Large-granular boric acid, continuously cooling recrystallization preparation process and continuously cooling recrystallization preparation method thereof

A preparation process and large particle technology, applied in the direction of boron oxides, etc., can solve the problems of palliatives but not the root cause, and cannot completely eliminate the problem of floating crystals, and achieve good fluidity, eliminate floating crystals, and reduce floating crystals.

Inactive Publication Date: 2016-01-13
CHENGDU CHENGDE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is essentially a fine-grain elimination technology, which has a certain effect on reducing the impact of floating crystals, but this method is a temporary solution, not the root cause, and still cannot completely eliminate the problem of floating crystals

Method used

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  • Large-granular boric acid, continuously cooling recrystallization preparation process and continuously cooling recrystallization preparation method thereof
  • Large-granular boric acid, continuously cooling recrystallization preparation process and continuously cooling recrystallization preparation method thereof

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Effect test

Embodiment 1

[0028] A preparation process for continuous cooling and recrystallization of large boric acid particles. Boron-containing waste water or powdery boric acid crude product and deionized water are mixed according to the ratio of mass ratio (10-35): 100, and 10-1000ppm of surface tension changing agent is added to obtain Mixture, then raise the temperature and stir the mixture until it is completely dissolved, and then lower the temperature for the first time. When the temperature reaches 1-3°C before the crystallization point, add boric acid seeds with a particle size of 0.1-0.3mm, and lower the temperature for the second time to 10-3°C. The mother liquor of continuous crystallization is obtained at 20°C, and the mother liquor is preheated to 50-90°C and then undergoes three processes of cyclic crystallization, centrifugation and washing, and finally dried to obtain large particle boric acid products, and the cycle crystallization time is controlled at 2~8h;

[0029] Wherein the a...

Embodiment 2

[0031] Mix the concentrated boric acid waste liquid and deionized water, wherein the mass ratio between boric acid waste liquid and deionized water is 15.6:100, heat up to 50-90°C and stir to dissolve completely, then add 10-1000ppm sodium sulfate decahydrate , and then slowly lower the temperature at a rate of 2-10°C / h. When the temperature of the solution reaches 1-3°C before the crystallization point of boric acid, add boric acid seed crystals with a particle size of 0.1-0.3mm, and the amount added is the mass of boric acid waste liquid. 10‰, continue to cool down, the cooling rate is 5-15°C / h, until the temperature drops to 15°C to obtain the mother liquor, preheat the mother liquor to 50-90°C, and then carry out continuous crystallization, and control the crystal growth (crystallization) time at 4h, Then centrifuge, wash, and dry to obtain uniform boric acid particle products. The centrifuge and washing liquid are recycled after being concentrated. The crystallization syst...

Embodiment 3

[0033] Mix crude boric acid powder and deionized water, wherein the mass ratio between crude boric acid powder and deionized water is 35:100, heat up to 50-90°C and stir to dissolve completely, then add 10-600ppm of potassium sulfate, slowly cool down , the cooling rate is 2-10°C / h, when the temperature of the solution reaches 1-3°C before the crystallization point of boric acid, add boric acid seed crystals, the particle size is 0.1-0.3mm, and the amount added is 1‰ of the mass of the crude product of powdery boric acid, Continue to cool down at a cooling rate of 5-15°C / h until the temperature drops to 10°C to obtain the mother liquor. Preheat the mother liquor to 50-90°C for continuous crystallization, and control the crystal growth (crystallization) time to 6 hours, followed by centrifugation , washing, and drying to obtain uniform boric acid particle products, and the centrifuge and washing liquid are recycled after being concentrated. The crystallization system uses an ext...

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Abstract

The invention discloses large-granular boric acid, a continuously cooling recrystallization preparation process and a continuously cooling recrystallization preparation method thereof. The process includes the steps of: mixing boron-containing waste water or a powdery boric acid crude product with deionzied water according to mass ratio of (10-35):100; adding 10-1000 ppm of a surface tension change agent to obtain a mixture; increasing the temperature of the mixture with stirring until the raw materials are dissolved completely; performing primary temperature reduction, when the temperature is reduced to be higher than a crystal forming point by 1-3 DEG C, adding a boric acid crystal seed being 0.1-0.3 mm in granularity and performing secondary temperature reduction to 10-20 DEG C to prepare continuously-crystallized mother liquid; performing cyclic crystallization, centrifugation and washing to the mother liquid at 50-90 DEG C; and finally drying the crystals to obtain the large-granular boric acid product, wherein the cyclic crystallization is controlled within 2-8 h. The process is stable and is free of any crystal floatation problem. The large-granular boric acid is 0.6-1.2 mm in granularity, is high in purity, is mono-dispersed, is good in flowability and is free of blocking in storage and transportation.

Description

technical field [0001] The invention belongs to the technical field of chemical crystallization, and in particular relates to a preparation process for continuous cooling and recrystallization of uniform boric acid particles. Background technique [0002] Boric acid is an important inorganic chemical raw material, which is widely used in glass fiber, ceramics, pharmaceutical industry, flame retardant, metallurgy, leather, rust inhibitor, adhesive, nuclear industry, chemical industry and other fields, and plays an important role in the national economy. status. Domestic boric acid products are mostly powdery crystals with no obvious shape and serious agglomeration, while the purity, shape, grade and other indicators of imported boric acid are much higher than domestic products. High-purity boric acid is used as a high-purity reagent and produces various high-purity borate crystals. It is widely used in high-tech fields. Most of the nuclear industry uses nuclear-grade boric a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/10
Inventor 徐程浩杨德建杨军白涛
Owner CHENGDU CHENGDE CHEM TECH
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