CN105819551A - Method for preparing novel and efficient reduced ion particle fillers - Google Patents
Method for preparing novel and efficient reduced ion particle fillers Download PDFInfo
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- CN105819551A CN105819551A CN201610205767.7A CN201610205767A CN105819551A CN 105819551 A CN105819551 A CN 105819551A CN 201610205767 A CN201610205767 A CN 201610205767A CN 105819551 A CN105819551 A CN 105819551A
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- zinc
- powder
- copper
- chloride
- mesh sieves
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Classifications
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- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
- C02F1/4678—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction of metals
-
- 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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
The invention discloses a method for preparing novel and efficient reduced ion particle fillers, and relates to the technical field of preparation of chemical fillers. The method comprises the following steps: selecting the following raw materials by weight: 70%-80% of iron powder, 6%-10% of a mixture of copper and copper chloride, 5%-15% of manganese dioxide, 3%-5% of graphite powder, 1%-2% of a mixture of zinc and zinc chloride; crushing, screening and uniformly mixing all the raw materials; uniformly spraying 8% of a potassium hydroxide solution to a mixed material according to a mass ratio of the mixed material to the potassium hydroxide solution being 12:1; then performing molding, baking, staged high-temperature firing, cooling, crushing and sieving treatments to obtain the novel and efficient reduced ion particle fillers. Compared with single copper chloride or zinc chloride selected as a catalyst, a composite catalyst has a higher catalytic efficiency and has advantages in overcoming surface passivation of fillers; in addition, the 8% of potassium hydroxide solution is used as a spraying agent, so that the firing cost is greatly reduced without degrading the product performance.
Description
Technical field:
The present invention relates to the preparation method of new and effective reduced iron granular filler, belong to the preparing technical field of chemistry filler.
Background technology:
Ferrum is active metal, and chemical property is active, is the most often used to degrade the organic pollution in water body.The mechanism of ferrum purifying water body mainly has three aspects: (1) reduction, Zero-valent Iron has stronger reproducibility, and the pollutant in water body can directly carry out reduction decomposition.(2) light electrolysis effect, [H] and the Fe that Zero-valent Iron is produced by light electrolysis2+Can be with the pollution components generation redox reaction in waste water, thus degradation of contaminant.(3) Coagulation and Adsorption effect, ferrum can generate Fe (OH) at the ion that reduction process produces2With Fe (OH)3Precipitation, Adsorption pollutant.
Removing the subject matter of pollutant in water body currently with reduced iron is that reduced iron is relatively low to the deoxidization, degradation speed of many polluters；Be exactly also reduced iron only under sour environment competence exertion go out higher reactivity, under the conditions of neutral or alkalescence, the degradation efficiency of polluter is extremely low；The most in use find that ferrum filling surface passivation phenomenon is obvious.For this, many scholars attempt the reducing power by strengthening ferrum at the another kind of metal of iron surface addition.Conventional metal has Au, Pt, Co, Cu, Ni, Pd, Ag etc..The surface nature different due to different metal and pollutant structure are different, cause these materials different to the degradation pathway of pollutant, complicated mechanism.A kind of micro-electrolysis environment-friendly filling material of Publication No. CN201010245779.5 and raw materials for production and preparation method thereof are exactly the filler being combined with copper, carbon by ferrum, and environment-friendly filler prepared by this method can increase cathodic discharge point, improve the reactivity of filler.But problem is the phenomenon of this filling surface passivation not to be obviously improved；The ferrum reactivity additionally constantly raised along with pH value of waste water when waste water flows through packing layer and cause declines obvious problem and is not the most overcome.
Summary of the invention:
For the problems referred to above, the technical problem to be solved in the present invention is to provide the preparation method of new and effective reduced iron granular filler.
The preparation method of the efficient reduced iron granule of the present invention is: step one: the selection of raw material, selects the raw material of following percentage by weight: 70%～80% iron powder, 6%～10% bronze medal and the mixture of copper chloride, 5%～15% manganese dioxide, 3%～5% graphite powder, 1%～2% mixture of zinc and zinc chloride；
Step 2: the process of raw material, takes the iron powder in step one raw material, crosses 100 mesh sieves, then taking manganese dioxide, pulverizing is milled, and crosses 100 mesh sieves, take graphite, pulverizing is milled, and crosses 100 mesh sieves, takes zinc powder and zinc chloride, wherein zinc powder is 1:3 with the weight ratio of zinc chloride, pulverize respectively and mill, cross 100 mesh sieves, be sufficiently mixed uniformly；Taking copper powder and copper chloride, wherein copper powder is 8:1 with the weight ratio of copper chloride, pulverizes respectively and mills, cross 100 mesh sieves, is sufficiently mixed uniformly；
Step 3: material of pulverizing all of in step 2 being milled is mixed together uniformly, it is that 12:1 uniformly sprays 8% potassium hydroxide solution in compound by compound and potassium hydroxide solution mass ratio, then molding, drying, interim high-temperature firing, cooling 6-8 hour, pulverize and sieve and obtain product after process.
As preferably, in described step 3, the detailed process of interim high-temperature firing is: first isolation atmosphere temperature rising 1 hour to 300 DEG C, then heats up 4 hours to 750 DEG C, is incubated 4 hours, heats up 3 hours to 980 DEG C, be incubated 8～10 hours.
As preferably, in the raw material of described step one, zinc chloride and copper chloride are catalyst.
As preferably, first copper and copper chloride to be sufficiently mixed resulting mixture in described step 2 in the processing procedure of raw material, zinc and zinc chloride are sufficiently mixed resulting mixture.
Beneficial effects of the present invention: reduced iron filler passes through hot stage roasting, both the specific surface area of filler burnt out can be made bigger, it is also ensured that the fusion between different raw materials, due to ferrum, copper in the new packing of sintering, the existence of the materials such as manganese, in acid waste water, ferrum and copper can occur electrode reaction, and electrode reaction produces [H] and the Fe of a large amount of nascent states2+Can be with the harmful constituent generation redox in waste water, so that polluter is degraded；When pH value of waste water is increased to neutrality or alkalescence, and the electrode reaction between ferrum and manganese dioxide is reinforced, thus ensure filler continuous discharge, reach the sustaining degradation to polluter.The catalyst that the most importantly zinc chloride and copper chloride are combined into can significantly increase these electrode reaction speed.Relative to single choose copper chloride or zinc chloride as catalyst for, the catalytic efficiency of composite catalyst is higher, and more advantage in terms of overcoming filling surface passivation.Additionally with 8% potassium hydroxide solution as spray agent, it is ensured that in the case of properties of product do not decline, make the temperature fired be reduced to 980 DEG C by 1120 DEG C when being not added with potassium hydroxide solution, significantly reduce and fire cost.
Accompanying drawing illustrates:
For ease of explanation, the present invention is embodied as and accompanying drawing is described in detail by following.
Fig. 1 is the data analysis table that the phenol wastewater that certain gas generator produces under equal conditions is processed by the reduced iron environment-friendly filler made in the embodiment of the present invention 1 with commercially available conventional iron carbon filler；
Fig. 2 is the data analysis table that the phenol wastewater that certain gas generator produces under equal conditions is processed by the reduced iron environment-friendly filler made in the embodiment of the present invention 2 with commercially available conventional iron carbon filler；
Fig. 3 is the data analysis table that the phenol wastewater that certain gas generator produces under equal conditions is processed by the reduced iron environment-friendly filler made in the embodiment of the present invention 2 with commercially available conventional iron carbon filler.
Detailed description of the invention:
This detailed description of the invention is by the following technical solutions: its preparation method is: step one: the selection of raw material, selects the raw material of following percentage by weight: 70%～80% iron powder, 6%～10% bronze medal and the mixture of copper chloride, 5%～15% manganese dioxide, 3%～5% graphite powder, 1%～2% mixture of zinc and zinc chloride.
Step 2: the process of raw material, takes the iron powder in step one raw material, crosses 100 mesh sieves, then taking manganese dioxide, pulverizing is milled, and crosses 100 mesh sieves, take graphite, pulverizing is milled, and crosses 100 mesh sieves, takes zinc powder and zinc chloride, wherein zinc powder is 1:3 with the weight ratio of zinc chloride, pulverize respectively and mill, cross 100 mesh sieves, be sufficiently mixed uniformly；Taking copper powder and copper chloride, wherein copper powder is 8:1 with the weight ratio of copper chloride, pulverizes respectively and mills, cross 100 mesh sieves, is sufficiently mixed uniformly；
Step 3: material of pulverizing all of in step 2 being milled is mixed together uniformly, it is that 12:1 uniformly sprays 8% potassium hydroxide solution in compound by compound and potassium hydroxide solution mass ratio, then molding, drying, interim high-temperature firing, cooling 6-8 hour, pulverize and sieve and obtain product after process.
As preferably, in described step 3, the detailed process of interim high-temperature firing is: first isolation atmosphere temperature rising 1 hour to 300 DEG C, then heats up 4 hours to 750 DEG C, is incubated 4 hours, heats up 3 hours to 980 DEG C, be incubated 8～10 hours.
As preferably, in the raw material of described step one, zinc chloride and copper chloride are catalyst.
As preferably, first copper and copper chloride to be sufficiently mixed resulting mixture in described step 2 in the processing procedure of raw material, zinc and zinc chloride are sufficiently mixed resulting mixture.
Embodiment 1:
Take iron powder, cross 100 mesh sieves.Taking manganese dioxide, pulverizing is milled, and crosses 100 mesh sieves.Taking graphite, pulverizing is milled, and crosses 100 mesh sieves；Taking zinc powder and zinc chloride respectively, pulverizing is milled, and crosses 100 mesh sieves, fully mixes with weight ratio 1:3.Iron powder, manganese dioxide, graphite powder, zinc powder and zinc chloride mixture after sieving obtains compound A after 80:10:5:1 is sufficiently mixed in mass ratio；Taking copper powder and copper chloride respectively, pulverizing is milled, and crosses 100 mesh sieves, fully mixes with weight ratio 8:1, for material B.Compound A is mixed with material B 10:1 in mass ratio, in compound, uniformly sprays 8% potassium hydroxide solution, molding by compound with potassium hydroxide solution mass ratio 12:1, dry, tinning, enter kiln, first isolation atmosphere temperature rising 1 hour to 300 DEG C；Then heat up 4 hours to 750 DEG C, be incubated 4 hours；Finally heat up 3 hours to 980 DEG C, be incubated 8～10 hours.Cooling, kiln discharge after cooling in 6 hours, broken sieving obtains product.Certain pesticide intermediate waste water is under equal conditions processed by the reduced iron environment-friendly filler using the present embodiment with commercially available conventional iron carbon filler, treatment effect such as Fig. 1.
Embodiment 2:
Take iron powder, cross 100 mesh sieves.Taking manganese dioxide, pulverizing is milled, and crosses 100 mesh sieves.Taking graphite, pulverizing is milled, and crosses 100 mesh sieves；Taking zinc powder and zinc chloride respectively, pulverizing is milled, and crosses 100 mesh sieves, fully mixes with weight ratio 1:3.Iron powder, manganese dioxide, graphite powder, zinc powder and zinc chloride mixture after sieving obtains compound A after 80:15:5:2 is sufficiently mixed in mass ratio, takes copper powder and copper chloride respectively, and pulverizing is milled, and crosses 100 mesh sieves, fully mixes with weight ratio 8:1, for material B；Compound A is mixed with material B 14:1 in mass ratio, in compound, uniformly sprays 8% potassium hydroxide solution, molding by compound with potassium hydroxide solution mass ratio 12:1, dry, tinning, enter kiln, then isolation atmosphere temperature rising 1 hour to 300 DEG C；Then heat up 4 hours to 750 DEG C, be incubated 4 hours；Finally heat up 3 hours to 980 DEG C, be incubated 8～10 hours.Cooling, kiln discharge after cooling in 6 hours, broken sieving obtains product.The phenol wastewater that certain gas generator is produced by the reduced iron environment-friendly filler of use the present embodiment and commercially available conventional iron carbon filler under equal conditions processes, treatment effect such as Fig. 2.
Embodiment 3:
Take iron powder, cross 100 mesh sieves.Taking manganese dioxide, pulverizing is milled, and crosses 100 mesh sieves.Taking graphite, pulverizing is milled, and crosses 100 mesh sieves；Taking zinc powder and zinc chloride respectively, pulverizing is milled, and crosses 100 mesh sieves, fully mixes with weight ratio 1:3.Iron powder, manganese dioxide, graphite powder, zinc powder and zinc chloride mixture after sieving obtains compound A after 80:15:5:1 is sufficiently mixed in mass ratio；Take copper powder and copper chloride respectively, pulverizing is milled, cross 100 mesh sieves, fully mix with weight ratio 8:1, for material B, compound A is mixed with material B 12:1 in mass ratio, in compound, uniformly spray 8% potassium hydroxide solution, molding by compound with potassium hydroxide solution mass ratio 12:1, dry, tinning, enters kiln.Then isolation atmosphere temperature rising 1 hour to 300 DEG C；Then heat up 4 hours to 750 DEG C, be incubated 4 hours；Finally heat up 3 hours to 980 DEG C, be incubated 8～10 hours.Cooling, kiln discharge after cooling in 6 hours, broken sieving obtains product.The reduced iron environment-friendly filler using the present embodiment produces waste water with commercially available conventional iron carbon filler to certain methyl ethyl ketone peroxide and under equal conditions processes, treatment effect such as Fig. 3；Graphic analyses: with reference to Fig. 1-3, it is higher that the reduced iron environment-friendly filler that the present embodiment is made and traditional ferrum carbon filler phase comparison produce the clearance of COD in waste water.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within scope of the claimed invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (4)
- The preparation method of the most new and effective reduced iron granular filler, it is characterized in that: step one: the selection of raw material, select the raw material of following percentage by weight: 70%～80% iron powder, 6%～10% bronze medal and the mixture of copper chloride, 5%～15% manganese dioxide, 3%～5% graphite powder, 1%～2% mixture of zinc and zinc chloride；Step 2: the process of raw material, takes the iron powder in step one raw material, crosses 100 mesh sieves, then taking manganese dioxide, pulverizing is milled, and crosses 100 mesh sieves, take graphite, pulverizing is milled, and crosses 100 mesh sieves, takes zinc powder and zinc chloride, wherein zinc powder is 1:3 with the weight ratio of zinc chloride, pulverize respectively and mill, cross 100 mesh sieves, be sufficiently mixed uniformly；Taking copper powder and copper chloride, wherein copper powder is 8:1 with the weight ratio of copper chloride, pulverizes respectively and mills, cross 100 mesh sieves, is sufficiently mixed uniformly；Step 3: material of pulverizing all of in step 2 being milled is mixed together uniformly, it is that 12:1 uniformly sprays 8% potassium hydroxide solution in compound by compound and potassium hydroxide solution mass ratio, then molding, drying, interim high-temperature firing, cooling 6-8 hour, pulverize and sieve and obtain product after process.
- 2. according to the preparation method of the new and effective reduced iron granular filler described in claim 1, it is characterized in that: in described step 3, the detailed process of interim high-temperature firing is: first isolation atmosphere temperature rising 1 hour to 300 DEG C, then heat up 4 hours to 750 DEG C, it is incubated 4 hours, heat up 3 hours to 980 DEG C, be incubated 8～10 hours.
- 3. according to the preparation method of the new and effective reduced iron granular filler described in claim 1, it is characterised in that: in the raw material of described step one, zinc chloride and copper chloride are catalyst.
- 4. according to the preparation method of the new and effective reduced iron granular filler described in claim 1, it is characterised in that: first copper and copper chloride to be sufficiently mixed resulting mixture in the processing procedure of raw material in described step 2, zinc and zinc chloride are sufficiently mixed resulting mixture.
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| CN201610205767.7A CN105819551A (en) | 2016-04-05 | 2016-04-05 | Method for preparing novel and efficient reduced ion particle fillers |
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| CN201610205767.7A CN105819551A (en) | 2016-04-05 | 2016-04-05 | Method for preparing novel and efficient reduced ion particle fillers |
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Citations (5)
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|---|---|---|---|---|
| WO2008115753A3 (en) * | 2007-03-16 | 2009-08-27 | Honda Motor Co., Ltd. | Method of preparing carbon nanotube containing electrodes |
| CN104003483A (en) * | 2014-06-19 | 2014-08-27 | 福州大学 | Bamboo charcoal-based microelectrolysis porous ceramsite filler and preparing method thereof |
| CN104150568A (en) * | 2014-09-05 | 2014-11-19 | 刘理方 | Catalytic micro-electrolysis material and preparation method thereof |
| CN104628091A (en) * | 2015-01-24 | 2015-05-20 | 杨强 | Multi-element catalytic microelectrolysis packing as well as preparation method and application thereof |
| CN105417643A (en) * | 2015-11-11 | 2016-03-23 | 南京格洛特环境工程股份有限公司 | Oxidation and reduction double-effect micro electrolysis combined reactor and application thereof |
-
2016
- 2016-04-05 CN CN201610205767.7A patent/CN105819551A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008115753A3 (en) * | 2007-03-16 | 2009-08-27 | Honda Motor Co., Ltd. | Method of preparing carbon nanotube containing electrodes |
| CN104003483A (en) * | 2014-06-19 | 2014-08-27 | 福州大学 | Bamboo charcoal-based microelectrolysis porous ceramsite filler and preparing method thereof |
| CN104150568A (en) * | 2014-09-05 | 2014-11-19 | 刘理方 | Catalytic micro-electrolysis material and preparation method thereof |
| CN104628091A (en) * | 2015-01-24 | 2015-05-20 | 杨强 | Multi-element catalytic microelectrolysis packing as well as preparation method and application thereof |
| CN105417643A (en) * | 2015-11-11 | 2016-03-23 | 南京格洛特环境工程股份有限公司 | Oxidation and reduction double-effect micro electrolysis combined reactor and application thereof |
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Application publication date: 20160803 |
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