CN113955818A - Preparation method of composite polyaluminum ferric chloride water treatment agent - Google Patents
Preparation method of composite polyaluminum ferric chloride water treatment agent Download PDFInfo
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- CN113955818A CN113955818A CN202111266739.3A CN202111266739A CN113955818A CN 113955818 A CN113955818 A CN 113955818A CN 202111266739 A CN202111266739 A CN 202111266739A CN 113955818 A CN113955818 A CN 113955818A
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- ferric chloride
- polyaluminum ferric
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 title claims abstract description 85
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims abstract description 85
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 60
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 60
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000010438 heat treatment Methods 0.000 claims abstract description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052742 iron Inorganic materials 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 18
- 239000003381 stabilizer Substances 0.000 claims abstract description 18
- 230000003213 activating effect Effects 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 15
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000013329 compounding Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 26
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000292 calcium oxide Substances 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 description 11
- 229910019142 PO4 Inorganic materials 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 239000010452 phosphate Substances 0.000 description 10
- -1 iron ions Chemical class 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- 238000002386 leaching Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000007873 sieving Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000012190 activator Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical group OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 230000033001 locomotion Effects 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/11—Turbidity
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a preparation method of a composite polyaluminum ferric chloride water treatment agent, and relates to the technical field of water treatment. A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps: crushing kaolin tailings, and calcining the crushed kaolin tailings and an activating agent at high temperature; adding the calcined kaolin tailings into acid liquor, and carrying out microwave heating; carrying out suction filtration on the supernatant after microwave heating, adding calcium aluminate powder, a stabilizer and an alkali regulator into the filtrate, carrying out curing polymerization, cooling and concentrating to obtain polyaluminum ferric chloride; compounding the polyaluminum ferric chloride and graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent. The composite polyaluminum ferric chloride water treatment agent with strong adsorption capacity can be prepared by the preparation method.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method of a compound polyaluminum ferric chloride water treatment agent.
Background
Water is a source of life and one of the most valuable natural resources on which humans rely for survival. With the development of economy and society and the increase of population, the shortage of water resources in China will face more and more serious challenges. However, the growing water pollution further exacerbates the otherwise serious water shortage contradiction. One is industrial pollution. The industrial wastewater is an important pollution source and has the characteristics of large amount, wide range, complex components, high toxicity, difficult purification, difficult treatment and the like. In China, the pollution discharge problem of village and town enterprises is not effectively solved all the time, and industrial wastewater pollutes farmlands and rivers and harms the life health of people. Secondly, agricultural pollution. Agricultural pollution includes livestock manure, pesticides, fertilizers, and the like. China is one of the most serious countries with water and soil loss in the world, and a large amount of pesticides and chemical fertilizers flow into rivers, lakes and reservoirs along with surface soil, so that two thirds of lakes are harmed by eutrophication pollution of different degrees, algae and other organisms are abnormally bred, the transparency of a water body and dissolved oxygen are changed, and the water quality is deteriorated. And thirdly, living pollution. The domestic pollution is mainly various detergents and sewage, garbage, excrement and the like used in urban life, and contains more nitrogen, phosphorus, sulfur and pathogenic bacteria.
With the progress of science and technology, many water treatment methods such as ion exchange, adsorption, chemical oxidation, biochemical, electrodialysis, and flocculation precipitation have been developed. The method with the widest application, the strongest applicability and the lowest cost is the flocculation precipitation method. Various suspended matter impurities and colloidal particles in a sol state exist in the wastewater body, relative sedimentation stability and polymerization stability are presented due to the action of Brownian motion and electrostatic repulsive force, and coagulant or flocculant is added into water to destroy the stability of sol, so that the colloid and the suspended matter particles in the water are flocculated into larger flocs to be separated from the water, and the purpose of purifying the water quality is achieved.
However, the effect of the existing flocculating agent is general, and the development of a new high-efficiency coagulant becomes a research focus.
Disclosure of Invention
The invention aims to provide a preparation method of a composite polyaluminum ferric chloride water treatment agent, and the composite polyaluminum ferric chloride water treatment agent with strong adsorption capacity can be prepared by the preparation method.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The embodiment of the application provides a preparation method of a composite polyaluminium chloride molten iron treatment agent, which comprises the following steps:
crushing kaolin tailings, and calcining the crushed kaolin tailings and an activating agent at high temperature;
adding the calcined kaolin tailings into acid liquor, and carrying out microwave heating;
carrying out suction filtration on the supernatant after microwave heating, adding calcium aluminate powder, a stabilizer and an alkali regulator into the filtrate, carrying out curing polymerization, cooling and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride and graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:
according to the invention, kaolin tailings are calcined, acid-leached and cured to form polyaluminum ferric chloride, and then the polyaluminum ferric chloride and graphite powder are compounded to obtain the composite polyaluminum ferric chloride water treatment agent with strong adsorption capacity. The addition of an activator during the calcination step can modify the crystalline form of the alumina, thereby allowing faster leaching during the acid leaching step; the stabilizer is added in the curing polymerization step and can be complexed with iron ions in the solution through P-O bonds, so that the coordination of the iron ions and hydroxyl groups in the solution can be reduced, the dehydrogenation reaction is not easy to occur, the hydrolysis of ferric chloride is inhibited, the stability of the polyaluminum ferric chloride can be effectively improved, and the better stability performance is achieved. The high-purity graphite powder is adopted to compound the polyaluminum ferric chloride, and a macromolecular structure with an ultra-large specific surface area can be formed by the interaction of the high-purity graphite powder and metal ions, so that the macromolecular structure is more beneficial to the adsorption of pollutants in water. The water treatment agent which has extremely strong effect of reducing COD and turbidity in water can be prepared by adopting the preparation method.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
crushing kaolin tailings, and calcining the crushed kaolin tailings and an activating agent at high temperature;
adding the calcined kaolin tailings into acid liquor, and carrying out microwave heating;
carrying out suction filtration on the supernatant after microwave heating, adding calcium aluminate powder, a stabilizer and an alkali regulator into the filtrate, carrying out curing polymerization, cooling and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride and graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
The kaolin tailing contains other useful components such as silicon dioxide, aluminum oxide, potassium oxide, sodium oxide, calcium oxide and the like, and the aluminum oxide in the kaolin tailing is mainly alpha-Al2O3Is present in a form which is very low in activity and hardly reacts with an acid, and therefore, it is necessary to subject α -Al to2O3Conversion to gamma-Al2O3So that the aluminum element in the kaolin tailings can be effectively utilized. Soaking the calcined kaolin tailings with acid so as to leach aluminum and iron; and (2) heating and polymerizing the filtrate containing the aluminum element and the iron element, concentrating to obtain polyaluminum ferric chloride containing the aluminum element and the iron element, and compounding the polyaluminum ferric chloride with high-purity graphite powder to finally obtain the water treatment agent with strong adsorption capacity.
In some embodiments of the present invention, the activating agent is sodium carbonate and sodium hydroxide in a weight ratio of (2-3): 1. Both sodium carbonate and sodium hydroxide can alter the crystalline form of the alumina, allowing it to leach more quickly in the acid leaching step.
In some embodiments of the present invention, the weight ratio of the kaolin tailing to the activator is 1: (0.6-0.8). The mixture of sodium carbonate and sodium hydroxide is used as an activating agent, so that a better activating effect can be achieved, and the using amount of the activating agent is reduced.
In some embodiments of the inventionThe calcining temperature is 600-800 ℃, and the calcining time is 1.5-3 h. When the calcining temperature is more than 800 ℃, the gamma-Al2O3Will generate reverse reaction to generate alpha-Al2O3Therefore, calcination at 800 ℃ or lower is required to prevent the activity of alumina from being lowered.
In some embodiments of the present invention, the ratio of the acid solution to the solid raw material is (3-5): 1, the acid solution is hydrochloric acid with the mass fraction of 15-20%. Hydrochloric acid has certain volatility, the leaching rate of aluminum is higher when the concentration of hydrochloric acid is too high, but the reaction is too violent after the concentration of hydrochloric acid is too high, the operation is inconvenient, danger is easy to cause, and in addition, the volatilization of hydrochloric acid is promoted by the too high concentration of hydrochloric acid, the loss is increased, and the environment is also adversely affected.
In some embodiments of the present invention, the microwave heating power is 250-300W, the microwave heating time is 5-8 min, and the temperature is 65-80 ℃. The microwave heating can increase the movement of acid liquor and kaolin and accelerate the acid leaching process.
In some embodiments of the present invention, the alkali regulator is one or more of calcium oxide, ammonia water, sodium hydroxide and sodium carbonate, and the alkali regulator regulates the alkalization degree of the filtrate to be 0.5 to 1.5. The alkalizer is also used for adjusting the pH value of the solution, when the pH value is increased, the hydrolysis speed of iron ions is reduced, the iron ions are easy to saturate, the proportion of aluminum elements and iron elements in the final polyaluminum ferric chloride is influenced, and the adsorption capacity of the water treatment agent is further influenced.
In some embodiments of the invention, the calcium aluminate powder adjusts the mass ratio of aluminum to iron in the filtrate to be (7-9): 1, the polyaluminum ferric chloride in this ratio can have better adsorption capacity. Meanwhile, the calcium aluminate powder can also improve the basicity of the whole solution and promote polymerization.
In some embodiments of the invention, the stabilizer is a dihydrogen phosphate or a phosphate. The addition of the substance containing phosphate radical can effectively improve the stability of the polyaluminum ferric chloride and achieve better stability, and the principle is that the phosphate radical can be complexed with iron ions in the solution through P-O bonds, so that the coordination of the iron ions and hydroxyl in the solution can be reduced, the dehydrogenation reaction is not easy to occur, and the hydrolysis of ferric chloride is inhibited.
In some embodiments of the present invention, the curing polymerization temperature is 50 to 60 ℃, and the curing polymerization time is 6 to 8 hours. If the aging temperature is too high or the aging polymerization time is too long, excessive hydrolysis may occur, resulting in a large aluminum hydroxide content in the polyaluminum ferric chloride.
In some embodiments of the present invention, the mass ratio of the polyaluminum ferric chloride to the graphite powder is (2-3): 1, the carbon content of the graphite powder is more than or equal to 99.99 percent. According to the invention, the polymeric aluminum ferric chloride is compounded by adopting the high-purity graphite powder, and a macromolecular structure with an overlarge specific surface area can be formed by utilizing the interaction of the high-purity graphite powder and metal ions, and the macromolecular structure is more beneficial to the adsorption of pollutants in water.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 300g of kaolin tailings, crushing and sieving the kaolin tailings by a 60-mesh sieve, collecting sieved powder, adding 60g of sodium hydroxide and 120g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at 700 ℃ for 2 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 3 times of 20% (mass fraction) hydrochloric acid, soaking the kaolin tailings, and then transferring the kaolin tailings into a microwave heating device, wherein the heating power is set to be 300W, the heating temperature is set to be 70 ℃, and the heating time is set to be 8 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 1 and the pH value to 2.5, heating to 55 ℃ for curing polymerization, stopping heating after curing for 8h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.5 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Example 2
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 300g of kaolin tailings, crushing and sieving the kaolin tailings by a sieve of 80 meshes, collecting sieved powder, adding 60g of sodium hydroxide and 180g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at 800 ℃ for 1.5 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 15% (mass fraction) hydrochloric acid in an amount which is 5 times the mass of the calcined kaolin tailings, soaking the kaolin tailings, and then transferring the kaolin tailings into a microwave heating device, wherein the heating power is set to be 250W, the heating temperature is set to be 70 ℃, and the heating time is set to be 7 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 1.5 and the pH value to 3, heating to 60 ℃ for curing polymerization, stopping heating after curing for 6h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.4 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Example 3
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 300g of kaolin tailings, crushing and sieving the kaolin tailings by a 60-mesh sieve, collecting sieved powder, adding 80g of sodium hydroxide and 160g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at the temperature of 600 ℃ for 1.5 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 18 mass percent (mass fraction) hydrochloric acid 4 times of the calcined kaolin tailings, soaking the calcined kaolin tailings, and then transferring the calcined kaolin tailings into a microwave heating device, wherein the heating power is set to be 2850W, the heating temperature is set to be 75 ℃, and the heating time is set to be 6 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 2.5 and the pH value to 2, heating to 50 ℃ for curing polymerization, stopping heating after curing for 6.5h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.5 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Example 4
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 300g of kaolin tailings, crushing and sieving the kaolin tailings by a sieve of 80 meshes, collecting sieved powder, adding 60g of sodium hydroxide and 120g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at the temperature of 650 ℃ for 2.5 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 4 times of 20% (mass fraction) hydrochloric acid, soaking the kaolin tailings, and then transferring the kaolin tailings into a microwave heating device, wherein the heating power is set to be 300W, the heating temperature is set to be 80 ℃, and the heating time is set to be 5 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 1.5 and the pH value to 3, heating to 60 ℃ for curing polymerization, stopping heating after curing for 7h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.5 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Example 5
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 300g of kaolin tailings, crushing and sieving the kaolin tailings by a 60-mesh sieve, collecting sieved powder, adding 60g of sodium hydroxide and 180g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at the temperature of 650 ℃ for 2.5 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 15% (mass fraction) hydrochloric acid in an amount which is 5 times the mass of the calcined kaolin tailings, soaking the kaolin tailings, and then transferring the kaolin tailings into a microwave heating device, wherein the heating power is set to be 250W, the heating temperature is set to be 75 ℃, and the heating time is set to be 7 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 2.5 and the pH value to 2.5, heating to 60 ℃ for curing polymerization, stopping heating after curing for 6h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.4 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Example 6
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 400g of kaolin tailings, crushing and sieving the kaolin tailings by a sieve of 80 meshes, collecting sieved powder, adding 100g of sodium hydroxide and 200g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at the calcining temperature of 750 ℃ for 1.5 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 20% (mass fraction) hydrochloric acid in an amount which is 5 times the mass of the calcined kaolin tailings, soaking the kaolin tailings, and then transferring the kaolin tailings into a microwave heating device, wherein the heating power is set to be 300W, the heating temperature is set to be 70 ℃, and the heating time is set to be 8 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 1.5 and the pH value to 3, heating to 55 ℃ for curing polymerization, stopping heating after curing for 8h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.4 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Example 7
A preparation method of a compound polyaluminium chloride molten iron treatment agent comprises the following steps:
weighing 400g of kaolin tailings, crushing and sieving the kaolin tailings by a 60-mesh sieve, collecting sieved powder, adding 100g of sodium hydroxide and 200g of sodium carbonate as activating agents, uniformly mixing, transferring the mixture to a muffle furnace for calcining at the temperature of 700 ℃ for 3 hours;
placing the calcined kaolin tailings into a three-necked bottle, adding 3 times of 20% (mass fraction) hydrochloric acid, soaking the kaolin tailings, and then transferring the kaolin tailings into a microwave heating device, wherein the heating power is set to be 300W, the heating temperature is set to be 70 ℃, and the heating time is set to be 6 min;
filtering the supernatant heated by microwave, adding calcium aluminate powder, dihydric phosphate and calcium oxide into the filtrate, adjusting the alkalization degree of the filtrate to 1.5 and the pH value to 2.5, heating to 55 ℃ for curing polymerization, stopping heating after curing for 8h, cooling to room temperature, and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride with 0.4 times of high-purity graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
Experimental example 1
Experiments were carried out on the composite polyaluminum ferric chloride water treatment agent prepared in embodiments 1 to 7 of the present invention, and a commercially available single aluminum chloride water treatment agent, a commercially available ferric chloride water treatment agent, and a non-compounded aluminum ferric chloride water treatment agent.
The experimental process is as follows: 1kg of yellow river water is taken, is rapidly and evenly distributed into 10 beakers after being stirred at a high speed, experiment groups 1-10 are numbered in the beakers, the solution is absorbed after being fully stirred to measure COD, turbidity and light transmittance, the compound polyaluminum ferric chloride water treatment agent prepared in the embodiments 1-7 is added into the beakers of the experiment groups 1-7, a commercially available aluminum chloride water treatment agent product is added into an experiment group 8, a commercially available ferric chloride water treatment agent product is added into an experiment group 9, and a non-compounded polyaluminum ferric chloride water treatment agent is added into an experiment group 10. The quality of the added water treatment was the same in 10 experimental groups. After the addition, the mixture was stirred at a speed of 50r/min for 10min, and the supernatant was taken by a pipette 3cm below the liquid surface to measure COD, turbidity and light transmittance, and the results were shown in Table 1 by comparing the data before the treatment.
TABLE 1
As can be seen from Table 1, the composite polyaluminum ferric chloride water treatment agent prepared in examples 1 to 7 has a good and stable treatment effect on yellow river water, the COD removal rate can reach more than 70%, the turbidity reduction rate can reach more than 99%, and the light transmittance is obviously improved; the effect of the water treatment agent is better than that of finished aluminum chloride water treatment agents and ferric chloride water treatment agents purchased from the market, and in addition, the effect of the polyaluminum ferric chloride water treatment agent which is not compounded with high-purity graphite powder is obviously reduced compared with that of experimental groups 1-7, which shows that the graphite powder can increase the adsorption capacity of the polyaluminum ferric chloride water treatment agent.
Experimental example 2
This example explores the effect of the addition of the stabilizer on the polyaluminum ferric chloride water treatment agent.
This experimental example was provided with 7 experimental groups, differing from example 1 in that: the stabilizer is not added in the experimental group 1, the adding amount of the stabilizer in the experimental group 2 is P/Fe of 0.03, the adding amount of the stabilizer in the experimental group 3 is P/Fe of 0.05, the adding amount of the stabilizer in the experimental group 4 is P/Fe of 0.08, the adding amount of the stabilizer in the experimental group 5 is P/Fe of 0.1, the adding amount of the stabilizer in the experimental group 6 is P/Fe of 0.15, and the adding amount of the stabilizer in the experimental group 7 is P/Fe of 0.2. The experimental groups were sealed and left to stand, and after 7 days, the experimental groups were added to yellow river water in the same mass, and after the addition, the mixture was stirred at a speed of 50r/min for 10min, and then the supernatant was taken 3cm below the liquid surface by a pipette, and COD and turbidity were measured, and the results of the treatment were calculated by comparing the raw data of the yellow river water, and the results are shown in table 2.
TABLE 2
| Grouping | COD reduction ratio (%) | Turbidity removal rate (%) |
| Experimental group 1 | 66.1 | 98.73 |
| Experimental group 2 | 68.5 | 99.21 |
| Experimental group 3 | 71 | 99.62 |
| Experimental group 4 | 71.2 | 99.52 |
| Experimental group 5 | 72.3 | 99.87 |
| Experimental group 6 | 72.4 | 99.62 |
| Experimental group 7 | 72.1 | 99.65 |
As can be seen from Table 2, the COD reduction rate and turbidity removal rate of the experimental group 1 are obviously lower than those of the other groups, which indicates that the ferric chloride is hydrolyzed without adding a stabilizer, so that the stability of the polyaluminum ferric chloride is influenced, and the adsorption effect of the polyaluminum ferric chloride is influenced; as can be seen from experimental groups 2-7, the COD reduction rate and the turbidity removal rate gradually increase to be stable or decrease with the increase of the addition amount of the stabilizer, and the stabilization effect is the best when the addition amount of the stabilizer is P/Fe equal to 0.1.
In summary, the embodiment of the invention provides a preparation method of a composite polyaluminum ferric chloride water treatment agent. According to the invention, kaolin tailings are calcined, acid-leached and cured to form polyaluminum ferric chloride, and then the polyaluminum ferric chloride and graphite powder are compounded to obtain the composite polyaluminum ferric chloride water treatment agent with strong adsorption capacity. The addition of an activator during the calcination step can modify the crystalline form of the alumina, thereby allowing faster leaching during the acid leaching step; the stabilizer is added in the curing polymerization step and can be complexed with iron ions in the solution through P-O bonds, so that the coordination of the iron ions and hydroxyl groups in the solution can be reduced, the dehydrogenation reaction is not easy to occur, the hydrolysis of ferric chloride is inhibited, the stability of the polyaluminum ferric chloride can be effectively improved, and the better stability performance is achieved. The high-purity graphite powder is adopted to compound the polyaluminum ferric chloride, and a macromolecular structure with an ultra-large specific surface area can be formed by the interaction of the high-purity graphite powder and metal ions, so that the macromolecular structure is more beneficial to the adsorption of pollutants in water. The water treatment agent which has extremely strong effect of reducing COD and turbidity in water can be prepared by adopting the preparation method.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a compound polyaluminium chloride molten iron treating agent is characterized by comprising the following steps:
crushing kaolin tailings, and calcining the crushed kaolin tailings and an activating agent at high temperature;
adding the calcined kaolin tailings into acid liquor, and carrying out microwave heating;
carrying out suction filtration on the supernatant after microwave heating, adding calcium aluminate powder, a stabilizer and an alkali regulator into the filtrate, carrying out curing polymerization, cooling and concentrating to obtain polyaluminum ferric chloride;
compounding the polyaluminum ferric chloride and graphite powder to obtain the composite polyaluminum ferric chloride water treatment agent.
2. The preparation method of the compound polyaluminum ferric chloride treating agent according to claim 1, wherein the activating agent is sodium carbonate and sodium hydroxide in a weight ratio of (2-3): 1.
3. The preparation method of the composite polyaluminum ferric chloride treating agent according to claim 2, wherein the ratio of the kaolin tailings to the activating agent is 1: (0.6-0.8).
4. The preparation method of the composite polyaluminum ferric chloride treating agent according to claim 1, wherein the calcining temperature is 600-800 ℃ and the calcining time is 1.5-3 h.
5. The preparation method of the composite polyaluminum ferric chloride treating agent according to claim 1, wherein the ratio of the acid liquid to the solid raw material is (3-5): 1, the acid solution is hydrochloric acid with the mass fraction of 15-20%.
6. The preparation method of the composite polyaluminum ferric chloride treating agent according to claim 1, wherein the microwave heating power is 250-300W, the microwave heating time is 5-8 min, and the temperature is 65-80 ℃.
7. The preparation method of the compound polyaluminum ferric chloride treating agent according to claim 1, wherein the alkali regulator is one or more of calcium oxide, ammonia water, sodium hydroxide and sodium carbonate, and the alkali regulator regulates the alkalization degree of the filtrate to be 0.5-1.5.
8. The preparation method of the compound polyaluminium chloride molten iron treatment agent according to claim 1, wherein the calcium aluminate powder is used for adjusting the mass ratio of aluminum to iron in the filtrate to (7-9): 1.
9. the preparation method of the composite polyaluminum ferric chloride treating agent according to claim 1, wherein the curing and polymerizing temperature is 50-60 ℃ and the curing and polymerizing time is 6-8 h.
10. The preparation method of the composite polyaluminum ferric chloride treating agent according to claim 1, wherein the mass ratio of the polyaluminum ferric chloride to the graphite powder is (2-3): 1, the carbon content of the graphite powder is more than or equal to 99.99 percent.
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