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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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

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

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Example Embodiment

[0020] Example 1:

[0021] The raw walnut shells are crushed to a particle size of 0.5~1cm and washed, and dried at 100°C until constant weight; the washed and dried raw walnut shells are carbonized in a tube furnace under nitrogen protection for 1 hour, and the carbonization temperature is 600°C. The heating rate is 10℃ / min; the carbonized material and the activator potassium hydroxide are mixed uniformly in a certain proportion, and then they are placed in a tube furnace for nitrogen protection and activation for 1 hour. The mass ratio of the carbonized material to the activator potassium hydroxide is 1 :2, the activation temperature is 800℃, the heating rate is 10℃ / min; wash the activated walnut shell sample with 0.1mol / L hydrochloric acid twice, and rinse with hot distilled water to neutrality, the washed sample is constant weight at 110℃ Then the walnut shell activated carbon is obtained; the walnut shell activated carbon is subjected to metal loading modification treatment,...

Example Embodiment

[0024] Example 2:

[0025] The raw walnut shells are crushed to a particle size of 0.5~1cm and washed, and dried at 100°C until constant weight; the washed and dried raw walnut shells are carbonized in a tube furnace under nitrogen protection for 1 hour, where the carbonization temperature is 700°C. The heating rate is 20℃ / min; the carbonized material and the activator potassium hydroxide are mixed uniformly according to a certain ratio, and then they are placed in a tube furnace for nitrogen protection and activation for 1 hour. The mass ratio of the carbonized material to the activator potassium hydroxide is 1 :2, the activation temperature is 900℃, the heating rate is 15℃ / min; the activated walnut shell samples are washed twice with 0.1mol / L hydrochloric acid, and rinsed with hot distilled water to neutrality, the washed sample is constant weight at 110℃ Then the walnut shell activated carbon is obtained; the walnut shell activated carbon is subjected to metal loading modifica...

Example Embodiment

[0028] Example 3:

[0029] The raw walnut shells are crushed to a particle size of 0.5~1cm and washed, and dried at 100°C until constant weight; the washed and dried raw walnut shells are carbonized in a tube furnace under nitrogen protection for 1 hour, where the carbonization temperature is 700°C. The heating rate is 5℃ / min; the carbonized material and the activator potassium hydroxide are mixed uniformly in a certain proportion, and then they are placed in a tube furnace for nitrogen protection and activation for 1 hour. The mass ratio of the carbonized material to the activator potassium hydroxide is 1 :4, the activation temperature is 700℃, the heating rate is 20℃ / min; wash the activated walnut shell sample with 0.1mol / L hydrochloric acid twice, and rinse with hot distilled water to neutrality, the washed sample will be constant weight at 110℃ Then the walnut shell activated carbon is obtained; the walnut shell activated carbon is subjected to metal loading modification trea...

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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

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Claims

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Application Information

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Owner KUNMING UNIV OF SCI & TECH
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