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A method for recovering ammonia and high-quality gypsum from ammonium sulfate

A kind of ammonium sulfate, high-quality technology, applied in chemical instruments and methods, preparation/separation of ammonia, calcium/strontium/barium sulfate, etc., to achieve the effect of low energy consumption and simple process

Active Publication Date: 2021-06-18
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the outlet problem of a large amount of by-product ammonium sulfate in industrial processes such as caprolactam, the present invention proposes a method for recovering ammonia and high-quality gypsum using ammonium sulfate

Method used

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  • A method for recovering ammonia and high-quality gypsum from ammonium sulfate
  • A method for recovering ammonia and high-quality gypsum from ammonium sulfate
  • A method for recovering ammonia and high-quality gypsum from ammonium sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0037] The crystallization law of the mixed reaction of ammonium sulfate and milk of lime was investigated experimentally in a 2L stirred tank. First, 900ml of Ca(OH) with a concentration of 1.1mol / L is charged into the stirred tank. 2 solution, mechanically stirred, the outer jacket of the reactor was passed into heat conduction oil to heat and control the temperature, and the temperature was controlled at 100°C; then, 450ml concentration of 2.0mol / L (NH 4 ) 2 SO 4 The solution (21.2wt%) is quickly poured into the reactor at one time, and the lime milk is kept in excess, and is uniformly mixed by mechanical stirring. After the reaction starts, samples are regularly taken to measure the pH value, calcium ion concentration and sulfate ion concentration of the solution, and the crystal form and particle size of the generated gypsum crystals are analyzed at the same time. During the reaction process, 50ml / min of nitrogen gas is blown into the liquid phase, and the generated ga...

Embodiment 2

[0040] The same as in Example 1, in a 2L stirred tank, the crystallization law of the mixed reaction of ammonium sulfate and milk of lime was experimentally investigated. The reaction temperature considered was also 100°C. The difference was the feeding method, and the milk of lime was added to sulfuric acid at one time under stirring conditions in ammonium solution. It is 2.0mol / L (NH 4 ) 2 SO 4 solution (21.2wt%), and then 900ml of Ca(OH) with a concentration of 1.1mol / L 2 The solution is quickly poured into the reactor at one time, and the milk of lime is kept in excess, and mechanical stirring is added to keep the mixture uniform, and 50ml / min of nitrogen gas is blown into the liquid phase at the same time. After reacting for 60 minutes, the ammonium ion concentration in the tail gas absorption bottle was sampled and analyzed, and the ammonia recovery rate calculated based on the added ammonium sulfate was 98.5wt%, indicating that the ammonia was basically completely re...

Embodiment 3

[0042] The same as in Example 1, in a 2L stirred tank, the crystallization law of the mixed reaction of ammonium sulfate and milk of lime was experimentally investigated. The difference was the reaction temperature and feeding method. The reaction temperature was 120 ° C. Under stirring conditions, the ammonium sulfate solution was pumped Continuously added to milk of lime. First put 900ml of Ca(OH) with a concentration of 1.1mol / L in a 2L stirred tank 2 solution, and then 450ml concentration of 2.0mol / L (NH 4 ) 2 SO 4 Solution (21.2wt%) was continuously added to the reactor at a flow rate of 50ml / min, and the ammonium sulfate solution was added in 9 minutes, mechanically stirred to keep mixing evenly, and nitrogen gas of 50ml / min was blown into the liquid phase simultaneously. The jacket of the reactor is heated and kept with heat conduction oil, and the temperature is controlled at 120°C. After reacting for 60 minutes, the ammonium ion concentration in the tail gas absor...

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Abstract

The invention discloses a method for recovering ammonia gas and high-quality gypsum from ammonium sulfate: first, the milk of lime solution and ammonium sulfate (or ammonium sulfate aqueous solution) are mixed and reacted to generate ammonia and calcium sulfate; the generated ammonia can be recovered from the gas phase After the reaction, the slurry rich in calcium sulfate crystals is steam stripped to completely recover ammonia; the calcium sulfate in the slurry is filtered, dried, and dehydrated to recover high-quality gypsum products. This technology adopts multi-stage stripping to distill ammonia to ensure the complete recovery of ammonia in the reaction mother liquor; the mixing and reaction in the process of this technology should be operated under pressurized or slightly positive pressure, and the temperature of subsequent steam stripping, solid-liquid separation and other processes Both should be kept higher than 95°C. On the one hand, it can prevent the formation of dihydrate gypsum and scarring, and at the same time, it can also ensure that the gypsum crystals are mainly low-binding water gypsum, reduce process energy consumption, and ensure the quality of gypsum products. The technology can efficiently recover ammonia gas and gypsum products with low bound water from ammonium sulfate, with low process energy consumption and good economic benefits.

Description

technical field [0001] The invention relates to a method for recovering ammonia and high-quality gypsum from ammonium sulfate, especially for the chemical process with ammonium sulfate as a by-product, which can realize the recycling of ammonia. Background technique [0002] Ammonium sulfate is a by-product of a chemical process, especially in the production process of caprolactam. For every ton of caprolactam product produced, about 1.5-2.0 tons of ammonium sulfate will be produced as a by-product. In recent years, with the promotion of ammonia desulfurization technology, the production of ammonium sulfate has increased significantly. Ammonium sulfate is mainly used as nitrogen fertilizer, but long-term application will cause soil acidification, and the market is limited. Therefore, the supply of ammonium sulfate has been exceeding the demand for a long time, and the price has been depressed. Each ton of ammonium sulfate by-product needs to consume 258kg of liquid ammonia...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C1/02C01C1/12C01F11/46
CPCC01C1/022C01C1/026C01C1/12C01F11/46C01F11/468
Inventor 成有为潘腾秦伟王丽军李希
Owner ZHEJIANG UNIV