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Iron removal method for preparing 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 the problem that the production technology of high-purity boron products has not been broken through, and the content of iron borate ions cannot reach high-purity boric acid. Removal methods and other issues to achieve the effect of saving iron removal costs, reducing iron removal costs, and avoiding waste

Active Publication Date: 2021-12-21
青海利亚达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In recent years, although my country's boric acid production process has been greatly developed and improved, the production technology of high-purity boron products has not been broken through. The removal method caused the iron ion content in boric acid to not reach the standard of high-purity boric acid

Method used

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  • Iron removal method for preparing high-purity boric acid
  • Iron removal method for preparing high-purity boric acid
  • Iron removal method for preparing high-purity boric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0139] The salt lake crude boric acid is used as the raw material, and the iron is removed after pretreatment and washing.

[0140] Put salt lake crude boric acid in a container, add tap water and stir for 30 minutes at room temperature, use a centrifuge to separate solid and liquid, and obtain wet material crude boric acid, wherein the dosage ratio of salt lake crude boric acid and tap water is 1kg:1L.

[0141] The appearance of crude boric acid in salt lake is gray-white viscous fine particles and needle-like crystals, and the composition content is as follows in terms of mass fraction: H 3 BO 3 94.08%, MgO 0.18%, CaO 0.082%, Cl 0.73%, SO 4 2- 0.061%, Fe0.0220%;

[0142] The crude boric acid appearance after washing pretreatment is white fine particle and needle-like crystal, by mass fraction, composition content is as follows: H 3 BO 3 89.47%, MgO 0.0027%, CaO 0.012%, Cl 0.055%, SO 4 2- 0.032%, Fe 0.0120%.

[0143] The specific steps of iron removal are as follows: ...

Embodiment 2

[0151] The salt lake crude boric acid is used as the raw material, and the iron is removed after pretreatment and washing.

[0152] Put salt lake crude boric acid in a container, add tap water and stir for 30 minutes at room temperature, use a centrifuge to separate solid and liquid to obtain wet material crude boric acid, wherein the dosage ratio of salt lake crude boric acid to tap water is 1kg:1L.

[0153]The appearance of crude boric acid in salt lake is gray white viscous slippery fine particles and needle-like crystals, and the composition content is analyzed as follows in terms of mass fraction: H 3 BO 3 89.78%, MgO 0.26%, CaO 0.19%, Cl 0.56%, SO 4 2- 0.022%, Fe0.021%;

[0154] The appearance of crude boric acid after washing and pretreatment is white fine particles and needle-like crystals, and the component analysis content is as follows: H 3 BO 3 90.78%, MgO 0.0031%, CaO 0.022%, Cl 0.010%, SO 4 2- 0.0087%, Fe 0.0098%.

[0155] (1) Get 6kg of the crude boric a...

Embodiment 3

[0162] Adopt the purchased industrial boric acid as raw material to carry out iron removal, the industrial boric acid appearance is white fine particles, in terms of mass fraction, the composition content analysis is as follows: H 3 BO 3 99.54%, MgO—, CaO—, Cl0.01%, SO 4 2- 0.30%, Fe 0.0015%;

[0163] (1) Get the above-mentioned industrial boric acid of 8kg, drop into the container of 56L deironing mother liquor, start stirring and heating; Described container is the cylinder of 100L stainless steel material, and supporting stainless steel stirring and speed reducer are set; The component content of deironing mother liquor is :H 3 BO 3 48.57g / L, MgO 0.011g / L, CaO 0.10g / L, Cl0.36g / L, SO 4 2- 0.11g / L, Fe0.0008g / L.

[0164] (2) Heating the feed liquid in step (1) to 40°C, adding 5g of hydrogen peroxide according to 0.05% of the boric acid mass, heating until the raw material is completely dissolved, at this moment, the temperature of the feed liquid is 73°C, the pH value i...

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Abstract

The invention relates to the technical field of high-purity boric acid production, and provides an iron removal method for preparing high-purity boric acid. According to different iron contents in the crude boric acid (raw material), different methods are adopted to remove iron. When the content of iron in the crude boric acid is greater than or equal to 0.001%, the crude boric acid, water and hydrogen peroxide are mixed, oxidation reaction is conducted to obtain an oxidation reaction solution with the boric acid concentration of less than 180g / L, heat preservation flocculation treatment is conducted on the oxidation reaction solution at the temperature of 65 DEG C or more for 30 minutes or more, and then solid-liquid separation and cooling crystallization are conducted. When the iron content in the crude boric acid is less than or equal to 0.0015%, after high-concentration crystallization of boric acid, a produced mother liquor and hydrogen peroxide are mixed for oxidation reaction, thus the mother liquor is recycled after flocculation and filtration, so that the iron in the system is maintained at a low balance level, and the product quality is ensured. The method provided by the invention breaks through the bottleneck that a recrystallization method has harsh requirements on the quality of raw materials, is simple in steps and low in cost, and is convenient for realizing large-scale production of high-purity boric acid products.

Description

technical field [0001] The invention relates to the technical field of high-purity boric acid, in particular to an iron removal method for preparing high-purity boric acid. Background technique [0002] High-purity boric acid is an important inorganic salt, widely used in high-end fields such as capacitor manufacturing, electronics industry, high-purity analytical reagents, optoelectronics industry, metallurgy, medicine, glass, ceramics, textiles, leather, pigments, paints and national defense , occupies an important position in the national economy. The national standard GB538-2018 requires that the impurity content of type II boric acid (high-purity boric acid) is between 1 and 3 ppm, and the iron content is required to be below 2 ppm. [0003] At present, high-purity boric acid is generally purified by industrial boric acid. The purification methods of boric acid mainly include recrystallization method, esterification-distillation method, ion exchange method, electroche...

Claims

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Application Information

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IPC IPC(8): C01B35/10
CPCC01B35/109Y02P20/129
Inventor 李洪岭张宁红
Owner 青海利亚达化工有限公司
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