CN101876087A - Method for preparing calcium sulphate whiskers used for absorbing heavy metal ions in waste incineration flue gas - Google Patents
Method for preparing calcium sulphate whiskers used for absorbing heavy metal ions in waste incineration flue gas Download PDFInfo
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- CN101876087A CN101876087A CN 201010141450 CN201010141450A CN101876087A CN 101876087 A CN101876087 A CN 101876087A CN 201010141450 CN201010141450 CN 201010141450 CN 201010141450 A CN201010141450 A CN 201010141450A CN 101876087 A CN101876087 A CN 101876087A
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Abstract
The invention discloses a method for preparing calcium sulphate whiskers used for absorbing heavy metal ions in a waste incineration flue gas. The method comprises the following steps of: selecting a gypsum raw material; mixing the gypsum raw material and water to prepare slurry with the weight percentage concentration of 2 percent to 6 percent; putting the slurry into a microwave reactor; stirring and heating the slurry at the temperature of between 120 and 130 DEG C for 1 to 2 hours to prepare a crude product of the calcium sulphate whiskers; soaking the crude product of the calcium sulphate whiskers in alkaline solution for a certain time; and after taking out and drying naturally, activating the calcium sulphate whiskers at a high temperature in a muffle furnace to prepare a finished product of the calcium sulphate whiskers used for absorbing the heavy metal ions in the waste incineration flue gas. The finished product of the calcium sulphate whiskers prepared by using method has the characteristics of larger specific surface area, developed pore structure, capability of effectively adsorbing the heavy metal ions in the waste incineration flue gas, and equivalent adsorption effect to that of activate carbon.
Description
Technical field
The present invention relates to a kind of Preparation methods of gypsum whiskers method, be specifically related to a kind of calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion.
Background technology
Heavy metal is a kind of principal pollutant in the flue gas of refuse burning, and the heavy metal ion that adopts absorption method to catch in the flue gas of refuse burning has become one of main method of control heavy metal contamination at present.Traditional sorbent material is a gac, and gac has very strong adsorptive power, the heavy metal removing rate height, but owing to cost an arm and a leg, application is very limited.In recent years, develop a series of charcoal non activated solid adsorbent, mainly contained clay class sorbent material, humic acids sorbent material, waste sorbent material etc.Clay class absorbent component mainly contains the oxide compound of metal ions such as Si, Al, Ca, Mg, if you would take off stone, kaolin, attapulgite etc.; The humic acids sorbent material mainly is to utilize the absorption of the abundant surperficial organo-functional group realization of humic acid to heavy metal ion, and the general weathered coal, brown coal or the coal slime that are rich in humic acid of adopting made sorbing material; The complicated mechanism of waste adsorbents adsorb heavy metal ion, waste sorbent material commonly used at present mainly contains flyash, slag, alkaline residue etc.Above-mentioned charcoal non activated sorbent material is not all realized industrial applications at present owing to have preparation and problem such as modified technique complexity, production cost height, adsorption efficiency be undesirable.
Summary of the invention
Deficiency at above-mentioned sorbent material exists the present invention proposes a kind of calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion.Its technical solution is:
A kind of calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion may further comprise the steps:
(1) choose the gypsum raw material that mean particle size is 30～60 μ m, it is 2%～6% slip that itself and water are mixed with weight percent concentration;
(2) slip for preparing in the step (1) is put into microwave reactor, add the whisker morphology conditioning agent, pH with slip is adjusted into 8～10 then, be under 120～130 ℃ the condition in normal pressure, temperature, stirring heating 1～2h, the control stir speed (S.S.) is 200～500rpm, and reaction finishes after-filtration, obtains calcium sulfate crystal whiskers crude product (unmodified calcium sulfate crystal whiskers);
(3) the calcium sulfate crystal whiskers crude product of producing in the step (2) is soaked for some time in basic solution, after taking out seasoning, put into retort furnace, under the condition of starvation, be warming up to 600～900 ℃ of postactivated 2～4h, promptly make the calcium sulfate crystal whiskers finished product (wastewaters with modified calcium sulfate whiskers) that is used for adsorbing the flue gas of refuse burning heavy metal ion.
In the above-mentioned steps (1), described gypsum raw material is the plaster of paris or industrially desulfurized gypsum.
In the above-mentioned steps (2), described whisker morphology conditioning agent is magnesium chloride or vitriolate of tartar; The add-on of whisker morphology conditioning agent is the whisker morphology conditioning agent that adds 0.02～0.05mol in the 1L slip.
In the above-mentioned steps (3), described basic solution is sodium hydroxide or potassium hydroxide; The ratio that is soaked in sodium hydroxide that 5～10ml concentration is 0.1～0.3mol/L or potassium hydroxide solution in 1g calcium sulfate crystal whiskers crude product is soaked, and soak time is 24～72h.
The present invention can have following useful technique effect:
1, the calcium sulfate crystal whiskers of the present invention preparation has bigger specific surface area, flourishing pore texture, the heavy metal ion in can the active adsorption flue gas of refuse burning, and adsorption effect and gac are suitable; Utilize calcium sulfate crystal whiskers (unmodified calcium sulfate crystal whiskers) specific surface area of microwave reactor preparation to be about 4.38m after testing
2/ g, the specific surface area of calcium sulfate crystal whiskers (wastewaters with modified calcium sulfate whiskers) is 4.89～5.13m after the high-temperature activation modification is handled
2/ g; In addition, the present invention have that production cost is low, preparation cycle short, easy to operate, characteristics such as can produce in batches.
2, the present invention uses earlier microwave heating in the process of producing calcium sulfate crystal whiskers, this method have rate of heating fast, energy-conservation, be easy to control and characteristics such as selectivity heating, and preparing differently with high pressure of the prior art, microwave heating just can be reacted under normal pressure; The calcium sulfate crystal whiskers that utilizes microwave method to prepare can significantly improve the speed of crystallization reaction, shortens the reflection cycle.The calcium sulfate crystal whiskers crude product that the present invention also makes microwave heating carries out modification to be handled, and promptly earlier the calcium sulfate crystal whiskers crude product is immersed in the basic solution, carries out high-temperature activation then; Can improve the calcium sulfate crystal whiskers surface pH value after utilizing basic solution fully to soak, and along with the rising of calcium sulfate crystal whiskers surface p H value, calcium sulfate crystal whiskers will strengthen to the adsorption of heavy metal ion; High-temperature activation can enlarge the interior hole dimension of whisker, makes Na simultaneously
+Or K
+With the Ca in the whisker
2+Ion forms eutectic under high temperature action, for the absorption of heavy metal ion provides active sites.
Description of drawings
Fig. 1 is the SEM photo of calcium sulfate crystal whiskers crude product.
Fig. 2 is the SEM photo of calcium sulfate crystal whiskers finished product.
Embodiment
Embodiment 1
Taking by weighing the 30g mean particle size is the industrially desulfurized gypsum of 50 μ m, it is joined in the 1L water fully form slip after the dissolving, and slip is joined in the microwave reactor, adds 0.02molMgCl then
2As the whisker morphology conditioning agent, dropping sodium solution is adjusted into 8 with the pH value of slip; Start whipping appts, the control stir speed (S.S.) is 200rpm, under non-pressurized condition the temperature in the microwave reactor is risen to 130 ℃, and under this temperature sustained reaction 1h, postcooling, filtration are finished in reaction, obtain calcium sulfate crystal whiskers crude product (unmodified calcium sulfate crystal whiskers).Then the calcium sulfate crystal whiskers crude product that makes is immersed in 24h in the NaOH solution that 250ml concentration is 0.1mol/L, after finishing, immersion takes out seasoning, put into retort furnace then, under the condition of starvation, retort furnace is warming up to 700 ℃, and under this temperature, activate 2h, and promptly make the calcium sulfate crystal whiskers finished product (wastewaters with modified calcium sulfate whiskers) that the present invention is used for adsorbing the flue gas of refuse burning heavy metal ion, pack stand-by after the cooling.
Carry out heavy metal ion adsorbed field experiment in the flue gas at certain municipal solid waste incinerator, adsorption temp is 500 ℃, the residence time of flue gas in sorbent material is 5s, and the calcium sulfate crystal whiskers of selecting method for preparing for use is as flue gas adsorbent, and the consumption of sorbent material is for handling 1Nm
3Waste gas needs the 0.1kg sorbent material, concrete experimental result such as following table:
| Heavy metal in the flue gas | Mercury | Cadmium | Plumbous |
| Concentration c 1 (mg/Nm before the absorption 3) | ??0.073 | ??1.65 | ??86.7 |
| Unmodified calcium sulfate crystal whiskers absorption back concentration c 2 (mg/Nm 3) | ??0.017 | ??0.29 | ??16.3 |
| Heavy metal in the flue gas | Mercury | Cadmium | Plumbous |
| Unmodified calcium sulfate crystal whiskers adsorption rate | ??76.7％ | ??82.4％ | ??81.2％ |
| Wastewaters with modified calcium sulfate whiskers absorption back concentration c 3 (mg/Nm 3) | ??0.011 | ??0.09 | ??5.3 |
| The wastewaters with modified calcium sulfate whiskers adsorption rate | ??84.9％ | ??94.5％ | ??93.9％ |
Embodiment 2
Taking by weighing the 40g mean particle size is the industrially desulfurized gypsum of 40 μ m, it is joined in the 1L water fully form slip after the dissolving, and slip is joined in the microwave reactor, adds 0.03molK then
2SO
4As the whisker morphology conditioning agent, dropping sodium solution is adjusted into 9 with the pH value of slip; Start whipping appts, the control stir speed (S.S.) is 300rpm, under non-pressurized condition the temperature in the microwave reactor is risen to 130 ℃, and under this temperature sustained reaction 1.5h, the reaction finish postcooling, filtration, obtain the calcium sulfate crystal whiskers crude product.Then the calcium sulfate crystal whiskers crude product that makes is immersed in 48h in the NaOH solution that 200ml concentration is 0.2mol/L, after finishing, immersion takes out seasoning, put into retort furnace then, under the condition of starvation, retort furnace is warming up to 800 ℃, and under this temperature, activate 3h, and promptly make the calcium sulfate crystal whiskers finished product that the present invention is used for adsorbing the flue gas of refuse burning heavy metal ion, pack stand-by after the cooling.
Carry out heavy metal ion adsorbed field experiment in the flue gas at certain municipal solid waste incinerator, adsorption temp is 450 ℃, the residence time of flue gas in sorbent material is 8s, and the calcium sulfate crystal whiskers finished product of selecting method for preparing for use is as flue gas adsorbent, and the consumption of sorbent material is for handling 1Nm
3Waste gas needs the 0.1kg sorbent material, concrete experimental result such as following table:
| Heavy metal in the flue gas | Mercury | Cadmium | Plumbous |
| Concentration c 1 (mg/Nm before the absorption 3) | ??0.085 | ??2.13 | ??71.4 |
| Unmodified calcium sulfate crystal whiskers absorption back concentration c 2 (mg/Nm 3) | ??0.021 | ??0.47 | ??10.9 |
| Unmodified calcium sulfate crystal whiskers adsorption rate | ??75.3％ | ??77.9％ | ??84.7％ |
| Wastewaters with modified calcium sulfate whiskers absorption back concentration c 3 (mg/Nm 3) | ??0.009 | ??0.11 | ??1.6 |
| The wastewaters with modified calcium sulfate whiskers adsorption rate | ??89.4％ | ??94.8％ | ??97.8％ |
Embodiment 3
Taking by weighing the 60g mean particle size is the industrially desulfurized gypsum of 30 μ m, it is joined in the 1L water fully form slip after the dissolving, and slip is joined in the microwave reactor, adds an amount of 0.05molK then
2SO
4As the whisker morphology conditioning agent, dropping sodium solution is adjusted into 10 with the pH value of slip; Start whipping appts, the control stir speed (S.S.) is 400rpm, under non-pressurized condition the temperature in the microwave reactor is risen to 130 ℃, and under this temperature sustained reaction 2h, the reaction finish postcooling, filtration, obtain the calcium sulfate crystal whiskers crude product.Then the calcium sulfate crystal whiskers crude product that makes is immersed in 72h in the NaOH solution that 200ml concentration is 0.3mol/L, after finishing, immersion takes out seasoning, put into retort furnace then, under the condition of starvation, retort furnace is warming up to 900 ℃, and under this temperature, activate 4h, and promptly make the calcium sulfate crystal whiskers finished product that the present invention is used for adsorbing the flue gas of refuse burning heavy metal ion, pack stand-by after the cooling.
Carry out heavy metal ion adsorbed field experiment in the flue gas at certain municipal solid waste incinerator, adsorption temp is 400 ℃, the residence time of flue gas in sorbent material is 10s, and the calcium sulfate crystal whiskers finished product of selecting method for preparing for use is as flue gas adsorbent, and the consumption of sorbent material is for handling 1Nm
3Waste gas needs the 0.1kg sorbent material, concrete experimental result such as following table:
| Heavy metal in the flue gas | Mercury | Cadmium | Plumbous |
| Concentration c 1 (mg/Nm before the absorption 3) | ??0.089 | ??1.97 | ??81.3 |
| Unmodified calcium sulfate crystal whiskers absorption back concentration c 2 (mg/Nm 3) | ??0.021 | ??0.40 | ??11.5 |
| Unmodified calcium sulfate crystal whiskers adsorption rate | ??76.4％ | ??79.7％ | ??85.8％ |
| Wastewaters with modified calcium sulfate whiskers absorption back concentration c 3 (mg/Nm 3) | ??0.005 | ??0.06 | ??1.1 |
| The wastewaters with modified calcium sulfate whiskers adsorption rate | ??94.4％ | ??97.2％ | ??98.6％ |
In addition, the applicant also uses scanning electronic microscope respectively calcium sulfate crystal whiskers before and after the modification to be characterized.As shown in drawings: length shortens the calcium sulfate crystal whiskers after the modification (calcium sulfate crystal whiskers finished product), the whisker surface ratio is more coarse, and by a large amount of flocculent substances parcels, illustrate sodium hydroxide or potassium hydroxide successful attached to the whisker surface.
Claims (4)
1. calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion is characterized in that may further comprise the steps:
(1) choose the gypsum raw material that mean particle size is 30～60 μ m, it is 2%～6% slip that itself and water are mixed with weight percent concentration;
(2) slip for preparing in the step (1) is put into microwave reactor, add the whisker morphology conditioning agent, pH with slip is adjusted into 8～10 then, be under 120～130 ℃ the condition in normal pressure, temperature, stirring heating 1～2h, the control stir speed (S.S.) is 200～500rpm, and reaction finishes after-filtration, obtains the calcium sulfate crystal whiskers crude product;
(3) the calcium sulfate crystal whiskers crude product of producing in the step (2) is soaked for some time in basic solution, after taking out seasoning, put into retort furnace, under the condition of starvation, be warming up to 600～900 ℃ of postactivated 2～4h, promptly make the calcium sulfate crystal whiskers finished product that is used for adsorbing the flue gas of refuse burning heavy metal ion.
2. a kind of calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion according to claim 1 is characterized in that: in the step (1), described gypsum raw material is the plaster of paris or industrially desulfurized gypsum.
3. a kind of calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion according to claim 1 is characterized in that: in the step (2), described whisker morphology conditioning agent is magnesium chloride or vitriolate of tartar; The add-on of whisker morphology conditioning agent is the whisker morphology conditioning agent that adds 0.02～0.05mol in the 1L slip.
4. a kind of calcium sulphate crystal whisker preparation method that is used for adsorbing the flue gas of refuse burning heavy metal ion according to claim 1 is characterized in that: in the step (3), described basic solution is sodium hydroxide or potassium hydroxide; The ratio that is soaked in sodium hydroxide that 5～10ml concentration is 0.1～0.3mol/L or potassium hydroxide solution in 1g calcium sulfate crystal whiskers crude product is soaked, and soak time is 24～72h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| 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 |
| CN104651944A (en) * | 2015-02-12 | 2015-05-27 | 湘潭大学 | Preparation method of calcium-sulfate-based calcium sulfate crystal whisker |
| CN105036577A (en) * | 2015-07-06 | 2015-11-11 | 四川理工学院 | Method for improving strength of circulating fluidized bed power station fly ash in cement |
| CN105350084A (en) * | 2015-11-11 | 2016-02-24 | 山东科技大学 | Surface modification method for calcium sulfate whiskers |
| CN108914205A (en) * | 2017-03-30 | 2018-11-30 | 奕通工程顾问股份有限公司 | The manufacturing method of ca sulphate fibre and the coating for using it |
| CN110257915A (en) * | 2018-12-04 | 2019-09-20 | 天津科技大学 | A method of high-quality hemihydrate calcium sulfate crystal whisker is produced by waste of dense brine |
| CN110653247A (en) * | 2019-09-30 | 2020-01-07 | 中国矿业大学 | Soil phosphorus condition improvement method based on red mud-based composite solid waste material recycling |
| CN111450630A (en) * | 2020-04-13 | 2020-07-28 | 郑大鹏 | Smoke treatment equipment for rubber processing |
| CN113816509A (en) * | 2021-09-28 | 2021-12-21 | 石文建 | Method for adsorbing rare metal ions in aqueous solution by using calcium sulfate whiskers |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323974A (en) * | 2008-07-08 | 2008-12-17 | 浙江大学 | Method for preparing calcium sulphate crystal whisker from dolomite |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323974A (en) * | 2008-07-08 | 2008-12-17 | 浙江大学 | Method for preparing calcium sulphate crystal whisker from dolomite |
Non-Patent Citations (1)
| Title |
|---|
| 《无机材料学报》 20060331 杨晓庆等 微波作用下硫酸钙结晶过程中的"特殊效应"研究 第363-368 第21卷, 第2期 2 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| 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 |
| CN102352535B (en) * | 2011-09-22 | 2014-01-29 | 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 |
| CN104651944B (en) * | 2015-02-12 | 2017-04-05 | 湘潭大学 | A kind of preparation method of the heavy metal absorbent based on calcium sulfate crystal whiskers |
| CN104651944A (en) * | 2015-02-12 | 2015-05-27 | 湘潭大学 | Preparation method of calcium-sulfate-based calcium sulfate crystal whisker |
| CN105036577A (en) * | 2015-07-06 | 2015-11-11 | 四川理工学院 | Method for improving strength of circulating fluidized bed power station fly ash in cement |
| CN105036577B (en) * | 2015-07-06 | 2017-06-06 | 四川理工学院 | A kind of method for improving recirculating fluidized bed power station flyash intensity in cement |
| CN105350084A (en) * | 2015-11-11 | 2016-02-24 | 山东科技大学 | Surface modification method for calcium sulfate whiskers |
| CN108914205A (en) * | 2017-03-30 | 2018-11-30 | 奕通工程顾问股份有限公司 | The manufacturing method of ca sulphate fibre and the coating for using it |
| CN110257915A (en) * | 2018-12-04 | 2019-09-20 | 天津科技大学 | A method of high-quality hemihydrate calcium sulfate crystal whisker is produced by waste of dense brine |
| CN110653247A (en) * | 2019-09-30 | 2020-01-07 | 中国矿业大学 | Soil phosphorus condition improvement method based on red mud-based composite solid waste material recycling |
| CN111450630A (en) * | 2020-04-13 | 2020-07-28 | 郑大鹏 | Smoke treatment equipment for rubber processing |
| CN113816509A (en) * | 2021-09-28 | 2021-12-21 | 石文建 | Method for adsorbing rare metal ions in aqueous solution by using calcium sulfate whiskers |
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