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Method for recycling benzoic acid and crude terephthalic acid from PTA oxidation residues

A technology of crude terephthalic acid and benzoic acid is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., to achieve the effects of abundant raw material sources, easy operation, and easy large-scale production

Active Publication Date: 2016-06-22
福建洋屿环保科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides a method for recovering benzoic acid and crude terephthalic acid from PTA oxidation residue, which can effectively solve the problem of comprehensive recovery and utilization of solid waste resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 10kg recycled Co 2+ and Mn 2+ Add 30 kg of water to the final PTA oxidation residue, stir at 98° C. for 1 h, and filter while hot to obtain a hot filter cake. The filtrate is cooled for 1 h and then filtered to obtain a white precipitate. Recrystallize the white precipitate at 95°C, filter, dry, and pulverize to obtain the benzoic acid product. Add 20% NaOH solution to the hot filter cake, adjust the pH to 8.0 and filter. Add 360g activated carbon and 100ml15%H to the filtrate 2 o 2 , Stir at 50°C for 3h, and filter while hot. Add 5% H to the filtrate 2 SO 4 solution, adjust its pH value to 3.0, and filter after standing for 2 hours. The filter cake is washed and dried, that is, the crude terephthalic acid product.

Embodiment 2

[0025] 10kg recycled Co 2+ and Mn 2+ Add 25 kg of water to the final PTA oxidation residue, stir at 96° C. for 1.5 h, and filter while hot to obtain a hot filter cake. The filtrate is cooled for 2 h and then filtered to obtain a white precipitate. Recrystallize the white precipitate at 96°C, filter, dry, and pulverize to obtain the benzoic acid product. Add 15% NaOH solution to the hot filter cake, adjust the pH to 9.0 and filter. Add 300g of activated carbon and 200ml of 10%H to the filtrate 2 o 2 , Stir at 60°C for 2h, and filter while hot. Add 7% H to the filtrate 2 SO 4 Solution, adjust its pH value to 2.5, and filter after standing for 1.5h. The filter cake is washed and dried, that is, the crude terephthalic acid product.

Embodiment 3

[0027] 10kg recycled Co 2+ and Mn 2+ Add 40 kg of water to the final PTA oxidation residue, stir at 95°C for 2 hours, and filter while hot to obtain a hot filter cake. The filtrate is cooled for 1 hour and then filtered to obtain a white precipitate. Recrystallize the white precipitate at 98°C, filter, dry, and pulverize to obtain the benzoic acid product. Add 10% NaOH solution to the hot filter cake, adjust the pH to 8.0 and filter. Add 400g of activated carbon and 150ml of 30%H to the filtrate 2 o 2 , stirred at 70°C for 1h, and filtered while hot. Add 10% H to the filtrate2 SO 4 solution, adjust its pH value to 2.0, let it sit for 1 hour and then filter it. The filter cake is washed and dried, which is the crude terephthalic acid product.

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Abstract

The invention discloses a method for recycling benzoic acid and crude terephthalic acid from purified terephthalic acid (PTA) oxidation residues respectively. The method is characterized by comprising the following steps that 1, the utilized PTA oxidation residues are obtained after Co2+ and Mn2+ are recycled, and a small quantity of Fe2+ is removed; 2, the mentioned PTA oxidation residues are mixed with water, stirred for a period of time at a certain temperature and filtered while the mixture is still hot, hot filter cakes are obtained, filtrate stands still and filtered, and white sediment is obtained; 3, the white sediment is subjected to recrystallization, filtered, dried and crushed, and then a benzoic acid product is obtained; 4, a NaOH solution is added to the hot filter cakes obtained after treatment of step 2, the pH is regulated to 8.0-10.0, and filtering is conducted; 5, activated carbon and H2O2 are added to the filtrate obtained after treatment of step 4, the mixture is stirred for a period of time at a certain temperature and then filtered while the mixture is still hot; 6, a H2SO4 solution is added to the filtrate obtained after treatment in step 5, the pH value is regulated to 2.0-3.0, the mixture stands still and is filtered to obtain white flocculent sediment, washing and drying are conducted, and a crude terephthalic acid product is obtained. The method is simple in process and convenient to operate.

Description

technical field [0001] The invention relates to the technical field of comprehensive recovery and utilization of solid waste resources, in particular to a method for recovering benzoic acid and crude terephthalic acid from PTA oxidation residues. Background technique [0002] Purified terephthalic acid (PTA) is one of the important bulk organic raw materials. It is widely used in various fields of the national economy such as chemical fiber, light industry, electronics, and construction. At the same time, the application of PTA is mainly concentrated in polyethylene terephthalate. Production of polyester products such as glycol esters (referred to as polyester, PET), poly-1,4-butylene terephthalate (PBT) and poly-1,3-trimethylene terephthalate (PTT). According to statistics, more than 90% of the world's PTA is used in the production of PET. It can be seen that the downstream extension products of PTA are mainly polyester fibers, and the production of 1 ton of PET requires 0...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C51/43C07C63/06C07C51/487C07C63/26
CPCC07C51/42C07C51/43C07C51/487C07C63/06C07C63/26
Inventor 黄紫洋钟云峰钟云平邱妹妹原瑞泽
Owner 福建洋屿环保科技股份有限公司
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