Method for preparing transitional metal ion copper modified adsorbent for purifying low-concentration phosphine

A transition metal ion, phosphine technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of complex process, consumption of oxidant, increase operation, control difficulty, etc., and achieve the effect of high adsorption activity

Inactive Publication Date: 2009-10-28
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 oxidizing agent (such as sodium hypochlorite, potassium permanganate, sulfuric acid, hydrogen peroxide, phosphoric acid, etc.) to realize the purification of phosphine. Consumption of oxidant, dephosphorization efficiency is closely related to oxidant concentration, while 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) has reported the method for washing out phosphine from acetylene gas, and this method uses 70% phosphoric acid solution, but this method flow process is complicated, and gas needs to pass through lime milk scrubber pretreatment, also needs consumption The scrubbing acid is regenerated with pure oxygen and no mention is made of the residual concentration of phosphine after scrubbing
[0006] Chinese patent CN 1398658A (publication number) discloses a method for purifying yellow phosphorus tail gas by catalytic oxidation in a fixed bed, and develops a series of catalysts for catalytic adsorption of pH

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0024] Example 1:

[0025] Take 10.00 g of activated carbon carrier with a certain particle size, ultrasonically wash it with deionized water, and then place it in a constant temperature drying oven to dry at a constant temperature of 110 °C for 24 hours, and then dry it at a constant temperature of 110 °C for 24 hours. Weigh 1.26g of Cu(SO 4 ) 2 ·5H 2 The O solid was dissolved in 50 ml of distilled water, then ultrasonically impregnated activated carbon for 0.5 h, dried in a constant temperature drying oven at 120 °C for 24 h, and then placed in a muffle furnace for activation at 400 °C for 6 h. The adsorption process conditions are: adsorbent 4.50g, temperature 70℃, space velocity 3000h-1, phosphine concentration in feed gas 650ppm, oxygen volume fraction 1.0%. This adsorbent is placed in a fixed bed reactor, and the efficiency of this adsorbent for phosphine purification is shown in the following table:

[0026] time (min)

Example Embodiment

[0027] Example 2:

[0028] Take 10.00 g of activated carbon carrier with a certain particle size, ultrasonically wash it with deionized water, and then place it in a constant temperature drying oven to dry at a constant temperature of 110 °C for 24 hours, and then dry it at a constant temperature of 110 °C for 24 hours. Weigh 0.86g of CuCl 2 ·2H 2 The O solid was dissolved in 50 ml of distilled water, then ultrasonically impregnated activated carbon for 0.5 h, dried in a constant temperature drying oven at 120 °C for 24 h, and then placed in a muffle furnace for activation at 400 °C for 6 h. The conditions of the adsorption process were: 5.25g adsorbent, 70°C temperature, 1500h-1 space velocity, 610ppm phosphine concentration in the feed gas, and 1.0% oxygen volume fraction. This adsorbent is placed in a fixed bed reactor, and the efficiency of this adsorbent for phosphine purification is shown in the following table:

[0029] time (min)

Example Embodiment

[0030] Example 3:

[0031] Take 10.00 g of activated carbon carrier with a certain particle size, ultrasonically wash it with deionized water, and then place it in a constant temperature drying oven to dry at a constant temperature of 110 °C for 24 hours, and then dry it at a constant temperature of 110 °C for 24 hours. Weigh 1.00g of Cu(CH 3 COO) 2 ·H 2 The O solid was dissolved in 50 ml of distilled water, then ultrasonically impregnated activated carbon for 0.5 h, dried in a constant temperature drying oven at 120 °C for 24 h, and then placed in a muffle furnace for activation at 400 °C for 6 h. The adsorption process conditions are: adsorbent 4.21g, temperature 70°C, space velocity 3000h-1, phosphine concentration in feed gas 850ppm, oxygen volume fraction 1.0%. This adsorbent is placed in a fixed bed reactor, and the efficiency of this adsorbent for phosphine purification is shown in the following table:

[0032] time (min)

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Abstract

The method relates to a method for preparing transitional metal ion copper modified adsorbent for purifying low-concentration phosphine, which is mainly used for removing low-concentration phosphine in industrial production tail gases and belongs to the technical field of application of adsorption separation technique in atmospheric pollution purification. The method comprises the following steps of: (1) carrying out ultrasonic washing and repeated drying treatment to an adsorbing material carrier until a constant-weight carrier is formed; (2) selecting a soluble copper salt to carry out ultrasonic immersing modification to the pretreated adsorbent carrier; (3) washing and drying the immersed adsorbent carrier; and (4) roasting the dried adsorbent carrier, and reducing the temperature to room temperature. The adsorbent prepared in the invention is unnecessary to add accelerating agents, such as noble metals or high-contamination heavy metals and the like; when the adsorbent is used for adsorbing waste gas containing phosphine, the adsorption is conducted by the surface of the modified adsorbent; waste gas dephophorization can be realized after the adsorption is saturated; and the adsorption activity is higher within in a certain temperature range.

Description

1. Technical field [0001] The invention relates to a preparation method of a transition metal ion copper modified adsorbent for purifying low-concentration phosphine, which is mainly used for removing low-concentration phosphine in industrial production tail gas, and belongs to the technical field of application of adsorption separation technology to air pollution purification . 2. Technical Background [0002] Phosphine gas is present in certain concentrations in the gases produced in the processes of yellow phosphorus preparation, magnesium powder preparation, sodium hypophosphite production, acetylene production, feed fermentation, grain fumigation, and semiconductor industry production. Direct discharge of phosphine gas in the tail 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 due to the presence o...

Claims

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Application Information

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IPC IPC(8): B01J20/32B01J20/20
Inventor 唐晓龙余琼粉易红宏宁平杨丽萍
Owner KUNMING UNIV OF SCI & TECH
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