Method for removing metallic impurities in boric acid by complex crystallizing method
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A metal impurity, crystallization technology, applied in the direction of boron oxide compounds, can solve the problems of high cost, complex equipment, harsh process requirements, etc., and achieve the effect of remarkable product performance, no environmental pollution, and simple and easy-to-control process.
Inactive Publication Date: 2009-11-11
DALIAN UNIV OF TECH
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Most of the existing methods for preparing high-purity boric acid use industrial boric acid or boric anhydride and alcohol through azeotropic dehydration esterification reaction to obtain boric acid ester, and then hydrolyze to obtain boric acid. The whole process requires harsh requirements, complex equipment, and high cost. industrial application
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Embodiment 1
[0012] Example 1: Take 1000g of industrial boric acid, add distilled water to dissolve, stir, heat to 90°C, add 2-5g of acidic oxidizing additive, react for about 20 minutes, add 5-8 grams of complexing agent (organic alkali metal salt) , reacted at 90°C for 3 hours, filtered the obtained solution, cooled it at 70-80°C and filtered it again, continued to cool and recrystallize, separated the obtained crystal from the mother liquor, dried the crystal at 90°C in vacuum, and obtained a high-purity boric acid sample with a product purity of 99.99% %, where the impurity content is: Fe 0.00034%, Ca0.00089%, Co 0.00008%, Cu 0.00026%, Ni 0.00005%, Cr 0.00008%, Ti 0.00002%.
Embodiment 2
[0013] Embodiment 2: Get 1000g of industrial boric acid, add distilled water to dissolve, stir, heat to 90°C, add 10-15g of oxidizing auxiliary agent, react for about 60 minutes, add complexing agent (ammonia or C 4 The following monohydric alcohol amine) 10 ~ 20 grams, heated to 100 ° C, reacted for about 8 hours, obtained solution filtered, cooled to about 80 ° C for secondary filtration, continued cooling and recrystallization, separated the obtained crystals from the mother liquor, and vacuumed the crystals at 100 ° C Dry to obtain a high-purity boric acid sample, the product purity is 99.99%, and the impurity content is: Fe 0.00058%, Ca 0.00096%, Co 0.00006%, Cu 0.00023%, Ni 0.00008%, Cr 0.00006%, Ti 0.00008%.
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Abstract
The invention discloses a method for removing metallic impurities in boric acid by complex crystallizing method, belonging to the technical field of producing refine chemical products. The method comprises the following steps: taking industrial boric acid as raw material, mixing with solvent, dissolving at a certain temperature, and adding auxiliary agent and complexing agent, after agitating and reacting for certain time, hot filtering, cooling and re-crystallizing, centrifugally separating, washing, drying to obtain the crystal product, which is highly pure boric acid, wherein purity of the product is 99.99%. The invention has evident advantages on the aspect of raw material cost, product performance, technical flow, friendly environment and economical benefit, is suitable for industrial production, and can satisfy the special requirements on boric acid in high technology fields such as optical material, special glass, communication optical fiber and crystal material.
Description
technical field [0001] The invention belongs to the technical field of fine chemicals production, and relates to a method for removing metal impurities in boric acid by a complex crystallization method. Background technique [0002] As a multifunctional and important chemical raw material, boric acid is not only widely used in traditional industries (including glass, enamel, electroplating, metallurgy, medicine, rubber, detergent, etc.), but also a key factor in national security, aerospace and nuclear industries. necessity. The purity of boric acid is the key to its application in the field of special materials and high-tech fields. Taking boric acid for nonlinear optical materials as an example, the purity requirement should reach more than 99.9%. At present, domestic boric acid has a purity of 95.0% to 99.5% due to restrictions on the grade of boron ore and production methods. It usually contains impurities such as iron, calcium, lead, arsenic, magnesium, aluminum, halog...
Claims
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