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Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate

An ion exchange device and ion exchange technology, applied in the direction of ion exchange column/bed method, hydroxylamine, non-metallic elements, etc., can solve the problems of large consumption of raw materials, low production capacity, high cost, etc., to avoid empty towers or overflow towers, The effect of reducing material residue and reducing raw material consumption

Pending Publication Date: 2020-05-08
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yang Xinfa [Preparation and performance analysis of hydroxylamine perchlorate, Journal of Explosives and Explosives, 1987, 2], Chang Zhihua [Research on hydroxylamine perchlorate for propellant synthesis by ion exchange method, Propulsion Technology, 1999, V(20) :4], Zhang Mengmeng [Synthesis and Characterization of Hydroxylamine Perchlorate, Journal of Explosives and Explosives, 2013, V(36): 4; Influencing Factors of Exchange Resin and Hydroxylamine Ion Exchange in HAP Synthesis, 2014, V(12): 1 ] and others have reported the experimental research on the synthesis of hydroxylamine perchlorate by ion exchange method. The documents all adopt the feeding process from top to bottom, and have investigated in detail the effects of resin grade, feed coefficient, feed rate, etc. on resin exchange capacity and perchloric acid. The impact of hydroxylamine yield does not involve the impact of ion exchange process on test operation and test results
[0006] The study found that the following problems existed when the existing ion exchange process was used to prepare hydroxylamine nitrate or hydroxylamine perchlorate from hydroxylamine hydrochloride (sulfuric acid): (1) comparison of the repeated exchange phenomenon caused by the exchange band during the alternate process of adsorption-acid elution Obviously, a part of the resin bed in the ion exchange column cannot be effectively utilized, the consumption of raw materials is large, and the production capacity is low; It is difficult to keep the balance of the material output rate at all times, and the operator needs to monitor and adjust it carefully at all times. If there is a slight carelessness, there will be air resistance, which will lead to an empty tower, or overflow the tower. The operation procedures are cumbersome and the stability is poor.
Therefore, the actual production preparation of hydroxylamine nitrate or hydroxylamine perchlorate is relatively difficult, and the cost is higher

Method used

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  • Ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Switch the valve, add 682mL of 10% hydroxylamine sulfate aqueous solution to the Φ3.5×40cm (resin loading capacity: 370mL) ion exchange column from bottom to top at a flow rate of 11-12mL / min, and absorb the residual liquid from the ion exchange column through the IV three-way valve e. The top of the exchange column flows out; after the adsorption is completed, add pure water to the ion exchange column for washing according to the above method, until no sulfate ions are detected in the washing liquid; switch the valve again, adjust the flow rate to 5-6mL / min, from top to bottom Add 152mL nitric acid aqueous solution down to the ion exchange column, the eluent flows out from the bottom of the column through the third three-way valve h, passes upward through the fourth three-way valve e, and is discharged and collected in the discharge pipe b, and the pH value of the eluent is detected , it is advisable that the pH value of the eluent is not lower than 3.0; finally wash wi...

Embodiment 2

[0026] Add 322mL of 10% aqueous solution of hydroxylamine sulfate to the Φ3.5×40cm ion exchange column, and the others are the same as in Example 1. Detect the eluent and washing solution with a pH value greater than 3.0, which contains 22.8g of hydroxylamine nitrate, the resin utilization efficiency is 49.2%, and the consumption of raw material hydroxylamine sulfate is reduced by 52.7%.

Embodiment 3

[0028] Add 276mL of 10% aqueous solution of hydroxylamine hydrochloride to the Φ3.5×40cm ion exchange column, and the others are the same as in Example 1. The eluate and washing solution with a pH value greater than 3.0 were detected, which contained 22.9g of hydroxylamine nitrate, and the resin utilization efficiency was 49.3%. The amount of raw material hydroxylamine hydrochloride is reduced by 52.7%.

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Abstract

The invention discloses an ion exchange device and application thereof in preparation of hydroxylamine nitrate or hydroxylamine perchlorate. The ion exchange device comprises an ion exchange column and a three-way valve, the bottom end of the ion exchange column is provided with a third three-way valve, and the top end of the ion exchange column is provided with a fourth three-way valve and a fifth three-way valve; one end of the third three-way valve is connected with an emptying pipeline, and the other end of the third three-way valve is connected with a second three-way valve; one end of the fourth three-way valve is connected with an emptying pipeline, and the other end of the fourth three-way valve is connected with a discharge pipe; one end of the fifth three-way valve is connected with an emptying pipeline, the other end of the fifth three-way valve is connected with a first three-way valve; one end of the first three-way valve is connected with a feeding pipe, another end of the first three-way valve is connected with the second three-way valve, and the other end of the second three-way valve is connected with a discharge pipe; the first three-way valve and the second three-way valve are installed at the same height, the fourth three-way valve and the fifth three-way valve are installed at the same height and are higher than the first three-way valve and the second three-way valve. The device can improve the utilization efficiency of resin and can reduce the consumption of raw materials; the phenomenon of empty tower or tower overflow is avoided; and pollution of residual materials in the pipeline to subsequent operation is avoided.

Description

technical field [0001] The invention relates to a preparation process of hydroxylamine nitrate or hydroxylamine perchlorate, in particular to a process and a device for preparing hydroxylamine nitrate or hydroxylamine perchlorate by using a cation exchange resin. Background technique [0002] Hydroxylamine salt is a kind of compound formed by hydroxylamine and acid, mainly including hydroxylamine hydrochloride, hydroxylamine sulfate, hydroxylamine nitrate and hydroxylamine perchlorate. Divided according to the route of raw materials, there are two main types of synthesis methods of hydroxylamine salts, one is to directly synthesize from scratch by catalytic reduction and other methods, and the other is to prepare from other existing water-soluble hydroxylamine salts through metathesis reactions and other methods. . [0003] Hydroxylamine hydrochloride and hydroxylamine sulfate are stable in nature. In industry, they are generally processed through nitric oxide reduction met...

Claims

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Application Information

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IPC IPC(8): B01J47/02C01B21/14
CPCB01J47/02C01B21/1409
Inventor 王学敏张志勇桂林于海成许华新滕奕刚陈兴强
Owner LIMING RES INST OF CHEM IND
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