CN116899258A - A system and method for post-treatment of ion exchange purified phosphoric acid - Google Patents
A system and method for post-treatment of ion exchange purified phosphoric acid Download PDFInfo
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Abstract
本发明公开了一种离子交换净化磷酸后处理的系统及方法，该系统硫酸钙结晶槽底部出口与硫酸钙过滤机进料端相连，硫酸钙结晶槽侧面出口与硫酸镁结晶槽顶部B进口相连，硫酸镁结晶槽底部出口与硫酸镁过滤机进料端相连。来自离子交换净化磷酸系统洗钙镁液中的硫酸钙在硫酸钙结晶槽中结晶，硫酸钙结晶槽中的硫酸钙结晶去硫酸钙过滤机过滤、分离，硫酸钙结晶槽中的溶液去硫酸镁结晶槽中结晶，硫酸镁结晶去硫酸镁过滤机过滤、分离。采用以上系统及方法，回收硫酸钙和硫酸镁等工业盐去界区，回收的稀硫酸去离子交换净化磷酸系统使用、回收的硫酸去离子交换净化磷酸树脂再生系统使用，本专利旨在节能降耗、降低生产装置碳排放、减少操作和维修费用。
The invention discloses a system and method for post-treatment of ion exchange purified phosphoric acid. The bottom outlet of the calcium sulfate crystallization tank of the system is connected to the feed end of the calcium sulfate filter, and the side outlet of the calcium sulfate crystallization tank is connected to the top B inlet of the magnesium sulfate crystallization tank. , the outlet at the bottom of the magnesium sulfate crystallization tank is connected to the feed end of the magnesium sulfate filter. The calcium sulfate in the calcium and magnesium washing solution from the ion exchange purification phosphoric acid system is crystallized in the calcium sulfate crystallization tank. The calcium sulfate crystallization in the calcium sulfate crystallization tank is filtered and separated by the calcium sulfate filter. The solution in the calcium sulfate crystallization tank is removed from magnesium sulfate. Crystallize in the crystallization tank, and the magnesium sulfate crystallization is filtered and separated by the magnesium sulfate filter. Using the above system and method, industrial salts such as calcium sulfate and magnesium sulfate are recovered and removed from the boundary area. The recovered dilute sulfuric acid is used in the deionization exchange purification phosphoric acid system, and the recovered sulfuric acid is used in the deionization exchange purification phosphoric acid resin regeneration system. This patent aims to save energy and reduce costs. consumption, reduce carbon emissions of production equipment, and reduce operating and maintenance costs.
Description
技术领域Technical field
本发明涉及化工领域，具体涉及一种离子交换净化磷酸后处理的系统及方法，具体说是一种利用结晶、过滤、分离，将来自离子交换净化磷酸系统洗钙镁液进行处理，回收硫酸钙和硫酸镁等工业盐去界区，回收稀硫酸去离子交换净化磷酸系统使用、回收硫酸去离子交换净化磷酸树脂再生系统使用的新工艺。The invention relates to the field of chemical industry, specifically to a system and method for post-treatment of ion exchange purified phosphoric acid. Specifically, it is a method that uses crystallization, filtration and separation to process the calcium and magnesium washing liquid from the ion exchange purified phosphoric acid system to recover calcium sulfate. It is a new process used to remove boundary areas with industrial salts such as magnesium sulfate, recover dilute sulfuric acid for deionization exchange purification and phosphoric acid systems, and recover sulfuric acid for deionization exchange purification and phosphoric acid resin regeneration systems.
背景技术Background technique
磷酸是一种重要的中间化学产品，其用途概括起来有两个方面，即化肥生产和工业磷酸盐生产，用酸分解磷矿生产的湿法磷酸由于其杂质含量高则主要用于化肥生产，除了化肥以外的其它工业领域，湿法磷酸难以得到广泛的应用，通常在这些场合使用热法磷酸。与湿法磷酸相比，热法磷酸是一种高能耗、高污染的产品，如需用湿法磷酸制出优质的磷酸盐，就要对湿法磷酸进行净化处理。Phosphoric acid is an important intermediate chemical product. Its uses can be summarized in two aspects, namely chemical fertilizer production and industrial phosphate production. Wet phosphoric acid produced by acid decomposition of phosphate rock is mainly used in chemical fertilizer production due to its high impurity content. In addition to other industrial fields other than chemical fertilizers, wet phosphoric acid is difficult to be widely used, and thermal phosphoric acid is usually used in these situations. Compared with wet phosphoric acid, thermal phosphoric acid is a product with high energy consumption and high pollution. If wet phosphoric acid is to be used to produce high-quality phosphate, wet phosphoric acid must be purified.
离子交换净化磷酸是净化磷酸系统及方法的一种，主要分为离子交换净化磷酸、离子交换净化磷酸树脂再生、离子交换净化磷酸后处理等三个部分，离子交换净化磷酸后处理主要有硫酸钙稀硫酸回收、硫酸镁硫酸回收二个工艺过程，其特点是流程简单、设备少、装机功率小，不消耗蒸汽。Ion exchange purified phosphoric acid is a type of purified phosphoric acid system and method. It is mainly divided into three parts: ion exchange purified phosphoric acid, ion exchange purified phosphoric acid resin regeneration, and ion exchange purified phosphoric acid post-treatment. The main post-treatment of ion exchange purified phosphoric acid is calcium sulfate. The two processes of dilute sulfuric acid recovery and magnesium sulfate sulfuric acid recovery are characterized by simple processes, less equipment, low installed power, and no steam consumption.
发明内容Contents of the invention
本发明的目的在于提供一种离子交换净化磷酸后处理的系统及方法，该系统包括硫酸钙结晶槽，硫酸钙过滤机，硫酸钙输送机，硫酸镁结晶槽，硫酸镁循环泵，硫酸镁冷却器，硫酸镁过滤机，硫酸镁输送机等。来自离子交换净化磷酸系统的洗钙镁液从硫酸钙结晶槽顶部A进口进入硫酸钙结晶槽，来自离子交换净化磷酸树脂再生系统的稀硫酸从硫酸钙结晶槽顶部B进口进入硫酸钙结晶槽，在硫酸钙结晶槽中硫酸钙结晶，利用硫酸钙结晶槽耙机将硫酸钙结晶槽底部的硫酸钙结晶从硫酸钙结晶槽底部出口送入硫酸钙过滤机进料端。硫酸钙过滤机过滤出的固体硫酸钙结晶从硫酸钙过滤机固体出料端去硫酸钙输送机进料端，由硫酸钙输送机将硫酸钙结晶送去界区；硫酸钙过滤机过滤出的液体稀硫酸从硫酸钙过滤机液体出料端经稀硫酸贮槽顶部进口进入稀硫酸贮槽，稀硫酸贮槽中的稀硫酸从稀硫酸贮槽下部出口由稀硫酸泵送去离子交换净化磷酸系统使用。硫酸钙结晶槽上部的含镁溶液，从硫酸钙结晶槽侧面出口经硫酸镁结晶槽顶部B进口进入硫酸镁结晶槽，来自界区的浓硫酸从硫酸镁结晶槽顶部A进口进入硫酸镁结晶槽，硫酸镁结晶槽中的溶液从硫酸镁结晶槽侧面下部出口经硫酸镁循环泵进入硫酸镁冷却器中进行冷却后通过硫酸镁结晶槽侧面上部进口返回硫酸镁结晶槽。在硫酸镁结晶槽中硫酸镁结晶，利用硫酸镁结晶槽耙机将硫酸镁结晶槽底部的硫酸镁结晶从硫酸镁结晶槽底部出口送入硫酸镁过滤机进料端。硫酸镁过滤机过滤出的固体硫酸镁结晶从硫酸镁过滤机固体出料端去硫酸镁输送机进料端，由硫酸镁输送机将硫酸镁结晶送去界区；硫酸镁过滤机过滤出的液体硫酸从硫酸镁过滤机液体出料端经硫酸贮槽顶部进口进入硫酸贮槽，硫酸贮槽中的硫酸从硫酸贮槽下部出口由硫酸泵送去离子交换净化磷酸树脂再生系统使用。The object of the present invention is to provide a system and method for post-treatment of ion exchange purified phosphoric acid. The system includes a calcium sulfate crystallization tank, a calcium sulfate filter, a calcium sulfate conveyor, a magnesium sulfate crystallization tank, a magnesium sulfate circulation pump, and a magnesium sulfate cooling system. machine, magnesium sulfate filter, magnesium sulfate conveyor, etc. The calcium and magnesium washing liquid from the ion exchange purification phosphoric acid system enters the calcium sulfate crystallization tank through inlet A at the top of the calcium sulfate crystallization tank. The dilute sulfuric acid from the ion exchange purification phosphoric acid resin regeneration system enters the calcium sulfate crystallization tank from inlet B at the top of the calcium sulfate crystallization tank. Calcium sulfate crystallizes in the calcium sulfate crystallization tank, and the calcium sulfate crystallization at the bottom of the calcium sulfate crystallization tank is sent to the feed end of the calcium sulfate filter from the outlet at the bottom of the calcium sulfate crystallization tank using a calcium sulfate crystallization tank rake. The solid calcium sulfate crystals filtered out by the calcium sulfate filter go from the solid discharge end of the calcium sulfate filter to the feed end of the calcium sulfate conveyor, and the calcium sulfate crystals are sent to the boundary area by the calcium sulfate conveyor; the solid calcium sulfate crystals filtered out by the calcium sulfate filter Liquid dilute sulfuric acid enters the dilute sulfuric acid storage tank from the liquid discharge end of the calcium sulfate filter through the top inlet of the dilute sulfuric acid storage tank. The dilute sulfuric acid in the dilute sulfuric acid storage tank is sent from the lower outlet of the dilute sulfuric acid storage tank to the ion exchange purified phosphoric acid by the dilute sulfuric acid pump. System usage. The magnesium-containing solution in the upper part of the calcium sulfate crystallization tank enters the magnesium sulfate crystallization tank from the side outlet of the calcium sulfate crystallization tank through inlet B at the top of the magnesium sulfate crystallization tank. The concentrated sulfuric acid from the boundary area enters the magnesium sulfate crystallization tank from inlet A at the top of the magnesium sulfate crystallization tank. , the solution in the magnesium sulfate crystallization tank enters the magnesium sulfate cooler from the lower outlet on the side of the magnesium sulfate crystallization tank through the magnesium sulfate circulation pump, is cooled, and then returns to the magnesium sulfate crystallization tank through the upper inlet on the side of the magnesium sulfate crystallization tank. The magnesium sulfate crystallizes in the magnesium sulfate crystallization tank. The magnesium sulfate crystallization tank rake is used to transport the magnesium sulfate crystals at the bottom of the magnesium sulfate crystallization tank from the outlet at the bottom of the magnesium sulfate crystallization tank to the feed end of the magnesium sulfate filter. The solid magnesium sulfate crystals filtered out by the magnesium sulfate filter go from the solid discharge end of the magnesium sulfate filter to the feed end of the magnesium sulfate conveyor, and the magnesium sulfate crystals are sent to the boundary area by the magnesium sulfate conveyor; the solid magnesium sulfate crystals filtered out by the magnesium sulfate filter Liquid sulfuric acid enters the sulfuric acid storage tank from the liquid discharge end of the magnesium sulfate filter through the top inlet of the sulfuric acid storage tank. The sulfuric acid in the sulfuric acid storage tank is sent by the sulfuric acid pump to the ion exchange purification phosphoric acid resin regeneration system from the lower outlet of the sulfuric acid storage tank.
采用以上系统及方法，回收硫酸钙和硫酸镁等工业盐去界区，回收稀硫酸去离子交换净化磷酸系统使用、回收硫酸去离子交换净化磷酸树脂再生系统使用。本专利旨在节能降耗、降低生产装置碳排放、减少操作和维修费用。The above systems and methods are used to recover industrial salts such as calcium sulfate and magnesium sulfate to remove boundary areas, recover dilute sulfuric acid for use in deionization exchange purification phosphoric acid systems, and recover sulfuric acid for use in deionization exchange purification phosphoric acid resin regeneration systems. This patent aims to save energy and reduce consumption, reduce carbon emissions from production equipment, and reduce operating and maintenance costs.
本发明的目的可以通过以下技术方案实现：The object of the present invention can be achieved through the following technical solutions:
一种离子交换净化磷酸后处理的系统，该系统包括硫酸钙结晶槽、硫酸钙过滤机、硫酸钙输送机、硫酸镁结晶槽、硫酸镁循环泵、硫酸镁冷却器、硫酸镁过滤机、硫酸镁输送机等，所述的硫酸钙结晶槽顶部A进口与来自离子交换净化磷酸系统的洗钙镁液管道相连，硫酸钙结晶槽顶部B进口与来自离子交换净化磷酸树脂再生系统的稀硫酸管道相连，硫酸钙结晶槽底部出口与硫酸钙过滤机进料端相连，硫酸钙结晶槽侧面出口与硫酸镁结晶槽顶部B进口相连，硫酸镁结晶槽顶部A进口与来自界区的浓硫酸管道相连，硫酸镁结晶槽底部出口与硫酸镁过滤机进料端相连，硫酸镁结晶槽侧面下部出口通过硫酸镁循环泵、硫酸镁冷却器与硫酸镁结晶槽侧面上部进口相连，硫酸镁冷却器侧面上部进口与来自界区的冷却上水管道相连，硫酸镁冷却器侧面下部出口与去界区的冷却回水管道相连。An ion exchange purification phosphoric acid post-treatment system, the system includes a calcium sulfate crystallization tank, a calcium sulfate filter, a calcium sulfate conveyor, a magnesium sulfate crystallization tank, a magnesium sulfate circulation pump, a magnesium sulfate cooler, a magnesium sulfate filter, a sulfuric acid Magnesium conveyor, etc., the A inlet at the top of the calcium sulfate crystallization tank is connected to the calcium washing magnesium liquid pipeline from the ion exchange purified phosphoric acid system, and the B inlet at the top of the calcium sulfate crystallization tank is connected to the dilute sulfuric acid pipeline from the ion exchange purified phosphoric acid resin regeneration system. Connected, the bottom outlet of the calcium sulfate crystallization tank is connected to the feed end of the calcium sulfate filter, the side outlet of the calcium sulfate crystallization tank is connected to the B inlet at the top of the magnesium sulfate crystallization tank, and the A inlet at the top of the magnesium sulfate crystallization tank is connected to the concentrated sulfuric acid pipeline from the boundary area. , the bottom outlet of the magnesium sulfate crystallization tank is connected to the feed end of the magnesium sulfate filter. The lower outlet of the side of the magnesium sulfate crystallization tank is connected to the upper inlet of the side of the magnesium sulfate crystallization tank through a magnesium sulfate circulation pump and a magnesium sulfate cooler. The upper side of the magnesium sulfate cooler The inlet is connected to the cooling water pipe from the boundary area, and the lower outlet on the side of the magnesium sulfate cooler is connected to the cooling return water pipeline to the boundary area.
上述系统中：硫酸钙过滤机固体出料端与硫酸钙输送机进料端相连，硫酸钙输送机出料端去界区；硫酸钙过滤机液体出料端与稀硫酸贮槽顶部进口相连，稀硫酸贮槽下部出口通过稀硫酸泵与去离子交换净化磷酸系统的稀硫酸管道相连。In the above system: the solid discharge end of the calcium sulfate filter is connected to the feed end of the calcium sulfate conveyor, and the discharge end of the calcium sulfate conveyor is removed from the boundary area; the liquid discharge end of the calcium sulfate filter is connected to the top inlet of the dilute sulfuric acid storage tank. The lower outlet of the dilute sulfuric acid storage tank is connected to the dilute sulfuric acid pipeline of the deionization exchange purification phosphoric acid system through a dilute sulfuric acid pump.
上述系统中：硫酸镁过滤机固体出料端与硫酸镁输送机进料端相连，硫酸镁输送机出料端去界区；硫酸镁过滤机液体出料端与硫酸贮槽顶部进口相连，硫酸贮槽下部出口通过硫酸泵与去离子交换净化磷酸树脂再生系统的硫酸管道相连。In the above system: the solid discharge end of the magnesium sulfate filter is connected to the feed end of the magnesium sulfate conveyor, and the discharge end of the magnesium sulfate conveyor goes to the boundary area; the liquid discharge end of the magnesium sulfate filter is connected to the top inlet of the sulfuric acid storage tank, and the sulfuric acid The lower outlet of the storage tank is connected to the sulfuric acid pipeline of the deionization exchange purification phosphoric acid resin regeneration system through a sulfuric acid pump.
上述系统中：硫酸钙结晶槽带有硫酸钙结晶槽耙机，硫酸镁结晶槽带有硫酸镁结晶槽耙机。In the above system: the calcium sulfate crystallization tank is equipped with a calcium sulfate crystallization tank rake, and the magnesium sulfate crystallization tank is equipped with a magnesium sulfate crystallization tank rake.
一种利用上述的系统实现离子交换净化磷酸后处理的生产方法，该方法包括以下步骤，可回收的物质不止一种：A production method that utilizes the above-mentioned system to realize post-treatment of ion exchange purified phosphoric acid. The method includes the following steps, and more than one recyclable substance is available:
(1)硫酸钙稀硫酸回收工段：来自离子交换净化磷酸系统的洗钙镁液从硫酸钙结晶槽顶部A进口进入硫酸钙结晶槽，来自离子交换净化磷酸树脂再生系统的稀硫酸从硫酸钙结晶槽顶部B进口进入硫酸钙结晶槽，在硫酸钙结晶槽中硫酸钙结晶，利用硫酸钙结晶槽耙机将硫酸钙结晶槽底部的硫酸钙结晶从硫酸钙结晶槽底部出口送入硫酸钙过滤机进料端。硫酸钙过滤机过滤出的固体硫酸钙结晶从硫酸钙过滤机固体出料端去硫酸钙输送机进料端，由硫酸钙输送机将硫酸钙结晶送去界区；硫酸钙过滤机过滤出的液体稀硫酸从硫酸钙过滤机液体出料端经稀硫酸贮槽顶部进口进入稀硫酸贮槽，稀硫酸贮槽中的稀硫酸从稀硫酸贮槽下部出口由稀硫酸泵送去离子交换净化磷酸系统使用。硫酸钙结晶槽上部的含镁溶液，从硫酸钙结晶槽侧面出口去硫酸镁硫酸回收工段。(1) Calcium sulfate dilute sulfuric acid recovery section: the calcium and magnesium washing liquid from the ion exchange purification phosphoric acid system enters the calcium sulfate crystallization tank from the top A of the calcium sulfate crystallization tank, and the dilute sulfuric acid from the ion exchange purification phosphoric acid resin regeneration system crystallizes from calcium sulfate Inlet B at the top of the tank enters the calcium sulfate crystallization tank. In the calcium sulfate crystallization tank, calcium sulfate crystallizes. The calcium sulfate crystallization tank rake is used to send the calcium sulfate crystals at the bottom of the calcium sulfate crystallization tank from the outlet at the bottom of the calcium sulfate crystallization tank to the calcium sulfate filter. Feed end. The solid calcium sulfate crystals filtered out by the calcium sulfate filter go from the solid discharge end of the calcium sulfate filter to the feed end of the calcium sulfate conveyor, and the calcium sulfate crystals are sent to the boundary area by the calcium sulfate conveyor; the solid calcium sulfate crystals filtered out by the calcium sulfate filter Liquid dilute sulfuric acid enters the dilute sulfuric acid storage tank from the liquid discharge end of the calcium sulfate filter through the top inlet of the dilute sulfuric acid storage tank. The dilute sulfuric acid in the dilute sulfuric acid storage tank is sent from the lower outlet of the dilute sulfuric acid storage tank to the ion exchange purified phosphoric acid by the dilute sulfuric acid pump. System usage. The magnesium-containing solution in the upper part of the calcium sulfate crystallization tank is removed from the magnesium sulfate sulfuric acid recovery section from the side outlet of the calcium sulfate crystallization tank.
(2)硫酸镁硫酸回收工段：来自硫酸钙稀硫酸回收工段的含镁溶液，从硫酸镁结晶槽顶部B进口进入硫酸镁结晶槽，来自界区的浓硫酸从硫酸镁结晶槽顶部A进口进入硫酸镁结晶槽，硫酸镁结晶槽中的溶液从硫酸镁结晶槽侧面下部出口经硫酸镁循环泵进入硫酸镁冷却器中进行冷却后通过硫酸镁结晶槽侧面上部进口返回硫酸镁结晶槽。在硫酸镁结晶槽中硫酸镁结晶，利用硫酸镁结晶槽耙机将硫酸镁结晶槽底部的硫酸镁结晶从硫酸镁结晶槽底部出口送入硫酸镁过滤机进料端。硫酸镁过滤机过滤出的固体硫酸镁结晶从硫酸镁过滤机固体出料端去硫酸镁输送机进料端，由硫酸镁输送机将硫酸镁结晶送去界区；硫酸镁过滤机过滤出的液体硫酸从硫酸镁过滤机液体出料端经硫酸贮槽顶部进口进入硫酸贮槽，硫酸贮槽中的硫酸从硫酸贮槽下部出口由硫酸泵送去离子交换净化磷酸树脂再生系统使用。(2) Magnesium sulfate sulfuric acid recovery section: The magnesium-containing solution from the calcium sulfate dilute sulfuric acid recovery section enters the magnesium sulfate crystallization tank from inlet B at the top of the magnesium sulfate crystallization tank, and the concentrated sulfuric acid from the boundary area enters from inlet A at the top of the magnesium sulfate crystallization tank. Magnesium sulfate crystallization tank, the solution in the magnesium sulfate crystallization tank enters the magnesium sulfate cooler from the lower outlet on the side of the magnesium sulfate crystallization tank through the magnesium sulfate circulation pump for cooling, and then returns to the magnesium sulfate crystallization tank through the upper inlet on the side of the magnesium sulfate crystallization tank. The magnesium sulfate crystallizes in the magnesium sulfate crystallization tank. The magnesium sulfate crystallization tank rake is used to transport the magnesium sulfate crystals at the bottom of the magnesium sulfate crystallization tank from the outlet at the bottom of the magnesium sulfate crystallization tank to the feed end of the magnesium sulfate filter. The solid magnesium sulfate crystals filtered out by the magnesium sulfate filter go from the solid discharge end of the magnesium sulfate filter to the feed end of the magnesium sulfate conveyor, and the magnesium sulfate crystals are sent to the boundary area by the magnesium sulfate conveyor; the solid magnesium sulfate crystals filtered out by the magnesium sulfate filter Liquid sulfuric acid enters the sulfuric acid storage tank from the liquid discharge end of the magnesium sulfate filter through the top inlet of the sulfuric acid storage tank. The sulfuric acid in the sulfuric acid storage tank is sent by the sulfuric acid pump from the lower outlet of the sulfuric acid storage tank to the ion exchange purification phosphoric acid resin regeneration system for use.
一种离子交换净化磷酸后处理的方法，包括洗钙镁液结晶、过滤、分离，含镁溶液冷却、结晶、过滤、分离，回收硫酸钙、硫酸镁、稀硫酸、硫酸，其特征在于所述生产过程包括：硫酸钙稀硫酸回收工段、硫酸镁硫酸回收工段，步骤如下，可回收的物质不止一种，现以硫酸钙、硫酸镁、稀硫酸、硫酸为例：A method for post-treatment of ion exchange purified phosphoric acid, which includes crystallization, filtration and separation of calcium-washed magnesium liquid, cooling, crystallization, filtration and separation of magnesium-containing solution, recovery of calcium sulfate, magnesium sulfate, dilute sulfuric acid and sulfuric acid, characterized by the following The production process includes: calcium sulfate dilute sulfuric acid recovery section and magnesium sulfate sulfuric acid recovery section. The steps are as follows. There is more than one recyclable substance. Take calcium sulfate, magnesium sulfate, dilute sulfuric acid, and sulfuric acid as examples:
(1)硫酸钙稀硫酸回收工段：来自离子交换净化磷酸系统的洗钙镁液从硫酸钙结晶槽顶部A进口进入硫酸钙结晶槽，来自离子交换净化磷酸树脂再生系统的稀硫酸H2SO4质量浓度≤45％从硫酸钙结晶槽顶部B进口进入硫酸钙结晶槽，硫酸钙结晶槽内温度控制在＞44℃。在硫酸钙结晶槽中硫酸钙结晶，利用硫酸钙结晶槽耙机将硫酸钙结晶槽底部的硫酸钙结晶从硫酸钙结晶槽底部出口送入硫酸钙过滤机进料端。硫酸钙过滤机过滤出的固体硫酸钙结晶从硫酸钙过滤机固体出料端去硫酸钙输送机进料端，由硫酸钙输送机将硫酸钙结晶送去界区；硫酸钙过滤机过滤出的液体稀硫酸H2SO4质量浓度≤35％从硫酸钙过滤机液体出料端经稀硫酸贮槽顶部进口进入稀硫酸贮槽，稀硫酸贮槽中的稀硫酸从稀硫酸贮槽下部出口由稀硫酸泵送去离子交换净化磷酸系统使用。硫酸钙结晶槽上部的含镁溶液，从硫酸钙结晶槽侧面出口去硫酸镁硫酸回收工段。(1) Calcium sulfate dilute sulfuric acid recovery section: The calcium and magnesium washing liquid from the ion exchange purification phosphoric acid system enters the calcium sulfate crystallization tank through inlet A at the top of the calcium sulfate crystallization tank, and the dilute sulfuric acid H 2 SO 4 from the ion exchange purification phosphoric acid resin regeneration system enters the calcium sulfate crystallization tank. The mass concentration ≤45% enters the calcium sulfate crystallization tank from inlet B at the top of the calcium sulfate crystallization tank. The temperature in the calcium sulfate crystallization tank is controlled at >44°C. Calcium sulfate crystallizes in the calcium sulfate crystallization tank, and the calcium sulfate crystallization at the bottom of the calcium sulfate crystallization tank is sent to the feed end of the calcium sulfate filter from the outlet at the bottom of the calcium sulfate crystallization tank using a calcium sulfate crystallization tank rake. The solid calcium sulfate crystals filtered out by the calcium sulfate filter go from the solid discharge end of the calcium sulfate filter to the feed end of the calcium sulfate conveyor, and the calcium sulfate crystals are sent to the boundary area by the calcium sulfate conveyor; the solid calcium sulfate crystals filtered out by the calcium sulfate filter Liquid dilute sulfuric acid H 2 SO 4 mass concentration ≤ 35% enters the dilute sulfuric acid storage tank from the liquid discharge end of the calcium sulfate filter through the top inlet of the dilute sulfuric acid storage tank. The dilute sulfuric acid in the dilute sulfuric acid storage tank exits from the lower part of the dilute sulfuric acid storage tank. The dilute sulfuric acid is pumped to the ion exchange purified phosphoric acid system for use. The magnesium-containing solution in the upper part of the calcium sulfate crystallization tank is removed from the magnesium sulfate sulfuric acid recovery section from the side outlet of the calcium sulfate crystallization tank.
(2)硫酸镁硫酸回收工段：来自硫酸钙稀硫酸回收工段的含镁溶液，从硫酸镁结晶槽顶部B进口进入硫酸镁结晶槽，来自界区的浓硫酸H2SO4质量浓度≤98％从硫酸镁结晶槽顶部A进口进入硫酸镁结晶槽，硫酸镁结晶槽中的溶液从硫酸镁结晶槽侧面下部出口经硫酸镁循环泵进入硫酸镁冷却器中进行冷却后通过硫酸镁结晶槽侧面上部进口返回硫酸镁结晶槽，硫酸镁结晶槽内温度控制在≤44℃。在硫酸镁结晶槽中硫酸镁结晶，利用硫酸镁结晶槽耙机将硫酸镁结晶槽底部的硫酸镁结晶从硫酸镁结晶槽底部出口送入硫酸镁过滤机进料端。硫酸镁过滤机过滤出的固体硫酸镁结晶从硫酸镁过滤机固体出料端去硫酸镁输送机进料端，由硫酸镁输送机将硫酸镁结晶送去界区；硫酸镁过滤机过滤出的液体硫酸H2SO4质量浓度≥73％从硫酸镁过滤机液体出料端经硫酸贮槽顶部进口进入硫酸贮槽，硫酸贮槽中的硫酸从硫酸贮槽下部出口由硫酸泵送去离子交换净化磷酸树脂再生系统使用。(2) Magnesium sulfate sulfuric acid recovery section: The magnesium-containing solution from the calcium sulfate dilute sulfuric acid recovery section enters the magnesium sulfate crystallization tank from inlet B at the top of the magnesium sulfate crystallization tank. The mass concentration of concentrated sulfuric acid H 2 SO 4 from the boundary area is ≤98%. Enter the magnesium sulfate crystallization tank from inlet A at the top of the magnesium sulfate crystallization tank. The solution in the magnesium sulfate crystallization tank enters the magnesium sulfate cooler from the lower outlet on the side of the magnesium sulfate crystallization tank through the magnesium sulfate circulation pump. After cooling, it passes through the upper side of the magnesium sulfate crystallization tank. The inlet returns to the magnesium sulfate crystallization tank, and the temperature in the magnesium sulfate crystallization tank is controlled at ≤44°C. The magnesium sulfate crystallizes in the magnesium sulfate crystallization tank. The magnesium sulfate crystallization tank rake is used to transport the magnesium sulfate crystals at the bottom of the magnesium sulfate crystallization tank from the outlet at the bottom of the magnesium sulfate crystallization tank to the feed end of the magnesium sulfate filter. The solid magnesium sulfate crystals filtered out by the magnesium sulfate filter go from the solid discharge end of the magnesium sulfate filter to the feed end of the magnesium sulfate conveyor, and the magnesium sulfate crystals are sent to the boundary area by the magnesium sulfate conveyor; the solid magnesium sulfate crystals filtered out by the magnesium sulfate filter Liquid sulfuric acid H 2 SO 4 mass concentration ≥73% enters the sulfuric acid storage tank from the liquid discharge end of the magnesium sulfate filter through the top inlet of the sulfuric acid storage tank. The sulfuric acid in the sulfuric acid storage tank is sent to the sulfuric acid pump for ion exchange from the lower outlet of the sulfuric acid storage tank. Purified phosphoric acid resin regeneration system is used.
本发明的有益效果：Beneficial effects of the present invention:
本发明提供一种离子交换净化磷酸后处理的系统及方法，采用该系统及方法可将来自离子交换净化磷酸系统洗钙镁液进行处理，回收硫酸钙和硫酸镁等工业盐去界区，回收稀硫酸去离子交换净化磷酸系统使用、回收硫酸去离子交换净化磷酸树脂再生系统使用。本专利旨在节能降耗、降低离子交换净化磷酸生产成本、降低生产装置碳排放、减少操作和维修费用。The invention provides a system and method for post-treatment of ion exchange purified phosphoric acid. The system and method can be used to process the calcium and magnesium washing liquid from the ion exchange purified phosphoric acid system, recover industrial salts such as calcium sulfate and magnesium sulfate, remove the boundary area, and recover It is used in the dilute sulfuric acid deionization exchange purification phosphoric acid system and the recovered sulfuric acid deionization exchange purification phosphoric acid resin regeneration system. This patent aims to save energy and reduce consumption, reduce the production cost of ion exchange purified phosphoric acid, reduce carbon emissions of production equipment, and reduce operation and maintenance costs.
附图说明Description of the drawings
图1为本专利中工艺流程原理图Figure 1 is a schematic diagram of the process flow in this patent.
其中，硫酸钙结晶槽1，硫酸钙结晶槽耙机2，硫酸钙过滤机3，硫酸钙输送机4，稀硫酸贮槽5，稀硫酸泵6，硫酸镁结晶槽7，硫酸镁结晶槽耙机8，硫酸镁循环泵9，硫酸镁冷却器10，硫酸镁过滤机11，硫酸镁输送机12，硫酸贮槽13，硫酸泵14。Among them, calcium sulfate crystallization tank 1, calcium sulfate crystallization tank rake 2, calcium sulfate filter 3, calcium sulfate conveyor 4, dilute sulfuric acid storage tank 5, dilute sulfuric acid pump 6, magnesium sulfate crystallization tank 7, magnesium sulfate crystallization tank rake Machine 8, magnesium sulfate circulation pump 9, magnesium sulfate cooler 10, magnesium sulfate filter 11, magnesium sulfate conveyor 12, sulfuric acid storage tank 13, sulfuric acid pump 14.
具体实施方式Detailed ways
下面结合实施例对本发明做进一步说明，但本发明的保护范围不限于此：The present invention will be further described below in conjunction with the examples, but the protection scope of the present invention is not limited thereto:
如图1一种离子交换净化磷酸后处理的系统，该系统包括硫酸钙结晶槽1、硫酸钙过滤机3、硫酸钙输送机4、硫酸镁结晶槽7、硫酸镁循环泵9、硫酸镁冷却器10、硫酸镁过滤机11、硫酸镁输送机12等，所述的硫酸钙结晶槽1顶部A进口与来自离子交换净化磷酸系统的洗钙镁液管道相连，硫酸钙结晶槽1顶部B进口与来自离子交换净化磷酸树脂再生系统的稀硫酸管道相连，硫酸钙结晶槽1底部出口与硫酸钙过滤机3进料端相连，硫酸钙结晶槽1侧面出口与硫酸镁结晶槽7顶部B进口相连，硫酸镁结晶槽7顶部A进口与来自界区的浓硫酸管道相连，硫酸镁结晶槽7底部出口与硫酸镁过滤机11进料端相连，硫酸镁结晶槽7侧面下部出口通过硫酸镁循环泵9、硫酸镁冷却器10与硫酸镁结晶槽7侧面上部进口相连，硫酸镁冷却器10侧面上部进口与来自界区的冷却上水管道相连，硫酸镁冷却器10侧面下部出口与去界区的冷却回水管道相连。As shown in Figure 1, a system for ion exchange purification of phosphoric acid post-treatment, the system includes calcium sulfate crystallization tank 1, calcium sulfate filter 3, calcium sulfate conveyor 4, magnesium sulfate crystallization tank 7, magnesium sulfate circulation pump 9, magnesium sulfate cooling 10, magnesium sulfate filter 11, magnesium sulfate conveyor 12, etc., the A inlet at the top of the calcium sulfate crystallization tank 1 is connected to the calcium and magnesium washing liquid pipeline from the ion exchange purification phosphoric acid system, and the B inlet at the top of the calcium sulfate crystallization tank 1 Connected to the dilute sulfuric acid pipeline from the ion exchange purification phosphoric acid resin regeneration system, the bottom outlet of the calcium sulfate crystallization tank 1 is connected to the feed end of the calcium sulfate filter 3, and the side outlet of the calcium sulfate crystallization tank 1 is connected to the top B inlet of the magnesium sulfate crystallization tank 7 , the top A inlet of the magnesium sulfate crystallization tank 7 is connected to the concentrated sulfuric acid pipeline from the boundary area, the bottom outlet of the magnesium sulfate crystallization tank 7 is connected to the feed end of the magnesium sulfate filter 11, and the lower outlet of the side of the magnesium sulfate crystallization tank 7 passes through the magnesium sulfate circulation pump 9. The magnesium sulfate cooler 10 is connected to the upper inlet on the side of the magnesium sulfate crystallization tank 7. The upper inlet on the side of the magnesium sulfate cooler 10 is connected to the cooling water pipe from the boundary area. The lower outlet of the magnesium sulfate cooler 10 is connected to the outlet of the boundary area. The cooling return pipe is connected.
硫酸钙过滤机3固体出料端与硫酸钙输送机4进料端相连，硫酸钙输送机4出料端去界区；硫酸钙过滤机3液体出料端与稀硫酸贮槽5顶部进口相连，稀硫酸贮槽5下部出口通过稀硫酸泵6与去离子交换净化磷酸系统的稀硫酸管道相连。The solid discharge end of the calcium sulfate filter 3 is connected to the feed end of the calcium sulfate conveyor 4, and the discharge end of the calcium sulfate conveyor 4 is removed from the boundary area; the liquid discharge end of the calcium sulfate filter 3 is connected to the top inlet of the dilute sulfuric acid storage tank 5 , the lower outlet of the dilute sulfuric acid storage tank 5 is connected to the dilute sulfuric acid pipeline of the deionization exchange purification phosphoric acid system through the dilute sulfuric acid pump 6.
硫酸镁过滤机11固体出料端与硫酸镁输送机12进料端相连，硫酸镁输送机12出料端去界区；硫酸镁过滤机11液体出料端与硫酸贮槽13顶部进口相连，硫酸贮槽13下部出口通过硫酸泵14与去离子交换净化磷酸树脂再生系统的硫酸管道相连。The solid discharge end of the magnesium sulfate filter 11 is connected to the feed end of the magnesium sulfate conveyor 12, and the discharge end of the magnesium sulfate conveyor 12 is connected to the boundary area; the liquid discharge end of the magnesium sulfate filter 11 is connected to the top inlet of the sulfuric acid storage tank 13. The lower outlet of the sulfuric acid storage tank 13 is connected to the sulfuric acid pipeline of the deionization exchange purification phosphoric acid resin regeneration system through a sulfuric acid pump 14.
硫酸钙结晶槽1带有硫酸钙结晶槽耙机2，硫酸镁结晶槽7带有硫酸镁结晶槽耙机8。The calcium sulfate crystallization tank 1 is equipped with a calcium sulfate crystallization tank rake 2, and the magnesium sulfate crystallization tank 7 is equipped with a magnesium sulfate crystallization tank rake 8.
利用上述系统实现离子交换净化磷酸后处理的生产方法包括以下步骤，可回收的物质不止一种，现以硫酸钙、硫酸镁、稀硫酸、硫酸为例：The production method of using the above system to achieve post-treatment of ion exchange purified phosphoric acid includes the following steps. There is more than one recyclable substance. Calcium sulfate, magnesium sulfate, dilute sulfuric acid, and sulfuric acid are taken as examples:
(1)硫酸钙稀硫酸回收工段：来自离子交换净化磷酸系统的洗钙镁液从硫酸钙结晶槽1顶部A进口进入硫酸钙结晶槽1，来自离子交换净化磷酸树脂再生系统的稀硫酸H2SO4质量浓度42％从硫酸钙结晶槽1顶部B进口进入硫酸钙结晶槽1，硫酸钙结晶槽内温度控制在＞44℃。在硫酸钙结晶槽1中硫酸钙结晶，利用硫酸钙结晶槽耙机2将硫酸钙结晶槽1底部的硫酸钙结晶从硫酸钙结晶槽1底部出口送入硫酸钙过滤机3进料端。硫酸钙过滤机3过滤出的固体硫酸钙结晶从硫酸钙过滤机3固体出料端去硫酸钙输送机4进料端，由硫酸钙输送机4将硫酸钙结晶送去界区；硫酸钙过滤机3过滤出的液体稀硫酸H2SO4质量浓度30％从硫酸钙过滤机3液体出料端经稀硫酸贮槽5顶部进口进入稀硫酸贮槽5，稀硫酸贮槽5中的稀硫酸从稀硫酸贮槽5下部出口由稀硫酸泵6送去离子交换净化磷酸系统使用。硫酸钙结晶槽1上部的含镁溶液，从硫酸钙结晶槽1侧面出口去硫酸镁硫酸回收工段。(1) Calcium sulfate dilute sulfuric acid recovery section: the calcium and magnesium washing liquid from the ion exchange purification phosphoric acid system enters the calcium sulfate crystallization tank 1 from the top A of the calcium sulfate crystallization tank 1, and the dilute sulfuric acid H 2 from the ion exchange purification phosphoric acid resin regeneration system SO 4 with a mass concentration of 42% enters the calcium sulfate crystallization tank 1 from the top B inlet of the calcium sulfate crystallization tank 1. The temperature in the calcium sulfate crystallization tank is controlled at >44°C. Calcium sulfate crystallizes in the calcium sulfate crystallization tank 1, and the calcium sulfate crystallization tank rake 2 is used to send the calcium sulfate crystals at the bottom of the calcium sulfate crystallization tank 1 from the bottom outlet of the calcium sulfate crystallization tank 1 to the feed end of the calcium sulfate filter 3. The solid calcium sulfate crystals filtered out by the calcium sulfate filter 3 go from the solid discharge end of the calcium sulfate filter 3 to the feed end of the calcium sulfate conveyor 4, and the calcium sulfate crystals are sent to the boundary area by the calcium sulfate conveyor 4; calcium sulfate filter The liquid dilute sulfuric acid H 2 SO 4 filtered out by the machine 3 has a mass concentration of 30% and enters the dilute sulfuric acid storage tank 5 from the liquid discharge end of the calcium sulfate filter 3 through the top inlet of the dilute sulfuric acid storage tank 5. The dilute sulfuric acid in the dilute sulfuric acid storage tank 5 The dilute sulfuric acid pump 6 sends the dilute sulfuric acid from the lower outlet of the dilute sulfuric acid storage tank 5 to the ion exchange purified phosphoric acid system for use. The magnesium-containing solution in the upper part of the calcium sulfate crystallization tank 1 is discharged from the side outlet of the calcium sulfate crystallization tank 1 to the magnesium sulfate sulfuric acid recovery section.
(2)硫酸镁硫酸回收工段：来自硫酸钙稀硫酸回收工段的含镁溶液，从硫酸镁结晶槽7顶部B进口进入硫酸镁结晶槽7，来自界区的浓硫酸H2SO4质量浓度93％从硫酸镁结晶槽7顶部A进口进入硫酸镁结晶槽7，硫酸镁结晶槽7中的溶液从硫酸镁结晶槽7侧面下部出口经硫酸镁循环泵9进入硫酸镁冷却器10中进行冷却后通过硫酸镁结晶槽7侧面上部进口返回硫酸镁结晶槽7，硫酸镁结晶槽内温度控制在≤44℃。在硫酸镁结晶槽7中硫酸镁结晶，利用硫酸镁结晶槽耙机8将硫酸镁结晶槽7底部的硫酸镁结晶从硫酸镁结晶槽7底部出口送入硫酸镁过滤机11进料端。硫酸镁过滤机11过滤出的固体硫酸镁结晶从硫酸镁过滤机11固体出料端去硫酸镁输送机12进料端，由硫酸镁输送机12将硫酸镁结晶送去界区；硫酸镁过滤机11过滤出的液体硫酸H2SO4质量浓度75％从硫酸镁过滤机11液体出料端经硫酸贮槽13顶部进口进入硫酸贮槽13，硫酸贮槽13中的硫酸从硫酸贮槽13下部出口由硫酸泵14送去离子交换净化磷酸树脂再生系统使用。使用本发明运行结果实例如表1所示(2) Magnesium sulfate sulfuric acid recovery section: The magnesium-containing solution from the calcium sulfate dilute sulfuric acid recovery section enters the magnesium sulfate crystallization tank 7 from the top B inlet of the magnesium sulfate crystallization tank 7. The mass concentration of concentrated sulfuric acid H 2 SO 4 from the boundary area is 93 % enters the magnesium sulfate crystallization tank 7 from the top A inlet of the magnesium sulfate crystallization tank 7. The solution in the magnesium sulfate crystallization tank 7 enters the magnesium sulfate cooler 10 from the lower outlet on the side of the magnesium sulfate crystallization tank 7 through the magnesium sulfate circulation pump 9 for cooling. Return to the magnesium sulfate crystallization tank 7 through the upper inlet on the side of the magnesium sulfate crystallization tank 7, and the temperature in the magnesium sulfate crystallization tank is controlled at ≤44°C. Magnesium sulfate crystallizes in the magnesium sulfate crystallization tank 7, and the magnesium sulfate crystallization at the bottom of the magnesium sulfate crystallization tank 7 is sent to the feed end of the magnesium sulfate filter 11 from the bottom outlet of the magnesium sulfate crystallization tank 7 by using the magnesium sulfate crystallization tank rake 8. The solid magnesium sulfate crystals filtered out by the magnesium sulfate filter 11 go from the solid discharge end of the magnesium sulfate filter 11 to the feed end of the magnesium sulfate conveyor 12, and the magnesium sulfate crystals are sent to the boundary area by the magnesium sulfate conveyor 12; magnesium sulfate filter The liquid sulfuric acid H2SO4 filtered out by the machine 11 has a mass concentration of 75% and enters the sulfuric acid storage tank 13 from the liquid discharge end of the magnesium sulfate filter 11 through the top inlet of the sulfuric acid storage tank 13. The sulfuric acid in the sulfuric acid storage tank 13 flows from the sulfuric acid storage tank 13 The lower outlet is sent to the ion exchange purification phosphate resin regeneration system by the sulfuric acid pump 14 for use. Examples of running results using the present invention are shown in Table 1
表1 1万吨/年离子交换净化磷酸后处理装置性能考核结果表Table 1 Performance assessment results of 10,000 tons/year ion exchange purification phosphoric acid post-treatment device
表1 1万吨/年离子交换净化磷酸后处理装置性能考核结果表Table 1 Performance assessment results of 10,000 tons/year ion exchange purification phosphoric acid post-treatment device
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| US4363880A (en) * | 1981-06-22 | 1982-12-14 | American Petro Mart, Inc. | Method of selectively removing adsorbed calcium and magnesium from cation exchange resins |
| EP0068413A2 (en) * | 1981-06-22 | 1983-01-05 | American Petro Mart, Inc. | Method of using higher concentration sulfuric acid for stripping and precipitation of adsorbed magnesium |
| US4493907A (en) * | 1981-06-22 | 1985-01-15 | American Petro Mart, Inc. | Method of using higher concentration sulfuric acid for stripping and precipitation of adsorbed magnesium |
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| US5021216A (en) * | 1990-05-17 | 1991-06-04 | American Pembroke, Inc. | Method of removing and crystallizing cation resin absorbed calcium and magnesium |
| US5500193A (en) * | 1993-06-14 | 1996-03-19 | University Of South Florida | Method for ION exchange based leaching of the carbonates of calcium and magnesium from phosphate rock |
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