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A kind of preparation method of supported flower-shaped copper oxide and method for deep removal of phosphine in yellow phosphorus tail gas

A yellow phosphorus tail gas, copper oxide technology, applied in chemical instruments and methods, separation methods, other chemical processes, etc., can solve the problems of complex process, influence of purification efficiency, preparation complexity, etc. effect, good effect

Active Publication Date: 2017-12-01
WUHAN POLYTECHNIC UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The liquid-phase chemical oxidation adsorption method uses sodium hypochlorite, potassium permanganate, sulfuric acid, phosphoric acid and hydrogen peroxide to undergo liquid-phase oxidation with phosphine. This method has a certain purification effect, but the purification process will consume oxidants and the purification efficiency Affected by the concentration of oxidant, poor stability
[0004] Chinese patent CN00116136.9 proposes a method for purifying yellow phosphorus tail gas by pressure swing temperature swing adsorption, which utilizes the different adsorption effects of adsorbents on phosphine under different temperatures and pressures to achieve the purpose of separation and removal, but the equipment is complicated, And the regeneration process will consume part of the purified gas or use nitrogen containing trace oxygen, the process is more complicated
[0006] In Chinese patent CN201110457379.5, it is proposed to use metal phosphate or metal pyrophosphate as the catalytic active component and load it on the surface of activated carbon to avoid the problem of frequent regeneration of the catalyst, but the purification effect of the active component is not very prominent. The total phosphorus content in the yellow phosphorus tail gas exceeds 15ppm, and the deep purification cannot be completed
[0007] U.S. Patent US 5182088 proposes copper and zinc oxides as active components, adding Ag 2 O, HgO, and CdO can be used as accelerators to improve purification efficiency and adsorption capacity, but the price of Ag is high, and Hg and Cd are heavy metals with high pollution, which brings difficulties to preparation and use.
[0008] In Chinese patent CN200910095076.6, the purification effect of copper oxide is further improved by adding Ce and La, and relatively excellent purification efficiency and adsorption capacity are obtained, but this brings complexity in preparation
Most of the research focuses on the optimization of purification processes such as oxygen concentration, adsorption temperature, carrier, and environmental factors. There is a lack of research on the impact of controlling the morphology of the key active components of the catalyst to improve the adsorption effect. Its adsorption capacity and catalytic activity still need further research. Improvement and other issues

Method used

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  • A kind of preparation method of supported flower-shaped copper oxide and method for deep removal of phosphine in yellow phosphorus tail gas
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  • A kind of preparation method of supported flower-shaped copper oxide and method for deep removal of phosphine in yellow phosphorus tail gas

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Embodiment 1

[0038] Example 1, see figure 1 Shown:

[0039] The invention provides a preparation method of loaded flower-shaped copper oxide, comprising the following steps: crushing coconut shell activated carbon and sifting it into 20-40 meshes and putting it into a beaker, adding a certain amount of distilled water, heating to 80°C and washing for 1 hour, After washing, filter, then add 1M KOH solution for washing for 1h, after washing, put it in an oven for 12h at 110°C; disperse 200g of the above-mentioned activated carbon into 2.0L of water, stir for 1h to make it fully soaked and dispersed; In the mixture, add 100g CuCl to the solution while stirring 2 2H 20, then add 200g sodium citrate and 60g NaOH, fully stir for 4h; transfer the above mixed solution into the polytetrafluoro liner of the hydrothermal reaction kettle, then put the hydrothermal reaction kettle into the constant temperature drying box, The hydrothermal reaction was carried out at ℃ for 24 hours. After the reactio...

Embodiment 2

[0048] Example 2, such as figure 2 Shown:

[0049] The invention provides a preparation method of loaded flower-shaped copper oxide, comprising the following steps: crushing commercial ZSM-5 molecular sieves and sieving them into 20-40 meshes and putting them into a beaker, adding a certain amount of distilled water, and heating to 80 Wash at ℃ for 1 hour, filter after washing, then add 1M KOH solution for washing for 1 hour, put it in an oven for 12 hours at 110 ℃ after washing; take 200g of the treated ZSM-5 molecular sieve and disperse it into 1.5L of 1:1 volume ratio In the mixed solvent of ethanol and isopropanol, stir for 1 h to make it fully soaked and dispersed; in the above mixed solution, add 25g Cu(CH 3 COO) 2 ·H 2 O, then add 50g of sodium citrate and 15g of NaOH, and fully stir for 4h; transfer the above mixed solution into the polytetrafluoro liner of the hydrothermal reaction kettle, and then put the hydrothermal reaction kettle into a constant temperature d...

Embodiment 3

[0053] The invention provides a preparation method of loaded flower-shaped copper oxide, which comprises the following steps: crushing silica gel and sifting it into 20-40 meshes and putting it into a beaker, adding a certain amount of distilled water, heating to 80°C for 1 hour, and washing Filter, then add 1M KOH solution for washing for 1 hour, after washing, put it into an oven and dry it for 12 hours; disperse 200g of the above-mentioned treated silica gel into 2.0L ethanol, stir for 1 hour, make it fully infiltrated and dispersed, and form a mixed solution; In the mixed solution, add 50g Cu(NO 3 ) 2 ·3H 2 0, then add 500ml ammoniacal liquor (25%) and 40gNaOH, fully stir 4h; Above-mentioned solution is transferred in the PTFE liner of hydrothermal reactor, then hydrothermal reactor is put into constant temperature drying oven, at 180 The hydrothermal reaction was carried out at ℃ for 6 hours. After the reaction was complete, it was taken out and allowed to cool naturall...

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Abstract

The invention provides a preparation method of loaded flower-shaped copper oxide and a method for deeply removing phosphine in yellow phosphorus tail gas. The preparation of loaded flower-shaped copper oxide is carried out by hydrothermal method, including crushing of activated carbon or other porous materials. , sieving, dispersing, loading copper, hydrothermal reaction, suction filtration, drying, roasting and other preparation processes; the method of deep removal of phosphine in yellow phosphorus tail gas uses loaded flower-shaped copper oxide as the adsorbent, including pretreatment, Preheating, adsorption purification, cooling separation and other processes. The loaded flower-shaped copper oxide of the present invention has the ability to deeply purify phosphine, and can deeply remove the phosphine impurity in the yellow phosphorus tail gas to make the concentration less than 1ppm.

Description

technical field [0001] The invention relates to the technical field of purification treatment of yellow phosphorus tail gas, in particular to a preparation method of loaded flower-shaped copper oxide and a method for deep removal of phosphine in yellow phosphorus tail gas. Background technique [0002] my country is the main producer and supplier of yellow phosphorus in the world. Since 2000, my country has completely replaced the international monopoly position of the United States and Kazakhstan, occupying the yellow phosphorus market in Asia, Latin America and Africa. In recent years, the output of yellow phosphorus in my country has accounted for more than 50% of the world share, and the export volume over the years has accounted for about 15% of the output. According to statistical data, the total installed capacity of yellow phosphorus in the country is nearly 2 million t / a. Among them, Yunnan, Sichuan, Guizhou and Hubei are the main producing areas of yellow phosphoru...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/32B01J20/20B01D53/04
Inventor 任占冬杨明朱玉婵任占海许芳吴祯祯袁敏张标邓文星
Owner WUHAN POLYTECHNIC UNIVERSITY