CN117487350B - Polydopamine chelated polymer membrane liquid and preparation method and application thereof - Google Patents
Polydopamine chelated polymer membrane liquid and preparation method and application thereof Download PDFInfo
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- CN117487350B CN117487350B CN202311428636.1A CN202311428636A CN117487350B CN 117487350 B CN117487350 B CN 117487350B CN 202311428636 A CN202311428636 A CN 202311428636A CN 117487350 B CN117487350 B CN 117487350B
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- 229920001690 polydopamine Polymers 0.000 title claims abstract description 130
- 229920005597 polymer membrane Polymers 0.000 title claims abstract description 97
- 239000007788 liquid Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 79
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 26
- 229920001661 Chitosan Polymers 0.000 claims abstract description 22
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229960000583 acetic acid Drugs 0.000 claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 19
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 19
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- 238000009333 weeding Methods 0.000 claims abstract description 16
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 15
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- 239000002994 raw material Substances 0.000 claims abstract description 13
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- 235000011187 glycerol Nutrition 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
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- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 14
- 239000013522 chelant Substances 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003306 harvesting Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
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- 235000001602 Digitaria X umfolozi Nutrition 0.000 claims description 2
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- 235000006830 Digitaria didactyla Nutrition 0.000 claims description 2
- 235000005804 Digitaria eriantha ssp. eriantha Nutrition 0.000 claims description 2
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- 241001191006 Phlomoides rotata Species 0.000 claims 1
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- 230000012010 growth Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 230000007226 seed germination Effects 0.000 abstract description 2
- 102100029469 WD repeat and HMG-box DNA-binding protein 1 Human genes 0.000 abstract 1
- 101710097421 WD repeat and HMG-box DNA-binding protein 1 Proteins 0.000 abstract 1
- 230000035784 germination Effects 0.000 description 32
- 239000012528 membrane Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 10
- 241000196324 Embryophyta Species 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
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- 210000003763 chloroplast Anatomy 0.000 description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 4
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- 239000000575 pesticide Substances 0.000 description 3
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- XMTQQYYKAHVGBJ-UHFFFAOYSA-N 3-(3,4-DICHLOROPHENYL)-1,1-DIMETHYLUREA Chemical compound CN(C)C(=O)NC1=CC=C(Cl)C(Cl)=C1 XMTQQYYKAHVGBJ-UHFFFAOYSA-N 0.000 description 2
- 240000006497 Dianthus caryophyllus Species 0.000 description 2
- 235000009355 Dianthus caryophyllus Nutrition 0.000 description 2
- 239000005510 Diuron Substances 0.000 description 2
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- MXWJVTOOROXGIU-UHFFFAOYSA-N atrazine Chemical compound CCNC1=NC(Cl)=NC(NC(C)C)=N1 MXWJVTOOROXGIU-UHFFFAOYSA-N 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
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- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 2
- 229940097068 glyphosate Drugs 0.000 description 2
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- 102000004169 proteins and genes Human genes 0.000 description 2
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- 230000027756 respiratory electron transport chain Effects 0.000 description 2
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- 244000025254 Cannabis sativa Species 0.000 description 1
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- 231100000277 DNA damage Toxicity 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 241000238814 Orthoptera Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
- A01G2013/004—Liquid mulch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
- C08J2439/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
- C08J2439/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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Abstract
The invention relates to the technical field of herbicides, and discloses polydopamine chelating polymer membrane liquid, and a preparation method and application thereof, wherein the polydopamine chelating polymer membrane liquid comprises the following raw materials: 3.6 to 10.8g of dopamine hydrochloride, 120 to 200mL of distilled water, 120 to 200mL of absolute ethyl alcohol, 3.6 to 10.8mL of ammonia water solution, 1 to 5g of chitosan, 90 to 100mL of 1% glacial acetic acid solution, 902 to 4g of polyvinylpyrrolidone K and1 to 2mL of 1% glycerol. The preparation method comprises the following steps: and (3) preparing polydopamine, and preparing mixed liquid and polydopamine chelating polymer membrane liquid. The polydopamine chelating polymer membrane liquid is used for weeding. The polydopamine chelating polymer membrane liquid prepared by the invention can obviously inhibit seed germination and seedling growth in soil after being sprayed, achieves the weeding effect of chemical herbicide, does not damage the environment required by plant growth, generates less secondary pollution, has good treatment effect, can be treated in situ, is simple to operate, and has small influence on the environment.
Description
Technical Field
The invention belongs to the technical field of herbicides, and particularly relates to polydopamine chelating polymer membrane liquid, and a preparation method and application thereof.
Background
The commercial popularization of herbicide-resistant transgenic soybean, corn and other crops leads the use demand of herbicide to be increased sharply. In recent years, the farmland demand for chemical herbicides continues to increase. Since 1970, the use amount of herbicide is always the first of three general pesticides in the world, and the proportion of herbicide in pesticides is gradually increased to 37%. According to statistics, the effective components of the existing chemical herbicides in the market are more than 100, and the glyphosate, the diuron and the atrazine are respectively used in the top order. Although the use of pesticides reduces the risk of crop damage, it also results in pollution of soil and other related environmental resources. The use of large numbers of chemical herbicides has long led to a number of ecological safety and health risks. At present, worldwide, amphibians are significantly reduced, and herbicide pollution therein causes species and populations to decline and vanish at a striking rate, again striking the herbicide pollution alarm. After the common herbicides glyphosate, diuron, atrazine and the like are applied, a part of the herbicide is attached to the surface of plants, and the herbicide is immersed into the plants along with rainfall or other water bodies, so that various grain crops and economic crops are polluted; the other part of the water flows on the soil layer surface or permeates to the deep soil layer along with the water flow, flows into rivers and lakes along with rainfall and farmland drainage, and influences and pollutes aquatic organisms and water body environment. Therefore, there is an urgent need to develop a substance which does not destroy the environment required for plant growth and can achieve herbicidal effects.
Disclosure of Invention
The invention discloses polydopamine chelating polymer membrane liquid and a preparation method and application thereof, and solves the problem that the existing herbicide can pollute crops and water.
The polydopamine chelated polymer membrane solution comprises the following raw materials: 3.6 to 10.8g of dopamine hydrochloride, 120 to 200mL of distilled water, 120 to 200mL of absolute ethyl alcohol, 3.6 to 10.8mL of ammonia water solution, 1 to 5g of chitosan, 90 to 100mL of 1% glacial acetic acid solution, 902 to 4g of polyvinylpyrrolidone K and 1 to 2mL of 1% glycerol.
Preferably, the method comprises the following raw materials: 5.4-9.0 g of dopamine hydrochloride, 150-170 mL of distilled water, 140-190 mL of absolute ethyl alcohol, 5.4-9.0 mL of ammonia water solution, 2-4 g of chitosan, 94-96 mL of 1% glacial acetic acid solution, 902.5-3.5 g of polyvinylpyrrolidone K and 1-2 mL of 1% glycerol.
Preferably, the method comprises the following raw materials: 7.2g of dopamine hydrochloride, 160mL of distilled water, 180mL of absolute ethyl alcohol, 7.2mL of ammonia water solution, 3g of chitosan, 95mL of 1% glacial acetic acid solution, 903 g of polyvinylpyrrolidone and 1.5mL of 1% glycerol.
Preferably, the mass concentration of the ammonia water solution is 25%.
The second purpose of the invention is to protect the preparation method of the polydopamine chelating polymer membrane liquid, which specifically comprises the following steps:
Producing polydopamine: dissolving dopamine hydrochloride with the formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with the formula amount, uniformly stirring, standing for 20-30 h, and collecting precipitate to obtain polydopamine;
Preparing mixed feed liquid: uniformly mixing the prepared polydopamine with formula amount of polyvinylpyrrolidone K90 and 1% of glycerol to obtain mixed liquid; polydopamine polyvinylpyrrolidone K90:1% glycerol = 7.2g: 2-4 g:1mL;
Preparing polydopamine chelating polymer membrane liquid: dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 40-60 min at 90 ℃, cooling to 70-80 ℃, adding the prepared mixed solution, and stirring for 1-1.5 h to obtain polydopamine chelating polymer membrane solution.
Preferably, when the polydopamine is generated, the method for collecting the precipitate is centrifugal collection, 8000-10000 r/min, and centrifugal separation for 3-6 min.
The third object of the invention is to protect the polydopamine chelating polymer membrane liquid for weeding.
Preferably, the herbicidal species include barnyard grass, green bristlegrass, crabgrass, goosegrass, cricket grass, purslane, clematis root, plantain.
Preferably, the herbicide is used in the following method: before sowing or after 6 months of summer harvest, the herbicide is diluted and sprayed, and the volume ratio of the herbicide to the water is 1:12-15.
Preferably, the spraying amount of the herbicide is 20-30L of diluted herbicide sprayed per mu.
Compared with the prior art, the invention has the beneficial effects that:
The polydopamine chelating polymer membrane liquid prepared by the invention can obviously inhibit plant germination after being sprayed, achieves the weeding effect of chemical herbicide, does not damage the environment required by plant growth, generates less secondary pollution, has good treatment effect, can be treated in situ, is simple to operate and has little influence on the environment.
The polydopamine in the raw material has excellent heat absorption property, so that plants are stressed by high temperature, the light respiration and dark respiration of the plants are enhanced, and the photosynthesis rate is reduced. And the structure and the function of chloroplasts and cytoplasm are destroyed at high temperature, a series of enzymes related to photosynthetic electron transfer on the chloroplasts are inactivated, active oxygen is excessively generated, membrane lipid peroxidation, pigment discoloration, protein inactivation and DNA damage in plant cells are caused, and cell death is finally caused. Meanwhile, PVP in the raw materials and chitosan have excellent binding capacity, so that the permeability of oxygen and carbon dioxide on the soil surface is reduced.
Drawings
FIG. 1 is a graph showing the endothermic performance test of the polydopamine chelate polymer membrane prepared in example 3 of the present invention;
FIG. 2 is a graph showing carbon dioxide permeability test of polydopamine chelate polymer membrane prepared in example 3 of the present invention;
FIG. 3 is a thermogravimetric analysis and degradation analysis chart of the polydopamine chelate polymer membrane solution prepared in example 3 of the present invention;
FIG. 4 is a 20-day membrane degradation picture of the polydopamine chelate polymer membrane solution prepared in example 3 of the present invention;
Fig. 5 is a graph for testing germination rate of carnation after spraying polydopamine chelate polymer membrane prepared in example 3 of the present invention; wherein A is germination vigor; panel B shows germination rate; panel C shows germination on the fourth day, the upper two pots are two parallel tests of normal germination, and the lower two pots are two parallel tests of germination after spraying polydopamine chelating polymer membrane liquid; the graph D shows germination on the sixth day, the upper two basins are two groups of parallel tests of normal germination, and the lower two basins are two groups of parallel tests of germination after polydopamine chelating polymer membrane liquid is sprayed; and E, the graph E shows germination on the eighth day, the upper two basins are two groups of parallel tests for normal germination, and the lower two basins are two groups of parallel tests for germination after polydopamine chelating polymer membrane liquid is sprayed.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The polydopamine chelated polymer membrane solution comprises the following raw materials: 3.6g of dopamine hydrochloride, 120mL of distilled water, 120mL of absolute ethyl alcohol, 3.6mL of ammonia water solution, 1g of chitosan, 90mL of 1% glacial acetic acid solution, 902 g of polyvinylpyrrolidone and 1mL of 1% glycerol.
The preparation method of the polydopamine chelating polymer membrane liquid specifically comprises the following steps:
(1) Producing polydopamine: dissolving dopamine hydrochloride with formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with formula amount, uniformly stirring, standing for 20 hours, collecting precipitate by a centrifugal method, centrifuging for 3min at 8000r/min, and collecting precipitate to obtain polydopamine. The mass concentration of the ammonia water solution is 25%.
(2) Preparing mixed feed liquid: uniformly mixing the polydopamine prepared in the step (1) with polyvinylpyrrolidone K90 and 1% glycerol in a formula amount to obtain mixed liquid; polydopamine polyvinylpyrrolidone k90:1% glycerol=7.2g:2g:1 ml.
(3) Preparing polydopamine chelating polymer membrane liquid: and (3) dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 1h at 90 ℃, cooling to 80 ℃, adding the mixed solution prepared in step (2), and stirring for 1h to obtain the polydopamine chelating polymer membrane solution.
The polydopamine chelating polymer membrane liquid is used for weeding, and the using method is as follows: after summer harvest before sowing or 6 months, the polydopamine chelating polymer membrane liquid is diluted and sprayed, wherein the volume ratio of the polydopamine chelating polymer membrane liquid to water is 1:12, and the spraying dosage is 20L of diluted polydopamine chelating polymer membrane liquid per mu.
Example 2
A polydopamine chelating polymer membrane solution comprising: 5.4g of dopamine hydrochloride, 150mL of distilled water, 140mL of absolute ethyl alcohol, 5.4mL of ammonia water solution, 2g of chitosan, 94mL of 1% glacial acetic acid solution, 902.5 g of polyvinylpyrrolidone K and 1mL of 1% glycerol.
The preparation method of the polydopamine chelating polymer membrane liquid specifically comprises the following steps:
(1) Producing polydopamine: dissolving dopamine hydrochloride with formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with formula amount, uniformly stirring, standing for 20 hours, collecting precipitate by a centrifugal method, centrifuging for 4min at 8000r/min, and collecting precipitate to obtain polydopamine. The mass concentration of the ammonia water solution is 25%.
(2) Preparing mixed feed liquid: uniformly mixing the polydopamine prepared in the step (1) with polyvinylpyrrolidone K90 and 1% glycerol in a formula amount to obtain mixed liquid; polydopamine polyvinylpyrrolidone k90:1% glycerol=7.2g:2g:1 ml.
(3) Preparing polydopamine chelating polymer membrane liquid: and (3) dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 1h at 90 ℃, cooling to 80 ℃, adding the mixed solution prepared in step (2), and stirring for 1h to obtain the polydopamine chelating polymer membrane solution.
The polydopamine chelating polymer membrane liquid is used for weeding, and the using method is as follows: after summer harvest before sowing or 6 months, the polydopamine chelating polymer membrane liquid is diluted and sprayed, wherein the volume ratio of the polydopamine chelating polymer membrane liquid to water is 1:12, and the spraying dosage is 20L of diluted polydopamine chelating polymer membrane liquid per mu.
Example 3
The polydopamine chelating polymer membrane solution comprises the following raw materials: 7.2g of dopamine hydrochloride, 160mL of distilled water, 180mL of absolute ethyl alcohol, 7.2mL of ammonia water solution, 3g of chitosan, 95mL of 1% glacial acetic acid solution, 903 g of polyvinylpyrrolidone and 1.5mL of 1% glycerol.
The preparation method of the polydopamine chelating polymer membrane liquid specifically comprises the following steps:
(1) Producing polydopamine: dissolving dopamine hydrochloride with formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with formula amount, uniformly stirring, standing for 25 hours, collecting precipitate by using a centrifugal method, centrifuging for 4min at the rotating speed of 9000r/min, and collecting precipitate to obtain polydopamine. The mass concentration of the ammonia water solution is 25%.
(2) Preparing mixed feed liquid: uniformly mixing the polydopamine prepared in the step (1) with polyvinylpyrrolidone K90 and 1% glycerol in a formula amount to obtain mixed liquid; polydopamine polyvinylpyrrolidone k90:1% glycerol=7.2g:3 g:1ml.
(3) Preparing polydopamine chelating polymer membrane liquid: and (3) dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 1h at 90 ℃, cooling to 80 ℃, adding the mixed solution prepared in step (2), and stirring for 1h to obtain the polydopamine chelating polymer membrane solution.
The polydopamine chelating polymer membrane liquid is used for weeding, and the using method is as follows: after summer harvest before sowing or 6 months, the polydopamine chelating polymer membrane liquid is diluted and sprayed, wherein the volume ratio of the polydopamine chelating polymer membrane liquid to water=1:13, and the spraying dosage is 25L of diluted polydopamine chelating polymer membrane liquid per mu.
Example 4
The polydopamine chelating polymer membrane solution comprises the following raw materials: 9.0g of dopamine hydrochloride, 170mL of distilled water, 190mL of absolute ethyl alcohol, 9.0mL of ammonia water solution, 4g of chitosan, 96mL of 1% glacial acetic acid solution, 903.5 g of polyvinylpyrrolidone K and 2mL of 1% glycerol.
The preparation method of the polydopamine chelating polymer membrane liquid specifically comprises the following steps:
(1) Producing polydopamine: dissolving dopamine hydrochloride with formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with formula amount, uniformly stirring, standing for 30 hours, collecting precipitate by a centrifugal method, centrifuging for 6min at 10000r/min, and collecting precipitate to obtain polydopamine. The mass concentration of the ammonia water solution is 25%.
(2) Preparing mixed feed liquid: uniformly mixing the polydopamine prepared in the step (1) with polyvinylpyrrolidone K90 and 1% glycerol in a formula amount to obtain mixed liquid; polydopamine polyvinylpyrrolidone k90:1% glycerol=7.2g:4 g:1ml.
(3) Preparing polydopamine chelating polymer membrane liquid: and (3) dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 1h at 90 ℃, cooling to 80 ℃, adding the mixed solution prepared in step (2), and stirring for 1h to obtain the polydopamine chelating polymer membrane solution.
The polydopamine chelating polymer membrane liquid is used for weeding, and the using method is as follows: after summer harvest before sowing or 6 months, the polydopamine chelating polymer membrane liquid is diluted and sprayed, wherein the volume ratio of the polydopamine chelating polymer membrane liquid to water is 1:14, and the spraying dosage is 30L of diluted polydopamine chelating polymer membrane liquid per mu.
Example 5
The polydopamine chelating polymer membrane solution comprises the following raw materials: 10.8g of dopamine hydrochloride, 200mL of distilled water, 200mL of absolute ethyl alcohol, 10.8mL of ammonia water solution, 5g of chitosan, 100mL of 1% glacial acetic acid solution, 904 g of polyvinylpyrrolidone K and 2mL of 1% glycerol.
The preparation method of the polydopamine chelating polymer membrane liquid specifically comprises the following steps:
(1) Producing polydopamine: dissolving dopamine hydrochloride with formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with formula amount, uniformly stirring, standing for 30 hours, collecting precipitate by a centrifugal method, centrifuging for 6min at 10000r/min, and collecting precipitate to obtain polydopamine. The mass concentration of the ammonia water solution is 25%.
(2) Preparing mixed feed liquid: uniformly mixing the polydopamine prepared in the step (1) with polyvinylpyrrolidone K90 and 1% glycerol in a formula amount to obtain mixed liquid; polydopamine polyvinylpyrrolidone k90:1% glycerol=7.2g:4 g:1ml.
(3) Preparing polydopamine chelating polymer membrane liquid: and (3) dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 1h at 90 ℃, cooling to 80 ℃, adding the mixed solution prepared in step (2), and stirring for 1h to obtain the polydopamine chelating polymer membrane solution.
The polydopamine chelating polymer membrane liquid is used for weeding, and the using method is as follows: after summer harvest before sowing or 6 months, the polydopamine chelating polymer membrane liquid is diluted and sprayed, wherein the volume ratio of the polydopamine chelating polymer membrane liquid to water is 1:15, and the spraying dosage is 30L of diluted polydopamine chelating polymer membrane liquid per mu.
Performance testing
The polydopamine chelate polymer membrane solutions prepared in examples 1, 2, 4 and 5 have substantially the same heat absorption performance, oxygen permeability, carbon dioxide permeability, thermogravimetric and degradation effects and seed germination rate inhibition effects as the polydopamine chelate polymer membrane solution prepared in example 3, and the polydopamine chelate polymer membrane solution prepared in example 3 is used for testing the performance.
1. Endothermic Performance test
Spraying the polydopamine chelating polymer membrane solution prepared in the embodiment 3 on the surface of the flowerpot soil to form a composite membrane; the blank soil was used as a control and the surface temperature was recorded at 10 to 14 hours in the morning the next day. As shown in figure 1, after the polydopamine chelating polymer membrane liquid is sprayed, the surface layer temperature of the ground can be obviously improved, and after 200min, the temperature can be raised to above 36 ℃, so that obvious inhibition effect on plant growth is generated.
2. Oxygen permeability
5G of deoxidizer with reduced iron powder as a main component is placed in a constant-weight weighing bottle which is dried, polydopamine chelating polymer membrane liquid prepared in the embodiment 3 is sprayed on a flat plate, after the flat plate is dried at room temperature, a membrane liquid drying membrane material with the thickness of 0.17mm is prepared, the membrane liquid drying membrane material is cut into a sample with the length of 5cm and the width of 5cm, then the membrane sample is tightly covered on a bottle mouth and fixed by a rubber band, and the weighing M 0 is placed in a constant-temperature constant-humidity box with the temperature of 25 ℃ and the humidity of 70%, and after the membrane liquid drying membrane material is placed for 48 hours, the mass M 1 of the weighing bottle is measured.
The oxygen permeability formula of the membrane is: q (O 2)＝(M0-M1)/(t.times.s)
Wherein Q (O 2) is the O 2 transmission rate/[ g/(M 2·h)];M0) is the initial mass/g, M 1 is the final mass/g, and t is time/h, s.
3. Permeability to carbon dioxide
5G KOH is placed in a weighing bottle which is dried to constant weight, a film liquid drying film material is cut into a sample with the length of 5cm and the width of 5cm, then the sample is tightly covered on a bottle mouth and fixed by a rubber band, the weighing M 0 is placed in a constant temperature and humidity box with the temperature of 25 ℃ and the humidity of 70 percent RH, and after the weighing bottle is placed for 48 hours, the mass M 1 of the weighing bottle is measured.
The CO 2 transmission rate formula of the membrane is: q (CO 2)＝(M0-M1)/(t.times.s)
Where Q (CO 2) is CO 2 rate/[ g/(M 2·h)];M0) is the starting mass/g, M 1 is the final mass/g, t is time/h, s is the effective area of the membrane/M 2.
As can be seen from fig. 2, the membrane fluid dry film material has lower oxygen transmission rate and CO 2 transmission rate, which is related to excellent adhesion property of PVP k90 and increased addition crystallization degree of dopamine particles, reduced oxygen vacancies, and reduced under-oxygen level.
4. Thermogravimetric analysis and degradation analysis
Thermogravimetric analysis is an important method for assessing the thermal stability and degradative behaviour of films. As shown in fig. 3, the initial weight loss of the thermal degradation of the film prepared with polydopamine chelated polymer membrane solution is due to the evaporation of residual water in the composite film; the weight loss is due to decomposition of urethane bonds and the like, and evaporation of glycerin and bound water; then the thermal decomposition of chitosan and PVP is finally the decomposition of polydopamine. The results show that the film prepared by the polydopamine chelating polymer membrane liquid shows excellent thermal stability.
In order to depolymerize the degradation performance of the dopamine chelate polymer membrane liquid, the polydopamine chelate polymer membrane liquid is sprayed on a glass plate, dried into a film with the thickness of 0.15-0.20 mm, and then buried in organic cultivation soil with the depth of 5cm under natural conditions. The film was taken out after 20 days, cleaned and weighed. The film was found to have been completely disintegrated and the weight was reduced by 40 to 50%, which is closely related to the loss of water therein and the excellent degradation properties of the film. Fig. 4 is a film degradation picture on day 20, fig. 4a is a film shape before day 20, and fig. 4b is a film shape after day 20.
5. Experiment of germination inhibition
Adopting a potting method, selecting caryophyllus seeds with consistent sizes and plump grains, and sterilizing: soaking in 7.5% H 2O2 for 30min, washing with water until odorless, and drying with sterile filter paper. The sterilized caryophyllus seeds are selected and placed in flowerpots, and 10 seeds are placed in each flowerpot. And uniformly spraying the polydopamine chelating polymer membrane liquid on the surface of the flowerpot soil. The non-sprayed seeds are used as blank control, and the germination rate, germination vigor, germination time lag and germination length of the seeds are recorded in the same outdoor environment.
Germination percentage (%) =total number of germinated seeds in 7 d/total number of test seeds×100%;
germination vigor (%) =4d number of germinated seeds/total number of test seeds×100%;
As shown in FIG. 5, the germination vigor is shown in the graph A; panel B shows germination rate; panel C shows germination on day four; panel D shows germination on day six; panel E shows germination on day eight; in the graph C, the graph D and the graph E, the upper two basins are used for normal germination, and the lower two basins are used for germination photographs after polydopamine chelating polymer membrane liquid is sprayed.
The result shows that under normal conditions, the carnation has the characteristic of rapid germination and growth, the germination potential in the fourth day can reach 21.67%, the germination rate in the seventh day is 98.33%, and the plant germination can be obviously inhibited after the polydopamine chelating polymer membrane liquid is sprayed, and the germination rate in the seventh day is 0%. The polydopamine has excellent endothermic characteristics, so that plants are stressed at high temperature, the light respiration and dark respiration of the plants are enhanced, and the photosynthesis rate is reduced. And the structure and the function of chloroplasts and cytoplasm are destroyed at high temperature, a series of enzymes related to photosynthetic electron transfer on the chloroplasts are inactivated, active oxygen is excessively generated, and the like, so that membrane lipid peroxidation, pigment discoloration, protein inactivation and DNA destruction in plant cells are caused, and finally, cell death is caused. Meanwhile, the substrate material PVP of the polydopamine chelating polymer membrane liquid has excellent adhesion capability with chitosan, so that the permeability of oxygen and carbon dioxide on the soil surface is reduced.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (10)
1. The polydopamine chelating polymer membrane solution for weeding is characterized by comprising the following raw materials: 3.6-10.8 g of dopamine hydrochloride, 120-200 mL of distilled water, 120-200 mL g of absolute ethyl alcohol, 3.6-10.8 mL of ammonia water solution, 1-5 g of chitosan, 90-100 mL of 1% glacial acetic acid solution, 90-4 g of polyvinylpyrrolidone K and 1-2 mL of 1% glycerol.
2. The polydopamine chelating polymer membrane solution for weeding according to claim 1, wherein the polydopamine chelating polymer membrane solution comprises the following raw materials: 5.4-9.0 g of dopamine hydrochloride, 150-170 mL of distilled water, 140-190 mL of absolute ethyl alcohol, 5.4-9.0 mL of ammonia water solution, 2-4 g of chitosan, 94-96 mL of 1% glacial acetic acid solution, 2.5-3.5 g of polyvinylpyrrolidone K and 1-2 mL of 1% glycerol.
3. The polydopamine chelating polymer membrane solution for weeding according to claim 2, which is characterized by comprising the following raw materials: dopamine hydrochloride 7.2 g, distilled water 160 mL, absolute ethyl alcohol 180 mL, ammonia water solution 7.2 mL, chitosan 3 g, 1% glacial acetic acid solution 95 mL, polyvinylpyrrolidone K90 3 g, 1% glycerin 1.5 mL.
4. The polydopamine chelating polymer membrane solution for weeding according to any one of claims 1-3, wherein the mass concentration of the ammonia water solution is 25%.
5. The method for preparing the polydopamine chelating polymer membrane liquid for weeding according to claim 1, which is characterized by comprising the following steps:
Producing polydopamine: dissolving dopamine hydrochloride with a formula amount into a mixed solution of distilled water and absolute ethyl alcohol, adding ammonia water solution with a formula amount, uniformly stirring, standing for 20-30 h, and collecting precipitate to obtain polydopamine;
Preparing mixed feed liquid: uniformly mixing the prepared polydopamine with formula amount of polyvinylpyrrolidone K90 and 1% of glycerol to obtain mixed liquid; polydopamine is polyvinylpyrrolidone K90, 1% glycerol=7.2 g:2-4 g:1 mL;
Preparing polydopamine chelating polymer membrane liquid: and dissolving chitosan with the formula amount in 1% glacial acetic acid solution, stirring for 40-60 min at 90 ℃, cooling to 70-80 ℃, adding the prepared mixed solution, and stirring for 1-1.5 h to obtain polydopamine chelating polymer membrane solution.
6. The method for preparing the polydopamine chelate polymer membrane solution for weeding according to claim 5, wherein the method for collecting the precipitate is centrifugal collection, 8000-10000 r/min and centrifugal collection for 3-6 min when polydopamine is generated.
7. The use of a polydopamine chelating polymer membrane solution according to claim 1, wherein said polydopamine chelating polymer membrane solution is used for weeding.
8. The use of polydopamine chelate polymer membrane according to claim 7 wherein said herbicidal species comprises barnyard grass, green bristlegrass, crabgrass, goosegrass, purslane, lamiophlomis rotata, plantain.
9. The application of the polydopamine chelating polymer membrane liquid according to claim 8, wherein the application method of the polydopamine chelating polymer membrane liquid is as follows: and before sowing or after 6 months of summer harvest, diluting the polydopamine chelating polymer membrane liquid, and then spraying the polydopamine chelating polymer membrane liquid according to the volume ratio of polydopamine chelating polymer membrane liquid to water=1:12-15.
10. The application of the polydopamine chelating polymer membrane liquid according to claim 9, wherein the spraying dosage of the polydopamine chelating polymer membrane liquid is 20-30L diluted polydopamine chelating polymer membrane liquid sprayed per mu.
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