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Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine

A technology of activated carbon adsorption and walnut shell, applied in chemical instruments and methods, separation methods, other chemical processes, etc., can solve the problems of small adsorption capacity, consumption of oxidants, and the remaining concentration of phosphine is not mentioned, and achieve high adsorption activity. , the effect of saving processing costs

Inactive Publication Date: 2012-04-25
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
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Problems solved by technology

[0005] The oxidation-reduction absorption method uses the reducing property of phosphine to react with a solution containing an oxidant (such as sodium hypochlorite, potassium permanganate, concentrated sulfuric acid, hydrogen peroxide, phosphoric acid, etc.) to purify phosphine. Consumption of oxidant, dephosphorization efficiency is closely related to oxidant concentration, and the concentration of oxidant drops rapidly during the absorption reaction, so there are disadvantages such as high operating cost, easy fluctuation of dephosphorization efficiency, and poor operability of the device
Chinese patent CN 85105317 (publication number) reports a method for washing phosphine from acetylene gas. This method uses 70% phosphoric acid solution, but the process is complicated, and the gas needs to be pretreated by a milk of lime scrubber. The scrubbing acid is regenerated with pure oxygen and no mention is made of the residual concentration of phosphine after scrubbing
Considering that the adsorption capacity of blank activated carbon for phosphine is poor, in order to improve the adsorption effect of activated carbon for phosphine, the researchers modified activated carbon by acid-base modification, vulcanization modification and metal modification. Generally speaking, the adsorption capacity of activated carbon adsorbents for phosphine is small. The saturated adsorption capacity of activated carbon adsorbents prepared in previous studies for phosphine is only about 140mg / g. Therefore, the development of adsorption capacity for phosphine Larger activated carbon adsorbent becomes the key content of the present invention
In recent years, the preparation of activated carbon from agricultural and forestry wastes has attracted the attention of many researchers, but the use of activated carbon prepared from walnut shells from agricultural and forestry wastes to purify low-concentration phosphine has not been reported.

Method used

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  • Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine

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Experimental program
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Effect test

Embodiment 1

[0021] The raw walnut shells were crushed to a particle size of 0.5-1 cm, washed, and dried at 100°C until constant weight; the washed and dried raw walnut shells were carbonized in a tube furnace for 1 hour under nitrogen protection, and the carbonization temperature was 600°C. The heating rate is 10°C / min; the carbonized material and the activator potassium hydroxide are mixed evenly in a certain proportion, and then placed in a tube furnace for activation under nitrogen protection for 1 hour, wherein the mass ratio of the carbonized material to the activator potassium hydroxide is 1 : 2, the activation temperature is 800°C, and the heating rate is 10°C / min; the walnut shell activation sample is washed twice with 0.1mol / L hydrochloric acid, and rinsed to neutrality with hot distilled water, and the washed sample is constant at 110°C After that, walnut shell activated carbon is obtained; the walnut shell activated carbon is modified by metal loading, and the metal active compo...

Embodiment 2

[0025]The raw walnut shells were crushed to a particle size of 0.5-1 cm, washed, and dried at 100°C until constant weight; the washed and dried raw walnut shells were carbonized in a tube furnace for 1 hour under nitrogen protection, and the carbonization temperature was 700°C. The heating rate is 20°C / min; the carbonized material and the activator potassium hydroxide are mixed evenly in a certain proportion, and then placed in a tube furnace for activation under nitrogen protection for 1 hour, wherein the mass ratio of the carbonized material to the activator potassium hydroxide is 1 : 2, the activation temperature is 900°C, and the heating rate is 15°C / min; the walnut shell activation sample is washed twice with 0.1mol / L hydrochloric acid, and rinsed to neutrality with hot distilled water, and the washed sample is constant at 110°C After that, walnut shell activated carbon is obtained; the walnut shell activated carbon is modified by metal loading, and the metal active compon...

Embodiment 3

[0029] The raw walnut shells were crushed to a particle size of 0.5-1 cm, washed, and dried at 100°C until constant weight; the washed and dried raw walnut shells were carbonized in a tube furnace for 1 hour under nitrogen protection, and the carbonization temperature was 700°C. The heating rate is 5°C / min; the carbonized material and the activator potassium hydroxide are mixed evenly in a certain proportion, and then placed in a tube furnace for activation under nitrogen protection for 1 hour, wherein the mass ratio of the carbonized material to the activator potassium hydroxide is 1 : 4, the activation temperature is 700°C, and the heating rate is 20°C / min; the walnut shell activation sample is washed twice with 0.1mol / L hydrochloric acid, and rinsed to neutrality with hot distilled water, and the washed sample is constant at 110°C After that, walnut shell activated carbon is obtained; the walnut shell activated carbon is modified by metal loading, and the metal active compon...

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Abstract

The present invention discloses a preparation method for a walnut shell active carbon adsorbent for purifying low concentration phosphine. According to the preparation method, a walnut shell raw material is subjected to treatments of crushing, washing and drying; the treated walnut shells are placed in a tube type furnace to carry out carbonization for 1 hour at a certain temperature under protection of nitrogen to obtain a carbonized material; the carbonized material is uniformly mixed with an activator potassium hydroxide according to a certain ratio; the resulting mixture is place in the tube type furnace to carry out activation for 1 hour at a certain temperature under protection of nitrogen; the walnut shells are washed by hydrochloric acid, and rinsed by hot distilled water until the pH value of the walnut shells is neutral, then the walnut shells are dried to obtain the walnut shell active carbon; the walnut shell active carbon is subjected to a metal supported modification treatment, wherein metal active components comprise copper, zinc and lanthanum; then treatments of ultrasonic impregnation, drying and baking are performed to prepare the walnut shell active carbon adsorbent. The walnut shell active carbon adsorbent is characterized in that: with adopting the walnut shell active carbon adsorbent to treat the waste gas containing the phosphine, advantages of high purification efficiency, large adsorption capacity, low cost and the like are provided; the development of the adsorbent provides a simple and feasible approach for comprehensive utilization of the agricultural and forestry waste walnut shells and purification of the phosphine waste gas.

Description

technical field [0001] The invention relates to a walnut shell activated carbon adsorbent for purifying low-concentration phosphine and a preparation method thereof, belonging to the technical field of material preparation technology applied to air pollution purification. technical background [0002] Phosphine is present in certain concentrations in the gases produced in processes such as yellow phosphorus preparation, magnesium powder preparation, sodium hypophosphite production, acetylene production, feed fermentation, grain fumigation, and semiconductor industry production. Direct discharge of phosphine in the exhaust gas into the atmosphere will cause environmental pollution and endanger human health. If the phosphine-containing tail gas, especially the yellow phosphorus tail gas rich in CO, is utilized, the catalyst will be poisoned by the presence of phosphine, which seriously restricts the resource utilization of waste. Phosphine is included in the US EPA's list of ...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/30B01D53/02
Inventor 易红宏余琼粉唐晓龙宁平杨丽萍张艳
Owner KUNMING UNIV OF SCI & TECH
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