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Method for recovering titanium from waste hydrochloric acid generated in production of titanium dioxide by chlorination process

A technology of titanium dioxide and waste hydrochloric acid, which is applied in the field of titanium recovery, can solve the problems of many stages, high price and consumption of neutral phosphorus-type extractants, achieve large extraction saturation capacity, realize resource reuse, and eliminate environmental pollution Effect

Active Publication Date: 2014-05-07
CITIC JINZHOU METAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the chemical precipitation method are: a large amount of raw materials are consumed, a large amount of sludge is produced, waste acid and valuable elements are not comprehensively utilized
Acidic extractants have good selectivity to titanium, but the extraction speed is relatively slow, generally taking 1h to 2h, which is not suitable for industrial applications; neutral phosphorus extractants have poor selectivity to titanium, and neutral phosphorus extractants The agent is expensive, the medium-strength alkaline extractant (such as N1923) has low extraction saturation, the extraction time is 20min to 30min, the extraction tank is large, and the number of stages is large

Method used

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  • Method for recovering titanium from waste hydrochloric acid generated in production of titanium dioxide by chlorination process

Examples

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Effect test

Embodiment 1

[0016] 1) Take 5L of molten salt for chlorination to produce titanium dioxide waste hydrochloric acid (component HCl: 25.2%, Ti: 21.8 g / L), and use a composite extractant (15%LK-N21 +5 % isoamyl alcohol + 80% sulfonated kerosene), the said LK-N21 has a direct or branched chain with 14-24 carbon molecules and a relative molecular mass of 300-400; the three-stage Extraction, compared to O:A=2:3, mixing time 1min, clarification time 5min, extract titanium in hydrochloric acid into organic phase, after extraction, get purified hydrochloric acid (containing Ti: 0.1 g / L) and negative titanium The organic phase;

[0017] 2) Using a mixed solution of 0.5mol / L sulfuric acid and 0.8mol / L hydrogen peroxide as the stripping agent, the negative titanium organic phase was subjected to five-stage stripping in a countercurrent contact at 10°C. Compared with O:A= 3:2, mixing time 3min, clarification time 10min, back-extract titanium from negative titanium organic phase to water phase, after b...

Embodiment 2

[0019] 1) Take 5L of boiling chlorination to produce titanium dioxide by-product hydrochloric acid (component HCl: 28.5%, Ti: 24.3 g / L), and use a composite extractant (15%LK-N21+5 %LK-N21X+80% propane), said LK-N21 is a direct chain or branched chain with 14-24 carbon molecules and a relative molecular mass of 300-400; three-stage extraction is carried out by means of countercurrent contact at 10°C, Compared with O:A=1:2, the mixing time is 3 minutes, the clarification time is 3 minutes, and purified hydrochloric acid (containing Ti: 0.05 g / L) is obtained after extraction;

[0020] 2) Using a mixed solution of 0.6mol / L sulfuric acid and 0.6mol / L hydrogen peroxide as the stripping agent, the negative titanium organic phase was subjected to five-stage stripping in a countercurrent contact at 20°C, compared to O:A=3: 2. The mixing time is 5 minutes, and the clarification time is 5 minutes. The titanium is back-extracted from the negative titanium organic phase to the water phas...

Embodiment 3

[0022] 1) Take 5L of molten salt for chlorination to produce titanium dioxide by-product hydrochloric acid (HCl: 24.5%, containing Ti: 23.6 g / L), and use a composite extractant (15%LK-N21 + 5% multi-branched hexadecyl tertiary carbon primary amine (Primene JMT molecular weight 297.5) + 80% carbon tetrachloride), the LK-N21 carbon molecule number is 14-24 straight or branched chain, relative molecular mass 300~400; three-stage extraction was carried out by means of countercurrent contact at 30°C, compared to O:A=1:2, mixing time 3min, clarification time 5min, purified hydrochloric acid (containing Ti: 0.12 g / L );

[0023] 2) Using a mixed solution of 0.5 mol / L hydrochloric acid and 1 mol / L hydrogen peroxide as the stripping agent, the negative titanium organic phase is subjected to five-stage stripping in a countercurrent contact at 30°C, compared to O:A=3:2 , the mixing time is 3 minutes, and the clarification time is 10 minutes. After stripping, a titanium-containing soluti...

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Abstract

The invention discloses a method for recovering titanium from waste hydrochloric acid generated in production of titanium dioxide by a chlorination process. The method comprises the following steps of: carrying out extraction reaction by using a countercurrent contact mode of the titanium dioxide and waste hydrochloric acid in production of the titanium dioxide by the chlorination process, extracting the titanium in the hydrochloric acid into an organic phase and obtaining hydrochloric acid and an organic phase of negative titanium; adopting acid liquor added with hydrogen peroxide as reverse extraction liquor, carrying out reverse extraction according to the countercurrent contact mode, reversely extracting the titanium from the organic phase of the negative titanium into a water phase and obtaining titanium-containing solution and an organic phase. The method disclosed by the invention has the advantages that the characteristic of low-temperature selective extraction is achieved, the extraction time is short, the saturation capacity of extraction is large and the number of extraction stages is less; recovery and utilization of resources such as the titanium and the hydrochloric acid are realized, the emission of the waste acid is reduced, the reutilization of the resources is realized and the environmental pollution is eliminated.

Description

technical field [0001] The invention relates to a method for recovering titanium from waste hydrochloric acid produced by chlorination to produce titanium dioxide. Background technique [0002] Titanium dioxide is an important chemical raw material and occupies an important position in the national economy. The chlorination process to produce titanium dioxide mainly includes molten salt chlorination and boiling chlorination. Each ton of titanium dioxide produces 0.5t-0.6t of waste hydrochloric acid (HCl: 20%-30%, Ti: 20 g / L-30 g / L). Waste hydrochloric acid containing titanium impurities has no use value. Usually, waste hydrochloric acid is discharged directly after simple neutralization treatment, which not only causes waste of resources, but also seriously pollutes the environment. [0003] Titanium mainly exists in three forms of TiO2+, TiOCl+, and TiOCl2 in the waste hydrochloric acid medium. With the increase of hydrochloric acid concentration or chloride ion concentr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B3/40C22B34/12
CPCY02P10/20
Inventor 齐牧崔传海赵华王向阳庄立军杨锦铭梁职王志敏马锦红
Owner CITIC JINZHOU METAL
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