CN113830879B - Modified rope-shaped artificial aquatic weed coated on chitosan surface and preparation method thereof - Google Patents
Modified rope-shaped artificial aquatic weed coated on chitosan surface and preparation method thereof Download PDFInfo
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 67
- 241000196324 Embryophyta Species 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000835 fiber Substances 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- -1 2, 3-epoxypropyl trimethyl isopropanol chloride Chemical compound 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000004448 titration Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 abstract description 13
- 238000012986 modification Methods 0.000 abstract description 13
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 244000005700 microbiome Species 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- 239000012209 synthetic fiber Substances 0.000 abstract description 4
- 229920002994 synthetic fiber Polymers 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000000813 microbial effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920006317 cationic polymer Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- MSWZFWKMSRAUBD-IVMDWMLBSA-N glucosamine group Chemical group OC1[C@H](N)[C@@H](O)[C@H](O)[C@H](O1)CO MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2203/00—Apparatus and plants for the biological treatment of water, waste water or sewage
- C02F2203/006—Apparatus and plants for the biological treatment of water, waste water or sewage details of construction, e.g. specially adapted seals, modules, connections
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Microbiology (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Catching Or Destruction (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a method for coating modified rope-shaped artificial aquatic weed on the surface of chitosan, which comprises the following steps: preparing modified chitosan; immersing rope-shaped artificial aquatic weed in the modified chitosan solution to obtain the modified rope-shaped artificial aquatic weed. A chitosan surface coated modified rope-shaped artificial aquatic weed is prepared by the method. The effect is as follows: the hydrophilicity of the modified rope-shaped artificial aquatic plants is improved, the starting film forming time is shortened, the microorganism film forming efficiency is improved, the pollutant reduction efficiency is improved, and in addition, the modified rope-shaped artificial aquatic plants can be widely applied to the modification of synthetic fibers due to the characteristics of energy conservation, high efficiency, easiness in coating and good effect.
Description
Technical Field
The invention relates to the field of artificial aquatic weeds, in particular to a chitosan surface-coated modified rope-shaped artificial aquatic weed and a preparation method thereof.
Background
Chitosan is the only known natural alkaline cationic polymer, has the characteristics of excellent biological functionality, biocompatibility, innocuity, antibacterial property, biodegradability and the like, and is widely applied to the fields of medicine, environmental protection, textile, food, cosmetic industry and the like. The chitosan has a complex double-helix structure, and groups such as primary hydroxyl, secondary hydroxyl, amino and the like on a glucosamine unit in a molecular chain have stronger reactivity, so that the chitosan can be endowed with various functional characteristics while the dissolubility of the chitosan is improved by a functional modification or modification method, and novel chitosan derivatives with excellent performances are prepared and developed. In order to meet the functional requirements of more application fields, the modification of chitosan has become one of the most active research fields.
At present, the rope-shaped artificial aquatic weed used in the biomembrane method mainly comprises synthetic fibers such as terylene and polypropylene, and the general synthetic fibers have poor hydrophilic and biocompatible properties, so that the rope-shaped artificial aquatic weed has defects in the aspects of film forming speed, biological quality, connection tightness of the biomembrane and a carrier and the like. The reference data shows that the bioaffinity modification can better improve the bioaffinity and the hydrophilia of the fiber, increase the film forming starting speed of microorganisms on the fiber, promote the metabolism of the microorganisms, and greatly improve the reduction rate of pollutants. Proper bioaffinity modification is carried out on the rope-shaped artificial aquatic weed, so that the film-forming speed, the film-forming quantity and the abundance and stability of microbial colonies can be effectively improved.
The rope-shaped artificial aquatic weed surface modification can be divided into physical modification and chemical modification, the active groups are firmly fixed on the surface of the carrier by the chemical modification in a chemical reaction mode, and the effect is obvious, but the rope-shaped artificial aquatic weed surface modification is only suitable for theoretical research due to high energy consumption and complex process, and industrial continuous treatment is difficult to realize.
Disclosure of Invention
The invention aims to provide a chitosan surface coating modified rope-shaped artificial aquatic weed and a preparation method thereof, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a preparation method of chitosan surface coated modified rope-shaped artificial aquatic weed comprises the following steps:
s100, preparing modified chitosan;
s200, dipping the rope-shaped artificial aquatic weed into the modified chitosan solution to obtain the modified rope-shaped artificial aquatic weed with the chitosan surface coated.
On the basis of the technical scheme, the invention can be improved as follows.
Further, S100 is specifically:
s110, mixing chitosan, acetic acid and NaOH solution to obtain white precipitate;
s120, mixing the white precipitate and isopropanol at a preset temperature, and then dropwise adding 2, 3-epoxypropyl trimethyl isopropyl chloride;
and S130, adding absolute ethyl alcohol for precipitation after the reaction is finished, and sequentially carrying out suction filtration, washing and vacuum drying to obtain the modified chitosan.
Further, S110 is specifically:
chitosan is dissolved in 0.1% -50% acetic acid solution, and 0.1 mol/L-3 mol/L NaOH solution is added dropwise after dissolution until the pH is 9, so that white precipitate is obtained.
Further, S120 is specifically:
mixing the white precipitate and isopropanol, stirring and heating to 40-120 ℃, and dripping 0.1-50 mg/mL of 2, 3-epoxypropyl trimethyl isopropanol chloride solution every 0.1-5 h, wherein the titration time is 1 min-5 h.
Further, S130 is specifically:
and after the reaction is finished, adding absolute ethyl alcohol for precipitation, filtering, washing with absolute ethyl alcohol, and drying in vacuum at 25-150 ℃ for 2-72 h to obtain the modified chitosan.
Further, S200 is specifically:
preparing 0.01-10wt% of modified chitosan, placing 10 min-72 h after dissolution, then soaking rope-shaped artificial aquatic weed in the modified chitosan for 0.5-72 h, taking out the modified chitosan for dehydration, and then placing the modified chitosan in a vacuum drying environment at 25-150 ℃ for drying, thus obtaining the modified rope-shaped artificial aquatic weed coated on the surface of the chitosan.
Further, the contact angle of the modified rope-shaped artificial aquatic weed is 5-90 degrees.
Further, the surface particle number of the modified rope-shaped artificial aquatic weed fiber is 1-1000 pieces/cm 2 The area percentage of the fiber surface particles is 0.1% -100%.
A chitosan surface coated modified rope-shaped artificial aquatic weed is prepared by the preparation method.
The beneficial effects of the invention are as follows: the hydrophilicity of the modified rope-shaped artificial aquatic plants is improved, the starting film forming time is shortened, the microorganism film forming efficiency is improved, the pollutant reduction efficiency is improved, and in addition, the modified rope-shaped artificial aquatic plants can be widely applied to the modification of synthetic fibers due to the characteristics of energy conservation, high efficiency, easiness in coating and good effect.
Drawings
FIG. 1 is an infrared spectrum analysis chart of each treatment group of rope-shaped artificial aquatic weeds in application examples;
FIG. 2 is an SEM image of the fibers of each rope-shaped artificial aquatic weed treatment group according to the application example;
FIG. 3 is a diagram showing the condition of rope-shaped artificial aquatic weed film formation before and after chitosan modification on day 10 of application example test.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
A preparation method of chitosan surface coated modified rope-shaped artificial aquatic weed comprises the following steps:
s100, preparing modified chitosan;
s200, dipping the rope-shaped artificial aquatic weed into the modified chitosan solution to obtain the modified rope-shaped artificial aquatic weed with the chitosan surface coated.
Example 2
This example is a further optimization performed on the basis of example 1, which is specifically as follows:
s100 is specifically as follows:
s110, mixing chitosan, acetic acid and NaOH solution to obtain white precipitate;
s120, mixing the white precipitate and isopropanol at a preset temperature, and then dropwise adding 2, 3-epoxypropyl trimethyl isopropyl chloride;
and S130, adding absolute ethyl alcohol for precipitation after the reaction is finished, and sequentially carrying out suction filtration, washing and vacuum drying to obtain the modified chitosan.
Example 3
This example is a further optimization performed on the basis of example 2, which is specifically as follows:
s110 is specifically:
chitosan is dissolved in 0.1% -50% acetic acid solution, and 0.1 mol/L-3 mol/L NaOH solution is added dropwise after dissolution until the pH is 9, so that white precipitate is obtained.
Example 4
This example is a further optimization performed on the basis of example 3, which is specifically as follows:
s120 specifically comprises the following steps:
mixing the white precipitate and isopropanol, stirring and heating to 40-120 ℃, and dripping 0.1-50 mg/mL of 2, 3-epoxypropyl trimethyl isopropanol chloride solution every 0.1-5 h, wherein the titration time is 1 min-5 h.
Example 5
This example is a further optimization performed on the basis of example 4, which is specifically as follows:
s130 specifically comprises the following steps:
and after the reaction is finished, adding absolute ethyl alcohol for precipitation, filtering, washing with absolute ethyl alcohol, and drying in vacuum at 25-150 ℃ for 2-72 h to obtain the modified chitosan.
Example 6
This example is a further optimization performed on the basis of any one of examples 1 to 5, which is specifically as follows:
s200 specifically comprises the following steps:
preparing 0.01-10wt% of modified chitosan, placing 10 min-72 h after dissolution, then soaking rope-shaped artificial aquatic weed in the modified chitosan for 0.5-72 h, taking out the modified chitosan for dehydration, and then placing the modified chitosan in a vacuum drying environment at 25-150 ℃ for drying, thus obtaining the modified rope-shaped artificial aquatic weed coated on the surface of the chitosan.
Example 7
As shown in fig. 1, this embodiment is a further optimization performed on the basis of any one of embodiments 1 to 6, and is specifically as follows:
the contact angle of the obtained modified rope-shaped artificial aquatic weed is 5-90 degrees, and in addition, the number of particles on the surface of the modified rope-shaped artificial aquatic weed fiber is 1-1000 particles/cm 2 The area percentage of the fiber surface particles is 0.1% -100%.
Example 8
A chitosan surface coated modified rope-shaped artificial aquatic weed is prepared by the preparation method.
Application example:
dissolving chitosan in 2% acetic acid solution, and dropwise adding 1mol/L NaOH solution to pH 9 after dissolving to obtain white precipitate;
mixing the white precipitate and isopropanol, stirring and heating to 80 ℃, and dripping 0.5mg/mL of 2, 3-epoxypropyl trimethyl isopropanol chloride solution every 2 hours, wherein the titration time is 0.5 hour;
after the reaction is finished, adding absolute ethyl alcohol for precipitation, washing with absolute ethyl alcohol after suction filtration, and vacuum drying at 65 ℃ for 24 hours to obtain modified chitosan;
preparing 2wt% of modified chitosan, dissolving, standing for 12 hours, soaking rope-shaped artificial aquatic weed in the solution for finishing for 24 hours, taking out the solution for dehydration, and then drying the solution in a vacuum drying environment at 50 ℃ to obtain the modified rope-shaped artificial aquatic weed with the surface coated with the chitosan.
According to the invention, chitosan is modified so that the chitosan can be well dissolved in water to be attached to rope-shaped artificial aquatic weeds, so that the biological affinity of the artificial aquatic weeds is improved, and common chitosan can not be basically dissolved in water, so that the artificial aquatic weeds can not obtain good biological affinity.
The test shows that the contact angle of the obtained modified rope-shaped artificial aquatic weed is 25.7 degrees, and in the normal case, the contact angle of the unmodified rope-shaped artificial aquatic weed is 52.3 degrees, and in general, the smaller the contact angle is, the better the hydrophilicity is, so that the hydrophilicity of the modified rope-shaped artificial aquatic weed of the chitosan is obviously improved from the angle of contact angle change; as shown in FIG. 1, from the infrared spectrum analysis chart, it can be seen that the rope-shaped artificial aquatic weed is 3500cm in length before and after modification -1 The positions of the chitosan modified rope-shaped artificial aquatic weed are provided with telescopic vibration peaks of hydroxyl groups, and the relative sizes of the peaks can show that the hydrophilicity of the chitosan modified rope-shaped artificial aquatic weed is obviously improved compared with that of the non-modified rope-shaped artificial aquatic weed.
The surface particle number of the modified rope-shaped artificial aquatic weed fiber is 94.37/cm 2 The area percentage of the particles on the surface of the fiber is 9.049 percent, and the number of the particles on the surface of the unmodified rope-shaped artificial aquatic weed fiber is 38 per cm in general cases 2 The area percentage of the particles on the surface of the fiber is 0.98%; it can be seen that the two indexes for measuring the roughness show that the rope-shaped artificial aquatic weed roughness is obviously increased after the chitosan is modified, as shown in fig. 2, the surface roughness condition of the fiber before and after the chitosan is modified is obviously shown in an SEM image, the surface roughness of the fiber is obviously rough compared with that of the fiber which is not modified, and in general, the larger the roughness is, the larger the specific surface area is, so that the growth and the attachment of microorganisms are facilitated.
In addition, the obtained chitosan surface coating modified rope-shaped artificial aquatic weed has good film forming speed:
the film-forming condition of the rope-shaped artificial aquatic weed is observed, the film-forming time of the modified rope-shaped artificial aquatic weed coated on the surface of the chitosan is 4 days, the film-forming time of the rope-shaped artificial aquatic weed which is not modified is 9 days, the film-forming time of the modified rope-shaped artificial aquatic weed coated on the surface of the chitosan is obviously shortened, the film-forming condition of the rope-shaped artificial aquatic weed coated on the surface of the chitosan is shown in fig. 3, and the yellow brown plaque is the microbial flora which is already hung, and the microbial flora amount after the modification treatment of the chitosan is obviously larger than that of the rope-shaped artificial aquatic weed which is not modified.
Pollutant reduction effect: the reduction rates of the modified rope-shaped artificial aquatic weed coated on the surface of the chitosan on COD, total nitrogen and total phosphorus are 95.39%, 61.63% and 92.68 respectively, and are improved by 10.30%, 20.37% and 13.94% respectively compared with the unmodified treatment group.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (2)
1. The preparation method of the chitosan surface coated modified rope-shaped artificial aquatic weed is characterized by comprising the following steps of:
s100, dissolving chitosan in 2% acetic acid solution, and dropwise adding 1mol/L NaOH solution to the pH value of 9 after dissolving to obtain a white precipitate;
mixing the white precipitate and isopropanol, stirring and heating to 80 ℃, and dripping 0.5mg/mL of 2, 3-epoxypropyl trimethyl isopropanol chloride solution every 2 hours, wherein the titration time is 0.5 hour;
after the reaction is finished, adding absolute ethyl alcohol for precipitation, washing with absolute ethyl alcohol after suction filtration, and vacuum drying at 65 ℃ for 24 hours to obtain modified chitosan;
s200, preparing 2wt% of modified chitosan, dissolving, standing for 12 hours, soaking rope-shaped artificial aquatic weed in the solution for 24 hours, taking out the solution for dehydration, and then drying the solution in a vacuum drying environment at 50 ℃ to obtain the modified rope-shaped artificial aquatic weed with the surface coated with the modified chitosan, wherein the contact angle of the modified rope-shaped artificial aquatic weed is 25.7 DEG, and the modified rope-shaped artificial aquatic weed is preparedThe surface particle number of the aquatic weed fiber is 94.37/cm 2 The area percentage of the fiber surface particles was 9.049%.
2. A chitosan surface coated modified rope-like artificial aquatic weed prepared by the preparation method of claim 1.
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| CN202111026508.5A CN113830879B (en) | 2021-09-02 | 2021-09-02 | Modified rope-shaped artificial aquatic weed coated on chitosan surface and preparation method thereof |
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|---|---|---|---|---|
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| WO2008087845A1 (en) * | 2007-01-16 | 2008-07-24 | Dainichiseika Color & Chemicals Mfg. Co., Ltd. | Aqueous solution composition |
| KR20140090793A (en) * | 2013-01-10 | 2014-07-18 | 가톨릭대학교 산학협력단 | Method of hydrophilic modification the surface of polyethylene plastic stent |
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| CN108330686A (en) * | 2018-01-02 | 2018-07-27 | 江苏大学 | The preparation method of the chitin modified basalt fibre carrier of hydrophily |
| CN108529766A (en) * | 2018-03-30 | 2018-09-14 | 河南金盾环保设备安装工程有限公司 | A kind of coating sewage-treating agent and preparation method thereof |
| CN110862155A (en) * | 2019-12-26 | 2020-03-06 | 南京公诚节能新材料研究院有限公司 | Artificial aquatic weed for water ecological restoration |
-
2021
- 2021-09-02 CN CN202111026508.5A patent/CN113830879B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2005329351A1 (en) * | 2005-03-17 | 2006-09-21 | Lantor (Uk) Limited | The preparing method and the use of antiseptic medical dressing. |
| WO2008087845A1 (en) * | 2007-01-16 | 2008-07-24 | Dainichiseika Color & Chemicals Mfg. Co., Ltd. | Aqueous solution composition |
| KR20140090793A (en) * | 2013-01-10 | 2014-07-18 | 가톨릭대학교 산학협력단 | Method of hydrophilic modification the surface of polyethylene plastic stent |
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