A high-efficiency anti-caking micro-electrolysis filler and its preparation method

By preparing high-efficiency anti-caking micro-electrolysis fillers, the problems of low reaction efficiency and easy caking of micro-electrolysis fillers were solved, and a stable sewage treatment effect was achieved.

CN115893597BActive Publication Date: 2025-09-05EAST CHINA ENGINEERING SCIENCE AND TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202211661363.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-23
Publication Date
2025-09-05
Estimated Expiration
2042-12-23

AI Technical Summary

Technical Problem

Existing micro-electrolysis fillers have low reaction efficiency and are prone to compaction, which leads to obstruction of electron transfer in the reactor and affects the sewage treatment effect.

Method used

A specific proportion of iron powder, carbon powder, buffer material, adhesive and catalyst are mixed and sintered at high temperature to prepare ellipsoidal particle filler. Iron powder of different mesh sizes is used to form the skeleton, the buffer material reduces the melting temperature, the catalyst enhances the reaction activity, and the adhesive ensures stable molding.

Benefits of technology

It improves the efficiency of micro-electrolysis reaction, avoids the phenomenon of caking, ensures the stable performance of the filler during the water treatment process, and improves the sewage treatment effect.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a high-efficiency anti-caking micro-electrolysis filler and a preparation method thereof. The filler comprises, in parts by mass, 35-50 parts of iron powder, 20-30 parts of carbon powder, 30-40 parts of buffer material, 2-5 parts of adhesive, 8-10 parts of catalyst, and 20-30 parts of water; the buffer material comprises, in parts by mass, 12-18 parts of bentonite, 8-15 parts of heavy calcium carbonate, and 5-15 parts of magnesium aluminum silicate; the adhesive comprises, in parts by mass, 1-3 parts of white dextrin and 1-3 parts of sodium silicate; the catalyst comprises, in parts by mass, 2-5 parts of chromium ore powder, 3-8 parts of titanium oxide powder, and 3-8 parts of brass powder. The iron powder, carbon powder, buffer material, and catalyst are preliminarily mixed, and then the adhesive and water are added to the preliminarily mixed material and mixed again. The morphology of the mixed material during the mixing process is controlled by reaction exotherm to ensure that the mixed material is uniform. The mixed material is placed in a mold to form ellipsoidal particles, and the micro-electrolysis filler is obtained by naturally air-drying and heating and drying with blast drying, followed by high-temperature sintering and cooling. The filler has no compaction inside or outside, has stable and excellent performance, is easy to form into balls, and has certain cold strength.
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Description

Technical Field

[0001] The invention belongs to the technical field of wastewater treatment materials, and particularly relates to a high-efficiency anti-caking micro-electrolysis filler and a preparation method thereof. Background Art

[0002] Microelectrolysis technology utilizes the potential difference between iron and carbon elements in solution to form a primary cell, which causes the long chains of macromolecular organic matter or aromatic hydrocarbon rings to open and break, thereby improving the biodegradability of wastewater. It is also highly effective in destroying heavy metal complexes and replacing heavy metal ions. The mechanism of action of microelectrolysis primarily involves the microbattery principle, redox reactions, flocculation, adsorption, and coprecipitation. The redox reactions between the generated ferrous ions, reduced hydrogen, and reactive oxygen species and wastewater pollutants lead to degradation, adsorption, flocculation, and precipitation, resulting in the removal of pollutants. While iron-carbon micro-electrolysis technology is highly efficient, economical, and practical, it suffers from the following limitations: 1) Reaction efficiency is relatively low. Compared to other physicochemical treatment technologies, micro-electrolysis degradation efficiency is lower, with most reactions taking longer than two hours. 2) Iron-carbon micro-electrolysis materials are prone to caking, which hinders electron transfer between the iron and carbon. As caking progresses, this can eventually lead to short circuits and agglomeration within the micro-electrolysis reactor, significantly reducing the efficiency of the micro-electrolysis reaction until it fails and becomes ineffective in the long-term wastewater treatment process. Therefore, a highly efficient and caking-resistant filler is urgently needed in the industrial park wastewater treatment sector. Summary of the Invention

[0003] The purpose of the present invention is to provide a high-efficiency and anti-caking micro-electrolytic filler and a preparation method thereof, so as to solve the technical problems of low reaction efficiency, easy caking and poor durability of the current micro-electrolytic filler.

[0004] To achieve this purpose, the present invention adopts the following technical solutions:

[0005] A high-efficiency anti-caking micro-electrolytic filler, the components of which are calculated by mass:

[0006] 35-50 parts iron powder, 20-30 parts carbon powder, 30-40 parts buffer material, 2-5 parts adhesive, 8-10 parts catalyst, 20-30 parts water;

[0007] The buffer material is composed of 12 to 18 parts of bentonite, 8 to 15 parts of heavy calcium carbonate, and 5 to 15 parts of magnesium aluminum silicate in parts by mass;

[0008] The adhesive is composed of 1 to 3 parts of white dextrin and 1 to 3 parts of sodium silicate in parts by mass;

[0009] The catalyst is composed of 2 to 5 parts of chromium ore powder, 3 to 8 parts of titanium oxide powder, and 3 to 8 parts of brass powder in parts by mass.

[0010] Furthermore, the configuration of the buffer material includes the following steps: taking parts by weight of bentonite, heavy calcium carbonate, and magnesium aluminum silicate and mixing them at a stirring speed of 60-80 rpm and a stirring time of 10-15 minutes.

[0011] Furthermore, the configuration of the catalyst includes the following steps: mixing chromium ore powder, titanium oxide powder, and brass powder in parts by mass, stirring at a speed of 60-80 rpm for 10-15 minutes.

[0012] Furthermore, the preparation of the adhesive includes the following steps: taking parts by weight of white dextrin and sodium silicate, mixing and stirring at a speed of 50-60 rpm for 8-10 minutes.

[0013] Furthermore, the present invention also discloses a method for preparing the above-mentioned high-efficiency anti-caking micro-electrolytic filler, comprising the following steps:

[0014] Take 12-18 parts of bentonite, 8-15 parts of heavy calcium carbonate, and 5-15 parts of magnesium aluminum silicate to prepare the buffer material;

[0015] Take 2-5 parts of chromium ore powder, 3-8 parts of titanium oxide powder, and 2-8 parts of brass powder to prepare the catalyst by mass;

[0016] Take 1-3 parts of white dextrin and 1-3 parts of sodium silicate to prepare the adhesive;

[0017] Take parts by weight of iron powder, carbon powder, buffer material, and catalyst and mix them preliminarily. Then add parts by weight of adhesive to the mixture and mix again. After the powders are evenly mixed, add 10-15 parts by weight of water and stir until the mixed wet material is evenly moistened and becomes slightly wet.

[0018] Preferably, the weight percentage of the iron powder is 25-40 parts of 40-60 mesh iron powder and 10-20 parts of 200 mesh iron powder;

[0019] After the wet material is aged and cooled for 4 to 6 hours, 10 to 15 parts by mass of water are added again for mixing;

[0020] The secondary water-wetted material is slowly introduced into the mold, and ellipsoidal particles are formed after pressing and demoulding;

[0021] The initial mixing is carried out by stirring, with a stirring speed of 60-80 rpm and a stirring time of 20-40 min;

[0022] During the water addition process after re-mixing, the mixture will release heat to 50~70℃, so water needs to be added intermittently. The stirring speed is 40~60rpm and the stirring time is 10~30min.

[0023] After demolding, the ellipsoidal fillers are naturally air-dried for more than 24 hours and then put into the drying oven in batches for drying at a temperature of 80-100°C for more than 8 hours.

[0024] The dried filler is loaded into the crucible, the gap between the filler and the crucible is filled with coal powder, and the top of the filler is covered with 1-3 mm thick cordierite powder;

[0025] The crucible is placed in a muffle furnace or a tunnel furnace for high-temperature sintering, and after natural cooling, a high-efficiency anti-caking micro-electrolytic filler is obtained;

[0026] The high temperature sintering steps are as follows:

[0027] When the temperature in the furnace is below 300℃, the heating rate should be controlled to be no more than 5℃ / min;

[0028] When the temperature in the furnace is between 300 and 800°C, control the heating rate to no more than 3°C / min; and when the temperature rises to 800°C, keep it warm for 2 to 4 hours;

[0029] When the temperature in the furnace is between 800 and 1150°C, control the heating rate to no more than 2°C / min, and when the temperature reaches 1150°C, keep it warm for 4 to 8 hours;

[0030] After completing the above procedures, when the temperature in the furnace drops below 100°C, take out the crucible, remove the coal powder, and allow the sintered filler to dry naturally and cool to room temperature to obtain the micro-electrolysis filler.

[0031] Compared with the prior art, the beneficial effects of the present invention are as follows: iron powder, carbon powder, buffer material, and catalyst in parts by mass within the scope of the present invention are preliminarily mixed, and then parts by mass of adhesive and water are added to the preliminarily mixed material and mixed again, and the morphology of the mixture during the mixing process is controlled by the reaction exotherm to ensure that the mixture is uniform; the mixture is placed in a mold to form ellipsoidal particles, and micro-electrolytic filler is obtained through high-temperature sintering and cooling steps after natural air drying and heated blower drying. The binder has a good effect, making the mixture easy to form into balls and having a certain cold strength, ensuring that the filler will not break before and during sintering; iron powder of different mesh sizes can form a skeleton of the filler after the mixture is balled, ensuring the uniformity and stability of the filler; the addition of buffer material not only reduces the melting temperature of the micro-electrolysis filler, but also maintains the micro-electrolysis reaction on a stable reaction curve; copper, chromium, titanium, etc. in the catalyst can enhance the activity of the micro-electrolysis reaction and ensure the hardness of the micro-electrolysis filler, which not only prevents the micro-electrolysis reaction from passivation, polarization and other phenomena with the extension of reaction time, but also ensures that the filler preferentially degrades pollutants on the surface of the reaction filler during water treatment, and improves the efficiency of the micro-electrolysis reaction by consuming and peeling off the filler layer by layer. There is no compaction inside and outside the filler, and the performance is stable and excellent. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] The present invention will be further described below with reference to the accompanying drawings.

[0033] Figure 1 Flow chart of the preparation method of Example 1 of the present invention;

[0034] Figure 2 Flow chart of the preparation method of Example 2 of the present invention;

[0035] Figure 3 Flow chart of the preparation method steps of Comparative Example 1 of the present invention;

[0036] Figure 4 This is a flow chart of the preparation method steps of Comparative Example 2 of the present invention;

[0037] Figure 5 This is a raw material diagram of the high-efficiency anti-caking micro-electrolytic filler prepared in Example 1 of the present invention;

[0038] Figure 6 This is a finished product of the high-efficiency anti-caking micro-electrolytic filler prepared in Example 1;

[0039] Figure 7 This is the raw material diagram of the high-efficiency anti-caking micro-electrolysis filler prepared in Example 2;

[0040] Figure 8 This is the finished product of the high-efficiency anti-caking micro-electrolytic filler prepared in Example 2;

[0041] Figure 9 This is the raw material diagram of the high-efficiency anti-caking micro-electrolysis filler prepared in Comparative Example 1;

[0042] Figure 10 This is a sample of a high-efficiency anti-caking micro-electrolysis filler prepared after 90 days of reaction in Comparative Example 2;

[0043] Figure 11 This is the SEM image of Example 1 of the present invention;

[0044] Figure 12 This is the SEM image of Example 2 of the present invention. DETAILED DESCRIPTION

[0045] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention and the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments.

[0046] Example 1:

[0047] See also Figure 1 The present invention provides a method for preparing a high-efficiency anti-caking micro-electrolysis filler, the steps of which are as follows:

[0048] S1: Prepare 30 parts of buffer material;

[0049] S2: Prepare 8 parts of catalyst;

[0050] S3: prepare 2 parts of adhesive;

[0051] S4: Mix 30 parts of 40-mesh iron powder, 15 parts of 200-mesh iron powder, 20 parts of carbon powder, 30 parts of buffer material, and 8 parts of catalyst, stirring at 60 rpm for 30 minutes, then add 2 parts of adhesive to the initial mixture and continue mixing. At the same time, add 25 parts of water intermittently, stirring at 40 rpm for 10 minutes, and maintain the temperature of the mixture at around 50°C (add water intermittently to control the temperature) to form a mixture with a certain viscosity;

[0052] S5: After the mixed material is aged and cooled, it is introduced into a mold to form ellipsoidal particles;

[0053] S6: Place the obtained ellipsoidal particles in a cool and ventilated place to dry naturally for 24 hours, and then put them into an oven for drying at 80°C for 14 hours;

[0054] S7: After the ellipsoidal particles are cooled naturally, they are loaded into a crucible. The gap between the filler and the crucible is filled with coal powder, and the top of the filler is covered with 3 mm thick cordierite powder.

[0055] S8: The crucible loaded with filler is sent into a muffle furnace for high-temperature sintering. During sintering, when the temperature in the furnace is below 300°C, the heating rate is controlled to be 3°C / min, and when the temperature in the furnace is between 300 and 800°C, the heating rate is controlled to be 2°C / min; and when the temperature rises to 800°C, it is kept warm for 2 hours. When the temperature in the furnace is between 800 and 1150°C, the heating rate is controlled to be 1°C / min, and when the temperature rises to 1150 degrees Celsius, it is kept warm for 4 hours. When the temperature in the furnace drops below 100°C, the crucible is taken out, the coal powder is removed, and the sintered filler is naturally air-dried and cooled to obtain a micro-electrolysis filler.

[0056] In this embodiment, 2 parts of an adhesive are prepared by mixing 1 part of white dextrin and 1 part of sodium silicate; then 3 parts of chromium ore powder, 3 parts of titanium oxide powder, and 2 parts of brass powder are mixed to form a catalyst; then 15 parts of bentonite, 10 parts of heavy calcium carbonate, and 5 parts of magnesium aluminum silicate are mixed to form 30 parts of a buffer material; then, carbon powder, catalyst, buffer material, and iron powder of different mesh sizes are mixed to form a primary mixture, and then the adhesive and parts by mass of water are added and continued to be stirred and mixed, and the exothermic reaction in the process is used to ensure the uniformity of the raw materials, ensure the uniformity of the prepared micro-electrolytic filler, and allow the micro-electrolytic filler to remain stable in water after molding. The addition of white dextrin and sodium silicate facilitates the stable molding of the mixture on the one hand, and on the other hand, both materials will not bring about side reactions after high-temperature sintering; the presence of the buffer material ensures the stable dissolution of the anode of the micro-electrolysis reaction, allowing a certain amount of ions to exist in the sewage, thereby improving the efficiency of the micro-electrolysis reaction; iron powders of different mesh sizes can form a uniform and strong skeleton after the filler is balled, allowing the filler to achieve a layer-by-layer peeling effect; the addition of the catalyst can greatly enhance the strength of the micro-electrolysis filler and further improve the efficiency of the micro-electrolysis reaction during sewage treatment. The operation of first air-drying and then drying the filler before high-temperature sintering can avoid the problem of high moisture content of the filler destroying the filler structure when the temperature is raised in the muffle furnace; under the action of the buffer material, the melting temperature of the filler in the present invention is reduced, and after high-temperature sintering and cooling, no compaction, perforation, etc. will occur on the surface and inside of the filler, and it has the advantages of high activity, excellent treatment effect, and no passivation. Filling coal powder between the crucible and the filler, and between the fillers, can ensure that the micro-electrolysis filler is in a reducing atmosphere during sintering, thereby ensuring the stability of the content of effective ingredients in the obtained filler and effectively improving the quality and efficiency of the obtained micro-electrolysis filler.

[0057] Example 2:

[0058] See also Figure 2 The present invention provides a method for preparing a high-efficiency anti-caking micro-electrolysis filler, the steps of which are as follows:

[0059] S1: Prepare 35 parts of buffer material;

[0060] S2: prepare 10 parts of catalyst;

[0061] S3: Prepare 5 parts of adhesive;

[0062] S4: Mix 25 parts of 40-mesh iron powder, 15 parts of 200-mesh iron powder, 20 parts of carbon powder, 25 parts of buffer material, 10 parts of catalyst, and 15 parts of water at 50 rpm for 30 minutes. After cooling and aging the mixture for 2 hours, add 5 parts of adhesive and continue adding 12 parts of water, stirring again until it is slightly damp.

[0063] S5: Pressing and demoulding the mixed slightly wet material to form ellipsoidal particles;

[0064] S6: Place the ellipsoidal particles in a cool and ventilated place and dry for 26 hours, then place them in a blast oven for further drying at 90°C for 12 hours.

[0065] S7: After the ellipsoidal particles are cooled, they are placed in a crucible. The gaps between the particles and between the particles and the crucible are filled with coal powder, and the top of the filler is covered with 2 mm thick cordierite powder;

[0066] S8: Place the crucible loaded with filler into a muffle furnace for sintering. During sintering, when the temperature in the furnace is below 800°C, control the heating rate to 2°C / min; and when the temperature rises to 800°C, keep it warm for 2 hours. When the temperature in the furnace is between 800 and 1150°C, control the heating rate to 1°C / min, and when the temperature rises to 1150 degrees Celsius, keep it warm for 6 hours. When the temperature in the furnace drops below 100°C, take out the crucible, remove the coal powder, and naturally air-dry and cool the sintered filler to obtain micro-electrolysis filler.

[0067] In this embodiment, 3 parts of white dextrin and 2 parts of sodium silicate are mixed to prepare 5 parts of adhesive, and then 2 parts of chromium ore powder, 2 parts of titanium oxide powder, and 4 parts of brass powder are mixed to prepare a catalyst; then 12 parts of bentonite, 8 parts of heavy calcium carbonate, and 5 parts of magnesium aluminum silicate are mixed to form 25 parts of buffer material; then water, carbon powder, catalyst, buffer material, and iron powder of different mesh sizes are added and mixed, and the natural heat release of this process is used to ensure the uniformity of the mixture. Then, after the mixture is aged and cooled, 5 parts of adhesive and 12 parts of water are continued to be added to ensure the smooth completion of the subsequent pressing and demolding processes. The binder mainly composed of white dextrin is decomposed at high temperature, ensuring that the filler after high-temperature sintering will not bring new pollutants to the water body; the presence of calcium and magnesium ions in the buffer material ensures the stable dissolution of the anode of the micro-electrolysis reaction, allowing a certain amount of anions and cations to exist in the sewage, thereby improving the mass transfer efficiency of the micro-electrolysis reaction; iron powders of different mesh sizes can form a uniform and strong skeleton after the filler is balled, allowing the filler to achieve the effect of layer-by-layer peeling; the addition of catalysts can greatly enhance the strength of the micro-electrolysis filler and further improve the efficiency of the micro-electrolysis reaction during sewage treatment. The operation of first air-drying and then drying the filler before high-temperature sintering can avoid the problem of excessive moisture content of the filler destroying the internal structure of the filler when the temperature is raised in the muffle furnace; under the action of the buffer material, the melting temperature of the filler in the present invention is reduced, and after high-temperature sintering and cooling, the surface and interior of the filler will not be hardened or perforated, and it has the advantages of high activity, excellent treatment effect, and no passivation. Filling coal powder between the crucible and the filler, and between the fillers, can ensure that the micro-electrolysis filler is in a reducing atmosphere during sintering, thereby ensuring the stability of the content of effective ingredients in the obtained filler and effectively improving the quality and efficiency of the obtained micro-electrolysis filler.

[0068] Comparative Example 1:

[0069] In order to fully demonstrate the beneficial effects of the present invention, the preparation of Comparative Example 1 was carried out. Figure 3 , the steps are as follows.

[0070] S1: Prepare 30 parts of buffer material;

[0071] S2: prepare 10 parts of catalyst;

[0072] S3: 30 parts of 40-mesh iron powder, 15 parts of 200-mesh iron powder, 20 parts of carbon powder, 30 parts of buffer material, and 10 parts of catalyst were mixed at a stirring speed of 60 rpm for 30 minutes. At the same time, 25 parts of water were added intermittently at a stirring speed of 40 rpm for 10 minutes. The temperature of the mixture was maintained at about 50°C (water was added intermittently to control the temperature) to form a mixture.

[0073] S4: After the mixture is cooled, it is introduced into a mold and pressurized to form ellipsoidal particles;

[0074] S5: Place the obtained ellipsoidal particles in a cool and ventilated place to dry naturally for 24 hours, and then put them into an oven for drying at 80°C for 14 hours.

[0075] S6: After the ellipsoidal particles are cooled naturally, they are loaded into a crucible. The gap between the filler and the crucible is filled with coal powder, and the top of the filler is covered with 3 mm thick cordierite powder;

[0076] S7: The crucible loaded with the filler is sent into a muffle furnace for high-temperature sintering. During sintering, when the temperature in the furnace is below 300°C, the heating rate is controlled to be 3°C / min, and when the temperature in the furnace is between 300 and 800°C, the heating rate is controlled to be 2°C / min; and when the temperature rises to 800°C, it is kept warm for 2 hours. When the temperature in the furnace is between 800 and 1150°C, the heating rate is controlled to be 1°C / min, and when the temperature rises to 1150 degrees Celsius, it is kept warm for 4 hours. When the temperature in the furnace drops below 100°C, the crucible is taken out, the coal powder is removed, and the sintered filler is naturally air-dried and cooled to obtain the filler.

[0077] In this comparative example 1, no binder was added, and the micro-electrolysis pellets were made only by the material and water themselves, and then sintered. During the operation, it was found that the micro-electrolysis pellets made by this method had poor cold strength, and the breakage rate of the filler during handling and transportation reached more than 22%, which seriously restricted the reduction of the final pellet manufacturing cost. The physical properties of this filler are compared with those of Example 1 and Example 2 in Attached Table 1, and the breakage of this filler is detailed in Attached Table 2. Figure 5 .

[0078] Comparative Example 2:

[0079] In order to fully demonstrate the beneficial effects of the present invention, the preparation of Comparative Example 2 was carried out. Figure 4, the steps are as follows.

[0080] S1: Prepare 5 portions of buffer material;

[0081] S2: prepare 3 parts of catalyst;

[0082] S3: prepare 2 parts of adhesive;

[0083] S4: Mix 50 parts of 40-mesh iron powder, 25 parts of 200-mesh iron powder, 20 parts of carbon powder, 5 parts of buffer material, and 3 parts of catalyst at a stirring speed of 60 rpm for 30 minutes. Then, add 2 parts of adhesive to the primary mixture and continue mixing. At the same time, add 25 parts of water intermittently at a stirring speed of 40 rpm for 10 minutes. Maintain the temperature of the mixture at around 50°C (add water intermittently to control the temperature) to form a mixture with a certain viscosity.

[0084] S5: After the mixed material is aged and cooled, it is introduced into a mold to form ellipsoidal particles;

[0085] S6: Place the obtained ellipsoidal particles in a cool and ventilated place to dry naturally for 24 hours, and then put them into an oven for drying at 80°C for 14 hours;

[0086] S7: After the ellipsoidal particles are cooled naturally, they are loaded into a crucible. The gap between the filler and the crucible is filled with coal powder, and the top of the filler is covered with 3 mm thick cordierite powder.

[0087] S8: The crucible loaded with filler is sent into a muffle furnace for high-temperature sintering. During sintering, when the temperature in the furnace is below 300°C, the heating rate is controlled to be 3°C / min, and when the temperature in the furnace is between 300 and 800°C, the heating rate is controlled to be 2°C / min; and when the temperature rises to 800°C, it is kept warm for 2 hours. When the temperature in the furnace is between 800 and 1150°C, the heating rate is controlled to be 1°C / min, and when the temperature rises to 1150 degrees Celsius, it is kept warm for 4 hours. When the temperature in the furnace drops below 100°C, the crucible is taken out, the coal powder is removed, and the sintered filler is naturally air-dried and cooled to obtain a micro-electrolysis filler.

[0088] In this comparative example 2, only 5 parts of buffer material were added, which is far less than the 30-40 parts required by the present invention, and the iron content in the filler was correspondingly increased. During the whole process of filler mixing, ball pressing and sintering, the filler yield decreased and the strength increased. During the laboratory test, it was found that the filler prepared in comparative example 2 had a strong effect on the degradation of pollutants in the initial stage of the reaction, but the attenuation effect was obvious. The amount of iron mud covering the surface of the filler was large, which restricted its long-term stable operation. Figure 7 .

[0089] The performance of the micro-electrolysis fillers of Example 1, Example 2 and Comparative Example 1 of the present invention was tested, and the results are shown in Table 1 below.

[0090] Table 1 is a performance table of Example 1, Example 2 and Comparative Example 1.

[0091] Raw material crushing strength (before sintering) (N) Clinker crushing strength (after sintering) (N) Specific surface area (m² / g) Average pore size (nm) Example 1 563N 6319N 12.6684 9.7552 Example 2 427N 6227N 14.1453 8.6647 Comparative Example 1 96N 3874N 16.2267 6.3956

[0092] Through the data, we found that the micro-electrolytic filler obtained by the present invention is easy to form into balls, has certain cold strength, high hardness, and stable and excellent performance.

Claims

1. A high-efficiency anti-caking micro-electrolysis filler, characterized in that: Its ingredients in parts by mass include: 35-50 parts iron powder, 20-30 parts carbon powder, 30-40 parts buffer material, 2-5 parts adhesive, 8-10 parts catalyst, 20-30 parts water; The buffer material is composed of 12 to 18 parts of bentonite, 8 to 15 parts of heavy calcium carbonate, and 5 to 15 parts of magnesium aluminum silicate in parts by mass; The adhesive is composed of 1 to 3 parts of white dextrin and 1 to 3 parts of sodium silicate in parts by mass; The catalyst is composed of 2 to 5 parts of chromium ore powder, 3 to 8 parts of titanium oxide powder, and 3 to 8 parts of brass powder in parts by mass; The preparation method of the high-efficiency anti-caking micro-electrolysis filler comprises the following steps: (1) configuring the buffer material; (2) preparing the catalyst; (3) preparing the adhesive; (4) Preliminary mixing of the iron powder, carbon powder, buffer material, and catalyst in the above-mentioned parts by weight is performed, and then the above-mentioned parts by weight of binder are added to the mixture and mixed again. After the powders are evenly mixed, 10 to 15 parts by weight of water are intermittently added to mix until the moisture content of the mixed wet material is uniform. After the wet material is aged and cooled, 10 to 15 parts by weight of water are added again to mix; (5) The secondary water-wetted material is slowly introduced into the mold, and ellipsoidal particles are formed after pressing and demolding; (6) The ellipsoidal particles after demolding are dried naturally and then air-dried until the weight no longer changes; (7) The dried ellipsoidal particles are placed in a muffle furnace for sintering, and the filler is obtained after cooling to room temperature.

2. The high-efficiency anti-caking micro-electrolysis filler according to claim 1, characterized in that: The preparation of the buffer material comprises the following steps: taking parts by weight of bentonite, heavy calcium carbonate, and magnesium aluminum silicate and mixing them, stirring at a speed of 60-80 rpm and for 10-15 minutes.

3. The high-efficiency anti-caking micro-electrolysis filler according to claim 1, characterized in that: The catalyst is prepared by mixing chromium ore powder, titanium oxide powder and brass powder in parts by weight, stirring at a speed of 60-80 rpm for 10-15 minutes.

4. The high-efficiency anti-caking micro-electrolysis filler according to claim 1, characterized in that: The preparation of the adhesive comprises the following steps: taking parts by weight of white dextrin and sodium silicate, mixing and stirring at a speed of 50-60 rpm for 8-10 minutes.

5. A method for preparing a high-efficiency anti-caking micro-electrolytic filler according to claim 1, characterized in that: The steps include: (1) configuring the buffer material; (2) preparing the catalyst; (3) preparing the adhesive; (4) Preliminary mixing of the iron powder, carbon powder, buffer material, and catalyst in the above-mentioned parts by weight is performed, and then the above-mentioned parts by weight of binder are added to the mixture and mixed again. After the powders are evenly mixed, 10 to 15 parts by weight of water are intermittently added to mix until the moisture content of the mixed wet material is uniform. After the wet material is aged and cooled, 10 to 15 parts by weight of water are added again to mix; (5) The secondary water-wetted material is slowly introduced into the mold, and ellipsoidal particles are formed after pressing and demolding; (6) The ellipsoidal particles after demolding are dried naturally and then air-dried until the weight no longer changes; (7) The dried ellipsoidal particles are placed in a muffle furnace for sintering, and the filler is obtained after cooling to room temperature.

6. The method for preparing a high-efficiency anti-caking micro-electrolytic filler according to claim 5, characterized in that: In the step (4), the mass proportions of 40-mesh iron powder and 200-mesh iron powder in the 35-50 parts of iron powder are 25-40 parts and 10-20 parts respectively; during the preliminary mixing, the stirring speed is 60-80 rpm and the stirring time is 20-40 min; When mixing again, the mixing speed is 40~60rpm and the stirring time is 10~30min; The aging cooling time after the first addition of water and mixing is 4 to 6 hours.

7. The method for preparing a high-efficiency anti-caking micro-electrolytic filler according to claim 5, characterized in that: In the step (6), For natural air drying, choose a cool and ventilated place and the air drying time should be more than 24 hours. The blast drying temperature is 80~100℃ and the drying time is more than 8 hours.

8. The method for preparing a high-efficiency anti-caking micro-electrolytic filler according to claim 5, characterized in that: In step (7): When the temperature in the furnace is below 300℃, the heating rate should be controlled to be no more than 5℃ / min; When the temperature in the furnace is between 300 and 800°C, control the heating rate to no more than 3°C / min; and when the temperature rises to 800°C, keep it warm for 2 to 4 hours; When the temperature in the furnace is between 800 and 1150°C, the heating rate is controlled to be no more than 2°C / min, and when the temperature rises to 1150 degrees Celsius, it is kept warm for 4 to 8 hours.

9. The method for preparing a high-efficiency anti-caking micro-electrolytic filler according to claim 5, characterized in that: In the step (7): after the temperature in the muffle furnace drops to 100° C., the muffle furnace is taken out and naturally air-dried and cooled to room temperature to obtain the micro-electrolysis filler.

Citation Information

Patent Citations

  • Composite micro-electrolysis filler as well as preparation method and application thereof

    CN105110427A

  • Phosphorus removal ceramsite as well as preparation method and application thereof

    CN114409029A