CN111099842A - Super-hydrophobic glass fiber prepared based on two-step method, modification method and application - Google Patents
Super-hydrophobic glass fiber prepared based on two-step method, modification method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/40—Organo-silicon compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2003—Glass or glassy material
- B01D39/2017—Glass or glassy material the material being filamentary or fibrous
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/0216—Bicomponent or multicomponent fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
Abstract
The invention belongs to the technical field of material modification, and particularly relates to super-hydrophobic glass fiber prepared based on a two-step method, a modification method and application. The glass fiber is subjected to super-hydrophobic grafting modification treatment by adopting a chemical grafting copolymerization technology and based on an amination and silanization continuous modification method in cooperation with an initiator and a coupling agent. The invention also discloses application of the modified glass fiber prepared by the method in separation of oil-water mixed liquid. The hyperbranched polymer with hydrophobic property is introduced on the surface of the glass fiber, the affinity effect of the hydrophobic group and the organic phase is utilized, the adhesive force of the interface organic phase is improved, the plasticity and the wear resistance of the glass fiber are improved, the hydrophobic property of the glass fiber is obviously improved, and the reinforced separation effect on the oil phase in the oil-water mixed solution is realized. The glass fiber modified by the method has excellent oleophylic and hydrophobic properties, is reliable and stable, and has wide applicability.
Description
Technical Field
The invention relates to the technical field of material modification, in particular to super-hydrophobic glass fiber prepared based on a two-step method, a modification method and application.
Background
In the chemical machinery industry, a large amount of organic waste liquid with complex components, high toxicity and difficult treatment is generated while a specific product is prepared, and the research and development of novel efficient organic waste liquid separation materials have attracted great attention of people. Although the hydrophobic property and oleophylic property of the novel material researched and manufactured around the high hydrophobic property are improved, the practical application of the novel material is greatly hindered by the complicated manufacturing process, high manufacturing cost and extremely limited application conditions. On the contrary, the functional modification of the low-cost material as a matrix to prepare a material with high hydrophobic property has become a current research hotspot.
The glass fiber is an inorganic non-metallic material with excellent performance, has the advantages of good corrosion resistance, strong heat resistance, good insulativity and high tensile strength, is a fiber filler obtained by mixing and weaving the glass fiber and the polymer fiber, has good mechanical strength, and can be used as a main component of a fiber bed to realize the separation of oil-water mixed liquid. However, the glass fiber does not have obvious hydrophilic and hydrophobic characteristics, and the surface modification of the glass fiber can endow the glass fiber with specific hydrophilic and hydrophobic characteristics, so that the glass fiber is an effective way for enhancing the oil-water separation performance of the fiber filler.
The Chinese invention patent CN 105293955A discloses a glass fiber modification method and application thereof. The method is based on a glass fiber raw material with micron scale, namely the length of 10-50 mu m and the diameter of 8-15 mu m, and adopts continuous processes of hydroxylation, silanization and ammonia grafting end capping in sequence to obtain the modified glass fiber. However, because the method involves continuous chemical reaction under the action of various initiators, the modification process is complex, the modification period is long, the stability is poor, the reliability is low, the preparation cost is high, and the method is not suitable for the requirements of glass fiber super-hydrophobic modification.
Graft copolymerization is a chemical modification method of polymer, and the principle is that through graft copolymerization, the kind of atoms or atom groups on a macromolecular chain and the combination mode thereof are changed, and hydrophilic or lipophilic, acidic or basic, plastic groups can be introduced, so that the original performance of the material is enhanced or new characteristics are endowed to the material. The chemical graft copolymerization has the advantages of simple process, low requirements on equipment and environment, stable modification performance, no pollution and the like, and is widely applied to the modification of polymers.
Disclosure of Invention
The invention aims to solve the technical problem of developing a glass fiber super-hydrophobic modification method with excellent and reliable performance and simple and flexible process.
In order to solve the problems, the invention provides a super-hydrophobic glass fiber modification method based on a two-step method, which comprises the following steps:
the method comprises the following steps: carrying out amination treatment on the glass fiber subjected to the pre-cleaning treatment to prepare aminated glass fiber;
step two: performing silanization treatment on the aminated glass fiber to prepare the super-hydrophobic glass fiber;
step one, the diameter of the raw material glass fiber is 10-20 μm;
soaking a certain mass of glass fiber raw material for 1-2 hours by sequentially adopting an acetone solution (20-50% volume fraction) and an ethanol solution (20-50% volume fraction), then transferring the glass fiber raw material into deionized water for ultrasonic treatment for 15-30 minutes, and finally drying the glass fiber raw material in a vacuum constant temperature box for later use, wherein the drying temperature is controlled to be 60-80 ℃, and the drying time is 6-12 hours;
step one, the glass fiber after the pre-cleaning treatment is placed in a Tri-HCl buffer solution, 0.5-1.0% (mass fraction) of dopamine hydrochloride is added into the glass fiber under the stirring condition (150-200rpm), and the reaction lasts for 10-12 hours. After the reaction is finished, washing the aminated glass fiber for 3-4 times by sequentially adopting 10-20% (volume fraction) ethanol solution and deionized water. Drying at low temperature in a vacuum incubator for 4-6 hours at the drying temperature of 30-40 ℃;
step one, the preparation process of the Tri-HCl buffer solution comprises the following steps: weighing 100-120g of tris (hydroxymethyl) aminomethane, and placing the tris (hydroxymethyl) aminomethane in 800-1000mL of deionized water to be fully stirred and dissolved. Dropwise adding a hydrochloric acid solution into the solution, adjusting the pH to 8.0-8.5, sterilizing at high temperature and high pressure, and storing at room temperature;
and step two, adding the aminated glass fiber obtained in the step one into an absolute ethyl alcohol solution containing 10-20 mass percent of APTES by taking glacial acetic acid as an initiator, and stirring and reacting for 6-12 hours at the constant temperature of 80-90 ℃ by taking the glacial acetic acid as the initiator. After the reaction is finished, cleaning the silanized glass fiber for 2-3 times by sequentially adopting 10-20% (volume fraction) of ethanol solution and deionized water. And drying at low temperature in a vacuum incubator for 10-12 hours at the drying temperature of 30-40 ℃.
Has the advantages that:
the invention provides a super-hydrophobic glass fiber modification method based on a two-step method. And then APTES is used as a grafting monomer, and a chemical graft copolymerization technology is utilized to introduce hydrophobic silane groups into a matrix, so that the glass fiber is endowed with high hydrophobic property. Compared with the reported continuous grafting copolymerization modification method of the glass fiber, the super-hydrophobic modification method of the glass fiber has the advantages of simple and flexible process, low material cost, no toxicity, stable and reliable reinforced hydrophobic performance and low requirement on experimental equipment. The method of the invention is adopted to carry out surface super-hydrophobic modification on glass sheets (with the thickness of 0.17mm) of the same material, and a contact angle meter is utilized to measure the contact angle of water drops on the glass sheets before and after modification, and the contact angle is increased from 123.187 degrees to 157.643 degrees. The modified glass fiber and the polymer fiber are co-woven in combination with the post-treatment process, so that the novel high-hydrophobicity fiber filler suitable for treating the oil-water mixed liquid of a complex system can be prepared, and the application prospect is wide.
Drawings
FIG. 1 is a process flow diagram of a super-hydrophobic glass fiber modification method based on a two-step method.
Fig. 2 is a dopamine silanization modification mechanism.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The method comprises the following steps: 100g of glass fiber (diameter 20 μm) is weighed, and is firstly subjected to the following pre-cleaning treatment to remove original oily substances and other impurities on the surface of the raw material glass fiber:
1, sequentially soaking in 50 percent (volume fraction) acetone solution (national drug group chemical reagent Co., Ltd.) and 50 percent (volume fraction) ethanol for 2 hours respectively;
2, transferring the mixture into deionized water for ultrasonic treatment for 30 minutes;
and 3, drying the cleaned glass fiber in a vacuum constant temperature oven at the temperature of 60 ℃ for 8 hours for later use.
The method comprises the following steps: preparing Tri-HCl buffer solution: 120g of tris (hydroxymethyl) aminomethane was weighed into 800mL of deionized water and stirred well. 35mL of concentrated hydrochloric acid was added dropwise thereto to adjust the pH of the solution to 8.5. The solution is subjected to constant volume to 1L, sterilized at high temperature and high pressure, and then stored at room temperature.
The method comprises the following steps: the glass fiber after the pre-washing treatment was placed in a Tri-HCl buffer solution, 0.5% (mass fraction) of dopamine hydrochloride was added thereto, and the reaction was carried out at room temperature for 10 hours under stirring at 150 rpm. After the reaction is finished, the aminated glass fiber is sequentially washed for 3 times by using 20 percent (volume fraction) of ethanol solution and deionized water. And drying at low temperature in a vacuum incubator for 6 hours at the drying temperature of 30 ℃. Thereby obtaining the aminated glass fiber.
Step two: and (3) placing the aminated glass fiber obtained in the step one into an absolute ethyl alcohol solution containing 10 mass percent of APTES, matching with an initiator glacial acetic acid, and stirring and reacting for 6 hours at a constant temperature of 80 ℃ to obtain the silanized glass fiber. The alkylated modified glass fibers were washed 2 times with 20% (volume fraction) ethanol solution and deionized water in sequence. And drying at a low temperature of 30 ℃ for 12 hours in a vacuum incubator. And preparing the super-hydrophobic glass fiber.
Hydrophobic silane groups are not completely attached to the surfaces of the super-hydrophobic glass fibers obtained under the conditions, the super-hydrophobic glass fibers and the polypropylene fibers are co-woven into a fiber net for separating oil-water mixed liquid (the volume ratio of n-octane to water is 1:1), and the separation efficiency is only 75%. This is because the dopamine hydrochloride concentration is low during the amination process, so that the polydopamine modified layer formed on the surface of the glass fiber by the self-polymerization reaction of dopamine in the Tri-HCl buffer solution is not uniform, and complete adhesion to the fiber surface cannot be achieved. And in the subsequent silanization modification process, the hydrophobic silane groups introduced by graft copolymerization are unevenly distributed on the surface of the glass fiber and are fewer in number. In addition, there is also a mutual occlusion between the fibers during the weaving into a web. The above factors act together to finally influence the super-hydrophobic property and the application of the modified glass fiber.
Example 2
The method comprises the following steps: after the glass fiber was subjected to the preliminary washing treatment as described in example 1, it was placed in Tri-HCl buffer, 1.0% (mass fraction) of dopamine hydrochloride was added thereto, and the mixture was reacted at room temperature for 12 hours under stirring at 150 rpm. After the reaction is finished, the aminated glass fiber is sequentially washed for 3 times by using 20 percent (volume fraction) of ethanol solution and deionized water. And drying at low temperature in a vacuum incubator for 6 hours at the drying temperature of 30 ℃. Thereby obtaining the aminated glass fiber.
Step two: placing the aminated glass fiber obtained in the step one into an absolute ethyl alcohol solution containing 20 percent (mass fraction) of APTES, matching with an initiator glacial acetic acid, and stirring and reacting for 10 hours at a constant temperature of 90 ℃ to obtain the silanized glass fiber. The alkylated modified glass fibers were washed 2 times with 20% (volume fraction) ethanol solution and deionized water in sequence. And drying at a low temperature of 40 ℃ for 12 hours in a vacuum incubator. And preparing the super-hydrophobic glass fiber.
Under the condition, a large number of hydrophobic silane groups are attached to the surface of the obtained super-hydrophobic glass fiber, but the obtained hydrophobic modified layer is poor in stability and can partially fall off in the process of being co-woven with polypropylene fiber into a fiber net, so that the separation efficiency of the oil-water mixed liquid (the volume ratio of n-octane to water is 1:1) is only 83%. In addition, along with the increase of the use times of the co-woven fiber, the silanization modified layer gradually falls off, the separation efficiency gradually decreases, and the super-hydrophobic property and the application of the modified glass fiber are influenced.
Example 3
The method comprises the following steps: aminated glass fibers were obtained as described in example 2;
step two: and (3) placing the aminated glass fiber obtained in the step one into an absolute ethyl alcohol solution containing 10 mass percent of APTES, matching with an initiator glacial acetic acid, and stirring and reacting for 8 hours at a constant temperature of 80 ℃ to obtain the silanized glass fiber. The alkylated modified glass fibers were washed 2 times with 20% (volume fraction) ethanol solution and deionized water in sequence. And drying at a low temperature of 40 ℃ for 12 hours in a vacuum incubator. And preparing the super-hydrophobic glass fiber.
A large amount of hydrophobic silane groups are attached to the surface of the super-hydrophobic glass fiber obtained under the condition, meanwhile, the modified layer has good stability, the super-hydrophobic glass fiber and the polypropylene fiber are co-woven into a fiber net and applied to separation of an oil-water mixed solution (the volume ratio of n-octane to water is 1:1), and the separation efficiency is improved to 93%. The dopamine molecule forms a compact and stable amino modified layer on the surface of the glass fiber, and APTES forms a silane graft copolymer with uniform distribution and high hydrophobic property on the surface of the amino modified layer under the initiation action of glacial acetic acid, so that the hydrophobic and oleophilic properties of the glass fiber are obviously improved.
Claims (8)
1. A super-hydrophobic glass fiber prepared based on a two-step method is characterized in that firstly, amination treatment is carried out on pre-cleaned glass fiber, an amino modified layer is attached to the surface of the glass fiber, the specific surface area of the fiber is increased, and silanization modified binding sites are provided; and then, introducing hydrophobic silane groups into a matrix by using APTES as a grafting monomer and utilizing a chemical graft copolymerization technology to prepare the super-hydrophobic glass fiber.
2. The super-hydrophobic glass fiber modification method based on the two-step method is characterized by comprising the following specific modification steps:
the method comprises the following steps: carrying out amination treatment on the glass fiber subjected to the pre-cleaning treatment to prepare aminated glass fiber;
step two: and performing silanization treatment on the aminated glass fiber to prepare the super-hydrophobic glass fiber.
3. The method of claim 2, wherein the diameter of the raw glass fiber in the first step is 10-20 μm.
4. The method for modifying superhydrophobic glass fiber according to two-step method, according to claim 2, wherein the pre-washing treatment of raw glass fiber in the first step is: soaking the raw material glass fiber in an acetone solution accounting for 20-50% of the total volume and an ethanol solution accounting for 20-50% of the total volume for 1-2 hours, then transferring the raw material glass fiber into deionized water for ultrasonic treatment for 15-30 minutes, and finally drying the raw material glass fiber in a vacuum thermostat at 60-80 ℃ for later use and drying the raw material glass fiber for 6-12 hours.
5. The method of claim 2, wherein the method comprises: the amination treatment after the pre-cleaning treatment in the step one is as follows: placing the glass fiber in Tri-HCl buffer solution, adding dopamine hydrochloride accounting for 0.5-1.0% of the total mass under the stirring condition of 150-; after the reaction is finished, sequentially cleaning the aminated glass fiber for 3-4 times by using an ethanol solution accounting for 10-20% of the total volume and deionized water; drying at low temperature in vacuum incubator, controlling drying temperature at 30-40 deg.C, and drying for 4-6 hr.
6. The method for modifying superhydrophobic glass fiber according to claim 1, wherein the method comprises: the Tri-HCl buffer solution is prepared by the following steps: weighing 100-120g of trihydroxymethyl aminomethane, and fully stirring and dissolving in 800-1000mL of deionized water; adding hydrochloric acid solution into the above solution, adjusting pH to 8.0-8.5, sterilizing at high temperature and high pressure, and storing at room temperature.
7. The method of claim 2, wherein the method comprises: the silanization treatment of the aminated glass fiber in the second step comprises the following steps: 3-amino-triethoxy silane APTES is adopted to carry out silanization modification on the aminated glass fiber; adding the aminated glass fiber obtained in the step one into an absolute ethyl alcohol solution containing APTES with the mass fraction of 10-20% of the total mass, taking glacial acetic acid as an initiator, and stirring and reacting for 6-12 hours at the constant temperature of 80-90 ℃; after the reaction is finished, sequentially cleaning the silanized glass fiber for 2-3 times by using ethanol solution and deionized water which account for 10-20% of the total volume; drying at low temperature of 30-40 deg.C for 10-12 hr in vacuum incubator; and preparing the super-hydrophobic glass fiber.
8. The application of the super-hydrophobic glass fiber prepared based on the two-step method is characterized in that the super-hydrophobic glass fiber prepared by the two-step method and polymer fiber are co-woven to prepare the novel high-hydrophobic fiber filler suitable for oil-water mixed liquid.
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| CN112322064A (en) * | 2020-11-12 | 2021-02-05 | 东北林业大学 | Method for reinforcing wood powder/polyolefin composite material by using surface-treated continuous aramid fiber |
| CN112429978A (en) * | 2020-12-14 | 2021-03-02 | 山东明珠材料科技有限公司 | Glass fiber material modification reinforced molding treatment method |
| CN114653349A (en) * | 2022-03-17 | 2022-06-24 | 中国原子能科学研究院 | Modified glass fiber membrane and preparation method and application thereof |
| CN115975289A (en) * | 2022-12-27 | 2023-04-18 | 富联裕展科技(深圳)有限公司 | Plastic composite material and manufacturing method thereof |
| CN115975289B (en) * | 2022-12-27 | 2024-05-17 | 富联裕展科技(深圳)有限公司 | Plastic composite material and manufacturing method thereof |
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