CN117088639A - Preparation method and application of ceramic filler for sewage treatment - Google Patents
Preparation method and application of ceramic filler for sewage treatment Download PDFInfo
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- CN117088639A CN117088639A CN202311126839.5A CN202311126839A CN117088639A CN 117088639 A CN117088639 A CN 117088639A CN 202311126839 A CN202311126839 A CN 202311126839A CN 117088639 A CN117088639 A CN 117088639A
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- 239000010865 sewage Substances 0.000 title claims abstract description 71
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 239000000945 filler Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920001661 Chitosan Polymers 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000004088 foaming agent Substances 0.000 claims abstract description 18
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010802 sludge Substances 0.000 claims abstract description 13
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical class O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000018417 cysteine Nutrition 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 229940074391 gallic acid Drugs 0.000 claims abstract description 8
- 235000004515 gallic acid Nutrition 0.000 claims abstract description 8
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims abstract description 7
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims abstract description 7
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 16
- 239000002351 wastewater Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000013067 intermediate product Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000012856 packing Methods 0.000 claims 2
- 230000001580 bacterial effect Effects 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000001172 regenerating effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 5
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 1
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical group [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/28—Polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
- C02F3/10—Packings; Fillings; Grids
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/28—Anaerobic digestion processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/74—Underwater applications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Environmental & Geological Engineering (AREA)
- Ceramic Engineering (AREA)
- Water Supply & Treatment (AREA)
- Biodiversity & Conservation Biology (AREA)
- Hydrology & Water Resources (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Biological Treatment Of Waste Water (AREA)
Abstract
The invention relates to a preparation method of ceramic filler for sewage treatment, which comprises the following steps: s1, mixing river bottom mud, domestic sludge, a foaming agent, an adhesive and water, baking, cooling, crushing and sieving to obtain coarse materials; s2, ball-milling and granulating the coarse material to obtain a precursor; s3, heating the precursor to 100-120 ℃ in a gradient way, keeping the temperature constant, and cooling to obtain the ceramic filler for sewage treatment; wherein the adhesive adopts components including modified chitosan, modified polyacrylate and hydroxylated kaolin; the modified chitosan is a product obtained by reacting chitosan with cysteine; the modified polyacrylate is a product obtained by reacting isobornyl acrylate, butyl acrylate, hydroxypropyl methacrylate and gallic acid. The porous ceramic filler structure with ideal morphology can be prepared, and is favorable for attaching, metabolizing and regenerating bacterial groups, so that the waste in sewage can be treated efficiently and continuously.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to a preparation method and application of ceramic filler for sewage treatment.
Background
Industrial sewage is one of byproducts of industrial production, has the characteristics of large discharge amount, high concentration, complex components and the like, has serious harm to the ecological environment, and how to purify and harmlessly treat the industrial sewage is an important subject of researches in a plurality of fields.
The current method for treating wastewater mainly comprises the following steps: insoluble, poorly soluble contaminants are separated by physical means or the contaminants are converted by chemical means. However, the method has the defects of high operation cost, high energy consumption, complex management, incomplete treatment and easy secondary pollution. The sewage treatment by the microbial technology has the advantages of low energy consumption, high efficiency, sustainability, economy and thoroughness, and therefore, the sewage treatment is attracting attention.
The filler is the core part of the wastewater treated by biological means and plays roles in fixing biological membranes and adsorbing pollutants. The ceramic filler has the advantages of large specific surface area, quick microbial film formation, acid and alkali resistance, oxidation resistance and stable performance, and has a good purifying effect on heavy metal ions and organic pollutants in sewage.
CN104072090A, CN109231960a et al discloses a technical solution for applying porous ceramic filler to the field of sewage treatment, however, the prior art still cannot guarantee the sewage treatment effect under turbulent flow conditions. Along with the continuous change and accumulation of the water flow speed and the working time, the active bacterial group can be seriously lost and lose efficacy, and ceramics can be increasingly aged and decomposed, so that the processing capacity of the filler is greatly reduced, and finally, the ideal technical effect cannot be realized.
In view of the foregoing, there is a need to develop a new technical solution to solve the drawbacks of the prior art.
Disclosure of Invention
Based on the above, the invention develops a preparation method of ceramic filler for sewage treatment, wherein the adopted base materials are common soil and sludge, and are matched with special adhesives and foaming agents, and a porous ceramic filler structure with ideal appearance can be formed after heat treatment, which is beneficial to the attachment, metabolism and regeneration of flora, so that the waste in sewage can be treated efficiently and continuously.
An object of the present invention is to provide a method for preparing a ceramic filler for sewage treatment, comprising the steps of:
s1, mixing river bottom mud, domestic sludge, a foaming agent, an adhesive and water, baking, cooling, crushing and sieving to obtain coarse materials;
s2, ball-milling and granulating the coarse material to obtain a precursor;
s3, heating the precursor to 100-120 ℃ in a gradient way, keeping the temperature constant, and cooling to obtain the ceramic filler for sewage treatment;
wherein the adhesive adopts components including modified chitosan, modified polyacrylate and hydroxylated kaolin;
the modified chitosan is a product obtained by reacting chitosan with cysteine;
the modified polyacrylate is a product obtained by reacting isobornyl acrylate, butyl acrylate, hydroxypropyl methacrylate and gallic acid.
Further, the preparation method of the modified polyacrylate comprises the following steps:
m1, adding isobornyl acrylate, butyl acrylate and hydroxypropyl methacrylate into a solvent, stirring, adding an initiator, heating under inert gas for reaction, and purifying to obtain an intermediate product;
and M2, adding the intermediate product, the catalyst and the gallic acid into a solvent, stirring for reaction, cooling, adding a cross-linking agent, continuing the reaction, and purifying to obtain the modified polyacrylate.
Further, the preparation method of the modified chitosan comprises the following steps:
l1, dissolving chitosan in an aqueous solution of acetic acid to form a solution;
l2, heating the solution, gradually adding cysteine, reacting 6-10 h, removing the solvent and the residual raw materials, and drying to obtain the modified chitosan.
Further, in step S3, the gradient heating method is as follows: heating the precursor to 60-80 ℃ and keeping the temperature constant at 1-2 h; then heating to 100-120 deg.C, and keeping the temperature at 1-2 h deg.C.
Further, in step S1, the mass parts of the river sediment and the domestic sludge are as follows: 40-50 parts of river bottom mud and 50-60 parts of domestic sludge.
Further, in the step S1, the foaming agent is 3-5 wt% of coarse materials; the binder is 3-5 wt% of the coarse material.
Further, in the step S1, the modified chitosan is 50-70 wt% of the foaming agent.
Further, the foaming agent is sodium bicarbonate.
Another object of the present invention is to provide an application of the ceramic filler for sewage treatment prepared by the preparation method of the ceramic filler for sewage treatment in sewage treatment.
Further, the application of the ceramic filler for sewage treatment prepared by the preparation method of the ceramic filler for sewage treatment in sewage treatment comprises the following steps:
c1, regulating the pH value of the wastewater to 6-9, and regulating the temperature to 15-35 ℃;
c2, putting the ceramic filler for sewage treatment into the wastewater, and carrying out aerobic or anaerobic treatment for 7-10 days;
and C3, testing the index of the wastewater.
Further, the ceramic filler for sewage treatment is 10-30 wt% of the wastewater.
The invention has the following beneficial effects:
the invention discloses a preparation method of ceramic filler for sewage treatment, wherein an adhesive is a composition of modified chitosan, modified polyacrylate and hydroxylated kaolin, the modified chitosan is a product obtained by reacting chitosan with cysteine, and gallic acid branched chains are introduced into the modified polyacrylate. On one hand, the modified chitosan contains amino and sulfhydryl groups, the modified polyacrylate has a large number of active functional groups such as phenolic hydroxyl groups, and the strong polar groups can better adsorb the foaming agent particles, so that the foaming agent particles are relatively stably adsorbed on the adhesive, and the adsorption sites of pollutants are increased; on the other hand, chitosan itself is used as a high polymer structure, and after being compounded with components such as modified polyacrylate, a three-dimensional network structure is easier to form in the base material, so that the foaming agent can be dispersed to each part of the base material along with the polymer chain segments, and meanwhile, the addition of the hydroxylated kaolin promotes the dispersion effect of solid particles, so that pores which are more uniform, compact and smaller in particle size are formed in the foaming process, and the ceramic filler is favorable for durable, stable and efficient sewage treatment.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are set forth. The starting materials, reactions and workup procedures used in the examples are those commonly practiced in the market and known to those skilled in the art unless otherwise indicated.
The words "preferred," "more preferred," and the like in the present disclosure refer to embodiments of the present disclosure that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
It should be understood that, except in any operating examples, or where otherwise indicated, quantities or all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.
The chitosan in the embodiment of the invention is purchased from Qingdao Hongsha biotechnology Co., ltd, and has the molecular weight of 100 kDa, the deacetylation degree of 91.0% and the viscosity of 45 mPa.s.
The river bottom mud is collected from Guangzhou river sections of Zhujiang (collection region: near subway entrance of Zhujiang newcastle);
the domestic sludge is collected from Guangzhou municipal sewage treatment Limited liability company;
the foaming agent is sodium bicarbonate, and the particle size is 0.02 mu m;
the rest reagents are all common substances on the market.
The parts are all parts by weight.
The adhesive comprises the following components: 60 parts of modified chitosan, 10 parts of modified polyacrylate, 20 parts of hydroxylated kaolin and 20 parts of water.
The modified chitosan is a product obtained by reacting chitosan with cysteine. The method comprises the following specific steps:
l1, dissolving chitosan in a sufficient amount of 15 wt% acetic acid aqueous solution to form a solution;
l2, heating the solution to 50 ℃, then gradually adding cysteine (the cysteine is excessive relative to chitosan), stirring for reaction 6 h, then removing the solvent and the residual raw materials, and drying to obtain the modified chitosan.
The preparation method of the modified polyacrylate comprises the following steps:
m1, taking ethanol as a solvent, blending isobornyl acrylate, butyl acrylate and hydroxypropyl methacrylate (isobornyl acrylate: butyl acrylate: hydroxypropyl methacrylate=4:5:1, n/n/n), stirring, adding an initiator AIBN (1.5% of the total mass of the monomers), reacting at 68 ℃ under a nitrogen atmosphere for 12 h, cooling, washing with deionized water, and drying to obtain an intermediate product;
and M2, taking tetrahydrofuran as a solvent, blending the intermediate product and gallic acid, adding a catalyst 4-dimethylaminopyridine (0.7% of the mass of the intermediate product), stirring for 10 min under a nitrogen atmosphere, cooling to 4 ℃ under an ice bath, adding a cross-linking agent N, N '-dicyclohexylcarbodiimide (the intermediate product: gallic acid: N, N' -dicyclohexylcarbodiimide=7.3:1:1.2, M/M), continuing stirring for reacting for 8 h, and filtering, washing and drying after the reaction is finished to obtain the modified polyacrylate.
The preparation method of the hydroxylated kaolin comprises the following steps:
soaking kaolin powder in 5 mol/L sodium hydroxide solution, carrying out ultrasonic treatment for 3 h, washing to neutrality, mixing with glucose (kaolin: glucose=1:5, m/m) after drying, carrying out ball milling treatment (ball-to-material ratio 5:1), washing, centrifuging, and drying to obtain the hydroxylated kaolin.
Example 1: the preparation method of the ceramic filler for sewage treatment comprises the following steps:
s1, uniformly blending 50 parts of river bottom mud, 50 parts of domestic sludge, 7 parts of foaming agent, 10 parts of adhesive and 30 parts of water, baking at 110 ℃ until the mixture becomes hard, cooling, crushing by a crushing device and sieving by a 100-mesh sieve to obtain coarse material;
s2, ball milling and granulating the coarse material into spheres with the particle size of 7 mm by using a ball mill to obtain a precursor;
s3, heating the precursor in a two-stage gradient manner, and firstly, heating the precursor to 60 ℃ from normal temperature at a speed of 3 ℃/min and keeping the temperature constant at 1 h; then the temperature is increased to 100 ℃ at the speed of 3 ℃/min, the constant temperature is 1 h, and then the ceramic filler for sewage treatment is obtained after cooling.
Example 2: the preparation method of the ceramic filler for sewage treatment comprises the following steps:
s1, uniformly mixing 45 parts of river sediment, 55 parts of domestic sludge, 8 parts of foaming agent, 12 parts of adhesive and 35 parts of water, baking at 115 ℃ until the mixture becomes hard, cooling, crushing by a crushing device and sieving by a 100-mesh sieve to obtain coarse materials;
s2, ball milling and granulating the coarse material into spheres with the particle size of 7 mm by using a ball mill to obtain a precursor;
s3, heating the precursor in a two-stage gradient manner, and firstly, heating the precursor to 70 ℃ from normal temperature at a speed of 4 ℃/min and keeping the temperature constant for 2 h; then the temperature is increased to 120 ℃ at the speed of 4 ℃/min, the constant temperature is 2 h, and then the ceramic filler for sewage treatment is obtained after cooling.
Example 3: the preparation method of the ceramic filler for sewage treatment comprises the following steps:
s1, uniformly mixing 47 parts of river sediment, 60 parts of domestic sludge, 10 parts of foaming agent, 15 parts of adhesive and 47 parts of water, baking at 105 ℃ until the mixture becomes hard, cooling, crushing by a crushing device and sieving by a 100-mesh sieve to obtain coarse materials;
s2, ball milling and granulating the coarse material into spheres with the particle size of 7 mm by using a ball mill to obtain a precursor;
s3, heating the precursor in a two-stage gradient manner, and firstly, heating the precursor to 75 ℃ from normal temperature at a speed of 4 ℃/min and keeping the temperature constant at 2 h; then the temperature is increased to 110 ℃ at the speed of 4 ℃/min, the constant temperature is 1 h, and then the ceramic filler for sewage treatment is obtained after cooling.
Example 4: the preparation method of the ceramic filler for sewage treatment comprises the following steps:
s1, uniformly mixing 45 parts of river sediment, 62 parts of domestic sludge, 11 parts of foaming agent, 17 parts of adhesive and 55 parts of water, baking at 108 ℃ until the mixture becomes hard, cooling, crushing by a crushing device and sieving by a 100-mesh sieve to obtain coarse materials;
s2, ball milling and granulating the coarse material into spheres with the particle size of 8 mm by using a ball mill to obtain a precursor;
s3, heating the precursor in a two-stage gradient manner, and firstly, heating the precursor to 80 ℃ from normal temperature at a speed of 3 ℃/min and keeping the temperature at 1.5 h; then the temperature is increased to 115 ℃ at the speed of 4 ℃/min, the constant temperature is 1.5 h, and then the ceramic filler for sewage treatment is obtained after cooling.
Comparative example 1: the ceramic filler for sewage treatment of comparative example 1 was prepared in the same manner as in example 1 except that the modified chitosan was not used in comparative example 1, but instead, the same amount of chitosan was directly used in the same manner.
Comparative example 2: the ceramic filler for sewage treatment of comparative example 2 was prepared in the same manner as in example 1 except that the modified polyacrylate was not used in comparative example 2, but the intermediate product prepared in step M1 was replaced with the modified polyacrylate in the preparation method.
Test example 1: the ceramic fillers for sewage treatment obtained in examples 1-2 and comparative examples 1-2 were used in sewage treatment experiments. The sewage is taken from the water body of the aerobic section and the anaerobic section of the Guangzhou municipal sewage treatment limited responsibility company, and is mixed according to the volume ratio of 1:1, and the obtained water body is enough to complete the test case.
The test steps are as follows:
c1, sub-packaging the wastewater to be tested into a plurality of water pools (volume 10 m) which are built by reinforced cement with equal volume 3 ) The pH value of the wastewater to be measured is regulated to 7.5, the temperature is regulated to 25+/-1 ℃, a stirrer is arranged on the wastewater, and the wastewater in a water tank is continuously stirred (the rotating speed is 30 revolutions per minute), so that a turbulent environment is caused;
c2, aerobic treatment: the ceramic fillers for sewage treatment obtained in the examples 1-2 and the comparative examples 1-2 are respectively put into the bottoms of four different pools (the ceramic fillers for sewage treatment are 20 wt% of sewage), and are aerated for 7 days, and the oxygen content in the sewage is ensured to be 3-5 mg/L;
c2', anaerobic treatment: taking ceramic fillers for sewage treatment obtained in examples 1-2 and comparative examples 1-2, respectively putting the ceramic fillers into the bottoms of four different pools (the ceramic fillers for sewage treatment are 20 wt% of sewage), sealing the tops of the pools by using plastic cloth, performing anaerobic treatment for 7 days, and ensuring that the oxygen content in the sewage is 0.2 mg/L;
and C3, testing the index of the wastewater treated by the ceramic filler for sewage treatment, and comparing with the index before treatment.
The results obtained are shown in Table 1.
TABLE 1 comparison of SS and COD indicators before and after wastewater treatment
As can be seen from Table 1, the examples have significant advantages over the comparative examples, both after aerobic and anaerobic treatment, mainly because the ceramic filler for sewage treatment formed in the examples has a desirable morphology, is more suitable for stable and healthy survival of microbial flora, and can be relatively firmly attached in ceramic pores even in turbulent environment, thereby efficiently treating SS and COD in wastewater.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The preparation method of the ceramic filler for sewage treatment is characterized by comprising the following steps of:
s1, mixing river bottom mud, domestic sludge, a foaming agent, an adhesive and water, baking, cooling, crushing and sieving to obtain coarse materials;
s2, ball-milling and granulating the coarse material to obtain a precursor;
s3, heating the precursor to 100-120 ℃ in a gradient way, keeping the temperature constant, and cooling to obtain the ceramic filler for sewage treatment;
wherein the adhesive adopts components including modified chitosan, modified polyacrylate and hydroxylated kaolin;
the modified chitosan is a product obtained by reacting chitosan with cysteine;
the modified polyacrylate is a product obtained by reacting isobornyl acrylate, butyl acrylate, hydroxypropyl methacrylate and gallic acid.
2. The method for preparing ceramic filler for sewage treatment according to claim 1, wherein the method for preparing the modified polyacrylate comprises the steps of:
m1, adding isobornyl acrylate, butyl acrylate and hydroxypropyl methacrylate into a solvent, stirring, adding an initiator, heating under inert gas for reaction, and purifying to obtain an intermediate product;
and M2, adding the intermediate product, the catalyst and the gallic acid into a solvent, stirring for reaction, cooling, adding a cross-linking agent, continuing the reaction, and purifying to obtain the modified polyacrylate.
3. The method for preparing ceramic filler for sewage treatment according to claim 1, wherein the method for preparing the modified chitosan is as follows:
l1, dissolving chitosan in an aqueous solution of acetic acid to form a solution;
l2, heating the solution, gradually adding cysteine, reacting 6-10 h, removing the solvent and the residual raw materials, and drying to obtain the modified chitosan.
4. The method for preparing ceramic packing for sewage treatment according to claim 1, wherein in step S3, the gradient heating method is as follows: heating the precursor to 60-80 ℃ and keeping the temperature constant at 1-2 h; then heating to 100-120 deg.C, and keeping the temperature at 1-2 h deg.C.
5. The method for preparing ceramic packing for sewage treatment according to claim 1, wherein in step S1, the mass parts of the river sediment and the domestic sludge are: 40-50 parts of river bottom mud and 50-60 parts of domestic sludge.
6. The method for producing a ceramic filler for sewage treatment according to claim 1, wherein in step S1, the foaming agent is 3 to 10 wt% of coarse material; the adhesive is 3-10 wt% of coarse materials; the modified chitosan accounts for 50-70 wt% of the foaming agent.
7. The method for producing a ceramic filler for sewage treatment according to claim 1, wherein the foaming agent is sodium bicarbonate.
8. The use of the ceramic filler for sewage treatment prepared by the method for preparing a ceramic filler for sewage treatment according to any one of claims 1 to 7 in sewage treatment.
9. The use of the ceramic filler for sewage treatment prepared by the preparation method of the ceramic filler for sewage treatment according to claim 8 in sewage treatment, characterized by comprising the following steps:
c1, regulating the pH value of the wastewater to 6-9, and regulating the temperature to 15-35 ℃;
c2, putting the ceramic filler for sewage treatment into the wastewater, and carrying out aerobic or anaerobic treatment for 7-10 days;
and C3, testing the index of the wastewater.
10. The use of the ceramic filler for sewage treatment prepared by the method for preparing ceramic filler for sewage treatment according to claim 9, wherein the ceramic filler for sewage treatment is 10-30 wt% of wastewater.
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