Preparation method for high-dispersion loaded silver phosphate photo-catalyst

The technical field of

[0001] the invention belongs to water treatment field this utility model claims a high dispersing load silver phosphate light catalyst and preparation method especially claims a method and device for processing organic waste water by photocatalytic material and preparation method thereof.

Background technology

[0002] is accompanied with current technology the rapid development of human lai the existence of water source is controlled by the different degree of the polluted water source pollution it has been as world of various national facing the * to solve the problem of. In the water pollution especially the toxic organic pollutant in the presence of it is not only environmental pollution ecological damage but seriously harmful to human health. These organic pollutant comprising polycyclic aromatic hydrocarbon polychlorinated biphenyl pesticide environment interferon such as dyes and so on. 2010*6 yue material research institute of research stuff the silver phosphate with light catalyst effect of the light oxidation effect the present known the invention claims a photo-catalyst of the data more than ten times. The research shows of the catalyst particles to severely affect the activity of catalyst particle is smaller it has higher. So it is not less that power research institute for the nanometre catalyst.

[0003] nanometer grain it has large specific surface area and the special surface properties and exhibit excellent catalytic activity it is composed of the metal nanometer grain it has high surface energy to make it in the using process it is easy to agglomerate so as to reduce the catalytic activity. Keep the excellent dispersion performance is metal nanometre particle in the process of using the key problem of the. Using porous medium load metal nanometer granule is to realize particle dispersed method for efficiently. And the loading amount and distribution the uniformity of the invention claims a process of the key at the same time of a suitable carrier to load process it has important influence. In order to make nanometer particle at loads are uniformly carrier with heat stability and chemical stability at the same time also has even the load of the site; The material with large specific surface area suitable pore structure and macro appearance. Which is often used by the catalyst carrier with an ion exchange resin mesoporous silicon dioxide zeolite and so on these materials do not have light transmittance at the load catalyst the carrier will not affect the optical catalyst with light absorbing so that it can reduce the catalytic effect.

The content of invention

[0004] the purpose of this invention is to overcome the disadvantages of existing technology the invention claims a high dispersing load silver phosphate photocatalyst preparation method of.

[0005] the purpose of this invention can be obtained through following technology scheme it realizes:

[0006] this invention claims a highly dispersed supported silver phosphate light of the catalyst preparation method adopts the following method to prepare:

[0007] the silver nitrate solution sodium chloride solution with sodium hydroxide solution stirring under indoor temperature time is 10***30 minutes to obtain a silver deposition the deposition filter and wash and then adding into a solution with sodium persulfate in the water solution at 60 *** 70° c the stirring reaction after the stirring time is small when 2***4; The temperature is reduced in room temperature to obtain a high silver ions of the solution; Wherein silver nitrate solution sodium chloride solution with sodium hydroxide solution of the molar concentration is 0.2 *** lmol g/l silver nitrate and sodium chloride the mole ratio is 1: 0.5; Silver nitrate and sodium hydroxide the mol ratio of 1: 1; With silver deposition and the sodium sulphate of the mass ratio is 0.1: 1 0.5 ***: 1;

[0008] 2 of taking l in the 3g subcritical under the condition of water after etching with a sphericalal shell structure of grain diameter is 8-150 mu m a porous glass micro ball the porous glass micro ball in the concentration is 2 to 4mm *** mmol/l of the hydrofluoric acid liquor to dip in 20***30 min separation and then the porous glass micro ball is set in the thickness of 30mm is 20 *** mmol/l hydrochloric acid solution for dipping 40***60 min then separation washing by de-ionized water to pass 2***3 105° c;

[0009] 3 to obtain porous glass micro sphere into 15***20 ml having high valence of silver ion in solution slow speed stirring 12***24 h solid-liquid separation washing by de-ionized water to 2***3 *** 150 times to 180 degrees c 2***4 h and then adding the concentration is 20 *** 100 mmol/l the phosphoric acid solution to stir then preparing a highly dispersed supported silver phosphate photocatalyst.

[0010] said sub-critical condition is: The temperature is 250 *** 300° c pressure of 1mpa of subcritical condition.

[0011] sub-critical water after etching with a sphericalal shell structure of the porous glass micro ball with the positive ion exchange property and the silver complex positive ion exchange after the silver complex positive ion is fixed to the glass micro ball the channel and then drying and roasting to form silver oxide and sulphide the silver oxide and phosphoric acid as the holes generated silver phosphate.

[0012] this invention has the beneficial effects of this utility model is that:

[0013] 1 the invention is a sub-critical water after etching with a sphericalal shell structure of the porous glass microsphere as carrier it through ion exchange technology of target metal ion in the form of chemical bond is used for carrier carrier and the acting force between is strong it can effectively prevent the metal ion aggregation.

[0014] 2 the metal ion exchange after finishing the drying and then through the oxidation effect of the metal ion is transformed into the metal oxide can be avoided on the rotating of the silver phosphate during the process of generating and ion exchange effect and the silver ion exchange to the solution to reduce the surface of carrier active component the quantity of.

[0015] using a porous glass microsphere as carrier because the glass is transparent object the light catalyst in the process of the carrier will not obstruct light able to fully exert the photocatalyst effect.

[0016] 4 by the hydrofluoric acid cleaning can be expanded pore canal structure so as to through hydrochloric acid dipping it is able to the positive ion surface promoting exchange.

[0017] 5 silver phosphate able to fully exert nanometer effect and it is easy to separate from water.

Specific implementing manner

[0018] embodiment 1

[0019] the molar concentration is lmol g/l of the silver nitrate solution of mol concentration of the lmol g/l of sodium chloride solution and mol concentration is lmol g/l of sodium hydroxide solution stirring under indoor temperature time is 30 minutes to obtain a silver deposition the deposition filter and wash and then adding into a solution with sodium persulfate in the aqueous solution of the c the 70° after stirring and reacting the stirring time is 4 hours; The temperature is reduced in room temperature to obtain a high silver ions of the solution; Wherein silver nitrate and sodium chloride the mole ratio is 1: 0.5; Silver nitrate and sodium hydroxide the mol ratio of 1: 1; With silver deposition and the sodium sulphate of the mass ratio is 0.5: 1; Weighing 3g the temperature is 300° c pressure of 1mpa of subcritical under the condition of water after etching with a sphericalal shell structure of grain diameter is 150 mu m a porous glass micro ball the porous glass micro ball in the concentration is 4mm mmol/l of the hydrofluoric acid solution to dip for 30 min and then separating the porous glass micro ball is set in the thickness is 30 mm mmol/l of the hydrochloric acid solution to dip in for 60 min then separation washing by de-ionized water to 3 times 105° c; The obtained porous glass micro sphere into 20ml having high valence of silver ion in solution slow speed stirring for 24 hours solid-liquid separation washing by de-ionized water to 3 times to 180 degrees c 4 hours then adding concentration is 100 mmol/l the phosphoric acid solution to stir then preparing a highly dispersed supported silver phosphate photocatalyst.

[0020] to obtain highly dispersed supported silver phosphate light catalyst to carry out the specific surface area analyzing its specific surface area of m2 634.2 or g. To obtain highly dispersed supported silver phosphate light catalyst into the concentration 10ml 30mg of orangeii g/l waste water in the 300w tungsten iodine lamp irradiating the reaction for 30 minutes decolouring ratio is 94.8%. The same condition the same amount of phosphoric acid silver for the pollutant removing efficiency is only 81.2%.

[0021] embodiment 2

[0022] the molar concentration is 0.2 mol/l of the silver nitrate solution of mol concentration is 0.2 mol/l of sodium chloride solution and mol concentration is 0.2 mol/l of sodium hydroxide solution stirring under indoor temperature time being 10 minutes to obtain a silver deposition the deposition filter and wash and then adding into a solution with sodium persulfate in the water solution in 60 degree c the stirring reaction after the stirring time is 2 hours; The temperature is reduced in room temperature to obtain a high silver ions of the solution; Wherein silver nitrate and sodium chloride the mole ratio is 1:

0.5; Silver nitrate and sodium hydroxide the mol ratio of 1: 1; With silver deposition and the sodium sulphate of the mass ratio is 0.1: 1; Weighing l 3g the temperature is 250° c pressure of 1mpa of subcritical under the condition of water after etching with a sphericalal shell structure is 8 m grain size mu of the porous glass micro ball the porous glass micro ball in the thickness is 2mm mmol/l of the hydrofluoric acid liquor to dip in for 20 min after separating and then the porous glass micro ball is set in the thickness 20 mm mmol/l the hydrochloric acid solution to immerse for 40 minutes then separation washing by de-ionized water to 2 times 105° c; The obtained porous glass micro ball adding 15 ml having high valence of silver ion in solution slow speed stirring at a solid-liquid separation washing by de-ionized water to 2 times of 150 degrees c drying for 2 hours then add the thickness 20 mm mmol/l the phosphoric acid solution to stir then preparing a highly dispersed supported silver phosphate photocatalyst.

[0023] the gained bentonite load he phosphoric acid silver catalyst is added to the concentration is set with 10ml 30mg g/l orangeii of the waste water in the 300w tungsten iodine lamp irradiating the reaction for 30 minutes decolouring ratio is 93.1%.

[0024] embodiment 3

[0025] the molar concentration of is 0.5 mol/l silver nitrate solution mole concentration is 0.5 mol/l sodium chloride solution and mole concentration is 0.5 mol/l of sodium hydroxide solution stirring under indoor temperature time is 20 minutes to obtain a silver deposition the deposition filter and wash and then adding into a solution with sodium persulfate in the aqueous solution of the c the 70° after stirring and reacting the stirring time is 4 hours; The temperature is reduced in room temperature to obtain a high silver ions of the solution; Wherein silver nitrate and sodium chloride the mole ratio is 1:

0.5; Silver nitrate and sodium hydroxide the mol ratio of 1: 1; With silver deposition and the sodium sulphate the weight ratio of 0.3: 1; Taking 2g the temperature is 300° c pressure of 1mpa of subcritical under the condition of water after etching with a sphericalal shell structure is 120 m grain size mu of the porous glass micro ball the porous glass micro ball in the concentration is 4mm mmol/l of the hydrofluoric acid solution to dip for 30 min and then separating the porous glass micro ball is set in the thickness is 30 mm mmol/l the hydrochloric acid solution to immerse for 50min then separation washing by de-ionized water to 3 times 105° c; The obtained porous glass micro sphere into 20ml having high valence of silver ion in solution slow speed stirring for 24 hours solid-liquid separation washing by de-ionized water to 3 times 160° c drying 3h and then adding the concentration is 100 mmol/l the phosphoric acid solution to stir then preparing a highly dispersed supported silver phosphate photocatalyst.

[0026] to obtain the bentonite load phosphotungstic acid silver catalyst is added to the concentration is set with 10ml 30mg per l of the methylene blue waste water in the 300w tungsten iodine lamp irradiating the reaction for 30 minutes decolouring ratio is 96.3%.