CN114100052A - Preparation method of mineral phase coating agent - Google Patents
Preparation method of mineral phase coating agent Download PDFInfo
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- CN114100052A CN114100052A CN202111402601.1A CN202111402601A CN114100052A CN 114100052 A CN114100052 A CN 114100052A CN 202111402601 A CN202111402601 A CN 202111402601A CN 114100052 A CN114100052 A CN 114100052A
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- aminosilane
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- 239000011248 coating agent Substances 0.000 title claims abstract description 75
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 24
- 239000011707 mineral Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 11
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 84
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 238000000576 coating method Methods 0.000 claims abstract description 24
- 239000012429 reaction media Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 22
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 6
- RPDAUEIUDPHABB-UHFFFAOYSA-N potassium ethoxide Chemical compound [K+].CC[O-] RPDAUEIUDPHABB-UHFFFAOYSA-N 0.000 claims description 3
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 12
- 239000010881 fly ash Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 125000000524 functional group Chemical group 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 description 8
- 238000002386 leaching Methods 0.000 description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- 239000010813 municipal solid waste Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004056 waste incineration Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000002738 chelating agent Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- ZOTKGMAKADCEDH-UHFFFAOYSA-N 5-triethoxysilylpentane-1,3-diamine Chemical compound CCO[Si](OCC)(OCC)CCC(N)CCN ZOTKGMAKADCEDH-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/33—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by chemical fixing the harmful substance, e.g. by chelation or complexation
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/24—Organic substances containing heavy metals
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/40—Inorganic substances
- A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
Landscapes
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Paints Or Removers (AREA)
Abstract
The application provides a preparation method of a mineral phase coating agent, which comprises the steps of adding aminosilane, carbon disulfide and an alkaline agent in a first specified molar ratio into a reaction medium, and reacting at a first specified temperature for a first specified time to obtain a target coating agent; or at least one of alumina or silicon oxide is added into water, and then aminosilane and alkaline agent are added to react for a second designated time at a second designated temperature to obtain aminosilane coating; and adding the aminosilane coating material, the carbon disulfide and the alkaline agent in a second specified molar ratio into a reaction medium, and reacting at a third specified temperature for a third specified time to obtain the target coating agent. The mineral phase coating agent has an active functional group capable of chelating heavy metal elements, and simultaneously contains a functional group which forms a bonding effect with siliceous and calcareous materials in fly ash, so that the chelating effect and stability can be greatly improved; the preparation method is simple and efficient, and the obtained product has stable quality and high content of effective substances.
Description
Technical Field
The application relates to the technical field of environmental protection, in particular to a preparation method of a mineral phase coating agent.
Background
The waste can be greatly reduced in volume by the incineration technology, the harmless degree is high, the waste heat can be utilized, and the three-transformation (reduction, harmless and recycling) principle of garbage treatment is met. Therefore, the incineration technology will become an important research and development direction of the garbage disposal technology in China. However, fly ash produced by incineration may contain various heavy metal elements, such as Pb (lead), Cr (chromium), Cd (cadmium), etc., at high leaching concentrations, which are harmful to the ecological environment. Heavy metals are harmful in that they cannot be decomposed by microorganisms and can concentrate or form other more toxic compounds in the organism, which ultimately pose a hazard to humans through the food chain.
In recent years, chelating agent materials are widely used for stabilizing heavy metals in waste incineration fly ash. Although the inorganic chelating agent is inexpensive, it has an unsatisfactory effect of stabilizing heavy metals and is generally added in a large amount. The heavy metal complexes formed by the organic agents are more stable, but the heavy metals are easily leached out again during storage.
Disclosure of Invention
In view of the problem, the present application is proposed in order to provide a method for the preparation of a mineral phase coating agent that overcomes or at least partially solves the problem, comprising:
a method of preparing a mineral phase coating agent, the method comprising:
adding aminosilane, carbon disulfide and an alkaline agent in a first specified molar ratio into a reaction medium, and reacting at a first specified temperature for a first specified time to obtain a target coating agent;
or:
adding at least one of alumina or silicon oxide into water, adding aminosilane and an alkaline agent, and reacting for a second designated time at a second designated temperature to obtain an aminosilane coating;
and adding the aminosilane coating, carbon disulfide and an alkaline agent in a second specified molar ratio into a reaction medium, and reacting at a third specified temperature for a third specified time to obtain the target coating agent.
Preferably, the aminosilane is one or a combination of KH-540, KH-550, KH-554, KH-602, KH-792, KH-793, and KH-902.
Preferably, the alkaline agent is one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium ethoxide and potassium ethoxide.
Preferably, the reaction medium is one or more combinations of water, ethanol, isopropanol, ethylene glycol, and propylene glycol.
Preferably, the first specified molar ratio means that the molar ratio of the aminosilane, the carbon disulfide and the alkaline agent is 1: 1.1-2.5: 1.1 to 2.5.
Preferably, the second specified molar ratio is that the molar ratio of the aminosilane coating, the carbon disulfide and the alkaline agent is 1: 1.1-2.5: 1.1 to 2.5.
Preferably, the concentration of the aluminum oxide is 10-40 wt%, the concentration of the silicon oxide is 10-40 wt%, the concentration of the aminosilane is 5-20 wt%, and the concentration of the alkaline agent is 0.001-0.1 wt%.
Preferably, the mass concentration of the aminosilane in the reaction system is 5-30 wt%, and the mass concentration of the aminosilane coating in the reaction system is 5-30 wt%.
Preferably, the first specified temperature is 20-60 ℃, the second specified temperature is 50-90 ℃, and the third specified temperature is 20-60 ℃.
Preferably, the first designated time is 10-30 hours, the second designated time is 3-6 hours, and the third designated time is 10-30 hours.
The application has the following advantages:
in the embodiment of the application, the target coating agent is obtained by adding aminosilane, carbon disulfide and an alkaline agent in a first specified molar ratio into a reaction medium and reacting at a first specified temperature for a first specified time; or: adding at least one of alumina or silicon oxide into water, adding aminosilane and an alkaline agent, and reacting for a second designated time at a second designated temperature to obtain an aminosilane coating; and adding the aminosilane coating, carbon disulfide and an alkaline agent in a second specified molar ratio into a reaction medium, and reacting at a third specified temperature for a third specified time to obtain the target coating agent. The mineral phase coating agent has an active functional group capable of chelating heavy metal elements, and simultaneously contains a functional group capable of forming a bonding effect with siliceous and calcareous materials in fly ash, so that the chelating effect can be greatly improved, and the stability is improved. The preparation method of the mineral phase coating agent is simple and efficient, and the obtained mineral phase coating agent is stable in quality and high in effective substance content.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present application more comprehensible, the present application is described in further detail with reference to the following embodiments. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. 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 application.
In any embodiment of the present application, the preparation method of the mineral phase coating agent is applied to the field of environmental protection, including the application of disposing hazardous solid wastes such as incineration fly ash containing various heavy metal pollutants, e.g., waste incineration fly ash, industrial solid waste incineration ash, and the like.
The embodiment of the application discloses a preparation method of a mineral phase coating agent;
the method comprises the following steps:
adding aminosilane, carbon disulfide and an alkaline agent in a first specified molar ratio into a reaction medium, and reacting at a first specified temperature for a first specified time to obtain a target coating agent;
or:
adding at least one of alumina or silicon oxide into water, adding aminosilane and an alkaline agent, and reacting for a second designated time at a second designated temperature to obtain an aminosilane coating;
and adding the aminosilane coating, carbon disulfide and an alkaline agent in a second specified molar ratio into a reaction medium, and reacting at a third specified temperature for a third specified time to obtain the target coating agent.
In the embodiment of the application, the target coating agent is obtained by adding aminosilane, carbon disulfide and an alkaline agent in a first specified molar ratio into a reaction medium and reacting at a first specified temperature for a first specified time; or: adding at least one of alumina or silicon oxide into water, adding aminosilane and an alkaline agent, and reacting for a second designated time at a second designated temperature to obtain an aminosilane coating; and adding the aminosilane coating, carbon disulfide and an alkaline agent in a second specified molar ratio into a reaction medium, and reacting at a third specified temperature for a third specified time to obtain the target coating agent. The mineral phase coating agent has an active functional group capable of chelating heavy metal elements, and simultaneously contains a functional group capable of forming a bonding effect with siliceous and calcareous materials in fly ash, so that the chelating effect can be greatly improved, and the stability is improved. The preparation method of the mineral phase coating agent is simple and efficient, and the obtained mineral phase coating agent is stable in quality and high in effective substance content.
Next, a method for producing a mineral phase coating agent in the present exemplary embodiment will be further described.
The mineral phase coating agent is prepared through chemical reaction, can realize long-acting safe curing of heavy metal ions, and meets the national landfill requirement.
As an example, the mineral phase coating agent is a reaction product of an aminosilane and carbon disulfide, and has a molecular formula as follows:
or:
in the structural formula: x is any integer of 1-3, R1Is one of Li, Na and K, R2、 R3Are respectively CH3、CH2-CH3One of (1);
the second is a compound which takes silicon oxide or aluminum oxide as a core and takes a reaction product of aminosilane and carbon disulfide as a shell, and the molecular structural formula of the shell is as follows:
or:
in the structural formula: x is any integer of 1-3, R1Is one of Li, Na and K, R2、 R3Are respectively CH3、CH2-CH3One kind of (1).
In one embodiment of the present application, the aminosilane is one or more combinations of KH-540 (gamma-aminopropyltrimethoxysilane), KH-550 (gamma-aminopropyltriethoxysilane), KH-554 (gamma-aminopropylmethyldimethoxysilane), KH-602 (N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane), KH-792 (N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane), KH-793 (3-2-aminoethyl-aminopropyltriethoxysilane), and KH-902 (gamma-aminopropylmethyldiethoxysilane).
In one embodiment of the present application, the alkaline agent is one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium ethoxide and potassium ethoxide.
In one embodiment of the present application, the reaction medium is one or more of water, ethanol, isopropanol, ethylene glycol, and propylene glycol.
In an embodiment of the present application, the first specific molar ratio is that the molar ratio of the aminosilane, the carbon disulfide, and the alkaline agent is 1: 1.1-2.5: 1.1 to 2.5; the dosage of the carbon disulfide and the alkaline agent is too low, the grafting reaction is insufficient, and the product quality is influenced; the consumption of carbon disulfide and alkaline agent is too high, which causes raw material waste and increases the manufacturing cost.
In an embodiment of the present application, the second specified molar ratio is a molar ratio of the aminosilane coating, the carbon disulfide, and the alkaline agent of 1: 1.1-2.5: 1.1 to 2.5; the dosage of the carbon disulfide and the alkaline agent is too low, the grafting reaction is insufficient, and the product quality is influenced; the consumption of carbon disulfide and alkaline agent is too high, which causes raw material waste and increases the manufacturing cost.
In an embodiment of the present application, the concentration of the aluminum oxide is 10 to 40 wt%, the concentration of the silicon oxide is 10 to 40 wt%, the concentration of the aminosilane is 5 to 20 wt%, and the concentration of the alkaline agent is 0.001 to 0.1 wt%. The concentration is too low, the content of a reaction medium in a reaction system is too large, and the content of a product actually prepared is lower; the concentration is too high, the reaction system is too viscous, and agglomeration is easy to generate, so that the quality of the product is influenced.
In an embodiment of the application, the mass concentration of the aminosilane in the reaction system is 5-30 wt%, and the mass concentration of the aminosilane coating in the reaction system is 5-30 wt%; the reaction system is a whole formed by combining various connected parts related to chemical reaction in a relatively closed environment.
In one embodiment of the present application, the first specified temperature is 20 to 60 ℃, the second specified temperature is 50 to 90 ℃, and the third specified temperature is 20 to 60 ℃; the reaction temperature is too low, the reaction rate of a reaction system is low, the reaction efficiency is low, the reaction time is long, the conversion rate of partial reactants is low, and the purity of the product is influenced; the reaction temperature is too high, the reaction is too violent, the heat release is large, and the reaction process is not easy to control.
In an embodiment of the present application, the first designated time is 10 to 30 hours, the second designated time is 3 to 6 hours, and the third designated time is 10 to 30 hours.
The following are specific examples.
Example 1
The molar ratio is 1: 1.1: 1.1 wt% of aminosilane (KH-540), carbon disulfide and 0.001 wt% of alkaline agent (lithium hydroxide) were added to the reaction medium (water) and reacted at 20 ℃ for 30 hours to obtain the objective coating agent.
The target coating agent is a reaction product of aminosilane and carbon disulfide, and the structural formula of the target coating agent is as follows:
in the structural formula: x is 3, R1Is Li, R2、R3Are respectively CH3。
Example 2
The molar ratio is 1: 1.2: 1.3 wt% of aminosilane (KH-540), carbon disulfide and 0.05 wt% of alkaline agent (sodium hydroxide) were added to the reaction medium (ethanol) and reacted at 40 ℃ for 10 hours to obtain the objective coating agent.
The target coating agent is a reaction product of aminosilane and carbon disulfide, and the structural formula of the target coating agent is as follows:
in the structural formula: x is 3, R1Is Na, R2、R3Are respectively CH3。
Example 3
The molar ratio is 1: 2.5: 2.5 wt% of aminosilane (KH-602), carbon disulfide and 0.1 wt% of alkaline agent (potassium hydroxide) were added to the reaction medium (water) and reacted at 60 ℃ for 15 hours to obtain the objective coating agent.
The target coating agent is a reaction product of aminosilane and carbon disulfide, and the structural formula of the target coating agent is as follows:
in the structural formula: x is 2, R1Is K, R2、R3Are respectively CH3。
Example 4
Adding 10 wt% of alumina into water, adding 5 wt% of aminosilane (KH-792) and 0.001 wt% of alkaline agent (lithium hydroxide), and reacting at 50 ℃ for 3 hours to obtain an aminosilane coating;
the molar ratio is 1: 2.1: 2.1 the aminosilane coating, carbon disulfide and 0.001 wt% of an alkaline agent (lithium hydroxide) were added to a reaction medium (water) and reacted at 20 ℃ for 30 hours to obtain the objective coating agent.
The target coating agent is a compound taking silicon oxide or aluminum oxide as a core and taking a reaction product of aminosilane and carbon disulfide as a shell, and the structural formula of the shell is as follows:
in the structural formula: x is 3, R1Is Li, R2、R3Are respectively CH3。
Example 5
Adding 25 wt% of alumina into water, adding 12 wt% of aminosilane (KH-550) and 0.05 wt% of alkaline agent (sodium hydroxide), and reacting at 70 ℃ for 4.5 hours to obtain an aminosilane coating;
the molar ratio is 1: 1.1: 1.1, adding the aminosilane coating, carbon disulfide and 0.05 wt% of alkaline agent (sodium hydroxide) into a reaction medium (ethanol), and reacting at 40 ℃ for 20 hours to obtain the target coating agent.
The target coating agent is a compound taking silicon oxide or aluminum oxide as a core and taking a reaction product of aminosilane and carbon disulfide as a shell, and the structural formula of the shell is as follows:
in the structural formula: x is any integer of 3, R1Is Na, R2、R3Are respectively CH2-CH3。
Example 6
Adding 40 wt% of silicon oxide into water, adding 20 wt% of aminosilane (KH-792) and 0.1 wt% of alkaline agent (lithium hydroxide), and reacting at 90 ℃ for 6 hours to obtain an aminosilane coating;
the molar ratio is 1: 2.1: 2.1, adding the aminosilane coating, carbon disulfide and 0.1 wt% of alkaline agent (potassium hydroxide) into a reaction medium (water), and reacting at 60 ℃ for 30 hours to obtain the target coating agent.
The target coating agent is a compound taking silicon oxide or aluminum oxide as a core and taking a reaction product of aminosilane and carbon disulfide as a shell, and the structural formula of the shell is as follows:
in the structural formula: x is 3, R1Is K, R2、R3Are respectively CH3。
The following are test data:
adding 2% of mineral phase coating agent into the household garbage incineration fly ash, and stirring and reacting for 30 min. Leaching for 1 day and 30 days respectively according to pollution control standard of domestic garbage landfill (GB16889-2008), and testing the heavy metal content of the leaching liquor by using ICP (inductively coupled plasma Spectroscopy) instrument.
The comparative example is a chelant prepared with 1% sodium sulfide and 1% sodium fermet.
The test results of the Pb leaching content of the incineration fly ash of household garbage are shown in the following table:
| leaching for 1 day Pb content (mg/L) | Leaching for 30 days Pb content (mg/L) | |
| Example 1 | 0.02 | 0.04 |
| Example 2 | 0.02 | 0.027 |
| Example 3 | 0.01 | 0.02 |
| Example 4 | 0.009 | 0.01 |
| Example 5 | 0.007 | 0.02 |
| Example 6 | 0.05 | 0.08 |
| Comparative example | 0.045 | 0.12 |
As can be seen from the above table, the mineral phase coating agent prepared by the present application has good stabilizing effect, fast chelating speed, and the leaching time does not greatly affect the leaching content of Pb, and examples 4 and 5 are preferred in each example.
While preferred embodiments of the present application have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all such alterations and modifications as fall within the true scope of the embodiments of the application.
Finally, it should also be noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or terminal. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or terminal that comprises the element.
The above detailed description of the preparation method of a mineral phase coating agent provided by the present application, and the principle and the embodiment of the present application are explained by applying specific examples, and the above description of the examples is only used to help understanding the method and the core concept of the present application; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (10)
1. A method for preparing a mineral phase coating agent, the method comprising:
adding aminosilane, carbon disulfide and an alkaline agent in a first specified molar ratio into a reaction medium, and reacting at a first specified temperature for a first specified time to obtain a target coating agent;
or:
adding at least one of alumina or silicon oxide into water, adding aminosilane and an alkaline agent, and reacting for a second designated time at a second designated temperature to obtain an aminosilane coating;
and adding the aminosilane coating, carbon disulfide and an alkaline agent in a second specified molar ratio into a reaction medium, and reacting at a third specified temperature for a third specified time to obtain the target coating agent.
2. The method of claim 1, wherein the aminosilane is a combination of one or more of KH-540, KH-550, KH-554, KH-602, KH-792, KH-793, and KH-902.
3. The method for preparing the mineral phase coating agent according to claim 1, wherein the alkaline agent is one or more of lithium hydroxide, sodium hydroxide, potassium hydroxide, sodium ethoxide and potassium ethoxide.
4. The method of claim 1, wherein the reaction medium is one or more of water, ethanol, isopropanol, ethylene glycol, and propylene glycol.
5. The method of claim 1, wherein the first specified molar ratio is a molar ratio of the aminosilane, the carbon disulfide, and the alkaline agent of 1: 1.1-2.5: 1.1 to 2.5.
6. The method of claim 1, wherein the second specified molar ratio is a molar ratio of the aminosilane coating, the carbon disulfide, and the alkaline agent of 1: 1.1-2.5: 1.1 to 2.5.
7. The method according to claim 1, wherein the concentration of the alumina is 10 to 40 wt%, the concentration of the silica is 10 to 40 wt%, the concentration of the aminosilane is 5 to 20 wt%, and the concentration of the alkali agent is 0.001 to 0.1 wt%.
8. The method according to claim 1, wherein the mass concentration of the aminosilane in the reaction system is 5 to 30 wt%, and the mass concentration of the aminosilane coating in the reaction system is 5 to 30 wt%.
9. The method for preparing a mineral phase coating agent according to claim 1, wherein the first specified temperature is 20 to 60 ℃, the second specified temperature is 50 to 90 ℃, and the third specified temperature is 20 to 60 ℃.
10. The method according to claim 1, wherein the first specified time is 10 to 30 hours, the second specified time is 3 to 6 hours, and the third specified time is 10 to 30 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116271680A (en) * | 2023-02-03 | 2023-06-23 | 乐尔环境科技有限公司 | Fly ash chelating agent for effectively inhibiting arsenic and selenium leaching and preparation method thereof |
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| CN104609526A (en) * | 2014-12-29 | 2015-05-13 | 许昌学院 | Heavy metal collector and preparation method thereof |
| CN112897671A (en) * | 2021-01-19 | 2021-06-04 | 西南科技大学 | Heavy metal ion capturing material and preparation method thereof |
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| CN104609526A (en) * | 2014-12-29 | 2015-05-13 | 许昌学院 | Heavy metal collector and preparation method thereof |
| CN112897671A (en) * | 2021-01-19 | 2021-06-04 | 西南科技大学 | Heavy metal ion capturing material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116271680A (en) * | 2023-02-03 | 2023-06-23 | 乐尔环境科技有限公司 | Fly ash chelating agent for effectively inhibiting arsenic and selenium leaching and preparation method thereof |
| CN116271680B (en) * | 2023-02-03 | 2024-02-06 | 乐尔环境科技有限公司 | Fly ash chelating agent for effectively inhibiting arsenic and selenium leaching and preparation method thereof |
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Application publication date: 20220301 |