Preparation method of porous nano stannous oxide

A technology of stannous oxide and stannous chloride, applied in the direction of tin oxide, nanotechnology, nanotechnology, etc., can solve the problems of poor uniformity and porosity, and achieve uniformity, uniform pore diameter, and improved uniformity Effect

Active Publication Date: 2018-08-31
王芸芸
4 Cites 3 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0008] The technical problem mainly solved by the present invention is to provide a preparation method of porous nano-stannou...
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Abstract

The invention discloses a preparation method of porous nano stannous oxide and belongs to the technical field of preparation of nanomaterials. The preparation method comprises the following steps: a pre-modified porous material and a stannous oxide solution are mixed in a mass ratio being 1:5-1:6, filtering and drying are performed after stirring and mixing, a modified porous material is obtainedand mixed with water in a mass ratio being 1:10-1:15, protease accounting for 0.2-0.3 times the mass of the modified porous material is added, filtering is performed after stirring and mixing, then aproduct is washed until a washing liquid contains no chloride ion under detection of silver nitrate, vacuum drying is performed, and a pretreated modified porous material is obtained; the pretreated modified porous material is heated in an argon atmosphere, cooling and discharging are performed, a porous nano stannous oxide blank is obtained and mixed with an ammonium chloride solution in a mass ratio being 1:5-1:8, filtering and drying are performed after stirring and mixing, and porous nano stannous oxide is obtained. Porous nano stannous oxide prepared with the technical scheme has the characteristics of excellent particle size uniformity and porosity.

Application Domain

Material nanotechnologyTin oxides

Technology Topic

IonSTANNOUS OXIDE +9

Examples

  • Experimental program(3)
  • Comparison scheme(1)
  • Effect test(1)

Example Embodiment

[0024] Example 1
[0025]Mix soybean protein isolate and sodium hydroxide solution with a mass fraction of 5% in a beaker at a mass ratio of 1:3, and add distilled water with 10 times the amount of soybean protein isolate into the beaker, at a temperature of 88°C and a rotation speed of 400r/ After stirring and mixing for 50 minutes under the condition of Soybean protein gel was crushed, frozen in liquid nitrogen for 6 minutes, and then vacuum-dried to obtain a protein porous material; the protein porous material and trioctylamine were mixed in a flask in a mass ratio of 1:8, and the mass of the protein porous material was added to the flask. 3 times of oxalic acid, stirred and mixed for 40min under the condition of temperature of 55℃ and rotation speed of 400r/min, filtered to obtain pretreated porous material; cupric chloride and water were mixed in a three-necked flask in a mass ratio of 1:1000 , and add the pretreated porous material with 0.10 times the mass of water into the three-necked flask, stir and mix for 30 minutes at a temperature of 60 ° C and a rotating speed of 300 r/min, and adjust the pH of the material in the three-necked flask to 12.0 with sodium hydroxide, 15 times the mass of copper chloride was added to the three-necked flask, stirred and mixed for 60 min at a temperature of 65°C and a rotational speed of 380 r/min, and filtered to obtain a pre-modified porous material; the pre-modified porous material was The material and the stannous chloride solution are mixed at a mass ratio of 1:60, under the conditions of a temperature of 65 ° C and a rotating speed of 400 r/min, after stirring and mixing for 60 min, filtration to obtain a filter cake, and the filter cake is heated at a temperature of 70 ° C. After drying under the conditions for 2 hours, the modified porous material was obtained. The modified porous material was mixed with water in a mass ratio of 1:15, and 0.3 times the mass of the modified porous material was added to the mixture of the modified porous material and water. After stirring and mixing for 2 hours at a temperature of 38 °C and a rotating speed of 400 r/min, the filter residue was filtered to obtain a filter residue. After vacuum drying at 105 °C for 5 hours, the pretreated modified porous material was obtained; the pretreated modified porous material was moved into the reaction kettle, and nitrogen was introduced into the reaction kettle at a rate of 20 mL/min, and the reaction kettle was filled with nitrogen. Nitrogen, heated at 550°C for 2 hours, the temperature in the reaction kettle was lowered to room temperature, and the material was discharged to obtain a porous nano-stannous oxide billet. The porous nano-stannous oxide billet was mixed with 15% chloride The ammonium solution was mixed at a mass ratio of 1:8, stirred and dissolved for 60 minutes at a temperature of 40 °C and a rotational speed of 400 r/min, and filtered to obtain the pretreated porous nano-stannous oxide. After drying for 80 min under the condition of 80 ℃, the porous nano-tin oxide was obtained. The aldehyde solution is a glutaraldehyde solution with a mass fraction of 15%. The unsaturated fatty acid is oleic acid. The protease is papain. The stannous chloride solution is obtained by mixing stannous chloride and absolute ethanol in a mass ratio of 1:10 to obtain a stannous chloride solution.

Example Embodiment

[0026] Example 2
[0027] Mix soybean protein isolate and sodium hydroxide solution with a mass fraction of 5% in a beaker at a mass ratio of 1:3, and add distilled water with 10 times the amount of soybean protein isolate into the beaker, at a temperature of 88°C and a rotation speed of 400r/ After stirring and mixing for 50 minutes under the condition of Soybean protein gel was crushed, frozen in liquid nitrogen for 6 minutes, and then vacuum-dried to obtain a protein porous material; the protein porous material and trioctylamine were mixed in a flask in a mass ratio of 1:8, and the mass of the protein porous material was added to the flask. 3 times of oxalic acid, stirred and mixed for 40min under the condition of temperature of 55℃ and rotation speed of 400r/min, filtered to obtain pretreated porous material; cupric chloride and water were mixed in a three-necked flask in a mass ratio of 1:1000 , and add the pretreated porous material with 0.10 times the mass of water into the three-necked flask, stir and mix for 30 minutes at a temperature of 60 ° C and a rotating speed of 300 r/min, and adjust the pH of the material in the three-necked flask to 12.0 with sodium hydroxide, After stirring and mixing for 60 minutes at a temperature of 65 ° C and a rotation speed of 380 r/min, the pre-modified porous material was obtained by filtration; the pre-modified porous material was mixed with a stannous chloride solution in a mass ratio of 1:60, and the pre-modified porous material was mixed at a temperature of 1:60. Under the conditions of 65 °C and 400 r/min of rotation speed, after stirring and mixing for 60 minutes, filter to obtain a filter cake, and after drying the filter cake at a temperature of 70 °C for 2 hours, a modified porous material is obtained. Mix with water at a mass ratio of 1:15, add protease with 0.3 times the mass of the modified porous material to the mixture of the modified porous material and water, and stir and mix for 2 hours at a temperature of 38 °C and a rotation speed of 400 r/min. , filter to get the filter residue, wash the filter residue with deionized water until the washing solution is free of chloride ions by silver nitrate, and vacuum-dry the washed filter residue at a temperature of 105 ° C for 5 hours to obtain a pretreated modified porous material ; Move the pretreated modified porous material into the reaction kettle, and feed nitrogen into the reaction kettle at a rate of 20 mL/min. After the reaction kettle is filled with nitrogen, heat treatment for 2 hours at a temperature of 550 °C, and the reaction The temperature in the kettle is lowered to room temperature and the material is discharged to obtain a porous nano-stannous oxide billet. The porous nano-stannous oxide billet is mixed with an ammonium chloride solution with a mass fraction of 15% at a mass ratio of 1:8, and the temperature is 40 ° C. Rotation speed After stirring and dissolving for 60min under the condition of 400r/min, filter to obtain the pretreated porous nano stannous oxide, and after drying the pretreated porous nano stannous oxide at a temperature of 80 ℃ for 80min, obtain the porous nanometer stannous oxide. The aldehyde solution is a glutaraldehyde solution with a mass fraction of 15%. The protease is papain. The stannous chloride solution is obtained by mixing stannous chloride and absolute ethanol in a mass ratio of 1:10 to obtain a stannous chloride solution.

Example Embodiment

[0028] Example 3
[0029] Mix soybean protein isolate and sodium hydroxide solution with a mass fraction of 5% in a beaker at a mass ratio of 1:3, and add distilled water with 10 times the amount of soybean protein isolate into the beaker, at a temperature of 88°C and a rotation speed of 400r/ After stirring and mixing for 50 minutes under the condition of Soybean protein gel was crushed, frozen in liquid nitrogen for 6 minutes, and then vacuum-dried to obtain a protein porous material; the protein porous material and trioctylamine were mixed in a flask in a mass ratio of 1:8, and the mass of the protein porous material was added to the flask. 3 times of oxalic acid was stirred and mixed for 40 minutes at a temperature of 55°C and a rotational speed of 400r/min, and then filtered to obtain a pretreated porous material; the porous material was mixed with a stannous chloride solution in a mass ratio of 1:60, Under the condition that the temperature is 65°C and the rotation speed is 400r/min, after stirring and mixing for 60min, filter to obtain a filter cake. After drying the filter cake at a temperature of 70°C for 2 hours, a modified porous material is obtained. The porous material is mixed with water at a mass ratio of 1:15, and the protease with 0.3 times the mass of the modified porous material is added to the mixture of the modified porous material and water, and the mixture is stirred and mixed at a temperature of 38 °C and a rotation speed of 400 r/min. After 2 hours, filter to obtain the filter residue, wash the filter residue with deionized water until the washing solution is free of chloride ions by silver nitrate, and vacuum dry the washed filter residue at a temperature of 105 ° C for 5 hours to obtain a pretreatment modification. Porous material; the pretreated modified porous material was moved into the reaction kettle, and nitrogen was introduced into the reaction kettle at a rate of 20 mL/min. The temperature in the reaction kettle is lowered to room temperature and the material is discharged to obtain a porous nano-stannous oxide billet. The porous nano-stannous oxide billet is mixed with a mass fraction of 15% ammonium chloride solution at a mass ratio of 1:8, and the temperature is 40 ° C. , after stirring and dissolving for 60 min under the condition of a rotating speed of 400 r/min, and filtering to obtain the pretreated porous nano-stannous oxide. tin. The aldehyde solution is a glutaraldehyde solution with a mass fraction of 15%. The protease is papain. The stannous chloride solution is obtained by mixing stannous chloride and absolute ethanol in a mass ratio of 1:10 to obtain a stannous chloride solution.

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