WO2012055257A1 - Bioceramic with selective adsorption and digestion effects and production method thereof - Google Patents

Abstract

A bioceramic with selective adsorption and digestion effects and production method thereof are provided. The bioceramic is mainly produced by the following raw materials, by weight: 30-70 parts of sludge, 2-15 parts of kaolin, 1-5 parts of metal M or oxide of metal M. The bioceramic has a structure of amorphous Si-C-M and a specific surface area of 400-500m²/g. The method comprises using sludge from paper-making wastewater, food industry and wastewater treatment plant and kaolin as raw materials, adding crop husk, oxygen-free sintering and microwave activating the porous bioceramic particles or powders to obtain the bioceramic. The product obtained has the function of adsorbing benzene, phenol, multiple hydrocarbons, dimethyl sulfide and thioether malodorous substance, and can be used for air filtration. The bioceramic can provide effective carbon source and mineral for microorganism, and can be used as biological media filter material for air filtration and wastewater treatment. The bioceramic also can adsorb the phosphate ion in water and remove the oxygen rich components in water.

Description

 Biological pottery with selective adsorption digestion function and preparation method thereof

 Technical field

 The invention belongs to the technical field of air filtration new materials and wastewater treatment, and particularly relates to a biological ceramic with selective adsorption digestion function and a preparation method thereof.

 Background technique

 A large amount of waste sludge is produced after the paper industry wastewater, the food industry and sewage treatment plants, treatment facilities and other wastewaters are biologically treated. Because sludge contains a large amount of harmful substances such as bacterial microorganisms, heavy metals, and odors, the harmless treatment and reuse of sludge has become a worldwide technical problem. For example, harmful substances such as pathogenic bacteria and heavy metals in sludge make it difficult to use as a fertilizer. The traditional treatment method is dehydration, drying, and landfill landfill, but landfills occupy a large number of sites. Another treatment is to use aerobic incineration to reduce sludge volume, but harmful substances such as dioxins are polluted during the incineration process.

 The existing adsorbent materials are mainly large-surface mediums such as activated carbon and carbon fiber materials, which are used for adsorbing air and phenolic substances in water. However, the production of activated carbon, including the production of shells and coals, requires a large amount of fossil fuels. It also produces dust pollution, which is costly and expensive. Moreover, these activated carbons and fibers only physically adsorb to the phenols and do not have the digestion function of the subsequent biological medium. In addition, porous rock, slag or plastic media, porous rock, slag or plastic media are widely used as filter media or bacterial attachment growth media, but the media does not have adsorption function for benzene, phenol, polyhydrocarbons, dimethyl sulfide. .

 In the prior art, the heating or incineration of the sludge is mostly carried out in an aerobic environment, the carbon source is lost during the firing process, ceramsite or ash, ash and slag are formed, and a large amount of odorous exhaust gas is generated, and the generated material does not adsorb malodor and Decolorization function. In addition, the prior art has not found a new material in which a certain crop skin is added to the formulation, and the adsorption function of the activated carbon and the digestion function of the biological medium are combined.

 Summary of the invention

 SUMMARY OF THE INVENTION The object of the present invention is to overcome the above problems in the prior art and to provide a bioceramic having a selective adsorption digestion function and a preparation method thereof.

 In order to achieve the above object, the technical solution adopted by the present invention is as follows:

 The bioceramic having the selective adsorption digestion function of the present invention is mainly made of the following raw materials by weight: sludge 30-70, kaolin 2-15, metal or metal oxide 1-5. The selective bioceramic has an amorphous Si-C-M structure having a specific surface area of 400-500 m2/g.

The sludge is activated sludge, and the sludge has a microbial content of 70%. The bioceramic having the selective adsorption digestion function of the present invention is preferably made of the following raw materials by weight: sludge

30-70, kaolin 2-15, metal or metal oxide 1-5, 糠 8-12.

 The bioceramic having the selective adsorption digestion function of the present invention is preferably made of the following raw materials by weight: sludge 30-70, kaolin 2-15, metal M or oxide of metal M 1-5, 糠8 -12, calcium carbonate 3-5.

 The preparation method of the bioceramic having the selective adsorption digestion function of the invention is carried out according to the following steps:

(1) mixing raw materials of biological ceramics according to the above formula, forming into a shape by extrusion or disk granulation, and drying and molding;

 (2) The preform obtained in the step (1) is placed in a high-temperature oven under vacuum or fired under nitrogen atmosphere, and the oven temperature is raised to 295-305 ° C at a temperature increase rate of 90-110 ° C / h. 1~2 hours, the volatile odor gas generated here is burned into the gas furnace, and the heat is used for self-insulation;

 (3) The oven temperature is raised to 740-76 CTC at a temperature increase rate of 90-110 ° C / h for 2-3 hours; then cooled to room temperature at a cooling rate of 150-200 ° C / h to obtain a biological ceramic medium;

 (4) The bio-ceramic medium obtained in the step (3) is added to the water vapor for 1-1.5 hours, and activated by an industrial microwave oven for 0.5-1 hour to obtain the bioceramic of the present invention.

 When vacuum sintering is used in step (2), the vacuum in the high temperature oven is -0.08-0.09 Mpa.

 In the step (2), when nitrogen gas is used for sintering, the pressure of nitrogen gas in the high temperature oven is 0.1-0.12 MPa. The metal M described in the present invention is any one of Fe or Ti or Cu or Zn.

 The crucible in the present invention may be replaced by grass clippings, and other suitable raw materials such as liquid paraffin, coal powder, expanded soil and the like may be added as needed.

 The bioceramic of the present invention can be formed into columnar particles or pellets having a diameter of 0.1 to 0.5 cm as needed, or a powdery material having a diameter of less than 0.15 mm.

 The bio-ceramic having the selective adsorption digestion function of the invention can be used for the adsorption of benzene, phenols, aldehydes, naphthalenes and the like of petroleum crude oil residual oil, petrochemical waste gas, automobile exhaust gas, etc. to achieve air purification and filtration; It can be applied to biofilters, trickling filters, and biological media for granular sludge beds in anaerobic treatment.

The invention adopts a formulation of waste water and food industry of the papermaking industry, and waste sludge and kaolin of the sewage treatment plant and adds the waste material of the crop crust, and performs the anaerobic heating firing, the microwave activation of the porous bioceramic particles or the powder, forming a kind Bioselective bioceramics. The obtained bioceramic material has the function of selectively adsorbing odorous substances of benzene, phenol, polyhydrocarbons, dimethyl sulfide and thioethers, and is used for air filtration; bio-ceramic and has an effective carbon source and mineral for microorganisms. Biofilter media for air filtration and wastewater treatment; this material also has phosphate ion work in adsorbed water Can remove oxygen-rich ingredients from water. The core concept of the present invention is waste manufacturing a new active material with both adsorption and biological media for air purification and wastewater treatment.

 The bioceramic of the present invention has a function of shrinkable pores and immobilization of microorganisms. The technical features are as follows:

 1. Selective adsorption capacity of benzene and phenols

 In the process of bioceramic firing, a surface active material of amorphous Si-C-M is produced, and a benzene ring material such as benzene, phenol or naphthalene has an adsorption structure with a specific adsorption capacity of more than 350 mg/g. The adsorption capacities for benzene, phenol, and naphthalene are 360 mg/g, 560 mg/g, and 600 mg/g, respectively.

 The above petroleum-based residual substances are not adsorbed to the salty substances in seawater or fresh water, and the bioceramics of the present invention still have an adsorption capacity of 350 mg/g or more.

 The petroleum crude oil benzene is adsorbed in seawater for 24 hours, 1 liter of seawater contains 12000 ng/ml, 10 g of bio-potassy is added, and adsorption is carried out for 24 hours, and the benzene content in seawater is not detected.

 2. Adsorption of thioethers on digestion. After the thioether is adsorbed on the surface of the micropores of the bio-ceramics, it reacts with iron and titanium powders to form FeS and the like, thereby eliminating malodor.

 The digestion ability is calculated as: digestion ability (%) = (adsorption capacity - pickling dissolution amount) / adsorption capacity X 100%.

 The chemical digestion rate of bio-ceramics is 70%-90% of the total adsorption capacity.

 3, microbial biological fixation is the ability of biological digestion

 The firing process is heated in an anoxic environment to carbonize the organic matter in the sludge, which not only retains the carbon source for the growth of the next generation of microorganisms, but also acts as a nutrient for the growth of bacteria. The remaining inorganic elements in the biological pottery are the new ones that are trapped. A generation of microbial growth provides growth elements; a bacterial carrier that can be used for denitrification (nitrate) in a nitrification-denitrification process.

 4. Fixed microorganisms to digest the adsorbed benzene and phenols. For coke wastewater containing llppm phenolic substances, all bio-ceramics were added and microbial inoculation, and phenolic substances were reduced by half after 12 hours.

 5. Bio-ceramics used as adsorption or biological carriers are the most fuel incineration. The dried bioceramic particles have a heat of 2000 kg/kg to 3750 kcal I kg, and the adsorbed volatile substances can be burned at temperatures above 600 degrees. The used particles can be used as a fuel and coal after combustion.

Compared with the prior art, the invention has the beneficial effects that the bio-ceramic having the selective adsorption digestion function of the invention can solve many technical problems existing in the prior art: (1) selective adsorption of phenolic carcinogens; (2) At the same time, it has the function of adsorption and chemical digestion of thioether; (3) The new biological formula of the invention and the firing process will make the sludge heavy The metal element is immobilized and will not be released during application. (4) Nitrification-denitrification water treatment as a microbial carrier, and microbial digestion of phenolic substances. (5) After use, the bio-ceramic has a calorific value of 2000 ka/kg or more, which can be burned together with pulverized coal to solve the problem of leaving solid waste.

 The material of the present invention has round particles of different diameters, columnar particles, and powders, and the biological pottery of the present invention has a wider application prospect such as air and water filtration.

 For the application of the bioceramic of the present invention, the alternative uses include any of the following:

 1. As an air purifier material, it adsorbs volatile and semi-volatile substances such as benzene, phenols, formaldehyde, and hydrocarbons in the air. For example, it is used as a breathable yarn bag to absorb organic discharges such as newly-decorated floors and furniture; an adsorbent for volatile gas emitted from chemical plants; and a residue of automobile exhaust gas.

 2. Treatment of adsorbents containing phenol and benzene wastewater, such as waste water loaded into adsorption towers for adsorbing explosives, coke, ceramics, etc., for terminal purification treatment.

 3. Filtration and biological digestion materials for oil leakage and residual poison in water. The carcinogens after the leakage of crude oil mainly include benzene, phenols and polyhydrocarbon pollutants. Especially in seawater, bioceramic particles or powders can be adsorbed quickly and selectively, thus reducing the environmental hazards of these substances.

 4. Produce bio-potential crafts and deodorant insole additives with adsorption function.

 5. As a biochemical medium for sewage treatment, such as biological filter media for sewage treatment plants. Since the bio-ceramic is subjected to anoxic firing during the firing process, the organic matter in the microorganism is directly carbonized. The remaining carbon can be used as a carbon source by the microorganisms, so the use of bio-ceramics as a filter material does not require the addition of a carbon source in the digestion and denitrification projects. In the existing sewage treatment and denitrification process, it is necessary to add methanol or glucose as a carbon source to maintain the growth and metabolism of microorganisms.

 6. Used to clean up the eutrophication of lakes. Bio-ceramics can be directly hoisted in cages or net buckets to adsorb facultative microorganisms to treat organic contaminants in the water.

 7. The surface roughness of the bioceramic particles helps to improve the process of anaerobic treatment.

 8. Used as a biological pottery for the immobilization of transgenic bacteria.

 DRAWINGS

 BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a photograph showing a 3000-fold electronic scanning of a bioceramic of the present invention. The bioceramic particles have 1-3 m voids and irregular structures inside, and are selected to adsorb benzene and phenols.

 detailed description

Example 1 The bioceramic having the selective adsorption digestion function of the present embodiment is made of the following raw materials by weight: sludge 30, kaolin 2, and iron powder 1.

 The preparation method is as follows:

 (1) mixing raw materials of bio-bioceramics according to the above formula, forming by extrusion or disc granulation, and drying and forming;

 (2) The preform obtained in the step (1) is placed in a high-temperature oven and fired under vacuum. The vacuum degree in the high-temperature oven is -0.08-0.09 Mpao, and the oven temperature is raised at a temperature increase rate of 90 ° C / h. Maintaining at 300 ° C for 1.5 hours, the volatile odor gas generated here is burned into the gas furnace, and the heat is used for self-heating;

 (3) The oven temperature is raised to 740 ° C at a temperature increase rate of 90 ° C / h for 3 hours; then cooled to room temperature at a cooling rate of 150 ° C / h to obtain a biological ceramic medium;

 (4) The bio-ceramic medium obtained in the step (3) was subjected to water vapor absorption for 1.5 hours, and activated by an industrial microwave oven for 0.5 hour to obtain the bio-bioceramic of the present invention.

 The selective bioceramic of the present embodiment has an amorphous Si-C-Fe structure having a specific surface area of 400 m2.

 The bioceramic having the selective adsorption digestion function of the present embodiment is made of the following raw materials by weight: sludge

50, kaolin 10, copper powder 3, wheat glutinous rice 8.

 The preparation method is as follows:

 (1) mixing raw materials of bio-bioceramics according to the above formula, forming by extrusion or disc granulation, and drying and forming;

 (2) The preform obtained in the step (1) is placed in a high-temperature oven and fired under a nitrogen atmosphere, and the pressure of the nitrogen gas introduced into the high-temperature oven is 0.1-0.12 MPa. The oven temperature is raised to 300 ° C at a heating rate of 100 ° C / h for 1.5 hours, and the volatile odor gas generated here is burned into a gas furnace, and the heat is used for self-heating;

 (3) The oven temperature is raised to 750 ° C at a heating rate of 100 ° C / h for 2.5 hours; then cooled to room temperature at a cooling rate of 180 ° C / h to obtain a biological ceramic medium;

 (4) The bio-ceramic medium obtained in the step (3) was subjected to water vapor absorption for 1.2 hours, and activated by an industrial microwave oven for 0.8 hours to obtain the bio-bioceramic of the present invention.

 The selective bioceramic of the present embodiment has an amorphous Si-C-Cu structure having a specific surface area of 420 m2.

The bioceramic having the selective adsorption digestion function of the present embodiment is made of the following raw materials by weight: sludge 30-70, kaolin 2-15, Zn l-5, 糠8-12, calcium carbonate 3-5.

 The preparation method is as follows:

 (1) mixing raw materials of bio-bioceramics according to the above formula, forming by extrusion or disc granulation, and drying and forming;

 (2) The preform obtained in the step (1) is placed in a high-temperature oven and fired under a nitrogen atmosphere, and the pressure of the nitrogen gas introduced into the high-temperature oven is 0.1-0.12 MPa. The oven temperature is raised to 305 ° C at a heating rate of 110 ° C / h for 1 hour, and the volatile odor gas generated here is burned into a gas furnace, and the heat is used for self-heating;

 (3) The temperature of the oven is raised to 760 ° C for 2 hours at a heating rate of 110 ° C / h; then the temperature is lowered to room temperature at a cooling rate of 200 ° C / h to obtain a biological ceramic medium;

 (4) The bio-ceramic medium obtained in the step (3) was absorbed by water vapor for 1 hour, and activated by an industrial microwave oven for 1 hour to obtain the bio-bioceramic of the present invention.

 The selective bioceramic of the present embodiment has an amorphous Si-C-Zn structure having a specific surface area of 460 ml/g o.

 The bioceramic having the selective adsorption digestion function of the present embodiment is made of the following raw materials by weight: 70 parts of sludge, 10 parts of wheat bran, 2 parts of kaolin, 1 part of reduced iron powder, and 2 parts of expanded soil.

 The preparation method is the same as the preparation method of Example 2.

 The selective bioceramic of this embodiment has an amorphous Si-C-Fe structure having a specific surface area of 500 m2/go.

 The bioceramic having the selective adsorption digestion function of the present embodiment is made of the following raw materials by weight: 34-55 parts of sludge, 8-10 parts of titanium dioxide, 3-4 parts of calcium carbonate, 8-10 parts of kaolin, 1-2 parts of liquid wax, 5-6 parts of copper oxide powder.

 The preparation method is the same as the preparation method of Example 2, and is prepared into a columnar bioceramic having a diameter of less than 0.1 to 0.5 cm for use as a filter for air filtration.

 The selective bioceramic of this embodiment has an amorphous Si-C-Fe structure having a specific surface area of 460 m2/g. Example 6

 The bioceramic having the selective adsorption digestion function of the present embodiment is made of the following raw materials by weight: 65 parts of paper industry sludge, 8 parts of calcium carbonate, 15 parts of clay, 6-8 parts of grass clippings, zinc powder 1 Parts, 1-3 parts of iron powder, 1-3 parts of coal powder.

The preparation method thereof is the same as the preparation method of the embodiment 2, and is prepared to have a diameter smaller than that used in the chemical wastewater reactor. 0.1-0.5 cm spherical bio-ceramic.

 The selective bioceramic of this embodiment has an amorphous Si-C-Fe structure having a specific surface area of 460 m2/g. The performance test method and test results of the bioceramic of the present invention are as follows:

 1. Refinery flue gas / exhaust gas filtration experiment

 100 g of 0.5 mm diameter granules were placed in a 5 cm diameter glass cylinder; 15 ml of water was added to maintain the wettability of the granules, the benzene volatile content was 0.5 ug/L, and the removal rate was greater than 98%. Air flow rate 5 liters / minute; On-line GC-MT homogeneous quality and timely detection, determination of removal rate, 100 grams of ceramsite removal rate at different stages, 0-36 cubic meters 98%; 36-68 cubic meters, 90%; 68- 100 cubic meters; 85% removal rate; 100-300 cubic meters, 80%.

 2. Adsorption experiments of benzene, xylene and formaldehyde in static air

 2 cubic meters sealed container; initial concentration of pollutants volatilized benzene 2 mg / cubic meter; formaldehyde 2 mg / cubic meter; xylene 1.8 mg I cubic meter; hoisting 5 grams of bio-bioceramic nylon bags; determination of 24 hours adsorption speed. Fully static, no mixed adsorption experiments, the adsorption test results are shown in Table 1.

 Table 1 Experimental results of adsorption of benzene, xylene and formaldehyde in static air

 3. Adsorption test of benzene series in seawater

 Experimental methods: (1) Take 50 liters of Qinhuangdao natural seawater into a closed container vat, add crude oil at 1:1000, and occlude for 24 hours to obtain the mother liquor belt. (2) Add 20 grams of bio-bioceramics and yarn bags, hang them in a seawater bucket, and continue to oscillate. (3) Sampling 20 ml according to 0, 2, 4, 8, 12, 24, 48, 72, 96 hours, sealed for inspection. (4) The content of each phenolic substance was detected by a temperament and quality joint detector, and the results are shown in Table 2.

 Table 2 Results of adsorption test of benzene series in seawater

_/ __ Sample original number (adsorption time) 0 (ck) 1 (2 hours) 2 (4 hours) Analysis item -

Detection No. YJ10073001 YJ10073002 YJ10073003 Volatile Organic Units Reporting Limit 0 2 4 Benzene ng/mL 1.00 11725 9042 4393 toluene ng/mL 1.00 5151 4042 1357 ethylbenzene ng/mL 1.00 341 230 130 p-xylene ng/mL 1.00 1223 824 170 o-xylene ng/mL 1.00 765 598 326 benzene /mL 1.00 <1.00 <1.00 <1.00 Alternative Recovery Rate % Control Limit

 Dibromofluoromethane % 60- 130 98.3 94.0 100.8 Fluorobenzene % 60- 130 96.7 92.5 98.1 Toluene -D8 % 60- 130 94.5 92.2 95.6

4-bromofluorobenzene % 60- 130 97.1 93.1 97.7

1,2-Dichlorobenzene-D4 % 60- 130 95.6 91.2 97.9 Sample No. 3 (8 hours) 4 (12 hours) 5 (24 hours)

 Detection No. YJ10073004 YJ10073005 YJ10073006 Volatile Organic Units Revenue Limit 8 12 24 Benzene ng/mL 1.00 2499 408.9 0 Toluene ng/mL 1.00 627 2.91 0 Ethylbenzene ng/mL 1.00 1 0 0 Para-xylene ng/mL 1.00 1 0 0 o-xylene ng/mL 1.00 107 0 0 phenyl b recording ng/mL 1.00 <1.00 <1.00 <1.00 alternative recovery rate % control limit

 Dibromofluoromethane % 60- 130 98.7 105 103 Fluorobenzene % 60- 130 94.0 98.1 97.1 Toluene -D8 % 60- 130 92.5 100 94.9

4-bromofluorobenzene % 60- 130 91.9 102 95.1

1,2-dichlorobenzene-D4 % 60- 130 93.9 102 97.0 Sample No. 6 (48 hours) Ί (72) 8 ( 96) Analytical Project

 Detection No. YJ10073007 YJ10073008 YJ10073009 Volatile Organic Compounds

Benzene ng/mL 1.00 <1.00 23.2 <1.00 toluene ng/mL 1.00 <1.00 2.00 <1.00 ethylbenzene ng/mL 1.00 <1.00 <1.00 <1.00 m-xylene ng/mL 1.00 <1.00 <1.00 <1.00 o-xylene ng /mL 1.00 <1.00 <1.00 <1.00 苯乙录ng/mL 1.00 <1.00 <1.00 <1.00 alternative recovery rate % control limit

 Dibromofluoromethane % 60- 130 91.4 93.6 91.9 Fluorobenzene % 60- 130 88.5 88.7 88.2 Toluene -D8 % 60- 130 89.4 85.9 89.0

4-bromofluorobenzene % 60- 130 88.6 85.7 90.5

1,2-Dichlorobenzene-D4% 60-130 87.0 90.3 90.8, the detection report of the removal effect of the bio-ceramic of the present invention on benzene, toluene and xylene in indoor air.

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Submit. Yixian: Beijing *'Xuanwu District. Guang'an

 Editor: 100053

Electric tli 86- 01 -S31.228!)5

Fax: 86 - 010 - 8311440/

 Address: China Indoor Environment

E-mail II: Is! a|@v I „ s I na. com

Claims

Claim 1. A bioceramic having a selective adsorption digestion function, characterized in that it is mainly made of the following raw materials by weight: sludge 30-70, kaolin 2-15, metal M or metal M oxide 1 The selective activated carbon ceramic has an amorphous Si-CM structure and has a specific surface area of 400 to 500 m ² /g.  2. The bioceramic having a selective adsorption digestion function according to claim 1, wherein the sludge is activated sludge, and the microbial content in the sludge is 70%.  3. The bioceramic having a selective adsorption digestion function according to claim 1 or 2, characterized in that it is mainly made of the following raw materials by weight, sludge 30-70, kaolin 2-15, metal M Or oxides 1-5, 糠 8-12 of metal M.  4. The bioceramic having a selective adsorption digestion function according to claim 3, which is made of the following raw materials by weight, sludge 30-70, kaolin 2-15, metal M or metal M Oxide 1-5, 糠 8-12, calcium carbonate 3-5.  5. The bioceramic having selective adsorption digestion function according to claim 4, characterized in that it is made of the following raw materials by weight: the metal M is any of Fe or Ti or Cu or Zn. One.  6. The bioceramic having a selective adsorption digestion function according to claim 1, wherein the bioceramic is characterized by the following steps:  (1) mixing raw materials of biological activated carbon ceramics according to the above formula, forming by extrusion or disc granulation, and drying and forming;  (2) The preform obtained in the step (1) is placed in a high-temperature oven under vacuum or fired under nitrogen atmosphere, and the oven temperature is raised to 295-305 ° C at a temperature increase rate of 90-110 ° C / h. 1~2 hours, the volatile odor gas generated here is burned into the gas furnace, and the heat is used for self-insulation;  (3) The oven temperature is raised to 740-76 CTC at a temperature increase rate of 90-110 ° C / h for 2-3 hours; then cooled to room temperature at a cooling rate of 150-200 ° C / h to obtain a biological ceramic medium;  (4) The charcoal medium obtained in the step (3) is added to water vapor for 1-1.5 hours, and activated by an industrial microwave oven for 0.5-1 hour to obtain the bioceramic of the present invention.  7. The bioceramic having a selective adsorption digestion function according to claim 6, wherein the step is carried out as follows: Step (2) The degree of vacuum in the high temperature oven is -0.08 - 0.09 Mpa.  8. The bioceramic having selective adsorption digestion function according to claim 6, wherein the step is carried out according to the following steps: Step (2) The pressure of the nitrogen gas in the high temperature oven is 0.1-0.12 MPa. .