CN112267298A - Preparation method of hydrophobic cotton fabric and hydrophobic cotton - Google Patents
Preparation method of hydrophobic cotton fabric and hydrophobic cotton Download PDFInfo
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- CN112267298A CN112267298A CN202011175668.1A CN202011175668A CN112267298A CN 112267298 A CN112267298 A CN 112267298A CN 202011175668 A CN202011175668 A CN 202011175668A CN 112267298 A CN112267298 A CN 112267298A
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 140
- 239000004744 fabric Substances 0.000 title claims abstract description 120
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title abstract description 12
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000243 solution Substances 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 28
- 229940074391 gallic acid Drugs 0.000 claims abstract description 25
- 235000004515 gallic acid Nutrition 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000001412 amines Chemical class 0.000 claims abstract description 15
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 15
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 15
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical class [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 9
- 239000011593 sulfur Substances 0.000 claims abstract description 9
- 239000002262 Schiff base Substances 0.000 claims abstract description 7
- 150000004753 Schiff bases Chemical class 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 238000006845 Michael addition reaction Methods 0.000 claims abstract description 6
- 239000010949 copper Substances 0.000 claims description 41
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 24
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 8
- 229910001431 copper ion Inorganic materials 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000009795 derivation Methods 0.000 description 2
- RRQQLCXFGWWLPQ-UHFFFAOYSA-N ethanol;octadecan-1-amine Chemical compound CCO.CCCCCCCCCCCCCCCCCCN RRQQLCXFGWWLPQ-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000003075 superhydrophobic effect Effects 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明提出了一种疏水棉织物的制备方法及疏水棉，其中，方法包括：将棉织物依次浸没在铜离子盐溶液和没食子酸溶液中以使所述棉织物表面形成GA‑Cu(Ⅱ)络合物改性层；在碱性条件下，通过迈克尔加成或席夫碱反应使得GA‑Cu(Ⅱ)络合物改性层与含胺、硫或醇的分子反应以生成长链烃类物质而获得疏水性能。本发明通过在棉织物表面形成GA‑Cu(Ⅱ)络合物改性层，从而使得棉织物具备初步的疏水性能，并且具有良好的耐用性；而后，将GA‑Cu(Ⅱ)络合物改性层与含胺、硫或醇的分子反应以生成长链烃类物质，用以进一步降低棉织物的表面能，从而加强了本发明棉织物的疏水性能及耐污能力。此外，本发明的疏水棉的制备方法还具有操作简单成本低廉等特点。
The present invention provides a method for preparing a hydrophobic cotton fabric and a hydrophobic cotton, wherein the method comprises: immersing the cotton fabric in a copper ion salt solution and a gallic acid solution in sequence to make the surface of the cotton fabric form GA-Cu(II) Complex-modified layer; the GA-Cu(II) complex-modified layer reacts with amine, sulfur, or alcohol-containing molecules to generate long-chain hydrocarbons by Michael addition or Schiff base reaction under alkaline conditions similar substances to obtain hydrophobic properties. In the present invention, the modified layer of GA-Cu(II) complex is formed on the surface of the cotton fabric, so that the cotton fabric has preliminary hydrophobic performance and good durability; then, the GA-Cu(II) complex is The modified layer reacts with amine, sulfur or alcohol-containing molecules to generate long-chain hydrocarbon substances to further reduce the surface energy of the cotton fabric, thereby enhancing the hydrophobicity and stain resistance of the cotton fabric of the present invention. In addition, the preparation method of the hydrophobic cotton of the present invention also has the characteristics of simple operation and low cost.
Description
Technical Field
The invention relates to the field of textile processing, in particular to a preparation method of hydrophobic cotton fabric and the hydrophobic cotton.
Background
Cotton fabrics are widely used in daily life due to their unique softness, air permeability, warmth retention, comfort and biodegradability. In recent years, more and more researchers have attracted interest by giving the fabric self-cleaning, antibacterial, anti-pollution, water-oil separation and other functions through surface hydrophobic modification.
Many methods for preparing superhydrophobic fabrics have been developed through various methods, such as sol-gel method, chemical etching method, dip coating method, chemical bath deposition method, and chemical vapor deposition method, etc. Most of the existing methods for preparing the super-hydrophobic fabric are time-consuming and complex to operate, and most of the manufacturing methods involve the application of fluorine compounds, are easy to cause pollution and have high cost.
Disclosure of Invention
In order to solve the technical problems in the background art, in one aspect of the present invention, a method for preparing a hydrophobic cotton fabric is provided, the method comprising: sequentially immersing a cotton fabric in a copper ion salt solution and a gallic acid solution to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric; hydrophobic properties are obtained by reacting the GA-Cu (ii) complex modification layer with an amine, sulfur or alcohol containing molecule under basic conditions by michael addition or schiff base reaction to produce long chain hydrocarbon species.
In one or more embodiments, the copper ion salt solution comprises: copper sulfate solution or copper chloride solution.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: immersing the cotton fabric in copper sulfate solution with the concentration of 2.5mg/ml-15mg/ml, and preserving the temperature for 30min at 70-100 ℃.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: immersing the cotton fabric in copper sulfate solution with the concentration of 10mg/ml, and keeping the temperature at 80 ℃ for 30 min.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: immersing the cotton fabric taken out of the copper sulfate solution in a gallic acid solution with the concentration of 2mg/ml-14mg/ml so as to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: immersing the cotton fabric taken out of the copper sulfate solution in a gallic acid solution with the concentration of 12.8mg/ml so as to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: immersing the cotton fabric with the GA-Cu (II) complex modified layer in an octadecyl amine ethanol aqueous solution with the concentration of 2mg/ml-10mg/ml, and preserving the temperature for 1h-8h at room temperature, so that the GA-Cu (II) complex modified layer of the cotton fabric reacts with molecules containing amine and alcohol to generate long-chain hydrocarbon substances to obtain the hydrophobic property.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: immersing the cotton fabric with the GA-Cu (II) complex modified layer in an octadecyl amine ethanol water solution with the concentration of 8mg/ml, and preserving the temperature for 4h at room temperature, so that the GA-Cu (II) complex modified layer of the cotton fabric reacts with molecules containing amine and alcohol to generate long-chain hydrocarbon substances to obtain the hydrophobic property.
In one or more embodiments, the method of making a hydrophobic cotton fabric further comprises: before immersing the cotton fabric with the GA-Cu (II) complex modified layer in an octadecyl amine ethanol water solution, washing and drying the cotton fabric with the GA-Cu (II) complex modified layer by using deionized water.
In another aspect of the invention, the invention also provides a hydrophobic cotton fabric, and the hydrophobic cotton fabric is prepared by the preparation method of the hydrophobic cotton fabric.
The beneficial effects of the invention include: according to the invention, the GA-Cu (II) complex modified layer is formed on the surface of the cotton fabric, so that the cotton fabric obtains hydrophobic property preliminarily, and the structure of the GA-Cu (II) complex is stable, so that the durability of the hydrophobic cotton is ensured; and then, the GA-Cu (II) complex modified layer reacts with molecules containing amine, sulfur or alcohol to generate long-chain hydrocarbon substances through Michael addition or Schiff base reaction, so that the surface energy of the cotton fabric is further reduced, the hydrophobic property of the cotton fabric is enhanced, and the hydrophobic cotton fabric has better stain resistance due to lower surface energy. In addition, the preparation method of the hydrophobic cotton has the characteristics of simple operation, low cost and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other embodiments can be obtained by using the drawings without creative efforts.
FIG. 1 is a flow chart of a method of making hydrophobic cotton according to an embodiment of the present invention;
FIG. 2 is an infrared spectrum of cotton fabric at various stages of preparation according to an embodiment of the present invention;
FIG. 3 is a comparative schematic of the hydrophobic capacity of hydrophobic cotton of an embodiment of the present invention;
FIG. 4 is a state diagram before oil-water separation according to an embodiment of the present invention;
FIG. 5 is a state diagram after oil-water separation according to an embodiment of the present invention;
FIG. 6 is a diagram showing the hydrophobic cotton of the embodiment of the present invention before oil-water separation;
fig. 7 is a diagram showing the state of the hydrophobic cotton according to the embodiment of the present invention after oil-water separation.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following embodiments of the present invention are described in further detail with reference to the accompanying drawings.
The invention provides a preparation method of hydrophobic cotton, which is generally completed in two steps, wherein in the first step, a GA-Cu (II) complex modified layer is formed on cotton fabric through the quick coordination assembly reaction of GA (gallic acid) and Cu (II) (divalent copper ions), the reaction is very quick, and the color of the cotton fabric is changed from white to light yellow; in the second step, the GA-Cu (ii) complex modification layer is reacted with an amine, sulfur or alcohol containing molecule to produce a long chain hydrocarbon species by michael addition or schiff base reaction under basic conditions to produce a hydrophobic surface.
The method comprises the following steps of preparing a GA-Cu (II) complex modified layer, preparing a Schiff base reaction product, and reacting the GA-Cu (II) complex modified layer with a molecular containing amine, sulfur or alcohol to generate long-chain hydrocarbon substances, wherein the GA-Cu (II) complex modified layer formed by GA and Cu (II) is relatively stable and has relatively high reaction speed, and the cotton fabric has certain hydrophobic capacity. The more specific preparation method of the hydrophobic cotton comprises the following steps:
FIG. 1 is a flow chart of the process for making hydrophobic cotton according to the present invention. In the example shown in fig. 1, the hydrophobic cotton preparation method comprises: step S1, immersing the cotton fabric in the copper ion salt solution and the gallic acid solution in sequence to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric; and step S2, reacting the GA-Cu (II) complex modified layer with amine, sulfur or alcohol containing molecules to generate long chain hydrocarbon substances by Michael addition or Schiff base reaction under alkaline conditions to obtain hydrophobic property. The copper ion salt solution comprises a copper sulfate solution or a copper chloride solution. The description will be made below with reference to a copper sulfate solution.
In a further embodiment, step S1 specifically includes immersing the cotton fabric in a copper sulfate solution having a concentration of 2.5mg/ml to 15mg/ml, and incubating at 70 ℃ to 100 ℃ for 30 min. The purpose of the step is to make the divalent copper ions uniformly adsorbed on the surface of the cotton fabric; the cotton fabric can be diluted by deionized water to remove redundant divalent copper ions, and ultrasonic oscillation can be assisted to ensure a better removal effect.
Further, the step S1 specifically includes immersing the cotton fabric taken out of the copper sulfate solution in a gallic acid solution with a concentration of 2mg/ml to 14mg/ml, so that a GA-Cu (ii) complex modified layer is formed on the surface of the cotton fabric. The cotton fabric has certain hydrophobic property, and the GA-Cu (II) complex structure is stable, so that the hydrophobic cotton prepared by the method has good durability.
In the embodiment of step S1, the present invention further provides a preferred embodiment, which includes: immersing the cotton fabric in a copper sulfate solution with the concentration of 10mg/ml, and preserving the heat for 30min at 80 ℃; then, the cotton fabric taken out of the copper sulfate solution is immersed in a gallic acid solution with the concentration of 12.8mg/ml, so that a GA-Cu (II) complex modified layer is formed on the surface of the cotton fabric. The preferred embodiments are presented with the objective of having hydrophobic properties as a first priority, and other combinations of preferred embodiments may be created with other objectives such as cost, etc. as a priority or consideration, and the invention is not limited in this regard. Various combinations are listed below in table 1 to illustrate the derivation of the preferred embodiment.
TABLE 1 Effect of CuSO4 concentration on the hydrophobic Properties of modified Cotton fabrics
As shown in table 1, when the concentration of the gallic acid solution was constant (specifically, 12.8mg/ml), the contact angle of the cotton fabric prepared by the step S1 with deionized water increased and then decreased as the concentration of the copper sulfate solution increased, and had the largest contact angle at the concentration of the copper sulfate solution of 10 mg/ml. As can be seen from Table 1, in another embodiment for cost savings, a copper sulfate solution concentration of 7.5mg/ml may be used. Of course, Table 1 is only made at a gallic acid solution concentration of 12.8mg/ml, and other preferred examples obtained by the same method using other gallic acid solutions are also within the protection of the present invention, and the comparison of the present invention is not limited.
Based on the above step S1 embodiment, in the specific embodiment of step S2, step S2 specifically includes immersing the cotton fabric with the GA-Cu (II) complex modified layer in an ethanol aqueous solution of octadecylamine with the concentration of 2mg/ml to 10mg/ml, and keeping the temperature at room temperature for 1h to 8h, so that the GA-Cu (II) complex modified layer of the cotton fabric reacts with molecules containing amine and alcohol to generate long-chain hydrocarbon substances to obtain hydrophobic property. The principle is that after the gallic acid and bivalent copper ion generate GA-Cu (II) complex, the free carboxyl of the gallic acid can also react with molecules containing amine, sulfur or alcohol to generate long-chain hydrocarbon substances, so that the surface energy of the hydrophobic cotton is further reduced, and the hydrophobic performance of the hydrophobic cotton is increased.
In the embodiment of step S2, the present invention also provides a preferred embodiment, which comprises immersing the cotton fabric with the GA-Cu (ii) complex modified layer in an aqueous solution of octadecyl amine alcohol with a concentration of 8mg/ml, and incubating at room temperature for 4h, so that the GA-Cu (ii) complex modified layer of the cotton fabric reacts with molecules containing amine and alcohol to generate long-chain hydrocarbon substances to obtain hydrophobic properties. The preferred embodiments are presented with the objective of providing hydrophobic properties, and other combinations of preferred embodiments may be created with the objective of priority or consideration of other objectives, such as manufacturing costs, and the invention is not limited in this regard. Various combinations are listed below in table 2 to illustrate the derivation of the preferred embodiment.
TABLE 2 Effect of octadecylamine concentration on the hydrophobic Properties of modified Cotton fabrics
In table 2, for simpler characterization of the concentration of the octadecylamine ethanol solution, the Octadecylamine (ODA) concentration was substituted. Wherein, when the concentration (12.8mg/ml) of the gallic acid solution and the concentration (10mg/ml) of the copper sulfate solution are unchanged, the contact angle of the cotton fabric prepared by the step S2 and the deionized water is increased and then decreased along with the increase of the concentration of the Octadecylamine (ODA) and the increase of the reaction time, and when the concentration of the Octadecylamine (ODA) is 8mg/ml and the reaction time is 4h, the contact angle of the prepared cotton fabric is the largest, and the hydrophobic property is the best. Of course, Table 2 is only made for the case where the concentration of gallic acid solution is 12.8mg/ml and the concentration of copper sulfate solution is 10mg/ml, and other preferred embodiments obtained by using gallic acid solution with other concentrations are also within the protection of the present invention, and the present invention is not limited thereto.
In a more complete example, the procedure for preparing hydrophobic cotton in the experiments of the present invention is as follows:
a piece of 5cm by 5cm pure cotton fabric was placed in a 500ml beaker, washed clean with deionized water, and then laid flat in the beaker and dried in a vacuum oven at 80 ℃. After drying, putting the washed fabric into a 500ml beaker, adding 20ml of copper sulfate solution with a certain concentration into the beaker, flatly spreading the fabric as much as possible so as to completely soak the fabric, adding 60ml of deionized water after soaking for 30min, ultrasonically shaking the fabric at room temperature until the fabric is fully diluted, adding 20ml of 12.8mg/ml gallic acid solution, ultrasonically shaking the fabric for 30min again, taking out the cotton fabric, washing the cotton fabric with a large amount of deionized water, and drying the cotton fabric in a vacuum oven at 60 ℃ to obtain the gallic acid-metal copper ion complex modified cotton fabric.
And (3) putting the dried modified cotton fabric into 80ml of octadecylamine ethanol aqueous solution with a certain concentration, and reacting for 4 hours at room temperature. And taking out the fabric, washing the fabric with ethanol and a large amount of deionized water, and drying the fabric in a vacuum oven at 60 ℃ to obtain the hydrophobic modified cotton fabric.
Wherein, the comparison graph of the infrared spectrum of the cotton fabric with hydrophobic property obtained primarily in the step S1 and the hydrophobic cotton prepared in the step S2 is shown as the following graph:
FIG. 2 is an infrared spectrogram of cotton fabric at each preparation stage of the present invention. As shown in figure 2, after the gallic acid-copper ion complex-octadecylamine copolymerization modification, the infrared spectrum of the cotton fabric is compared with that before the modification, and the stretching vibration absorption peak of hydroxyl at 3341cm < -1 > is weakened, because part of phenolic hydroxyl is consumed by octadecylamine reaction, so that the hydrophilic hydroxyl on the surface of the cotton fabric is greatly reduced, the surface energy is reduced, and the hydrophobicity of the material is enhanced. In FIG. 2, 2920cm-1 shows an asymmetric stretching vibration absorption peak of-CH 2-in octadecylamine, and 2856cm-1 shows a symmetric stretching vibration absorption peak of-CH 2-in octadecylamine. 1340cm-1 is the-NH-in-plane bending vibration peak of a primary or secondary amine. 1160cm-1, 1110cm-1, 1057cm-1 and 980cm-1 are the stretching vibration absorption peak of-C-O-C-, and 500cm-1 is the characteristic peak of cotton fiber. As can be seen from fig. 2, the surface energy of the hydrophobic cotton prepared through step S2 is significantly reduced compared to the hydrophobic cotton primarily obtained through step S1 and the original cotton fabric, so that the hydrophobic cotton prepared by the method of the present invention has better hydrophobicity, and in addition, the lower surface energy is also stronger in the stain resistance of the hydrophobic cotton prepared by the present invention. FIG. 3 is a comparative graph of the hydrophobic capacity of the hydrophobic cotton of the present invention. As shown in fig. 3, substances such as ink, milk or water are not easily soaked on the hydrophobic cotton fabric of the invention.
In addition, the invention also carries out an oil-water separation experiment of the hydrophobic cotton, and particularly, the experiment is shown in figures 4 to 7. Fig. 4 is a state diagram before oil-water separation. Wherein the water is dyed blue with a water soluble pigment (such as copper sulfate) for convenient discrimination between oil and water. FIG. 5 is a diagram showing a state after oil-water separation. FIG. 6 is a state diagram of the hydrophobic cotton of the present invention before oil-water separation. FIG. 7 is a diagram showing the state of the hydrophobic cotton of the present invention after oil-water separation. In fig. 7 water is blocked on the surface of the hydrophobic cotton fabric. And as can be seen from the results shown in fig. 5, the hydrophobic cotton of the present invention has a good oil-water separation effect.
The method comprises the steps of forming a GA-Cu (II) complex attachment layer by coordination assembly of Gallic Acid (GA) and copper sulfate (CuSO4) on the surface of cotton fabric, and then forming a hydrophobic modification layer on the surface of the cotton fabric by reaction of Octadecylamine (ODA) and carboxyl of the gallic acid. Water-oil separation research shows that the prepared hydrophobic cotton fabric has good separation capacity on oil-water mixtures such as vegetable oil/water, engine oil/water and the like, and the hydrophobic cotton fabric has excellent hydrophobic effect by reflecting from the side.
In addition, the invention also provides the hydrophobic cotton which is obtained by the preparation method described in each embodiment and has the beneficial effects of each hydrophobic cotton in each embodiment.
The foregoing is an exemplary embodiment of the present disclosure, but it should be noted that various changes and modifications could be made herein without departing from the scope of the present disclosure as defined by the appended claims. The functions, steps and/or actions of the method claims in accordance with the disclosed embodiments described herein need not be performed in any particular order. Furthermore, although elements of the disclosed embodiments of the invention may be described or claimed in the singular, the plural is contemplated unless limitation to the singular is explicitly stated.
The numbers of the embodiments disclosed in the embodiments of the present invention are merely for description, and do not represent the merits of the embodiments.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, of embodiments of the invention is limited to these examples; within the idea of an embodiment of the invention, also technical features in the above embodiment or in different embodiments may be combined and there are many other variations of the different aspects of the embodiments of the invention as described above, which are not provided in detail for the sake of brevity. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of the embodiments of the present invention are intended to be included within the scope of the embodiments of the present invention.
Claims (10)
1. A method for preparing a hydrophobic cotton fabric, comprising:
sequentially immersing a cotton fabric in a copper ion salt solution and a gallic acid solution to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric;
hydrophobic properties are obtained by reacting the GA-Cu (ii) complex modification layer with an amine, sulfur or alcohol containing molecule under basic conditions by michael addition or schiff base reaction to produce long chain hydrocarbon species.
2. The method for preparing a hydrophobic cotton fabric according to claim 1, wherein the copper ion salt solution comprises: copper sulfate solution or copper chloride solution.
3. The method for preparing a hydrophobic cotton fabric according to claim 2, further comprising:
immersing the cotton fabric in copper sulfate solution with the concentration of 2.5mg/ml-15mg/ml, and preserving the temperature for 30min at 70-100 ℃.
4. The method for preparing a hydrophobic cotton fabric according to claim 2, further comprising:
immersing the cotton fabric in copper sulfate solution with the concentration of 10mg/ml, and keeping the temperature at 80 ℃ for 30 min.
5. The method for preparing a hydrophobic cotton fabric according to claim 3 or 4, further comprising:
immersing the cotton fabric taken out of the copper sulfate solution in a gallic acid solution with the concentration of 2mg/ml-14mg/ml so as to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric.
6. The method for preparing a hydrophobic cotton fabric according to claim 3 or 4, further comprising:
immersing the cotton fabric taken out of the copper sulfate solution in a gallic acid solution with the concentration of 12.8mg/ml so as to form a GA-Cu (II) complex modified layer on the surface of the cotton fabric.
7. The method for preparing a hydrophobic cotton fabric according to claim 6, further comprising:
immersing the cotton fabric with the GA-Cu (II) complex modified layer in an octadecyl amine ethanol aqueous solution with the concentration of 2mg/ml-10mg/ml, and preserving the temperature for 1h-8h at room temperature, so that the GA-Cu (II) complex modified layer of the cotton fabric reacts with molecules containing amine and alcohol to generate long-chain hydrocarbon substances to obtain the hydrophobic property.
8. The method for preparing a hydrophobic cotton fabric according to claim 6, further comprising:
immersing the cotton fabric with the GA-Cu (II) complex modified layer in an octadecyl amine ethanol water solution with the concentration of 8mg/ml, and preserving the temperature for 4h at room temperature, so that the GA-Cu (II) complex modified layer of the cotton fabric reacts with molecules containing amine and alcohol to generate long-chain hydrocarbon substances to obtain the hydrophobic property.
9. The method for preparing a hydrophobic cotton fabric according to claim 7 or 8, further comprising:
before immersing the cotton fabric with the GA-Cu (II) complex modified layer into an octadecyl amine ethanol water solution, washing and drying the cotton fabric with the GA-Cu (II) complex modified layer by using deionized water.
10. A hydrophobic cotton fabric prepared by the method of preparing a hydrophobic cotton fabric according to any one of claims 1 to 9.
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Application publication date: 20210126 |