A filter element material for water detection and preparation method thereof

The filter element material that combines modified zeolite with a polymer matrix solves the problems of low heavy metal and pollutant removal efficiency and poor stability of existing filter element materials, achieving efficient water purification and high water flux effects.

CN120154988BActive Publication Date: 2025-09-23QINGDAO AOBO ENVIRONMENTAL PROTECTION TECH CO LTD
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Patent Information

Application Number
CN202510324834.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-03-19
Publication Date
2025-09-23
Estimated Expiration
2045-03-19

AI Technical Summary

Technical Problem

Existing filter materials have problems with low efficiency, high cost and poor stability in removing heavy metals and pollutants. Traditional activated carbon has limited adsorption performance, while the preparation cost of new nanomaterials is high and the stability is insufficient.

Method used

Modified zeolite is used as a functional additive. The compatibility and stability of the zeolite are improved through the reaction of silane modification and amino-terminated polymer. A filter element material with a good combination of modified zeolite and polymer matrix is ​​prepared. The microporous structure and surface groups of the modified zeolite are utilized to achieve physical adsorption and chemical adsorption of heavy metals and pollutants, thus forming a filter element material combining physical absorption and chemical adsorption.

Benefits of technology

It significantly improves the filter element material's removal efficiency of pollutants in water and the adsorption effect of heavy metals, enhances the material's mechanical strength and durability, is suitable for a variety of complex water quality environments, and has good water purification effects and high water flux.

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Abstract

The present invention relates to the technical field of filter element materials, and specifically to a filter element material for water detection and a preparation method thereof. The filter element material for water detection is composed of the following raw materials in parts by weight: 30-60 parts by weight of polypropylene, 15-30 parts by weight of polyethersulfone, 3-8 parts by weight of a solubilizer, 8-15 parts by weight of activated carbon, 1-3 parts by weight of a coupling agent, and 4-8 parts by weight of a functional additive; the functional additive is a modified zeolite, which is obtained by reacting a silane-modified zeolite with an amino-terminated polymer. The filter element material for water detection prepared by the present invention has a good water purification effect when used in water detection, has good effects in decontamination and heavy metal adsorption, and also has a high water flux, thereby achieving a good water purification effect.
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Description

Technical Field

[0001] The present invention relates to the technical field of filter core materials, and in particular to a filter core material for water detection and a preparation method thereof. Background Art

[0002] With the growth of the global population and the acceleration of industrialization, water shortages and water pollution are becoming increasingly serious. According to statistics, approximately 20% of the world's population lacks safe drinking water, and the discharge of industrial wastewater, agricultural runoff, and domestic sewage further exacerbates water quality. These problems not only affect human health but also cause irreversible damage to ecosystems. Therefore, the development of efficient water quality monitoring and purification technologies has become crucial to solving the water crisis.

[0003] Water detection technology is an important component of water quality monitoring and water treatment. Traditional water quality testing methods rely on laboratory analysis, which is time-consuming and cannot monitor water quality changes in real time. Therefore, it is particularly important to develop water detection technology that can quickly and in real time detect water quality. As an emerging water quality monitoring tool, water detection filters can detect pollutants in water in real time through physical, chemical, or biological means, providing real-time data support for water quality management.

[0004] Water detection filters are of great significance in water quality monitoring and treatment. Their primary function is to detect and remove impurities, heavy metals, organic matter, and other contaminants from water, while also enabling real-time monitoring of water quality through the use of specialized materials. In recent years, advancements in materials science and fabrication technologies have continuously expanded the performance and application of water detection filters.

[0005] Current filter materials still face numerous challenges. For example, while traditional activated carbon filters offer excellent adsorption performance, their effectiveness in removing heavy metals is limited. While some new nanomaterials possess high adsorption capacity, they suffer from high production costs and poor stability. Therefore, the development of high-performance, low-cost filter materials is urgent. Summary of the Invention

[0006] In view of the above-mentioned deficiencies in the prior art, the present invention provides a filter element material for water detection and a preparation method thereof.

[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is:

[0008] A filter element material for water detection is composed of the following raw materials in parts by weight: 30-60 parts by weight of polypropylene, 15-30 parts by weight of polyethersulfone, 3-8 parts by weight of a solubilizer, 8-15 parts by weight of activated carbon, 1-3 parts by weight of a coupling agent, and 4-8 parts by weight of a functional additive; the functional additive is a modified zeolite obtained by reacting a silane-modified zeolite with an amino-terminated polymer.

[0009] Zeolite is a natural or synthetic microporous crystalline material with a porous structure that provides a huge specific surface area, which is conducive to the adsorption of pollutants in water. The cations in zeolite (such as Na⁺ and K⁺) can exchange with heavy metal ions (such as Pb²⁺ and Cd²⁺) in water to remove harmful substances. Although natural zeolite has good adsorption properties, the compatibility and dispersibility of zeolite in the filter element material matrix are extremely poor, and its surface activity and stability are limited. Therefore, it needs to be modified to improve the dispersibility and stability of zeolite in the polymer matrix (such as polypropylene and polyethersulfone) to avoid agglomeration.

[0010] Specific reaction mechanism: S1 uses zeolite and 3-chloropropyltrimethoxysilane as the main reaction raw materials, ethanol aqueous solution as the solvent, polyethylene glycol as the emulsifier, and under the condition of heating and stirring, the hydroxyl (-OH) on the surface of the zeolite reacts with the silane coupling agent to form a silicon-oxygen bond (Si-O-Si). The purpose of introducing the silane group is to improve the hydrophobicity and surface activity of the zeolite and provide reaction sites for the subsequent grafting of amino-terminated polymers; S2 uses polyethyleneimine and ethoxylated trimethylolpropane triacrylate as the reaction raw materials, triethylamine as the catalyst, and under the condition of heating and stirring, polyethyleneimine (containing amino groups) reacts with ethoxylated trimethylolpropane triacrylate (containing propylene glycol) to form a silicon-oxygen bond (Si-O-Si). The silane-modified zeolite and the amino-terminated polymer are reacted with each other to form a Michael addition reaction (with ester groups) to generate an amino-terminated polymer with a dendritic branched structure and containing a large number of terminal amino groups. The introduced terminal amino groups can not only enhance the adsorption capacity and chemical activity of the zeolite, but also improve the compatibility and affinity between the zeolite and the polymer matrix. S3 uses silane-modified zeolite and amino-terminated polymer as reaction raw materials and potassium hydroxide as catalyst. Under heating and stirring, the silane-modified zeolite and the amino-terminated polymer undergo a condensation reaction under alkaline conditions (catalyzed by potassium hydroxide) to generate a stable covalent bond, and the amino-terminated polymer is grafted onto the surface of the zeolite, further enhancing its adsorption performance and dispersibility, and improving the stability and durability of the modified zeolite in the filter element material.

[0011] The preparation method of the modified zeolite is as follows:

[0012] S1, mixing 8-14 parts by weight of zeolite, 80-160 parts by weight of ethanol aqueous solution, and 0.5-2 parts by weight of polyethylene glycol, adding 1-4 parts by weight of a silane coupling agent, heating and stirring to obtain a silane-modified zeolite;

[0013] S2, in an ice-water bath, dissolving 3-6 parts by weight of polyethyleneimine in 30-70 parts by weight of an aqueous ethanol solution, adding 3-7 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.5-1 parts by weight of triethylamine to react to obtain an amino-terminated polymer;

[0014] S3. Mix 5-10 parts by weight of the above-mentioned silane-modified zeolite, 4-8 parts by weight of the above-mentioned amino-terminated polymer, and 80-160 parts by weight of an ethanol aqueous solution, add 0.1-0.3 parts by weight of an aqueous potassium hydroxide solution, stir evenly, and heat to react to obtain a modified zeolite.

[0015] The modified zeolite prepared by the present invention has amino groups and siloxane groups on its surface, which can improve its good compatibility with the polymer matrix (polypropylene, polyethersulfone). At the same time, the addition of a coupling agent can further promote the interface bonding between the modified zeolite and the matrix, effectively avoid the agglomeration of the zeolite in the polymer matrix, and improve the uniformity and mechanical properties of the material. The addition of the modified zeolite can not only chemically adsorb heavy metal ions and organic pollutants (such as phenol and dyes) in water, but the microporous structure of the zeolite itself can also capture small molecular pollutants through physical adsorption. The combination of the two can not only adsorb heavy metal ions and pollutants in water through physical adsorption but also through chemical reaction, significantly improving the filter element material's removal efficiency of pollutants in water, heavy metal adsorption effect, filtration efficiency and effluent quality.

[0016] Preferably, the preparation method of the modified zeolite is as follows:

[0017] S1, 8-14 parts by weight of zeolite, 80-160 parts by weight of ethanol aqueous solution, and 0.5-2 parts by weight of polyethylene glycol are mixed, 1-4 parts by weight of a silane coupling agent is added, and the mixture is heated and stirred at 80-100° C. and 300-500 rpm for 30-60 min, filtered, washed, and freeze-dried to obtain a silane-modified zeolite;

[0018] S2. In an ice-water bath, dissolving 3-6 parts by weight of polyethyleneimine in 30-70 parts by weight of an aqueous ethanol solution, adding 3-7 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.5-1 part by weight of triethylamine, reacting at 40-60° C. and 100-300 rpm for 4-10 hours, adding acetone for precipitation, washing, and freeze-drying to obtain an amino-terminated polymer;

[0019] S3. Mix 5-10 parts by weight of the above-mentioned silane-modified zeolite, 4-8 parts by weight of the above-mentioned amino-terminated polymer, and 80-160 parts by weight of an ethanol aqueous solution, add 0.1-0.3 parts by weight of an aqueous potassium hydroxide solution, stir evenly, react at 70-85° C. and 100-300 rpm for 16-28 hours, filter, wash, and freeze-dry to obtain a modified zeolite.

[0020] Preferably, the silane coupling agent is at least one of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane, 3-chloropropyltrimethoxysilane, and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane; further, the silane coupling agent is a mixture of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane in a mass ratio of 2:3.

[0021] The coupling agent used in this application is a combination of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane. The reason is that N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane can provide amino and carboxyl groups to combine with heavy metal ions and pollutants through coordination bonds, thereby enhancing adsorption capacity; while N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane can improve The compatibility, dispersibility and stability of the modified zeolite with the polymer matrix avoid zeolite agglomeration, ensure that the adsorption sites are fully exposed, and ensure the durability of the adsorption performance. 3-Chloropropyltrimethoxysilane only contains chloropropyl and lacks active groups such as amino and carboxyl groups, and its adsorption capacity is limited. Therefore, the compound ratio of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane optimizes the balance between adsorption performance and dispersibility to achieve the best adsorption effect.

[0022] The solubilizer is at least one of styrene-maleic anhydride copolymer, butadiene-maleic anhydride copolymer, glycidyl methacrylate, and polydimethylsiloxane; preferably, the solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0023] The coupling agent is at least one of methyltrimethoxysilane, 3-aminopropylmethyldimethoxysilane, 3-(methacryloyloxy)propyltrimethoxysilane, bis-[3-(triethoxysilyl)propyl]-disulfide, silane coupling agent KH-550, N-phenyl-γ-aminopropyltrimethoxysilane, and bis(dioctyldiethanolamine pyrophosphoryl)ethylenediammonium titanate.

[0024] The method for preparing the water detection filter material comprises the following steps:

[0025] (1) Weigh each raw material by weight;

[0026] (2) adding polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additive into a twin-screw extruder and extruding to obtain an extrudate;

[0027] (3) The extruded material is fed into an injection molding machine for injection molding to obtain a filter element material for water detection.

[0028] The extrusion temperature program is 160-180°C, 210-230°C, 220-250°C, 220-250°C, 220-250°C, 220-250°C, 220-240°C, 210-230°C, the screw speed is 80-120rpm, and the screw torque is 25-35Nm.

[0029] The injection molding temperature is 200-260° C., the die head temperature is 200-230° C., and the extrusion pressure is 8-14 MPa.

[0030] The present invention provides a water detection filter element material and its preparation method. By adding modified zeolite, the material's adsorption performance, filtration accuracy, material compatibility, and chemical stability are enhanced. When used in water detection filter elements, the modified zeolite not only efficiently removes pollutants from water but also improves the filter element's mechanical strength and durability, making it suitable for a variety of complex water quality environments and possessing broad application prospects.

[0031] 2. The present invention provides a filter element material for water detection and a preparation method thereof. The prepared filter element material for water detection has a good water purification effect when used in water detection, has good effects in decontamination and heavy metal adsorption, and also has a high water flux, thereby achieving a good water purification effect.

[0032] 3. Compared with other processes, the preparation process of the present invention is simple, has low energy consumption, low raw material price and high safety. DETAILED DESCRIPTION

[0033] The above content of the present invention will be further described in detail below in conjunction with specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following embodiments.

[0034] Some of the raw materials described in this application are commercially available. Other raw materials not described are commercially available:

[0035] Polypropylene was purchased from Shanghai Yesu International Trading Co., Ltd. with the brand name R370Y.

[0036] Polyethersulfone was purchased from Dongguan Yitai Plastic Chemical Co., Ltd. with the brand name E6010.

[0037] Styrene-maleic anhydride copolymer was purchased from Wuhan Shuer Biotechnology Co., Ltd., model XH1370FSU1LO.

[0038] Polyethyleneimine was purchased from Shanghai Yushicheng Chemical Technology Co., Ltd., model Lugalvan G35.

[0039] Example 1

[0040] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0041] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0042] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0043] The functional auxiliary agent is zeolite.

[0044] The method for preparing the water detection filter material comprises the following steps:

[0045] (1) Weigh each raw material by weight;

[0046] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0047] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0048] Example 2

[0049] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0050] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0051] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0052] The functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows: 10 parts by weight of zeolite, 100 parts by weight of a 70wt% ethanol aqueous solution, and 1 part by weight of polyethylene glycol are mixed, 2 parts by weight of a silane coupling agent is added, and the mixture is heated and stirred at 90°C and 400 rpm for 45 minutes, filtered, washed, and freeze-dried to obtain a silane-modified zeolite; the silane coupling agent is N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane.

[0053] The method for preparing the water detection filter material comprises the following steps:

[0054] (1) Weigh each raw material by weight;

[0055] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0056] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0057] Example 3

[0058] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0059] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0060] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0061] The functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows:

[0062] S1. In an ice-water bath, 4 parts by weight of polyethyleneimine was dissolved in 40 parts by weight of a 60 wt% aqueous ethanol solution, 5 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.8 parts by weight of triethylamine were added, and the mixture was reacted at 45° C. and 200 rpm for 6 h. The mixture was precipitated by adding acetone, washed, and freeze-dried to obtain an amino-terminated polymer.

[0063] S2. 8 parts by weight of zeolite, 6 parts by weight of the above-mentioned amino-terminated polymer, and 100 parts by weight of a 30 wt% ethanol aqueous solution were mixed, 0.2 parts by weight of a 5 mol / L potassium hydroxide aqueous solution was added and stirred evenly, and the mixture was reacted at 78° C. and 200 rpm for 18 h. The mixture was filtered, washed, and freeze-dried to obtain a modified zeolite.

[0064] The method for preparing the water detection filter material comprises the following steps:

[0065] (1) Weigh each raw material by weight;

[0066] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0067] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0068] Example 4

[0069] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0070] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0071] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0072] The functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows:

[0073] S1. 10 parts by weight of zeolite, 100 parts by weight of 70 wt% ethanol aqueous solution, and 1 part by weight of polyethylene glycol were mixed, 2 parts by weight of a silane coupling agent was added, and the mixture was heated and stirred at 90° C. and 400 rpm for 45 min, filtered, washed, and freeze-dried to obtain a silane-modified zeolite; the silane coupling agent was N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane;

[0074] S2. In an ice-water bath, 4 parts by weight of polyethyleneimine was dissolved in 40 parts by weight of a 60 wt% aqueous ethanol solution, 5 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.8 parts by weight of triethylamine were added, and the mixture was reacted at 45° C. and 200 rpm for 6 h. The mixture was precipitated by adding acetone, washed, and freeze-dried to obtain an amino-terminated polymer;

[0075] S3. Mix 8 parts by weight of the above-mentioned silane-modified zeolite, 6 parts by weight of the above-mentioned amino-terminated polymer, and 100 parts by weight of a 30 wt% ethanol aqueous solution, add 0.2 parts by weight of a 5 mol / L potassium hydroxide aqueous solution and stir evenly, react at 78°C and 200 rpm for 18 hours, filter, wash, and freeze-dry to obtain a modified zeolite.

[0076] The method for preparing the water detection filter material comprises the following steps:

[0077] (1) Weigh each raw material by weight;

[0078] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0079] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0080] Example 5

[0081] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0082] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0083] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0084] The functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows:

[0085] S1, 10 parts by weight of zeolite, 100 parts by weight of 70 wt% ethanol aqueous solution, and 1 part by weight of polyethylene glycol were mixed, 2 parts by weight of a silane coupling agent was added, and the mixture was heated and stirred at 90° C. and 400 rpm for 45 min, filtered, washed, and freeze-dried to obtain a silane-modified zeolite; the silane coupling agent was N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane;

[0086] S2. In an ice-water bath, 4 parts by weight of polyethyleneimine was dissolved in 40 parts by weight of a 60 wt% aqueous ethanol solution, 5 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.8 parts by weight of triethylamine were added, and the mixture was reacted at 45° C. and 200 rpm for 6 h. The mixture was precipitated by adding acetone, washed, and freeze-dried to obtain an amino-terminated polymer;

[0087] S3. Mix 8 parts by weight of the above-mentioned silane-modified zeolite, 6 parts by weight of the above-mentioned amino-terminated polymer, and 100 parts by weight of a 30 wt% ethanol aqueous solution, add 0.2 parts by weight of a 5 mol / L potassium hydroxide aqueous solution and stir evenly, react at 78°C and 200 rpm for 18 hours, filter, wash, and freeze-dry to obtain a modified zeolite.

[0088] The method for preparing the water detection filter material comprises the following steps:

[0089] (1) Weigh each raw material by weight;

[0090] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0091] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0092] Example 6

[0093] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0094] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0095] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0096] The functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows:

[0097] S1. 10 parts by weight of zeolite, 100 parts by weight of 70 wt% ethanol aqueous solution, and 1 part by weight of polyethylene glycol were mixed, 2 parts by weight of a silane coupling agent was added, and the mixture was heated and stirred at 90° C. and 400 rpm for 45 min, filtered, washed, and freeze-dried to obtain a silane-modified zeolite; the silane coupling agent was a mixture of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane in a mass ratio of 2:3;

[0098] S2. In an ice-water bath, 4 parts by weight of polyethyleneimine was dissolved in 40 parts by weight of a 60 wt% aqueous ethanol solution, 5 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.8 parts by weight of triethylamine were added, and the mixture was reacted at 45° C. and 200 rpm for 6 h. The mixture was precipitated by adding acetone, washed, and freeze-dried to obtain an amino-terminated polymer;

[0099] S3. Mix 8 parts by weight of the above-mentioned silane-modified zeolite, 6 parts by weight of the above-mentioned amino-terminated polymer, and 100 parts by weight of a 30 wt% ethanol aqueous solution, add 0.2 parts by weight of a 5 mol / L potassium hydroxide aqueous solution and stir evenly, react at 78°C and 200 rpm for 18 hours, filter, wash, and freeze-dry to obtain a modified zeolite.

[0100] The method for preparing the water detection filter material comprises the following steps:

[0101] (1) Weigh each raw material by weight;

[0102] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0103] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0104] Example 7

[0105] A filter element material for water detection is composed of the following raw materials in parts by weight: 40 parts by weight of polypropylene, 20 parts by weight of polyethersulfone, 5 parts by weight of a solubilizer, 10 parts by weight of activated carbon, 2 parts by weight of a coupling agent, and 6 parts by weight of a functional additive.

[0106] The solubilizer is a mixture of styrene-maleic anhydride copolymer and glycidyl methacrylate in a mass ratio of 1:1.

[0107] The coupling agent is 3-(methacryloyloxy)propyltrimethoxysilane.

[0108] The functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows:

[0109] S1. 10 parts by weight of zeolite, 100 parts by weight of 70 wt% ethanol aqueous solution, and 1 part by weight of polyethylene glycol were mixed, 2 parts by weight of a silane coupling agent was added, and the mixture was heated and stirred at 90° C. and 400 rpm for 45 min, filtered, washed, and freeze-dried to obtain a silane-modified zeolite; the silane coupling agent was a mixture of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and 3-chloropropyltrimethoxysilane in a mass ratio of 2:3;

[0110] S2. In an ice-water bath, 4 parts by weight of polyethyleneimine was dissolved in 40 parts by weight of a 60 wt% aqueous ethanol solution, 5 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.8 parts by weight of triethylamine were added, and the mixture was reacted at 45° C. and 200 rpm for 6 h. The mixture was precipitated by adding acetone, washed, and freeze-dried to obtain an amino-terminated polymer;

[0111] S3. Mix 8 parts by weight of the above-mentioned silane-modified zeolite, 6 parts by weight of the above-mentioned amino-terminated polymer, and 100 parts by weight of a 30 wt% ethanol aqueous solution, add 0.2 parts by weight of a 5 mol / L potassium hydroxide aqueous solution and stir evenly, react at 78°C and 200 rpm for 18 hours, filter, wash, and freeze-dry to obtain a modified zeolite.

[0112] The method for preparing the water detection filter material comprises the following steps:

[0113] (1) Weigh each raw material by weight;

[0114] (2) Polypropylene, polyethersulfone, compatibilizer, diatomaceous earth, activated carbon, coupling agent and functional additives were added to a twin-screw extruder and extruded at a temperature of 170°C, 220°C, 240°C, 240°C, 240°C, 230°C and 220°C, a screw speed of 100 rpm and a screw torque of 30 Nm to obtain an extrudate;

[0115] (3) The extrudate is fed into an injection molding machine at an injection molding temperature of 240° C., a die head temperature of 220° C., and an extrusion pressure of 10 MPa, and injection molding is performed to obtain a filter element material for water detection.

[0116] Test Example 1

[0117] Decontamination efficiency test: The water detection filter material prepared in Examples 1-7 above was injection molded into a test filter element. When the test liquid passed through the tested filter element at a flow rate of 8 mm / s (effective filtration area of ​​10 cm 2 ), add test powder with a particle size of 10μm to the upstream of the filter at a rate of 10mg / min until the pressure difference of the filter element reaches 0.4MPa. Stop the test and calculate the cumulative amount of test dust added. The calculation formula is as follows: M=G×q×t÷S÷1000.

[0118] Where: M: dirt holding capacity (g / cm 2 ); G: average mass contamination in the dust adding device (mg / L); q: average injection flow rate (L / min); t: actual test time when the final pressure difference is reached (min); S: effective filtration area of ​​the filter element. Each group of samples was tested 5 times and the average value was taken.

[0119] Water flux testing: The water detection filter materials prepared in Examples 1-7 were injection-molded into test filter elements and placed in a filtration apparatus. 20 mL of water was added and circulated until the amount of water filtered stabilized within 5 minutes. Then, 20 mL of water was added to the filtration apparatus. Under no external pressure, the amount of water naturally filtered was measured. The volume of water passing through per unit area per unit time, i.e., the water flux (L / (m²·h)), was calculated. Each set of samples was tested five times, and the average value was taken. The results are shown in Table 1.

[0120] Table 1 Decontamination efficiency and water flux test results

[0121] Dirt holding capacity (g / cm2) Water flux L / (m2·h) Example 1 43.91 83.92 Example 2 54.58 94.76 Example 3 56.32 96.25 Example 4 64.97 97.35 Example 5 64.31 97.13 Example 6 67.35 98.34 Example 7 65.37 98.02

[0122] Test Example 2

[0123] Metal ion removal rate: Non-ferrous metal mine wastewater, particularly copper smelting wastewater, was collected as the standard test solution. The prepared water detection filter material was used to fabricate a filter element. This element was connected to the detection system and activated. The standard test solution was passed through the filter element at a flow rate of 8 mm / s for 2 hours. Samples were collected before and after filtration, and the copper ion concentration in the standard test solution was determined by titration. The metal ion removal rate was calculated using the following formula: Metal ion removal rate = 1 - (C·V / N·F) / (C·V0 / N·F) × 100%. Where: C: titrant concentration (mol / L); V: volume of titrant consumed in the post-filtration reaction (L); N: amount of ion substance consumed in the titration reaction; F: amount of ion substance; V0: volume of titrant consumed in the pre-filtration reaction (L). Each sample group was tested five times, and the average value was calculated. The results are shown in Table 2.

[0124] Table 2 Heavy metal ion removal rate test results

[0125] Heavy metal ion removal rate (%) Example 1 35.52 Example 2 67.28 Example 3 59.48 Example 4 92.47 Example 5 91.56 Example 6 96.35 Example 7 94.31

[0126] From the above results, it can be seen that the water detection filter material prepared by the present invention has a good effect on water purification when used in filter elements, and has obvious effects on heavy metal removal rate and decontamination. By comparing Examples 1-4, it can be seen that the modified zeolite prepared by the method of the present invention has good decontamination and heavy metal removal effects when used in filter element materials for water detection, and can also improve water flux. The reason is that the modified zeolite prepared by the present invention has amino groups and siloxane groups on the surface, which can improve the compatibility with the polymer matrix (polypropylene, polyethersulfone). At the same time, the addition of the coupling agent can further promote the interface bonding between the modified zeolite and the matrix, effectively avoid the agglomeration of the zeolite in the polymer matrix, and improve the uniformity and mechanical properties of the material. The addition of the modified zeolite can not only chemically adsorb heavy metal ions and organic pollutants (such as phenol and dyes) in the water, but the microporous structure of the zeolite itself can also capture small molecular pollutants through physical adsorption. The combination of the two can not only adsorb heavy metal ions and pollutants in water through physical adsorption but also through chemical reaction, significantly improving the removal efficiency of the filter element material for pollutants in water, the adsorption effect of heavy metals, the filtration efficiency and the water quality.

[0127] Further comparison of Examples 4-6 shows that the coupling agent used in this application is a combination of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane. The reason is that N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane can provide amino and carboxyl groups to combine with heavy metal ions and pollutants through coordination bonds, thereby enhancing the adsorption capacity; while N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane can provide amino and carboxyl groups to combine with heavy metal ions and pollutants through coordination bonds, thereby enhancing the adsorption capacity. Acyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane can improve the compatibility, dispersibility and stability of modified zeolite and polymer matrix, avoid zeolite agglomeration, ensure full exposure of adsorption sites, and ensure the durability of adsorption performance. Therefore, the compounding ratio of N-[β-(N,N-diacetoxy)aminoethyl]-γ-(N-acetoxy)aminopropyltrimethoxysilane and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane optimizes the balance between adsorption performance and dispersibility to achieve the best adsorption effect.

[0128] Finally, comparing Examples 6-7, the 3-chloropropyltrimethoxysilane used contained only chloropropyl groups and lacked active groups such as amino and carboxyl groups, resulting in limited adsorption capacity.

Claims

1. A filter element material for water detection, characterized in that: The invention is composed of the following raw materials in parts by weight: 30-60 parts by weight of polypropylene, 15-30 parts by weight of polyethersulfone, 3-8 parts by weight of a solubilizer, 8-15 parts by weight of activated carbon, 1-3 parts by weight of a coupling agent, and 4-8 parts by weight of a functional additive; the functional additive is a modified zeolite, and the preparation method of the modified zeolite is as follows: S1, mixing 8-14 parts by weight of zeolite, 80-160 parts by weight of ethanol aqueous solution, and 0.5-2 parts by weight of polyethylene glycol, adding 1-4 parts by weight of a silane coupling agent, heating and stirring to obtain a silane-modified zeolite; S2, in an ice-water bath, dissolving 3-6 parts by weight of polyethyleneimine in 30-70 parts by weight of an aqueous ethanol solution, adding 3-7 parts by weight of ethoxylated trimethylolpropane triacrylate and 0.5-1 parts by weight of triethylamine to react to obtain an amino-terminated polymer; S3. Mix 5-10 parts by weight of the above-mentioned silane-modified zeolite, 4-8 parts by weight of the above-mentioned amino-terminated polymer, and 80-160 parts by weight of an ethanol aqueous solution, add 0.1-0.3 parts by weight of an aqueous potassium hydroxide solution, stir evenly, and heat to react to obtain a modified zeolite.

2. The water detection filter element material according to claim 1, wherein: The heating temperature in S1 is 80-100° C., the stirring rate is 300-500 rpm, and the heating time is 30-60 min.

3. The water detection filter element material according to claim 1, wherein: The reaction temperature in S2 is 40-60° C., the stirring rate is 100-300 rpm, and the reaction time is 4-10 h.

4. The water detection filter element material according to claim 1, wherein: The heating temperature in S3 is 70-85° C., the stirring rate is 100-300 rpm, and the reaction time is 16-28 h.

5. The water detection filter element material according to claim 1, wherein: The solubilizer is at least one of styrene-maleic anhydride copolymer, butadiene-maleic anhydride copolymer, glycidyl methacrylate, and polydimethylsiloxane.

6. The water detection filter element material according to claim 1, wherein: The coupling agent is at least one of methyltrimethoxysilane, 3-aminopropylmethyldimethoxysilane, 3-(methacryloyloxy)propyltrimethoxysilane, bis-[3-(triethoxysilyl)propyl]-disulfide, silane coupling agent KH-550, N-phenyl-γ-aminopropyltrimethoxysilane, and bis(dioctyldiethanolamine pyrophosphoryl)ethylenediammonium titanate.

7. The water detection filter element material according to claim 6, wherein: The silane coupling agent is a mixture of N-[β-(N,N-diacetyl)aminoethyl]-γ-(N-acetyl)aminopropyltrimethoxysilane and N-(3-acryloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane in a mass ratio of 2:

3.

8. A method for preparing a water detection filter element material according to any one of claims 1 to 7, characterized in that: The steps include: (1) Weigh each raw material by weight; (2) adding polypropylene, polyethersulfone, solubilizer, activated carbon, coupling agent and functional additive into a twin-screw extruder and extruding to obtain an extrudate; (3) The extruded material is fed into an injection molding machine for injection molding to obtain a filter element material for water detection.

9. The method for preparing a water detection filter element material according to claim 8, wherein: The extrusion temperature in step (2) is 160-180°C, 210-230°C, 220-250°C, 220-250°C, 220-250°C, 220-250°C, 220-240°C and 210-230°C, the screw speed is 80-120rpm, and the screw torque is 25-35Nm.

10. The method for preparing a water detection filter element material according to claim 8, wherein: The injection molding conditions in step (3) are an injection temperature of 200-260° C., a die head temperature of 200-230° C., and an extrusion pressure of 8-14 MPa.

Citation Information

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