CN116657406A - Oil-water separation material based on polyester bottle flake regenerated fiber and preparation method thereof - Google Patents

Oil-water separation material based on polyester bottle flake regenerated fiber and preparation method thereof Download PDF

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CN116657406A
CN116657406A CN202310563279.3A CN202310563279A CN116657406A CN 116657406 A CN116657406 A CN 116657406A CN 202310563279 A CN202310563279 A CN 202310563279A CN 116657406 A CN116657406 A CN 116657406A
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oil
polyester bottle
water separation
regenerated fiber
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CN116657406B (en
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徐军
刘艳
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Yangzhou Guangtai Chemical Fiber Co ltd
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Yangzhou Guangtai Chemical Fiber Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326Condensation or reaction polymers
    • D04H1/435Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/45Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • D06M13/21Halogenated carboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/6436Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00Water conservation; Efficient water supply; Efficient water use
    • Y02A20/20Controlling water pollution; Waste water treatment
    • Y02A20/204Keeping clear the surface of open water from oil spills
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Water Treatment By Sorption (AREA)
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Abstract

The invention provides an oil-water separation material based on polyester bottle flake regenerated fibers and a preparation method thereof, and relates to the technical field of oil-water separation materials, wherein the oil-water separation material is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle chip, 12-16 parts of polyvinylpyrrolidone, 1-3 parts of coupling agent, 5-8 parts of carbon nanotube sponge, 5-8 parts of chloro pivaloyl chloride, 2-3 parts of adamantyl chloride, 5-10 parts of 4, 4-chloroformyl phenyl ether, 2-4 parts of anhydrous aluminum chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 15-25 parts. The material has high oil-water separation efficiency, good effect, good cycle performance and relatively low preparation cost.

Description

Oil-water separation material based on polyester bottle flake regenerated fiber and preparation method thereof
Technical Field
The invention relates to the technical field of oil-water separation materials, in particular to an oil-water separation material based on polyester bottle flake regenerated fibers and a preparation method thereof.
Background
The oil-water separation technology is a technology for realizing the processes of separating, purifying, concentrating and the like of organic and inorganic components of a material by utilizing the selective separation of the material, has the advantages of high efficiency, energy conservation, environmental protection, simple separation process, recycling and the like, and is widely applied to the fields of food, medicine, environmental protection, chemical industry, metallurgy, energy, petroleum, water treatment and the like. The oil-water separation material is the key of the oil-water separation technology, and the performance of the oil-water separation material directly determines the oil-water separation effect. Therefore, the development of the oil-water separation material with good comprehensive performance and performance stability is particularly important.
The traditional oil-water separation material (such as active carbon, graphite, clay, diatomite and the like) has the defects of unobvious interfacial infiltration characteristic, weak oil absorption and water repellency, low separation efficiency, difficult material recycling and influence on the using effect of the material, and absorbs a large amount of water at the same time of oil absorption. Other oil-water separation materials on the market have the defects of poor oil-water separation effect, complex preparation process, complicated steps, certain environmental pollution in the aspects of recycling and disposal, and further improvement of mechanical properties, recycling times and oil-water separation efficiency.
The polyester bottle flakes have the advantages of high strength, good brightness, light weight, good transparency, convenient processing, stable size and the like, the global market demand and the application amount are greatly increased, and the waste polyester bottle flakes are increased year by year along with the large-scale use of the polyester bottle flakes. These polyester bottle flakes are non-biodegradable, their waste is prone to "white pollution", and how to better process and reasonably reuse the waste recycled polyester bottle flakes has become a key issue for sustainable development of the polyester industry.
The regenerated fiber of the polyester bottle chip is a fiber material prepared by taking the recovered polyester bottle chip as a raw material, and the material is one of the most promising oil-water separation materials because the material is cheap and easy to obtain and has the property of hydrophobic and oleophilic, and after the material is processed into a three-dimensional porous material, the oil-water separation can be more effectively carried out. However, the existing oil-water separation material based on the regenerated fiber of the polyester bottle flake is rare, requires a complex preparation method and equipment, has high cost and is not beneficial to large-scale production and application.
In order to solve the above problems, chinese patent document CN100344341C discloses a super-hydrophobic/super-oleophilic oil-water separation net, mainly a fabric net formed by metal fibers such as stainless net, copper, iron, titanium, aluminum, or a fabric net formed by fibers such as polyester, nylon, vinylon, etc. is immersed in perfluoro-silicone to prepare a super-hydrophobic/super-oleophilic oil-water separation net covered with a thin layer of poly-perfluoroalkyl silicone film on the surface, the metal net has a complex preparation method, needs multiple soaking times, has a higher curing temperature, and basically belongs to physical adhesion between the poly-perfluoroalkyl silicone and the fabric net, and the poly-perfluoroalkyl silicone film is easy to fall off from the grid during use, so that the poly-perfluoroalkyl silicone film is difficult to reuse. A large amount of toxic organic solvents are used in the preparation process, so that serious pollution is caused. When a large amount of oily wastewater is treated, due to the limited action effect of the single-layer oil-water separation net, multiple layers of separation nets are often required to be used for common operation, and the large-area popularization and use cost is high.
Therefore, the field still needs an oil-water separation material based on the polyester bottle flake regenerated fiber, which has high oil-water separation efficiency, good effect, good cycle performance and relatively low preparation cost, and a preparation method thereof.
Disclosure of Invention
In view of the above problems, the invention aims to provide an oil-water separation material based on polyester bottle flake regenerated fibers, which has high oil-water separation efficiency, good effect and good cycle performance and relatively low preparation cost, and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the oil-water separation material based on the polyester bottle flake regenerated fiber is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle flake, 12-16 parts of polyvinylpyrrolidone, 1-3 parts of coupling agent, 5-8 parts of carbon nanotube sponge, 5-8 parts of chloro pivaloyl chloride and adamantane2-3 parts of acyl chloride, 5-10 parts of 4, 4-chloroformyl phenyl ether, 2-4 parts of anhydrous aluminum chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 15-25 parts.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30 provided by Shanghai Fuqing materials science and technology Co.
Preferably, the source of the carbon nanotube sponge is not particularly limited, and in one embodiment of the present invention, the carbon nanotube sponge is made according to the method of embodiment 1 in CN 106257597B.
Preferably, the amino-terminated hyperbranched polysiloxane HPSi-NH 2 In one embodiment of the invention, the amino-terminated hyperbranched polysiloxane HPSi-NH is of no particular origin 2 Is prepared as in example 1 of CN 110156948B.
The invention also aims at providing a preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber, which comprises the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding into isopropanol, stirring, soaking in the hot pressed regenerated fiber non-woven fabric base based on polyester bottle chip for 6-10 hr, taking out, and drying at 60-80deg.CDrying to constant weight.
Preferably, the melt blowing temperature is 270 to 290 ℃.
Preferably, the temperature of the rolling mill during rolling is 125-165 ℃, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 200-330 rpm.
Preferably, in step S2, the organic solvent is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1 (8-10).
Preferably, the process conditions of the hot press reinforcement are as follows: the hot pressing temperature is 120-130 ℃, the hot pressing pressure is 1800KG, the preheating time is 18-25min, the hot pressing time is 4-6min, and the die opening temperature is 55-65 ℃.
Preferably, the amino-terminated hyperbranched polysiloxane HPSi-NH described in step S3 2 The mass ratio of the isopropanol is 1 (5-8).
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber, disclosed by the invention, can be realized by adopting conventional equipment, has the advantages of low energy consumption and investment, high preparation efficiency and yield, simple preparation process, convenient operation control and suitability for industrial popularization and application.
(2) The oil-water separation material based on the polyester bottle flake regenerated fiber disclosed by the invention has the main raw materials of the recycled polyester bottle flake, belongs to recycling of solid waste, realizes waste recycling, saves resources, avoids waste, is beneficial to environmental protection and reduces production cost. The polyvinyl pyrrolidone is used for pore-forming and is made into a regenerated fiber material, and the regenerated fiber material and the carbon nanotube sponge cooperate to improve the mechanical properties of the regenerated fiber material, and the molecular transfer efficiency can be effectively improved through the introduction of pores, so that the adsorption rate is high, the adsorption performance is stable, and the oil-water separation efficiency and effect are improved.
(3) The invention discloses an oil-water separation material based on polyester bottle flake regenerated fibers, which is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle flake, 12-16 parts of polyvinylpyrrolidone, 1-3 parts of coupling agent, 5-8 parts of carbon nanotube sponge, 5-8 parts of chloro pivaloyl chloride and 2-3 parts of adamantyl chloride5-10 parts of 4, 4-chloroformyl phenyl ether, 2-4 parts of anhydrous aluminum chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 15-25 parts. Through the mutual coordination of the raw materials, the prepared oil-water separation material has the advantages of high oil-water separation efficiency, good effect, good circulation performance and relatively low preparation cost.
(4) The raw materials containing acyl chloride structures such as the chloro pivaloyl chloride, the adamantyl chloride and the 4, 4-chloroformyl phenyl ether can react with benzene rings on the recovered polyester bottle flakes under the catalysis of anhydrous aluminum chloride to form an interpenetrating network structure, and simultaneously, the structures such as adamantane, phenyl ether and ester are introduced, so that the oil-water separation efficiency and effect can be improved under the multiple effects of an electronic effect, a steric effect and a conjugation effect, and the performance stability and the circulation performance are improved.
(5) The invention discloses an oil-water separation material based on polyester bottle flake regenerated fiber, which is prepared by introducing amino hyperbranched polysiloxane HPSi-NH 2 The oil-water separation effect and efficiency can be further improved, amino groups in the molecular structure of the oil-water separation agent can interact with chlorine groups (such as chloro pivaloyl chloride introduced) on the surface of the non-woven fabric, so that loss of effective functional components is avoided, and the circulation performance and the environmental protection performance are effectively improved.
Detailed Description
In order to better understand the technical solution of the present invention, the following describes the product of the present invention in further detail with reference to examples.
Example 1
The oil-water separation material based on the polyester bottle flake regenerated fiber is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle chip, 12 parts of polyvinylpyrrolidone, 1 part of coupling agent, 5 parts of carbon nanotube sponge, 5 parts of chloro pivaloyl chloride, 2 parts of adamantyl chloride, 5 parts of 4, 4-chloroformyl phenyl ether, 2 parts of anhydrous aluminum chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 15 parts.
The coupling agent is a silane coupling agent KH550; the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30, and Shanghai Fuqing material technology is limitedCompany offerings; the carbon nanotube sponge was made according to the method of example 1 in CN 106257597B; the amino-terminated hyperbranched polysiloxane HPSi-NH 2 Is prepared as in example 1 of CN 110156948B.
The preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber comprises the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding the mixture into isopropanol, uniformly stirring, soaking the polyester bottle flake based regenerated fiber non-woven fabric blank after hot pressing and reinforcement in the mixture for 6 hours, taking out the mixture, and drying the mixture at 60 ℃ to constant weight.
The melt-blown temperature was 270 ℃; the temperature of the rolling mill during rolling is 125 ℃, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 200 revolutions per minute.
The organic solvent in the step S2 is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1:8; the process conditions of the hot-pressing reinforcement are as follows: the hot pressing temperature is 120 ℃, the hot pressing pressure is 1800KG, the preheating time is 18min, the hot pressing time is 4min, and the die opening temperature is 55 ℃.
The amino-terminated hyperbranched polysiloxane HPSi-NH in the step S3 2 The mass ratio of the isopropanol is 1:5.
Example 2
The oil-water separation material based on the polyester bottle flake regenerated fiber is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle chip, 13 parts of polyvinylpyrrolidone, 1.5 parts of coupling agent, 6 parts of carbon nanotube sponge, 6 parts of chloro pivaloyl chloride, 2.3 parts of adamantyl chloride, 6 parts of 4, 4-chloroformyl phenyl ether, 2.5 parts of anhydrous aluminum chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 17 parts.
The coupling agent is silane coupling agent KH560; the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30 provided by Shanghai Fuqing materials science and technology Co., ltd; the carbon nanotube sponge was made according to the method of example 1 in CN 106257597B; the amino-terminated hyperbranched polysiloxane HPSi-NH 2 Is prepared as in example 1 of CN 110156948B.
The preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber comprises the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press; carrying out dissolution and melting experiments on the hot-pressed crude product, and confirming that the product is neither soluble nor fusible, so as to form a cross-linked structure of the interpenetrating network; after the reaction, washing with water and methanol respectively, and then drying, and confirming that the chloro pivaloyl chloride, adamantyl chloride and 4, 4-chloroformyl phenyl ether are grafted to the regenerated fiber non-woven fabric blank based on the polyester bottle chip through the quality change before and after the reaction;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding into isopropanol, stirring, soaking in the hot-pressed and reinforced non-woven fabric blank for 7 hr, and taking outDrying at 65deg.C to constant weight; repeatedly washing the product with isopropanol, drying, and comparing the quality change before and after the reaction and before and after the washing to prove that the amino-terminated hyperbranched polysiloxane HPSi-NH 2 Interaction is formed with the nonwoven fabric blank.
The melt-blowing temperature is 275 ℃; the temperature of the rolling mill during rolling is 135 ℃, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 230 rpm.
The organic solvent in the step S2 is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1:8.5; the process conditions of the hot-pressing reinforcement are as follows: the hot pressing temperature is 123 ℃, the hot pressing pressure is 1800KG, the preheating time is 20min, the hot pressing time is 4.5min, and the die opening temperature is 58 ℃.
The amino-terminated hyperbranched polysiloxane HPSi-NH in the step S3 2 The mass ratio of the isopropanol is 1:6.
Example 3
The oil-water separation material based on the polyester bottle flake regenerated fiber is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle flake, 14 parts of polyvinylpyrrolidone, 2 parts of coupling agent, 6.5 parts of carbon nanotube sponge, 6.5 parts of chloro pivaloyl chloride, 2.5 parts of adamantyl chloride, 8 parts of 4, 4-chloroformyl phenyl ether, 3 parts of anhydrous aluminum chloride and 3 parts of amino-terminated hyperbranched polysiloxane HPSi-NH 2 20 parts.
The coupling agent is a silane coupling agent KH570; the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30 provided by Shanghai Fuqing materials science and technology Co., ltd; the carbon nanotube sponge was made according to the method of example 1 in CN 106257597B; the amino-terminated hyperbranched polysiloxane HPSi-NH 2 Is prepared as in example 1 of CN 110156948B.
The preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber comprises the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding the mixture into isopropanol, uniformly stirring, soaking the polyester bottle flake based regenerated fiber non-woven fabric blank after hot pressing and reinforcement in the mixture for 8 hours, taking out the mixture, and drying the mixture at 70 ℃ to constant weight.
The melt-blowing temperature is 280 ℃; the temperature of the rolling mill during rolling is 145 ℃, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 280 revolutions per minute.
The organic solvent in the step S2 is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1:9; the process conditions of the hot-pressing reinforcement are as follows: the hot pressing temperature is 125 ℃, the hot pressing pressure is 1800KG, the preheating time is 22min, the hot pressing time is 5min, and the die opening temperature is 60 ℃.
The amino-terminated hyperbranched polysiloxane HPSi-NH in the step S3 2 The mass ratio of the isopropanol is 1:6.5.
Example 4
The oil-water separation material based on the polyester bottle flake regenerated fiber is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle chip, 15 parts of polyvinylpyrrolidone, 2.5 parts of coupling agent, 7.5 parts of carbon nanotube sponge, 7.5 parts of chloro pivaloyl chloride, 2.8 parts of adamantyl chloride, 9 parts of 4, 4-chloroformyl phenyl ether, 3.5 parts of anhydrous aluminum chloride and 3.5 parts of amino-terminated hyperbranched polysiloxane HPSi-NH 2 23 parts.
The coupling agent is a mixture formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:2:2; the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30 provided by Shanghai Fuqing materials science and technology Co., ltd; the carbon nanotube sponge is as described in example 1 of CN106257597BThe method is used for manufacturing; the amino-terminated hyperbranched polysiloxane HPSi-NH 2 Is prepared as in example 1 of CN 110156948B.
The preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber comprises the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding the mixture into isopropanol, uniformly stirring, soaking the polyester bottle flake based regenerated fiber non-woven fabric blank after hot pressing and reinforcement in the mixture for 9.5 hours, taking out the mixture, and drying the mixture at 75 ℃ to constant weight.
The melt-blowing temperature is 285 ℃; the temperature of the rolling mill during rolling is 160 ℃, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 320 revolutions per minute.
The organic solvent in the step S2 is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1:9.5; the process conditions of the hot-pressing reinforcement are as follows: the hot pressing temperature is 128 ℃, the hot pressing pressure is 1800KG, the preheating time is 24min, the hot pressing time is 5.5min, and the die opening temperature is 63 DEG C
The amino-terminated hyperbranched polysiloxane HPSi-NH in the step S3 2 The mass ratio of the isopropanol is 1:7.5.
Example 5
The oil-water separation material based on the polyester bottle flake regenerated fiber is prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle chip, 16 parts of polyvinylpyrrolidone and coupling agent3 parts of carbon nanotube sponge, 8 parts of chloro pivaloyl chloride, 3 parts of adamantyl chloride, 10 parts of 4, 4-chloroformyl phenyl ether, 4 parts of anhydrous aluminum chloride and end amino hyperbranched polysiloxane HPSi-NH 2 25 parts.
The coupling agent is a silane coupling agent KH550; the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30 provided by Shanghai Fuqing materials science and technology Co., ltd; the carbon nanotube sponge was made according to the method of example 1 in CN 106257597B; the amino-terminated hyperbranched polysiloxane HPSi-NH 2 Is prepared as in example 1 of CN 110156948B.
The preparation method of the oil-water separation material based on the polyester bottle flake regenerated fiber comprises the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding the mixture into isopropanol, uniformly stirring, soaking the polyester bottle flake based regenerated fiber non-woven fabric blank after hot pressing and reinforcing in the mixture for 10 hours, taking out the mixture, and drying the mixture at 80 ℃ to constant weight.
The melt-blowing temperature is 290 ℃; the temperature of the rolling mill during rolling is 165 ℃, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 330 revolutions per minute; the organic solvent in the step S2 is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1:10; the process conditions of the hot-pressing reinforcement are as follows: the hot pressing temperature is 130 ℃, the hot pressing pressure is 1800KG, the preheating time is 25min, the hot pressing time is 6min, and the die opening temperature is 65 DEG C
The amino-terminated hyperbranched polysiloxane HPSi-NH in the step S3 2 The mass ratio of the isopropanol is 1:8.
Comparative example 1
An oil-water separation material based on a regenerated fiber of a polyester bottle chip was substantially the same as in example 1, except that a carbon nanotube sponge and adamantyl chloride were not added.
Comparative example 2
An oil-water separation material based on polyester bottle flake regenerated fiber, which is substantially the same as in example 1, except that no amino-terminated hyperbranched polysiloxane HPSi-NH was added 2 And chloro pivaloyl chloride.
In order to further illustrate the unexpected positive technical effects of the products of the embodiments of the invention, oil absorption performance of the oil-water separation material based on the regenerated fibers of the polyester bottle flakes prepared by the embodiments is detected, the test results are shown in table 1, and the test oil is gasoline, and is measured according to the current national standard of China. Wherein the cycle number is the maximum cycle number at which the saturated oil absorption magnification is maintained at 95% or more. The method for testing the oil-water separation effect of the filtering mode comprises the following steps: the prepared oil-water separation material is longitudinally cut into round pieces with the thickness of about 1.5mm, the round pieces are fixed between two glass tubes, an empty beaker is connected below each glass tube, then 200 milliliters of oil (n-hexane, sudan III is dyed red, the volume is 20 milliliters) water (pure water, the volume is 180 milliliters) mixture is poured above the material, the oil-water separation process is observed, and the time for completely separating the oil from the water is recorded. The above oil-water separation process test was repeated to examine the repeated (20 times) use ability of the material.
TABLE 1
From table 1, it can be seen that the oil-water separation material based on the polyester bottle flake regenerated fiber disclosed in the embodiment of the invention has excellent oil absorption capacity, cycle performance and oil-water separation effect. Carbon nanotube sponge, adamantyl chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 And the incorporation of chloro pivaloyl chloride is beneficial for improving the above properties.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way; those of ordinary skill in the art will readily implement the invention as described above; however, those skilled in the art will appreciate that many modifications, adaptations, and variations of the present invention are possible in light of the above teachings without departing from the scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the present invention.

Claims (9)

1. The oil-water separation material based on the polyester bottle flake regenerated fiber is characterized by being prepared from the following raw materials in parts by weight: 100 parts of recovered polyester bottle chip, 12-16 parts of polyvinylpyrrolidone, 1-3 parts of coupling agent, 5-8 parts of carbon nanotube sponge, 5-8 parts of chloro pivaloyl chloride, 2-3 parts of adamantyl chloride, 5-10 parts of 4, 4-chloroformyl phenyl ether, 2-4 parts of anhydrous aluminum chloride and amino-terminated hyperbranched polysiloxane HPSi-NH 2 15-25 parts.
2. The oil-water separation material based on the regenerated fiber of the polyester bottle flakes according to claim 1, wherein the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560, and a silane coupling agent KH 570.
3. The oil-water separation material based on the regenerated fiber of the polyester bottle flakes according to claim 1, wherein the polyvinylpyrrolidone is polyvinylpyrrolidone PVP K30.
4. A method for preparing the oil-water separation material based on the regenerated fiber of the polyester bottle flake according to any one of claims 1 to 3, comprising the following steps:
step S1, uniformly mixing and mixing the recycled polyester bottle flakes, polyvinylpyrrolidone, a coupling agent and carbon nanotube sponge according to parts by weight to obtain a mixed material, adding the mixed material into a double-screw extruder, sequentially carrying out melt blowing, net forming and rolling by a rolling mill to form cloth, placing the cloth into deionized water, removing the polyvinylpyrrolidone by an ultrasonic method, and drying to obtain a regenerated fiber non-woven fabric blank based on the polyester bottle flakes;
step S2, uniformly dispersing chloro pivaloyl chloride, adamantyl chloride, 4-chloroformyl phenyl ether and anhydrous aluminum chloride in an organic solvent, spraying the organic solvent on a regenerated fiber non-woven fabric blank based on a polyester bottle chip, and carrying out hot pressing reinforcement through a vacuum press;
s3, hyperbranched polysiloxane HPSi-NH with terminal amino groups 2 Adding into isopropanol, stirring, soaking the hot-pressed and reinforced regenerated fiber non-woven fabric blank based on polyester bottle flakes in the mixture for 6-10 hours, taking out, and drying at 60-80 ℃ to constant weight.
5. The method for producing an oil-water separation material based on recycled polyester bottle flakes according to claim 4, wherein the melt-blowing temperature is 270 to 290 ℃.
6. The method for preparing an oil-water separation material based on polyester bottle flake regenerated fiber according to claim 4, wherein the temperature of the rolling mill is 125-165 ℃ when the rolling mill rolls, and the speed of the non-woven fabric blank passing through the hot roller of the rolling mill is 200-330 rpm.
7. The method for producing an oil-water separation material based on recycled polyester bottle flakes according to claim 4, wherein the organic solvent in step S2 is chloroform; the mass ratio of the 4, 4-chloroformyl phenyl ether to the organic solvent is 1 (8-10).
8. The method for preparing the oil-water separation material based on the polyester bottle flake regenerated fiber according to claim 4, wherein the hot-press reinforcement process conditions are as follows: the hot pressing temperature is 120-130 ℃, the hot pressing pressure is 1800KG, the preheating time is 18-25min, the hot pressing time is 4-6min, and the die opening temperature is 55-65 ℃.
9. The method for producing an oil-water separation material based on recycled polyester bottle flakes according to claim 4, wherein the amino-terminated hyperbranched polysiloxane HPSi-NH in step S3 2 The mass ratio of the isopropanol is 1 (5-8).
CN202310563279.3A 2023-05-18 2023-05-18 Oil-water separation material based on polyester bottle flake regenerated fiber and preparation method thereof Active CN116657406B (en)

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