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Heavy metal removal process used in zinc borate preparation process

A preparation process, a technology of zinc borate, applied in the field of halogen-free flame retardants, can solve the problems of excessive heavy metals in the final product, reducing the accumulation of heavy metals, changing the distribution ratio of heavy metals, etc., achieving controllable conditions, simple process operation, and strong operability effect of reproducibility and reproducibility

Inactive Publication Date: 2019-01-04
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that the heavy metal accumulation in the process from commercially available zinc sulfate to zinc borate products in the zinc borate production process causes the heavy metals in the final product to exceed the standard, the present invention divides the zinc borate production process into three sections to carry out the heavy metal removal and purification technology respectively, (1) Zinc sulfate purification: use active zinc powder to replace and purify the commercially available zinc sulfate, and initially remove most of the heavy metals (including Pb, Cd, Mn and other inactive heavy metals); (2) Zinc borate synthesis and purification : By adding sulfuric acid to the boric acid-zinc hydroxide synthetic zinc borate reaction system, the acidity of the system is enhanced, the distribution ratio of heavy metals in the mother liquor / zinc borate product is changed, and the accumulation of heavy metals in the product is reduced; (3) mother liquor purification: due to boric acid The zinc mother liquor needs to be recycled in the process, and the heavy metal impurities will accumulate batch by batch. In order to solve the problem of the mother liquor, it is necessary to further replace and purify the boric acid mother liquor with active zinc powder to reduce the heavy metals in the mother liquor to an acceptable range.

Method used

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  • Heavy metal removal process used in zinc borate preparation process
  • Heavy metal removal process used in zinc borate preparation process

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Add 460g (1mol) of zinc sulfate solution to the reaction bottle, start stirring, keep the system temperature at 25°C, add 2.3g of 80 mesh zinc powder, stir for 15min, separate to obtain purified zinc sulfate solution, add 250g (2mol) Add dropwise this zinc sulfate solution in 32% liquid caustic soda, 25 ℃ of stirring reaction 40min, filter to obtain zinc hydroxide filter cake, dry to obtain zinc hydroxide 99.1g; (2) to 719.19g (3.49mol) boric acid 14g of 98% concentrated sulfuric acid was added dropwise to the solution, then 99.1g (0.997mol) of zinc hydroxide prepared was added to the mixed solution, stirred and heated to 95°C for 6 hours, and the zinc borate product with low heavy metal content was separated and obtained. Mother liquor; (3) Add 2.5 g of 80-mesh zinc powder to the obtained boric acid mother liquor, stir at 45° C. for 10 minutes, filter and separate to remove heavy metals, and the boric acid mother liquor can be used mechanically.

Embodiment 2

[0023] (1) Add 460g (1mol) of zinc sulfate solution to the reaction bottle, start stirring, keep the system temperature at 25°C, add 0.4g of 80 mesh zinc powder, stir for 15min, separate to obtain purified zinc sulfate solution, add 250g (2mol) Add dropwise this zinc sulfate solution in 32% liquid caustic soda, 25 ℃ of stirring reaction 40min, filter to obtain zinc hydroxide filter cake, dry to obtain zinc hydroxide 99.1g; (2) to 719.19g (3.49mol) boric acid 11g of 98% concentrated sulfuric acid was added dropwise in the solution, then 99.1g (0.997mol) of the prepared zinc hydroxide was added to the mixed solution, the temperature was stirred to 95°C for 6h, and the zinc borate product with low heavy metal content was separated and obtained. Mother liquor; (3) Add 0.5 g of 80-mesh zinc powder to the obtained boric acid mother liquor, stir at 45° C. for 10 minutes, filter and separate to remove heavy metals, and the boric acid mother liquor can be used mechanically.

Embodiment 3

[0025] (1) Add 460g (1mol) of zinc sulfate solution to the reaction bottle, start stirring, keep the system temperature at 25°C, add 4.6g of 80-mesh zinc powder, stir for 15min, separate to obtain purified zinc sulfate solution, and add 250g (2mol) Add dropwise this zinc sulfate solution in 32% liquid caustic soda, 25 ℃ of stirring reaction 40min, filter to obtain zinc hydroxide filter cake, dry to obtain zinc hydroxide 99.1g; (2) to 719.19g (3.49mol) boric acid 17g of 98% concentrated sulfuric acid was added dropwise into the solution, then 99.1g (0.997mol) of zinc hydroxide prepared was added to the mixed solution, stirred and heated to 95°C for 6 hours, and the zinc borate product with low heavy metal content was separated and obtained. Mother liquor; (3) Add 5.0 g of 80-mesh zinc powder to the obtained boric acid mother liquor, stir at 45° C. for 10 minutes, filter and separate to remove heavy metals, and the boric acid mother liquor can be used mechanically.

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Abstract

The invention discloses a heavy metal removal process used in a zinc borate preparation process. The heavy metal removal process is achieved through three-stage control of zinc sulfate purification, zinc borate synthesis and purification and mother liquid purification, that is, the content of heavy metals introduced into a raw material, namely zinc sulfate, is controlled, a distribution ratio of the heavy metals to zinc borate is controlled, and the content of heavy metals in a mother liquid which is used indiscriminately in a circulation manner. By using the three-stage control method of source removal, process distribution and mother liquid accumulation, heavy metals in the whole zinc borate preparation process are removed, preparation of high-quality zinc borate of a low heavy metal content is achieved, and the competitiveness of the domestic zinc borate in international markets is greatly improved.

Description

technical field [0001] The invention relates to a heavy metal removal method, in particular to a heavy metal removal process in the preparation process of zinc borate. The invention belongs to the field of halogen-free flame retardants. Background technique [0002] Zinc borate (Zinc borate) is an environmentally friendly non-halogen flame retardant, depending on the composition (XZnO 3 ·YB 2 O3·ZH 2 O), there are more than a dozen varieties of zinc borate flame retardants. The most commonly used variety is 2335 type zinc borate, which has the characteristics of non-toxicity, low water solubility, high thermal stability and good dispersibility. [0003] As an efficient flame retardant, 2335 type zinc borate is widely used in plastics, rubber processing, transportation, aerospace, fiber fabrics, ceramic glazes, coatings and other fields. As a multifunctional synergistic additive of antimony oxide or other halogen flame retardants, it can effectively improve the flame ret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/12
CPCC01B35/127
Inventor 冯维春岳涛邢文国陈琦付永丰夏学强苏伟伟
Owner QINGDAO UNIV OF SCI & TECH
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