CN107266718B - Hydrophobic natural high polymer material and preparation method thereof - Google Patents
Hydrophobic natural high polymer material and preparation method thereof Download PDFInfo
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- CN107266718B CN107266718B CN201610210003.7A CN201610210003A CN107266718B CN 107266718 B CN107266718 B CN 107266718B CN 201610210003 A CN201610210003 A CN 201610210003A CN 107266718 B CN107266718 B CN 107266718B
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- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a hydrophobic natural polymer material, which is characterized in that: the micro-morphology of the hydrophobic natural polymer material is sheet-shaped, and the adjustable range of the transverse size of the particle size is 0.1-20 microns. The raw materials of the hydrophobic natural polymer material comprise a natural polymer material and a hydrophobic polymer material, wherein the hydrophobic polymer material is starch, chitosan, chitin or alginic acid; the hydrophobic natural polymer material has good hydrophobicity, and the water contact angle can reach 120 degrees. Meanwhile, the invention also provides a preparation method for preparing the hydrophobic natural polymer material, and the hydrophobic modification method is a one-pot method, is green and solvent-free and has high efficiency.
Description
Technical Field
The invention relates to the technical field of hydrophobic polymer materials. More particularly, relates to a hydrophobic polymer material containing starch, chitosan, chitin or alginic acid, and a preparation method and application thereof.
Background
With the development of society and economy, petroleum and natural gas and the like are continuously consumed, and meanwhile, a large amount of white pollution is caused, and the natural environment on which people rely to live is seriously threatened. Natural high molecular compounds such as starch, chitosan and the like are not only rich in raw material sources but also biodegradable, so that development and application thereof are receiving increasing attention from researchers. Natural high molecular compounds are widely used in the fields of food, daily chemicals, paper making, textiles, medicine, and the like. However, the material has more active hydroxyl groups, so that the expected effect cannot be achieved in the application process, for example, the field of daily skin care products requires that the material has smooth powder characteristics, an excellent oil-in-water emulsion stabilizing system and a stable particle emulsion system. In order to meet these various requirements, it is necessary to subject the material to a certain modification treatment. For example, the Chinese patent with the publication number of CN 105017436A provides hydrophobic fluidity starch prepared by the cross-linking of oxidation esterification metal and a preparation method thereof. The Chinese patent with publication number CN 103382226A obtains starch micro-nano particles by acid degradation of native starch, and then uses Octyl Succinic Anhydride (OSA) to perform hydrophobic modification on the starch micro-nano particles to obtain the octyl succinic anhydride modified starch micro-nano particles. Chinese patent publications CN103613781A and CN103601907A disclose that super-hydrophobic taro leaf particles and polymethylhydroxysiloxane particles are assembled on the surface of chitosan sponge to obtain the super-hydrophobic chitosan composite sponge. These methods mostly use a large amount of organic solvents, and the process is complicated.
Therefore, it is necessary to provide a hydrophobic starch, chitosan, chitin or alginic acid material with good stability and hydrophobicity, and a green and efficient method for preparing these natural polymer materials.
Disclosure of Invention
The first purpose of the present invention is to provide a hydrophobic natural polymer material, which is a flake powder material, and has the advantages of adjustable size, good hydrophobicity and good stability.
The second purpose of the invention is to provide a preparation method of the hydrophobic natural polymer material, which has the advantages of simple process, low cost and environmental protection.
In order to achieve the first purpose, the invention adopts the following technical scheme:
a hydrophobic natural polymer material, wherein the water contact angle of the hydrophobic natural polymer material is 98-120 degrees; the raw materials of the hydrophobic natural polymer material consist of a natural polymer material and a hydrophobic polymer material; the natural polymer material is selected from starch, chitosan, chitin or alginic acid.
Further, the starch may be selected from corn starch, tapioca starch, potato starch or waxy corn starch.
Further, the hydrophobic polymer material can be selected from one or two of fluorine-containing polymer and polyamide;
preferably, the fluorine-containing polymer is selected from one or more of polytetrafluoroethylene, polyvinylidene fluoride, fluorinated ethylene propylene copolymer, ethylene chlorotrifluoroethylene or fluorinated alkyl silane;
preferably, the polyamide is selected from one or both of nylon 66 or nylon 1010.
Further, the particle size of the natural polymer material is 1-50 microns.
Furthermore, the micro-morphology of the hydrophobic natural polymer material is flaky, and the adjustable range of the transverse size of the particle size is 0.1-20 microns.
In order to achieve the second purpose, the invention adopts the following technical scheme:
a preparation method of a hydrophobic natural polymer material comprises the following steps:
mixing and grinding a natural polymer material and a hydrophobic polymer material; grinding to coat hydrophobic material on the surface of natural polymer material; and (4) separating and removing redundant hydrophobic substances to obtain the hydrophobic natural polymer material.
Preferably, the grinding is carried out in a ball mill or a grinding instrument, the grinding speed is 250-540rpm, and the grinding time is 2-30 h;
more preferably, the polishing speed is 450-540 rpm.
More preferably, the milling time is 10-30 h.
Preferably, the ball mill or mill is selected from a planetary ball mill, a vibratory ball mill or a mortar mill.
The invention has the following beneficial effects:
the invention prepares the hydrophobic natural polymer material powder with good hydrophobic property by mechanically compounding starch, chitosan, chitin or alginic acid and the hydrophobic material through a simple one-pot method without any solvent and through a simple and efficient process.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows the dispersion profile in water before and after hydrophobic modification of corn starch of example 1.
Figure 2 shows a water contact angle graph of the hydrophobic corn starch of example 1.
Figure 3 shows an SEM image of the hydrophobic corn starch of example 1.
Figure 4 shows a water contact angle graph of the hydrophobic chitosan of example 6.
Fig. 5 shows an SEM image of the hydrophobic chitosan of example 6.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. Similar parts in the figures are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
Vacuum drying corn starch at 105 deg.C for 4h, mechanically combining dried corn starch 30g with PTFE for 28h, and grinding with zirconia balls of diameter 20mm, 10mm, 6mm and mass 540g at 400 r/min. And separating the starch powder after compounding from the redundant PTFE by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet-like microstructure, a size of 0.1-4 μm, and a contact angle with water of 120 deg. FIG. 1 is a graph showing the dispersion in water of the starch of example 1 before and after hydrophobic modification, and it can be seen that the starch before hydrophobic modification settles in water without water repellency; the hydrophobically modified starch is strongly water repellent. FIG. 2 is a photograph of the contact angle of the hydrophobically modified starch of example 1, wherein the water contact angle of the hydrophobically modified starch is 120 °. FIG. 3 is an SEM image of the hydrophobic starch of example 1, showing that the modified starch is in the form of flakes having a particle size of 0.1-4 microns across.
Example 2
Vacuum drying corn starch at 105 deg.C for 4h, mechanically combining dried corn starch 30g with PTFE for 4h, and grinding with zirconia balls of diameter 20mm, 10mm, 6mm and mass 540g at 400 r/min. And separating the starch powder after compounding from the redundant PTFE by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet-like microstructure, a transverse dimension of 0.5-10 μm, and a water contact angle of 113 deg.
Example 3
Vacuum drying corn starch at 105 deg.C for 4h, mechanically combining dried corn starch 30g with PTFE for 10h, and grinding with zirconia balls of diameter 20mm, 10mm, 6mm and mass 540g at 400 r/min. And separating the starch powder after compounding from the redundant PTFE by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet-like microstructure, a transverse dimension of 0.5-5 μm, and a contact angle with water of 116 °.
Example 4
Vacuum drying corn starch at 105 deg.C for 4h, mechanically compounding 30g dried corn starch with PTFE for 16h, and grinding at 400r/min with grinding ball diameter of 20mm, 10mm, and 6mm and mass of 540 g. And separating the starch powder after compounding from the redundant PTFE by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet-like microstructure, a transverse dimension of 0.3-5 μm, and a contact angle with water of 115 deg.
Example 5
Vacuum drying corn starch at 105 deg.C for 4h, mechanically combining dried corn starch 30g with PTFE for 22h, and grinding at 400r/min with grinding ball diameter of 20mm, 10mm, and 6mm and mass of 540 g. And separating the starch powder after compounding from the redundant PTFE by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet-like microstructure, a transverse dimension of 0.1-4 μm, and a contact angle with water of 118 deg.
Example 6
The chitosan was dried under vacuum at 105 ℃ for 4 h. 30g of the obtained dried chitosan was taken to obtain hydrophobic chitosan powder according to the method of example 1.
The obtained hydrophobic chitosan powder has a sheet-shaped microstructure, the size of 1-10 microns and a water contact angle of 117 degrees. FIG. 4 is a photograph showing the water contact angle of the hydrophobically modified chitosan of example 6, which is as high as 117 ℃. FIG. 5 is an SEM image of the hydrophobic chitosan of example 6, and it can be seen that the modified chitosan is in the form of a flake with a particle size of 1-10 microns across.
Example 7
Alginic acid was dried under vacuum at 105 ℃ for 4 h. 30g of the obtained dry alginic acid was taken to obtain hydrophobic alginic acid powder according to the method of example 1.
The microstructure of the obtained hydrophobic alginic acid is sheet-shaped, the transverse dimension is 2-5 microns, and the water contact angle is 103 degrees.
Example 8
Vacuum drying corn starch at 105 deg.C for 4h, mechanically combining dried corn starch 30g with PVDF for 10h, and grinding at 400r/min with grinding ball diameter of 20mm, 10mm, and 6mm and mass of 540 g. And separating the starch powder after compounding from the redundant PVDF by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet microstructure, a transverse dimension of 0.1-8 μm, and a water contact angle of 100 deg.
Example 9
Vacuum drying corn starch at 105 deg.C for 4h, mechanically compounding 30g dried corn starch with PVDF-HFP for 10h, and grinding at 400r/min with zirconia balls of diameter 20mm, 10mm, 6mm and mass 540 g. And separating the compounded starch powder from the redundant PVDF-HFP by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet-like microstructure, a transverse dimension of 0.1-5 μm, and a water contact angle of 105 °.
Example 10
Vacuum drying corn starch at 105 deg.C for 4h, mechanically compounding 30g dried corn starch with nylon 1010 for 10h, and grinding at 400r/min with grinding ball diameter of 20mm, 10mm, 6mm and mass of 540 g. And separating the starch powder after compounding from the redundant nylon by using a stainless steel sieve to obtain the hydrophobic starch.
The obtained hydrophobic starch has a sheet microstructure, a transverse dimension of 1-10 μm, and a water contact angle of 98 deg.
Example 11
The chitin is dried in vacuum for 2h at 105 ℃. 30g of the obtained dried chitin was taken and the hydrophobic chitin powder was obtained according to the method of example 1.
The obtained hydrophobic chitin powder has a sheet microstructure, a transverse dimension of 0.1-3 μm, and a water contact angle of 112 °.
Example 12
Drying the cassava starch in vacuum at 105 ℃ for 4 h. 30g of the obtained tapioca starch was taken to obtain hydrophobic tapioca starch powder according to the method of example 1.
The obtained hydrophobic tapioca starch powder has a sheet-shaped microstructure, a transverse dimension of 0.1-5 μm, and a water contact angle of 114 deg.
Example 13
The corn starch was dried in vacuo at 105 ℃ for 4 h. Taking 30g of the obtained corn starch, mechanically compounding the corn starch with PTFE for 30h, wherein the grinding balls are zirconia balls with the diameters of 20mm, 10mm and 6mm and the mass of 540g, and the grinding speed is 250 r/min. Hydrophobic corn starch powder was obtained according to the method of example 1.
The obtained hydrophobic corn starch powder has a sheet-like microstructure, a transverse dimension of 0.1-6 μm, and a water contact angle of 111 °.
Example 14
The corn starch was dried in vacuo at 105 ℃ for 4 h. Taking 30g of the obtained corn starch, mechanically compounding the corn starch with PTFE for 10h, wherein grinding balls are zirconia balls with the diameter of 20mm, the mass of 10mm and the mass of 6mm of 540g, and the grinding speed is 540 r/min. Hydrophobic corn starch powder was obtained according to the method of example 1.
The obtained hydrophobic corn starch powder has a sheet-like microstructure, a transverse dimension of 0.1-3 μm, and a water contact angle of 118 °.
Example 15
Drying the cassava starch in vacuum at 105 ℃ for 4 h. Taking 30g of the obtained cassava starch, mechanically compounding the cassava starch with PTFE for 10 hours, wherein grinding balls are zirconia balls with the diameter of 20mm, the mass of 10mm and the mass of 6mm of 540g, and the grinding speed is 450 r/min. Hydrophobic tapioca powder was obtained according to the method of example 1.
The obtained hydrophobic tapioca starch powder has a sheet-shaped microstructure, a transverse dimension of 0.1-4 μm, and a water contact angle of 119 °.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (9)
1. A preparation method of a hydrophobic natural polymer material is characterized by comprising the following steps:
mixing and grinding a natural polymer material and a hydrophobic polymer material; grinding to coat hydrophobic material on the surface of natural polymer material; separating and removing redundant hydrophobic substances to obtain a hydrophobic natural polymer material;
wherein the water contact angle of the hydrophobic natural polymer material is 98-120 degrees;
the natural polymer material is selected from starch, chitosan, chitin or alginic acid;
the hydrophobic high molecular material is selected from fluorine-containing polymers;
the fluorine-containing polymer is selected from one or more of polytetrafluoroethylene, polyvinylidene fluoride and fluorinated ethylene propylene copolymer.
2. The method for preparing a hydrophobic natural polymer material according to claim 1, wherein the starch is selected from corn starch, tapioca starch, and potato starch.
3. The method of claim 2, wherein the corn starch is selected from waxy corn starch.
4. The method for preparing the hydrophobic natural polymer material according to claim 1, wherein the particle size of the natural polymer material is 1 to 50 μm.
5. The method according to claim 1, wherein the hydrophobic natural polymer material has a lamellar microstructure and a particle size of 0.1-20 μm.
6. The method for preparing hydrophobic natural polymer material as claimed in claim 1, wherein the grinding is performed in a ball mill or a grinding apparatus, the grinding speed is 250-540rpm, and the grinding time is 2-30 h.
7. The method as claimed in claim 6, wherein the polishing speed is 450-540 rpm.
8. The method for preparing the hydrophobic natural polymer material according to claim 6, wherein the grinding time is 10-30 h.
9. The method for preparing a hydrophobic natural polymer material according to claim 6, wherein the ball mill or the grinder is selected from a planetary ball mill, a vibration ball mill or a mortar grinder.
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