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Method and device for purifying silver nitrate through layered overall crystallization

A technology of silver nitrate and crystallization, applied in the field of saturated crystallization purification of silver nitrate solution, can solve the problems of limited application scope, difficult to use melt crystallization, difficult to apply, etc., and achieve the effects of improving product purity, high crystallization efficiency, and large heat transfer area

Pending Publication Date: 2022-07-29
浙江海钛新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Melting crystallization is the process of extracting and storing the target product in the process of cooling and crystallizing after the melting of the material. Because it involves the melting process, it is used for the crystallization and purification of organic substances, but it is difficult to be used for the melting crystallization of most inorganic compounds, which limits the scope of application.
Moreover, the unique purification process of sweating and discharging the residual liquid contained in crystals is used in the process of melt crystallization, but it is difficult to apply due to the high melting point of inorganic salts

Method used

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  • Method and device for purifying silver nitrate through layered overall crystallization
  • Method and device for purifying silver nitrate through layered overall crystallization

Examples

Experimental program
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Effect test

preparation example Construction

[0040] The preparation of the raw material of silver nitrate solution, the raw material is obtained by reacting national standard 2# silver ingot with analytical pure 63% nitric acid, and 87% wt silver nitrate solution is obtained after vacuum evaporation, and the temperature is 98°C.

[0041] The purity testing of silver nitrate raw materials and products uses the testing method in "GB / T 670-2007 Chemical Reagent Silver Nitrate", and the testing results are shown in Table 1.

Embodiment 1

[0043] use as figure 1 The device shown, first, liquid phase feeding: 830kg of silver nitrate raw material solution was added to a 1.2m3 falling film crystallizer (heat exchange crystallizer 4) through feed line 1; Distributor 3 distributes film inside the crystallizer tube; material enters 1m3 mother liquor storage tank 7 through discharge line 5; material circulation pump 8 circulates material through circulation line 10;

[0044] Then, cooling and crystallization: start the cooling cycle in the 4-shell side of the heat exchange crystallizer, the ethylene glycol solution is cooled at a cooling rate of 0.5°C / min, cooled from 95°C to 0°C, and the ethylene glycol solution is kept at a constant temperature of 0°C for 1 hour. The temperature is controlled by a programmed thermostat. The material circulation pump 8 was stopped, and after standing for 1 hour, the mother liquor adsorbed on the crystal surface in the tube pass of the heat exchange crystallizer 4 was drained and ent...

Embodiment 2

[0051] The high-purity silver nitrate prepared in Example 1 utilizes the method and device to re-crystallize again, and the results of the purity of the product obtained are shown in Table 1. The comparison between Example 2 and Example 1 found that the purity of silver nitrate was further improved. YS / T476-2005 "Silver Nitrate for Photographic Use" standard test, which can reach the second grade of silver nitrate for photographic use with higher purity.

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Abstract

The invention discloses a method and device for purifying silver nitrate through layered overall crystallization, the method comprises the steps of liquid phase feeding, cooling crystallization, draining, heating and residual liquid discharging, cleaning and material dissolving and discharging, the characteristic that silver nitrate is extremely high in solubility under the temperature rising condition is utilized, the silver nitrate is creatively and overall crystallized on a heat exchange surface, and the heat exchange efficiency is improved. And mother liquor contained in the crystals and among the crystals is discharged under a heating condition, so that the purity is improved. The device comprises a heat exchange crystallizer, a high-purity silver nitrate storage tank, a mother liquor storage tank, a material circulating pump, a product pump and a connecting pipeline. By changing the system structure of the device, the device is applied to the purification process of the silver nitrate solution, and the high-purity silver nitrate solution is prepared by dissolving silver nitrate crystals with pure water. The device is large in heat transfer area and high in crystallization efficiency, and the purity of the prepared high-purity silver nitrate can reach the photographic level.

Description

technical field [0001] The invention belongs to the technical field of saturated crystallization purification of silver nitrate solution, and particularly relates to a method and a device for purifying silver nitrate by layered monolithic crystallization. Background technique [0002] As a silver chemical product, silver nitrate is the raw material and basis for the production of other high value-added silver products. It is widely used in many fields such as mirror making, medicine, electroplating, and ultra-fine silver powder. With the improvement of product quality requirements in downstream industries, silver nitrate is gradually developing towards high purification. [0003] At present, the main method for preparing high-purity silver nitrate is the reaction process of adding nitric acid to dissolve silver, and then obtaining silver nitrate crystals through processes such as impurity removal, filtration, evaporation concentration, crystallization, centrifugation, drying...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/02B01D9/00C01G5/00
CPCB01D9/02B01D9/0013B01D9/0031B01D9/0059C01G5/00B01D2009/0086
Inventor 陈海贤曹佳培陈穆宸
Owner 浙江海钛新材料科技股份有限公司
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