CN104549387A - Preparation method and application of catalyst of novel light degradation phosphate organic dye - Google Patents
Preparation method and application of catalyst of novel light degradation phosphate organic dye Download PDFInfo
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- CN104549387A CN104549387A CN201510055135.2A CN201510055135A CN104549387A CN 104549387 A CN104549387 A CN 104549387A CN 201510055135 A CN201510055135 A CN 201510055135A CN 104549387 A CN104549387 A CN 104549387A
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Abstract
The invention relates to a novel phosphate photocatalytic material Ag3Ni6 (PO4)5 and a preparation method thereof, and belongs to the field of novel inorganic photocatalytic materials. The photocatalytic material is prepared by a high-temperature solid-phase method, a chemical solution method, and a co-precipitation method. The technology is simple and easy to operate, and is convenient for industrial production, and the prepared material has uniform particles, good chemical stability, relatively good photocatalytic effects, and good stability, can be used for degrading organic pollutants under the radiation of ultraviolet light and visible light, and is an ideal material for the photocatalyst.
Description
Technical field
The present invention relates to preparation method and the application thereof of a kind of ultraviolet light and visible light-responded phosphate catalysis material, particularly for the Ag of degradable organic pollutant
3ni
6(PO
4)
5photochemical catalyst and preparation method thereof, belongs to inorganic field of photocatalytic material.
Background technology
Since 21 century; environmental pollution and problem of energy crisis become two large key factors of restriction human civilization sustainable and stable development gradually; organic matter such as dyestuff, the agricultural chemicals etc. of some difficult degradations are often present in air, water body and soil with very low concentration; have a strong impact on the Health and Living of people; and the elimination of environmental contaminants more needs to consume a large amount of energy, this proposes huge challenge to increasingly serious energy crisis.
Therefore, the mankind start that sight is turned to solar energy, and this is inexhaustible, in the exploitation of nexhaustible clean energy resource, current semiconductor solar energy photocatalytic technology is then the key point combining the energy and environment two large problems well, because pass through solar energy photon irradiation, photochemical catalyst excites carrier mobility, water is made to be converted into the clean hydrogen energy source can carrying out practical application, effectively will solve lack of energy, gas greenhouse, the crisis that environmental effect etc. are brought, and light-catalyzed reaction refers to that photochemical catalyst is after absorbing the photon higher than its band-gap energy, generate hole and electronics, these holes and electronics carry out oxidation reaction and reduction reaction respectively, toxic organic pollutant can be eliminated very well, by approach feasible for the cheapness becoming solution problem of environmental pollution further.Therefore, Photocatalyst becomes a kind of desirable environmental pollution treatment technology, becomes the study hotspot of people.
Photochemical catalyst has many kinds, and wherein most representative is titanium dioxide (TiO
2), but titanium dioxide at indoor or the local work having uviol lamp, almost can only can not utilize visible ray, consider the practicality of photochemical catalyst in decomposing harmful substances, utilize sunshine to be indispensable as light source.And although modified titanium dioxide can realize visible light-responded, photocatalytic activity is not high, and this limits the use of titanium dioxide optical catalyst greatly.The novel photocatalysis material of other developments, as nitrogen oxide, titanate, tungstates, vanadate, niobates, chromate etc., is all devoted to the visible light responsible photocatalytic character of material, but still there is a lot of deficiencies, needs to drop into larger research.As pucherite BiVO
4be a kind of conductor photocatalysis material of typical visible-light response type, its structure has very large effect to performance.But in the process preparing pucherite, the organic additive can introduce high price, not easily removing, purity difference, is unfavorable for catalytic applications, does not also meet the theory of green syt.Have that light conversion efficiency is low equally, poor stability and the problem such as spectrum respective range is narrow, therefore research and develop the new visible light-responded high efficiency photocatalyst that has and be very important.
Although photocatalysis research has carried out the several years, at present report to have visible light-responded photochemical catalyst kind still very limited.In 2010, Japanese scholars professor Ye Jinhua took the lead on Nature materials magazine, report a kind of silver phosphate photocatalyst with efficiency light degradation of organic substances ability; Chinese patent CN 103464185 A also report silver pyrophosphate, tripolyphosphate silver and silver metaphosphate three kinds of photochemical catalysts, can under ultraviolet light, visible ray or natural daylight radiation photocatalytic degradation organic compound.On the basis of these reports, we have studied a kind of novel silver orthophosphate class photochemical catalyst Ag
3ni
6(PO
4)
5, find that this compounds has excellent ultraviolet light, visible light-responded photocatalysis performance, and there is no report at present.
Summary of the invention
Meaning of the present invention is to provide the phosphate photochemical catalyst and preparation method thereof that a kind of preparation method is simple, have good photocatalytic activity, stronger application prospect.
For reaching above object, the technical solution used in the present invention is:
A novel phosphate catalysis material, its chemical formula is Ag
3ni
6(PO
4)
5.Described phosphate catalysis material is under the irradiation of ultraviolet light and visible ray, and the clearance of 120 min to methylene blue reaches 77%.
Be 0.36 μm by the phosphate catalysis material sample average grain diameter prepared by solid phase method, sample average grain diameter prepared by chemical solution method is 60 nm.
The preparation method of the first phosphate catalysis material, is characterized in that adopting high temperature solid-state method to prepare powder, comprises the following steps:
(1) with the compound of silver ion, containing nickel ion, containing the compound of phosphonium ion for raw material, by general formula Ag
3ni
6(PO
4)
5the stoichiometric proportion of middle corresponding element takes each raw material, mixes after grinding;
(2) the mixture precalcining in air atmosphere step (1) obtained, precalcining temperature is 200 ~ 600 DEG C, and calcination time is 4 ~ 20 hours, naturally after cooling, grinds and mixes;
(3) calcined in air atmosphere by the mixture that step (2) obtains, calcining heat is 600 ~ 1000 DEG C, and calcination time is 5 ~ 20 hours, naturally after cooling, namely obtains a kind of phosphate catalysis material powder after grinding evenly.
Described in above-mentioned steps is one in silver oxide, silver nitrate or two kinds of combinations containing the compound of silver element; The described compound containing nickel element is one in nickel oxide, nickelous carbonate or two kinds of combinations; The described compound containing P elements is one or more combinations in phosphorus pentoxide, ammonium dihydrogen phosphate (ADP), phosphoric acid.
Calcining heat described in step (2) is 250 ~ 600 DEG C, and calcination time is 5 ~ 19 hours; Calcining heat described in step (3) is 650 ~ 950 DEG C, and calcination time is 6 ~ 19 hours.
The preparation method of another kind of phosphate catalysis material, is characterized in that adopting chemical solution method, comprises the following steps:
(1) by chemical formula Ag
3ni
6(PO
4)
5in the stoichiometric proportion of each element, first take containing silver ion Ag
+compound, be dissolved in appropriate dilute hydrochloric acid solution, add thermal agitation, until dissolve completely, add appropriate oxalic acid, obtain solution A; Take containing nickel ion Ni
2+compound, be dissolved in appropriate dilute hydrochloric acid solution, add thermal agitation, until dissolve completely, add appropriate oxalic acid, obtain B solution; Take containing phosphonium ion P
5+compound, be dissolved in appropriate dilute hydrochloric acid solution, add thermal agitation, until dissolve completely, obtain C solution.Finally, A, B, C solution is mixed;
(2) placed in baking oven by said mixture solution, temperature is 50 DEG C-100 DEG C, and the time is 12h, and ageing is also dried;
(3) after naturally cooling, take out presoma, calcine in air atmosphere, calcining heat is 600 ~ 950 DEG C, and calcination time is 5 ~ 20 hours, and naturally after cooling, namely grinding evenly obtains a kind of phosphate catalysis material powder.
The compound containing silver element described in above step is one or more combinations in silver oxide, silver nitrate, silver carbonate, silver sulfate; The described compound containing nickel element is one or more combinations in nickel oxide, nickelous carbonate, nickelous sulfate, nickel nitrate; The described compound containing P elements is one or more combinations in phosphorus pentoxide, ammonium dihydrogen phosphate (ADP), phosphoric acid.
Calcining heat described in step (3) is 650 ~ 900 DEG C, and calcination time is 6 ~ 19 hours.
A preparation method for phosphate catalysis material, is characterized in that adopting coprecipitation to prepare powder, comprises the following steps:
(1) form soluble silver salt solution, described solution concentration is 0.2 ~ 2mol/L;
(2) form soluble nickel salting liquid, described solution concentration is 0.2 ~ 2mol/L;
(3) form titanium pigment salting liquid, described solution concentration is 0.2 ~ 2mol/L;
(4) forming volume fraction is the ammonia spirit of 20 ~ 40%, stirs;
(5) by chemical formula Ag
3ni
6(PO
4)
5proportioning is by above-mentioned silver salt, nickel salt, microcosmic salt solution, and mix and blend, drips ammoniacal liquor to PH scope 9 ~ 10, and reaction precipitation thing, after separation, washing, drying, obtains presoma;
(6) by presoma at 600 ~ 950 DEG C of temperature lower calcinations, calcination time is 7 ~ 20 hours, obtains a kind of phosphate catalysis material powder.
Soluble silver salt described in above step can adopt one or more combinations in silver oxide, silver nitrate, silver carbonate, silver sulfate, is dissolved in deionized water or watery hydrochloric acid and adds thermal agitation gained.
Described soluble nickel salt can adopt one or more combinations in nickel oxide, nickelous carbonate, nickelous sulfate, nickel nitrate, is dissolved in deionized water or watery hydrochloric acid and adds thermal agitation gained.
Described solubility microcosmic salt can adopt one or more combinations in phosphorus pentoxide, ammonium metaphosphate, phosphoric acid, is dissolved in deionized water and adds thermal agitation gained.
Calcining heat described in step (6) is 650 ~ 900 DEG C, and calcination time is 8 ~ 19 hours.
Compared with prior art, technical solution of the present invention advantage is:
1, Ag
3ni
6(PO
4)
5photocatalyst material preparation method is simple, process equipment is simple, sample particle is little and evenly, the sample average grain diameter prepared by solid phase method is 0.36 μm, and sample average grain diameter prepared by chemical solution method is 60 nm;
2, prepared Ag
3ni
6(PO
4)
5photochemical catalyst all has absorption in very wide spectral region, thus under the irradiation of ultraviolet light and visible ray, Ag
3ni
6(PO
4)
5photochemical catalyst all can high efficiency photocatalysis degradation of methylene blue, has good photocatalytic activity;
3, the present invention discharges without waste water and gas, environmentally friendly, and is easy to suitability for industrialized production.
Accompanying drawing explanation
The Ag of Fig. 1 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5the X-ray powder diffraction pattern of sample;
The Ag of Fig. 2 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5the SEM(SEM of sample) collection of illustrative plates;
The Ag of Fig. 3 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5sample particle diameter analysis chart;
The Ag of Fig. 4 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5sample uv-visible absorption spectra, illustration is the picture of sample;
The Ag of Fig. 5 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5sample when illumination to the degradation curve of organic dyestuff methylene blue;
The Ag of Fig. 6 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5the kinetic curve figure of sample degradation methylene blue;
The Ag of Fig. 7 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5the SEM(SEM of sample) collection of illustrative plates;
The Ag of Fig. 8 obtained by the embodiment of the present invention 1
3ni
6(PO
4)
5sample particle diameter analysis chart.
Detailed description of the invention
Embodiment 1:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver oxide Ag respectively
2o:1.74 gram, nickel oxide NiO:2.24 gram, ammonium dihydrogen phosphate (ADP) NH
4h
2pO
4: 2.88 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining, temperature is 250 DEG C, calcination time 5 hours, naturally after cooling, taking-up sample; By the raw material of precalcining, fully mixed grinding is even again, again calcines, temperature 650 DEG C, calcination time 19 hours in air atmosphere, and namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
See accompanying drawing 1, it is the X-ray powder diffraction pattern by sample prepared by the present embodiment technical scheme, and XRD test result shows, prepared phosphate Ag
3ni
6(PO
4)
5for monophase materials, degree of crystallinity is better;
See accompanying drawing 2, it is the SEM(SEM by sample prepared by the present embodiment technical scheme) collection of illustrative plates;
See accompanying drawing 3, it is the granularmetric analysis figure by sample prepared by the present embodiment technical scheme, and as can be seen from the figure, gained sample particle is uniformly dispersed, and average grain diameter is 0.36 μm;
See accompanying drawing 4, it is the uv-visible absorption spectra by sample prepared by the present embodiment technical scheme, and accompanying drawing is the picture of the powder sample obtained, and as can be seen from the figure, this sample all has absorption in ultraviolet light and visible-range;
See accompanying drawing 5, it is by the degradation curve of sample prepared by the present embodiment technical scheme to organic dyestuff methylene blue under different visible light application times.As can be seen from the figure, degradation rate 120 min of this sample photocatalytic degradation methylene blue reaches 77%, and the phosphate Ag prepared is described
3ni
6(PO
4)
5material has certain photocatalytic activity;
See accompanying drawing 6, it is the kinetic curve figure by sample degradation methylene blue prepared by the present embodiment technical scheme, and as can be seen from the figure, the apparent kinetics speed constant of this sample photocatalytic degradation methylene blue is 0.011 min
-1.
Embodiment 2:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver nitrate AgNO respectively
3: 1.70 grams, nickelous carbonate NiCO
3: 2.37 grams, phosphorus pentoxide P
2o
5: 1.18 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining, temperature is 300 DEG C, calcination time 10 hours, naturally after cooling, taking-up sample; By the raw material of precalcining, fully mixed grinding is even again, again calcines, temperature 750 DEG C, calcination time 10 hours in air atmosphere, and namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 3:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver nitrate AgNO respectively
3: 1.70 grams, nickel oxide NiO:1.49 gram, phosphoric acid H
3pO
4: 1.63 grams, to grind in agate mortar and after mixing, select air atmosphere precalcining, temperature is 600 DEG C, calcination time 19 hours, naturally after cooling, taking-up sample; By the raw material of precalcining, fully mixed grinding is even again, again calcines, temperature 950 DEG C, calcination time 6 hours in air atmosphere, and namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 4:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver nitrate AgNO respectively
3: 1.70 grams, nickelous sulfate NiSO
46H
2o:5.26 gram, phosphoric acid H
3pO
4: 1.63 grams, dissolve respectively and add appropriate oxalic acid, after stirring, obtaining A, B, C solution, mixing, continuing to stir a period of time.Placed in baking oven by the mixed solution obtained, temperature is 100 DEG C, dries 12h, and naturally after cooling, take out presoma, calcine in air atmosphere, calcining heat is 650 DEG C, and calcination time is 19 hours, and namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
See accompanying drawing 7, it is the SEM(SEM by sample prepared by the present embodiment technical scheme) collection of illustrative plates, see accompanying drawing 8, it is the granularmetric analysis figure by sample prepared by the present embodiment technical scheme, as can be seen from the figure, gained sample particle dispersion evenly, average grain diameter is 60 nm;
Its main absorption spectrum, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 5:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver sulfate Ag respectively
2sO
4: 1.56 grams, nitric acid nickel (NO
3)
26H
2o:5.82 gram, phosphorus pentoxide P
2o
5: 1.18 grams, dissolve respectively and add appropriate oxalic acid, after stirring, obtaining A, B, C solution, mixing, continuing to stir a period of time.Placed in baking oven by the mixed solution obtained, temperature is 50 DEG C, dries 12h, and naturally after cooling, take out presoma, calcine in air atmosphere, calcining heat is 800 DEG C, and calcination time is 10 hours, and namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 4 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 6:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver carbonate Ag respectively
2cO
3: 1.38 grams, nickel oxide NiO:1.49 gram, ammonium dihydrogen phosphate (ADP) NH
4h
2pO
4: 1.92 grams, dissolve respectively and add appropriate oxalic acid, after stirring, obtaining A, B, C solution, mixing, continuing to stir a period of time.Placed in baking oven by the mixed solution obtained, temperature is 80 DEG C, dries 12h, and naturally after cooling, take out presoma, calcine in air atmosphere, calcining heat is 900 DEG C, and calcination time is 6 hours, and namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 4 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 7:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver oxide Ag
2o:1.16 gram, configuration concentration is the silver salt solution of 2mol/L, takes nitric acid nickel (NO
3)
26H
2o:5.82 gram, configuration concentration is the nickel salt solution of 2mol/L, takes phosphoric acid H
3pO
4: 1.63 grams, configuration concentration is the nickel salt solution of 2mol/L, mixing three kinds of solution & stir, is the ammonia spirit of 30% to mixed solution and dripping volume fraction, stops when PH is about 9 ~ 10, stir, after deionized water and ethanol washing, put into baking oven oven dry and obtain presoma, select air atmosphere precalcining, by above-mentioned presoma 650 DEG C of temperature lower calcinations 19 hours, namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 8:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver nitrate AgNO
3: 2.04 grams, configuration concentration is the silver salt solution of 2mol/L, takes nickelous carbonate NiCO
36H
2o:2.85 gram, configuration concentration is the nickel salt solution of 2mol/L, takes phosphorus pentoxide P
2o
5: 1.42 grams, configuration concentration is the nickel salt solution of 2mol/L, mixing three kinds of solution & stir, is the ammonia spirit of 30% to mixed solution and dripping volume fraction, stops when PH is about 9 ~ 10, stir, after deionized water and ethanol washing, put into baking oven oven dry and obtain presoma, select air atmosphere precalcining, by above-mentioned presoma 900 DEG C of temperature lower calcinations 8 hours, namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Embodiment 9:
Preparation Ag
3ni
6(PO
4)
5
According to chemical formula Ag
3ni
6(PO
4)
5, take silver sulfate Ag
2sO
4: 1.34 grams, configuration concentration is the silver salt solution of 2mol/L, takes nickelous sulfate NiSO
46H
2o:4.51 gram, configuration concentration is the nickel salt solution of 2mol/L, takes ammonium dihydrogen phosphate (ADP) NH
4h
2pO
4: 1.64 grams, configuration concentration is the nickel salt solution of 2mol/L, mixing three kinds of solution & stir, is the ammonia spirit of 30% to mixed solution and dripping volume fraction, stops when PH is about 9 ~ 10, stir, after deionized water and ethanol washing, put into baking oven oven dry and obtain presoma, select air atmosphere precalcining, by above-mentioned presoma 750 DEG C of temperature lower calcinations 15 hours, namely cooling grinding obtains phosphate Ag
3ni
6(PO
4)
5powder.
Its main structure and morphology, absorption spectrum, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Claims (13)
1. a novel phosphate catalysis material, is characterized in that: its chemical formula is Ag
3ni
6(PO
4)
5, described phosphate catalysis material is under the irradiation of ultraviolet light and visible ray, and the clearance of 120 min to methylene blue reaches 77%.
2. phosphate catalysis material according to claim 1, is characterized in that: the sample average grain diameter prepared by solid phase method is 0.36 μm, and sample average grain diameter prepared by chemical solution method is 60 nm.
3. a preparation method for phosphate catalysis material as claimed in claim 1, is characterized in that adopting high temperature solid-state method to prepare powder, comprises the following steps:
(1) with the compound of silver ion, containing nickel ion, containing the compound of phosphonium ion for raw material, by general formula Ag
3ni
6(PO
4)
5the stoichiometric proportion of middle corresponding element takes each raw material, mixes after grinding;
(2) the mixture precalcining in air atmosphere step (1) obtained, precalcining temperature is 200 ~ 600 DEG C, and calcination time is 4 ~ 20 hours, naturally after cooling, grinds and mixes;
(3) calcined in air atmosphere by the mixture that step (2) obtains, calcining heat is 600 ~ 1000 DEG C, and calcination time is 5 ~ 20 hours, naturally after cooling, namely obtains a kind of phosphate catalysis material powder after grinding evenly.
4. the preparation method of a kind of novel phosphate catalysis material according to claim 3, is characterized in that: the described compound containing silver element is one in silver oxide, silver nitrate or two kinds of combinations; The described compound containing nickel element is one in nickel oxide, nickelous carbonate or two kinds of combinations; The described compound containing P elements is one or more combinations in phosphorus pentoxide, ammonium dihydrogen phosphate (ADP), phosphoric acid.
5. the preparation method of a kind of novel phosphate catalysis material according to claim 3, it is characterized in that: the calcining heat described in step (2) is 250 ~ 600 DEG C, calcination time is 5 ~ 19 hours; Calcining heat described in step (3) is 650 ~ 950 DEG C, and calcination time is 6 ~ 19 hours.
6. a preparation method for phosphate catalysis material as claimed in claim 1, is characterized in that adopting chemical solution method, comprises the following steps:
(1) by chemical formula Ag
3ni
6(PO
4)
5in the stoichiometric proportion of each element, first take containing silver ion Ag
+compound, be dissolved in appropriate dilute hydrochloric acid solution, add thermal agitation, until dissolve completely, add appropriate oxalic acid, obtain solution A; Take containing nickel ion Ni
2+compound, be dissolved in appropriate dilute hydrochloric acid solution, add thermal agitation, until dissolve completely, add appropriate oxalic acid, obtain B solution; Take containing phosphonium ion P
5+compound, be dissolved in appropriate dilute hydrochloric acid solution, add thermal agitation, until dissolve completely, obtain C solution; Finally, A, B, C solution is mixed;
(2) placed in baking oven by said mixture solution, temperature is 50 DEG C-100 DEG C, and the time is 12h, and ageing is also dried;
(3) after naturally cooling, take out presoma, calcine in air atmosphere, calcining heat is 600 ~ 950 DEG C, and calcination time is 5 ~ 20 hours, and naturally after cooling, namely grinding evenly obtains a kind of phosphate catalysis material powder.
7. the preparation method of a kind of novel phosphate catalysis material according to claim 6, is characterized in that: the described compound containing silver element is one or more combinations in silver oxide, silver nitrate, silver carbonate, silver sulfate; The described compound containing nickel element is one or more combinations in nickel oxide, nickelous carbonate, nickelous sulfate, nickel nitrate; The described compound containing P elements is one or more combinations in phosphorus pentoxide, ammonium dihydrogen phosphate (ADP), phosphoric acid.
8. the preparation method of a kind of novel phosphate catalysis material according to claim 6, it is characterized in that: the calcining heat described in step (3) is 650 ~ 900 DEG C, calcination time is 6 ~ 19 hours.
9. a preparation method for phosphate catalysis material as claimed in claim 1, is characterized in that adopting coprecipitation to prepare powder, comprises the following steps:
(1) form soluble silver salt solution, described solution concentration is 0.2 ~ 2mol/L;
(2) form soluble nickel salting liquid, described solution concentration is 0.2 ~ 2mol/L;
(3) form titanium pigment salting liquid, described solution concentration is 0.2 ~ 2mol/L;
(4) forming volume fraction is the ammonia spirit of 20 ~ 40%, stirs;
(5) by chemical formula Ag
3ni
6(PO
4)
5proportioning is by above-mentioned silver salt, nickel salt, microcosmic salt solution, and mix and blend, drips ammoniacal liquor to PH scope 9 ~ 10, and reaction precipitation thing, after separation, washing, drying, obtains presoma;
(6) by presoma at 600 ~ 950 DEG C of temperature lower calcinations, calcination time is 7 ~ 20 hours, obtains a kind of phosphate catalysis material powder.
10. the preparation method of a kind of novel phosphate catalysis material according to claim 9, it is characterized in that: described soluble silver salt can adopt one or more combinations in silver oxide, silver nitrate, silver carbonate, silver sulfate, is dissolved in deionized water or watery hydrochloric acid and adds thermal agitation gained.
The preparation method of 11. a kind of novel phosphate catalysis materials according to claim 9, it is characterized in that: described soluble nickel salt can adopt one or more combinations in nickel oxide, nickelous carbonate, nickelous sulfate, nickel nitrate, is dissolved in deionized water or watery hydrochloric acid and adds thermal agitation gained.
The preparation method of 12. a kind of novel phosphate catalysis materials according to claim 9, it is characterized in that: described solubility microcosmic salt can adopt one or more combinations in phosphorus pentoxide, ammonium metaphosphate, phosphoric acid, is dissolved in deionized water and adds thermal agitation gained.
The preparation method of 13. a kind of novel phosphate catalysis materials according to claim 9, it is characterized in that: the calcining heat described in step (6) is 650 ~ 900 DEG C, calcination time is 8 ~ 19 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104888819A (en) * | 2015-06-18 | 2015-09-09 | 苏州德捷膜材料科技有限公司 | Preparation and photocatalytic application of Na4Ni3P4O15 photocatalyst |
| CN105854909A (en) * | 2016-04-21 | 2016-08-17 | 天津工业大学 | Nickel modified silver phosphate photocatalyst and synthesis method thereof |
| CN106423230A (en) * | 2016-10-19 | 2017-02-22 | 常州大学 | Preparation method of nickel oxide compound yttrium phosphate catalyst |
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| CN105854909A (en) * | 2016-04-21 | 2016-08-17 | 天津工业大学 | Nickel modified silver phosphate photocatalyst and synthesis method thereof |
| CN106423230A (en) * | 2016-10-19 | 2017-02-22 | 常州大学 | Preparation method of nickel oxide compound yttrium phosphate catalyst |
| CN106423230B (en) * | 2016-10-19 | 2018-10-16 | 常州大学 | A kind of preparation method of nickel oxide compound phosphoric acid yttrium catalyst |
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