CN110818034A - Heterogeneous catalysis micro-electrolysis filler and preparation method thereof - Google Patents
Heterogeneous catalysis micro-electrolysis filler and preparation method thereof Download PDFInfo
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- CN110818034A CN110818034A CN201911152852.1A CN201911152852A CN110818034A CN 110818034 A CN110818034 A CN 110818034A CN 201911152852 A CN201911152852 A CN 201911152852A CN 110818034 A CN110818034 A CN 110818034A
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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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46176—Galvanic cells
Abstract
The invention discloses a heterogeneous catalysis micro-electrolysis filler and a preparation method thereof, wherein the filler is prepared by mixing, molding and sintering the following components in percentage by weight: anthracite 5-25%, alumina powder 8-20%, clay 13-26%, Wanxian stone 5-10%, binder 1-2%, reduced iron powder 30-50%, rare noble metal 0.5-2%, composite plastic agent 0.5-3%, wherein the composite plastic agent comprises northeast China ash clay, Veronica clay, and Nanguo kaolin; the preparation method comprises the following steps of grinding, dehydrating, vacuum forming, drying and sintering. Compared with the simple iron-carbon reaction, the method has higher reaction efficiency; the wet forming technology is adopted for the first time, so that the product has stronger plasticity before forming, the specific surface area of the product is greatly improved, the faster reaction speed is realized, and the use dosage is reduced; the use strength of the product is ensured, and the product is not easy to passivate and harden.
Description
Technical Field
The invention relates to the fields of ceramic chemical industry and water treatment, in particular to a heterogeneous catalysis micro-electrolysis filler and a preparation method thereof.
Background
Along with the stricter and stricter national environmental protection requirements, the environmental protection investment of governments and enterprises is higher and higher, and the micro-electrolysis process is used as a wastewater pretreatment and advanced treatment process and is known and used by more and more enterprises, on one hand, the components of various industrial wastewater are more and more complex, and the concentration of organic matters in the wastewater is higher and more due to the investment of various water-saving processes and equipment, on the other hand, compared with other conventional pretreatment processes, the micro-electrolysis has the advantage of higher cost performance. As a result of the reaction, iron is corroded to become ferrous ions into solution. Because iron ions have a coagulation effect, the iron ions attract particles with weak negative charges in pollutants in an opposite way, and form stable flocs for removal. However, various iron-carbon micro-electrolysis filler products commonly found on the market have various use defects: for example, the traditional dry pressing process causes the problems of low molding plasticity, uneven iron-carbon distribution, hardening due to too low strength, passivation due to surface oxidation, small specific surface area, poor use effect due to improper raw material selection and the like, and in addition, the catalyst is improved in cost and low in catalytic efficiency by adopting a dipping or electroplating mode when the catalyst is added.
Disclosure of Invention
In order to overcome the defects of the micro-electrolysis filler in the prior art, the invention provides the multi-phase catalytic micro-electrolysis filler and the preparation method thereof from raw materials, solves the problems of hardening, passivation, low efficiency and the like, and ensures that the product has high use effect, long-term stability and very wide application prospect.
The technical scheme adopted by the technical problem to be solved by the invention is as follows: a heterogeneous catalysis micro-electrolysis filler is prepared by mixing, molding and sintering the following components, wherein the content of each component is 5-25% of anthracite, 8-20% of alumina powder, 13-26% of clay, 5-10% of Wangxianshi, 1-2% of binder, 30-50% of reduced iron powder, 0.5-2% of rare noble metal and 0.5-3% of composite plastic agent, and the composite plastic agent comprises, by mass, Quillaia clay, Veronica clay and Nanguo kaolin.
Furthermore, the components comprise 20 percent of anthracite, 10 percent of alumina powder, 24 percent of clay, 5 percent of Wangxianshi, 1 percent of binder powder, 38 percent of reduced iron powder, 1 percent of rare noble metal and 1 percent of composite plastic agent, which are all mass percentages.
Further, the binder is one or more of water glass, starch and sodium humate.
Further, the rare and noble metal is one or more of silver, ruthenium, platinum, palladium and rhodium.
The invention also provides a preparation method of the heterogeneous catalysis micro-electrolysis filler as described in claim 1, which comprises the following steps:
A. grinding: firstly, mixing anthracite, alumina powder, clay, Wangxianshi, a binder, reduced iron powder, rare-earth metal and a composite plastic agent according to a proportion, wherein the content of each component is 5-25% of anthracite, 8-20% of alumina powder, 13-26% of clay, 5-10% of Wangxianshi, 1-2% of binder, 30-50% of reduced iron powder, 0.5-2% of rare-earth metal and 0.1-3% of composite plastic agent, and the proportion ratio of the Fraxinus rhynchophylla clay, the Veronica ball clay and the Nanguo kaolin in the composite plastic agent is 1-2: 1-3: 1, and the components are mass percentages; mixing, grinding in ball mill for 18-24 hr with water of the same volume to obtain slurry,
B. and (3) dehydrating: discharging the slurry obtained in the step A into a stirring pool, stirring for 2-4 hours, pumping into a mud press through a slurry pump for dehydration to obtain dry mud with the water content of less than 3 percent (low water content),
C. vacuum: b, the dry mud obtained in the step B is processed by a vacuum pug mill to ensure that the air in the mud is exhausted, the dry mud becomes a firmer mud cake,
D. molding: c, cutting the mud cake into a proper shape, forming into a rough blank by a press or a plodder,
E. drying: d, placing the rough blank obtained in the step D into a drying room to be dried for 16-24h to obtain a blank body;
F. and (3) sintering: and E, putting the blank dried in the step E into a sintering furnace, then raising the temperature of the furnace body to 1100-1200 ℃, carrying out oxygen-insulated sintering, and cooling to obtain the heterogeneous catalytic micro-electrolysis filler.
In the above, the anthracite has a fixed carbon content of more than or equal to 90%, a breakage rate of less than or equal to 0.35%, a porosity of 47% -53%, a wear rate of less than or equal to 0.68%, a specific gravity of 1.4-1.6, and a hydrochloric acid solubility of less than or equal to 0.98%;
the Wangxiangshi comes from the porcelain stone produced in Pukou town of carine Ling city, Hunan province, and comprises the following main chemical components (wt%): a1２O３，≥14.71； ＳｉO２，≤77.83；Ｆｅ２O3, ≤ 1.5 ； ＴｉO２≤，0.09； ＣａO ，≤0.18； ＭｇO ，≤0.02 ；Ｋ２O ，≤2.87； Ｎａ2O, less than or equal to 0.11; 3.4, the thermal stability of the filler during high-temperature sintering can be improved, and the shape of the sintered filler is regular and ordered;
the Fraxinus mandshurica clay is from Fraxinus mandshurica town of Sulan county, Jilin province, and comprises the following main chemical components (wt%): a1２O３，≥28 ； ＳｉO２，≤60；Ｆｅ２O3, ≤1.70 ； ＴｉO２，≤1.27； ＣａO ，≤0.40； ＭｇO ，≤0.40 ；Ｋ２O ，≤0.75； Ｎａ2O, less than or equal to 0.40; MnO less than or equal to 0.007, ignition loss of 11, plasticity index of 19.75%;
the Veronica clay is from Virol, south Ningshi, Guangxi province, and comprises the following main chemical components (wt%): a1２O３，≥26.17 ； ＳｉO２，≤58.67 ；Ｆｅ２O3, ≤0.60 ； ＴｉO２，≤1.92； ＣａO ，≤0.13； ＭｇO ，≤0.14 ； Ｋ２O，≤0.14； Ｎａ2O, less than or equal to 0.03; causticity reduction, 12.06, plasticity index, 21.12%;
the kaolin in the south pit is from the town of the south pit in Luxi county, Pingxi province and Pingxi city, and comprises the following main chemical components (wt%): a1２O３，≥32.70 ； ＳｉO２，≤52.30 ；Ｆｅ２O3, ≤1.12 ； ＴｉO２，≤0.14； ＣａO ，≤0.15； ＭｇO ，≤0.20 ； Ｋ２O ，≤0.34； Ｎａ2O, less than or equal to 0.03; 13.07 parts of burn loss, 20.72 percent of plasticity index;
the mechanism of the invention is as follows: firstly, a plurality of metals participate in the micro-electrolysis reaction, and the reaction rate is higher than that of a simple iron-carbon reaction; secondly, the defect process of traditional dry pressing and dipping or electroplating of rare and precious metal catalysts is changed, iron, various rare and precious metal catalysts and carbon are contained together to form a framework type iron-carbon structure through the means of grinding, dehydration, vacuum, molding, high-temperature sintering and the like by a wet process, the iron and the carbon are uniformly distributed and are always integrated, the separation of the iron and the carbon is not easy to occur like the combination of iron and carbon, the reaction of a primary battery is influenced, the resistance of the primary battery can be reduced by the integration of the iron and the carbon, the transfer efficiency of electrons is improved, the treatment efficiency is improved, the generation of passivation hardening can be avoided by the integration of the iron and the carbon, and the defect of dipping or electroplating of the rare and precious metal catalysts in the traditional process is overcome; and moreover, through a new wet process and raw materials and the addition of a compound plasticizer with a strict proportion, the plasticity indexes of the three raw materials of the compound plasticizer are all more than 15%, sodium sources such as sodium carbonate and sodium humate are matched, the product has very strong plasticity before forming by utilizing the particularity and high plasticity of the process, and can reach very many appearance shapes through various dies, so that the specific surface area of the product is greatly improved, the faster reaction speed is finally realized, and the use dosage is reduced.
Compared with the prior art, the invention has the advantages that: the reaction efficiency is higher than that of a pure iron-carbon reaction; the wet forming technology is adopted for the first time, so that the product has very strong plasticity before forming, and can reach very many appearance shapes through various dies, thereby greatly improving the specific surface area of the product, finally realizing faster reaction speed and reducing the using dosage; by controlling the sintering temperature, the product is in a semi-ceramic state, the use strength of the product is ensured, and the product is not easy to passivate and harden.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention is further described in detail below according to specific embodiments.
Example 1
A preparation method of a heterogeneous catalysis micro-electrolysis filler comprises the following steps:
A. grinding: firstly, anthracite, alumina powder, clay, Wangxianshi, a binder, reduced iron powder, rare-earth metals and a composite plastic agent are mixed according to a proportion, wherein the content of each component is 25 percent of anthracite, 20 percent of alumina powder, 13 percent of clay, 9 percent of Wangxianshi, 2 percent of binder (water glass), 30 percent of reduced iron powder, 0.5 percent of rare-earth metals (silver and ruthenium respectively account for half), and 0.5 percent of composite plastic agent, and the proportion ratio of the sharia hydrous clay, the Veronica officinalis clay and the Nanguo kaolin in the composite plastic agent is 2: 3: 1, which are all mass percentages; mixing, grinding in ball mill for 24 hr with water (reused water) to obtain slurry,
B. and (3) dehydrating: discharging the slurry obtained in the step A into a stirring pool, stirring for 2 hours, pumping into a mud press through a slurry pump, dehydrating to obtain dry mud with the water content of less than 3 percent,
C. vacuum: b, the dry mud obtained in the step B is processed by a vacuum pug mill to ensure that the air in the mud is exhausted, the dry mud becomes a firmer mud cake,
D. molding: c, cutting the mud cake into a proper shape, forming into a rough blank by a press or a plodder,
E. drying: d, placing the rough blank obtained in the step D into a drying room to be dried for 24 hours to obtain a blank body;
F. and (3) sintering: and E, putting the blank dried in the step E into a sintering furnace, then heating the furnace body to 1200 ℃, carrying out oxygen-insulated sintering, and cooling to obtain the multi-phase catalytic micro-electrolysis filler.
The method is characterized in that the production wastewater of a certain local coking enterprise is taken as an experimental object, the quality of the wastewater is mostly discharged after the procedures of oil removal, air stripping, A/O and the like, the quality of raw water is 254.9mg/l COD and 546.143mg/l BOD, the quality of water is dark brown, and the pH value is 7.6. The heterogeneous catalysis micro-electrolysis filler is added into a micro-electrolysis reactor, the pH of the wastewater is adjusted to about 3.5, and the wastewater is aerated and reacted for 2 hours + after flocculation and precipitation. After the reaction, the effluent is nearly transparent and light yellow, the pH of the effluent is 6.5, the water quality of the effluent is measured to be 34.5mg/l of COD and BOD561.132mg/l, the removal rate of the COD is 86.46%, and the chroma and the smell are obviously improved. Continuously running for 3 weeks, and observing, wherein the heterogeneous catalysis micro-electrolysis filler does not have the phenomenon of passivation hardening.
Example 2
A preparation method of a heterogeneous catalysis micro-electrolysis filler comprises the following steps:
A. grinding: firstly, mixing anthracite, alumina powder, clay, Wangxianshi, a binder, reduced iron powder, rare-earth metals and a composite plastic agent according to a proportion, wherein the content of each component is 10 percent of anthracite, 8 percent of alumina powder, 24 percent of clay, 5 percent of Wangxianshi, 1 percent of binder (half of starch and sodium humate), 50 percent of reduced iron powder, 1 percent of rare-earth metals (platinum, palladium and rhodium are in a proportion of 1:1: 1), and 1 percent of composite plastic agent, wherein the proportion of the Fraxinus rhynchophylla clay, the Veronica ball clay and the Nanguo kaolin in the composite plastic agent is in a proportion of 1:1: 1:1, and the components are all in percentage by mass; mixing, grinding in ball mill for 18 hr with water (tap water) to obtain slurry,
B. and (3) dehydrating: discharging the slurry obtained in the step A into a stirring pool, stirring for 4 hours, pumping into a mud press by a slurry pump for dehydration to obtain dry mud with the water content of less than 1 percent,
C. vacuum: b, the dry mud obtained in the step B is processed by a vacuum pug mill to ensure that the air in the mud is exhausted, the dry mud becomes a firmer mud cake,
D. molding: c, cutting the mud cake into a proper shape, forming into a rough blank by a press or a plodder,
E. drying: d, placing the rough blank obtained in the step D into a drying room to be dried for 16 hours to obtain a blank body;
F. and (3) sintering: and E, putting the blank dried in the step E into a sintering furnace, heating the furnace body to 1100 ℃, carrying out oxygen-insulated sintering, and cooling to obtain the multi-phase catalytic micro-electrolysis filler.
The waste water from a certain chemical plant is used as an experimental object, the water quality of raw water is COD 9321mg/l, the main components comprise acetaldehyde, paraldehyde, hydrobromic acid and trace metaldehyde, the waste water has pungent smell, the temperature is 25 ℃, and the pH is 3.5. The heterogeneous catalysis micro-electrolysis filler is added into a micro-electrolysis reactor, and air aeration reaction is carried out for 3 hours + after flocculation precipitation. The effluent after the reaction is transparent and has no obvious pungent smell, the pH value of the effluent is 6, the water quality of the effluent is 1957mg/l, the removal rate of COD is 79 percent, and the chroma and the smell are obviously improved. Continuously operating for 11 weeks, and observing, wherein the heterogeneous catalysis micro-electrolysis filler does not have the phenomenon of passivation hardening.
Claims (5)
1. A heterogeneous catalysis micro-electrolysis filler is characterized in that: the composite plastic material is prepared by mixing, molding and sintering the following components, wherein the components comprise, by mass, 5-25% of anthracite, 8-20% of alumina powder, 13-26% of clay, 5-10% of Wangxianshi, 1-2% of binder, 30-50% of reduced iron powder, 0.5-2% of rare noble metal and 0.5-3% of composite plastic agent, and the composite plastic agent comprises northeast China ash clay, Veronica clay and Nanguo kaolin.
2. The heterogeneously catalyzed microelectrolytic filler according to claim 1, wherein: the components comprise, by mass, 20% of anthracite, 10% of alumina powder, 24% of clay, 5% of Wangxiang stone, 1% of binder powder, 38% of reduced iron powder, 1% of rare noble metal and 1% of composite plastic agent.
3. The heterogeneously catalyzed microelectrolytic filler according to claim 1 or 2, wherein: the binder is one or more of water glass, starch and sodium humate.
4. The heterogeneously catalyzed microelectrolytic filler according to claim 1 or 2, wherein: the rare noble metal is one or more of silver, ruthenium, platinum, palladium and rhodium.
5. The method of claim 1 for preparing a heterogeneously catalyzed microelectrolytic filler, wherein: the method comprises the following steps:
A. grinding: firstly, mixing anthracite, alumina powder, clay, Wangxianshi, a binder, reduced iron powder, rare-earth metal and a composite plastic agent according to a proportion, wherein the content of each component is 5-25% of anthracite, 8-20% of alumina powder, 13-26% of clay, 5-10% of Wangxianshi, 1-2% of binder, 30-50% of reduced iron powder, 0.5-2% of rare-earth metal and 0.1-3% of composite plastic agent, and the proportion ratio of the Fraxinus rhynchophylla clay, the Veronica ball clay and the Nanguo kaolin in the composite plastic agent is 1-2: 1-3: 1, and the components are mass percentages; mixing, grinding in ball mill for 18-24 hr with water of the same volume to obtain slurry,
B. and (3) dehydrating: discharging the slurry obtained in the step A into a stirring pool, stirring for 2-4 hours, pumping into a mud press through a slurry pump for dehydration to obtain dry mud with the water content of less than 3 percent,
C. vacuum: b, the dry mud obtained in the step B is processed by a vacuum pug mill to ensure that the air in the mud is exhausted, the dry mud becomes a firmer mud cake,
D. molding: c, cutting the mud cake into a proper shape, forming into a rough blank by a press or a plodder,
E. drying: d, placing the rough blank obtained in the step D into a drying room to be dried for 16-24h to obtain a blank body;
F. and (3) sintering: and E, putting the blank dried in the step E into a sintering furnace, then raising the temperature of the furnace body to 1100-1200 ℃, carrying out oxygen-insulated sintering, and cooling to obtain the heterogeneous catalytic micro-electrolysis filler.
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