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A kind of preparation method of macromolecular ratio potassium fluoroaluminate

A technology of potassium fluoroaluminate and high molecular ratio, which is applied in the field of preparation of potassium fluoroaluminate with high molecular ratio, can solve the problems of high energy consumption in the preparation process, small equipment capacity, and high product cost, and achieve high economic benefits and reduce production costs. The effect of high cost and production cost

Active Publication Date: 2020-10-20
福建省漳平市九鼎氟化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method has many disadvantages. First, because potassium fluoride is extremely water-absorbing, and aluminum fluoride is easily hydrolyzed at high temperature, it is not easy to obtain high-quality potassium fluoride and aluminum fluoride raw materials; The corrosiveness of fluoride is strong, and it is difficult to prevent corrosion of equipment; in addition, due to the high temperature required for the preparation of potassium fluoroaluminate by high temperature melting method, the energy consumption of the preparation process is high, the equipment capacity is small, and the product cost is high, so it is not suitable for mass production

Method used

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preparation example Construction

[0023] The present invention relates to a kind of preparation method of macromolecular specific potassium fluoroaluminate, comprising the following steps:

[0024] (1) Fluoroaluminic acid solution preparation: aluminum hydroxide is reacted with hydrofluoric acid whose mass concentration is 25 to 35 wt%, to obtain a fluoroaluminic acid solution, and the molar ratio of hydrogen fluoride to aluminum hydroxide is 6.1 to 6.5: 1;

[0025] (2) Preparation of ammonium fluoroaluminate: add ammonium chloride solution to the fluoroaluminic acid solution obtained in step (1) under stirring, and then stir and react after the addition to obtain a suspension; wherein, ammonium chloride and fluoroaluminic acid The molar ratio of the ammonium chloride solution is 3.1~3.5: 1, and the mass concentration of the ammonium chloride solution is 20~35wt%;

[0026] (3) Filtration and washing: filter the suspension obtained in step (2), and then wash with water to obtain ammonium fluoroaluminate filter ...

Embodiment 1

[0038] (1) Preparation of fluoroaluminic acid solution: Weigh 39.0g (0.5mol) of aluminum hydroxide, add under stirring to a polytetrafluoroethylene beaker containing 260g of hydrofluoric acid solution with a concentration of 25wt%, and add about 1 / 2 Finally, pay attention to observe the reaction in the beaker, and add the material slowly to prevent the material from splashing out due to excessive reaction. Continue to stir for 10 minutes after the feeding is complete to obtain a fluoroaluminic acid solution, the molar ratio of hydrogen fluoride to aluminum hydroxide is 6.5:1, and the stirring speed of the reactor is 200 r / min;

[0039] (2) Preparation of ammonium fluoroaluminate: under stirring, 267.4 g of ammonium chloride solution with a concentration of 35 wt % was added to the fluoroaluminic acid solution obtained in step (1), and the addition time was 1 h. After the addition, the stirring reaction was continued for 20 min to obtain Suspension; Wherein, the mol ratio of am...

Embodiment 2

[0046] (1) Fluoroaluminic acid solution preparation: Weigh 39.0g (0.5mol) of aluminum hydroxide, add under stirring the Teflon beaker that 210g concentration is 30wt% hydrofluoric acid solution is housed, feed about 1 / 2 Finally, pay attention to observe the reaction in the beaker, and add the material slowly to prevent the material from splashing out due to excessive reaction. Stirring was continued for 15 minutes after the feeding was completed to obtain a fluoroaluminic acid solution, the molar ratio of hydrogen fluoride to aluminum hydroxide was 6.3:1, and the stirring speed of the reactor was 250 r / min;

[0047] (2) Preparation of ammonium fluoroaluminate: adding 294.3 g of ammonium chloride solution with a concentration of 30 wt% to the fluoroaluminic acid solution obtained in step (1) under stirring, the addition time is 45 min, and the stirring reaction is continued for 15 min after the addition is completed to obtain Suspension; Wherein, the mol ratio of ammonium chlor...

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Abstract

The invention provides a preparation method of high molecular ratio potassium fluoroaluminate. The method comprises the following steps: (1) preparing a fluoaluminic acid solution enabling aluminum hydroxide to react with hydrofluoric acid to obtain the fluoaluminic acid solution; (2) preparing ammonium fluoroaluminate: adding an ammonium chloride solution into the fluoaluminic acid solution, obtained in the step (1), under the condition of stirring, and stirring for carrying out a reaction after the end of the addition so as to obtain suspension; (3) filtering the suspension obtained in the step (2), and then washing with water to obtain an ammonium fluoroaluminate filter cake; (4) adding a potassium chloride solution to a reactor, adding the ammonium fluoroaluminate filter cake, obtainedin the step (3), under the condition of stirring, and heating and stirring for carrying out a reaction after the end of the addition so as to obtain suspension; (5) filtering the suspension obtainedin the step (4), and then washing with water to obtain a potassium fluoroaluminate filter cake; (6) drying the potassium fluoroaluminate filter cake obtained in the step (5), and pulverizing to obtainthe high molecular ratio potassium fluoroaluminate powder. The preparation method is simple to operate, easy to control, low in production cost, high in economic benefit, and the like.

Description

technical field [0001] The invention relates to a method for preparing potassium fluoroaluminate, in particular to a method for preparing potassium fluoroaluminate with a high molecular weight ratio. Background technique [0002] Potassium fluoroaluminate is mainly used as a brazing flux for aluminum and aluminum alloys, as a flux in the glass ceramic industry and as an active filler for grinding wheel abrasives. [0003] Potassium fluoroaluminate is a complex salt of fluorine and aluminum, the general formula is nKF·AlF 3 . In the formula, n is the molar ratio of potassium fluoride to aluminum fluoride in the product, which is called the molecular ratio of the product. According to the performance and application of the product, potassium fluoroaluminate products can be divided into three types: low molecular ratio (n<1.5), medium molecular ratio (n=1.5-2.5) and high molecular ratio (n>2.5). Among the three types of products, because the coordination number of fluo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/54
CPCC01F7/54
Inventor 喻鼎辉朱云沈甫原李杰陈克强
Owner 福建省漳平市九鼎氟化工有限公司