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Method for recovering ammonia from rare earth separation waste liquid

A technology for separating waste liquid and recovering ammonia, which is applied in the preparation/separation of ammonia, chemical instruments and methods, ammonia compounds, etc., which can solve the problems of high processing cost, high processing energy consumption, and low ammonia yield, and achieve improved recovery efficiency and capacity, efficient and thorough recovery, and the effect of increasing the reaction rate

Active Publication Date: 2018-10-30
全南县新资源稀土有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A method for reclaiming ammonium chloride as described in the patent application document CN1224694A as the publication number, which obtains ammonium chloride by directly concentrating, evaporating and crystallizing, but this method is because the concentration of ammonium chloride in the waste liquid is low, resulting in The processing cost is high, so it has not been popularized; a kind of recovery method that is recorded in the patent application document CN1504413A as the publication number, it is to add a circulating agent in the ammonium chloride solution, and reclaim ammonia and hydrochloric acid by evaporation, but this method Because the ammoniacal liquor and hydrochloric acid concentration of recovery are too low, useless, so do not obtain industrial application; In addition, the patent document that publication number is CN101475194B also discloses a kind of method that reclaims ammonia from low-concentration ammonium chloride waste water, and this method is Alkaline substances are added to low-concentration ammonium chloride wastewater to generate ammonia water and chloride salts, and then separated and concentrated to obtain valuable ammonia water. This method has been widely used by rare earth separation companies because of its high industrial application value, but Due to the limitations of the current technological process and equipment, this method has the problems of low ammonia yield and high processing energy consumption. The recovery rate of ammonia in this method is only 70.0-80.0%, and the ammonia content in the final discharge is still relatively high. The discharge will still cause certain environmental pollution, and the concentration of ammonia water produced is only 3.0-5.0mol / L, while the steam consumption is ≥1.5 tons / ton of ammonia water

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  • Method for recovering ammonia from rare earth separation waste liquid

Examples

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Embodiment 1

[0044] A method for recovering ammonia from rare earth separation waste liquid, such as figure 1 as shown, figure 1 Be the process flow diagram of this embodiment, concrete steps are:

[0045]Step 1, stir evenly; put the ammonium chloride wastewater discharged in the rare earth processing and extraction production with a concentration range of 1.7-2.1mol / L and an acidity range of 0.2-0.3mol / L in the solution pool I1 and stir evenly to obtain the concentration and A solution with a consistent pH.

[0046] Step 2, heating and concentrating; pump the low-concentration ammonium chloride solution obtained in step 1 into the energy-saving concentrator 2 and heat and concentrate it to obtain a high-concentration ammonium chloride solution and place it in the solution pool II3. The concentration of ammonium chloride in the high-concentration ammonium chloride solution is controlled at 3.6mol / L.

[0047] Step 3, replacement reaction; the high-concentration ammonium chloride solution...

Embodiment 2

[0052] A method for recovering ammonia from rare earth separation waste liquid, such as figure 1 as shown, figure 1 Be the process flow diagram of this embodiment, concrete steps are:

[0053] Step 1. Stir evenly; combine ammonium chloride wastewater with a concentration range of 1.8-2.3mol / L and an acidity range of 0.2-2.3mol / L discharged from the rare earth processing and extraction production with a concentration range of 0.4-1.0 discharged from the precipitation production mol / L, neutral to weakly alkaline ammonium chloride wastewater is placed in the solution pool Ⅰ1 and stirred evenly to obtain a solution with the same concentration and pH. The concentration of ammonium chloride wastewater after stirring is 1.9±0.1mol / L , The acidity is 0.3±0.05mol / L.

[0054] Step 2, heating and concentrating; pump the low-concentration ammonium chloride solution obtained in step 1 into the energy-saving concentrator 2 and heat and concentrate it to obtain a high-concentration ammoniu...

Embodiment 3

[0060] A method for recovering ammonia from rare earth separation waste liquid, such as figure 1 as shown, figure 1 Be the process flow diagram of this embodiment, concrete steps are:

[0061] Step 1. Stir evenly; put the ammonium chloride wastewater discharged from the rare earth processing and precipitation production with a concentration range of 0.4-1.0mol / L and a neutral to slightly alkaline acidity in the solution pool I1 and stir evenly to obtain the concentration and pH consistent solution.

[0062] Step 2, heating and concentrating; pump the low-concentration ammonium chloride solution obtained in step 1 into the energy-saving concentrator 2 and heat and concentrate it to obtain a high-concentration ammonium chloride solution and place it in the solution pool II3. The concentration of ammonium chloride in the high-concentration ammonium chloride solution is controlled at 2.6mol / L.

[0063] Step 3, replacement reaction; the high-concentration ammonium chloride solut...

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Abstract

The invention discloses a method for recovering ammonia from rare earth separation waste liquid. The method especially includes the steps of mixing and concentrating a low-concentration ammonium chloride solution to be recovered; allowing the low-concentration ammonium chloride solution to be recovered to react with calcium oxide; recovering ammonia from reaction overflow through a water-jet pumpI and a vacuum ammonia absorption tank I; recovering a solution obtained from reaction with a tube heat exchanger, an evaporation tower, an ammonia vacuum transfer tank and the like. The ammonia is recovered with the method, the recovery rate of the ammonia is greater than or equal to 99.5%, the concentration of ammonia water obtained finally reaches 8.0-10.0mol L, and efficient and thorough recovery is achieved; meanwhile, the ammonia nitrogen content in the waste liquid discharged by this method is less than or equal to 5.0ppm, far less than the national first-level discharge standard of 15.0ppm, and low discharge and low pollution are achieved; in addition, with the method, the consumption of steam is only 0.8-1.0tons / ton of ammonia water, the amount of steam needed for the operation isgreatly saved, and energy is saved.

Description

technical field [0001] The invention belongs to the field of rare earth separation resource recovery, in particular to a method for recovering ammonia from rare earth separation waste liquid. Background technique [0002] my country is a major producer of rare earths, with an annual output of more than 250,000 tons of rare earths, and a huge amount of mining and processing. In today's rare earth wet separation process, ammonia water saponification and ammonium bicarbonate precipitation are usually used in the rare earth extraction and rare earth precipitation process sections respectively. The ammonia water and ammonium bicarbonate auxiliary materials used in them cause the waste liquid after separation of rare earth elements to contain ammonium chloride, which is rare earth Separation of sources of ammonia nitrogen pollution in waste liquid. The discharge of waste liquid not only causes serious environmental pollution, but also causes a large amount of ammonia to be wasted...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01C1/02C02F101/16C02F103/16
CPCC01C1/022C01C1/026C02F1/04C02F9/00C02F2101/16C02F2103/16Y02P20/10
Inventor 樊佐军赵军峰张虎军
Owner 全南县新资源稀土有限责任公司
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