CN105435795A - Method and application for preparing catalyst by using red mud as raw materials - Google Patents
Method and application for preparing catalyst by using red mud as raw materials Download PDFInfo
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- CN105435795A CN105435795A CN201610061796.0A CN201610061796A CN105435795A CN 105435795 A CN105435795 A CN 105435795A CN 201610061796 A CN201610061796 A CN 201610061796A CN 105435795 A CN105435795 A CN 105435795A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/12—Silica and alumina
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
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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
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The invention provides a method and application for preparing a catalyst by using red mud as raw materials. The catalyst includes red mud, coal ash, an adhesion agent, a pore-foaming agent, water glass and clay and further comprises iron ore or iron compounds. The method for preparing the catalyst comprises the steps of drying, smashing, mixing, extrusion forming, solidification, activation and finished product obtaining. The obtained catalyst is added into wastewater containing organic matter for electrocatalytic oxidation degradation, and therefore the organic matter is removed and indexes such as wastewater COD are decreased. The method for preparing the catalyst by using the red mud as the raw materials is easy to implement, short in technological process and capable of solving the problem of environmental pollution and achieving recycling of solid waste; the method is applied to the electrocatalytic oxidation process, no medicament is added, and the method is environmentally friendly and controllable.
Description
Technical field
The invention belongs to resource and field of environmental technology, relate to a kind of method and the application of catalyst in By Electro-catalytic Oxidation Process organic wastewater that utilize red mud and flyash Kaolinite Preparation of Catalyst.
Background technology
Red mud is the pureed strong basicity solid waste of smelting the high-moisture of discharging in alumina process, primarily of fine grain mud and coarse grained sand composition.Growing along with aluminum i ndustry, the red mud amount of producing aluminium oxide discharge is huge, often produce 1 ton of aluminium oxide according to statistics and will discharge 1 ~ 1.8 ton of red mud, China is as large alumina producing state of the world the 4th, only domestic five large Aluminum bases (Shandong, Shanxi, Great Wall, Guizhou and Guangxi), the red mud of annual generation just reaches about 6,000,000 tons, accumulative nearly 200,000,000 tons of red mud storage, and utilization rate is only about 15%.Damming with red mud is stored up and is not only taken a large amount of land resource, expend huge stockyard construction and maintenance cost, and strong basicity, high salinity waste red mud residues store up for a long time and can cause alkalization of soils, polluted surface and underground water source, serious harm is caused to ecological environment, therefore, the comprehensive development and utilization of red mud has become China's aluminum oxide industry and has realized one of important channel of recycling economy and sustainable development.
China is the big producing country of aluminium oxide, and the red mud produced for 2009 accounts for 30% of Gross World Product.The red mud comprehensive utilization ratio of current China is only 4%.Along with China's aluminium oxide output increases the reduction gradually with bauxite grade year by year, the volume of cargo in storage of red mud also will constantly increase.At present, red mud comprehensive utilization still belongs to global problem, in the world red mud is mainly adopted to the disposal options of storing up earthing.Alkali content in red mud is very high, and therefore this disposal options can be brought periphery animals and plants, the not predictable harm such as underground water.The red mud comprehensive utilization work of China obtains the great attention of each side in recent years, has carried out the research work of interdiscipline, multi-field comprehensive utilization.
The catalyst of existing By Electro-catalytic Oxidation Process organic wastewater, production cost is very high, drops into and is difficult to balance with income; Also someone studies the application of the low cost raw materials such as red mud, but does not all develop the good catalyst of degrading waste water effect.
Prior art has following defect: the operating cost of (1) By Electro-catalytic Oxidation Process organic wastewater is high; (2) for high COD, difficult degradation, difficult sewage, degradation efficiency is low, weak effect; (3) the noxious waste pollution environment such as red mud, fails effectively to utilize.
Summary of the invention
The invention provides a kind of utilize red mud to be raw material Kaolinite Preparation of Catalyst method and application, realize following goal of the invention:
1, reduce the operating cost of By Electro-catalytic Oxidation Process organic wastewater, improve the treatment effect of degradation of organic waste water; For high COD, difficult degradation, difficult sewage, improve catalytic oxidation efficiency;
2, to shorten By Electro-catalytic Oxidation Process organic wastewater, save power consumption energy consumption;
3, adopt the solid waste such as red mud, flyash to be raw material, reduce environmental pollution;
4, simplify the preparation method of catalyst, realize not producing pollutant in production process.
For achieving the above object, the present invention is by the following technical solutions:
Utilize red mud for a method for raw material Kaolinite Preparation of Catalyst, it is characterized in that: described catalyst comprises following raw material: red mud, flyash, binding agent, pore-foaming agent, material, waterglass and clay containing ferro element.
Below the further improvement to technique scheme:
The described material containing ferro element is iron ore or iron compound.
The weight portion of each raw material of described catalyst is:
Red mud 1000 ~ 1500 parts, iron compound 500 ~ 1000 parts, 250 ~ 500 parts, flyash, binding agent 10 ~ 100 parts, pore-foaming agent 30 ~ 500 parts, waterglass 54 ~ 200 parts, clay 100 ~ 500 parts.
The weight portion of each raw material of described catalyst is:
Red mud 1000 ~ 1500 parts, iron compound 500 ~ 1000 parts, 250 ~ 500 parts, flyash, binding agent 50 ~ 100 parts, pore-foaming agent 250 ~ 500 parts, waterglass 100 ~ 200 parts, clay 250 ~ 500 parts.
The weight portion of each raw material of described catalyst is:
Red mud 1500 parts, iron compound 500 parts, 250 parts, flyash, binding agent 10 parts, pore-foaming agent 30 parts, waterglass 54 parts, clay 100 parts.
Described flyash: phosphorus content is 15% ~ 60%;
Described iron compound is any one in ferric nitrate, iron oxide, tri-iron tetroxide.
Utilize red mud for a method for raw material Kaolinite Preparation of Catalyst, comprise dry broken, mixing, extruded, solidification with activation, obtain finished product step.
Described solidification and activation: solidification temperature is 120 ~ 180 DEG C, hardening time is 2 ~ 5 hours;
Activation temperature is 500 ~ 650 DEG C, and soak time is 6 ~ 8 hours.
Described oven dry is broken: to dry to moisture lower than 5%, be crushed to particle diameter and be less than 1 millimeter;
Described extruded: shaping product is not adhered to one another, flawless.
An application for the catalyst utilizing red mud to prepare for raw material, adopt catalyst electrolysis containing organic waste water, the amount ratio of catalyst and waste water is 100 ~ 200g:1000mL, and control decomposition voltage is 12 ~ 20V, and control electrolysis time is 0.5 ~ 2.5h.
Compared with prior art, the present invention has following beneficial effect:
1, catalyst application of the present invention is in By Electro-catalytic Oxidation Process organic wastewater process, reduces operating cost, and the treatment effect of degradation of organic waste water is good; For high COD, difficult degradation, difficult sewage, greatly improve catalytic oxidation efficiency;
2, compared with conventional catalyst, reach same catalytic oxidation effect, degradation time 30% can be shortened, save power consumption energy consumption 30%;
3, the solid waste such as red mud, flyash is that composite catalyst prepared by raw material, and raw materials market is sufficient and achieve solid waste resource recovery and utilize, and decreases environmental pollution, promotes the development of China's recycling economy;
4, method for preparing catalyst of the present invention is simple, easy to operate, does not produce any other pollutant in production process.
The present invention is with the solid waste such as red mud, flyash for composite catalyst prepared by raw material, and preparation method is simple to operate, and technological process is short, solves the problem of environmental pollution, also realizes the recycling of solid waste simultaneously; Be applied in By Electro-catalytic Oxidation Process organic sewage process do not add medicament, environmental protection is controlled.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Red mud of the present invention chooses the red mud from Bayer process.
Embodiment 1 one kinds utilizes red mud for the method for raw material Kaolinite Preparation of Catalyst
Described catalyst comprises following raw material: red mud, iron compound, flyash, binding agent, pore-foaming agent, waterglass and clay;
The weight portion of each raw material of described catalyst is:
Red mud 1000 parts, iron compound 500 parts, 250 parts, flyash, binding agent 50 parts, pore-foaming agent 250 parts, waterglass 100 parts, clay 250 parts;
Described red mud can directly use, and does not need through dealkalize process;
Described flyash: phosphorus content is 15%;
Described iron compound is ferric nitrate.
The preparation method of above-mentioned catalyst:
The first step is dried broken
By red mud at 100 DEG C of dry 12h, make moisture lower than 5%;
By flyash, iron compound, bonding agent, pore-foaming agent and clay, dry respectively to moisture lower than 5%;
Above-mentioned raw materials is all crushed to particle diameter and is less than 1 millimeter;
Second step mixes
Red mud, flyash, iron compound, bonding agent, pore-foaming agent, waterglass and clay is taken according to formula rate;
Red mud, iron compound and flyash are mixed, puts into mixer, stir, in whipping process, add binding agent, pore-foaming agent, waterglass and clay;
3rd step is extruded
The material stirred is put into shaping extruder, carries out extruded, can be spherical, the shape such as column, hollow columnar;
Spherical diameter can be 2 ~ 20 millimeters, and cylindrical length can be 4 ~ 70 millimeters, can adjust flexibly according to on-the-spot size;
Shaping product: not adhered to one another, flawless;
4th step solidification and activation
By shaping catalyst, carry out baking and curing and high-temperature calcination activation;
By shaping catalyst at 120 DEG C of temperature, baking and curing 2 hours;
6 hours are activated again at 500 DEG C of temperature lower calcinations;
5th step obtains finished product
After having activated, take out catalyst, get product, pack, rear storage or transport.
Embodiment 2 one kinds utilizes red mud for the method for raw material Kaolinite Preparation of Catalyst
Described catalyst comprises following raw material: red mud, iron compound, flyash, binding agent, pore-foaming agent, waterglass and clay;
The weight portion of each raw material of described catalyst is:
Red mud 1200 parts, iron compound 600 parts, 300 parts, flyash, binding agent 70 parts, pore-foaming agent 350 parts, waterglass 120 parts, clay 280 parts;
Described red mud can directly use, and does not need through dealkalize process;
Described flyash: phosphorus content is 30%;
Described iron compound is iron oxide.
The preparation method of above-mentioned catalyst:
Identical with the preparation method of embodiment 1, only change:
4th step solidification and activation
By shaping catalyst, carry out baking and curing and high-temperature calcination activation;
By shaping catalyst at 150 DEG C of temperature, baking and curing 3 hours;
6 hours are activated again at 550 DEG C of temperature lower calcinations.
Embodiment 3 one kinds utilizes red mud for the method for raw material Kaolinite Preparation of Catalyst
Described catalyst comprises following raw material: red mud, iron compound, flyash, binding agent, pore-foaming agent, waterglass and clay;
The weight portion of each raw material of described catalyst is:
Red mud 1400 parts, iron compound 900 parts, 450 parts, flyash, binding agent 90 parts, pore-foaming agent 460 parts, waterglass 180 parts, clay 400 parts;
Described red mud can directly use, and does not need through dealkalize process;
Described flyash: phosphorus content is 45%;
Described iron compound is tri-iron tetroxide.
The preparation method of above-mentioned catalyst:
Identical with the preparation method of embodiment 1, only change:
4th step solidification and activation
By shaping catalyst, carry out baking and curing and high-temperature calcination activation;
By shaping catalyst at 170 DEG C of temperature, baking and curing 4 hours;
7 hours are activated again at 600 DEG C of temperature lower calcinations.
Embodiment 4 one kinds utilizes red mud for the method for raw material Kaolinite Preparation of Catalyst
Described catalyst comprises following raw material: red mud, iron ore, flyash, binding agent, pore-foaming agent, waterglass and clay;
Red mud 1500 parts, iron ore 1000 parts, 500 parts, flyash, binding agent 100 parts, pore-foaming agent 500 parts, waterglass 200 parts, clay 500 parts;
Described red mud can directly use, and does not need through dealkalize process;
Described flyash: phosphorus content is 60%;
Described iron ore: iron content is higher than 60%.
The preparation method of above-mentioned catalyst:
Identical with the preparation method of embodiment 1, change iron compound is iron ore, changes the 4th step to be:
4th step solidification and activation
By shaping catalyst, carry out baking and curing and high-temperature calcination activation;
By shaping catalyst at 180 DEG C of temperature, baking and curing 5 hours;
8 hours are activated again at 650 DEG C of temperature lower calcinations.
Embodiment 5 one kinds utilizes red mud for the method for raw material Kaolinite Preparation of Catalyst
Described catalyst comprises following raw material: red mud, iron compound, flyash, binding agent, pore-foaming agent, waterglass and clay;
The weight portion of each raw material of described catalyst is:
Red mud 1500 parts, iron compound 500 parts, 250 parts, flyash, binding agent 10 parts, pore-foaming agent 30 parts, waterglass 54 parts, clay 100 parts;
Described iron compound is iron oxide;
Described pore-foaming agent is sesbania powder;
Described clay is kaolin.
The preparation method of above-mentioned catalyst:
Identical with the preparation method of embodiment 1, only change:
4th step solidification and activation
By shaping catalyst, carry out baking and curing and high-temperature calcination activation;
By shaping catalyst at 120 DEG C of temperature, baking and curing 5 hours;
6 hours are activated again at 550 DEG C of temperature lower calcinations.
Embodiment 6 one kinds of catalyst application in By Electro-catalytic Oxidation Process organic wastewater
Catalyst fill can be permeable corbie in, between the positive/negative plate then basket being put into electrolytic cell, bottom of electrolytic tank is equipped with aeration tube, and is connected with the small-sized fan of electrolytic cell outside;
To add containing organic waste water in electrolytic cell, liquid level be identical with catalyst height or slightly high; The amount ratio controlling catalyst and waste water is 100 ~ 200g:1000mL;
Positive/negative plate is connected to respectively the both positive and negative polarity of rectifier with cable, connects electrolytic cell positive and negative power supply and fan power, micro-aeration catalytic oxidation is carried out to organic wastewater in electrolytic cell, the organic matter in degrading waste water;
Control decomposition voltage is 12 ~ 20V, and controlling the cell reaction time is 0.5 ~ 2.5h.
Applied analysis is tested:
The organic wastewater adopting Coal Chemical Industry to discharge is tested: the COD content of organic wastewater is 5350mg/L;
Adopt the application process degradation of organic waste water of embodiment 6;
1, the catalyst degradation organic wastewater adopting embodiment 1 to prepare, the catalyst amount of employing, decomposition voltage and reaction time are in table 1;
The design parameter of catalyst in degradation of organic waste water of table 1 embodiment 1
To the organic wastewater after experimental group 1-3 degraded, the COD value of wastewater measurement; Measurement result is in table 2;
Table 2
Drawn by table 2, catalyst amount is preferably: the amount ratio of catalyst and waste water is 200g:1000mL.
2, adopt the catalyst degradation organic wastewater of embodiment 1, the catalyst amount of employing, decomposition voltage and reaction time are in table 3;
The design parameter of catalyst in degradation of organic waste water of table 3 embodiment 1
To the organic wastewater after experimental group 4-6 degraded, the COD value of wastewater measurement; Measurement result is in table 4;
Table 4
Draw according to table 4, the decomposition voltage of catalyst degradation organic wastewater is preferably 18V.
3, adopt the catalyst degradation organic wastewater of embodiment 1, the catalyst amount of employing, decomposition voltage and reaction time are in table 5;
The design parameter of catalyst in degradation of organic waste water of table 5 embodiment 1
To the organic wastewater after experimental group 7-9 degraded, the COD value of wastewater measurement; Measurement result is in table 6;
Table 6
Draw according to table 6, the cell reaction time of catalyst degradation organic wastewater is preferably 1h.
4, the catalyst degradation organic wastewater adopting embodiment 1-5 to prepare respectively, the amount ratio controlling catalyst and waste water is 200g:1000mL, and decomposition voltage is 18V, and the reaction time is 1h, measures the COD value of waste water after degraded; Measurement result is in table 7;
Table 7
Show that the best results of embodiment 5 catalyst is preferred embodiment according to table 7.
Percentage of the present invention is mass percent.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.The above is the citing of best mode for carrying out the invention, and the part wherein do not addressed in detail is the common practise of those of ordinary skill in the art; Protection scope of the present invention is as the criterion with the content of claim, and any equivalent transformation carried out based on technology enlightenment of the present invention, also within protection scope of the present invention.
Claims (10)
1. utilize red mud for a method for raw material Kaolinite Preparation of Catalyst, it is characterized in that: described catalyst comprises following raw material: red mud, flyash, binding agent, pore-foaming agent, material, waterglass and clay containing ferro element.
2. a kind of red mud that utilizes according to claim 1 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that: the described material containing ferro element is iron ore or iron compound.
3. a kind of red mud that utilizes according to claim 1 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that: the weight portion of each raw material of described catalyst is:
Red mud 1000 ~ 1500 parts, iron compound 500 ~ 1000 parts, 250 ~ 500 parts, flyash, binding agent 10 ~ 100 parts, pore-foaming agent 30 ~ 500 parts, waterglass 54 ~ 200 parts, clay 100 ~ 500 parts.
4. a kind of red mud that utilizes according to claim 1 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that: the weight portion of each raw material of described catalyst is:
Red mud 1000 ~ 1500 parts, iron compound 500 ~ 1000 parts, 250 ~ 500 parts, flyash, binding agent 50 ~ 100 parts, pore-foaming agent 250 ~ 500 parts, waterglass 100 ~ 200 parts, clay 250 ~ 500 parts.
5. a kind of red mud that utilizes according to claim 1 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that: the weight portion of each raw material of described catalyst is:
Red mud 1500 parts, iron compound 500 parts, 250 parts, flyash, binding agent 10 parts, pore-foaming agent 30 parts, waterglass 54 parts, clay 100 parts.
6. a kind of red mud that utilizes according to claim 1 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that:
Described flyash: phosphorus content is 15% ~ 60%;
Described iron compound is any one in ferric nitrate, iron oxide, tri-iron tetroxide.
7. a kind of red mud that utilizes according to claim 1 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that:
Comprise dry broken, mixing, extruded, solidification with activation, obtain finished product step.
8. a kind of red mud that utilizes according to claim 7 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that:
Described solidification and activation: solidification temperature is 120 ~ 180 DEG C, hardening time is 2 ~ 5 hours;
Activation temperature is 500 ~ 650 DEG C, and soak time is 6 ~ 8 hours.
9. a kind of red mud that utilizes according to claim 7 is for the method for raw material Kaolinite Preparation of Catalyst, it is characterized in that:
Described oven dry is broken: to dry to moisture lower than 5%, be crushed to particle diameter and be less than 1 millimeter;
Described extruded: shaping product is not adhered to one another, flawless.
10. the application of the catalyst utilizing red mud to prepare for raw material, it is characterized in that: adopt catalyst electrolysis containing organic waste water, the amount ratio of catalyst and waste water is 100 ~ 200g:1000mL, and control decomposition voltage is 12 ~ 20V, and control electrolysis time is 0.5 ~ 2.5h.
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