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Method for recovering bromine from pure terephthalic acid (PTA) waste water

A waste water and bromine simple substance technology, which is applied in the direction of chemical instruments and methods, bromine/hydrogen bromide, organic compound preparation, etc., can solve the problems that PTA devices cannot be applied, and achieve reduction of adverse effects, reduction of bromine consumption, strong economy benefit effect

Inactive Publication Date: 2013-02-13
绍兴汉青环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have their own advantages and disadvantages, but due to the particularity of the PTA device, they cannot be directly applied to the PTA device.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The raw material waste water used in this embodiment comes from the pulping waste water of the blanking residue of the PTA device thin film evaporator, and sampling analysis shows that the bromide ion concentration in the sample is 1.5%wt;

[0021] This embodiment includes the following steps:

[0022] Step 1, take 500g of waste water, add hydrochloric acid to adjust the pH to 2, add 1000ml stirring reactor, slowly add 6g of 28% hydrogen peroxide dropwise to it, control the reaction temperature at 40°C, and install a condenser on the top of the reactor to prevent the generation of bromine simple substance out, the reaction ends after 1h;

[0023] Step 2, take the waste water after the reaction, add 250g p-xylene for the first extraction at 40°C; take the bottom aqueous phase of the first extraction, add 250g p-xylene for the second extraction at 40°C; take the second Add 250g p-xylene to the water phase at the bottom of the second extraction and carry out the third ext...

Embodiment 2

[0026] The raw waste water used in this embodiment is the same as that of Example 1, and the first step of the implementation steps is also the same, now the second step and the third step are described;

[0027] The 2nd step, get the waste water that has reacted, carry out purging with air, air flow rate is 10L / min, blows out gas and carries out five-stage absorption with acetic acid, and the consumption of every stage of acetic acid is 200g, through analyzing the 1st step and the 2nd step bromine The total recovery is 94%;

[0028] Step 3, dilute the concentration of bromine in the absorption liquid to 330mg / kg with acetic acid, add 1 / 3 of the mass of p-xylene, and add catalyst cobalt acetate and manganese acetate, the concentration of cobalt and manganese is the same as bromine, in 3L The p-xylene oxidation experiment was carried out in the titanium material experiment kettle. The experiment temperature was 180°C, the pressure was 20barg, the air flow rate was 10L / min, and ...

Embodiment 3

[0030] The raw waste water used in this embodiment is the same as in Example 1, and the first step of the implementation steps is also the same, now the second step and the third step are described

[0031] The 2nd step, take the waste water that has reacted, carry out purging with air, and air flow rate is 10L / min, and p-xylene is carried out five-stage absorption with p-xylene for blowing out gas, and the p-xylene consumption of every stage is 200g, after analyzing the first step and the second step The total yield of 2 steps of bromine is 93%;

[0032] Step 3: Dilute the concentration of bromine in the absorption solution to 1000 mg / kg with p-xylene, add 3 times the mass of acetic acid, and add catalyst cobalt acetate and manganese acetate. The concentration of cobalt and manganese is the same as that of bromine. The p-xylene oxidation experiment was carried out in the material experiment kettle, the experiment temperature was 180°C, the pressure was 20 barg, the air flow r...

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Abstract

The invention relates to a method for recovering bromine from pure terephthalic acid (PTA) waste water. The method includes oxidation, distillation and dilution for recovering. By means of the method, more than 90% of bromine ion can be distilled from the PTA waste water and then returned back to a PTA device for use, so that consumption of catalyst bromine is greatly reduced.

Description

technical field [0001] The invention relates to a method for recovering catalyst in a PTA production device, in particular to a method for recovering and utilizing bromine from PTA waste water. Background technique [0002] Purified terephthalic acid (PTA for short) is an important raw material for the production of polyester, which is currently produced mainly by air oxidation of p-xylene. The method is to dissolve p-xylene as a raw material in an acetic acid-water solvent containing catalyst cobalt acetate, manganese acetate and hydrogen bromide in a p-xylene oxidation reactor, and then pass air or enriched oxygen for oxidation to generate a solid product. Phthalic acid. In the production process, the catalyst hydrogen bromide needs to be continuously replenished due to consumption, and its consumption mainly includes: after the mother liquor evaporates and removes impurities, bromide ions enter the beating wastewater of the thin film evaporator blanking residue; the brom...

Claims

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Application Information

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IPC IPC(8): C01B7/09C07C63/26C07C51/265C02F9/04
Inventor 徐海波谢刚王献忠
Owner 绍兴汉青环保科技有限公司
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