CN117736463A - Preparation method of cassava starch-based liquid mulching film - Google Patents
Preparation method of cassava starch-based liquid mulching film Download PDFInfo
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- CN117736463A CN117736463A CN202311761232.4A CN202311761232A CN117736463A CN 117736463 A CN117736463 A CN 117736463A CN 202311761232 A CN202311761232 A CN 202311761232A CN 117736463 A CN117736463 A CN 117736463A
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- Prior art keywords
- starch
- stirring
- tetraethoxysilane
- silica sol
- linking agent
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- 229920002472 Starch Polymers 0.000 title claims abstract description 47
- 239000008107 starch Substances 0.000 title claims abstract description 47
- 235000019698 starch Nutrition 0.000 title claims abstract description 47
- 239000007788 liquid Substances 0.000 title claims abstract description 26
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 241000658379 Manihot esculenta subsp. esculenta Species 0.000 title 1
- 240000003183 Manihot esculenta Species 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 12
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 12
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 150000001718 carbodiimides Chemical class 0.000 claims abstract description 10
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- 108010009736 Protein Hydrolysates Proteins 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- 239000000413 hydrolysate Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002362 mulch Substances 0.000 abstract description 28
- 239000002689 soil Substances 0.000 abstract description 6
- 230000008020 evaporation Effects 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract description 3
- 239000007921 spray Substances 0.000 abstract description 3
- 239000004576 sand Substances 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000005507 spraying Methods 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 244000105624 Arachis hypogaea Species 0.000 description 3
- 230000035784 germination Effects 0.000 description 3
- 235000020232 peanut Nutrition 0.000 description 3
- 235000013311 vegetables Nutrition 0.000 description 3
- 235000017060 Arachis glabrata Nutrition 0.000 description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 description 2
- 235000018262 Arachis monticola Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- -1 Polyethylene Polymers 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 239000002420 orchard Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001896 polybutyrate Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/28—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture specially adapted for farming
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- Protection Of Plants (AREA)
Abstract
The invention discloses a preparation method of a tapioca starch-based liquid mulch film, which comprises the following steps: (1) Preparing tetraethoxysilane, ethanol, deionized water and 0.8-1.2mol/L hydrochloric acid into tetraethoxysilane hydrolysate, and stirring at room temperature until the tetraethoxysilane hydrolysate is completely hydrolyzed to obtain silica sol serving as a cross-linking agent; (2) Adding tapioca starch into silica sol, and stirring and mixing to obtain a starch solution containing a cross-linking agent; (3) Adding carboxymethyl cellulose and carbodiimide into a starch solution containing a cross-linking agent, and stirring and mixing uniformly to obtain emulsion, namely the cassava starch-based liquid mulching film. The mulch emulsion prepared by the invention is easy to spray and use, can help to keep soil moist, reduce water evaporation and rainwater loss, maintain the surface temperature and reduce soil heat loss.
Description
Technical Field
The invention provides a preparation method of a biodegradable liquid mulching film, and belongs to the technical field of agricultural mulching films.
Background
The China has been a large agricultural country since ancient times, the total planting area of the Chinese crops reaches 25 hundred million mu nowadays, and the planting of vegetables and fruit trees needs mulch protection. The total vegetable planting area of China is about 3.22 hundred million mu, which accounts for about 12.8 percent of the total crop planting area, the orchard area is about 2 hundred million mu, which accounts for about 7.56 percent of the total crop planting area.
The agricultural mulching film is introduced from China, the Polyethylene (PE) mulching film is rapidly and widely popularized and applied in China, the mulching film mulching crops have remarkable water saving and yield increasing effects on agriculture, the water utilization efficiency and yield of the crops can be respectively improved by about 30%, great contribution is made to yield and income increase of agricultural products, grain safety, annual supply of vegetables and the like are ensured, and the direct economic benefit of 1200-1400 hundred million yuan is generated in China each year.
In order to solve the recycling and degradation problems caused by the use of the traditional PE mulch, researchers try to prepare the mulch by taking various bio-based degradable materials as the base to replace the PE mulch, such as PBAT, PLA, PBS and the like. These mulch films all have excellent degradability and environmental friendly properties. But prevents the popularization of cost or production process.
Wherein, the starch degradable mulch film only needs a simple production process. And cassava is defined by the government of our country as a non-grain energy crop, called "the king of starch". The yield of the cassava starch in 2022 is about 22 ten thousand tons, and the cassava starch is mainly used for modified starch, alcohol, feed and the like, is less to eat, and therefore, the cost is low. However, the starch degradable mulch film has the fatal defects of quick degradation time, short shelf life and difficult commercialization.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a biodegradable liquid mulching film using tapioca starch as a basic raw material, which has the advantages of simple preparation process, easily obtained raw materials, long shelf life and adjustable degradation time, and the prepared mulching film has the performances of heat preservation, moisture preservation and seedling protection.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a cassava starch-based liquid mulching film comprises the following steps:
(1) Preparing tetraethoxysilane, ethanol, deionized water and 0.8-1.2mol/L hydrochloric acid into tetraethoxysilane hydrolysate, and stirring at room temperature until the tetraethoxysilane hydrolysate is completely hydrolyzed to obtain silica sol serving as a cross-linking agent; the mass ratio of the tetraethoxysilane to the ethanol to the water to the hydrochloric acid is 25-55: 23:9:0.08 to 0.2;
(2) Adding tapioca starch into silica sol, wherein the mass ratio of the tapioca starch to the silica sol is 8-15: 100, stirring and mixing to obtain a starch solution containing a cross-linking agent;
(3) Adding carboxymethyl cellulose and carbodiimide to a starch solution containing a cross-linking agent, wherein the carboxymethyl cellulose: carbodiimide: the mass ratio of the starch solution is 9-15: 0.009-0.015: 1000, stirring and mixing uniformly to obtain emulsion, namely the cassava starch-based liquid mulching film.
Preferably, in the step (1), a mixed solution of ethanol and water is prepared, ethyl orthosilicate is added, hydrochloric acid is added, and the mixture is stirred and mixed and then hydrolyzed for 1 to 2 hours at room temperature.
Preferably, in the step (1), the hydrochloric acid concentration is 1mol/L.
Preferably, the tapioca starch in the step (2) is industrial grade starch.
Preferably, the step (2) of stirring and mixing to obtain a starch solution means that the tapioca starch is added into the silica sol and stirred until the starch is completely dissolved, and the starch is crosslinked while stirring to form a network structure, so that a uniform and stable mixture is formed.
Preferably, in the stirring and mixing step (3), the starch mixed solution added with the carboxymethyl cellulose and the carbodiimide is uniformly dispersed by a homogenizer, so that the carbodiimide catalyzes the starch and the carboxymethyl cellulose to start esterification reaction at room temperature, and the mixed emulsion is left for 1 to 1.5 hours to fully react to form a micro-crosslinking structure.
Compared with the prior art, the invention has the beneficial effects that:
(1) The mulch emulsion prepared by the invention is easy to spray and use, and a single person can conveniently and rapidly form a layer of film on the surface of a large-scale field through a sprayer. The starch-based mulching film prepared by the invention can help keep soil moist, reduce water evaporation and rainwater loss, maintain the surface temperature and reduce soil heat loss.
(2) The liquid mulch emulsion has low synthesis cost, simple formula and convenient process, and can be prepared and used in various places.
(3) The liquid mulching film of the invention is used as a disposable mulching film, is free from adding non-degradable auxiliary agents, is a completely biodegradable material, reduces plastic pollution in fields, and meets the national policy requirements.
Drawings
FIG. 1 shows the hydrolysis of ethyl orthosilicate to orthosilicic acid under the catalysis of ethanol and hydrochloric acid.
The left diagram of fig. 2 is a tapioca starch structural formula, and the right diagram is a simplified structural formula.
FIG. 3 shows the cross-linking of the dehydration condensation of orthosilicic acid and tapioca starch.
FIG. 4 shows the esterification of carboxymethyl cellulose with tapioca starch under carbodiimide action.
Detailed Description
The technical scheme of the invention will be clearly and completely described below. It will be apparent that the described embodiments are only a part of the invention, but not all. 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.
The specific conditions are not noted in the examples of the present invention, and are carried out according to conventional conditions or conditions suggested by the manufacturer. The reagents or apparatus used are conventional products, which are available by conventional technical means or commercially available, without the manufacturer's knowledge.
Example 1:
(1) 556.5g of ethyl orthosilicate was added to a mixture of 96.4g of water and 246.1g of ethanol, 1g of 1mol/L hydrochloric acid was added dropwise, and after stirring and mixing, the mixture was hydrolyzed at room temperature for 1 hour to obtain a silica sol as a crosslinking agent.
(2) Adding 90g of tapioca starch into the silica sol, and stirring and mixing to obtain nearly 1kg of starch solution containing a cross-linking agent;
(3) Adding 9g of carboxymethyl cellulose and 0.009g of carbodiimide into a starch solution containing a crosslinking agent, dispersing uniformly by a homogenizer at a rotating speed of 2000r/m for 10min, and standing for 1 hour to fully react to form a micro-crosslinking structure, thus obtaining emulsion, namely the tapioca starch-based liquid mulch film.
(4) Filling 100-300 mu m diameter completely dried sand grains in three containers (without sealing covers) with length, width and height of 30cm, 30cm and 20cm respectively, uniformly spraying 1kg of water into the containers by using a spray can, spraying liquid mulch emulsion until the surface of the sand grains is completely covered after the water completely permeates the sand grains, weighing, marking as No. 1, no. 2 and No. 3, standing for two days at room temperature, and weighing. The average moisture retention was 78%.
TABLE 1
Example 2:
liquid mulch film and sand container were the same as in example 1, except that three sand containers were each inserted with 2 thermometers to a depth of 10cm into the container, the temperatures thereof were shown as 1-1, 1-2, 2-1, 2-2, 3-1, 3-2, and the three sand containers were heated to 50 ℃ using an oven, left at room temperature for 24 hours and the temperatures before and after were recorded. Compared with a control group, the heat preservation effect of the sprayed mulching film is obvious.
TABLE 2
Example 3:
10 peanut seeds were planted in the same manner as in example 1 except that the seeds were dispersed at a depth of 5cm in sand containers No. 1, no. 2 and No. 3, respectively, and the germination rate was recorded for 10 days.
TABLE 3 Table 3
Example 4:
otherwise, the same as in example 1, but No. 1, no. 2 and No. 3 sand containers were placed outdoors, and the time when the mulch film on the sand surface was completely degraded was observed.
TABLE 4 Table 4
| Sample of | Number of days when mulch film is basically intact | Days of complete degradation of mulch film |
| 1 | 38 | 51 |
| 2 | 41 | 55 |
| 3 | 40 | 53 |
Example 5:
the liquid mulch was obtained in the same manner as in example 1 except that the amount of ethyl orthosilicate was changed. Then, the operation was performed as in example 2 and example 4, and the amount of heat preservation and the number of degradation days of the liquid mulch film were observed.
TABLE 5
Example 6:
otherwise, the same as in example 1, but with the amount of carboxymethyl cellulose changed, a liquid mulch film was obtained. And observing the water retention rate and degradation days of the liquid mulching film.
TABLE 6
| Carboxymethyl cellulose addition (g) | Water retention (%) | Days of complete degradation of mulch film |
| 10.5 | 81 | 50 |
| 12 | 85 | 53 |
| 13.5 | 86 | 53 |
Comparative example 1:
the sample was left for two days at room temperature and weighed as in example 1, except that the liquid mulch was not sprayed.
TABLE 7
As can be seen from a comparison of example 1 and comparative example 1, the liquid mulch film can help to keep the soil moist and reduce the evaporation of water after spraying.
Comparative example 2:
the procedure of example 2 was followed except that the liquid mulch film was not sprayed, and the film was left at room temperature for 24 hours to compare the temperatures before and after the film was used.
TABLE 8
As can be seen from a comparison of example 2 and comparative example 2, the liquid mulch film can help to maintain the surface temperature and reduce the heat loss of soil after spraying.
Comparative example 3:
the germination of peanuts after 10 days was recorded as in example 3, but without spraying a liquid mulch film.
TABLE 9
As is clear from comparative example 3 and comparative example 3, the container sprayed with the liquid mulch film is superior to peanut sprouts not sprayed with the liquid mulch film in both germination rate and sprout length.
Claims (5)
1. A preparation method of a cassava starch-based liquid mulching film is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) Preparing tetraethoxysilane, ethanol, deionized water and 0.8-1.2mol/L hydrochloric acid into tetraethoxysilane hydrolysate, and stirring at room temperature until the tetraethoxysilane hydrolysate is completely hydrolyzed to obtain silica sol serving as a cross-linking agent; the mass ratio of the tetraethoxysilane to the ethanol to the water to the hydrochloric acid is 25-55: 23:9:0.08 to 0.2;
(2) Adding tapioca starch into silica sol, wherein the mass ratio of the tapioca starch to the silica sol is 8-15: 100, stirring and mixing to obtain a starch solution containing a cross-linking agent;
(3) Adding carboxymethyl cellulose and carbodiimide to a starch solution containing a cross-linking agent, wherein the carboxymethyl cellulose: carbodiimide: the mass ratio of the starch solution is 9-15: 0.009-0.015: 1000, stirring and mixing uniformly to obtain emulsion, namely the cassava starch-based liquid mulching film.
2. The method of manufacturing according to claim 1, wherein: in the step (1), a mixed solution of ethanol and water is prepared, then tetraethoxysilane is added, hydrochloric acid is added, and the mixture is stirred and mixed and then hydrolyzed for 1 to 2 hours at room temperature.
3. The method of manufacturing according to claim 1, wherein: in the step (1), the concentration of hydrochloric acid is 1mol/L.
4. The method of manufacturing according to claim 1, wherein: and (2) stirring and mixing to obtain a starch solution, namely adding the cassava starch into the silica sol, stirring until the starch is completely dissolved, and forming a network structure by crosslinking while stirring to form a uniform and stable mixture.
5. The method of manufacturing according to claim 1, wherein: and (3) stirring and mixing, namely uniformly dispersing the starch mixed solution added with the carboxymethyl cellulose and the carbodiimide by a homogenizer, and standing for 1-1.5 hours to enable the mixed emulsion to fully react to form a micro-crosslinking structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311761232.4A CN117736463A (en) | 2023-12-20 | 2023-12-20 | Preparation method of cassava starch-based liquid mulching film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311761232.4A CN117736463A (en) | 2023-12-20 | 2023-12-20 | Preparation method of cassava starch-based liquid mulching film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117736463A true CN117736463A (en) | 2024-03-22 |
Family
ID=90277120
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311761232.4A Pending CN117736463A (en) | 2023-12-20 | 2023-12-20 | Preparation method of cassava starch-based liquid mulching film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117736463A (en) |
-
2023
- 2023-12-20 CN CN202311761232.4A patent/CN117736463A/en active Pending
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