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Method and device for purifying, absorbing and recycling chlorinated gas in benzene chlorination process

A technology for chlorinating tail gas and benzene, applied in chemical instruments and methods, separation methods, chlorine/hydrogen chloride and other directions, can solve the problems of not realizing the effective utilization of hydrogen chloride, removing by-product hydrogen chloride gas, increasing processing costs, etc. The effect of improving the economic benefit of the enterprise, improving the product yield and saving the processing cost

Active Publication Date: 2016-10-12
ZHEJIANG RUNTU NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the use of water and alkali washing directly removes chlorine and hydrogen chloride gas in the tail gas, which does not realize the effective utilization of hydrogen chloride, and is accompanied by the generation of organic acids and salty wastewater
[0005] Patent document CN 101077466A discloses a method for recovering and recycling the tail gas containing benzene and hydrogen chloride in the production of chlorinated benzene. The benzene gas is condensed, gas-liquid separated, and the captured benzene is sent to the chlorinated benzene workshop. The concentrated hydrochloric acid produced is analyzed by the desorption tower and then enters the low-temperature condenser for condensation. The concentrated sulfuric acid is dried, and the dried hydrogen chloride gas is sent to the polyvinyl chloride VCM The synthesis production line has achieved that almost all the benzene and hydrogen chloride entrained in the chlorinated benzene tail gas are recovered and recycled, but the captured chlorinated benzene is acidic chlorinated benzene, which needs to be neutralized before returning to the chlorinated benzene production system Therefore, it is bound to be accompanied by the generation of organic wastewater and high-salt wastewater; in addition, the tail gas containing hydrogen chloride is absorbed by water or low-concentration acid, and the organic matter will inevitably enter the hydrochloric acid solution, and the hydrogen chloride gas obtained by the analysis of concentrated hydrochloric acid with organic matter must be Contains organic matter, and whether the organic matter contained will affect the subsequent PVC products. The inventor has no experimental data to verify. At the same time, it increases the number of processing steps and increases the processing cost to a certain extent.
[0006] Another patent document CN 102849681A realizes the removal of chlorine gas contained in the by-product hydrogen chloride gas in the organic chloride production process, but the method needs to be equipped with a purification liquid, and does not remove the by-product hydrogen chloride gas generated in the organic by-product process. Organic matter works, therefore, the hydrogen chloride gas produced should contain organic matter, the patent does not explicitly mention

Method used

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  • Method and device for purifying, absorbing and recycling chlorinated gas in benzene chlorination process
  • Method and device for purifying, absorbing and recycling chlorinated gas in benzene chlorination process
  • Method and device for purifying, absorbing and recycling chlorinated gas in benzene chlorination process

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Effect test

Embodiment 1

[0060] (1) Synthesis of ethyl chloride

[0061] The first batch: Add 107kg of alcohol and 224kg of water to the reactor, then add 600kg of zinc chloride, beat for 0.5h, and then pass in 102kg of hydrogen chloride gas obtained by purifying the chlorination tail gas, after the addition, slowly raise the temperature to 80°C for 3h, then raise the temperature Heat at 100°C for 3 hours, then raise the temperature to 110°C for 2 hours, and stop the reaction when the weight of the reaction pot remains basically unchanged. The mixed gas coming out of the reaction kettle is cooled to about 50°C by primary cooling, buffered, and cooled to 30°C by secondary cooling, first-stage water absorption, secondary water absorption, finished product cooling and condensation to about 0°C, and water separator separation. The finished product ethyl chloride has a content of 99.5% as detected by gas chromatography, and 128 kg of ethyl chloride is obtained by weighing, with a yield of 85.3%.

[0062] ...

Embodiment 2

[0068] Preparation of N-cyanoethylaniline

[0069] Add 2g of hydroquinone, 5g of tetraethylammonium chloride, and 855g of bottom water into a 3L reaction kettle, add 10.0g of crystalline aluminum trichloride and make a slurry, and slowly inject 25g of chlorinated tail gas after the aluminum trichloride is completely dissolved Purify the obtained hydrogen chloride gas, then slowly add 466g of aniline under stirring, raise the temperature to 45°C, slowly add 300g of acrylonitrile dropwise under stirring, slowly raise the temperature to 85°C after the dropwise addition, keep it for 12h, then raise the temperature to 90°C and keep it for 8h .

[0070] After the reaction was completed, the layers were separated after standing still for 1 hour. The organic phase was distilled to recover acrylonitrile, cooled and filtered, and the obtained solid was N-cyanoethylaniline product, and then the product was analyzed by liquid chromatography, aniline = 0.46%, N- Cyanoethylaniline=97.4%, N...

Embodiment 3

[0086] (1) Preparation of Disperse Blue 291:3 filter cake

[0087] Add 3800kg of nitrosyl sulfuric acid and 800kg of 98% sulfuric acid into the reactor, and add 2,4-dinitro-6-chloroaniline and 2,4-dinitro-6-bromoaniline with a mass ratio of 3:1 2000kg, stir to dissolve, control the temperature at 25-30°C to react, use starch potassium iodide test paper to detect the reaction end point, and obtain the diazonium salt solution. Add 2600kg (dried) 2-methoxy-5-acetylamino-N, N-diallylaniline and 5kg Pingpingjia O-15 to 32 tons of sulfuric acid aqueous solution with an acid value of 8%, beat for 2 hours use. Slowly add the above-prepared diazonium salt solution into the prepared coupling solution, add 20 tons of ice, and carry out the coupling reaction at -5 ~ 0°C. After the reaction is completed, press filter, and the filtrate is 46 tons of mother liquor water. The filter cake is washed with water until the neutral disperse blue 291:3 filter cake is 12 tons, and the water content...

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Abstract

The invention discloses a method and device for purifying, absorbing and recycling chlorinated gas in a benzene chlorination process. The method comprises the steps that end gas produced in benzene chlorination reaction is led to a buffer tank, the gas from the buffer tank directly flows into a cascade reaction unit containing solid ferrous chloride for dechlorination and debenzolization, the end gas subjected to dechlorination and debenzolization enters a primary low-temperature heat exchange system, the cooled end gas enters a cascade dryer containing concentrated sulfuric acid for drying, the dried end gas enters a secondary low-temperature heat exchange system, the hydrogen chloride gas from the secondary low-temperature heat exchange system enters a finished product tank with a demister. The method utilizes the ferrous chloride to absorb chlorine gas in the end gas and convert the chlorine gas into ferric trichloride, the ferric trichloride catalyzes benzene and chlorine gas reaction to generate chlorinated benzene, a reactant is directly fed into a chlorinated benzene workshop for reuse, the end gas subjected to dechlorination and debenzolization is dried and purified by the concentrated sulfuric acid, sulfuric acid obtained through drying can be directly reused for disperse dye synthesis, efficient utilization of the chlorinated end gas is achieved, and the green, low-carbon and cyclic development requirements are met.

Description

technical field [0001] The invention relates to the technical field of waste gas treatment, in particular to a method and device for purification, absorption and recycling of chlorination tail gas in a benzene chlorination process. Background technique [0002] Chlorinated benzene and dichlorobenzene are generally produced through the chlorination reaction of benzene and chlorine, so the chlorination tail gas usually contains a large amount of hydrogen chloride, as well as non-condensable gases such as benzene, chlorine, nitrogen, and hydrogen. A large amount of hydrogen chloride gas produced in the production process of chlorinated benzene and dichlorobenzene will not only cause waste of resources, but also cause serious harm to the environment. Therefore, for the tail gas produced by the chlorination process of benzene, it is of great practical significance to research and develop a method that can effectively recover hydrogen chloride and other useful components. It can n...

Claims

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Application Information

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IPC IPC(8): B01D53/81B01D53/86B01D53/72B01D53/68B01D53/75C01B7/07
CPCB01D53/263B01D53/28B01D53/75B01D53/81B01D53/8659B01D53/8668B01D2251/60B01D2255/20738B01D2257/2025B01D2257/7027C01B7/0706
Inventor 周杰文刘伟高国泉傅哉荣
Owner ZHEJIANG RUNTU NEW MATERIAL CO LTD
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