CN102701620A - Method utilizing microwave technique to induce modified ardealite - Google Patents
Method utilizing microwave technique to induce modified ardealite Download PDFInfo
- Publication number
- CN102701620A CN102701620A CN2012102151331A CN201210215133A CN102701620A CN 102701620 A CN102701620 A CN 102701620A CN 2012102151331 A CN2012102151331 A CN 2012102151331A CN 201210215133 A CN201210215133 A CN 201210215133A CN 102701620 A CN102701620 A CN 102701620A
- Authority
- CN
- China
- Prior art keywords
- microwave
- phosphogypsum
- ardealite
- modified ardealite
- dielectric material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000003989 dielectric material Substances 0.000 claims abstract description 11
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 51
- 238000005516 engineering process Methods 0.000 claims description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims description 8
- 150000004706 metal oxides Chemical class 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 5
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000000498 ball milling Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 8
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002686 phosphate fertilizer Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011507 gypsum plaster Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a method utilizing a microwave technique to induce modified ardealite. The method comprises the following steps of: ball-milling the ardealite to 160-200meshes; according to the mass ratio of the ardealite and an amorphous dielectric material being 1-2: 0.05-0.1, adding the amorphous dielectric material to be mixed; putting the mixture under the conditions of 2350MHz of microwave frequencies, 750-950W of power and 100-150 DEG C of temperature to carry out microwave processing for 10-15 minutes, and then naturally cooling to the room temperature; and finally obtaining microwave induced modified ardealite. According to the method, the surface free energy, the electric potential, the average pore size and the specific surface area of the ardealite can be significantly increased. The prepared microwave induced modified ardealite can be used for adsorption of heavy metal wastewater. The method has the advantages of simple operation, low cost and high efficiency, a lot of energy sources are saved, and the secondary pollution is avoided.
Description
Technical field
The present invention relates to phosphogypsum modification and utilize technical field, specifically a kind of method of utilizing microwave technology to induce modified ardealite.
Background technology
Phosphogypsum is the solid waste that produces in the Wet-process phosphoric acid (WPPA) technological process, and its staple is CaSO
42H
2O also contains section H simultaneously
3PO
4, Ca (H
2PO
4)
2H
2O, CaHPO
42H
2O, Ca
3(PO
4)
2And sulfide (NaF, Na
2SiF
6, Na
3AlF
6, Na
3FeF
6, CaF
2).China's phosphogypsum comprehensive utilization ratio is merely 15% at present.The whole nation has been piled up more than 100,000,000 ton, and annual also with 2,000 ten thousand tons speed increase, only more than 4,000 ten thousand tons of phosphogypsums have just been piled up in Yunnan Province.In May, 2006, State Environmental Protection Administration was with the form of ring letter (2006) No. 176 literary compositions, with phosphogypsum qualitative be dangerous solid waste, classify the controlling object of national noxious waste pollution environment as.The recycling of phosphogypsum has become the key that the phosphate fertilizer industry realizes Sustainable development.Therefore, how to fully utilize pollution, the treatment of wastes with processes of wastes against one another that phosphogypsum, control phosphogypsum produce, improve the utility value of phosphogypsum, create good social benefit and environmental benefit and just seem and be even more important.
The research of the microwave induced processing phosphogypsum of employing both at home and abroad mainly concentrates on and adopts microwave technology that phosphogypsum is carried out purifying treatment.The method that the microwave treatment preparation is used for the modified activated carbon of hydrogen iodide catalytically decomposed, publication number is disclosed in being the application of CN101811016A.The method comprising the steps of: gac is placed microwave oven, under the protection of protection gas, carry out microwave treatment 5～30min with the power of 100～800W, the frequency of 2450MHz, promptly get modified activated carbon.The preparation method of the active sludge carbon that utilizes flue gas desulfurization is disclosed in patent CN200610130548.3.This method comprises the pre-treatment of (1) mud, (2) microwave treatment thousand mud, and (3) charing, (4) are physically activated, the step of (5) microwave modification.Prepare in gac and the municipal sludge research direction at microwave modification, microwave technology is applied to during recycling of solid wastes utilizes as a kind of comparatively sophisticated means, but as the less research of the means of modified ardealite.Both at home and abroad methods such as ball milled, sudden strain of a muscle burning method, lime neutralisation that adopt are carried out modification to phosphogypsum more; Obviously these methods can be removed the impurity in the phosphogypsum to a great extent, but do not have contribution for improving the distribution of phosphogypsum surface charge, surface energy, increase specific surface area.
Do not see breakthrough research at home and abroad as yet to utilizing the microwave technology modified ardealite.Be necessary to study and use microwave technology that phosphogypsum is induced processing, change its surface charge and distribute, improve surface energy, increase specific surface area.If can have on the basis of certain loading capacity at phosphogypsum; Adopt microwave means; The inner vesicular structure of phosphogypsum is transformed into open hole; Make the phosphogypsum particle surface be polynuclear plane, increase its specific surface area and then can improve the practicality of phosphogypsum in handling heavy metal wastewater thereby greatly, widen its recycling approach.
Summary of the invention
For improving the distribution of phosphogypsum surface charge, surface energy, increase specific surface area; The present invention provides a kind of method of utilizing microwave technology to induce modified ardealite; Phosphogypsum specific surface area behind microwave modification is big, loading capacity is high, and the surface free energy of phosphogypsum and current potential also are improved and change.
The present invention realizes through following technical proposal: a kind of method of utilizing microwave technology to induce modified ardealite, and following each step of process:
Phosphogypsum ball is milled to 160～200 orders; Mass ratio by phosphogypsum and amorphous dielectric material is 1～2 ︰ 0.05～0.1 again; After adding amorphous dielectric material mixing; Placing microwave frequency is that 2350MHZ, power are that 750～950w, temperature are to carry out microwave treatment 10～15 minutes under 100～150 ℃ the condition, naturally cools to room temperature then, promptly obtains microwave induced modified ardealite.
Said phosphogypsum is that the plaster of paris, desulfurated plaster, phosphate fertilizer plant are residue phosphogypsums.
Said amorphous dielectric material is an inorganic, metal oxide, like Fe
2O
3, Al
2O
3Deng.
Principle of the present invention is according in weak absorption material by microwave application, adding strong absorption material by microwave application, heating rapidly thereby absorb material by microwave application a little less than making.Its essence is: (one) utilizes the strong material absorbing microwave that absorbs microwave to heat up rapidly, through contact transferred heat and microwave energy input dual mode the weak material temperature that absorbs microwave is raise rapidly; (2) in the microwave heating process because the variation of dielectric loss factor and particulate electric conductivity has changed the rate of heating of weak absorption material by microwave application.
Amorphous dielectric material is as the strong material that absorbs microwave among the present invention; When himself heating up rapidly; Because the variation of its dielectric loss factor and particulate electric conductivity discharges heat; Thereby strengthened this weak rate of heating of inhaling the ripple material of phosphogypsum, made the rate of heating of phosphogypsum than the fast several times of existing conventional rate of heating, and therefore make phosphogypsum change below producing:
(1) free state moisture in the phosphogypsum and organism evaporate fully or decompose;
(2) the linearity increase of heat will cause the migrations such as room, distortion, peritectoid, cleavage, crackle and impurity of the more weak water layer room of bonding force on the phosphogypsum crystal;
(3) room is moved to and is disappeared behind the surface of phosphogypsum thereupon and form the dew point and then form crackle; Efflorescence is stablized nucleus then and is formed, and the growth diffusion; Make the surface free energy and the current potential of phosphogypsum improve, the specific surface area of phosphogypsum and mean pore size increase.
Because the heating of ardealite comes down to the heating to pure gypsum and its impurity; Because the characteristic of microwave; Its heating characteristics are classification heating; Whole heating; So the heating ardealite can be regarded as and heat pure gypsum and ardealite impurity respectively, the efficiency of heating surface is higher than traditional mode of heating, can save the energy in a large number; And what adopt is electric energy, has avoided secondary pollution.
The present invention adopts microwave technology to induce modified ardealite, has overcome the shortcoming of other physics of independent employing or chemical process modified ardealite, and other technologies exist secondary pollution, calcination processing modified ardealite speed slow; The amorphous dielectric material of inorganics class is as the adding of modifying agent, increased substantially the speed that microwave technology is induced modified ardealite, significantly improved the physico-chemical property of phosphogypsum.
The present invention adopts microwave technology that phosphogypsum is carried out radiation modification, under radiation environment, makes specific inductivity, apparent activation energy and the microvoid structure of phosphogypsum, thereby improves the porosity and the specific surface area of phosphogypsum.The specific surface area and the mean pore size of the phosphogypsum before and after the modification see the following form 1.
The specific surface area and the mean pore size of the phosphogypsum before and after table 1 modification
Compared with prior art, the invention has the advantages that:
(1) the present invention carries out microwave induced processing to phosphogypsum, and directly with the amorphous dielectric material of inorganics class as modifying agent, can significantly improve phosphogypsum surface free energy, current potential, mean pore size and specific surface area;
(2) the microwave induced modified ardealite that makes of the present invention can be used for heavy metal wastewater thereby absorption aspect;
(3) the present invention is simple to operate, with low cost, efficient is high, save the energy in a large number, avoided secondary pollution; When widening solid waste and utilizing approach, realize the treatment of wastes with processes of wastes against one another, create good economic benefit and environment social benefit.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1
The 100g phosphogypsum ball is milled to 160 orders, and the mass ratio by phosphogypsum and inorganic, metal oxide is 1 ︰ 0.1 again, adds 10g inorganic, metal oxide Fe
2After O mixed, placing microwave frequency was that 2350MHZ, power are that 750w, temperature are to carry out microwave treatment 10 minutes under 100 ℃ the condition, naturally cools to room temperature then, promptly obtains microwave induced modified ardealite.
Embodiment 2
The 100g phosphogypsum ball is milled to 180 orders, and the mass ratio by phosphogypsum and inorganic, metal oxide is 1 ︰ 0.05 again, adds 5g inorganic, metal oxide Al
2O
3After the mixing, placing microwave frequency is that 2350MHZ, power are that 850w, temperature are to carry out microwave treatment 12 minutes under 120 ℃ the condition, naturally cools to room temperature then, promptly obtains microwave induced modified ardealite.
Embodiment 3
The 100g phosphogypsum ball is milled to 200 orders, and the mass ratio by phosphogypsum and inorganic, metal oxide is 2 ︰ 0.05 again, adds 2.5g inorganic, metal oxide Al
2O
3After the mixing, placing microwave frequency is that 2350MHZ, power are that 950w, temperature are to carry out microwave treatment 15 minutes under 150 ℃ the condition, naturally cools to room temperature then, promptly obtains microwave induced modified ardealite.
The present invention takes off absorption representation analysis and contrast to utilizing microwave technology to induce the prepared modified ardealite of embodiment of modified ardealite to carry out BET nitrogen, and the result sees table 2:
Table 2 embodiment test result
Can find out from table 2; At high-temperature, under high-power early stage; Suitably prolong the microwave induced time and adopt the little phosphogypsum of particle diameter, the specific surface area of the phosphogypsum after microwave induced has obtained raising significantly with mean pore size, and this technology has improved surface free energy, current potential, mean pore size and the specific surface area of phosphogypsum significantly; Avoid adding MOX too muchly, reduced cost.
What more than enumerate only is specific embodiment of the present invention.Obviously the invention is not restricted to above embodiment, many distortion can also be arranged.In all distortion that the those of ordinary skill of microwave technical field can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (2)
1. method of utilizing microwave technology to induce modified ardealite is characterized in that through following each step:
Phosphogypsum ball is milled to 160～200 orders; Mass ratio by phosphogypsum and amorphous dielectric material is 1～2 ︰ 0.05～0.1 again; After adding amorphous dielectric material mixing; Placing microwave frequency is that 2350MHZ, power are that 750～950w, temperature are to carry out microwave treatment 10～15 minutes under 100～150 ℃ the condition, naturally cools to room temperature then, promptly obtains microwave induced modified ardealite.
2. the method for utilizing microwave technology to induce modified ardealite according to claim 1 is characterized in that: said amorphous dielectric material is an inorganic, metal oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210215133.1A CN102701620B (en) | 2012-06-27 | 2012-06-27 | Method utilizing microwave technique to induce modified ardealite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210215133.1A CN102701620B (en) | 2012-06-27 | 2012-06-27 | Method utilizing microwave technique to induce modified ardealite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102701620A true CN102701620A (en) | 2012-10-03 |
| CN102701620B CN102701620B (en) | 2014-09-03 |
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ID=46894751
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|---|---|---|---|
| CN201210215133.1A Expired - Fee Related CN102701620B (en) | 2012-06-27 | 2012-06-27 | Method utilizing microwave technique to induce modified ardealite |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105197977A (en) * | 2015-09-09 | 2015-12-30 | 昆明理工大学 | Preparation method for developing beta type phosphor building gypsum by utilizing microwaves |
| CN106477529A (en) * | 2016-11-02 | 2017-03-08 | 昆明冶金研究院 | A kind of method of microwave method reducing and decomposing phosphogypsum |
| CN108147762A (en) * | 2017-12-28 | 2018-06-12 | 四川绵竹三佳饲料有限责任公司 | A kind of modified ardealite imitates wood plank and preparation method thereof |
| CN108314341A (en) * | 2018-03-12 | 2018-07-24 | 湘潭大学 | The manufacturing technique method of one kind of multiple strength character gypsum powder bodies |
| CN110038890A (en) * | 2019-05-15 | 2019-07-23 | 山东虎力机械有限公司 | A kind of ecological, environmental protective soil remediation method |
| CN113860773A (en) * | 2021-11-04 | 2021-12-31 | 云南云天化环保科技有限公司 | Microwave-enhanced fluidized phosphogypsum dehydration device and method |
-
2012
- 2012-06-27 CN CN201210215133.1A patent/CN102701620B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 唐霜露: "磷石膏介电性及其微波分解模拟仿真研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105197977A (en) * | 2015-09-09 | 2015-12-30 | 昆明理工大学 | Preparation method for developing beta type phosphor building gypsum by utilizing microwaves |
| CN106477529A (en) * | 2016-11-02 | 2017-03-08 | 昆明冶金研究院 | A kind of method of microwave method reducing and decomposing phosphogypsum |
| CN106477529B (en) * | 2016-11-02 | 2018-07-20 | 昆明冶金研究院 | A kind of method of microwave method reducing and decomposing phosphogypsum |
| CN108147762A (en) * | 2017-12-28 | 2018-06-12 | 四川绵竹三佳饲料有限责任公司 | A kind of modified ardealite imitates wood plank and preparation method thereof |
| CN108314341A (en) * | 2018-03-12 | 2018-07-24 | 湘潭大学 | The manufacturing technique method of one kind of multiple strength character gypsum powder bodies |
| CN108314341B (en) * | 2018-03-12 | 2021-01-12 | 湘潭大学 | Production process method of gypsum powder with various strength properties |
| CN110038890A (en) * | 2019-05-15 | 2019-07-23 | 山东虎力机械有限公司 | A kind of ecological, environmental protective soil remediation method |
| CN110038890B (en) * | 2019-05-15 | 2019-11-26 | 湖北同惠生物工程有限公司 | A kind of ecological, environmental protective soil remediation method |
| CN113860773A (en) * | 2021-11-04 | 2021-12-31 | 云南云天化环保科技有限公司 | Microwave-enhanced fluidized phosphogypsum dehydration device and method |
| CN113860773B (en) * | 2021-11-04 | 2022-06-14 | 云南云天化环保科技有限公司 | Device and method for dehydrating microwave-enhanced fluidized phosphogypsum |
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| Publication number | Publication date |
|---|---|
| CN102701620B (en) | 2014-09-03 |
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