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Method for high-value utilization of PTA residue high-concentration bromine-containing wastewater

A high-value waste water technology, applied in chemical instruments and methods, copper halides, water pollutants, etc., can solve the problems of difficult waste water treatment, high post-processing difficulty, and a large number of equipment, so as to realize high-value resource utilization Utilize, realize the process of resource utilization, and improve the effect of economic benefits

Active Publication Date: 2021-10-22
JIANGSU UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0007] Patented technology CN109371416B passes the pretreated bromine-containing wastewater into the electrolysis device, and the bromine-containing wastewater is passed through a direct current in the electrolysis device, and the bromine ions undergo an electrolysis reaction to generate elemental bromine; the extractant is contacted with the electrolyzed aqueous solution, and the phase recovery of elemental bromine; the extracted water phase is stripped to recover the extractant and then sent to the subsequent wastewater treatment unit. The whole process is complicated, and the amount of wastewater in the bromine removal process is large, and post-treatment is difficult.
Patent application CN102923663A acidifies the wastewater to a certain pH value and then adds an oxidant to oxidize the bromide ions in the wastewater to bromine element, then extracts the bromine solution by extraction and air blowing, and then dilutes the bromine element solution to a certain concentration with a solvent Returning to the PTA unit for use as a catalyst involves a large number of equipment and complicated processes
[0008] Patent application CN111087047A adds bromine-containing organic waste water into the electrolysis reactor, connects the power supply on the cathode and anode electrodes in the reactor, and reacts for a certain period of time. The bromide ions in the waste water are oxidized into bromine, and the bromine reacts with water rapidly. Generate highly oxidizing hypobromous acid, which can oxidize and degrade refractory organic matter in wastewater, achieve the purpose of reducing wastewater COD and improving the biodegradability of wastewater, the process is more complicated, and bromine cannot be fully utilized as a resource
[0009] The above treatment methods have disadvantages such as complicated process, low product purity, and difficult wastewater treatment.

Method used

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  • Method for high-value utilization of PTA residue high-concentration bromine-containing wastewater
  • Method for high-value utilization of PTA residue high-concentration bromine-containing wastewater
  • Method for high-value utilization of PTA residue high-concentration bromine-containing wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] First, add a sulfuric acid solution with a concentration of 2mol / L to adjust the pH of the PTA residue wastewater to 0.5, 1, 1.2, 1.5, and 2 respectively. At the same time, add an appropriate amount of distilled water to prepare the bromide ion concentration of PTA to 50g / L, and add cuprous oxide in batches. (adding in three times, 50wt% for the first time, 30wt% for the second time, 20wt% for the third time, each interval of 1min), the total copper oxide addition is based on NaBr and Cu 2 The molar ratio of O is calculated as 1:0.5. Under anaerobic conditions (nitrogen protection), 2mol / L sulfuric acid solution is continuously added to maintain its pH stability, and the stirring speed is 400r / min. Copper, centrifuged to obtain crude cuprous bromide, add a certain volume of sulfuric acid solution with pH = 2 to wash the solid phase crude product, centrifuge, repeat the operation once to obtain acid-washed cuprous bromide, then add a certain volume of absolute ethanol to ...

Embodiment 2

[0061] The operating steps are the same as in Example 1, and the selected pH is 1.2 at this time, changing NaBr: Cu 2 The O molar ratios were 1:0.45 and 1:0.55, respectively, and the results are shown in Table 2. It can be seen that different additions of cuprous oxide have a certain influence on the bromine removal rate, but the influence is not significant. But when NaBr:Cu 2 When O=1:0.55, the removal rate of bromine and product yield are the best.

[0062] Table 2. Effect of molar ratio on debromine effect

[0063] NaBr:Cu 2 o

[0064] Reaction conditions: Br - (50g / L), pH=1.2, room temperature, 5min, stirring speed 400r / min.

Embodiment 3

[0066] The operating steps are the same as in Example 1, and the selected pH is 1.2 at this time, changing NaBr: Cu 2 The O molar ratio was 1:0.55, and the reaction times were 3, 10, and 20 min, respectively. The results are shown in Table 3. It can be seen that increasing the reaction time can improve the bromine removal rate, but the improvement effect is very limited, and a good bromine removal effect can be obtained within 3 to 20 minutes, but the time is too short or too long to reduce the purity of the product.

[0067] The influence of table 3 stirring time on debromine effect

[0068] T / min 3 5 10 20 Bromine removal rate 95.1％ 97.1％ 97.5％ 98.1％ CuBr yield 91.4％ 92.6％ 92.8％ 93.5％ CuBr purity 93.2％ 95.8％ 95.3％ 90.2％ Na 2 SO 4 purity

[0069] Reaction conditions: Br - (50g / L), pH value=1.2, molar ratio NaBr: Cu 2 O=1:0.55, room temperature, stirring speed 400r / min.

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Abstract

The invention discloses a method for high-value utilization of PTA residue high-concentration bromine-containing wastewater, and belongs to the field of PTA residue treatment. The method comprises the following steps: firstly, adjusting the pH value of bromine-containing wastewater to 0.5-2, adding cuprous oxide in batches, performing reacting for 3-20 minutes after all cuprous oxide is added to generate cuprous bromide, carrying out solid-liquid separation to obtain a solid, carrying out acid washing, alcohol washing and drying to obtain cuprous bromide, concentrating a liquid phase to recover inorganic salt, and using the residual wastewater as process water for application, wherein the cuprous oxide is added in batches, namely the cuprous oxide is added in 2-5 times, and the interval of each time is 0.5-1 minute. By adding the cuprous oxide and regulating the method, the bromine removal rate reaches 95% or above, the yield of cuprous bromide reaches 90% or above, the purity can reach 95%, the cuprous bromide can be used as a high-value product, meanwhile, sodium sulfate with the purity reaching 90% or above can be obtained, and the high-value utilization of PTA residue high-concentration bromine-containing wastewater is truly achieved.

Description

technical field [0001] The invention relates to a method for high-value utilization of bromine-containing wastewater, in particular to a method for high-value utilization of bromine-containing wastewater with high concentration of PTA residues, and belongs to the field of PTA residue treatment. Background technique [0002] Purified terephthalic acid (PTA) is one of the important bulk organic raw materials, its main use is to produce polyester fiber (polyester), polyester bottle flakes and polyester film, widely used in chemical fiber, light industry , electronics, construction and other fields. With the development of society, the demand and production of PTA are gradually increasing, and the pollution of "three wastes" is becoming more and more serious. How to realize the efficient treatment and utilization of PTA residues is a huge environmental protection problem faced by its manufacturers. The content of bromine in the PTA residue washing wastewater of an enterprise in...

Claims

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Application Information

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IPC IPC(8): C02F9/04C01G3/04C01D5/02C02F101/12
CPCC02F9/00C01G3/04C01D5/02C02F2101/12C02F1/66C02F1/38C02F1/58C01P2006/80C01P2002/72C02F1/5236C02F2103/36C02F2209/06C02F2209/44C02F2103/34
Inventor 林伟李科陈霄峰梁国斌印霞棐周伟豪韦奕瞳周全法
Owner JIANGSU UNIVERSITY OF TECHNOLOGY
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