒸馏釜1中，塔釜液位控制在1/3，开启冷凝器3循环水，开启蒸馏釜1蒸汽调节阀，开始连续蒸馏，低沸物和高沸物单独采出，取中间段采出物用于高纯试剂硝酸生产，观察记录塔釜温度T1、塔顶温度T2、塔顶压力P1、冷凝液温度T3。
②将①生产的中段冷凝液经0.05μm聚四氟乙烯过滤器4过滤后接收于已加入定量高纯水的内衬四氟接收罐5，待接收罐5液位到达规定含量液位时，切换另一接收罐，对接收罐5继续吹白。
③上述②中所述内衬四氟接收罐内有特制鼓泡器，鼓泡器性能要求高纯压缩空气进入后可在接收罐内均匀分布，且分布的气泡可使接收罐内液体翻滚流动、混合均匀，达到吹白和搅拌均匀的目的。
④经鼓泡吹扫的硝酸混合液中溶解的有色气体被高纯压缩空气吹扫出来，不带入新杂质，经检验该系统生产的65～70％超高纯硝酸达到UPS级。
实施例2
①将工业级98％浓硝酸经0.2μm聚四氟乙烯过滤器过滤后打入蒸馏釜1中，塔釜液位控制在1/2之间，开启冷凝器3循环水，开启蒸馏釜1蒸汽调节阀，开始连续蒸馏，低沸物和高沸物单独采出，取中间段采出物用于高纯试剂硝酸生产，观察记录塔釜温度TA、塔顶温度TB、塔顶压力PA、冷凝液温度TC。
②将①生产的中段冷凝液经0.05μm聚四氟乙烯过滤器4过滤后接收于已加入定量高纯水的内衬四氟接收罐5，待接收罐5液位到达规定含量液位时，切换另一接收罐，对接收罐5继续吹白。
③上述②中所述内衬四氟接收罐内有特制鼓泡器，鼓泡器性能要求高纯压缩空气进入后可在接收罐内均匀分布，且分布的气泡可使接收罐内液体翻滚流动、混合均匀，达到吹白和搅拌均匀的目的。
④经鼓泡吹扫的硝酸混合液中溶解的有色气体被高纯压缩空气吹扫出来，不带入新杂质，经检验该系统生产的67～70％超高纯硝酸达到UPS级。
实施例3
①将工业级98％浓硝酸经0.2μm聚四氟乙烯过滤器过滤后打入蒸馏釜1中，塔釜液位控制在2/3之间，开启冷凝器3循环水，开启蒸馏釜1蒸汽调节阀，开始连续蒸馏，低沸物和高沸物单独采出，取中间段采出物用于高纯试剂硝酸生产，观察记录塔釜温度TA、塔顶温度TB、塔顶压力PA、冷凝液温度TC。
②将①生产的中段冷凝液经0.05μm聚四氟乙烯过滤器4过滤后接收于已加入定量高纯水的内衬四氟接收罐5，待接收罐5液位到达规定含量液位时，切换另一接收罐，对接收罐5继续吹白。
③上述②中所述内衬四氟接收罐内有特制鼓泡器，鼓泡器性能要求高纯压缩空气进入后可在接收罐内均匀分布，且分布的气泡可使接收罐内液体翻滚流动、混合均匀，达到吹白和搅拌均匀的目的。
④经鼓泡吹扫的硝酸混合液中溶解的有色气体被高纯压缩空气吹扫出来，不带入新杂质，经检验该系统生产的68～70％超高纯硝酸达到UPS级
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种高纯试剂硝酸的制备方法，其特征在于，包括以下步骤：
S1、将工业级浓硝酸泵入蒸馏釜，进行减压蒸馏，接收冷凝液，
S2、将冷凝液经高精度聚四氟乙烯过滤器过滤后，接收入已经提前加入定量高纯水的内衬四氟碳钢吹白罐，
S3、待接收液位达到规定硝酸含量液位时，切换接收吹白罐，对已经接收好的吹白罐进行鼓吹高纯压缩空气吹白，经特制鼓泡器鼓泡带走接收液中溶解的NO2和NO，并顺带混合均匀，
S4、吹白的尾气用三级碱洗喷淋塔进行尾气吸收，最后尾气经液封吸收后排空，达到净化生产尾气作用，实现清洁生产；
所述S1步骤中工业级浓硝酸其含量浓度为98％。
2.根据权利要求1所述的一种高纯试剂硝酸的制备方法，其特征是：所述S2步骤中高纯水通过反渗透膜过滤系统生产制得，达到实验室三级用水标准。
3.根据权利要求1所述的一种高纯试剂硝酸的制备方法，其特征是：所述S4步骤中三级碱洗喷淋塔用尾气吸收液为10％含量的氢氧化钠溶液。
4.根据权利要求1～3任意一项所述的一种高纯试剂硝酸的制备方法，其特征是：所述S1～S4各步骤中，需保持无尘作业，确保成品的纯度。
5.根据权利要求1～2任意一项所述的一种高纯试剂硝酸的制备方法，其特征是：所述S2步骤中聚四氟乙烯为具有良好防腐固体材料。
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| GB1262756A (en) * | 1968-05-31 | 1972-02-09 | Sumitomo Chemical Co | Process for producing nitric acid |
| CN201190105Y (zh) * | 2008-04-03 | 2009-02-04 | 江阴市润玛电子材料有限公司 | 超高纯硝酸连续生产的装置 |
| CN103523761A (zh) * | 2013-10-15 | 2014-01-22 | 苏州市晶协高新电子材料有限公司 | 一种硝酸连续脱色装置及其方法 |
| CN203558853U (zh) * | 2013-10-15 | 2014-04-23 | 苏州市晶协高新电子材料有限公司 | 一种硝酸连续脱色装置 |
| CN105293455A (zh) * | 2015-10-28 | 2016-02-03 | 多氟多化工股份有限公司 | 一种电子级硝酸吹白装置及电子级硝酸吹白方法 |
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| GB1262756A (en) * | 1968-05-31 | 1972-02-09 | Sumitomo Chemical Co | Process for producing nitric acid |
| CN201190105Y (zh) * | 2008-04-03 | 2009-02-04 | 江阴市润玛电子材料有限公司 | 超高纯硝酸连续生产的装置 |
| CN103523761A (zh) * | 2013-10-15 | 2014-01-22 | 苏州市晶协高新电子材料有限公司 | 一种硝酸连续脱色装置及其方法 |
| CN203558853U (zh) * | 2013-10-15 | 2014-04-23 | 苏州市晶协高新电子材料有限公司 | 一种硝酸连续脱色装置 |
| CN105293455A (zh) * | 2015-10-28 | 2016-02-03 | 多氟多化工股份有限公司 | 一种电子级硝酸吹白装置及电子级硝酸吹白方法 |
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Denomination of invention: A method for preparing high-purity reagent nitric acid Granted publication date: 20230711 Pledgee: China Construction Bank Corporation Laiyang Sub branch Pledgor: Yantai Far East Fine Chemical Co.,Ltd. Registration number: Y2024980018259 |