CN108654552A - A kind of preparation method and purposes of half-H 2 O calcium sulphate adsorbent - Google Patents
A kind of preparation method and purposes of half-H 2 O calcium sulphate adsorbent Download PDFInfo
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- CN108654552A CN108654552A CN201710192385.XA CN201710192385A CN108654552A CN 108654552 A CN108654552 A CN 108654552A CN 201710192385 A CN201710192385 A CN 201710192385A CN 108654552 A CN108654552 A CN 108654552A
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- desulfurated plaster
- calcium sulphate
- adsorbent
- method described
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
This application discloses a kind of preparation methods and purposes of half-H 2 O calcium sulphate adsorbent, wherein the method includes following step：Desulfurated plaster is dried, free water therein is removed；Sieving, removes large granular impurity therein；Desulfurated plaster after sieving is worn into fine powder；Finely disintegrated desulfurated plaster is added in acid, stirring, ultrasound, stands a period of time to carry out acidification regenerative response；It filters；Washing；It is dry.The purposes is absorption dyestuff, such as Congo red purposes.The preparation method of the application is extremely simple, and the half-H 2 O calcium sulphate adsorbent prepared has great suction-operated to Congo red, this is following to desulfurated plaster to study, potentially application and water technology provide certain foundation.
Description
Technical field
This application involves but be not limited to desulfurated plaster processing and water-treatment technology field, and in particular to but be not limited to a kind of half
The preparation method and purposes of H 2 O calcium sulphate adsorbent.
Background technology
Desulfurized gesso of flue gas is that the enterprises such as thermal power plant, oil plant are based on a kind of industrial by-product obtained from Wet Flue Gas Desulfurization Technique
Object, main object are mutually calcium sulphate dihydrate.Impurity, the complexity of crystal phase structure and particle size, microscopic appearance in desulfurated plaster
Scrambling limit its resource recycling.The domestic resource technology about desulfurated plaster mainly directly will at present
It, which is filled, is used for the improvement in salt-soda soil into salt-soda soil, prepares β-semi-hydrated gypsum as cement retarder and calcining and then be processed into
Plasterboard and building block etc., but since the yield of desulfurated plaster is huge, the desulfurated plaster of part still exists in the form of stockpiling and storing, and causes
The waste of land resource and the secondary pollution of environment.
Currently, relatively about report of the calcium sulphate-based material in terms of Dye Adsorption removing is with heavy metal removal
It is few.Song Gong forces seminar of Hubei University is prepared for calcium sulfate crystal whiskers using hydrothermal synthesis method and shows it using ardealite as raw material
It can be used for adsorbing methylene blue；M.A.Rauf et al. has studied under room temperature gypsum, and para-totuidine is blue in aqueous solution and methylene
Blue absorption removes, and the single layer maximal absorptive capacity of para-totuidine indigo plant reaches 28mg/g, to the single layer maximal absorptive capacity of methylene blue
Reach 36mg/g；C.C.Obunwo etc. equally has studied under the gypsum room temperature of different-grain diameter in aqueous solution to the absorption of active red
It removes.But up to the present, the calcium sulphate-based material reported is to the adsorbance of organic dyestuff but very little.
Invention content
It is the general introduction of the theme to being described in detail herein below.This general introduction is not to limit the protection model of claim
It encloses.
This application provides a kind of preparation method and purposes of half-H 2 O calcium sulphate adsorbent, the method passes through to desulfurization stone
Cream is handled, and the rodlike half-H 2 O calcium sulphate adsorbent for having superpower adsorption capacity to dyestuff is prepared.
Specifically, this application provides a kind of preparation method of half-H 2 O calcium sulphate adsorbent, the method includes following steps
Suddenly：
Desulfurated plaster is dried, free water therein is removed；
Sieving, removes large granular impurity therein；
Desulfurated plaster after sieving is worn into fine powder；
Finely disintegrated desulfurated plaster is added in acid, stirring, ultrasound, it is anti-to carry out acidification regeneration to stand a period of time
It answers；
It filters；
Washing；
It is dry.
It is described to dry desulfurated plaster as desulfurated plaster is dried 4- at 40-50 DEG C in presently filed embodiment
6h。
In presently filed embodiment, the drying after the washing is the dry 6-8h at 40-50 DEG C.
In presently filed embodiment, the sieving was 70-100 mesh sieve.
Optionally, the sieving was 80 mesh sieve.
In presently filed embodiment, the grain size of the fine powder is 40-80 μm.
Optionally, the grain size of the fine powder is 50 μm.
In presently filed embodiment, the time of ultrasound need not be limited, because of double of water sulphur of the length of ultrasonic time
The performance of sour calcium adsorbent has little effect, and in order to save time, can select the ultrasonic time of 5min.
In presently filed embodiment, the acid used in the acidification regenerative response is hydrochloric acid.
Optionally, the hydrochloric acid that the acid used in the acidification regenerative response is a concentration of 10mol/L.
In presently filed embodiment, the mass ratio of desulfurated plaster fine powder and hydrochloric acid is 8-10:100.
In presently filed embodiment, described standing a period of time is standing 15-30min.
In presently filed embodiment, the washing is the filter cake filtered at room temperature with eluent solvent.
Optionally, the solvent is ethyl alcohol.
It is thin rodlike according to half-H 2 O calcium sulphate adsorbent prepared by the above method, draw ratio is about 20-30.
Present invention also provides the use that a kind of half-H 2 O calcium sulphate adsorbent prepared according to the above method is used to adsorb dyestuff
On the way.
In presently filed embodiment, the purposes is that absorption is Congo red.
In presently filed embodiment, the purposes does not include absorption rhodamine B.
Industrial by-products desulfurated plaster directly can be prepared into rodlike half by the application in a kind of extremely simple effective method
H 2 O calcium sulphate, the rodlike half-H 2 O calcium sulphate have great suction-operated to Congo red, this is following to desulfurated plaster to study, dives
Application and water technology provide certain foundation.
Other features and advantage will illustrate in the following description, also, partly become from specification
It obtains it is clear that being understood by implementing the application.The purpose of the application and other advantages can be by specification, rights
Specifically noted structure is realized and is obtained in claim and attached drawing.
Description of the drawings
Attached drawing is used for providing further understanding technical scheme, and a part for constitution instruction, with this
The embodiment of application is used to explain the technical solution of the application together, does not constitute the limitation to technical scheme.
Fig. 1 is the XRD spectrum of desulfurated plaster raw material.
Fig. 2 is the SEM spectrum of desulfurated plaster raw material under different amplification.
Fig. 3 is the XRD spectrum of rodlike half-H 2 O calcium sulphate adsorbent prepared by the embodiment of the present application 1.
SEM figures of the Fig. 4 for the rodlike half-H 2 O calcium sulphate adsorbent of the preparation of the embodiment of the present application 1 and its absorption after Congo red
Spectrum, a) SEM spectrum of rodlike half-H 2 O calcium sulphate adsorbent, b) rodlike half-H 2 O calcium sulphate adsorbent adsorb it is Congo red after SEM figures
Spectrum.
Fig. 5 is that rodlike half-H 2 O calcium sulphate adsorbent prepared by the embodiment of the present application 1 adsorbs Congo red a) Langmuir, b)
Freundlich, c) D-R and d) Temkin thermodynamical models.
Specific implementation mode
To make the purpose, technical scheme and advantage of the application be more clearly understood, below in conjunction with attached drawing to the application
Embodiment be described in detail.It should be noted that in the absence of conflict, in the embodiment and embodiment in the application
Feature mutually can arbitrarily combine.
Used reagent in following embodiment is unless otherwise instructed common commercial product.
Embodiment 1：
A. the selection of raw material：Choose the trade waste desulfurated plaster raw material 1g in Zhongweiof Ningxia, northwest China power plant；
B. the drying of raw material：The desulfurated plaster raw material chosen is sent into drying box, the temperature for adjusting drying box is 40 DEG C,
Dry 4h, the free water in raw material is removed；
C. the screening of raw material：1g desulfurated plaster raw materials after drying are crossed 80 mesh to sieve, are removed big in raw material
Granule foreign；
D. the grinding of raw material：The desulfurization gypsum powder for removing large granular impurity is worn into uniform fine powder；
E. the acidification regeneration of raw material：Finely disintegrated desulfurated plaster is added to the 10mol/L's of pre-prepared 8ml
In hydrochloric acid, reaction 18min is stood after stirring, ultrasound；
F. it filters：The slurry after reacting will be stood and carry out rapid filtration under suction, obtain white filter cake；
G. it washs：The filter cake obtained after suction filtration is directly washed with absolute ethyl alcohol at room temperature；
H. it dries：The washed filter cake of ethyl alcohol is dried into 6h at 40 DEG C, obtains rodlike half-H 2 O calcium sulphate adsorbent.
Embodiment 2：
A. the selection of raw material：Choose the trade waste desulfurated plaster raw material 2g in Zhongweiof Ningxia, northwest China power plant；
B. the drying of raw material：The desulfurated plaster raw material chosen is sent into drying box, the temperature for adjusting drying box is 50 DEG C,
Dry 4h, the free water in raw material is removed；
C. the screening of raw material：2g desulfurated plaster raw materials after drying are crossed 80 mesh to sieve, are removed big in raw material
Granule foreign；
D. the grinding of raw material：The desulfurization gypsum powder for removing large granular impurity is worn into uniform fine powder；
E. the acidification regeneration of raw material：Finely disintegrated desulfurated plaster is added to the 10mol/L of pre-prepared 20ml
Hydrochloric acid in, stirring, ultrasound after stand reaction 20min；
F. it filters：The slurry after reacting will be stood and carry out rapid filtration under suction, obtain white filter cake；
G. it washs：The filter cake obtained after suction filtration is directly washed with absolute ethyl alcohol at room temperature；
H. it dries：The washed filter cake of ethyl alcohol is dried into 6h at 50 DEG C, obtains rodlike half-H 2 O calcium sulphate adsorbent.
Embodiment 3：
A. the selection of raw material：Choose the trade waste desulfurated plaster raw material 5g in Zhongweiof Ningxia, northwest China power plant；
B. the drying of raw material：The desulfurated plaster raw material chosen is sent into drying box, the temperature for adjusting drying box is 50 DEG C,
Dry 4h, the free water in raw material is removed；
C. the screening of raw material：5g desulfurated plaster raw materials after drying are crossed 80 mesh to sieve, are removed big in raw material
Granule foreign；
D. the grinding of raw material：The desulfurization gypsum powder for removing large granular impurity is worn into uniform fine powder；
E. the acidification regeneration of raw material：Finely disintegrated desulfurated plaster is added to the 10mol/L of pre-prepared 50ml
Hydrochloric acid in, stirring, ultrasound after stand reaction 30min；
F. it filters：The slurry after reacting will be stood and carry out rapid filtration under suction, obtain white filter cake；
G. it washs：The filter cake obtained after suction filtration is directly washed with absolute ethyl alcohol at room temperature；
H. it dries：The washed filter cake of ethyl alcohol is dried into 8h at 50 DEG C, obtains rodlike half-H 2 O calcium sulphate adsorbent.
Test case
Fig. 1 is the XRD spectrum of desulfurated plaster raw material.Fig. 3 is rodlike half-H 2 O calcium sulphate absorption prepared by the embodiment of the present application 1
The XRD spectrum of agent.Obtain Fig. 1, the test equipment used in 3 is SHIMADZU XRD-7000 type X-ray diffraction analysis instrument, use
Cu target K alpha rays source, tube voltage 40kV, tube current 30mA, sweep speed are 2 °/min.
The variation of comparison diagram 1 and Fig. 3, XRD characteristic peak positions illustrate that desulfurated plaster is converted through method described herein
Object mutually becomes half-H 2 O calcium sulphate from calcium sulphate dihydrate afterwards.
Fig. 2 is the SEM spectrum of desulfurated plaster raw material under different amplification.Fig. 4 is the rodlike of the preparation of the embodiment of the present application 1
SEM spectrum after half-H 2 O calcium sulphate adsorbent and its absorption are Congo red, a) SEM spectrum of rodlike half-H 2 O calcium sulphate adsorbent, b)
Rodlike half-H 2 O calcium sulphate adsorbent adsorb it is Congo red after SEM spectrum.Obtain Fig. 2, the test equipment used in 4 is S-4800 and sends out
Penetrate scanning electron microscope (FESEM), accelerating potential 15kV.
Comparison diagram 2 and Fig. 4 a, it can be seen that desulfurated plaster after method described herein conversion microscopic appearance by big
It is granular be changed into it is thin rodlike；Comparison diagram 4a and Fig. 4 b, it can be seen that microscopic appearance turns after rodlike half-H 2 O calcium sulphate absorption is Congo red
Become cotton-shaped.
Fig. 5 is that rodlike half-H 2 O calcium sulphate adsorbent prepared by the embodiment of the present application 1 adsorbs Congo red a) Langmuir, b)
Freundlich, c) D-R and d) Temkin thermodynamical models.It is UV-vis spectroscopy to obtain the test equipment used in attached drawing 5
Photometer.The rodlike half-H 2 O calcium sulphate of Fig. 5 adsorbs Congo red dynamic analysis, shows rodlike half-H 2 O calcium sulphate to Congo red
Adsorption Model meets Langmuir models, by Langmuir model expressions：
It is 1344.44mg/g to Congo red maximal absorptive capacity that rodlike half-H 2 O calcium sulphate, which is calculated,.
Although the embodiment disclosed by the application is as above, the content only for ease of understanding the application and use
Embodiment is not limited to the application.Technical staff in any the application fields, is taken off not departing from the application
Under the premise of the spirit and scope of dew, any modification and variation, but the application can be carried out in the form and details of implementation
Scope of patent protection, still should be subject to the scope of the claims as defined in the appended claims.
Claims (10)
1. a kind of preparation method of half-H 2 O calcium sulphate adsorbent, the method includes following step：
Desulfurated plaster is dried, free water therein is removed；
Sieving, removes large granular impurity therein；
Desulfurated plaster after sieving is worn into fine powder；
Finely disintegrated desulfurated plaster is added in acid, stirring, ultrasound, stands a period of time to carry out acidification regenerative response；
It filters；
Washing；
It is dry.
2. according to the method described in claim 1, wherein, it is described by desulfurated plaster drying for by desulfurated plaster at 40-50 DEG C
Dry 4-6h；Drying after the washing is the dry 6-8h at 40-50 DEG C.
3. according to the method described in claim 1, wherein, the sieving was 70-100 mesh sieve, optionally, to cross 80 mesh sieve.
4. according to the method described in claim 1, wherein, the grain size of the fine powder is 40-80 μm, is 50 μm optionally.
5. according to the method described in claim 1, wherein, the acid used in the acidification regenerative response is hydrochloric acid, is dense optionally
Degree is the hydrochloric acid of 10mol/L.
6. according to the method described in claim 5, wherein, the mass ratio of desulfurated plaster fine powder and hydrochloric acid is 8-10:100.
7. according to the method described in claim 1, wherein, described standing a period of time is standing 15-30min.
8. according to the method described in claim 1, wherein, the washing is the filter filtered at room temperature with eluent solvent
Cake, optionally, the solvent are ethyl alcohol.
9. half-H 2 O calcium sulphate adsorbent prepared by the method according to any one of claim 1-8 is used to adsorb the use of dyestuff
On the way；Optionally, the purposes is that absorption is Congo red.
10. purposes according to claim 9 does not include absorption rhodamine B.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710192385.XA CN108654552A (en) | 2017-03-28 | 2017-03-28 | A kind of preparation method and purposes of half-H 2 O calcium sulphate adsorbent |
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| CN201710192385.XA CN108654552A (en) | 2017-03-28 | 2017-03-28 | A kind of preparation method and purposes of half-H 2 O calcium sulphate adsorbent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607827A (en) * | 2019-07-16 | 2020-09-01 | 北新集团建材股份有限公司 | Post-treatment method of calcium sulfate whisker |
| CN112760716A (en) * | 2021-01-15 | 2021-05-07 | 海南蓝岛环保产业股份有限公司 | Phosphorus-containing desulfurized gypsum recycling treatment method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352535A (en) * | 2011-09-22 | 2012-02-15 | 东莞上海大学纳米技术研究院 | Method for preparing calcium sulfate crystal whiskers from desulfurized gypsum under normal pressure |
| CN102995102A (en) * | 2012-11-23 | 2013-03-27 | 西安建筑科技大学 | Method for recycling floating beads and preparing different morphologies of calcium sulfate hemihydrate mono-crystals by using desulfurized gypsum |
-
2017
- 2017-03-28 CN CN201710192385.XA patent/CN108654552A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352535A (en) * | 2011-09-22 | 2012-02-15 | 东莞上海大学纳米技术研究院 | Method for preparing calcium sulfate crystal whiskers from desulfurized gypsum under normal pressure |
| CN102995102A (en) * | 2012-11-23 | 2013-03-27 | 西安建筑科技大学 | Method for recycling floating beads and preparing different morphologies of calcium sulfate hemihydrate mono-crystals by using desulfurized gypsum |
Non-Patent Citations (2)
| Title |
|---|
| XIN-JIAN JIA ETAL.: "Bouquet-like calcium sulfate dihydrate: a highly efficient adsorbent for Congo red dye", 《RSC ADVANCES》 * |
| 吕智慧等: "一步常压酸化法制备无水硫酸钙晶须", 《无机盐工业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607827A (en) * | 2019-07-16 | 2020-09-01 | 北新集团建材股份有限公司 | Post-treatment method of calcium sulfate whisker |
| CN111607827B (en) * | 2019-07-16 | 2022-01-07 | 北新集团建材股份有限公司 | Post-treatment method of calcium sulfate whisker |
| CN112760716A (en) * | 2021-01-15 | 2021-05-07 | 海南蓝岛环保产业股份有限公司 | Phosphorus-containing desulfurized gypsum recycling treatment method |
| CN112760716B (en) * | 2021-01-15 | 2024-05-24 | 海南蓝岛环保产业股份有限公司 | Recycling treatment method of phosphogypsum |
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