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Combined purification method of o/p-chlorobenzaldehyde rectification raffinate and process wastewater

A p-chlorobenzaldehyde and rectification technology, which is applied in chemical instruments and methods, separation methods, water/sewage treatment, etc., can solve the problems of high process energy consumption, difficulty in industrialization, and high cost, and achieve low energy consumption and low cost. cost, the effect of achieving heat balance

Active Publication Date: 2017-08-04
南京资环工程技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process consumes a lot of energy and uses palladium as a catalyst, which is expensive and difficult to realize industrialization.

Method used

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  • Combined purification method of o/p-chlorobenzaldehyde rectification raffinate and process wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Get 500mL of o-chlorobenzaldehyde rectification raffinate, add 0.05g propylene glycol fatty acid ester (dispersant) and 2823mL process waste water, disperse 40min in dispersing kettle under 50 ℃, obtain the dispersion liquid that viscosity is 12mPa s; The calorific value of the liquid is 30000kJ / kg, and the COD in the process wastewater is 17000mgO 2 / L.

[0034] Catalytic cracking oxidation catalyst in fluidized bed is PtO 2 -MnO 2 / ZSM-5, the catalyst is prepared by spray drying method, the preparation method: mix 18gH 2 PtCl 6 and 400ml of 50% Mn(NO 3 ) 2 Dissolve the solution in 300ml of water, immerse 1000g of ZSM-5 molecular sieve in the above aqueous solution for 12 hours, add 100g of silica sol and stir evenly, spray into a spray dryer, dry at 120°C, and roast at 550°C for 3h to obtain a composite oxide catalyst , the catalyst particle size is 60-200μm, PtO 2 The loading amount is 1%, MnO 2 The loading capacity is 15%;

[0035] The catalytic oxidation c...

Embodiment 2

[0038] Take 500mL of rectification raffinate of o-chlorobenzaldehyde, add 0.07g glyceryl monostearate (dispersant) and 2000mL process wastewater, and disperse in a dispersion kettle for 50min at 50°C to obtain a dispersion with a viscosity of 23mPa·s; The heat value of distillation raffinate is 32000kJ / kg, and the COD in process wastewater is 18000mgO 2 / L.

[0039] Catalytic cracking oxidation catalyst in fluidized bed is PtO 2 -CrO 3 / Y, the catalyst is prepared by spray drying method, the preparation method: mix 18gH 2 PtCl 6 and 263g Cr(NO 3 ) 3 9H 2 O was dissolved in 300ml water, 1000gY molecular sieve was immersed in the above aqueous solution for 12h, then 100g of silica sol was added and stirred evenly, sprayed into a spray dryer, dried at 120°C, and calcined at 550°C for 3h to obtain a composite oxide catalyst, catalyst Particle size is 60~200μm, PtO 2 The loading amount is 1%, Cr 2 o 3 10% of the load;

[0040] The catalytic oxidation catalyst used in the...

Embodiment 3

[0043] Take 500mL of rectification raffinate of o-chlorobenzaldehyde, add 0.7g glyceryl monostearate (dispersant) and 1739mL process wastewater, and disperse in a dispersing kettle for 30min at 60°C to obtain a dispersion with a viscosity of 41mPa·s; The calorific value of the distillation raffinate is 16800kJ / kg, and the COD in the process wastewater is 9000mgO 2 / L.

[0044] The catalytic cracking oxidation catalyst in the fluidized bed is Cr 2 o 3 / Y, the catalyst is prepared by spray drying method, the preparation method: 790gCr(NO 3 ) 3 9H 2 O was dissolved in 300ml of water, 1000g of Y molecular sieve was immersed in the above aqueous solution for 12h, then 100g of aluminum sol was added and stirred evenly, sprayed into a spray dryer, dried at 120°C, and calcined at 550°C for 3h to obtain a composite oxide catalyst. Catalyst particle size is 60~200μm, Cr 2 o 3 The loading capacity is 15%;

[0045] The catalytic oxidation catalyst used in the fixed bed is CuO / Al ...

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Abstract

The invention discloses a combined purification method of o / p-chlorobenzaldehyde rectification raffinate and process wastewater. The method concretely comprises the following steps: adding a dispersant to the rectification raffinate and process wastewater to reduce the viscosity in order to form a dispersion; allowing the dispersion to enter a fluidized bed reactor and undergo catalytic cracking oxidation, and allowing the obtained dispersiont o enter a fixed bed reactor and undergo catalytic oxidation purification; carrying out heat transfer condensation and gas-liquid separation on the obtained fixed bed outlet gas, allowing the obtained liquid to enter a neutralization tank, neutralizing HCl and Cl2 dissolved in the liquid by a diluted alkali solution, discharging neutralized liquid to a rain discharging system, allowing the gas to enter an alkali solution absorption tower to absorb HCl and Cl2 in the gas, and directly discharging the absorbed gas to air. The method allows the rectification raffinate and process wastewater to be simultaneously treated at a low temperature through a raffinate emulsification-fluidized bed catalytic cracking oxidation-fixed bed catalytic oxidation purification technology, the content of VOCs in the treated gas is less than 45 mg / m<3>, the content of CODs in the liquid does not exceed 80 mg O2 / L, and the high-efficiency, low-cost and low-energy consumption treatment of the rectification raffinate and the process wastewater is realized in a one-step manner.

Description

technical field [0001] The invention relates to a method for purifying chlorine-containing organic matter, which belongs to the technical field of environmental protection, and in particular to a method for combined purification of o / p-chlorobenzaldehyde rectification raffinate and process wastewater. Background technique [0002] O- / p-chlorobenzaldehyde is an important fine chemical intermediate, which has a wide range of uses in new pesticides, medicines, dyes and other organic synthesis. At present, the industry mainly uses o / p-chlorotoluene as raw material, and adopts chlorination hydrolysis to synthesize o / p-chlorobenzaldehyde. [0003] During the production process of o- / p-chlorotoluene chlorination hydrolysis, distillation raffinate and process wastewater will be produced. Taking the production of o-chlorobenzaldehyde as an example, after the chlorinated mixture is hydrolyzed and rectified, there will be a black rectification residue in the kettle, accounting for abo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/04B01D53/78B01D53/44C02F101/36C02F103/36
CPCB01D53/44B01D53/78C02F1/66C02F1/725C02F2101/36C02F2301/08C02F2209/03C02F2209/02C02F2209/06C02F2209/08C02F2103/36B01D2257/708
Inventor 乔旭费兆阳李磊陈献刘清崔咪芬汤吉海张竹修
Owner 南京资环工程技术研究院有限公司
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