Low-sulfate radical sulfamate concentrated liquid preparation method and device thereof

A technology of sulfamate and sulfamic acid, which is applied in the field of preparation of sulfamate concentrate, can solve problems such as high sulfate content, large time and energy consumption, easy decomposition, etc., and achieve high decomposition of sulfate content and save Effects of energy consumption, time, and response time reduction

Inactive Publication Date: 2009-06-03
郑景宜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the nickel carbonate method that generally adopts now, its shortcoming is: (1) nickel carbonate solution and the sulfamic acid nickel solution nickel content of sulfamic acid solution reaction preparation preparation are low, only 100-140g/L, will prepare 180g/L The concentrated solution or cryst

Method used

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  • Low-sulfate radical sulfamate concentrated liquid preparation method and device thereof
  • Low-sulfate radical sulfamate concentrated liquid preparation method and device thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] see figure 1 , 2 , special equipment for the preparation method of low sulfate sulfamate concentrate, the equipment includes: reaction tank body 3, horizontal bar 7, support frame 1, tank cover 5, water inlet 8 with valve, body 1 is circular, The horizontal bar 7 is integrated with the reaction tank body 3, the horizontal bar 7 is fixed on the support frame 3, the tank cover 5 is on the top of one end of the reaction tank body 3, the horizontal bar is connected with the driving device, and the reaction tank body 3 is equipped with a fixed comb type The plow stirring device 4, the body 3 is also provided with a compressed air port 9 with a valve, and a filter device is provided in the tank cover; zirconia balls 2 are also housed in the reaction tank; the tank cover 5 is provided with a discharge valve. There is a discharge port 51 with a valve, and the filter device is a filter cloth 53 sandwiched between two layers of screens 52 .

Embodiment 2

[0041] Preparation method of nickel sulfamate concentrate with low sulfate radical

[0042] (A) by weight

[0043] Nickel carbonate (according to the amount of metal) 18 parts

[0044] 62 parts of dry powdered sulfamic acid

[0045] 85 parts of water;

[0046] (B) Open the cover 5, pour nickel carbonate and dry sulfamic acid into the reaction tank according to the ratio of (A), cover the tank cover 5, the motor drives the horizontal bar 7 to drive the reaction tank body 3 to rotate, and the comb type plow Stirring device 4 and zirconia ball 2 also rotate accordingly, mix and stir for 30 minutes, add hot pure water at 60°C from water inlet 8 according to the ratio (A), close water inlet 8, and stir for another 60 minutes in a closed reaction tank;

[0047] (C) inject compressed air from the compressed air port 9, open the discharge port 51, after the reactant is filtered by the filter device of the tank cover 5, the nickel sulfamate concentrated solution flows out from the d...

Embodiment 3

[0050] Proportion by weight

[0051] 15 parts of metal salt or metal base (according to the amount of metal)

[0052] 65 parts of dry powdered sulfamic acid

[0053] 90 parts of water

[0054] Other repeat embodiment 2.

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Abstract

The invention discloses a low-sulfate radical sulfamate concentrated liquid preparation method and a device thereof. The method comprises: taking 1 to 3 portions of nickel carbonate, or cobalt carbonate, or nickel hydroxide or cobalt hydroxide (counted in metal weight) and 3 to 9 portions of dry powder sulfamic acid; stirring uniformly in a reaction can, then adding 5 to 15 portions of pure hot water with the temperature of 30-40 DEG C and stirring for 50 to 70 minutes in the closed reaction can; a mode of rotating the reaction can is employed by the stirring; a fixed stirring device is arranged in the closed reaction can for stirring, and ball milling grinding, stirring while grinding, pressurizing and filtering are carried out to collect the concentrated liquid of nickel sulfamic acid or cobalt sulfamate; the concentration can achieve about 210g/L; the sulfate radicals are less than 600PPM; and crystallization can be obtained by heating and vaporizing for a while. The special device designed for the method integrates reaction and filtering, shortens the reaction time and improves the reaction effect.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a preparation method and special equipment for sulfamic acid salt concentrate. Background technique [0002] With the rapid development of the global electronics industry, the quality requirements of electronic products are constantly improving, and more and more manufacturers have higher and higher quality requirements for electroplated metal layers. The coating solution with low internal stress, good ductility and good uniformity is being vigorously advocated and promoted by many manufacturers. Sulfamic acid metal plating solution should be wider, especially nickel sulphamic acid (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. It can...

Claims

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Application Information

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IPC IPC(8): C01B21/096C25D3/12
Inventor 吕文广郑景宜吕宁刘垠仲崇何
Owner 郑景宜
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