CN105217773A - A kind of method utilizing Fe-based amorphous alloy to activate persulphate degraded pigment wastewater - Google Patents

A kind of method utilizing Fe-based amorphous alloy to activate persulphate degraded pigment wastewater Download PDF

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CN105217773A
CN105217773A CN201510743153.XA CN201510743153A CN105217773A CN 105217773 A CN105217773 A CN 105217773A CN 201510743153 A CN201510743153 A CN 201510743153A CN 105217773 A CN105217773 A CN 105217773A
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metal powder
waste water
ball milling
amorphous metal
crystaline amorphous
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CN105217773B (en
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马国峰
张鸿龄
刘岩
贺春林
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Shenyang University
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Abstract

Utilize Fe-based amorphous alloy to activate a method for persulphate degraded pigment wastewater, relate to a kind of method processing waste water, first described method prepares Fe 78si 9b 13non-crystaline amorphous metal powder dispersion, selection Fe-based amorphous alloy is Fe 78si 9b 13non-crystaline amorphous metal powder, its composition and atomic percent are: 78%Fe, 9%Si, 13%B; Then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution are mixed to form mixing solutions, add above-mentioned mixing solutions in the most backward waste water from dyestuff, utilize in mixing solutions the potentiometric titrations oxidative degradation waste water from dyestuff activating generation; Present invention process is simple, easy to operate, and catalyzer Fe-based amorphous alloy is prepared fairly simple, is easy to recycling.

Description

A kind of method utilizing Fe-based amorphous alloy to activate persulphate degraded pigment wastewater
Technical field
The present invention relates to a kind of method of wastewater treatment, be specially a kind of method utilizing Fe-based amorphous alloy to activate peroxydisulfate degradation of dye waste water.
Background technology
Along with industrialization develops rapidly, water consumption sharply increases, and discharged volume of industrial waste water also increases sharply.Wherein waste water from dyestuff accounts for 1/10th of trade effluent total release, has become the important source of pollution in water surrounding, and such waste water has complex structure, bio-refractory and forms the features such as harm to HUMAN HEALTH, is the organic waste water of generally acknowledged difficult degradation.
At present, dye waste water treatment method mainly contains physisorphtion, advanced oxidation processes, chemical oxidization method, biological degradation method and chemical flocculation etc., and the method for these degradation of dye waste water has limitation such as cost is high, efficiency is low, easy generation secondary pollution.Such as, utilizing hydrogen peroxide to produce the advanced oxidation processes of hydroxyl radical free radical has its weak point, and hydrogen peroxide utilization ratio is low, poor stability and the potential of hydrogen to waste water from dyestuff have the shortcomings such as specific requirement; Biological degradation method selectivity is too strong, and a kind of biological bacteria often only has degradation effect to certain or certain several dyestuff, and also has specific requirement to the potential of hydrogen of waste water from dyestuff; Chemical flocculation has very strong selectivity, and there is the shortcomings such as dosage is excessive, precipitating sludge is too much.
Recently, become study hotspot with persulfate oxidation method degradation of dye waste water, it utilizes potentiometric titrations to carry out degradation of dye waste water as oxygenant.And conventional persulphate activation method has thermal activation, transition metal activation and UV-activated.Wherein producing potentiometric titrations degradation of dye waste water with transition metal activation persulphate is also study hotspot.But utilize the efficiency of ferrous ion activation persulphate generation potentiometric titrations not high at present, cause being affected to the oxidative degradation effect of waste water from dyestuff; Although nano ferriferrous oxide activation persulphate degradation efficiency improves, nano ferriferrous oxide is easily reunited, and is difficult to ensure its characteristics of nanoparticles, is therefore unfavorable for recycling, and easily causes the shortcomings such as secondary pollution after reclaiming.
In Fe-based amorphous alloy, iron exists with atomic state, remain that iron itself has except look function, be a kind of material having very much the activation persulphate of using value.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing Fe-based amorphous alloy to activate peroxydisulfate degradation of dye waste water, both utilized iron itself in Fe-based amorphous alloy to have except look function, also to utilize in Fe-based amorphous alloy Zero-valent Iron activation persulphate can degradation of dye waste water quickly and efficiently simultaneously.The method technique is simple, easy to operate, and catalyzer Fe-based amorphous alloy is prepared fairly simple, is easy to recycling.
Technical scheme of the present invention is:
Utilize Fe-based amorphous alloy to activate a method for persulphate degraded pigment wastewater, the Fe-based amorphous alloy of this invention choice for use is Fe 78si 9b 13non-crystaline amorphous metal powder, its composition and atomic percent are: 78%Fe, 9%Si, 13%B.First Fe is prepared 78si 9b 13non-crystaline amorphous metal powder dispersion, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution are mixed to form mixing solutions, add above-mentioned mixing solutions in the most backward waste water from dyestuff, utilize in mixing solutions the potentiometric titrations oxidative degradation waste water from dyestuff activating generation.
A kind of method utilizing Fe-based amorphous alloy to activate persulphate degraded pigment wastewater described in it, concrete steps are as follows:
1, Fe-based amorphous alloy powder dispersion is prepared: adopt Mechanic Alloying Technology to prepare Fe 78si 9b 13non-crystaline amorphous metal powder, all devices is planetary ball mill.(1) testing simple substance raw material used is the powder of Fe, Si and B, and granularity is 200 orders, and purity is not less than 99.99%(mass percent).Select stainless steel as ball-milling medium, use three kinds of Stainless Steel Balls in test, be respectively the Stainless Steel Ball that 800 radiuses are 2 millimeters, 500 radiuses are 6 millimeters of Stainless Steel Balls, and 10 radiuses are the Stainless Steel Ball of 8 millimeters.(2) Fe of precise, Si and B powder is put into ball milling to fill with, more above-mentioned Stainless Steel Ball is put into ball milling filling, sealing ball milling is filled with.Then use vacuum pump evacuation, and be filled with high-purity argon gas as shielding gas, repeatedly carry out above-mentioned steps 5-6 time, ensure the purity of argon gas in the filling of last ball milling, finally check whether air valve has been tightened, with anti-gas-leak.3) ball milling filling be fixed on planetary ball mill, cover shield cap, start runs.The rotational speed of ball-mill 200-500 rev/min of this test, runs and within 1 hour, rests 1 hour, Ball-milling Time 30-80 hour.After the time that planetary ball mill has run setting, ball milling is filled with and is cooled by the time, opens the air valve of ball milling filling, discharges the argon gas that ball milling fills with the inside, then opens the Fe prepared by ball milling filling taking-up 78si 9b 13non-crystaline amorphous metal powder.4) by above-mentioned prepared Fe 78si 9b 13non-crystaline amorphous metal powder puts into the deionized water of 50-150 milliliter, with ultrasonic wave dispersion, forms Fe 78si 9b 13non-crystaline amorphous metal powder dispersion.
2, accurately taking 5-10 gram of Sodium Persulfate is dissolved in deionized water, to transfer in 1000 milliliters of volumetric flasks and to be diluted to volumetric flask groove with deionized water, preparing Sodium Persulfate solution, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution with volume ratio 1:1-3:1 mixing, form mixing solutions.
3, the degradation process of waste water from dyestuff: add above-mentioned mixing solutions in waste water from dyestuff, carry out the degraded of waste water from dyestuff, 500 ml beakers are adopted to be reactor, degrade to as if concentration be that the simulation Acid Orange II waste water of 5-15 mg/litre dissolves 150 milliliters, in reactor, add the above-mentioned mixing solutions of 20-100 milliliter, and be placed on magnetic stirring apparatus by reactor, adjust pH is 2-7, magnetic stirring apparatus rotating speed is 200 revs/min, and solution temperature is 25-50 DEG C.
The present invention has the following advantages:
1, the decrystallized powder of the present invention's Zero-valent Iron that utilized Mechanic Alloying Technology to prepare, had both remained the degrading waste water ability of iron atom itself, also to utilize in Fe-based amorphous alloy Zero-valent Iron activation persulphate can degradation of dye waste water quickly and efficiently.Fe-based amorphous alloy exists with powder state simultaneously, and its moderate specific surface area makes iron atom utilization ratio improve.
2, Fe-based amorphous alloy Forming ability of the present invention is strong, and production cost is low, technology maturation, and without the need to a large amount of funds, industrialization is easier to.
3, simplification of flowsheet of the present invention, easy and simple to handle, significantly improves the utilization ratio of Sodium Persulfate, reduce cost of water treatment.
Accompanying drawing explanation
Fe prepared by Fig. 1 embodiment 1 78si 9b 13the X-diffractogram of non-crystaline amorphous metal powder;
The Fe that Fig. 2 embodiment 2 is obtained 78si 9b 13non-crystaline amorphous metal powder electronic scanning photo;
Fig. 3 Fe 78si 9b 13the change in concentration figure of non-crystaline amorphous metal powder activation Sodium Persulfate degraded Acid Orange II.
In figure, curve a is the degraded situation of Acid Orange II in embodiment 1, and curve b is the degraded situation of Acid Orange II in embodiment 2, and curve c is the degraded situation of Acid Orange II in embodiment 3.
Embodiment
By the following examples in detail the present invention is described in detail.
Embodiment 1
1, Fe-based amorphous alloy powder dispersion is prepared: adopt Mechanic Alloying Technology to prepare Fe 78si 9b 13non-crystaline amorphous metal powder, all devices is planetary ball mill.(1) testing simple substance raw material used is the powder of Fe, Si and B, and granularity is 200 orders, and purity is not less than 99.99%(mass percent).Select stainless steel as ball-milling medium, use three kinds of Stainless Steel Balls in test, be respectively the Stainless Steel Ball that 800 radiuses are 2 millimeters, 500 radiuses are 6 millimeters of Stainless Steel Balls, and 10 radiuses are the Stainless Steel Ball of 8 millimeters.(2) Fe of precise, Si and B powder is put into ball milling to fill with, more above-mentioned Stainless Steel Ball is put into ball milling filling, sealing ball milling is filled with.Then use vacuum pump evacuation, and be filled with high-purity argon gas as shielding gas, repeatedly carry out above-mentioned steps 6 times, ensure the purity of argon gas in the filling of last ball milling, finally check whether air valve has been tightened, with anti-gas-leak.3) ball milling filling be fixed on planetary ball mill, cover shield cap, start runs.The rotational speed of ball-mill of this test 500 revs/min, runs and within 1 hour, rests 1 hour, Ball-milling Time 80 hours.After the time that planetary ball mill has run setting, ball milling is filled with and is cooled by the time, opens the air valve of ball milling filling, discharges the argon gas that ball milling fills with the inside, then opens the Fe-Si-B non-crystaline amorphous metal powder prepared by ball milling filling taking-up.4) by above-mentioned prepared Fe 78si 9b 13non-crystaline amorphous metal powder puts into the deionized water of 100 milliliters, with ultrasonic wave dispersion, forms Fe-Si-B non-crystaline amorphous metal powder dispersion.
2, accurately taking 8 grams of Sodium Persulfates is dissolved in deionized water, to transfer in 1000 milliliters of volumetric flasks and to be diluted to volumetric flask groove with deionized water, preparing Sodium Persulfate solution, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion adds in Sodium Persulfate solution and is mixed to form mixing solutions, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution with volume ratio 1:3 mixing, form mixing solutions.
3, the degradation process of waste water from dyestuff: add above-mentioned mixing solutions in waste water from dyestuff, carry out the degraded of waste water from dyestuff, 500 ml beakers are adopted to be reactor, degrade to as if concentration be that the simulation Acid Orange II waste water of 10 mg/litre dissolves 150 milliliters, in reactor, add 100 milliliters of above-mentioned mixing solutionss, and be placed on magnetic stirring apparatus by reactor, adjust pH is 5, magnetic stirring apparatus rotating speed is 200 revs/min, and solution temperature is 30 DEG C.
Embodiment 2
1, Fe-based amorphous alloy powder dispersion is prepared: adopt Mechanic Alloying Technology to prepare Fe 78si 9b 13non-crystaline amorphous metal powder, all devices is planetary ball mill.(1) testing simple substance raw material used is the powder of Fe, Si and B, and granularity is 200 orders, and purity is not less than 99.99%(mass percent).Select stainless steel as ball-milling medium, use three kinds of Stainless Steel Balls in test, be respectively the Stainless Steel Ball that 800 radiuses are 2 millimeters, 500 radiuses are 6 millimeters of Stainless Steel Balls, and 10 radiuses are the Stainless Steel Ball of 8 millimeters.(2) Fe of precise, Si and B powder is put into ball milling to fill with, more above-mentioned Stainless Steel Ball is put into ball milling filling, sealing ball milling is filled with.Then use vacuum pump evacuation, and be filled with high-purity argon gas as shielding gas, repeatedly carry out above-mentioned steps 6 times, ensure the purity of argon gas in the filling of last ball milling, finally check whether air valve has been tightened, with anti-gas-leak.3) ball milling filling be fixed on planetary ball mill, cover shield cap, start runs.The rotational speed of ball-mill of this test 300 revs/min, runs and within 1 hour, rests 1 hour, Ball-milling Time 50 hours.After the time that planetary ball mill has run setting, ball milling is filled with and is cooled by the time, opens the air valve of ball milling filling, discharges the argon gas that ball milling fills with the inside, then opens the Fe prepared by ball milling filling taking-up 78si 9b 13non-crystaline amorphous metal powder.4) by above-mentioned prepared Fe 78si 9b 13non-crystaline amorphous metal powder puts into the deionized water of 100 milliliters, with ultrasonic wave dispersion, forms Fe 78si 9b 13non-crystaline amorphous metal powder dispersion.
2, accurately taking 8 grams of Sodium Persulfates is dissolved in deionized water, to transfer in 1000 milliliters of volumetric flasks and to be diluted to volumetric flask groove with deionized water, preparing Sodium Persulfate solution, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion adds in Sodium Persulfate solution and is mixed to form mixing solutions, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution with volume ratio 1:2 mixing, form mixing solutions.
3, the degradation process of waste water from dyestuff: add above-mentioned mixing solutions in waste water from dyestuff, carry out the degraded of waste water from dyestuff, 500 ml beakers are adopted to be reactor, degrade to as if concentration be that the simulation Acid Orange II waste water of 10 mg/litre dissolves 150 milliliters, in reactor, add 100 milliliters of above-mentioned mixing solutionss, and be placed on magnetic stirring apparatus by reactor, adjust pH is 3, magnetic stirring apparatus rotating speed is 200 revs/min, and solution temperature is 30 DEG C.
Embodiment 3
1, Fe-based amorphous alloy powder dispersion is prepared: adopt Mechanic Alloying Technology to prepare Fe 78si 9b 13non-crystaline amorphous metal powder, all devices is planetary ball mill.(1) testing simple substance raw material used is the powder of Fe, Si and B, and granularity is 200 orders, and purity is not less than 99.99%(mass percent).Select stainless steel as ball-milling medium, use three kinds of Stainless Steel Balls in test, be respectively the Stainless Steel Ball that 800 radiuses are 2 millimeters, 500 radiuses are 6 millimeters of Stainless Steel Balls, and 10 radiuses are the Stainless Steel Ball of 8 millimeters.(2) Fe of precise, Si and B powder is put into ball milling to fill with, more above-mentioned Stainless Steel Ball is put into ball milling filling, sealing ball milling is filled with.Then use vacuum pump evacuation, and be filled with high-purity argon gas as shielding gas, repeatedly carry out above-mentioned steps 6 times, ensure the purity of argon gas in the filling of last ball milling, finally check whether air valve has been tightened, with anti-gas-leak.3) ball milling filling be fixed on planetary ball mill, cover shield cap, start runs.The rotational speed of ball-mill of this test 500 revs/min, runs and within 1 hour, rests 1 hour, Ball-milling Time 60 hours.After the time that planetary ball mill has run setting, ball milling is filled with and is cooled by the time, opens the air valve of ball milling filling, discharges the argon gas that ball milling fills with the inside, then opens the Fe prepared by ball milling filling taking-up 78si 9b 13non-crystaline amorphous metal powder.4) by above-mentioned prepared Fe 78si 9b 13non-crystaline amorphous metal powder puts into the deionized water of 100 milliliters, with ultrasonic wave dispersion, forms Fe 78si 9b 13non-crystaline amorphous metal powder dispersion.
2, accurately taking 6 grams of Sodium Persulfates is dissolved in deionized water, to transfer in 1000 milliliters of volumetric flasks and to be diluted to volumetric flask groove with deionized water, preparing Sodium Persulfate solution, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion adds in Sodium Persulfate solution and is mixed to form mixing solutions, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution with volume ratio 1:1 mixing, form mixing solutions.
3, the degradation process of waste water from dyestuff: add above-mentioned mixing solutions in waste water from dyestuff, carry out the degraded of waste water from dyestuff, 500 ml beakers are adopted to be reactor, degrade to as if concentration be that the simulation Acid Orange II waste water of 15 mg/litre dissolves 150 milliliters, in reactor, add 80 milliliters of above-mentioned mixing solutionss, and be placed on magnetic stirring apparatus by reactor, adjust pH is 7, magnetic stirring apparatus rotating speed is 200 revs/min, and solution temperature is 50 DEG C.

Claims (1)

1. utilize Fe-based amorphous alloy to activate a method for persulphate degraded pigment wastewater, it is characterized in that, first described method prepares Fe 78si 9b 13non-crystaline amorphous metal powder dispersion, selection Fe-based amorphous alloy is Fe 78si 9b 13non-crystaline amorphous metal powder, its composition and atomic percent are: 78%Fe, 9%Si, 13%B; Then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution are mixed to form mixing solutions, add above-mentioned mixing solutions in the most backward waste water from dyestuff, utilize in mixing solutions the potentiometric titrations oxidative degradation waste water from dyestuff activating generation; Comprise following detailed process:
1) prepare Fe-based amorphous alloy powder dispersion: the Fe of precise, Si and B powder is put into ball milling and filled with, more above-mentioned Stainless Steel Ball is put into ball milling filling, sealing ball milling is filled with; Then use vacuum pump evacuation, and be filled with high-purity argon gas as shielding gas, repeatedly carry out above-mentioned steps 5-6 time, ensure the purity of argon gas in the filling of last ball milling; Filled with by ball milling and be fixed on planetary ball mill, cover shield cap, start runs; By the time ball milling is filled with and is cooled, and opens the air valve of ball milling filling, discharges the argon gas that ball milling fills with the inside, then opens the Fe prepared by ball milling filling taking-up 78si 9b 13non-crystaline amorphous metal powder; By above-mentioned prepared Fe 78si 9b 13non-crystaline amorphous metal powder puts into the deionized water of 50-150 milliliter, with ultrasonic wave dispersion, forms Fe 78si 9b 13non-crystaline amorphous metal powder dispersion;
2) accurately taking 5-10 gram of Sodium Persulfate is dissolved in deionized water, to transfer in 1000 milliliters of volumetric flasks and to be diluted to volumetric flask groove with deionized water, preparing Sodium Persulfate solution, then by Fe 78si 9b 13non-crystaline amorphous metal powder dispersion and Sodium Persulfate solution with volume ratio 1:1-3:1 mixing, form mixing solutions;
3) degradation process of waste water from dyestuff: add above-mentioned mixing solutions in waste water from dyestuff, carry out the degraded of waste water from dyestuff, 500 ml beakers are adopted to be reactor, degrade to as if concentration be that the simulation Acid Orange II waste water of 5-15 mg/litre dissolves 150 milliliters, in reactor, add the above-mentioned mixing solutions of 20-100 milliliter, and be placed on magnetic stirring apparatus by reactor, adjust pH is 2-7, magnetic stirring apparatus rotating speed is 200 revs/min, and solution temperature is 25-50 DEG C.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106006916A (en) * 2016-07-18 2016-10-12 中国科学院金属研究所 Method for degradation of coking wastewater by utilizing Fe-base amorphous alloy
CN108046402A (en) * 2017-12-04 2018-05-18 沈阳大学 A kind of method using cu-based amorphous alloys degradation pigment wastewater
CN109095585A (en) * 2018-09-30 2018-12-28 湘潭大学 A method of for degrading azoic dye waste water
CN111644186A (en) * 2020-06-03 2020-09-11 中山大学 Method for removing ibuprofen by utilizing persulfate activation
CN113546653A (en) * 2021-07-23 2021-10-26 合肥工业大学 Fe-Si-B-P amorphous alloy catalyst for efficiently degrading dye and preparation method and application thereof
CN113769775A (en) * 2021-10-21 2021-12-10 沈阳大学 Novel magnetic composite catalyst and preparation method thereof
CN114873799A (en) * 2022-07-01 2022-08-09 深圳大学 Method for controlling disinfection by-products in drinking water by amorphous alloy strips

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CN102070236A (en) * 2009-11-20 2011-05-25 中国科学院金属研究所 Ferrum-based amorphous alloy strip for treating printing and dyeing wastewater and preparation method thereof
CN102633349A (en) * 2011-12-16 2012-08-15 华南理工大学 Method for treating track non-degradable organisms in water by aid of heterogenous sulfate radical oxidation
CN103831440A (en) * 2014-03-24 2014-06-04 山东大学 Method for smashing amorphous band Fe78Si9B13

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102070236A (en) * 2009-11-20 2011-05-25 中国科学院金属研究所 Ferrum-based amorphous alloy strip for treating printing and dyeing wastewater and preparation method thereof
CN102633349A (en) * 2011-12-16 2012-08-15 华南理工大学 Method for treating track non-degradable organisms in water by aid of heterogenous sulfate radical oxidation
CN103831440A (en) * 2014-03-24 2014-06-04 山东大学 Method for smashing amorphous band Fe78Si9B13

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106006916A (en) * 2016-07-18 2016-10-12 中国科学院金属研究所 Method for degradation of coking wastewater by utilizing Fe-base amorphous alloy
CN106006916B (en) * 2016-07-18 2020-01-07 中国科学院金属研究所 Method for degrading coking wastewater by using iron-based amorphous alloy
CN108046402A (en) * 2017-12-04 2018-05-18 沈阳大学 A kind of method using cu-based amorphous alloys degradation pigment wastewater
CN109095585A (en) * 2018-09-30 2018-12-28 湘潭大学 A method of for degrading azoic dye waste water
CN111644186A (en) * 2020-06-03 2020-09-11 中山大学 Method for removing ibuprofen by utilizing persulfate activation
CN113546653A (en) * 2021-07-23 2021-10-26 合肥工业大学 Fe-Si-B-P amorphous alloy catalyst for efficiently degrading dye and preparation method and application thereof
CN113769775A (en) * 2021-10-21 2021-12-10 沈阳大学 Novel magnetic composite catalyst and preparation method thereof
CN114873799A (en) * 2022-07-01 2022-08-09 深圳大学 Method for controlling disinfection by-products in drinking water by amorphous alloy strips
CN114873799B (en) * 2022-07-01 2022-11-01 深圳大学 Method for controlling disinfection by-products in drinking water by amorphous alloy strips

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