Fast production method of high-purity metal sulphamate

A technology of sulfamate and production method, applied in the directions of sulfamic acid, nitrogen and non-metallic compounds, etc., can solve problems such as slow reaction of sulfamate

Inactive Publication Date: 2013-01-23
郑景宜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is, in order to solve the problem that directly prepares sulfamate with metal powder and sulfamic acid to

Method used

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  • Fast production method of high-purity metal sulphamate
  • Fast production method of high-purity metal sulphamate

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Experimental program
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Effect test

Embodiment 1

[0021] Nickel powder, sulfamic acid powder and pure water in a ratio of 0.5︰1:4-6 by weight, heat the pure water to 40-60°C, add nickel powder, sulfamic acid powder and pure water into a ball (zirconia balls or agate balls), add high-pressure oxygen to a reaction pressure of 0.5 to 1 standard atmosphere, grind and stir the reaction for 90 minutes, and filter the reaction solution to obtain a nickel sulfamate solution. Nickel sulfamate crystals can be obtained after heating and evaporation. The average diameter of the nickel powder is less than 100nm.

Embodiment 2

[0023] Nickel powder, sulfamic acid powder and pure water in a ratio of 1.0:1:4-6 by weight, add nickel powder and sulfamic acid powder into a closed reaction tank equipped with grinding balls (zirconia balls or agate balls), and stir Ball mill for 90 minutes, add pure water at 40-60°C, add high-pressure oxygen until the reaction pressure is 0.5 to 1 standard atmosphere, grind and stir for 90 minutes, then filter the reaction solution to obtain nickel sulfamate solution. Nickel sulfamate crystals can be obtained after heating and evaporation; the average diameter of the nickel powder is 50-100nm.

Embodiment 3

[0025] Nickel powder, sulfamic acid powder and pure water are in the ratio of 1.5︰1:4-6 by weight, heat the pure water to 40-60°C, add nickel powder, sulfamic acid powder and pure water to the grinding ball (zirconia Balls or agate balls) in the reaction tank, the total volume of the balls is half of the volume of pure water, high pressure oxygen is added to the reaction pressure of 0.5 to 1 standard atmosphere, and after the ball mill is stirred for 90 minutes, the reaction solution is filtered to obtain nickel sulfamate solution. Nickel sulfamate crystals can be obtained after heating and evaporation. The average diameter of the nickel powder is 50-100nm.

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Abstract

The invention discloses a fast production method of high-purity metal sulphamate. The fast production method comprises the following steps of: adopting excess metal powder and sulphamic acid, wherein the average particle size of the metal powder is less than 100nm; introducing pure water at the temperature of 40-60 DEG C; grinding and stirring for reaction in a drum type closed reaction tank with a grinding device under the participation of high-pressure oxygen; filtering to obtain a sulphamate solution with the concentration which can be up to 180g/L (by weight of metal); and recovering the filter residue (the metal powder) for reutilizing nickel sulphamate and cobalt sulphamate. As raw materials are simple and strong acid, base and other initiators are not added during the production process, the pollution caused by other hetero ions is avoided, and the purity of the sulphamate is only affected by the metal powder and the purity of the sulphamic acid; the smaller the average particle size of the metal powder, the higher the yield; and sulfate radicals are less than 600ppm, and the content of sodium ions and other metal ions is very low, which can not be detected by a conventional method.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a rapid production method for producing metal sulfamate with high-purity metal sulfamate by direct reaction of metal powder and sulfamic acid. Background technique [0002] Sulfamate of various metals (nickel, cobalt, copper, chromium, etc.) is widely used in the electroplating industry. , easy to control, fast deposition speed, low toxicity and low corrosion, and the electroplating products have a beautiful luster and low internal stress, and their grain structure and ductility are very good. Especially nickel sulfamate (molecular formula: Ni(NH 2 SO 3 ) 2 English name: Nickel sulfate, CAS: 13770-89-3, EINECS: 237-396-1, physical and chemical properties: transparent dark green solution) concentrated solution is a kind of electroplating nickel main salt that has developed rapidly in the world in recent years, and can obtain Metal coatings with better mechanical properties tha...

Claims

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Application Information

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IPC IPC(8): C01B21/096
Inventor 吕文广郑景宜吕铂頣郑玉琪唱祺陈泽哲
Owner 郑景宜
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