Preparation method of self-cleaning water treatment filler

Abstract

The present application relates to a kind of preparation methods of self-cleaning water treatment filler, belong to environmental pollution purification material field.The method is first pickled stainless steel pail ring, the zinc ferrite film is generated after electrode reaction of pickled stainless steel pail ring, finally the zinc ferrite film is coated stainless steel pail ring is immersed into solution, and the pail ring of zinc ferrite-aluminum oxide composite coating, i.e.self-cleaning water treatment filler is obtained.The present application is by scientific design and optimization to raw material and preparation process, and zinc ferrite-aluminum oxide composite coating is prepared on stainless steel pail ring, the relative mass percentage content of zinc ferrite-aluminum oxide in the coating is optimized scientifically, so that self-cleaning water treatment filler has ideal purification organic pollutant activity, and can be widely used in the treatment process of various organic pollutants in water.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of environmental pollution purification materials, and particularly relates to a preparation method of a self-cleaning water treatment filler. BACKGROUND

[0002] There are a large number of organic pollutants in industrial and domestic wastewater, and the types of organic pollutants are various and pose great harm to the natural environment and human health. Wastewater polluted by such pollutants must be subjected to deep treatment before being discharged into natural water bodies.

[0003] Fillers are used in the process of biochemical treatment of organic pollutants. The fillers can trap pollutants in wastewater, and the microorganisms attached to the fillers can decompose and purify the trapped organic pollutants. Since some organic pollutants are highly toxic, they directly affect the efficiency of biochemical treatment and need to be treated by other methods.

[0004] Photocatalytic oxidation technology is widely used in the treatment of organic pollutants in the environment. Photocatalytic oxidation can degrade various organic pollutants, and this method can replace the role of microorganisms in the biochemical treatment process. It is an urgent technical problem to prepare water treatment fillers with photocatalytic purification activity. SUMMARY

[0005] In view of the problems existing in the prior art, the present application aims to provide a preparation method of a self-cleaning water treatment filler, which can be used for the purification treatment of organic pollutants in water.

[0006] A preparation method of a self-cleaning water treatment filler, comprising the following process steps:

[0007] Step 1: pickling of stainless steel Pall ring

[0008] (1) immerse the stainless steel Pall ring in a 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities on the stainless steel Pall ring;

[0009] (2) wash the stainless steel Pall ring treated above with pure water and dry at 80℃ for 2 h to obtain pickled stainless steel Pall ring;

[0010] Step 2: electrode reaction to generate zinc ferrite film

[0011] (1) add 320-360 mL of pure water, 20-23 mL of acetic acid, 10-12 g of ethylenediaminetetraacetic acid disodium salt and 15-17 g of zinc chloride in a beaker to form solution A;

[0012] (2) connect the anode of a 12V power supply to the stainless steel Pall ring and the cathode to a titanium plate, immerse the two electrodes in solution A, control the current between the two electrodes at 1.8 A, and power on for 15 min;

[0013] (3) The stainless steel Baoer ring after electrode reaction is cleaned with pure water, dried at 80℃ for 2h, and calcined at 260-280℃ for 1h to obtain a zinc ferrite film coated stainless steel Baoer ring;

[0014] Step 3: Sol-gel method for coating alumina film

[0015] (1) 4.5-5.3g emulsifier OP-10, 7.2-8.3g aluminum isopropoxide, and 2.7-3.1g dodecyl trimethyl ammonium bromide are added into 120-130mL ethanol to form solution B;

[0016] (2) 1.1-1.2mL concentrated hydrochloric acid is added into 18-21mL pure water to form solution C;

[0017] (3) Solution C is added into solution B to form solution D, and the zinc ferrite film coated stainless steel Baoer ring is immersed in solution D for 5min, and then taken out and left for 20min;

[0018] (4) The Baoer ring after treatment is dried at 90℃ for 8h, and then calcined at 335-360℃ for 3h to obtain a Baoer ring with zinc ferrite-alumina composite coating, which is a self-cleaning water treatment filler.

[0019] The stainless steel Baoer ring is punched from a metal sheet, and two rows of window holes with inner tongue leaves are opened on the ring wall, with a size of 25mmx25mmx0.6mm, and the specific surface area of the stainless steel Baoer ring is 219m 2 / m 3 , and the porosity is 0.93m 3 / m 3 .

[0020] A self-cleaning water treatment filler is prepared by the above method, and the specific surface area of the self-cleaning water treatment filler is 252-263m 2 / m 3 , and the porosity is 0.85-0.88m 3 / m 3 .

[0021] The total mass percentage of the zinc ferrite-alumina composite coating in the self-cleaning water treatment filler is 3.0%-3.3%, of which zinc ferrite accounts for 1.5%-1.7%, and alumina accounts for 1.5%-1.6%.

[0022] The various chemical raw materials are pure materials.

[0023] Compared with the prior art, the self-cleaning water treatment filler has the following advantages:

[0024] (1) The present application prepares a zinc ferrite-alumina composite coating on a stainless steel Bauer ring through scientific design and optimization of raw materials and preparation process. The relative mass percentage content of zinc ferrite-alumina in the coating is optimized to make the self-cleaning water treatment filler have ideal activity of purifying organic pollutants.

[0025] (2) The zinc ferrite-alumina composite coating has strong bonding force with the stainless steel Bauer ring, and the coating is dense and uniformly distributed, has strong mechanical strength, and has ideal corrosion resistance.

[0026] (3) The self-cleaning water treatment filler can quickly degrade organic pollutants under light, has the ability to continuously treat organic pollutants in water, and can be widely used in the treatment process of various organic pollutants in water. DETAILED DESCRIPTION

[0027] In order to further understand the present application, the present application will be further described in detail below in combination with examples.

[0028] The various chemical raw materials in the examples are pure materials.

[0029] Example 1

[0030] A preparation method of a self-cleaning water treatment filler, comprising the following process steps:

[0031] Step 1: pickling of stainless steel Bauer ring

[0032] (1) immerse the stainless steel Bauer ring in a 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities on the stainless steel Bauer ring;

[0033] (2) wash the stainless steel Bauer ring treated above with pure water, and dry at 80℃ for 2h to obtain a pickled stainless steel Bauer ring.

[0034] Step 2: electrode reaction to generate zinc ferrite film

[0035] (1) add 320 mL of pure water, 20 mL of acetic acid, 10 g of disodium ethylenediaminetetraacetate, and 15 g of zinc chloride into a beaker to form solution A;

[0036] (2) connect the anode of a 12V power supply to the stainless steel Bauer ring, and connect the cathode to a titanium plate. Immerse the two electrodes in solution A, control the current between the two electrodes at 1.8A, and power on for 15 min;

[0037] (3) wash the stainless steel Bauer ring subjected to the electrode reaction above with pure water, dry at 80℃ for 2h, and then calcine at 260℃ for 1h to obtain a zinc ferrite film coated stainless steel Bauer ring.

[0038] Step 3: sol-gel method for coating alumina film

[0039] (1) In 120 mL of ethanol, add 4.5 g of emulsifier OP-10, 7.2 g of aluminum isopropyl alcohol, and 2.7 g of dodecyl trimethyl ammonium bromide, and stir to form solution B;

[0040] (2) In 18 mL of pure water, add 1.1 mL of concentrated hydrochloric acid, and stir to form solution C;

[0041] (3) Add solution C to solution B, stir to form solution D, and immerse the zinc ferrite film coated stainless steel Pall ring in solution D, soak for 5 min, and take out, and stand for 20 min;

[0042] (4) Dry the above treated Pall ring at 90°C for 8 h, and then calcine at 335°C for 3 h, to obtain the Pall ring coated with aluminum oxide film, which is the self-cleaning water treatment filler.

[0043] The total mass percentage content of the zinc ferrite-aluminum oxide composite coating in the self-cleaning water treatment filler is 3.0%, of which zinc ferrite accounts for 1.5% and aluminum oxide accounts for 1.5%.

[0044] Example 2

[0045] A preparation method of a self-cleaning water treatment filler, comprising the following process steps:

[0046] Step 1: Pickling of stainless steel Pall ring

[0047] (1) Immerse the stainless steel Pall ring in a 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities on the stainless steel Pall ring;

[0048] (2) Wash the above treated stainless steel Pall ring with pure water, and dry at 80°C for 2 h to obtain the pickled stainless steel Pall ring.

[0049] Step 2: Electrode reaction to form zinc ferrite film

[0050] (1) In a beaker, add 330 mL of pure water, 21 mL of acetic acid, 10 g of ethylenediaminetetraacetic acid disodium salt, and 15.5 g of zinc chloride, and stir to form solution A;

[0051] (2) Connect the anode of a 12V power supply to the stainless steel Pall ring, and connect the cathode to a titanium plate, immerse the two electrodes in solution A, control the current between the two electrodes to be 1.8 A, and power on for 15 min;

[0052] (3) Wash the above treated stainless steel Pall ring with pure water, dry at 80°C for 2 h, and then calcine at 265°C for 1 h to obtain the zinc ferrite film coated stainless steel Pall ring.

[0053] Step 3: Sol-gel method for coating aluminum oxide film

[0054] (1) In 123 mL of ethanol, add 4.7 g of emulsifier OP-10, 7.4 g of aluminum isopropoxide, and 2.8 g of dodecyltrimethylammonium bromide, and stir to form solution B;

[0055] (2) In 18 mL of pure water, add 1.1 mL of concentrated hydrochloric acid, and stir to form solution C;

[0056] (3) Add solution C to solution B, and stir to form solution D. Immerse the zinc ferrite film-coated stainless steel Pall ring in solution D, soak for 5 min, and then take it out and stand for 20 min;

[0057] (4) Dry the above-processed Pall ring at 90°C for 8 h, and then calcine it at 340°C for 3 h to obtain the Pall ring coated with an aluminum oxide film, which is the self-cleaning water treatment filler.

[0058] The total mass percentage content of the zinc ferrite-aluminum oxide composite coating in the self-cleaning water treatment filler is 3.1%, of which zinc ferrite accounts for 1.6% and aluminum oxide accounts for 1.5%.

[0059] Example 3

[0060] A preparation method of a self-cleaning water treatment filler, comprising the following process steps:

[0061] Step 1: Pickling of stainless steel Pall ring

[0062] (1) Immerse the stainless steel Pall ring in a 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities on the stainless steel Pall ring;

[0063] (2) Wash the above-processed stainless steel Pall ring with pure water, and dry it at 80°C for 2 h to obtain the pickled stainless steel Pall ring.

[0064] Step 2: Electrode reaction to form zinc ferrite film

[0065] (1) In a beaker, add 340 mL of pure water, 21 mL of acetic acid, 11 g of disodium ethylenediaminetetraacetate, and 16 g of zinc chloride, and stir to form solution A;

[0066] (2) Connect the anode of a 12V power supply to the stainless steel Pall ring, and connect the cathode to a titanium plate. Immerse the two electrodes in solution A, control the current between the two electrodes at 1.8 A, and pass a current for 15 min;

[0067] (3) Wash the above-processed stainless steel Pall ring with pure water, dry it at 80°C for 2 h, and then calcine it at 270°C for 1 h to obtain the zinc ferrite film-coated stainless steel Pall ring.

[0068] Step 3: Sol-gel method for coating aluminum oxide film

[0069] (1) In 125 mL of ethanol, add 4.9 g of emulsifier OP-10, 7.8 g of aluminum isopropoxide, and 2.9 g of dodecyltrimethylammonium bromide, and stir to form solution B;

[0070] (2) In 19 mL of pure water, add 1.1 mL of concentrated hydrochloric acid, and stir to form solution C;

[0071] (3) Add solution C to solution B, stir to form solution D, and immerse the zinc ferrite film-coated stainless steel Pall ring in solution D, soak for 5 min, and then take it out and stand for 20 min;

[0072] (4) Dry the above-processed Pall ring at 90°C for 8 h, and then calcine it at 345°C for 3 h to obtain an alumina film-coated Pall ring, which is a self-cleaning water treatment filler.

[0073] The total mass percentage content of the zinc ferrite-alumina composite coating in the self-cleaning water treatment filler is 3.1%, of which zinc ferrite accounts for 1.6% and alumina accounts for 1.5%.

[0074] Example 4

[0075] A preparation method of a self-cleaning water treatment filler, comprising the following process steps:

[0076] Step 1: Pickling of stainless steel Pall ring

[0077] (1) Immerse the stainless steel Pall ring in a 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities on the stainless steel Pall ring;

[0078] (2) Wash the above-processed stainless steel Pall ring with pure water, and dry it at 80°C for 2 h to obtain a pickled stainless steel Pall ring.

[0079] Step 2: Electrode reaction to form zinc ferrite film

[0080] (1) In a beaker, add 350 mL of pure water, 22 mL of acetic acid, 11 g of disodium ethylenediaminetetraacetate, and 16 g of zinc chloride, and stir to form solution A;

[0081] (2) Connect the anode of a 12V power supply to the stainless steel Pall ring, and connect the cathode to a titanium plate, immerse the two electrodes in solution A, control the current between the two electrodes to be 1.8 A, and pass a current for 15 min;

[0082] (3) Wash the above-processed stainless steel Pall ring with pure water, dry it at 80°C for 2 h, and then calcine it at 275°C for 1 h to obtain a zinc ferrite film-coated stainless steel Pall ring.

[0083] Step 3: Sol-gel method for coating alumina film

[0084] (1) In 128 mL of ethanol, add 5.1 g of emulsifier OP-10, 8.0 g of aluminum isopropoxide, and 3.0 g of dodecyltrimethylammonium bromide, and stir to form solution B;

[0085] (2) In 20 mL of pure water, add 1.2 mL of concentrated hydrochloric acid, and stir to form solution C;

[0086] (3) Add solution C to solution B, stir to form solution D, and immerse the zinc ferrite film-coated stainless steel Pall ring in solution D, soak for 5 min, and then take it out and stand for 20 min;

[0087] (4) Dry the above-processed Pall ring at 90°C for 8 h, and then calcine it at 355°C for 3 h to obtain an alumina film-coated Pall ring, which is a self-cleaning water treatment filler.

[0088] The total mass percentage content of the zinc ferrite-alumina composite coating in the self-cleaning water treatment filler is 3.2%, of which zinc ferrite accounts for 1.6% and alumina accounts for 1.6%.

[0089] Example 5

[0090] A preparation method of a self-cleaning water treatment filler, comprising the following process steps:

[0091] Step 1: Pickling of a stainless steel Pall ring

[0092] (1) Immerse the stainless steel Pall ring in a 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities on the stainless steel Pall ring;

[0093] (2) Wash the above-processed stainless steel Pall ring with pure water, and dry it at 80°C for 2 h to obtain a pickled stainless steel Pall ring.

[0094] Step 2: Electrode reaction to form a zinc ferrite film

[0095] (1) In a beaker, add 360 mL of pure water, 23 mL of acetic acid, 12 g of disodium ethylenediaminetetraacetate, and 17 g of zinc chloride, and stir to form solution A;

[0096] (2) Connect the anode of a 12V power supply to the stainless steel Pall ring, and connect the cathode to a titanium plate, immerse the two electrodes in solution A, control the current between the two electrodes to be 1.8 A, and pass a current for 15 min;

[0097] (3) Wash the above-processed stainless steel Pall ring with pure water, dry it at 80°C for 2 h, and then calcine it at 280°C for 1 h to obtain a zinc ferrite film-coated stainless steel Pall ring.

[0098] Step 3: Sol-gel method for coating an alumina film

[0099] (1) In 130 mL of ethanol, 5.3 g of emulsifier OP-10, 8.3 g of aluminum isopropoxide, and 3.1 g of dodecyl trimethyl ammonium bromide were added to form solution B;

[0100] (2) In 21 mL of pure water, 1.2 mL of concentrated hydrochloric acid was added to form solution C;

[0101] (3) Solution C was added to solution B, and stirred to form solution D. A stainless steel Pau ring coated with zinc ferrite film was immersed in solution D, and taken out after 5 min, and left to stand for 20 min;

[0102] (4) The Pau ring treated above was dried at 90 °C for 8 h, and then calcined at 360 °C for 3 h to obtain a Pau ring coated with an alumina film, which was a self-cleaning water treatment filler.

[0103] The mass percentage content of the zinc ferrite-alumina composite coating in the self-cleaning water treatment filler was 3.3%, of which zinc ferrite accounted for 1.7%, and alumina accounted for 1.6%.

Claims

1. A method for preparing a self-cleaning water treatment packing material, characterized in that, The process includes the following steps: Step 1: Pickling of stainless steel Pall rings (1) Immerse the stainless steel Pall ring in 0.2 mol / L hydrochloric acid solution for 50 min to remove impurities from the stainless steel Pall ring; (2) The stainless steel Pall ring treated above was washed with pure water and dried at 80°C for 2 hours to obtain pickled stainless steel Pall ring. Step 2: Electrode reaction to form zinc ferrite film (1) Add 320-360 mL of pure water, 20-23 mL of acetic acid, 10-12 g of disodium ethylenediaminetetraacetate, and 15-17 g of zinc chloride to a beaker and stir to form solution A; (2) Connect the anode of the 12V power supply to a stainless steel Pall ring and the cathode to a titanium plate. Immerse the two electrodes in solution A, control the current between the two electrodes to 1.8A, and let the reaction proceed for 15 minutes. (3) The stainless steel Pall rings that have undergone the electrode reaction are washed with pure water, dried at 80°C for 2 hours, and then calcined at 260-280°C for 1 hour to obtain stainless steel Pall rings coated with zinc ferrite film. Step 3: Sol-gel coating of alumina film (1) Add 4.5-5.3g of emulsifier OP-10, 7.2-8.3g of aluminum isopropoxide, and 2.7-3.1g of dodecyltrimethylammonium bromide to 120-130mL of ethanol, and stir to form solution B; (2) Add 1.1 to 1.2 mL of concentrated hydrochloric acid to 18 to 21 mL of pure water and stir to form solution C; (3) Add solution C to solution B and stir until uniform to form solution D. Immerse the stainless steel Pall ring coated with zinc ferrite film into solution D, soak for 5 minutes, then remove and let stand for 20 minutes. (4) The Pall rings treated above are dried at 90°C for 8 hours and then calcined at 335-360°C for 3 hours to obtain Pall rings with zinc ferrite-alumina composite coating, which are self-cleaning water treatment fillers.

2. The method for preparing a self-cleaning water treatment packing material according to claim 1, characterized in that, The stainless steel Pall ring is made of sheet metal and has two rows of windows with inwardly extending tabs cut into its wall. The dimensions are 25mm × 25mm × 0.6mm. The specific surface area of ​​the stainless steel Pall ring is 219m². 2 / m 3 Porosity 0.93m 3 / m 3 .

3. A self-cleaning water treatment packing material, prepared using the method described in claim 1 or 2, characterized in that, The self-cleaning water treatment packing has a specific surface area of ​​252-263 m². 2 / m 3 Porosity 0.85–0.88 μm 3 / m 3 .

4. The self-cleaning water treatment packing material according to claim 3, characterized in that, The self-cleaning water treatment filler contains a zinc ferrite-alumina composite coating with a total mass percentage of 3.0% to 3.3%, of which zinc ferrite accounts for 1.5% to 1.7% and alumina accounts for 1.5% to 1.6%.