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A process for recovering bromine element from the mother liquor extraction liquid in the oxidation process of a terephthalic acid production unit

A technology for terephthalic acid and production equipment, which is applied in the field of bromine element recovery, and can solve the problems of increased equipment footprint, increased cumulative concentration, and increased operating consumption

Active Publication Date: 2021-10-08
佰仕邦水处理环保科技(大连)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0024] The aqueous solution obtained by treating the mother liquor extraction liquid through a series of means no matter how to choose the route c-Ⅰ, c-Ⅱ, c-Ⅲ, c-Ⅳ, c-Ⅴ, c-VI (including c-VI-a, c-VI- b or c-VI-c) is processed, and the solution that finally needs to be returned to the oxidation reaction system contains a certain concentration of BA, and the concentration is relatively high. BA is an impurity for the oxidation reaction system, which will affect the product quality of the oxidation process. Therefore, in order to avoid the adverse effects of the oxidation reaction system (the mother liquor in the oxidation process) that the cumulative concentration of BA in the overall oxidation reaction system (the mother liquor in the oxidation process) continues to increase significantly due to the high concentration of BA brought back by this part, it is necessary to increase the amount of the mother liquor in the oxidation process. Increasing the amount of the mother liquor extraction liquid in the oxidation process will lead to: (1) the equipment of the acetic acid removal unit of the mother liquor extraction liquid in the oxidation process needs to be increased (because the mother liquor extraction liquid (mainly acetic acid according to the concentration) treated by the acetic acid removal unit (increased amount), resulting in an increase in equipment cost and an increase in the area occupied by the equipment; (2) the operating consumption of the acetic acid removal unit equipment increases (the processing capacity of the mother liquor extract (mainly acetic acid according to the concentration) processed by the acetic acid removal unit increases), and the consumption increases ( e.g. steam consumption)

Method used

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  • A process for recovering bromine element from the mother liquor extraction liquid in the oxidation process of a terephthalic acid production unit
  • A process for recovering bromine element from the mother liquor extraction liquid in the oxidation process of a terephthalic acid production unit
  • A process for recovering bromine element from the mother liquor extraction liquid in the oxidation process of a terephthalic acid production unit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0127] Sampling of the mother liquor extract from the oxidation process of the terephthalic acid production plant was filtered through a conventional 5um filter, and then placed to cool down to normal temperature (at that time, the normal temperature was about 20°C), and filtered with an ultrafiltration membrane to obtain the liquid (this example 1 is referred to as liquid A in 1), sampling 800L, analysis composition: acetic acid 86.51%, cobalt ion 571ppm, manganese ion 328ppm, bromide ion 1100ppm, BA 16213ppm, 4-CBA 273ppm, PT acid 753ppm, sodium ion 61ppm, iron ion 6.2ppm , chromium ion 0.93ppm, nickel ion 2.76ppm.

[0128] experiment one

[0129] Liquid A is adsorbed by "resin with adsorption capacity for bromine under the condition of acetic acid solvent", the resin is filled with 10L, the flow rate of liquid A after resin treatment is controlled to 30L / hour, and the concentration in the acetic acid solution after resin treatment at different times is analyzed As shown in t...

Embodiment 2

[0177] Sampling of the filtrate from the oxidation process of the terephthalic acid production plant "the mother liquor extract was passed through the acetic acid removal unit by evaporation, and then the residual mixture was beaten with water and the temperature was lowered to about 95°C, followed by a 5um filter", and then cooled To room temperature (the room temperature was about 20°C at that time), filtrate I was obtained by ultrafiltration membrane filtration, the analysis composition: TA 7569ppm; BA6201ppm; 4-CBA 321ppm; PT acid 433ppm; sodium ion 2572ppm; cobalt ion 3842ppm; 3288ppm; iron ion 4.21ppm; chromium ion 0.46ppm; nickel ion 2.03ppm; acetic acid and its acid radical 12235ppm.

[0178] experiment one

[0179] Treat the filtrate I through the nanofiltration unit A, control the amount of water. Nanofiltration unit A fresh water: nanofiltration unit A concentrated water = 4:1, analyze the nanofiltration unit A fresh water sample: TA4135ppm; BA3162ppm; 4-CBA206ppm; ...

Embodiment 3

[0210] experiment one

[0211] The filtrate I of sampling embodiment 2 is 500L, adding sodium carbonate to promote PH=5.7 to produce a large number of bubbles, no obvious change in volume, with 13 kilograms of sodium carbonate, obtain filtrate II with ultrafiltration, analyze filtrate II: TA7601ppm; BA6188ppm; 4- CBA312ppm; PT acid 419ppm; sodium ion 13059ppm; cobalt ion 3675ppm; manganese ion 3284ppm; bromide ion 3237ppm; iron ion 0.25ppm; chromium ion 0.03ppm;

[0212] Conclusion: In the process of adding sodium carbonate, the concentrations of TA, BA, 4-CBA, PT acid, acetic acid and their acid radicals hardly decrease, and the concentrations of iron ions, chromium ions, and nickel ions decrease to some extent (the ratio of nickel removal to iron ions, chromium ions ions are low).

[0213] Experiment 2

[0214] Treat the filtrate II through the nanofiltration unit B, control the fresh water of the nanofiltration unit B: concentrated water of the nanofiltration unit B = 4:1...

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Abstract

The invention provides a process for recovering bromine element from the mother liquor extraction liquid in the oxidation process of a terephthalic acid production device, which belongs to the field of process recovery. The mother liquor extraction liquid of the oxidation process of the terephthalic acid production unit mainly contains acetic acid according to the material content, that is, acetic acid is used as a solvent to dissolve relatively low concentrations of cobalt ions, manganese ions, bromide ions, BA, sodium ions, iron ions, 4‑ CBA, PT acid, etc., apply the present invention to extract the bromine element therein to obtain the form recovery of hydrobromic acid or sodium bromide, reclaim the economic value of the bromine element; also avoid the bromine discharge of this part in the prior art and enter the sewage , bromine will have adverse effects on the biological flora of the sewage treatment unit and affect the activity of the biological flora.

Description

technical field [0001] The invention belongs to the field of process recovery, and in particular relates to a process for recovering bromine element from the mother liquor extraction liquid in the oxidation process of a terephthalic acid production device. Background technique [0002] Terephthalic acid is an important raw material for polyester production, so it has a wide range of industrial applications. The main production process of terephthalic acid is divided into two processes: oxidation and refining. [0003] In the oxidation process, the raw material p-xylene reacts with oxygen in the air in an oxidation reactor to generate terephthalic acid. During the reaction process, additional elements such as cobalt, manganese, and bromine are added as catalysts, and acetic acid is used as a solvent. The product terephthalic acid obtained after the reaction is separated from the solution containing acetic acid, cobalt, manganese, bromine, etc., and the solid is crude terepht...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B7/09C01D3/10C07C51/265C07C63/26C07C51/43C07C51/42C07C53/08
CPCC01B7/093C01D3/10C07C51/265C07C51/42C07C51/43C07C63/26C07C53/08
Inventor 李玉宽
Owner 佰仕邦水处理环保科技(大连)有限公司
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