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A combined purification method of process wastewater and rectification raffinate in the production process of aniline

A production process and wastewater technology, applied in chemical instruments and methods, neutralized water/sewage treatment, natural water treatment, etc., can solve the problems of strict operating environment requirements, low efficiency, high energy consumption, and reduce the difficulty of operation, The effect of reducing energy consumption, process environmental protection and energy saving

Active Publication Date: 2020-06-26
NANJING RESOURCES & ENVIRONMENT ENG TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In view of the problems existing in the above-mentioned prior art, the object of the present invention is to: provide a combined purification method of process wastewater and rectification raffinate in the production process of aniline, to solve the problem of high cost, high energy consumption, low efficiency, Strict operating environment requirements and other issues

Method used

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  • A combined purification method of process wastewater and rectification raffinate in the production process of aniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 500 mL of aniline rectification raffinate, 0.25 mL of glycerol monostearate and 3150 mL of wastewater into the emulsification kettle, stir and emulsify at 30 °C for 0.8 h to obtain an emulsion with a viscosity of 3.2 mPa·s; among them, the rectification raffinate The calorific value is 30000 kJ / kg, and the COD of wastewater is 19500 mgO 2 / L.

[0046] 0.05 kg 100-200 mesh LaMnO catalyst for fluidized bed reactor pyrolysis oxidation 3 The catalyst is prepared by a sol-gel method. Weigh 0.01 mol of lanthanum nitrate and 0.01 mol of manganese nitrate dissolved in 18 mL of deionized water and stir for 0.5 h, add 0.2 mol of citric acid and stir for 0.5 h, evaporate the solvent at 80 °C to form a gel, and place the gel in 100 ℃ oven for 12 h to form a xerogel. Then the xerogel was calcined at 800 °C for 6 h to form LaMnO 3 catalyst.

[0047] 0.05 kg 40-60 mesh LaCoO as the deep catalytic oxidation catalyst in fixed bed reactor 3 The catalyst is prepared by a sol-gel...

Embodiment 2

[0051] Add 500 mL of aniline rectification raffinate, 0.80 mL of propylene glycol fatty acid ester and 2400 mL of waste water into the emulsification kettle, stir and emulsify at 35 °C for 0.8 h to obtain an emulsion with a viscosity of 30 mPa·s; among them, the calorific value of the rectification raffinate is 25000 kJ / kg, and the COD of wastewater is 28000 mgO 2 / L.

[0052] 0.05 kg 100-200 mesh LaFeO for fluidized bed reactor pyrolysis oxidation catalyst 3 The catalyst is prepared by a sol-gel method. Weigh 0.01 mol lanthanum nitrate and 0.01 mol ferric nitrate dissolved in 18 mL deionized water and stir for 0.5 h, add 0.2 mol citric acid and stir for 0.5 h, evaporate the solvent at 80 °C to form a gel, and place the gel in 100 ℃ oven for 12 h to form a xerogel. Then the xerogel was calcined at 800 °C for 6 h to form LaFeO 3 catalyst.

[0053] The deep catalytic oxidation catalyst in the fixed bed reactor is 0.05 kg 40-60 mesh LaCrO 3 The catalyst is prepared by a sol...

Embodiment 3

[0057] Add 500 mL of aniline rectification raffinate, 1.10 mL of diethylene glycol monooleate and 2050 mL of waste water into the emulsification kettle, stir and emulsify at 45 °C for 0.8 h to obtain an emulsion with a viscosity of 110 mPa·s; among them, the rectification The heat value of raffinate is 24800kJ / kg, and the COD of waste water is 11000 mgO 2 / L.

[0058] 0.05 kg 100-200 mesh LaNiO catalyst for fluidized bed reactor pyrolysis oxidation 3 The catalyst is prepared by a sol-gel method. Weigh 0.01 mol of lanthanum nitrate and 0.01 mol of nickel nitrate dissolved in 18 mL of deionized water and stir for 0.5 h, add 0.2 mol of citric acid and stir for 0.5 h, evaporate the solvent at 80 °C to form a gel, and place the gel in 100 ℃ oven for 12 h to form a xerogel. Then the xerogel was calcined at 800 °C for 6 h to form LaNiO 3 catalyst.

[0059] 0.05 kg 40-60 mesh LaCuO catalyst for deep catalytic oxidation in fixed bed reactor 3 The catalyst is prepared by a sol-gel...

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Abstract

The invention discloses a combined purification method for process wastewater and rectification residue in an aniline production process. The method comprises the following steps: (1) stirring and emulsifying an emulsifier, process wastewater and rectification residue; (2) introducing emulsion from the top of a fluidized bed reactor, introducing preheated air from the bottom of the fluidized bed reactor, and enabling the emulsion to carry out a cracking and oxidation reaction under the actions of oxygen and a catalyst; (3) introducing gases cracked and oxidized by the fluidized bed reactor into a fixed bed reactor, performing deep catalytic oxidation under the catalyst effect, and producing oxidation reaction gases; (4) introducing the oxidation reaction gases into a heat exchanger to exchange heat with air, and introducing the preheated air into the bottom of the fluidized bed reactor; (5) cooling the oxidation reaction gases subjected to heat exchange, neutralizing the condensate with dilute alkali, enabling the neutralized condensate to directly enter a rainwater drain system, and directly draining non-condensable gases. According to the method disclosed by the invention, the aniline wastewater and rectification residue can be efficiently treated at low cost and low energy consumption, the discharge standard is directly reached after treatment, and secondary purification treatment is not needed.

Description

technical field [0001] The invention belongs to the field of chemical waste treatment and relates to a combined purification method of process wastewater and rectification raffinate in the production process of aniline. Background technique [0002] Aniline is an important organic chemical raw material and fine chemical intermediate, which is widely used in medicine, printing and dyeing, agriculture, paint, military industry and other industries. At present, the most important method for the industrial production of aniline is the catalytic hydrogenation of nitrobenzene, as follows: [0003] . [0004] In the production of aniline, the process wastewater mainly comes from the reduction process of nitrobenzene, and the rectification raffinate is unavoidable in the process of aniline refining. [0005] Both process wastewater and rectification raffinate contain aniline, and aniline is a "three-cause" substance that seriously pollutes the environment and endangers human hea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F9/04C02F103/36
CPCC02F1/66C02F1/725C02F9/00C02F2103/36C02F2301/08
Inventor 乔旭费兆阳王亮亮王明洪陈献刘清崔咪芬汤吉海张竹修
Owner NANJING RESOURCES & ENVIRONMENT ENG TECH RES INST CO LTD