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Recovery processing method of titanium-containing waste liquid

A technology for recycling and processing titanium waste liquid, which is applied in water/sewage treatment, chemical instruments and methods, heating water/sewage treatment, etc. It can solve the problems of waste of resources, increase the cost of waste liquid treatment, overflow of hydrogen chloride gas, etc. Ease of handling, avoidance of fouling and blocking tendency, improved recovery effect

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this treatment method produces a series of resource and environmental problems: a large amount of waste residue and waste liquid are produced; corrosive hydrogen chloride gas overflows due to incomplete absorption, causing environmental pollution; since titanium tetrachloride cannot be recycled, cause unnecessary waste of resources
Although this method improves the recovery rate of titanium tetrachloride in the waste liquid to a certain extent, it is necessary to add a thin film evaporator to realize the invention, which will greatly increase the treatment cost of the waste liquid

Method used

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  • Recovery processing method of titanium-containing waste liquid

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Experimental program
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Effect test

Embodiment 1

[0026] Add 1000ml of titanium-containing waste liquid produced by the polyolefin catalyst and 1000ml of phenol into the premix tank 1, then fully stir and mix evenly. The obtained mixed liquid is transferred to the still 2 through pipelines for distillation. The temperature of the tower bottom is controlled at 145-150°C, and the distillation time is 60 minutes. The titanium tetrachloride fraction at the top of the tower is collected and reused in the production process. Then the residual liquid in the still 2 is transferred to the recovery unit 3 through the pipeline, and 15% sodium hydroxide solution is added for hydrolysis treatment. Until the pH value of the mixed system is stabilized at 6.5, the layer is separated into a phenol layer and a hydrolyzate layer after standing, and the phenol and hydrolyzate are recovered. Phenol can be used back in distillation still 2. The rate of recovery of titanium tetrachloride is 98.5% in this embodiment.

Embodiment 2

[0028] Add 500 ml of titanium-containing waste liquid from polyolefin catalyst production and 1,000 ml of phenol into premix tank 1, then fully stir and mix evenly. The obtained mixed liquid is transferred to the still 2 through pipelines for distillation. The temperature of the tower kettle is controlled at 137-145°C, and the distillation time is 90 minutes. The titanium tetrachloride fraction at the top of the tower is collected and reused in the production process. Then transfer the residual liquid of the still 2 to the recovery unit 3 through the pipeline, add 5% sodium hydroxide solution for hydrolysis, until the pH value of the mixed system is stable at 6.0, let stand and separate, phenol and hydrolysis After liquid separation, phenol can be recovered for distillation still 2. The rate of recovery of titanium tetrachloride is 97.2% in this embodiment.

Embodiment 3

[0030] Add 1000 ml of titanium-containing waste liquid from polyolefin catalyst production and 500 ml of phenol into the premix tank 1, then fully stir and mix evenly. The obtained mixed liquid is transferred to the still 2 through pipelines for distillation. The temperature of the tower bottom is controlled at 155-160°C, and the distillation time is 30 minutes. The titanium tetrachloride fraction at the top of the tower is collected and reused in the production process. Then the tower still raffinate of still 2 is transferred in the recovery unit 3 through pipeline, adds 30% sodium hydroxide solution and carries out hydrolysis treatment. Until the pH value of the mixed system is stable at 7.0, the mixture is allowed to stand for stratification. After the phenol and hydrolyzate are separated, the phenol can be recovered and used in the still 2. The rate of recovery of titanium tetrachloride is 97.6% in this embodiment.

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Abstract

The invention discloses a recovery processing method of titanium containing waste liquid. The method comprises following steps: (1) adding an organic solvent into titanium-containing waste liquid, and fully mixing with the titanium-containing waste liquid; (2) distilling the obtained mixture in a distillation device, and separating titanium tetrachloride from the top of the distillation device; (3) adding an alkali solution in the residual mixed solution in the distillation device, and then carrying out a hydrolysis treatment to recycle the organic solvent. The recovery processing method avoids the scaling and obstruction tendencies in the conventional distillation process, and is capable of increasing recovery rate of titanium tetrachloride in the titanium-containing waste liquid. The recovery rate of titanium tetrachloride rises by 97% or more by adopting the recovery processing method. Furthermore, after the distillation treatment the distilled residual liquid contains little titanium tetrachloride, thus the waste liquid is easy to process, and the processing cost is low.

Description

technical field [0001] The invention belongs to the field of industrial waste liquid treatment, and relates to a treatment method for titanium-containing waste liquid, in particular to a recovery and treatment method for titanium-containing waste liquid produced in the production process of polyolefin catalysts. Background technique [0002] In the polyolefin industry, the most widely used Ziegler-Natta catalyst is a high-efficiency magnesium chloride carrier catalyst based on magnesium chloride, which mainly uses magnesium chloride as the carrier, titanium tetrachloride as the active component, and internal and external electron donors. composition. As we all know, in the preparation process of Ziegler-Natta catalyst, a large amount and excessive amount of titanium tetrachloride need to be used, so in addition to the output catalyst product, a large amount of titanium-containing mother liquor will be produced in the production process, which contains unreacted Titanium tet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F1/04C02F1/62C22B34/12C01G23/02
CPCY02P10/20
Inventor 程学文李海龙李昕阳高凤霞
Owner CHINA PETROLEUM & CHEM CORP
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