CN116921384B - Method for preparing polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash - Google Patents
Method for preparing polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash Download PDFInfo
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- CN116921384B CN116921384B CN202311200518.5A CN202311200518A CN116921384B CN 116921384 B CN116921384 B CN 116921384B CN 202311200518 A CN202311200518 A CN 202311200518A CN 116921384 B CN116921384 B CN 116921384B
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- aluminum ash
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- salt
- secondary aluminum
- polymeric flocculant
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- 239000004568 cement Substances 0.000 title claims abstract description 96
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 87
- 239000000460 chlorine Substances 0.000 title claims abstract description 55
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 55
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 70
- 238000005660 chlorination reaction Methods 0.000 claims description 70
- 238000009835 boiling Methods 0.000 claims description 60
- 238000010438 heat treatment Methods 0.000 claims description 47
- 238000002386 leaching Methods 0.000 claims description 44
- 239000002893 slag Substances 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000001354 calcination Methods 0.000 claims description 32
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 32
- 239000001095 magnesium carbonate Substances 0.000 claims description 31
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 31
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 31
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 30
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical class [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 20
- 239000000428 dust Substances 0.000 claims description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000003546 flue gas Substances 0.000 claims description 7
- 150000001804 chlorine Chemical class 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 35
- 238000001179 sorption measurement Methods 0.000 abstract description 22
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000002956 ash Substances 0.000 description 68
- 239000000243 solution Substances 0.000 description 37
- 150000003839 salts Chemical class 0.000 description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 13
- 239000000292 calcium oxide Substances 0.000 description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 12
- 239000002699 waste material Substances 0.000 description 12
- 239000002351 wastewater Substances 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 10
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 9
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 9
- 238000000746 purification Methods 0.000 description 9
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 8
- 239000001110 calcium chloride Substances 0.000 description 8
- 229910001628 calcium chloride Inorganic materials 0.000 description 8
- 238000004364 calculation method Methods 0.000 description 8
- 239000001569 carbon dioxide Substances 0.000 description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 229910002091 carbon monoxide Inorganic materials 0.000 description 7
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 125000001309 chloro group Chemical group Cl* 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 5
- 238000004043 dyeing Methods 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- 239000013535 sea water Substances 0.000 description 5
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 238000007725 thermal activation Methods 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GQCYCMFGFVGYJT-UHFFFAOYSA-N [AlH3].[S] Chemical compound [AlH3].[S] GQCYCMFGFVGYJT-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 239000011083 cement mortar Substances 0.000 description 2
- 150000003841 chloride salts Chemical class 0.000 description 2
- IQYKECCCHDLEPX-UHFFFAOYSA-N chloro hypochlorite;magnesium Chemical compound [Mg].ClOCl IQYKECCCHDLEPX-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 229960004887 ferric hydroxide Drugs 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- OLZDXDPSDUSGIS-UHFFFAOYSA-N sulfinylmagnesium Chemical compound [Mg].S=O OLZDXDPSDUSGIS-UHFFFAOYSA-N 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- IHGSAQHSAGRWNI-UHFFFAOYSA-N 1-(4-bromophenyl)-2,2,2-trifluoroethanone Chemical compound FC(F)(F)C(=O)C1=CC=C(Br)C=C1 IHGSAQHSAGRWNI-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- COOGPNLGKIHLSK-UHFFFAOYSA-N aluminium sulfide Chemical compound [Al+3].[Al+3].[S-2].[S-2].[S-2] COOGPNLGKIHLSK-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a method for preparing a polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash. The method has simple preparation process, can synchronously prepare the polymeric flocculant and the salt-tolerant cement by using the secondary aluminum ash, and realizes the efficient recycling utilization of the secondary aluminum ash. The highest COD adsorption capacity of the flocculant prepared by using the secondary aluminum ash is 1341mg/g, the highest compressive strength of the prepared salt-tolerant cement is 40.17MPa, and the strength loss rate of the salt-immersed test piece is lower than 4%.
Description
Technical Field
The invention belongs to the field of harmless disposal and resource utilization of hazardous wastes, and particularly relates to a method for preparing a polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash.
Background
At present, the annual output of secondary aluminum ash in China exceeds 200 ten thousand tons, and the secondary aluminum ash is produced after primary aluminum ash is extracted. Two (II)The secondary aluminum ash is a dangerous waste, and is mostly granular or powdery. The secondary aluminum ash contains 40-60 wt.% of aluminum oxide and 10-30 wt.% of aluminum nitride,wt.%) and salts (sodium chloride, potassium chloride, fluoride; 10% -30%,wt.% or the like. Aluminum nitride and a small amount of aluminum carbide, aluminum phosphide and aluminum sulfide contained in the secondary aluminum ash react with water (hydrolysis reaction) to generate toxic, harmful, inflammable and explosive gases. Meanwhile, soluble salts contained in the secondary aluminum ash are easy to permeate into water or soil. Therefore, if the secondary aluminum ash is directly buried, not only is the risk of environmental pollution existed, but also the resource is wasted.
At present, the disposal and resource utilization of the secondary aluminum ash mainly comprises a fire method and a wet method. And disposal of secondary aluminum ash using both wet and fire methods has a number of problems. The problem that aluminum hydroxide generated after the aluminum ash is contacted with water covers aluminum ash particles to inhibit outgassing is solved by using a wet method to treat secondary aluminum ash. Meanwhile, after the secondary aluminum ash contacts water, the released toxic, harmful, inflammable and explosive gases are reasonably treated, and the generated ammonium reagent needs further purification and a proper downstream receiving end. In the wet process, the water washing liquid also needs to be further treated, and the water washing liquid is subjected to impurity removal and evaporative crystallization. The filter residue generated in the impurity removal process of the water washing liquid and the fluorine-containing chlorine-containing impurity salt obtained by evaporation are subjected to closed-loop treatment, and a proper application port is found. For the water washing slag, additional material stirring, mixing, drying and calcining treatment are needed. Therefore, the wet process chain is generally longer, the generated waste gas, waste liquid and waste salt are all required to be reasonably treated, and the wet process chain is matched with a proper application port, so that the technical application limit condition is more. The pyrogenic process mainly utilizes the properties of aluminum nitride that is easily oxidized at high temperature and the boiling point of salt is relatively low, and aluminum nitride and salt are removed through high temperature. However, the prior system of the pyrogenic process has the problems of low desalting efficiency, unreasonable compatibility of the front-stage raw materials, lack of subsequent deep treatment process of the calcined material and the like. Therefore, the method for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement by using the secondary aluminum ash not only expands the prior technical application aiming at the secondary aluminum ash, but also provides a reference for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement.
Disclosure of Invention
The invention aims to: the invention aims to provide a method for preparing a polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash.
The technical scheme is as follows: the method for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement by utilizing the secondary aluminum ash comprises the following steps of:
(1) Mixing tar and secondary aluminum ash, uniformly stirring, and grinding to obtain tar aluminum ash fine powder;
(2) Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, collecting dust from flue gas generated in the heating process, and then circularly absorbing the dust through a leaching tower, and collecting the reacted leaching solution when the pH value of the leaching solution is 5.5-7.5 to obtain aluminum chloride slurry;
(3) Dripping hydrochloric acid solution into aluminum chloride slurry, filtering, spraying the liquid into a roller drying box, and drying to obtain a polymeric flocculant;
(4) Collecting slag of the boiling chlorination furnace, mixing phosphogypsum, magnesite and slag of the boiling chlorination furnace, and grinding to obtain fine powder of the salt-tolerant cement precursor;
(5) Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse materials; grinding the cement coarse material to obtain the high-chlorine-resistant cement.
Further, the mass ratio of the tar to the secondary aluminum ash in the step (1) is 1.5-4.5:100.
Further, the polishing time in the step (1) is 0.5-4.5 hours.
Further, the heating temperature of the boiling chlorination furnace in the step (2) is 650-850 ℃, and the chlorine content in the boiling chlorination furnace is 85-95%.
Further, the eluent in the step (2) is 0.5-7.5M sodium hydroxide solution.
Further, the concentration of the hydrochloric acid solution in the step (3) is 0.5-7.5M, and the pH of the aluminum chloride slurry after the hydrochloric acid solution is dripped is 3-5.
Further, the mass ratio of phosphogypsum, magnesite and slag of the boiling chlorination furnace in the step (4) is 5-25:5-25:100, and the grinding time is 0.5-4.5 hours.
Further, the calcination time in the step (5) is 0.5-2.5 hours, and the calcination temperature is 850-1250 ℃.
Further, the polishing time in the step (5) is 0.5-4.5 hours.
Reaction mechanism: in the thermal activation process of the boiling chlorination furnace, chlorine is dissociated into chlorine atoms on the surface of tar carbon, and the chlorine atoms react with aluminum oxide, ferric oxide, calcium oxide and the like in the secondary aluminum ash to generate mixed gas-phase gases such as aluminum chloride, ferric chloride, calcium chloride, carbon monoxide, carbon dioxide and the like. In the chlorination heating process, aluminum nitride and aluminum carbide in the secondary aluminum ash are catalytically decomposed, so that oxygen atoms in aluminum oxide, ferric oxide and calcium oxide are promoted to combine with carbon and nitrogen contained in the aluminum oxide, ferric oxide and calcium oxide to generate carbon monoxide, carbon dioxide and nitrogen oxide, and the chlorination reaction and the aluminum chloride, ferric chloride and calcium chloride generating process are enhanced. After the mixed gas phase gas enters the leaching tower, the gas phases of aluminum chloride, ferric chloride, calcium chloride and the like are trapped in a sodium hydroxide solution and react with hydroxide to generate mixed precipitation slurry of aluminum hydroxide, ferric hydroxide and calcium hydroxide. Hydrochloric acid is added into the phase mixed precipitation slurry to promote the dissolution and hydrolytic polymerization of the precipitation slurry, and the inorganic polymeric flocculant is obtained after filtering and drying. In the calcination process of the salt-tolerant cement precursor fine powder, unreacted carbon residue in the slag of the boiling chlorination furnace is oxidized into carbon dioxide, and the calcium silicate-aluminum salt, the chloride salt, the magnesite and the phosphogypsum react with each other to generate a sulfur aluminum, magnesium oxychloride, magnesium oxysulfide and silicate blending gel cement system.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages: the method has simple preparation process, can synchronously prepare the polymeric flocculant and the salt-tolerant cement by using the secondary aluminum ash, and realizes the efficient recycling utilization of the secondary aluminum ash. The highest COD adsorption capacity of the flocculant prepared by using the secondary aluminum ash is 1341mg/g, the highest compressive strength of the prepared salt-tolerant cement is 40.17MPa, and the strength loss rate of the salt-immersed test piece is lower than 4%.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Secondary aluminum ash: the secondary aluminum ash is taken from Xinchang aerospace machine tool equipment limited company, is flue ash generated in the aluminum casting process, is sealed and stored by a waterproof belt and is used as a test sample, and mainly comprises the following components: 72.24% Al 2 O 3 、3.32%SiO 2 、7.48%MgO、1.24%CaO、3.01%Na 2 O、0.86%K 2 O、2.43%Fe 2 O 3 1.52% F, 5.37% Cl and other components (unavoidable impurities and loss on ignition);
tar: tar is from Jiangsu Pu Le Si Biotech Co., ltd, and mainly comprises 89.12% C, 3.26% H, 2.75% O, 1.08% N, 0.57% S and other elements;
phosphogypsum: phosphogypsum is obtained from a phosphorus fertilizer plant of Beacon, and the phosphogypsum sample mainly contains 52.70% SO 3 、37.01%CaO、4.37%SiO 2 、2.07%Al 2 O 3 、1.63%P 2 O 5 And other components (unavoidable impurities and loss on ignition);
magnesite: magnesite is mainly derived from Anshan of Liaoning and mainly comprises 44.38% MgO, 51.39% CO 2 、1.61%CaO、0.86%FeO、0.53%Al 2 O 3 And other components (unavoidable impurities and loss on ignition).
Example 1 Tar to Secondary aluminum Ash Mass ratio influence on the Properties of the prepared polymeric flocculant and high chlorine salt-tolerant Water
Mixing tar and secondary aluminum ash according to the mass ratio of 0.75:100, 1:100, 1.25:100, 1.5:100, 3:100, 4.5:100, 5:100, 5.5:100 and 6:100, uniformly stirring, and grinding for 0.5 hour to obtain tar aluminum ash fine powder. Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, circularly absorbing smoke generated in the heating process through a leaching tower after dust collection, and collecting leaching solution after reaction when the pH value of leaching waste liquid is 5.5 to obtain aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 650 ℃, the chlorine content in the boiling chlorination furnace is 85% after chlorine is introduced, and the leaching solution is 0.5M sodium hydroxide solution. Dropwise adding 0.5M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 3, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. Collecting slag of the boiling chlorination furnace, mixing phosphogypsum, magnesite and slag according to a mass ratio of 5:5:100, and grinding for 0.5 hour to obtain fine powder of the salt-tolerant cement precursor. And calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 0.5 hour, and the calcining temperature is 850 ℃. Grinding the cement coarse material for 0.5 hour to obtain the high-chlorine-resistant cement.
Performance test: the high-chlorine-resistant cement slurry prepared in the embodiment is prepared into tested mortar, wherein the mixed mortar is ISO standard mortar specified in the method for testing cement mortar strength (ISO method) GB/T17671-1999, and tap water is selected as water. The preparation of the mortar, the preparation of the test piece, the maintenance of the test piece and the measurement of the compressive strength of the 28d test piece are all carried out according to the GB/T17671-1999 standard of the cement mortar strength test method (ISO method).
Seawater soaking and strength loss calculation: and (3) completely soaking the 28-day-age test piece in seawater for 30 days, taking out the test piece for strength test, wherein the strength loss rate of the salt-immersed test piece is equal to the difference of the strength of the non-immersed 28-day-age test piece minus the strength of the immersed test piece divided by the percentage of the strength of the non-immersed 28-day-age test piece.
Purifying test of printing and dyeing waste liquid: 2g of polyaluminum sulfate flocculant is weighed and added into 1L of wastewater, and the wastewater is continuously stirred for 30min and centrifuged to obtain purified wastewater. Wherein, the test wastewater is taken to a waste liquid disposal tank of a printing and dyeing wastewater factory which is commonly done in Jiangsu, and the COD measured value is 3014.53mg/L.
COD concentration detection before and after wastewater purification treatment and calculation of COD adsorption capacity: the COD concentration of the waste water is determined according to the national standard "determination of COD of Water quality" dichromate method (GB 11914-1989). COD adsorption capacity is calculated according to equation (1), wherein Q COD For COD adsorption capacity (mg/g), c o And c t COD concentrations (mg/L) before and after the wastewater purification treatment are respectively,mthe flocculant adding amount (g) is V, and the waste liquid volume (L).
（1）
The test results of this example are shown in Table 1.
TABLE 1 influence of Tar to Secondary aluminum Ash Mass ratio on the Polymer flocculant prepared and the high chlorine salt-tolerant Cement Properties
| Mass ratio of tar to secondary aluminum ash | Flocculant COD adsorption capacity (mg/g) | Uniaxial compressive strength (MPa) of cement | Strength loss rate of salt immersed test piece |
| 0.75:100 | 345.87 | 16.31 | 19.29% |
| 1:100 | 563.29 | 21.66 | 17.31% |
| 1.25:100 | 775.23 | 25.14 | 14.55% |
| 1.5:100 | 1024.15 | 33.42 | 8.26% |
| 3:100 | 1095.78 | 35.91 | 7.34% |
| 4.5:100 | 1167.34 | 36.72 | 6.19% |
| 5:100 | 824.75 | 29.45 | 11.35% |
| 5.5:100 | 643.03 | 23.67 | 14.74% |
| 6:100 | 397.56 | 19.85 | 15.82% |
As can be seen from table 1, when the mass ratio of tar to secondary aluminum ash is less than 1.5:100 (as in table 1, the mass ratio of tar to secondary aluminum ash=1.25:100, 1:100, 0.75:100, and lower ratios not listed in table 1), the amount of tar added is small, the carbothermal chlorination reaction during the chlorination heating is insufficient, resulting in a significant decrease in the COD adsorption capacity of the prepared flocculant and the uniaxial compressive strength of the cement as the mass ratio of tar to secondary aluminum ash decreases, and the strength loss rate of the prepared cement-salt-immersed test piece increases significantly as the mass ratio of tar to secondary aluminum ash decreases. When the mass ratio of the tar to the secondary aluminum ash is equal to 1.5-4.5:100 (as in table 1, when the mass ratio of the tar to the secondary aluminum ash=1.5:100, 3:100, 4.5:100), chlorine is dissociated into chlorine atoms on the surface of the tar carbon in the thermal activation process of the boiling chlorination furnace, and the chlorine atoms react with aluminum oxide, ferric oxide, calcium oxide and the like in the secondary aluminum ash to generate mixed gas phase gases such as aluminum chloride, ferric chloride, calcium chloride, carbon monoxide, carbon dioxide and the like. In the chlorination heating process, aluminum nitride and aluminum carbide in the secondary aluminum ash are catalytically decomposed, so that oxygen atoms in aluminum oxide, ferric oxide and calcium oxide are promoted to combine with carbon and nitrogen contained in the aluminum oxide, ferric oxide and calcium oxide to generate carbon monoxide, carbon dioxide and nitrogen oxide, and the chlorination reaction and the aluminum chloride, ferric chloride and calcium chloride generating process are enhanced. Finally, the COD adsorption capacity of the prepared flocculant is higher than 1024mg/g, the uniaxial compressive strength of the prepared cement is higher than 33MPa, and the strength loss rate of the salt leaching test piece is lower than 8.3%. When the mass ratio of tar to secondary aluminum ash is greater than 4.5:100 (as in table 1, the mass ratio of tar to secondary aluminum ash=5:100, 5.5:100, 6:100, and higher ratios not listed in table 1), the addition of tar is excessive, other chloride impurities generated during the chlorination heating process are increased, resulting in a significant decrease in the COD adsorption capacity and uniaxial compressive strength of the prepared flocculant as the mass ratio of tar to secondary aluminum ash is further increased, while the strength loss rate of the prepared cement salt leaching specimen is significantly increased as the mass ratio of tar to secondary aluminum ash is further increased. Therefore, when the mass ratio of tar to secondary aluminum ash is equal to 1.5-4.5:100, the combination of benefits and costs is most beneficial to improving the performances of the prepared polymeric flocculant and high-chlorine salt-tolerant water.
EXAMPLE 2 Effect of boiling chlorination furnace heating temperature on the Property of the prepared polymeric flocculant and high chlorine salt-tolerant brine
Mixing tar and secondary aluminum ash according to the mass ratio of 4.5:100, uniformly stirring, and grinding for 2.5 hours to obtain tar aluminum ash fine powder. Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, circularly absorbing smoke generated in the heating process through a leaching tower after dust collection, and collecting leaching solution after reaction when the pH value of leaching waste liquid is 6.5 to obtain aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 575 ℃, 600 ℃, 625 ℃, 650 ℃, 750 ℃, 850 ℃, 875 ℃, 900 ℃, 925 ℃ and the chlorine content in the boiling chlorination furnace is 90 percent after chlorine is introduced, and the leaching solution is 4M sodium hydroxide solution. And (3) dropwise adding a 4M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 4, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. And collecting slag of the boiling chlorination furnace, mixing phosphogypsum, magnesite and slag according to the mass ratio of 15:15:100, and grinding for 2.5 hours to obtain the salt-tolerant cement precursor fine powder. And calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 1.5 hours, and the calcining temperature is 1050 ℃. Grinding the cement coarse material for 2.5 hours to obtain the high-chlorine-resistant cement.
The performance test, seawater immersion and strength loss calculation, printing and dyeing waste liquid purification test, COD concentration detection before and after wastewater purification treatment and COD adsorption capacity calculation are all the same as those of example 1, and the test results of this example are shown in Table 2.
TABLE 2 influence of heating temperature of a fluidized bed chlorination furnace on the properties of the prepared polymeric flocculant and high chlorine salt-resistant cement
| Heating temperature of boiling chlorination furnace | Flocculant COD adsorption capacity (mg/g) | Uniaxial compressive strength (MPa) of cement | Strength loss rate of salt immersed test piece |
| 575℃ | 627.19 | 20.49 | 13.56% |
| 600℃ | 688.72 | 24.81 | 10.92% |
| 625℃ | 726.38 | 30.04 | 9.48% |
| 650℃ | 1198.51 | 37.43 | 5.82% |
| 750℃ | 1224.84 | 37.95 | 4.14% |
| 850℃ | 1256.75 | 39.17 | 3.79% |
| 875℃ | 967.52 | 32.62 | 7.28% |
| 900℃ | 883.63 | 26.34 | 10.34% |
| 925℃ | 714.18 | 24.53 | 11.79% |
As can be seen from table 2, when the boiling chlorination furnace heating temperature is less than 650 ℃ (as in table 2, boiling chlorination furnace heating temperature=625 ℃, 600 ℃, 575 ℃ and lower values not listed in table 2), carbonization and carbothermal chlorination reactions are insufficient, resulting in a significant decrease in COD adsorption capacity of the prepared flocculant and uniaxial compressive strength of cement with a decrease in boiling chlorination furnace heating temperature, and a significant increase in strength loss rate of the prepared cement salt-immersed test piece with a decrease in boiling chlorination furnace heating temperature. When the heating temperature of the boiling chlorination furnace is 650-850 ℃ (as shown in table 2, the heating temperature of the boiling chlorination furnace=650 ℃, 750 ℃, 850 ℃), in the thermal activation process of the boiling chlorination furnace, chlorine is dissociated into chlorine atoms on the surface of tar carbon, and the chlorine atoms react with alumina, ferric oxide, calcium oxide and the like in the secondary aluminum ash to generate mixed gas phase gases such as aluminum chloride, ferric chloride, calcium chloride, carbon monoxide, carbon dioxide and the like. In the chlorination heating process, aluminum nitride and aluminum carbide in the secondary aluminum ash are catalytically decomposed, so that oxygen atoms in aluminum oxide, ferric oxide and calcium oxide are promoted to combine with carbon and nitrogen contained in the aluminum oxide, ferric oxide and calcium oxide to generate carbon monoxide, carbon dioxide and nitrogen oxide, and the chlorination reaction and the aluminum chloride, ferric chloride and calcium chloride generating process are enhanced. After the mixed gas phase gas enters the leaching tower, the gas phases of aluminum chloride, ferric chloride, calcium chloride and the like are trapped in a sodium hydroxide solution and react with hydroxide to generate mixed precipitation slurry of aluminum hydroxide, ferric hydroxide and calcium hydroxide. Hydrochloric acid is added into the phase mixed precipitation slurry to promote the dissolution and hydrolytic polymerization of the precipitation slurry, and the inorganic polymeric flocculant is obtained after filtering and drying. Finally, the COD adsorption capacity of the prepared flocculant is higher than 1198mg/g, the uniaxial compressive strength of the prepared cement is higher than 37MPa, and the strength loss rate of the salt leaching test piece is lower than 5.9%. When the boiling chlorination furnace heating temperature is greater than 850 ℃ (as in table 2, boiling chlorination furnace heating temperature=875 ℃, 900 ℃, 925 ℃ and higher values not listed in table 2), the boiling chlorination furnace heating temperature is too high, the materials are overburden, resulting in a significant decrease in the COD adsorption capacity of the prepared flocculant and the uniaxial compressive strength of the cement as the boiling chlorination furnace heating temperature is further increased, and a significant increase in the strength loss rate of the prepared cement salt leaching specimen as the boiling chlorination furnace heating temperature is further increased. Therefore, when the heating temperature of the boiling chlorination furnace is 650-850 ℃, the combination of benefits and costs is most beneficial to improving the performances of the prepared polymeric flocculant and high-chlorine salt-resistant cement.
Example 3 effect of phosphogypsum, magnesite and slag Mass ratio on the Property of the prepared polymeric flocculant and high chlorine salt-tolerant Water
Mixing tar and secondary aluminum ash according to the mass ratio of 4.5:100, uniformly stirring, and grinding for 4.5 hours to obtain tar aluminum ash fine powder. Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, collecting dust from flue gas generated in the heating process, then circularly absorbing the dust through a leaching tower, and collecting the reacted leaching solution when the pH value of the leaching solution is 7.5 to obtain aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 850 ℃, the chlorine content in the boiling chlorination furnace is 95% after introducing chlorine, and the leaching solution is 7.5M sodium hydroxide solution. And (3) dropwise adding a 7.5M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 5, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. Collecting the boiling chlorination furnace slag and mixing phosphogypsum, magnesite and slag according to the mass ratio of 2.5:5:100, 3:5:100, 4:5:100, 5:2.5:100, 5:3:100, 5:4:100, 5:5:100, 15:5:100, 25:5:100, 5:15:100, 25:25:100, 15:25:100, 25:25:100, 25:27.5:100, 25:30:100, 25:32.5:100, 27.5:25:100, 30:25:100, 32.5:25:100, and grinding for 4.5 hours to obtain the salt-tolerant cement precursor fine powder. Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 2.5 hours, and the calcining temperature is 1250 ℃. Grinding the cement coarse material for 4.5 hours to obtain the high-chlorine-resistant cement.
The performance test, seawater immersion and strength loss calculation, printing and dyeing waste liquid purification test, COD concentration detection before and after wastewater purification treatment and COD adsorption capacity calculation are all the same as those of example 1, and the test results of this example are shown in Table 3.
TABLE 3 influence of phosphogypsum, magnesite and slag mass ratio on the Property of the prepared polymeric flocculant and high-chlorine salt-tolerant Water
| Phosphogypsum, magnesite and slag mass ratio | Flocculant COD adsorption capacity (mg/g) | Uniaxial compressive strength (MPa) of cement | Strength loss rate of salt immersed test piece |
| 2.5:5:100 | 815.37 | 23.35 | 12.93% |
| 3:5:100 | 928.42 | 27.53 | 11.65% |
| 4:5:100 | 1023.55 | 30.69 | 8.97% |
| 5:2.5:100 | 824.62 | 25.12 | 12.04% |
| 5:3:100 | 954.76 | 29.36 | 10.32% |
| 5:4:100 | 1087.84 | 32.77 | 7.84% |
| 5:5:100 | 1209.65 | 38.03 | 4.36% |
| 15:5:100 | 1278.82 | 38.91 | 4.19% |
| 25:5:100 | 1315.24 | 39.52 | 3.88% |
| 5:15:100 | 1267.47 | 38.24 | 3.95% |
| 15:15:100 | 1320.71 | 39.45 | 3.36% |
| 25:15:100 | 1332.96 | 39.73 | 2.94% |
| 5:25:100 | 1335.48 | 39.11 | 3.76% |
| 15:25:100 | 1337.89 | 39.86 | 2.87% |
| 25:25:100 | 1341.75 | 40.17 | 2.53% |
| 25:27.5:100 | 1168.93 | 35.39 | 5.15% |
| 25:30:100 | 1006.34 | 34.05 | 7.21% |
| 25:32.5:100 | 973.52 | 31.28 | 8.79% |
| 27.5:25:100 | 1149.27 | 33.42 | 5.35% |
| 30:25:100 | 1057.63 | 29.76 | 8.38% |
| 32.5:25:100 | 965.18 | 28.14 | 9.56% |
As can be seen from table 3, when the phosphogypsum, magnesite and slag mass ratio is less than 5:5:100 (as in table 3, phosphogypsum, magnesite and slag mass ratio=4:5:100, 3:5:100, 2.5:5:100, 5:4:100, 5:3:100 and 5:2.5:100 are not listed in table 3), the phosphogypsum and magnesite are added in small amounts, phosphogypsum, magnesite and slag react insufficiently during calcination, resulting in that the COD adsorption capacity and cement uniaxial compressive strength of the prepared flocculant are significantly reduced as the phosphogypsum, magnesite and slag mass ratio are reduced, and the strength loss rate of the prepared cement salt leaching test piece is significantly increased as the phosphogypsum, magnesite and slag mass ratio are reduced. When the mass ratio of phosphogypsum, magnesite and slag is equal to 5-25:5-25:100 (as in table 3, phosphogypsum, magnesite and slag mass ratio=5:5:100, 15:5:100, 25:5:100, 5:15:100, 15:15:100, 25:15:100, 5:25:100, 15:25:100, 25:25:100), unreacted carbon residue in the slag of the boiling chlorination furnace is oxidized into carbon dioxide in the calcination process of the fine powder of the salt-tolerant cement precursor, and the calcium silicate, chloride salt, magnesite and phosphogypsum react with each other to generate a sulfur-aluminum, magnesium oxychloride, magnesium oxysulfide and silicate blending gelling cement system. Finally, the COD adsorption capacity of the prepared flocculant is higher than 1209mg/g, the uniaxial compressive strength of the prepared cement is higher than 38MPa, and the strength loss rate of the salt leaching test piece is lower than 4.4%. When phosphogypsum, magnesite and slag mass ratio is greater than 25:25:100 (as in table 3, phosphogypsum, magnesite and slag mass ratio=25:27.5:100, 25:30:100, 25:32.5:100, 27.5:25:100, 30:25:100 and 32.5:25:100, and higher ratios not listed in table 3), phosphogypsum and magnesite are added in excess, the material reaction during calcination is unbalanced, resulting in that the COD adsorption capacity of the prepared flocculant and the uniaxial compressive strength of cement are significantly reduced as the phosphogypsum, magnesite and slag mass ratio are further increased, and the strength loss rate of the prepared cement salt leaching test piece is significantly increased as the phosphogypsum, magnesite and slag mass ratio are further increased. Therefore, when the mass ratio of phosphogypsum, magnesite and slag is equal to 5-25:5-25:100, the combination of benefits and costs is most beneficial to improving the performances of the prepared polymeric flocculant and high-chlorine salt-tolerant cement.
Comparative examples different preparation processes affect the properties of the prepared polymeric flocculant and high chlorine salt brine resistant
The process comprises the following steps: mixing tar and secondary aluminum ash according to the mass ratio of 4.5:100, uniformly stirring, and grinding for 4.5 hours to obtain tar aluminum ash fine powder. Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, collecting dust from flue gas generated in the heating process, then circularly absorbing the dust through a leaching tower, and collecting the reacted leaching solution when the pH value of the leaching solution is 7.5 to obtain aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 850 ℃, the chlorine content in the boiling chlorination furnace is 95% after introducing chlorine, and the leaching solution is 7.5M sodium hydroxide solution. And (3) dropwise adding a 7.5M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 5, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. Collecting slag of the boiling chlorination furnace, mixing phosphogypsum, magnesite and slag according to the mass ratio of 25:25:100, and grinding for 4.5 hours to obtain fine powder of the salt-tolerant cement precursor. Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 2.5 hours, and the calcining temperature is 1250 ℃. Grinding the cement coarse material for 4.5 hours to obtain the high-chlorine-resistant cement.
Comparison Process 1: and (3) blowing secondary aluminum ash into a boiling chlorination furnace for heating, wherein flue gas generated in the heating process is circularly absorbed through a leaching tower after dust collection, and when the pH of the leaching liquid is 7.5, the leaching liquid after reaction is collected to obtain aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 850 ℃, the chlorine content in the boiling chlorination furnace is 95% after chlorine is introduced, and the leaching liquid is 7.5M sodium hydroxide solution. And (3) dropwise adding a 7.5M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 5, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. Collecting slag of the boiling chlorination furnace, mixing phosphogypsum, magnesite and slag according to the mass ratio of 25:25:100, and grinding for 4.5 hours to obtain fine powder of the salt-tolerant cement precursor. Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 2.5 hours, and the calcining temperature is 1250 ℃. Grinding the cement coarse material for 4.5 hours to obtain the high-chlorine-resistant cement.
Comparison process 2: mixing tar and secondary aluminum ash according to the mass ratio of 4.5:100, uniformly stirring, and grinding for 4.5 hours to obtain tar aluminum ash fine powder. Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, collecting dust from flue gas generated in the heating process, then circularly absorbing the dust through a leaching tower, and collecting leaching solution after reaction when the pH value of the circularly leached waste liquid is 7.5, thereby obtaining aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 850 ℃, the chlorine content in the boiling chlorination furnace is 95% after introducing chlorine, and the leaching solution is 7.5M sodium hydroxide solution. And (3) dropwise adding a 7.5M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 5, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. Collecting slag of the boiling chlorination furnace, mixing magnesite and slag according to a mass ratio of 25:100, and grinding for 4.5 hours to obtain fine powder of the salt-tolerant cement precursor. Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 2.5 hours, and the calcining temperature is 1250 ℃. Grinding the cement coarse material for 4.5 hours to obtain the high-chlorine-resistant cement.
Contrast process 3: mixing tar and secondary aluminum ash according to the mass ratio of 4.5:100, uniformly stirring, and grinding for 4.5 hours to obtain tar aluminum ash fine powder. Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, collecting dust from flue gas generated in the heating process, then circularly absorbing the dust through a leaching tower, and collecting the reacted leaching solution when the pH value of the leaching solution is 7.5 to obtain aluminum chloride slurry, wherein the heating temperature of the boiling chlorination furnace is 850 ℃, the chlorine content in the boiling chlorination furnace is 95% after introducing chlorine, and the leaching solution is 7.5M sodium hydroxide solution. And (3) dropwise adding a 7.5M hydrochloric acid solution into the aluminum chloride slurry, adjusting the pH of the aluminum chloride slurry to 5, filtering, spraying the liquid into a roller drying box, and drying to obtain the polymeric flocculant. And collecting slag of the boiling chlorination furnace, mixing phosphogypsum and slag according to a mass ratio of 25:100, and grinding for 4.5 hours to obtain fine powder of the salt-tolerant cement precursor. Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse material, wherein the calcining time is 2.5 hours, and the calcining temperature is 1250 ℃. Grinding the cement coarse material for 4.5 hours to obtain the high-chlorine-resistant cement.
The performance test, seawater immersion and strength loss calculation, printing and dyeing waste liquid purification test, COD concentration detection before and after wastewater purification treatment and COD adsorption capacity calculation were all the same as in example 1, and the test results of this example are shown in Table 4.
TABLE 4 influence of different preparation processes on the properties of the prepared polymeric flocculant and high-chlorine salt-tolerant water
| Type of process | Flocculant COD adsorption capacity (mg/g) | Uniaxial compressive strength (MPa) of cement | Strength loss rate of salt immersed test piece |
| The process of the invention | 1341.75 | 40.17 | 2.53% |
| Comparative Process 1 | 467.08 | 16.64 | 45.95% |
| Comparative Process 2 | 1339.27 | 20.45 | 18.73% |
| Comparative Process 3 | 1334.11 | 19.37 | 24.86% |
As can be seen from Table 4, the COD adsorption capacity of the flocculant prepared by the process is far higher than that of the flocculant prepared by the contrast process 1, the uniaxial compressive strength of the cement prepared by the process is far higher than that of the cement prepared by the contrast process 1, the contrast process 2 and the contrast process 3, and the strength loss rate of the cement salt leaching test piece prepared by the process is far lower than that of the cement prepared by the contrast process 1, the contrast process 2 and the contrast process 3.
Claims (9)
1. A method for preparing a polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash, which is characterized by comprising the following steps:
(1) Mixing tar and secondary aluminum ash, uniformly stirring, and grinding to obtain tar aluminum ash fine powder;
(2) Blowing tar aluminum ash fine powder into a boiling chlorination furnace for heating, collecting dust from flue gas generated in the heating process, and then circularly absorbing the dust through a leaching tower, and collecting the reacted leaching solution when the pH value of the leaching solution is 5.5-7.5 to obtain aluminum chloride slurry;
(3) Dripping hydrochloric acid solution into aluminum chloride slurry, filtering, spraying the liquid into a roller drying box, and drying to obtain a polymeric flocculant;
(4) Collecting slag of the boiling chlorination furnace, mixing phosphogypsum, magnesite and slag of the boiling chlorination furnace, and grinding to obtain fine powder of the salt-tolerant cement precursor;
(5) Calcining the fine powder of the salt-tolerant cement precursor to obtain cement coarse materials; grinding the cement coarse material to obtain the high-chlorine-resistant cement.
2. The method for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement by using the secondary aluminum ash according to claim 1, wherein the mass ratio of tar to the secondary aluminum ash in the step (1) is 1.5-4.5:100.
3. The method for preparing a polymeric flocculant and high chlorine salt-tolerant cement using secondary aluminum ash according to claim 1, wherein the grinding time in the step (1) is 0.5 to 4.5 hours.
4. The method for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement by using the secondary aluminum ash according to claim 1, wherein the heating temperature of the boiling chlorination furnace in the step (2) is 650-850 ℃, and the chlorine content in the boiling chlorination furnace is 85% -95%.
5. The method for preparing a polymeric flocculant and high-chlorine salt-tolerant cement by using secondary aluminum ash according to claim 1, wherein the leaching solution in the step (2) is 0.5-7.5M sodium hydroxide solution.
6. The method for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement by using the secondary aluminum ash according to claim 1, wherein the concentration of the hydrochloric acid solution in the step (3) is 0.5-7.5M, and the pH of the aluminum chloride slurry after the hydrochloric acid solution is dripped is 3-5.
7. The method for preparing the polymeric flocculant and the high-chlorine salt-tolerant cement by using the secondary aluminum ash according to claim 1, wherein the mass ratio of phosphogypsum, magnesite and slag of a boiling chlorination furnace in the step (4) is 5-25:5-25:100, and the grinding time is 0.5-4.5 hours.
8. The method for preparing a polymeric flocculant and a high chlorine salt tolerant cement using secondary aluminum ash according to claim 1, wherein the calcination time in the step (5) is 0.5 to 2.5 hours, and the calcination temperature is 850 to 1250 ℃.
9. The method for preparing a polymeric flocculant and a high chlorine salt-tolerant cement using secondary aluminum ash according to claim 1, wherein the grinding time in the step (5) is 0.5 to 4.5 hours.
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