Technology for preparing nickel sulfamate through extraction method

A technology of nickel sulfamic acid and sulfamic acid, applied in the direction of sulfamic acid, nitrogen and non-metallic compounds, etc., can solve the problems of low concentration of nickel sulfamic acid, strong hydrolysis of sulfamic acid, low solubility at room temperature, etc. The effect of small loss, high product quality, energy dependence and low consumption

Active Publication Date: 2011-06-15
JILIN JIEN NICKEL IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prepare a solution with sulfamic acid and use it as a stripping agent to produce nickel sulfamate. This field has never been involved, mainly because the solubility of sulfamic acid at room temperature is small, and the concentration of nickel sulfamate in back extraction is low. Evaporation energy consumption is high in the later stage. If the method of simply increasing the solubility by increasing the temperature will not only cause strong hydrolysis of sulfamic acid, but also cause a large amount of volatilization of the organic phase, which is not worth the candle.

Method used

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  • Technology for preparing nickel sulfamate through extraction method
  • Technology for preparing nickel sulfamate through extraction method
  • Technology for preparing nickel sulfamate through extraction method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0055] Example 1, what stripping agent used for the first time is the sulfamic acid that deionized water dissolves. The concentration is 110 g / l.

[0056] The number of extraction tank stages: 4 stages of saponification, 8 stages of extraction, 6 stages of pickling, 6 stages of sulfamic acid stripping, and 2 stages of water washing.

[0057] Specifications: Width*height*length is 600*3400*1000 (single-stage size, the same below), the volume of the mixing chamber is 0.241m 3 , clarification chamber volume 1.428m 3 In the box, the liquid intake of each section is controlled by the flow meter as

[0058] Extraction section: stock solution (nickel concentration 45g / l) inlet volume is 0.4m 3 / h, organic phase flow rate is 2m 3 / h, sodium hydroxide solution (400g / l) flow rate 0.04m 3 / h, the saponification rate is 30%,

[0059] Pickling section: sulfuric acid aqueous solution flow rate 0.35m 3 / h;

[0060] Stripping section: stripping agent (concentration of sulfamic acid is...

example 2

[0063] Example 2, what stripping agent used is to contain the sulfamic acid nickel solution that sulfamic acid concentration is 90g / l, contains nickel 50g / l, controls each section liquid inlet amount by flowmeter to be

[0064] Extraction section: stock solution (nickel concentration 60g / l) inlet volume is 0.4m 3 / h, organic phase flow rate is 2m 3 / h, sodium hydroxide solution (400g / l) flow rate 0.045m 3 / h, saponification rate 45%;

[0065] Pickling section: sulfuric acid aqueous solution flow rate 0.35m 3 / h

[0066] Stripping section: Stripping agent (concentration of sulfamic acid is 90g / l, nickel concentration is 50g / l) flow rate is 0.25m 3 / h;

[0067] Washing section: deionized water flow rate 0.05m 3 / h.

[0068] Stripping output pH value is 3.6. Contains nickel 70g / l, copper 0.0005g / l, iron 0.0005g / l, the nickel sulfamate solution of sulfate radical 3.75g / l.

[0069] Note: Through the above control conditions, the extraction section produces a raffinate conta...

example 3

[0070] Example 3, what stripping agent used is to contain the sulfamic acid nickel solution that sulfamic acid concentration is 100g / l, contains nickel 70g / l, controls each section liquid inlet amount by flow meter to be

[0071] Extraction section: the feed volume of the stock solution (nickel concentration 80g / l) is 0.25m 3 / h, organic phase flow rate is 2m 3 / h, sodium hydroxide solution (400g / l) flow rate 0.052m 3 / h, saponification rate 60%;

[0072] Pickling section: sulfuric acid aqueous solution flow rate 0.35m 3 / h;

[0073] Stripping section: stripping agent (concentration of sulfamic acid is 100g / l, nickel concentration is 70g / l) flow rate is 0.25m 3 / h;

[0074] Washing section: deionized water flow rate 0.06m 3 / h.

[0075] The pH value of the stripping output is 4.0. Nickel sulfamate solution containing 100g / l nickel, 0.0005g / l copper, 0.0005g / l iron and 5g / l sulfate radical.

[0076] Therefore, the solution is removed from the entrained organic matter, a...

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Abstract

The invention relates to a technology for preparing nickel sulfamate through the extraction method, belonging to the technical field of fine chemicals. The technology is characterized by comprising the following steps: using the raffinate obtained by extracting the two-stage countercurrent leaching liquor of high grade matte nickel and removing impurities as a stock solution to perform an extraction reaction with hard soap which is prepared from an organic phase and a sodium hydroxide solution according to a specific ratio; and washing a loaded organic phase with acid, and using aminosulfonicacid as a stripping agent to prepare a nickel aminosulfonate solution; and performing evaporation concentration, centrifugation and other working procedures to prepare the finished nickel aminosulfonate product. The invention has a simple technology and less loss of nickel. The massive consumption of resources such as water, electricity and the like can be avoided and the invention is a low-carbon production method suitable for future development.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals and relates to a new preparation process of nickel sulfamate. Background technique [0002] In recent years, with the rapid development of the global electronics industry, the quality requirements of electronic products are even more refined. More and more manufacturers have higher and higher quality requirements for electroplated metal layers. Nickel sulfamate is an excellent electroplating main Salt, compared with other nickel baths, the coating has more toughness, lower internal stress, faster deposition speed, and higher hardness. Based on the characteristics of nickel sulfamate, it has been widely used in PCB, electronics, automobiles, aerospace, weapons , coinage, metallurgy, nickel mesh, radio, colored aluminum alloy and other industries. [0003] The production of nickel sulfamate began in foreign countries in 1940, and it was used in the above-mentioned industrial fields in the 19...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096
Inventor 赵瑞东陈阳周凤云张宝剑刘学奇马志伟高伟郑难忘
Owner JILIN JIEN NICKEL IND
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