Preparation method of high-purity boric acid

A technology of high-purity boric acid and boric acid, which is applied in the direction of boron oxyacids and boron oxide compounds, can solve problems such as heat loss, high production cost, and increased raw material loss, and achieve reduced surface tension, reduced production costs, and shortened process time. Effect

Active Publication Date: 2016-02-24
DANDONG CHEM REAGENT FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existing industrial boric acid purification methods have many technical deficiencies, including long process flow, high production cost, unsatisfactory product purity, etc. These purification preparation methods all use filtration to filter out impurities, but in actual operation, filtration needs to be It is carried out under high temperature conditions to prevent boric acid crystallization. The filtration process takes a long time and will increase the loss of raw materials. There is heat loss in the process, and the filtration effect of the filtration method is also limited, and the fine impurities in the solution will still pass through the filter. These fine impurity particles remain in the product, which also affects the purity of boric acid; the first and third schemes use additional materials, which will introduce more complex impurities, and the second scheme is finally obtained by cooling in a constant temperature bath. Crystals increase cost consumption; each preparation process also produces a large amount of waste that cannot be reused and is difficult to handle
The existing boric acid refining treatment methods are difficult to avoid the above-mentioned problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At room temperature, dissolve 4g of boric acid in 95.8g of deionized water, then add 0.2g of isopropanol to form 100g of initial circulating mother liquor, put it in a 500ml three-necked flask, then add 30g of industrial boric acid and 0.0006mol of sulfuric acid, stir and heat to 95 ℃, keep warm for 1 hour, stir and cool down to crystallize to room temperature, precipitate wet boric acid crystals, place them in a Buchner funnel, vacuum filter the mother liquor, the mother liquor passes through the cation exchange resin column and the anion exchange resin column in turn, and the obtained clean mother liquor is divided into two Wash the above-mentioned boric acid crystals, and quickly filter out the circulating mother liquor. The drained boric acid is placed in a vacuum drying oven and dried in vacuum at 70° C. for 3 hours to obtain 29 g of granular high-purity boric acid. The circulating mother liquor can be recycled repeatedly.

Embodiment 2

[0025] Add 60g of 95% industrial boric acid into a 1000ml three-necked flask, and 600g of boric acid saturated solution prepared at room temperature as the circulating mother liquor. The circulating mother liquor contains 0.6g of ethanol, then add 0.0012mol of hydrofluoric acid aqueous solution, stir and heat to 80°C, and keep warm for 2 hour, stirring and cooling down to crystallization to room temperature, separating out wet boric acid crystals and placing them in a Buchner funnel, vacuum-filtering the mother liquor, the mother liquor passing through a cation exchange resin column and an anion exchange resin column successively, and washing the boric acid crystals twice with the obtained clean mother liquor, and The circulating mother liquor was quickly filtered out, and the drained boric acid was placed in a vacuum drying oven, and vacuum-dried at 70° C. for 3 hours to obtain 55 g of granular high-purity boric acid.

Embodiment 3

[0027] Add 60g of industrial boric acid and 300g of the circulating mother liquor obtained from Example 2 into a 500ml three-necked flask, then add 0.001mol of nitric acid, stir and heat to 85°C, keep warm for 2 hours, stop stirring and naturally cool down to room temperature to obtain boric acid crystals, and wet boric acid The crystals are placed in a Buchner funnel, and the vacuum-filtered mother liquor passes through a cation exchange resin column and an anion exchange resin column in turn, and the obtained clean mother liquor washes the boric acid crystals twice, and quickly filters out the circulating mother liquor, and the dried boric acid crystals In a vacuum drying oven, vacuum-dry at 70°C for 3 hours to obtain 60 g of flaky high-purity boric acid, and the circulating mother liquor can be reused repeatedly.

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Abstract

The invention provides a preparation method of high-purity boric acid. The preparation method comprises the following steps: putting industrial boric acid into a mixed solution of circulating mother liquor and trace inorganic acid, stirring, and heating for dissolution; performing thermal reaction for 1-2 hours in a temperature range of 80-95 DEG C; cooling to obtain wet boric acid crystals; respectively washing the crystals by virtue of mother liquor alternately purified by a cation exchange resin column and an anion exchange resin column; and drying to prepare high-purity boric acid. Compared with the prior art, the technical scheme provided by the invention has the technical advantages of being simple in process flow, having no environmental pollution, being high in crystal purity and low in manufacturing cost, selecting between granular or lamellar crystals, and the like; moreover, the crystal particle size distribution can be greatly improved.

Description

technical field [0001] The application of the present invention relates to the purification process of industrial grade boric acid. Background technique [0002] Industrial boric acid is an industrial grade product obtained by performing sulfuric acid method, hydrochloric acid method, carbon ammonia method, nitric acid method and other processing methods on boron-containing minerals, and finally crystallized in aqueous solution, in which boric acid content is more than 95%. Boric acid is widely used in glass manufacturing, enamel, electronics industry, medicine, metallurgy, military industry, chemical reagents, nuclear power industry and aerospace and other fields. With the development of modern industry, the application fields of boric acid are constantly expanding, and the requirements for its product performance and quality are also gradually improving, and there have been researches on refining and purifying boric acid and related industries. [0003] Due to different m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/10
CPCC01B35/1045
Inventor 姜春玲郭嘉妮孟繁生吴北辰
Owner DANDONG CHEM REAGENT FACTORY
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