阅读说明：本技术 等离子裂解对硝基苯甲酰氯残液制备炭黑的方法 (Method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride residual liquid ) 是由 陈伟 余德平 张金刚 腾岩 王洁 薛攀 周廷廷 于 2019-09-24 设计创作，主要内容包括：本发明公开了一种等离子裂解对硝基苯甲酰氯残液制备炭黑的方法,包括：(1)将对硝基苯甲酰氯残液加热气化的步骤；(2)将气化后的残液直接喷入等离子裂解反应器的等离子火炬上,经高温裂解成炭黑以及裂解气；(3)将步骤(2)产生的炭黑以及裂解气依次通入余热回收器和喷雾急冷器,在喷雾急冷器降温后通入补集器,补集器收集炭黑；(4)将步骤(3)补集器排出的裂解气依次通入水洗塔和碱洗塔,再从烟囱排出。本发明采用环保的等离子系统进行废液的处理,该系统是一套密封循环和非焚化的过程,利用高能量密集的等离子场将废弃物的化学键分解并使其重组,转化成有价值的商品,无二噁英生成,并可以做到污染物的零排放。(The invention discloses a method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride residual liquid, which comprises the following steps: (1) heating and gasifying the paranitrobenzoyl chloride residual liquid; (2) directly spraying the gasified residual liquid onto a plasma torch of a plasma cracking reactor, and cracking the residual liquid into carbon black and cracking gas at high temperature; (3) sequentially introducing the carbon black and the pyrolysis gas generated in the step (2) into a waste heat recoverer and a spray quencher, introducing into a collector after the spray quencher is cooled, and collecting the carbon black by the collector; (4) and (4) introducing the cracked gas discharged by the supplementing and collecting device in the step (3) into a water washing tower and an alkali washing tower in sequence, and then discharging the cracked gas from a chimney. The invention adopts an environment-friendly plasma system to treat the waste liquid, the system is a set of sealed circulation and non-incineration process, and a high-energy dense plasma field is utilized to decompose and recombine chemical bonds of the waste and convert the chemical bonds into valuable commodities without generating dioxin, and zero emission of pollutants can be realized.)

1. A method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride raffinate is characterized by comprising the following steps:

(1) Heating and gasifying the paranitrobenzoyl chloride residual liquid;

(2) directly spraying the gasified residual liquid onto a plasma torch of a plasma cracking reactor, and cracking the residual liquid into carbon black and cracking gas at high temperature;

(3) Sequentially introducing the carbon black and the pyrolysis gas generated in the step (2) into a waste heat recoverer and a spray quencher, introducing into a collector after the spray quencher is cooled, and collecting the carbon black by the collector;

(4) And (4) introducing the cracked gas discharged by the supplementing and collecting device in the step (3) into a water washing tower and an alkali washing tower in sequence, and then discharging the cracked gas from a chimney.

2. The method for preparing carbon black by plasma cracking p-nitrobenzoyl chloride raffinate according to claim 1, wherein the raffinate in step (1) is heated and gasified by cracked gas in the waste heat recoverer in step (3).

3. the method for preparing carbon black by plasma cracking of p-nitrobenzoyl chloride raffinate as claimed in claim 1, wherein in step (2), the plasma torch inner flame temperature is 5000-7000 ℃, the outer flame temperature is 3000-5000 ℃, and the temperature of the discharged cracking gas after the gasified raffinate is subjected to high temperature cracking in the plasma cracking reactor is 1300-1500 ℃;

In the step, N ₂ is used as a carrier for plasma arcing;

The carbon black obtained by cracking is nano-scale particles.

4. The method for preparing carbon black by plasma cracking of p-nitrobenzoyl chloride raffinate as claimed in claim 1, wherein in step (3), the cracked gas is subjected to waste heat recovery in a waste heat recovery device, and is subjected to primary cooling by heat exchange with the raffinate, and is subjected to secondary cooling to a temperature of between 180 and 200 ℃ by a spray quencher, and the carbon black is subjected to waste heat recovery in the waste heat recovery device under the drive of non-condensable gases N ₂, CO ₂ and NO ₂, is cooled to a temperature of between 180 and 200 ℃ in the spray quencher, and is collected in a bag type collector.

5. The method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride raffinate according to claim 1, wherein in the step (4), the caustic washing tower uses 25% sodium hydroxide solution to carry out caustic washing on cracked gas, and fuel gas enriched with CO and H ₂ is obtained after the caustic washing.

Technical Field

The invention relates to a method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride residual liquid.

Background

The paranitrobenzoyl chloride is an important intermediate for synthesizing vitamin medicinal products such as folic acid, procaine hydrochloride, N-p-aminobenzoyl-L-glutamic acid and the like, and is also widely applied to the production of pigments and color developers. Particularly, in recent years, with the rise of the feed industry and the development of the information industry, the dosage of the paranitrobenzoyl chloride is increasing.

The common synthetic method is that the paranitrobenzoic acid and thionyl chloride are in reflux reaction under the action of a catalyst or the paranitrobenzoic acid and phosphorus trichloride are introduced to react under the condition that carbon tetrachloride is used as a solvent to prepare the compound.

no matter which synthetic route is adopted, the finally obtained product needs to be distilled and purified, materials such as p-nitrobenzoic acid and the like which do not react completely can be subjected to a certain condensation reaction in the heating and distillation process to generate macromolecular substances, and meanwhile, a certain amount of p-nitrobenzoyl chloride product remains at the bottom of the kettle to form organic waste liquid.

The organic waste liquid has complex composition, strong corrosivity and instability, and can generate a large amount of toxic and harmful media such as hydrogen chloride and the like through chemical reaction when meeting water and even moist air. The residual liquid cannot be treated by a physical and common chemical method, but can be treated only by burning, but because a large amount of chlorine and oxygen exist in the molecular structure, and the temperature of common burning can only reach 1200 ℃, harmful substances such as dioxin and the like are easily formed in the burning process, and serious damage can be caused to human bodies and the environment.

disclosure of Invention

the invention provides a method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride residual liquid, aiming at solving the problem that the existing organic waste liquid containing paranitrobenzoyl chloride generates dioxin during incineration treatment, and the method comprises the following steps:

(1) heating and gasifying the paranitrobenzoyl chloride residual liquid;

(2) Directly spraying the gasified residual liquid onto a plasma torch of a plasma cracking reactor, and cracking the residual liquid into carbon black and cracked gas consisting of H ₂, excess N ₂, a small amount of O, CL recombined trace CO, CO ₂, H ₂ O, NO ₂, CL ₂ and the like in a high temperature manner;

(3) Sequentially introducing the carbon black and the pyrolysis gas generated in the step (2) into a waste heat recoverer and a spray quencher, introducing into a collector after the spray quencher is cooled, and collecting the carbon black by the collector;

(4) And (4) introducing the cracked gas discharged by the supplementing and collecting device in the step (3) into a water washing tower and an alkali washing tower in sequence, and then discharging the cracked gas from a chimney.

Preferably, the residual liquid in the step (1) is heated to 300 ℃ by high-temperature pyrolysis gas in a step (3) waste heat recoverer and gasified.

Preferably, the plasma torch inner flame temperature in the step (2) is 5000-7000 ℃, the outer flame temperature is 3000-5000 ℃, and the temperature of the discharged pyrolysis gas is 1300-1500 ℃ after the gasified residual liquid is subjected to high-temperature pyrolysis in the plasma pyrolysis reactor;

in the step, N ₂ is used as a carrier for plasma arcing, the pressure of an arcing gas is 0.3-0.4MPa, and the flow rate of the arcing gas is 4-5m ³/h;

The carbon black obtained by cracking is nano-scale particles.

preferably, the pyrolysis gas in the step (3) recovers waste heat in a waste heat recoverer, exchanges heat with the residual liquid to perform primary temperature reduction, is sprayed by water mist through a spray quencher to perform secondary temperature reduction to 180-class 200 ℃, and the residual liquid is directly and monoatomic cracked into carbon black, so that the particle size of the carbon black is nano-scale, the carbon black enters the spray quencher to be cooled to 180-class 200 ℃ after being subjected to waste heat recovery by the waste heat recoverer under the drive of a small amount of non-condensable gas N ₂, CO ₂ and NO ₂, and then enters a bag type collector to be collected, the collected carbon black is sold as a commodity, and if the temperature is too low, water vapor is condensed into liquid, so that clear water appears, the carbon black is difficult to collect, and the corrosivity is strong.

Preferably, in the step (4), the caustic washing tower uses 25% sodium hydroxide solution to carry out caustic washing on the cracked gas, fuel gas enriched with CO and H ₂ is obtained after the caustic washing, and the fuel gas is recycled as energy at the outlet of a chimney.

The invention has the beneficial effects that:

The invention adopts an environment-friendly plasma system to treat the waste liquid, the system is a set of sealed circulation and non-incineration process, and a high-energy dense plasma field is utilized to decompose and recombine chemical bonds of the waste and convert the chemical bonds into valuable commodities without generating dioxin, and zero emission of pollutants can be realized.

Drawings

the invention will now be described, by way of example, with reference to the accompanying drawings, in which:

FIG. 1 is a schematic of the present invention.

Detailed Description

The present invention will now be described in further detail with reference to the accompanying drawings. These drawings are simplified schematic views illustrating only the basic structure of the present invention in a schematic manner, and thus show only the constitution related to the present invention.

as shown in figure 1, the method for preparing carbon black by plasma cracking of paranitrobenzoyl chloride raffinate comprises the following steps:

(1) heating and gasifying the paranitrobenzoyl chloride residual liquid to 300 ℃;

(2) Directly spraying the gasified residual liquid onto a plasma torch of a plasma cracking reactor, wherein the inner flame temperature of the plasma torch is 5000-fold 7000 ℃, the outer flame temperature is 3000-fold 5000 ℃, the gasified residual liquid is cracked into nano carbon black particles and cracking gas consisting of H ₂, excessive N ₂, a small amount of O, CL recombined trace amount of CO, CO ₂, H ₂ O, NO ₂, CL ₂ and the like through the plasma cracking reactor at high temperature, in the step, N ₂ is used as a carrier for plasma arc striking, the pressure of the arc striking gas is 0.3-0.4MPa, the flow of the arc striking gas is 4-5m ³/H, and the temperature of the discharged cracking gas is 1300-fold 1500 ℃;

(3) sequentially introducing the carbon black and the pyrolysis gas generated in the step (2) into a waste heat recoverer and a spray quencher, recovering waste heat of the pyrolysis gas in the waste heat recoverer, performing primary cooling by exchanging heat with residual liquid, performing secondary cooling to 180-class heat by spraying water mist through the spray quencher, wherein the particle size of the carbon black is nano-scale, recovering the waste heat by the waste heat recoverer under the drive of a small amount of non-condensable gas N ₂, CO ₂ and NO ₂, then cooling to 180-class heat 200 ℃ in the spray quencher, then collecting the carbon black in a bag type collector, and selling the collected carbon black as a commodity;

(4) and (3) sequentially introducing the cracked gas discharged by the supplementing and collecting device in the step (3) into a water washing tower and an alkali washing tower, wherein hydrochloric acid collected from the water washing tower can be sold as a byproduct, the alkali washing tower adopts 25% sodium hydroxide solution to carry out alkali washing on the cracked gas, fuel gas enriched with CO and H ₂ is obtained after alkali washing, the fuel gas is recycled as energy at the outlet of a chimney, and the salt collected by the alkali washing tower is pollution-free after evaporation and can be treated as general waste.

in light of the foregoing, it is to be understood that various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.