CN115703844A - Preparation method of starch with good compatibility with degradable polyester - Google Patents
Preparation method of starch with good compatibility with degradable polyester Download PDFInfo
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- CN115703844A CN115703844A CN202110897718.5A CN202110897718A CN115703844A CN 115703844 A CN115703844 A CN 115703844A CN 202110897718 A CN202110897718 A CN 202110897718A CN 115703844 A CN115703844 A CN 115703844A
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- degradable polyester
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Abstract
The invention discloses a preparation method of starch with good compatibility with degradable polyester, belonging to the technical field of starch modification. The invention discloses a preparation method of starch with good compatibility with degradable polyester, which comprises the steps of preparing starch into starch milk, adding metal salt, adjusting pH, adding glycidyl ether compound for reaction, neutralizing the obtained starch slurry with acid, filtering, washing and drying to obtain the modified starch with good compatibility with the degradable polyester. The starch is used as a main raw material, the starch is convenient to obtain, low in cost and easy to degrade, the prepared starch and the degradable polyester have good compatibility through reaction modification, meanwhile, the hydrophobicity is obviously improved, and the starch can be widely applied to the high-added-value fields of degradable packaging materials, high-grade paper, microcapsule wall materials and the like.
Description
Technical Field
The invention relates to the technical field of starch modification, in particular to a preparation method of starch with good compatibility with degradable polyester.
Background
The starch can be widely applied to industries such as papermaking, textile, food, feed, medicine, daily chemical, petroleum and the like, and is used as a natural renewable resource, and the starch becomes an important industrial raw material in modern life. In the field of completely biodegradable materials, the cost is reduced on the premise of ensuring the material performance by adopting a starch filling method. However, due to the hydrophilicity of the common starch, the common starch cannot have good compatibility with the degradable polyester material, so that the development and application range of the starch is limited.
However, the introduction of hydrophobic groups into starch molecules can significantly improve the properties of starch, and the application range thereof can be greatly expanded, and such modification methods also become hot spots of current domestic and foreign research. The starch can be better compatible with various degradable polyesters through hydrophobic modification, and the service performance of the starch is ensured. Meanwhile, the method has wide application in the fields of high added values of degradable packaging materials, high-grade paper, microcapsule wall materials and the like.
Therefore, it is a problem to be solved by those skilled in the art to provide a method for preparing starch with good compatibility with degradable polyester.
Disclosure of Invention
In view of the above, the invention provides a preparation method of starch having good compatibility with degradable polyester, so as to improve the dispersion effect of modified starch in application, and enable the modified starch to have better plasticizing property, compatibility and water resistance with a polymer.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of starch with good compatibility with degradable polyester comprises the following specific steps:
(1) Preparing starch milk with the concentration of 25-40% by using water;
(2) Adding metal salt accounting for 0.1-0.5% of the mass of the starch into the starch milk prepared in the step (1), adding 3% of sodium hydroxide solution, adjusting the pH value to 8.0-9.0, and uniformly stirring;
(3) Adding glycidyl ether compounds with the mass of 1-10% of the starch into the uniformly stirred mixture obtained in the step (2), uniformly stirring, and reacting for 2-10 h at the temperature of 30-60 ℃; neutralizing the obtained product with 3% hydrochloric acid until the pH value is 6.5-7.0, filtering, washing and drying the obtained product to obtain the modified starch.
Further, the starch in the step (1) is corn starch, cassava starch or potato starch.
Further, the metal salt in the step (2) is sodium chloride or sodium sulfate.
Further, the glycidyl ether compound in the step (3) is 1, 2-cyclohexanediol diglycidyl ether or o-tolylglycidyl ether.
The invention adopts a wet process, and 1, 2-cyclohexanediol diglycidyl ether or o-toluene glycidyl ether and different types of starch (corn starch, tapioca starch and potato starch) are reacted in a proper reaction system to prepare the modified starch.
According to the technical scheme, compared with the prior art, the invention discloses the preparation method of the starch with good compatibility with the degradable polyester, the starch is used as a main raw material, the raw material is natural, the source is wide, and the production cost is low; the prepared modified starch with good compatibility with the degradable polyester is non-toxic, harmless, degradable and environment-friendly; the hydroxyl of the starch reacts with the epoxy group of the 1, 2-cyclohexanediol diglycidyl ether or the o-tolylene glycidyl ether, and the hydrophobic group is introduced, so that the prepared hydrophobic modified starch and the degradable polyester have better plasticizing property, compatibility and water resistance, a new way is opened up for the efficient utilization of the starch, and the added value of the starch is improved; the preparation method disclosed by the invention is environment-friendly and efficient, is simple and convenient to operate, can improve the compatibility with the degradable polyester material, and is widely applied to the high-added-value fields of degradable packaging materials, high-grade paper, microcapsule wall materials and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a sample membrane electron microscope detection observation result of uniformly discharging a membrane by blowing the composite material of the hydrophobic modified starch prepared in example 1 and PBAT after mixing and extruding;
FIG. 2 is a graph showing the results of electron microscope examination and observation of sample films obtained by blowing and uniformly discharging films on a composite material obtained by mixing and extruding hydrophobically modified starch and PBAT prepared in example 2 of the present invention;
FIG. 3 is a sample membrane electron microscope examination observation result of uniformly discharging a membrane by blowing the composite material of the hydrophobic modified starch prepared in example 3 of the present invention after mixing and extruding with PBAT;
FIG. 4 is a sample membrane electron microscope examination observation result of uniformly discharging a membrane by blowing the composite material of the hydrophobic modified starch prepared in example 4 of the present invention after mixing and extruding with PBAT;
FIG. 5 is a sample membrane electron microscope examination observation result of the composite material after the common corn starch and PBAT are mixed and extruded, the composite material is subjected to membrane blowing, and the membrane is uniformly discharged;
FIG. 6 is a sample film electron microscope examination observation result of the composite material after common potato starch and PBAT mixing extrusion, film blowing and uniform film discharging;
FIG. 7 is a sample membrane electron microscope examination observation result of the film blowing and uniform film discharging of a composite material after the mixing and extrusion of common tapioca starch and PBAT.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of starch with good compatibility with degradable polyester comprises the following specific steps:
(1) Preparing corn starch into starch milk with the concentration of 35% by using water;
(2) Adding sodium chloride accounting for 0.2 percent of the mass of the corn starch into the starch milk prepared in the step (1), adding 3 percent sodium hydroxide solution, adjusting the pH value to 8.5, and uniformly stirring;
(3) Adding 1, 2-cyclohexanediol diglycidyl ether accounting for 5 percent of the mass of the corn starch, uniformly stirring, and reacting for 4 hours at 60 ℃; neutralizing with 3% hydrochloric acid until pH is 6.5, filtering, washing, and oven drying to obtain hydrophobically modified starch.
Example 2
A preparation method of starch with good compatibility with degradable polyester comprises the following specific steps:
(1) Preparing cassava starch into starch milk with the concentration of 30% by using water;
(2) Adding sodium chloride accounting for 0.3 percent of the mass of the cassava starch into the starch milk prepared in the step (1), adding 3 percent of sodium hydroxide solution to adjust the pH value to 9.0, and uniformly stirring;
(3) Adding 1, 2-cyclohexanediol diglycidyl ether accounting for 8% of the mass of the cassava starch, uniformly stirring, and reacting for 6 hours at 40 ℃; neutralizing the solution to pH 7.0 with 3% hydrochloric acid, filtering, washing and drying to obtain the hydrophobic modified starch.
Example 3
A preparation method of starch with good compatibility with degradable polyester comprises the following specific steps:
(1) Preparing potato starch into starch milk with the concentration of 40% by using water;
(2) Adding sodium sulfate accounting for 0.5 percent of the mass of the potato starch into the starch milk prepared in the step (1), adding 3 percent of sodium hydroxide solution to adjust the pH value to 8.0, and uniformly stirring;
(3) Adding o-toluene glycidyl ether accounting for 10% of the mass of the potato starch, uniformly stirring, and reacting for 3 hours at 50 ℃; neutralizing with 3% hydrochloric acid to pH 7.0, filtering, washing, and oven drying to obtain hydrophobically modified starch.
Example 4
A preparation method of starch with good compatibility with degradable polyester comprises the following specific steps:
(1) Preparing corn starch into starch milk with the concentration of 25% by using water;
(2) Adding sodium sulfate accounting for 0.1 percent of the mass of the corn starch into the starch milk prepared in the step (1), adding 3 percent sodium hydroxide solution, adjusting the pH value to 9.0, and uniformly stirring;
(3) Adding o-toluene glycidyl ether accounting for 1 percent of the mass of the corn starch, uniformly stirring, and reacting for 10 hours at 30 ℃; neutralizing the solution to pH6.5 with 3% hydrochloric acid, filtering, washing, and drying to obtain the hydrophobically modified starch.
Comparative example
Common corn starch, potato starch and tapioca starch are taken as comparative examples.
Test examples
The modified starch and the ordinary starch (corn starch, potato starch, tapioca starch) prepared in examples 1 to 4 of the present invention were mixed with PBAT (polybutylene adipate terephthalate) and extruded, respectively, to prepare a standard sample bar, and then the measurement was performed.
1) Water absorption test
At room temperature, firstly weighing the weight (G0) of the obtained standard sample strip, then flatly placing the standard sample strip in a sealed system with the relative humidity of 100%, taking out after 15 days to measure the mass (G1) of the standard sample strip, wherein the water absorption rate of the composite material is as follows:
water absorption (%) = (G1-G0)/G1 × 100%;
wherein G1 is the weight of the standard sample strip after absorbing moisture, G0 is the weight of the dried standard sample strip, and the average value of the test results of 3 times is taken as an experimental value. The water absorption results are shown in table 1.
TABLE 1
As can be seen from Table 1, the modified starches prepared in examples 1 to 4 of the present invention have a significantly lower water absorption than conventional starches, and significantly improved hydrophobicity, making them more compatible with PBAT, and extending the range of applications of the starches.
2) Mechanical Property test
At room temperature, the modified starch and the ordinary starch (corn starch, potato starch, tapioca starch) prepared in examples 1 to 4 of the present invention were respectively mixed with PBAT and extruded to prepare a standard dumbbell-shaped sample bar, and the tensile rate was set to 20mm/min. The results are shown in Table 2.
TABLE 2
As can be seen from Table 2, the mechanical properties of the modified starches prepared in examples 1 to 4 of the present invention are significantly higher than those of the conventional starches, both in terms of elongation at break and tensile strength; indicating that the starch is better compatible with the PBAT after being modified, so that the application field of the starch is wider.
3) Electron microscopy testing of the film after film formation
At room temperature, a film blowing machine is used for respectively blowing films of the modified starch prepared in the embodiments 1 to 4 and the composite material formed by mixing and extruding the common corn starch, the potato starch, the tapioca starch and the PBAT, and then electron microscope detection and observation are carried out on sample films which are uniformly discharged from the films. The results are shown in FIGS. 1 to 7.
As can be seen from FIGS. 1 to 7, the observation of an electron microscope can intuitively show that the modified starch prepared by the invention has better compatibility with PBAT than the common corn starch; the plasticizing effect of the modified starch and PBAT is obviously good.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A preparation method of starch with good compatibility with degradable polyester is characterized by comprising the following specific steps:
(1) Preparing starch into 25-40% starch milk with water;
(2) Adding metal salt with the mass of 0.1-0.5% of that of the starch into the starch milk prepared in the step (1), adding 3% of sodium hydroxide solution, adjusting the pH value to 8.0-9.0, and uniformly stirring;
(3) Adding a glycidyl ether compound accounting for 1-10% of the mass of the starch into the uniformly stirred mixture obtained in the step (2), uniformly stirring, and reacting for 2-10 h at the temperature of 30-60 ℃; neutralizing the mixture to pH6.5-7.0 with 3% hydrochloric acid, filtering, washing and drying to obtain the modified starch.
2. The method for preparing starch with good compatibility with degradable polyester according to claim 1, wherein the starch of step (1) is corn starch, tapioca starch or potato starch.
3. The method for preparing starch with good compatibility with degradable polyester as claimed in claim 1, wherein the metal salt in step (2) is sodium chloride or sodium sulfate.
4. The method for preparing starch with good compatibility with degradable polyester according to claim 1, wherein the glycidyl ether compound in step (3) is 1, 2-cyclohexanediol diglycidyl ether or o-tolylglycidyl ether.
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| CN202110897718.5A CN115703844A (en) | 2021-08-05 | 2021-08-05 | Preparation method of starch with good compatibility with degradable polyester |
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| CN202110897718.5A CN115703844A (en) | 2021-08-05 | 2021-08-05 | Preparation method of starch with good compatibility with degradable polyester |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3462283A (en) * | 1967-02-28 | 1969-08-19 | Penock & Ford Ltd | Monofunctionally substituted hydrophobic starch and film-forming dispersions prepared therefrom |
| CN106883302A (en) * | 2015-12-15 | 2017-06-23 | 罗门哈斯公司 | The phenyl glycidyl ether adduct of maltodextrin |
| CN111763410A (en) * | 2020-07-17 | 2020-10-13 | 万华化学（宁波）有限公司 | Biodegradable PBAT alloy with high starch content and preparation method thereof |
-
2021
- 2021-08-05 CN CN202110897718.5A patent/CN115703844A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3462283A (en) * | 1967-02-28 | 1969-08-19 | Penock & Ford Ltd | Monofunctionally substituted hydrophobic starch and film-forming dispersions prepared therefrom |
| CN106883302A (en) * | 2015-12-15 | 2017-06-23 | 罗门哈斯公司 | The phenyl glycidyl ether adduct of maltodextrin |
| CN111763410A (en) * | 2020-07-17 | 2020-10-13 | 万华化学（宁波）有限公司 | Biodegradable PBAT alloy with high starch content and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 鄢冬茂 等: "2-羟基-3-丁氧基丙基淀粉的制备", 精细化工, vol. 27, no. 08, pages 809 - 813 * |
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