CN103977758B - A kind of preparation method of tantalum doping hydrous antimony pentoxide (HAP) sorbing material - Google Patents

A kind of preparation method of tantalum doping hydrous antimony pentoxide (HAP) sorbing material Download PDF

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CN103977758B
CN103977758B CN201410249872.1A CN201410249872A CN103977758B CN 103977758 B CN103977758 B CN 103977758B CN 201410249872 A CN201410249872 A CN 201410249872A CN 103977758 B CN103977758 B CN 103977758B
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hap
parts
antimony pentoxide
solution
reactor
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CN103977758A (en
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张锐
牟婉君
李兴亮
谢翔
余钱红
吕开
魏洪源
蹇源
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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Abstract

The invention discloses the preparation method of a kind of tantalum doping hydrous antimony pentoxide (HAP) sorbing material, characterized in that getting concentration is 0.7 ~ 0.8mol/L? SbCl 5hydrochloric acid solution 15 ~ 18 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 0 ~ 18 part, is uniformly mixed; Does is in above-mentioned solution, add concentration 0.09 ~ 0.11mol/L? TaCl 5ethanolic solution 0 ~ 18 part, makes the mol ratio of Ta/Sb in solution be 0 ~ 0.18, stirs and makes it fully mix; In above-mentioned solution, add the ammoniacal liquor 19 ~ 21 parts that concentration is 8mol/L again, adjust ph to 1 ~ 2, stir 0.5 ~ 1h; Sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange intensification and rate of temperature fall be controlled as 1 DEG C/min, after at 160 ~ 180 DEG C, hydrothermal treatment consists 24 ~ 48h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality respectively, then is placed in-40 DEG C of freeze drier freeze dryings, obtain tantalum doping hydrous antimony pentoxide (HAP) material.

Description

A kind of preparation method of tantalum doping hydrous antimony pentoxide (HAP) sorbing material
Technical field
The present invention relates to the preparation method of a kind of tantalum doping hydrous antimony pentoxide (HAP) sorbing material, the Sr in neutral solution can be adsorbed 2+, belong to the Synthesis and applications field of inorganic functional material.
Background technology
Hydrous antimony pentoxide (HAP) (HAP) has special optionally Inorganic-ion-exchange material as one, and have the layered polymer of cubic cell structure, the hydrone in its layer structure provides tradable H with the form of hydrogen bond +, show cation exchange property.The preparations and applicatio of current researcher to hydrous antimony pentoxide (HAP) is paid much attention to, and particularly extremely payes attention in radionuclide Separation Research field always.The HAP successfully utilizing him to prepare as far back as people such as nineteen sixty-eight Girardi effectively is separated in concentrated hydrochloric acid medium 24na.Abe, systematically have studied preparation and the exchange adsorption performance of HAP, points out " exchange selectivity of HAP is comparatively large by the impact of preparation condition, and this performance is highly significant on separation science ".The people such as Zouad have studied HAP to Sr 2+ion-exchange absorption performance; The proposition HAP such as Weng Haomin are separated radioactivity 90the flow process of Sr; The HAP of people's synthesis such as Sun Zhaoxiang is to the Sc of 3 valencys 3+there is good adsorptive selectivity.Technique study HAP in dilute acid soln that Chen Hong etc. are combined with experiment by theory calculate adsorbs Sr 2+mechanism.At present HAP material is improved it to Sr by introducing metallic ion-doping modification 2+the method of adsorption capacity is there are no patent document and non-patent literature report.
Summary of the invention
The object of the invention is not enough for prior art and the preparation method that a kind of tantalum adulterates hydrous antimony pentoxide (HAP) sorbing material is provided, transition metal ions tantalum is characterized in introduce in hydrous antimony pentoxide (HAP) crystal structure, Emission in Cubic HPA material skeleton is changed, is conducive to Sr 2+with the H in duct +, Na +exchange fully, significantly improve HAP to Sr 2+adsorption capacity.By aperture, the hole of the amount controlled material skeleton of controlled doping element, obtain the novel porous materials that duct is unimpeded, voidage is high, physicochemical property is stable, thus realize Sr 2+ion is free exchange in enough large space, duct, improves the adsorption capacity of this material to Sr.
Object of the present invention is realized by following technical measures, and wherein said raw material number, except specified otherwise, is parts by weight.
The hydrous antimony pentoxide (HAP) preparation of tantalum doping is concrete according to the following steps:
1) getting concentration is 0.7 ~ 0.8mol/LSbCl 5hydrochloric acid solution 15 ~ 18 parts, is preferably 16 ~ 18 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 0 ~ 18 part, preferably 6 ~ 9 parts, be uniformly mixed;
2) in above-mentioned solution, adding concentration is 0.09 ~ 0.11mol/LTaCl 5ethanolic solution, 0 ~ 18 part, is preferably 9 ~ 12 parts, makes the mol ratio of Ta/Sb in solution be 0 ~ 0.18, stir and make it fully mix;
3) in above-mentioned solution, add the ammoniacal liquor 19 ~ 21 parts that concentration is 8mol/L again, be preferably 19 ~ 20 parts, adjust ph to 1 ~ 2, stir 0.5 ~ 1h;
4) polytetrafluoroethylene (PTFE) reactor is sealed, be placed in program baking oven, arrange intensification and rate of temperature fall be controlled as 1 DEG C/min, temperature 160 ~ 180 DEG C, after hydrothermal treatment consists 24-48h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality respectively, be placed in temperature-40 DEG C of freeze drier freeze dryings again, obtain tantalum doping hydrous antimony pentoxide (HAP) material.
The tantalum doping hydrous antimony pentoxide (HAP) sorbing material that the preparation method that tantalum adulterates hydrous antimony pentoxide (HAP) sorbing material prepares.
Tantalum doping hydrous antimony pentoxide (HAP) sorbing material improves this material to Sr 2+adsorption capacity.
Mix tantalum hydrous antimony pentoxide (HAP) absorption Sr 2+experiment as follows:
1) preparing 500mL concentration is the strontium nitrate solution of 200mg/L;
2) adsorption experiment carries out in constant temperature oscillator, the difference taking 200mg mixes the hydrous antimony pentoxide (HAP) of tantalum amount in 200mL volumetric flask, add the strontium nitrate solution that 100mL concentration is 200mg/L respectively, 25 DEG C of constant temperature oscillation 24h carry out adsorption experiment, above-mentioned solution is filtered, filtrate carries out, in centrifuging and taking supernatant liquor 5mL to 100ml volumetric flask, using redistilled water constant volume.With the Sr in atomic absorption detecting solution 2+content.Adsorbance Q is calculated with following formula e:
Q e = ( C 0 - C e ) m
Q in formula efor mixing the adsorbance (mg/g) of tantalum hydrous antimony pentoxide (HAP) during balance; C 0and C ebe respectively Sr in aqueous phase 2+initial concentration (mg/L) and equilibrium concentration (mg/L); M is the quality (g) of mixing tantalum hydrous antimony pentoxide (HAP) sample.
Structural characterization and performance test
1, Y-4Q type X-ray diffractometer (XRD) is adopted to analyze mutually, shown in Fig. 1 a and Fig. 1 b the thing that embodiment 1 and embodiment 6 obtain product.
Result shows: the XRD diffraction spectra obtaining product conforms to standard card JCPDS32-44, and after adulterate front and doping, sample is cubic four hydrous antimony pentoxide (HAP) (Sb 2o 54H 2o), the crystal structure not changing antimony pentoxide after tantalum doping does not change.
2, adopt Ultra55 type field emission scanning electron microscope (SEM) to observe pattern that embodiment 1 and embodiment 6 obtain sample, is learnt that by Fig. 2 a and Fig. 2 b the pattern of product is the nano particle be evenly distributed, is of a size of 10nm ~ 50nm.
3, the atomic absorption instrument of PE company is adopted to measure Sr after ion-exchange in solution 2+ion concentration, shown in Fig. 3, Fig. 4 and Fig. 5.
Fig. 3 is that tantalum doping adsorbs Sr to antimony pentoxide 2+the impact of absorption property
Result shows: along with the increase of tantalum doping, antimony pentoxide is to Sr 2+adsorption capacity strengthen, when the mol ratio of Ta/W in product is 0.1, antimony pentoxide is to Sr 2+adsorption effect best, therefore in adsorption experiment, we select Ta/W mol ratio in antimony pentoxide sample to be 0.1 as optimum doping amount.
Fig. 4 is that pH value is to tantalum doping antimony pentoxide absorption Sr 2+the impact of absorption property
Result shows: tantalum doping antimony pentoxide is to Sr 2+absorption property be obviously better than the antimony pentoxide that do not adulterate, reach maximum adsorption capacity when pH is 3, and reach adsorption equilibrium, illustrate that tantalum doping antimony pentoxide material is to Sr under acid and neutrallty condition 2+advantages of good adsorption effect.
Fig. 5 adulterates antimony pentoxide to Sr to tantalum the time 2+the impact of absorption property
Result shows: along with the increase of adsorption time, and antimony pentoxide and tantalum doping antimony pentoxide are to Sr 2+adsorption capacity significantly increase, be reach adsorption equilibrium in 20 minutes when the time.
Tool of the present invention has the following advantages:
Adopt hydro-thermal method by transition metal ions tantalum doping antimony pentoxide, regulate the aperture of its structure and pass, the hydrous antimony pentoxide (HAP) of acquisition, significantly improves this material to Sr 2+adsorption capacity, whole technological process is simple, is conducive to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 a is the XRD collection of illustrative plates of hydrous antimony pentoxide (HAP) of tantalum of not adulterating
Fig. 1 b is the XRD collection of illustrative plates of the hydrous antimony pentoxide (HAP) that tantalum doping obtains
Fig. 2 a be do not adulterate tantalum hydrous antimony pentoxide (HAP) SEM figure
Fig. 2 b is the SEM figure of the hydrous antimony pentoxide (HAP) that tantalum doping obtains
Fig. 3 tantalum doping adsorbs Sr to antimony pentoxide 2+the impact of absorption property
Fig. 4 is different, and pH value adsorbs Sr to antimony pentoxide 2+the impact of absorption property
Fig. 5 is different, and adsorption time adsorbs Sr to antimony pentoxide 2+the impact of absorption property
Specific embodiments
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only further described for the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Get the SbCl of 0.7mol/L 5hydrochloric acid solution 18 parts, be placed in polytetrafluoroethylene (PTFE) reactor, add redistilled water 18 parts, stirring makes it fully mix, the ammoniacal liquor 19 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.43, stir 0.5h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 160 DEG C, after hydrothermal treatment consists 48h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, be placed in temperature-40 DEG C of freeze drier freeze dryings again, the hydrous antimony pentoxide (HAP) material obtained.
Embodiment 2
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 15 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 16 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 2 parts, the mol ratio of Ta/Sb in solution is made to be that 0.02 stirring makes it fully mix, the ammoniacal liquor 19 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.35, liquid stirs 0.5h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 160 DEG C, after hydrothermal treatment consists 48h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, be placed in temperature-40 DEG C of freeze drier freeze dryings again, what obtain mixes tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 3
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 15 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 14 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 4 parts, the mol ratio of Ta/Sb in solution is made to be that 0.04 stirring makes it fully mix, the ammoniacal liquor 19 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.29, liquid stirs 0.5h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 160 DEG C, after hydrothermal treatment consists 48h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality respectively, be placed in temperature-40 DEG C of freeze drier freeze dryings again, what obtain mixes tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 4
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 15 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 12 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 6 parts, the mol ratio of Ta/Sb in solution is made to be that 0.06 stirring makes it fully mix, the ammoniacal liquor 20 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.84, liquid stirs 0.5h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 160 DEG C, after hydrothermal treatment consists 48h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, be placed in temperature-40 DEG C of freeze drier freeze dryings again, what obtain mixes tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 5
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 15 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 10 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 8 parts, the mol ratio of Ta/Sb in solution is made to be that 0.08 stirring makes it fully mix, the ammoniacal liquor 20 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.75, liquid stirs 0.75h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 170 DEG C, after hydrothermal treatment consists 36h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, be placed in temperature-40 DEG C of freeze drier freeze dryings again, what obtain mixes tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 6
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 16 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 8 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.10mol/LTaCl 5ethanolic solution 11 parts, makes the mol ratio of Ta/Sb in solution be that 0.1 stirring makes it fully mix.The ammoniacal liquor 20 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.62, liquid stirs 0.75h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 170 DEG C, after hydrothermal treatment consists 36h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 7
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 16 parts is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 6 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 12 parts, makes the mol ratio of Ta/Sb in solution be 0.12 mix and make it fully mix.The ammoniacal liquor 21 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.96, liquid stirs 0.75h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 170 DEG C, after hydrothermal treatment consists 36h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 8
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 16 parts is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 4, and stir and make it fully mix, in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 14 parts, makes the mol ratio of Ta/Sb in solution be that 0.14 stirring makes it fully mix.The ammoniacal liquor 21 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.85, liquid stirs 0.75h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 170 DEG C, after hydrothermal treatment consists 36h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 9
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 16 parts is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 2 parts, stir and make it fully mix, then in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 16 parts, makes the mol ratio of Ta/Sb in solution be that 0.16 stirring makes it fully mix.The ammoniacal liquor 21 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.79, liquid stirs 1h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 180 DEG C, after hydrothermal treatment consists 24h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 10
Get the SbCl of 0.8mol/L 5hydrochloric acid solution 16 parts is placed in polytetrafluoroethylene (PTFE) reactor, and stir and make it fully mix, in above-mentioned solution, add concentration is 0.11mol/LTaCl 5ethanolic solution 18 parts, makes the mol ratio of Ta/Sb in solution be that 0.18 stirring makes it fully mix.The ammoniacal liquor 21 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.71, liquid stirs 1h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 180 DEG C, after hydrothermal treatment consists 24h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 11
Get the SbCl of 0.7mol/L 5hydrochloric acid solution 18 parts is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 7 parts, and stir and make it fully mix, in above-mentioned solution, add concentration is 0.09mol/LTaCl 5ethanolic solution 11 parts, makes the mol ratio of Ta/Sb in solution be that 0.09 stirring makes it fully mix.The ammoniacal liquor 21 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.09, liquid stirs 1h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 180 DEG C, after hydrothermal treatment consists 24h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Embodiment 12
Get the SbCl of 0.7mol/L 5hydrochloric acid solution 18 parts is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 4.5 parts, and stir and make it fully mix, in above-mentioned solution, add concentration is 0.09mol/LTaCl 5ethanolic solution 13.5 parts, makes the mol ratio of Ta/Sb in solution be that 0.11 stirring makes it fully mix.The ammoniacal liquor 21 parts that concentration is 8mol/L is added again in above-mentioned solution, adjust ph to 1.02, liquid stirs 1h, sealing polytetrafluoroethylene (PTFE) reactor, be placed in program baking oven, arrange heat up and rate of temperature fall control be 1 DEG C/min, temperature 180 DEG C, after hydrothermal treatment consists 24h. has reacted, take out reactor, be cooled to room temperature. product is washed with distilled water to neutrality, then is placed in temperature-40 DEG C of freeze drier freeze dryings, acquisition mix tantalum hydrous antimony pentoxide (HAP) material.
Application example 1
Take each 200mg of sample of sample and other mol ratio (0.09 and 0.11) prepared in above 2 ~ 10 embodiments, join respectively 100ml by Sr (NO3) 2 prepare containing strontium 20mg/L solution in, reaction time 24h, by Sr in solution after atomic absorption spectrometry absorption 2+concentration, calculate the hydrous antimony pentoxide (HAP) of different tantalum doping to Sr 2+adsorption capacity, shown in Fig. 3.
Application example 2
To take in embodiment 1 and embodiment 6 each 200mg of sample of preparation, join respectively 100ml by Sr (NO3) 2 prepare containing in the different pH solution of strontium 20mg/L, reaction time 24h, by Sr in atomic absorption spectrometry absorption afterwards solution 2+concentration, calculated hydration antimony pentoxide and tantalum mix hydrous antimony pentoxide (HAP) to Sr 2+adsorption capacity, shown in Fig. 4.
Application example 3
Take each 200mg of sample of preparation in embodiment 1 and embodiment 6, join respectively 100ml by Sr (NO3) 2 prepare containing strontium 20mg/L solution in, reaction time is 1min, 3min, 5min, 7min, 10min, 15min, 30min, 60min, 120min, 180min, 240min respectively, by Sr in solution after atomic absorption spectrometry absorption 2+concentration, calculated hydration antimony pentoxide and tantalum mix hydrous antimony pentoxide (HAP) to Sr 2+adsorption capacity, shown in Fig. 5.

Claims (4)

1. a preparation method for tantalum doping hydrous antimony pentoxide (HAP) sorbing material, is characterized in that the method comprises the following steps:
1) getting concentration is 0.7 ~ 0.8mol/LSbCl 5hydrochloric acid solution 15 ~ 18 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 0 ~ 18 part, is uniformly mixed;
2) in above-mentioned solution, adding concentration is 0.09 ~ 0.11mol/LTaCl 5ethanolic solution 2 ~ 18 parts, makes the mol ratio of Ta/Sb in solution be 0.02 ~ 0.18, stirs and makes it fully mix;
3) in above-mentioned solution, add the ammoniacal liquor 19 ~ 21 parts that concentration is 8mol/L again, adjust ph to 1 ~ 2, stir 0.5 ~ 1h;
4) polytetrafluoroethylene (PTFE) reactor is sealed, be placed in program baking oven, arrange intensification and rate of temperature fall be controlled as 1 DEG C/min, temperature 160 ~ 180 DEG C, hydrothermal treatment consists 24 ~ 48h, after having reacted, be cooled to room temperature, take out reactor, product is washed with distilled water to neutrality, be placed in temperature-40 DEG C of freeze drier freeze dryings again, obtain tantalum doping hydrous antimony pentoxide (HAP) material;
The number of each raw material is except specified otherwise above, is volume parts.
2., according to the preparation method of tantalum doping hydrous antimony pentoxide (HAP) sorbing material described in claim 1, it is characterized in that the method comprises the following steps:
1) getting concentration is 0.7 ~ 0.8mol/LSbCl 5hydrochloric acid solution 16 ~ 18 parts, is placed in polytetrafluoroethylene (PTFE) reactor, adds redistilled water 6 ~ 9 parts, is uniformly mixed;
2) in above-mentioned solution, adding concentration is 0.09 ~ 0.11mol/LTaCl 5ethanolic solution 9 ~ 12 parts, makes the mol ratio of Ta/Sb in solution be 0.09 ~ 0.12, stirs and makes it fully mix;
3) in above-mentioned solution, add the ammoniacal liquor 19 ~ 20 parts that concentration is 8mol/L again, adjust ph to 1 ~ 2, stir 0.5 ~ 1h;
4) polytetrafluoroethylene (PTFE) reactor is sealed, be placed in program baking oven, arrange intensification and rate of temperature fall be controlled as 1 DEG C/min, temperature 160 ~ 180 DEG C, hydrothermal treatment consists 24 ~ 48h, after having reacted, be cooled to room temperature, take out reactor, product is washed with distilled water to neutrality, be placed in temperature-40 DEG C of freeze drier freeze dryings again, obtain tantalum doping hydrous antimony pentoxide (HAP) material;
The number of each raw material is except specified otherwise above, is volume parts.
3. according to the tantalum doping hydrous antimony pentoxide (HAP) sorbing material that the preparation method of tantalum doping hydrous antimony pentoxide (HAP) sorbing material described in claim 1 prepares.
4. adulterate hydrous antimony pentoxide (HAP) sorbing material for improving Sr according to tantalum described in claim 3 2+adsorption capacity.
CN201410249872.1A 2014-06-06 2014-06-06 A kind of preparation method of tantalum doping hydrous antimony pentoxide (HAP) sorbing material Expired - Fee Related CN103977758B (en)

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