Titanium capillary pollution purification material and preparation method thereof

Abstract

The invention provides a titanium capillary pollution purification material and a preparation method thereof, and belongs to the field of water treatment materials. According to the material, a titanium capillary tube serves as a base material, the surface of the titanium capillary tube is coated with a cerium tungstate-titanium oxide composite active layer through the two steps of titanium capillary tube oxidation and cerium tungstate coating, and the cerium tungstate accounts for 2.5%-2.6% by mass of the titanium capillary tube pollution purification material. The titanium oxide accounts for 3.2%-3.3% of the titanium capillary pollution purification material in percentage by mass. The titanium capillary pollution purification material can be used for continuous treatment of organic sewage, does not need frequent maintenance and reactivation, and is suitable for the large-scale purification process of organic pollutants in industrial and civil sewage.

Description

Technical Field

[0001] The invention belongs to the field of water treatment materials, and in particular relates to a titanium capillary pollution purification material and a preparation method thereof. Background Art

[0002] Since industrial and domestic sewage contain numerous organic pollutants, they must be intensively treated to purify organic pollutants before being discharged. Photocatalytic technology is an organic pollutant purification technology that has been widely studied and applied in the past half century. This technology can decompose organic pollutants under light to achieve the purpose of purification. The key to photocatalytic technology is the catalytic material. With the research on the application of photocatalytic technology in actual wastewater, an important focus is the way in which the catalytic material is used, which is a key factor in improving the efficiency of photocatalytic purification. Due to the limitations of the actual wastewater treatment process, in addition to having a high purification efficiency, the photocatalytic material must also adapt to the special requirements of the water treatment process. The photocatalytic material should be corrosion-resistant, stable in structure, simple to maintain, and have a high purification activity. Summary of the invention

[0003] In view of the problems existing in the prior art, the present invention aims to provide a method for preparing a titanium capillary pollution purification material. Such a titanium capillary can be used to purify organic pollutants in sewage.

[0004] A titanium capillary pollution purification material, wherein the base material of the pollution purification material is a titanium capillary, the mass percentage of titanium in the titanium capillary is 99.5%; the titanium capillary has an outer diameter of 5mm and a wall thickness of 0.5mm.

[0005] Furthermore, the titanium capillary pollution purification material is a cerium tungstate-titanium oxide composite active layer coated on the surface of the titanium capillary of the base material, wherein the mass percentage of cerium tungstate in the titanium capillary pollution purification material is 2.5% to 2.6%, and the mass percentage of titanium oxide in the titanium capillary pollution purification material is 3.2% to 3.3%.

[0006] A method for preparing a titanium capillary pollution purification material comprises the following process steps:

[0007] Step 1: Oxidation of titanium capillary

[0008] (1) Immerse the titanium capillary in a 0.15 mol / L hydrochloric acid solution, heat the solution to 60°C, and keep it warm for 50 min;

[0009] (2) taking out the titanium capillary after acid treatment, washing it with pure water, drying it at 80° C. for 5 h, and then calcining it at 480-510° C. for 1 h to obtain a titanium capillary with a titanium oxide film on the surface;

[0010] Step 2: Coating with cerium tungstate

[0011] (1) Add 4.5-4.8 g of polyethylene glycol with a molecular weight of 10,000, 3.2-3.6 g of emulsifier Span 60, and 5.2-5.7 g of ammonium metatungstate to 500 mL of ethanol and stir to form solution A;

[0012] (2) adding 5.6-6.0 g of cerium nitrate and 2.5-2.7 g of dodecyltrimethylammonium bromide to 80 mL of pure water and stirring to form solution B;

[0013] (3) adding solution B into solution A to form a transparent sol, and then immersing the titanium capillary coated with the titanium oxide film in step 1 into the sol for 15 minutes, taking it out and letting it stand for 30 minutes;

[0014] (4) drying the titanium capillary after standing at 110° C. for 8 h, and then calcining at 460-490° C. for 2 h to obtain a titanium capillary coated with cerium tungstate;

[0015] Step 3: Pickling and Activation

[0016] (1) Immerse the titanium capillary coated with cerium tungstate in a 0.25-0.30 mol / L hydrochloric acid solution, heat the solution to 50° C., keep the solution warm for 70 minutes, wash with pure water, and dry at 110° C. for 5 hours to obtain a titanium capillary contamination purification material.

[0017] Furthermore, the titanium capillary in step 1 has a titanium content of 99.5% by mass, an outer diameter of 5 mm, a wall thickness of 0.5 mm, and a length of 10 cm.

[0018] Compared with the prior art, the preparation method of the titanium capillary pollution purification material of the present invention has the following advantages:

[0019] The titanium capillary is used as the base material. Through the two steps of titanium capillary oxidation and coating with cerium tungstate, the cerium tungstate-titanium oxide composite active layer is coated on the surface of the titanium capillary. The composite active layer can quickly decompose organic pollutants in water under light. The cerium tungstate-titanium oxide composite active layer is tightly combined with the base titanium capillary, evenly distributed, and has high mechanical strength, which can meet the requirements of material strength in the water treatment process. The titanium capillary pollution purification material can be used for continuous treatment of organic sewage, has stable performance, does not require frequent maintenance and reactivation, and can be used in the purification process of organic pollutants in large-scale industrial and civil sewage. DETAILED DESCRIPTION

[0020] The present invention will be further described below with reference to examples.

[0021] Example 1

[0022] A method for preparing a titanium capillary pollution purification material comprises the following process steps:

[0023] Step 1: Oxidation of titanium capillary

[0024] (1) Immerse the titanium capillary in a 0.15 mol / L hydrochloric acid solution, heat the solution to 60°C, and keep it warm for 50 min;

[0025] (2) The titanium capillary after acid treatment was taken out, washed with pure water, dried at 80°C for 5 hours, and then calcined at 480°C for 1 hour to obtain a titanium capillary with a titanium oxide film on the surface.

[0026] Step 2: Coating with cerium tungstate

[0027] (1) Add 4.5 g of polyethylene glycol with a molecular weight of 10,000, 3.2 g of emulsifier Span 60, and 5.2 g of ammonium metatungstate to 500 mL of ethanol and stir to form solution A;

[0028] (2) adding 5.6 g of cerium nitrate and 2.5 g of dodecyltrimethylammonium bromide to 80 mL of pure water and stirring to form solution B;

[0029] (3) Add solution B to solution A to form a transparent sol, and then immerse the titanium capillary coated with titanium oxide film in step 1 in the sol for 15 minutes, take it out and let it stand for 30 minutes;

[0030] (4) The titanium capillary treated as above was dried at 110° C. for 8 h, and then calcined at 460° C. for 2 h to obtain a titanium capillary coated with cerium tungstate.

[0031] Step 3: Pickling and Activation

[0032] (1) Immerse the titanium capillary prepared in step 2 in a 0.25 mol / L hydrochloric acid solution, heat the solution to 50°C, keep the solution warm for 70 min, wash with pure water and dry at 110°C for 5 h to obtain a titanium capillary contamination purification material. The mass percentages of cerium tungstate and titanium oxide in the prepared titanium capillary contamination purification material are 2.5% and 3.2% respectively.

[0033] Example 2

[0034] A method for preparing a titanium capillary pollution purification material comprises the following process steps:

[0035] Step 1: Oxidation of titanium capillary

[0036] (1) Immerse the titanium capillary in a 0.15 mol / L hydrochloric acid solution, heat the solution to 60°C, and keep it warm for 50 min;

[0037] (2) The titanium capillary after acid treatment was taken out, washed with pure water, dried at 80°C for 5 hours, and then calcined at 490°C for 1 hour to obtain a titanium capillary with a titanium oxide film on the surface.

[0038] Step 2: Coating with cerium tungstate

[0039] (1) Add 4.6 g of polyethylene glycol with a molecular weight of 10,000, 3.3 g of emulsifier Span 60, and 5.3 g of ammonium metatungstate to 500 mL of ethanol and stir to form solution A;

[0040] (2) adding 5.7 g of cerium nitrate and 2.5 g of dodecyltrimethylammonium bromide to 80 mL of pure water and stirring to form solution B;

[0041] (3) Add solution B to solution A to form a transparent sol, and then immerse the titanium capillary coated with titanium oxide film in step 1 in the sol for 15 minutes, take it out and let it stand for 30 minutes;

[0042] (4) The titanium capillary treated as above was dried at 110° C. for 8 h, and then calcined at 470° C. for 2 h to obtain a titanium capillary coated with cerium tungstate.

[0043] Step 3: Pickling and Activation

[0044] (1) Immerse the titanium capillary prepared in step 2 in a 0.25 mol / L hydrochloric acid solution, heat the solution to 50°C, keep the solution warm for 70 min, wash with pure water and dry at 110°C for 5 h to obtain a titanium capillary contamination purification material. The mass percentages of cerium tungstate and titanium oxide in the prepared titanium capillary contamination purification material are 2.5% and 3.2% respectively.

[0045] Example 3

[0046] A method for preparing a titanium capillary pollution purification material comprises the following process steps:

[0047] Step 1: Oxidation of titanium capillary

[0048] (1) Immerse the titanium capillary in a 0.15 mol / L hydrochloric acid solution, heat the solution to 60°C, and keep it warm for 50 min;

[0049] (2) The titanium capillary after acid treatment was taken out, washed with pure water, dried at 80°C for 5 hours, and then calcined at 500°C for 1 hour to obtain a titanium capillary with a titanium oxide film on the surface.

[0050] Step 2: Coating with cerium tungstate

[0051] (1) Add 4.7 g of polyethylene glycol with a molecular weight of 10,000, 3.5 g of emulsifier Span 60, and 5.6 g of ammonium metatungstate to 500 mL of ethanol and stir to form solution A;

[0052] (2) adding 5.8 g of cerium nitrate and 2.6 g of dodecyltrimethylammonium bromide to 80 mL of pure water and stirring to form solution B;

[0053] (3) Add solution B to solution A to form a transparent sol, and then immerse the titanium capillary coated with titanium oxide film in step 1 in the sol for 15 minutes, take it out and let it stand for 30 minutes;

[0054] (4) The titanium capillary treated as above was dried at 110° C. for 8 h, and then calcined at 480° C. for 2 h to obtain a titanium capillary coated with cerium tungstate.

[0055] Step 3: Pickling and Activation

[0056] (1) Immerse the titanium capillary prepared in step 2 in a 0.30 mol / L hydrochloric acid solution, heat the solution to 50°C, keep the solution warm for 70 min, wash with pure water and dry at 110°C for 5 h to obtain a titanium capillary contamination purification material. The mass percentages of cerium tungstate and titanium oxide in the prepared titanium capillary contamination purification material are 2.6% and 3.3%, respectively.

[0057] Example 4

[0058] A method for preparing a titanium capillary pollution purification material comprises the following process steps:

[0059] Step 1: Oxidation of titanium capillary

[0060] (1) Immerse the titanium capillary in a 0.15 mol / L hydrochloric acid solution, heat the solution to 60°C, and keep it warm for 50 min;

[0061] (2) The titanium capillary after acid treatment was taken out, washed with pure water, dried at 80°C for 5 hours, and then calcined at 510°C for 1 hour to obtain a titanium capillary with a titanium oxide film on the surface.

[0062] Step 2: Coating with cerium tungstate

[0063] (1) Add 4.8 g of polyethylene glycol with a molecular weight of 10,000, 3.6 g of emulsifier Span 60, and 5.7 g of ammonium metatungstate to 500 mL of ethanol and stir to form solution A;

[0064] (2) adding 6.0 g of cerium nitrate and 2.7 g of dodecyltrimethylammonium bromide to 80 mL of pure water and stirring to form solution B;

[0065] (3) Add solution B to solution A to form a transparent sol, and then immerse the titanium capillary coated with titanium oxide film in step 1 in the sol for 15 minutes, take it out and let it stand for 30 minutes;

[0066] (4) The titanium capillary treated as above was dried at 110° C. for 8 h, and then calcined at 490° C. for 2 h to obtain a titanium capillary coated with cerium tungstate.

[0067] Step 3: Pickling and Activation

[0068] (1) Immerse the titanium capillary prepared in step 2 in a 0.30 mol / L hydrochloric acid solution, heat the solution to 50°C, keep the solution warm for 70 min, wash with pure water and dry at 110°C for 5 h to obtain a titanium capillary contamination purification material. The mass percentages of cerium tungstate and titanium oxide in the prepared titanium capillary contamination purification material are 2.6% and 3.3%, respectively.

[0069] The titanium capillary pollution purification material prepared in Example 1-4 was placed in parallel in a beaker, 200 mL of a 10 mg / L soap yellow solution was added, the solution was placed under a 20W ultraviolet germicidal lamp for irradiation, and after 60 minutes, a sample was taken to determine the concentration of the soap yellow solution, and the degradation rate of the soap yellow was calculated. The results are shown in Table 1.

[0070]

[0071] Table 1

[0072] The results show that the titanium capillary pollution purification materials prepared in Examples 1-4 have strong activity in degrading organic matter and can quickly and completely degrade organic pollutants under light.

Claims

1. A titanium capillary pollution purification material, characterized in that: The base material of the pollution purification material is a titanium capillary tube, the mass percentage of titanium in the titanium capillary tube is 99.5%; the outer diameter of the titanium capillary tube is 5 mm, and the wall thickness is 0.5 mm.

2. The titanium capillary contamination purification material according to claim 1, characterized in that: The titanium capillary pollution purification material is a titanium capillary substrate material with a cerium tungstate-titanium oxide composite active layer coated on its surface, wherein the mass percentage of cerium tungstate in the titanium capillary pollution purification material is 2.5% to 2.6%, and the mass percentage of titanium oxide in the titanium capillary pollution purification material is 3.2% to 3.3%.

3. A method for preparing the titanium capillary pollution purification material according to claim 1 or 2, characterized in that: The process steps include: Step 1: Oxidation of titanium capillary (1) Immerse the titanium capillary in a 0.15 mol / L hydrochloric acid solution, heat the solution to 60°C, and keep it warm for 50 min; (2) taking out the titanium capillary after acid treatment, washing it with pure water, drying it at 80° C. for 5 h, and then calcining it at 480-510° C. for 1 h to obtain a titanium capillary with a titanium oxide film on the surface; Step 2: Coating with cerium tungstate (1) Add 4.5-4.8 g of polyethylene glycol with a molecular weight of 10,000, 3.2-3.6 g of emulsifier Span 60, and 5.2-5.7 g of ammonium metatungstate to 500 mL of ethanol and stir to form solution A; (2) adding 5.6-6.0 g of cerium nitrate and 2.5-2.7 g of dodecyltrimethylammonium bromide to 80 mL of pure water and stirring to form solution B; (3) adding solution B to solution A to form a transparent sol, and then immersing the titanium capillary coated with the titanium oxide film in step 1 in the sol for 15 minutes, taking it out and letting it stand for 30 minutes; (4) drying the titanium capillary after standing at 110° C. for 8 h, and then calcining at 460-490° C. for 2 h to obtain a titanium capillary coated with cerium tungstate; Step 3: Pickling and Activation (1) Immerse the titanium capillary coated with cerium tungstate in a 0.25-0.30 mol / L hydrochloric acid solution, heat the solution to 50° C., keep the solution warm for 70 minutes, wash with pure water, and dry at 110° C. for 5 hours to obtain a titanium capillary contamination purification material.

4. The method for preparing a titanium capillary pollution purification material according to claim 3, characterized in that: The titanium capillary in step 1 has a titanium content of 99.5% by mass, an outer diameter of 5 mm, a wall thickness of 0.5 mm, and a length of 10 cm.

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