A method for recycling organic washing water from tantalum-niobium hydrometallurgy

Abstract

The present invention relates to a method for recycling organic washing water in tantalum-niobium hydrometallurgy. The present invention recycles washing water produced by refining sec-octanol, and respectively introduces the washing water into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and an acid washing agent modulation tank, and can be used for acid adjustment, descaling of the acid adjustment tank, preparation of reverse niobium agent, and preparation of acid washing agent; the amount of pure water used in tantalum-niobium hydrometallurgy is greatly reduced, and resource waste is reduced. Although the organic washing water contains a certain amount of impurities, according to the results of repeated tests of the present invention, the use of organic washing water instead of pure water in each process will not affect the purity of the final tantalum-niobium oxide product, proving that the method is also applicable to the production of ordinary tantalum-niobium oxide or high-purity tantalum-niobium oxide.

Description

Technical Field

[0001] The invention belongs to the technical field of tantalum-niobium metal preparation, and in particular relates to a method for recycling organic washing water from tantalum-niobium hydrometallurgy. Background Art

[0002] Tantalum (Ta) and niobium (Nb) are both rare metals with high melting and boiling points. my country is very rich in tantalum and niobium resources, with the largest reserves in the world. Tantalum and niobium are widely used as new materials in high-tech industries, chemical industry and special alloys.

[0003] The tantalum-niobium hydrometallurgy process mainly includes the decomposition of tantalum niobium ore, adjustment of acidity, extraction and separation, among which the extraction and separation process requires the use of anti-niobium agent and pickling agent.

[0004] In the extraction and separation process, 2-octanol is generally used as the extractant for the preliminary extraction of tantalum niobium. In order to prepare high-purity tantalum niobium products, the 2-octanol used needs to be refined, that is, it needs to be washed with water in advance to remove impurities. The 2-octanol refining process will produce a large amount of organic wash water, which is generally discharged directly as wastewater, resulting in high production costs and a large amount of resource waste. Summary of the invention

[0005] The present invention provides a method for recycling organic washing water from tantalum-niobium hydrometallurgy, which utilizes the organic washing water in other production processes, reduces the amount of wastewater treatment, greatly reduces the amount of pure water used, reduces production costs, and saves resources.

[0006] The specific technical scheme adopted by the present invention is: a method for utilizing organic wash water from tantalum-niobium hydrometallurgy, wherein the organic wash water is waste water from cleaning octanol, and the method is characterized in that the organic wash water is respectively introduced into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank for utilization.

[0007] Furthermore, the organic wash water is introduced into a tantalum-niobium ore decomposition tank for acid adjustment.

[0008] Furthermore, in the tantalum-niobium ore decomposition tank, when adjusting the acid, organic wash water is mixed with sulfuric acid to adjust the sulfuric acid concentration to 7-7.4 mol / L.

[0009] Furthermore, the organic washing water is introduced into the acid conditioning tank, and the acid conditioning tank is descaled after being heated.

[0010] Furthermore, the method for descaling the acid adjustment tank is: setting a steam generator and a steam pipe, passing organic wash water into the acid adjustment tank, using the steam pipe to pass the steam generated by the steam generator into the acid adjustment tank, heating the organic wash water, and discharging the organic wash water after soaking in the acid adjustment liquid storage tank.

[0011] Furthermore, the organic washing water is introduced into a reverse niobium agent preparation tank to prepare the reverse niobium agent.

[0012] Furthermore, when preparing the anti-niobium agent, organic washing water is mixed with sulfuric acid to adjust the sulfuric acid concentration to 1.5-1.8 mol / L.

[0013] Furthermore, the organic washing water is introduced into a pickling agent preparation tank for preparing the pickling agent.

[0014] Furthermore, when preparing the pickling agent, organic washing water is mixed with sulfuric acid to adjust the concentration of sulfuric acid to 3.5-3.9 mol / L.

[0015] Compared with the prior art, the present invention has the following beneficial effects:

[0016] The present invention recycles the washing water generated by refining 2-octanol, and respectively introduces the washing water into a tantalum-niobium ore decomposition tank, an acid regulating tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank, and can be used for acid regulating, descaling the acid regulating tank, preparing the reverse niobium agent, and preparing the pickling agent; the amount of pure water used in the tantalum-niobium hydrometallurgy is greatly reduced, and the waste of resources is reduced.

[0017] Although the organic washing water contains a certain amount of impurities, the results of repeated tests of the present invention show that the use of organic washing water instead of pure water in each process will not affect the purity of the final tantalum niobium oxide product, which proves that this method is also suitable for the production of ordinary tantalum niobium oxide or high-purity tantalum niobium oxide. DETAILED DESCRIPTION

[0018] The present invention is described in detail below through specific examples. Those skilled in the art will appreciate that these examples are only used to illustrate the present invention and do not limit the scope of the present invention in any way.

[0019] Example 1

[0020] A method for recycling organic washing water from tantalum-niobium hydrometallurgy, wherein the organic washing water is waste water from washing 2-octanol, and the organic washing water is respectively introduced into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank for utilization.

[0021] The organic wash water is introduced into the tantalum-niobium ore decomposition tank for acid adjustment; specifically, industrial sulfuric acid and organic wash water are introduced into the tantalum-niobium ore decomposition tank, the amount of organic wash water introduced is controlled, and the sulfuric acid concentration is adjusted to 7-7.4 mol / L. During the preparation process, the solution temperature is controlled to be ≤90°C. If the temperature is monitored to be over 90°C, the introduction of concentrated sulfuric acid and organic wash water is immediately stopped, and the temperature is re-adjusted when it drops below 60°C.

[0022] Example 2

[0023] A method for recycling organic washing water from tantalum-niobium hydrometallurgy, wherein the organic washing water is waste water from washing 2-octanol, and the organic washing water is respectively introduced into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank for utilization.

[0024] The organic wash water is passed into the acid adjusting tank, and the acid adjusting tank is descaled after being heated. The method is as follows: a steam generator and a steam pipe are set, the organic wash water is passed into the acid adjusting tank, the steam generated by the steam generator is passed into the acid adjusting tank through the steam pipe, the organic wash water is heated, and the organic wash water is discharged after being soaked in the acid adjusting liquid storage tank.

[0025] The heating temperature in this embodiment is 90° C., and in other embodiments it may be 80° C., 85° C. or 100° C.

[0026] Since the temperature of the organic washing water needs to be maintained during the soaking process of the acid adjustment solution storage tank, the organic washing water needs to be continuously heated.

[0027] Since it is not convenient to directly heat the acid adjustment liquid storage tank on the basis of the existing production line, the heating method adopted in this embodiment is to set a steam generator and a steam pipeline, and use the steam pipeline to pass the steam generated by the steam generator into the acid adjustment liquid storage tank. The steam pipeline adopts a flexible pipeline, and its upper end is movable.

[0028] In other embodiments, other heating methods may be used, such as arranging a heater in the acid adjustment liquid storage tank, but in actual production, the installation and layout design of the heater is relatively difficult, and the heater needs to be removed when descaling is not performed, which is relatively complicated and cumbersome. Compared with this, the use of steam pipes is much more convenient. When descaling is not required, the pipes can be raised away from the liquid surface, which is more suitable for actual production environments.

[0029] The soaking time of the acid conditioning solution storage tank is 8 hours, and in other embodiments, it can be 5 hours, 6 hours, 7 hours, 9 hours or 10 hours.

[0030] According to the scaling rate summarized in this embodiment, the descaling frequency is determined to be once every two months, which can ensure that the production quality is not affected.

[0031] The tantalum-niobium production line also includes a push-boat furnace for calcination. The push-boat furnace may generate high-temperature exhaust gas, which is generally discharged directly after being treated. In order to save energy, the present invention also utilizes the heat of the push-boat furnace during the descaling process of the acid adjustment solution storage tank.

[0032] The specific operation is: connect the exhaust pipe of the push boat furnace to the water tank with heat exchange pipes, the exhaust pipe is connected to the air inlet end of the heat exchange pipes, use the high-temperature flue gas to heat the water in the water tank, and then use the heated water to supply the steam generator to make steam, which reduces the energy consumption of the steam generator and saves costs. Of course, due to the low frequency of descaling, when descaling is not performed, the water in the water tank can be supplied to other parts of the factory after being heated, such as hot water for employees' daily life.

[0033] During the soaking process of the acid conditioning liquid storage tank, the organic washing water is stirred to ensure uniform temperature at all places and accelerate the dissolution of dirt. Since the acid conditioning liquid storage tank itself is equipped with a stirring paddle, the ready-made stirring paddle can be used.

[0034] The stirring paddle is set below the outlet of the steam pipe, and preferably the stirring paddle blade is 100-200mm away from the outlet of the steam pipe; this can make the heat brought by the steam diffuse fastest and the heating efficiency high.

[0035] To ensure the heating rate and reduce heat loss, the steam pipe should be set to be submerged in the liquid surface by at least 100mm during descaling.

[0036] Example 3

[0037] A method for recycling organic washing water from tantalum-niobium hydrometallurgy, wherein the organic washing water is waste water from washing 2-octanol, and the organic washing water is respectively introduced into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank for utilization.

[0038] The organic wash water is introduced into the reverse niobium agent preparation tank to prepare the reverse niobium agent. Specifically, industrial sulfuric acid and organic wash water are introduced into the reverse niobium agent preparation tank, and the introduction ratio of concentrated sulfuric acid and organic wash water is controlled to adjust the sulfuric acid concentration to 1.5-1.8 mol / L, which is 1.6 mol / L in this embodiment.

[0039] Example 4

[0040] A method for recycling organic washing water from tantalum-niobium hydrometallurgy, wherein the organic washing water is waste water from washing 2-octanol, and the organic washing water is respectively introduced into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank for utilization.

[0041] The organic wash water is introduced into the pickling agent preparation tank for preparing the pickling agent, specifically: industrial sulfuric acid and organic wash water are introduced into the pickling agent preparation tank, and the introduction ratio of concentrated sulfuric acid and organic wash water is controlled to adjust the sulfuric acid concentration to 3.5-3.9 mol / L, which is 3.8 mol / L in this embodiment.

[0042] Example 5

[0043] A method for recycling organic washing water from tantalum-niobium hydrometallurgy, wherein the organic washing water is waste water from washing 2-octanol, and the organic washing water is respectively introduced into a tantalum-niobium ore decomposition tank, an acid adjustment tank, a reverse niobium agent modulation tank, and a pickling agent modulation tank for utilization.

[0044] The organic wash water is introduced into the acid adjustment tank for acid adjustment. Specifically, industrial sulfuric acid and organic wash water are introduced into the acid adjustment tank, and the introduction ratio of concentrated sulfuric acid and organic wash water is controlled to adjust the sulfuric acid concentration to 7-7.4 mol / L, which is 7.2 mol / L in this embodiment.

Claims

1. A method for recycling organic washing water from tantalum and niobium hydrometallurgy, wherein the organic washing water is wastewater produced by washing 2-octanol, characterized in that: The organic washing water is respectively introduced into the niobium ore decomposition tank, the acid adjustment tank, the niobium reverse agent adjustment tank, and the pickling agent adjustment tank for utilization; The organic wash water is passed into the reverse niobium agent preparation tank to prepare the reverse niobium agent; when preparing the reverse niobium agent, the organic wash water is mixed with sulfuric acid to prepare the sulfuric acid concentration to be 1.5-1.8 mol / L; The organic wash water is passed into the tantalum-niobium ore decomposition tank to adjust the acidity; The organic washing water is introduced into the acid conditioning tank and descaled after being heated; The organic washing water is introduced into the pickling agent preparation tank to prepare the pickling agent.

2. The method for recycling organic washing water from tantalum-niobium hydrometallurgy according to claim 1, characterized in that: In the tantalum-niobium ore decomposition tank, when adjusting the acidity, organic washing water is mixed with sulfuric acid to adjust the sulfuric acid concentration to 7-7.4 mol / L.

3. The method for recycling organic washing water from tantalum-niobium hydrometallurgy according to claim 1, characterized in that: The method for descaling the acid conditioning tank comprises: providing a steam generator and a steam pipe, passing organic washing water into the acid conditioning tank, passing steam generated by the steam generator into the acid conditioning tank through the steam pipe, heating the organic washing water to 80-100° C., and discharging the organic washing water after soaking the acid conditioning tank with the organic washing water.

4. The method for recycling organic washing water from tantalum-niobium hydrometallurgy according to claim 1, characterized in that: When preparing the pickling agent, organic washing water is mixed with sulfuric acid to adjust the concentration of sulfuric acid to 3.5-3.9 mol / L.