CN110590999A - Hydrolysis-resistant cationic flocculant and preparation method and application method thereof - Google Patents
Hydrolysis-resistant cationic flocculant and preparation method and application method thereof Download PDFInfo
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- 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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/147—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
- C08F226/04—Diallylamine
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Abstract
The invention discloses an anti-hydrolysis cationic emulsion flocculant and a preparation method and an application method thereof, wherein the preparation method comprises the following steps: will be provided withAdding acrylamide, a cationic monomer, a functional monomer and a water-soluble oxidant into deionized water to obtain an aqueous phase solution; adding a nonionic emulsifier into the solvent oil to obtain an oil phase solution; slowly dripping the water phase solution into the oil phase solution, and uniformly stirring to obtain a water-in-oil pre-emulsion; introducing nitrogen to remove oxygen from the pre-emulsion; and adding a reducing agent into the pre-emulsion to initiate polymerization to obtain the hydrolysis-resistant cationic emulsion flocculant. The invention starts from improving the structure of the cationic emulsion flocculant, adds functional monomers, namely, introduces energy and Ca in the polymerization process2+、Mg2+Group reacted by plasma metal ion and coordination with organic acid to eliminate Ca2+、Mg2+The influence of the metal ions on the viscosity of the cationic emulsion flocculant can control the viscosity reduction of the flocculant within 20 percent at high temperature (35-45 ℃) within 24 hours.
Description
Technical Field
The invention belongs to synthesis and application of water treatment chemicals, and particularly relates to an anti-hydrolysis cationic flocculant as well as a preparation method and an application method thereof.
Background
With the increase of urban population and the rapid development of modern industry, domestic sewage and industrial wastewater are increased sharply, so that rivers are polluted to different degrees. At present, the polymeric flocculant is widely applied to the field of sewage treatment due to the advantages of controllable structure, wide pH application range, small dosage, good flocculation effect, no metal residue, small sludge production amount and the like. However, in the use process of the polymeric flocculant, the dissolved flocculant is mostly river water, lake water or river water, and the water contains more Ca2+、Mg2+Plasma metal ion, Ca2+、Mg2+The electrostatic attraction interaction is generated between the metal ions and carboxylate radicals generated by partial hydrolysis of the flocculating agent, the original charge density of the molecular surface of the flocculating agent is reduced, molecular chains are curled, and the solvation capacity of polar groups is weakened, so that the viscosity of the flocculating agent is obviously reduced, and the flocculation effect is influenced. In addition, the viscosity of the flocculant is further sticky due to factors such as field temperature, dissolution time and storage timeThe degree is reduced. Under the current general application environment, the viscosity of the existing cationic emulsion flocculant is reduced by more than 50% within 2 hours, and then the existing cationic emulsion flocculant further shows a descending trend along with the time extension.
At present, aiming at the influence of metal ions in water on the viscosity of a flocculating agent, different complexing agents are mainly used for inhibiting hydrolysis in the application process in the existing patents, for example, an organic treating agent is adopted in patent CN102849835A, and mainly comprises complexing agents such as 2, 3-dihydroxy sodium potassium succinate, hydroxy ethylidene diphosphate and the like for complexing the metal ions, so that the complexing agent is large in dosage, high in cost and poor in stability. In patent CN104232054B, a compound complexing agent is used for improving the viscosity stability of polyacrylamide, and the complexing agent has the advantages of multiple varieties, large dosage, high cost and poor stability.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides an anti-hydrolysis cationic emulsion flocculant and a preparation method and an application method thereof.
The technical scheme for realizing the aim of the invention is a preparation method of an anti-hydrolysis cationic emulsion flocculant, which comprises the following steps:
adding acrylamide, a cationic monomer, a functional monomer and a water-soluble oxidant into deionized water to obtain an aqueous phase solution;
adding a nonionic emulsifier into the solvent oil to obtain an oil phase solution;
slowly dripping the water phase solution into the oil phase solution, and uniformly stirring to obtain a water-in-oil pre-emulsion;
introducing nitrogen to remove oxygen from the pre-emulsion;
and adding a reducing agent into the pre-emulsion to initiate polymerization to obtain the hydrolysis-resistant cationic emulsion flocculant.
Further, the cationic monomer is selected from one or a combination of more of (meth) acryloyloxyethyltrimethyl ammonium chloride, dimethylaminoethyl (meth) acrylate, diethylaminoethyl (meth) acrylate, diallyl dimethyl ammonium chloride and dimethylaminopropyl acrylamide.
Further, the functional monomer is selected from one or a combination of more of sodium p-styrene sulfonate, maleic acid, acrylic acid, methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid.
Further, the acrylamide accounts for 10-40% of the total mass of the pre-emulsion, the cationic monomer accounts for 60-90% of the total mass of the pre-emulsion, and the functional monomer accounts for 1-5% of the total mass of the pre-emulsion.
Further, the water-soluble oxidizing agent is selected from one or a combination of more of ammonium persulfate, potassium persulfate, sodium persulfate, potassium bromate and sodium bromate, and the mass of the water-soluble oxidizing agent accounts for 0.5-2% of the total mass of the pre-emulsion.
Further, the reducing agent is one or a combination of several of sodium bisulfite, sodium sulfite, sodium metabisulfite, sodium thiosulfate, tetramethylethylenediamine and oxalic acid, and the mass of the reducing agent accounts for 0.5-2% of the total mass of the pre-emulsion.
Further, the non-ionic emulsifier is one or a combination of more of sorbitan monooleate, sorbitan tristearate, sorbitan monostearate, sorbitan monopalmitate, sorbitan laurate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan tristearate, polyoxyethylene sorbitan monolaurate and alkylphenol polyoxyethylene ether-10, and the mass of the non-ionic emulsifier accounts for 3-6% of the total mass of the pre-emulsion.
The invention also provides an anti-hydrolysis cationic emulsion flocculant prepared by the preparation method of the anti-hydrolysis cationic emulsion flocculant.
The invention also provides an application method of the hydrolysis-resistant cationic emulsion flocculant, which is used together with organic acid to inhibit hydrolysis.
Further, the organic acid is one or more of adipic acid, malic acid, citric acid and sebacic acid, and the mass of the organic acid accounts for 0.01-10%, preferably 0.01-1% of the total mass of the hydrolysis-resistant cationic emulsion flocculant and the organic acid.
After the technical scheme is adopted, the invention has the following positive effects: the inventionStarting from the improvement of the structure of the cationic emulsion flocculant, functional monomers are added, namely energy and Ca are introduced in the polymerization process2+、Mg2+Group reacted by plasma metal ion and coordination with organic acid to eliminate Ca2+、Mg2+The influence of the metal ions on the viscosity of the cationic emulsion flocculant can control the viscosity reduction of the flocculant within 20 percent at high temperature (35-45 ℃) within 24 hours. The flocculant and the application method thereof are suitable for different dissolved water qualities, are widely applied to the fields of sewage treatment, sludge treatment, mineral flotation, oil and gas exploitation, textile printing and dyeing and the like, and have good economic benefit and social benefit.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a graph of the effect of different formulations on the viscosity of cationic emulsion flocculants.
Detailed Description
(example 1)
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 with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, 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.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the embodiments of the present invention, it should be understood that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships that are usually placed when the product of the present invention is used, or orientations or positional relationships that are conventionally understood by those skilled in the art, which are used for convenience of description and simplicity of description, but do not indicate or imply that the equipment or element in question must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention.
In the description of the embodiments of the present invention, it should be further noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may include, for example, a fixed connection, a detachable connection, or an integral connection; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
(example 1)
In this example, three sample examples were used for comparison, namely, a cationic flocculant without introducing a functional monomer (sample 1), a cationic flocculant with introducing a functional monomer (sample 2), and a cationic flocculant with introducing a functional monomer and using the cationic flocculant in combination with an organic acid (sample 3), and as shown in fig. 1, it was confirmed that the introduction of a functional monomer and the use of a combination with an organic acid results in the lowest viscosity drop and the lowest hydrolysis of a cationic flocculant.
Sample 1: adding 108g of acrylamide, 259.2g of diallyldimethylammonium chloride (cationic monomer) and 224.8g of deionized water into a beaker, mechanically stirring until complete dissolution, and adding 0.005g of ammonium persulfate (water-soluble oxidizing agent) into the solution to obtain an aqueous phase; 168g of No. 5 industrial white oil, 14g of sorbitan monooleate and 26g of polyoxyethylene sorbitan monooleate are added into a reaction kettle and stirred to obtain an oil phase; slowly dripping the prepared water phase into the oil phase to obtain a pre-emulsion; and (3) dropwise adding 0.3% of sodium bisulfite (reducing agent) into the pre-emulsion for initiation to obtain the cationic emulsion flocculant. 10g of cationic emulsion flocculant is dissolved in 2000ml of river water (mineralization: 200-500 mg/L), stirred for 1 hour and then placed in a 45 ℃ oven for 24 hours, and the viscosity change is tested.
Sample 2: adding 108g of acrylamide, 252g of diallyldimethylammonium chloride, 7.2g of 2-acrylamide-2-methylpropanesulfonic acid and 224.8g of deionized water into a beaker, mechanically stirring until the acrylamide, the diallyldimethylammonium chloride, the 2-acrylamide-2-methylpropanesulfonic acid and the deionized water are completely dissolved, and adding 0.005g of ammonium persulfate into the solution to obtain a water phase; 168g of No. 5 industrial white oil, 14g of sorbitan monooleate and 26g of polyoxyethylene sorbitan monooleate are added into a reaction kettle and stirred to obtain an oil phase; slowly dripping the prepared water phase into the oil phase to obtain a pre-emulsion; and (3) dropwise adding 0.3% of sodium bisulfite into the pre-emulsion for initiation to obtain the hydrolysis-resistant cationic emulsion flocculant. 10g of hydrolysis-resistant cationic emulsion flocculant is dissolved in 2000ml of river water (mineralization degree: 200-500 mg/L), stirred for 1 hour and then placed in a 45 ℃ oven for 24 hours, and the viscosity change is tested.
Sample 3: adding 108g of acrylamide, 252g of diallyldimethylammonium chloride, 7.2g of 2-acrylamide-2-methylpropanesulfonic acid and 224.8g of deionized water into a beaker, mechanically stirring until the acrylamide, the diallyldimethylammonium chloride, the 2-acrylamide-2-methylpropanesulfonic acid and the deionized water are completely dissolved, and adding 0.005g of ammonium persulfate into the solution to obtain a water phase; 168g of No. 5 industrial white oil, 14g of sorbitan monooleate and 26g of polyoxyethylene sorbitan monooleate are added into a reaction kettle and stirred to obtain an oil phase; slowly dripping the prepared water phase into the oil phase to obtain a pre-emulsion; and (3) dropwise adding 0.3% of sodium bisulfite into the pre-emulsion for initiation to obtain the hydrolysis-resistant cationic emulsion flocculant. Taking 2000ml of river water (mineralization degree: 200-500 mg/l), firstly adding 0.5g of adipic acid (organic acid), and uniformly mixing; 10g of hydrolysis-resistant cationic emulsion flocculant is added, stirred for 1 hour and then placed in an oven at 45 ℃ for 24 hours, and the viscosity change is tested.
(example 2)
Adding 144g of acrylamide, 216g of methacryloyloxyethyl trimethyl ammonium chloride, 7.2g of methacrylic acid and 224.8g of deionized water into a beaker, mechanically stirring until the acrylamide, the methacryloyloxyethyl trimethyl ammonium chloride and the deionized water are completely dissolved, and adding 0.005g of ammonium persulfate into the solution to obtain a water phase; 168g of No. 5 industrial white oil, 14g of sorbitan monooleate and 26g of polyoxyethylene sorbitan monooleate are added into a reaction kettle and stirred to obtain an oil phase; slowly dripping the prepared water phase into the oil phase to obtain a pre-emulsion; and (3) dropwise adding 0.3% of sodium bisulfite into the pre-emulsion for initiation to obtain the hydrolysis-resistant cationic flocculant. Taking 2000ml of river water (the mineralization degree is 500-1000 mg/L), firstly adding 2g of adipic acid, and uniformly mixing; and finally, adding 10g of hydrolysis-resistant cationic flocculant, stirring for 1 hour, and then placing in a 45 ℃ oven for 24 hours, wherein the viscosity is reduced by less than or equal to 20%.
(example 3)
Adding 108g of acrylamide, 252g of diethylaminoethyl acrylate, 7.2g of acrylic acid and 224.8g of deionized water into a beaker, mechanically stirring until the acrylamide, the diethylaminoethyl acrylate, the acrylic acid and the deionized water are completely dissolved, and adding 0.005g of ammonium persulfate into the solution to obtain a water phase; 168g of No. 5 industrial white oil, 14g of sorbitan monooleate and 26g of polyoxyethylene sorbitan monooleate are added into a reaction kettle and stirred to obtain an oil phase; slowly dripping the prepared water phase into the oil phase to obtain a pre-emulsion; and (3) dropwise adding 0.3% of sodium bisulfite into the pre-emulsion for initiation to obtain the hydrolysis-resistant cationic flocculant. Taking 2000ml of river water (the mineralization degree is 500-1000 mg/L), firstly adding 0.5g of malic acid, and uniformly mixing; and finally, adding 10g of hydrolysis-resistant cationic flocculant, stirring for 1 hour, and then placing in a 45 ℃ oven for 24 hours, wherein the viscosity is reduced by less than or equal to 20%.
(example 4)
Adding 72kg of acrylamide, 288kg of diethylaminoethyl acrylate, 7.2kg of acrylic acid and 224.8kg of deionized water into a beaker, mechanically stirring until the acrylamide, the diethylaminoethyl acrylate, the acrylic acid and the deionized water are completely dissolved, and adding 5g of ammonium persulfate into the solution to obtain a water phase; 168kg of No. 5 industrial white oil, 14kg of sorbitan monooleate and 26kg of polyoxyethylene sorbitan monooleate are added into a reaction kettle and stirred to obtain an oil phase; slowly dripping the prepared water phase into the oil phase to obtain a pre-emulsion; and (3) dropwise adding 0.3% of sodium bisulfite into the pre-emulsion for initiation to obtain the hydrolysis-resistant cationic flocculant. Taking 10t of river water (the mineralization degree is 200-500 mg/L), firstly adding 2.5kg of malic acid, and uniformly mixing; and finally, adding 50kg of hydrolysis-resistant cationic flocculant, stirring for 1 hour, and then placing in an environment of 45 ℃ for 24 hours, wherein the viscosity is reduced by less than or equal to 20%.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of an anti-hydrolysis cationic emulsion flocculant is characterized by comprising the following steps:
adding acrylamide, a cationic monomer, a functional monomer and a water-soluble oxidant into deionized water to obtain an aqueous phase solution;
adding a nonionic emulsifier into the solvent oil to obtain an oil phase solution;
slowly dripping the water phase solution into the oil phase solution, and uniformly stirring to obtain a water-in-oil pre-emulsion;
introducing nitrogen to remove oxygen from the pre-emulsion;
and adding a reducing agent into the pre-emulsion to initiate polymerization to obtain the hydrolysis-resistant cationic emulsion flocculant.
2. The method for preparing the hydrolysis-resistant cationic emulsion flocculant according to claim 1, wherein the method comprises the following steps: the cationic monomer is selected from one or more of (methyl) acryloyloxyethyl trimethyl ammonium chloride, dimethylaminoethyl (methyl) acrylate, diethylaminoethyl (methyl) acrylate, diallyl dimethyl ammonium chloride and dimethylamino propyl acrylamide.
3. The method for preparing the hydrolysis-resistant cationic emulsion flocculant according to claim 1, wherein the method comprises the following steps: the functional monomer is selected from one or a combination of more of sodium p-styrene sulfonate, maleic acid, acrylic acid, methacrylic acid and 2-acrylamide-2-methylpropanesulfonic acid.
4. The method for preparing the hydrolysis-resistant cationic emulsion flocculant according to claim 1, wherein the method comprises the following steps: the acrylamide accounts for 10-40% of the total mass of the pre-emulsion, the cationic monomer accounts for 60-90% of the total mass of the pre-emulsion, and the functional monomer accounts for 1-5% of the total mass of the pre-emulsion.
5. The method for preparing the hydrolysis-resistant cationic emulsion flocculant according to claim 1, wherein the method comprises the following steps: the water-soluble oxidant is selected from one or a combination of more of ammonium persulfate, potassium persulfate, sodium persulfate, potassium bromate and sodium bromate, and the mass of the water-soluble oxidant accounts for 0.5-2% of the total mass of the pre-emulsion.
6. The method for preparing the hydrolysis-resistant cationic emulsion flocculant according to claim 1, wherein the method comprises the following steps: the reducing agent is one or a combination of more of sodium bisulfite, sodium sulfite, sodium metabisulfite, sodium thiosulfate, tetramethylethylenediamine and oxalic acid, and the mass of the reducing agent accounts for 0.5-2% of the total mass of the pre-emulsion.
7. The method for preparing the hydrolysis-resistant cationic emulsion flocculant according to claim 1, wherein the method comprises the following steps: the non-ionic emulsifier is one or a combination of more of sorbitan monooleate, sorbitan tristearate, sorbitan monostearate, sorbitan monopalmitate, sorbitan laurate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan tristearate, polyoxyethylene sorbitan monolaurate and alkylphenol polyoxyethylene ether-10, and the mass of the non-ionic emulsifier accounts for 3-6% of the total mass of the pre-emulsion.
8. The hydrolysis-resistant cationic emulsion flocculant of claim 1, wherein: the hydrolysis-resistant cationic emulsion flocculant as claimed in any one of claims 1 to 8.
9. The method of claim 1, wherein the application of the hydrolysis-resistant cationic emulsion flocculant is as follows: the hydrolysis-resistant cationic emulsion flocculant is used together with an organic acid to inhibit hydrolysis.
10. The method of claim 9, wherein the application of the hydrolysis-resistant cationic emulsion flocculant is as follows: the organic acid is one or a combination of more of adipic acid, malic acid, citric acid and sebacic acid, and the mass of the organic acid accounts for 0.01-10% of the total mass of the hydrolysis-resistant cationic emulsion flocculant and the organic acid.
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| CN113968933A (en) * | 2021-11-25 | 2022-01-25 | 江苏富淼科技股份有限公司 | Cationic polyacrylamide particles and preparation method thereof |
| CN113968933B (en) * | 2021-11-25 | 2022-11-11 | 江苏富淼科技股份有限公司 | Cationic polyacrylamide particles and preparation method thereof |
| CN114195357A (en) * | 2022-02-18 | 2022-03-18 | 河南博源新材料有限公司 | Polyacrylamide composition containing dianion coagulant aid and preparation method and application thereof |
| CN115260386A (en) * | 2022-09-23 | 2022-11-01 | 江苏富淼科技股份有限公司 | Cationic polyacrylamide reverse emulsion, preparation method and application thereof |
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