CN113150393A - Preparation method of intercalated modified montmorillonite/cassava starch composite film - Google Patents
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Abstract
The invention discloses a preparation method of an intercalation modified montmorillonite/cassava starch composite film. The method mainly comprises the steps of preparing an organic modified montmorillonite material by using natural montmorillonite and Dodecyl Trimethyl Ammonium Chloride (DTAC) as raw materials, preparing an intercalation modified montmorillonite and cassava starch composite film by a pouring forming method, and preparing the following raw materials in parts by weight: organic montmorillonite: 15-20 parts of a solvent; magnetic organic montmorillonite: 25-100 parts; distilled water: 100-150 parts; cassava starch: 5-10 parts of glycerol: 15-30 parts; absolutely dry montmorillonite: 15-100 parts; distilled water: 400-600 parts; dodecyl trimethyl ammonium chloride: 30-90 parts of intercalated modified montmorillonite and cassava starch composite film is synthesized by the scheme. The invention simultaneously explores the condition of taking the ultrasonic condition as the organic modification of the montmorillonite for the first time, and explores the improvement of the barrier property of the montmorillonite-cassava starch composite film which takes the intercalation reaction as the main body.
Description
The technical field is as follows:
the invention belongs to the technical field of composite film preparation, and particularly relates to a preparation method of an intercalation modified montmorillonite/cassava starch composite film.
Background art:
montmorillonite (MMT) is the main component of bentonite ore, has a unique layered structure, has the advantages of good expansibility, water absorbability, adsorbability, barrier property, flame retardance, thermal stability and the like, is particularly rich in resources and low in price, can be used in various fields of light industry, petroleum, coating, building, desert control, sewage treatment and the like, and is known as an 'all-purpose material' by people. Even a small amount of montmorillonite is added into the polymer material, the barrier property of the composite material can be obviously improved, and the montmorillonite is often used as a reinforcing agent of the barrier property of the polymer material in the preparation of the polymer material. In the age of widely utilizing montmorillonite, the montmorillonite is active in chemical property and can be used as a surfactant and the like, but the improvement of the barrier property of a high polymer material is invisible, the excellent barrier effect is achieved with the minimum addition amount, the introduction amount of the material is reduced, and the montmorillonite-montmorillonite composite material is also an idea of green and environment-friendly packaging.
As tuber plants, cassava, sweet potato, yam and the like have high starch content, the cassava starch extracted by cassava is the most important economic conversion form in Guangxi region at present, the economic benefit brought by the cassava starch is removed, the cassava residue which is a product obtained by extracting the cassava starch has strong economic utility, and the cassava residue can be continuously fermented to prepare industrial products such as ethanol and methane and can also be used as feed, fungus culture medium and other substances for secondary utilization. Tapioca starch and its derived products have become one of the six major economic shores in Guangxi.
The montmorillonite and the cassava starch in Guangxi province are combined, so that the additive with sufficient yield can enhance the biomass packaging material prepared from abundant local raw materials, resources are reasonably utilized, the additive is organic and environment-friendly, local industrial economy is improved, production cost is properly reduced, and the additive is green and pollution-free and has a use prospect. Therefore, the invention takes the cassava starch as the raw material for the first time, takes the dodecyl trimethyl ammonium chloride modified montmorillonite as the modifier, and adopts the pouring forming method to prepare the intercalation modified montmorillonite starch composite film.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an intercalation modified montmorillonite/cassava starch composite film, which has a simple preparation process. The addition of the dodecyl trimethyl ammonium chloride can carry out organic modification on the montmorillonite, the intercalation effect is obviously changed, and the interlayer distance of the montmorillonite is increased; the starch composite film prepared by the invention has smooth surface and good appearance; the mechanical property is improved, the oxygen resistance is improved, and the improvement of the barrier property of the starch composite film is proved.
The invention solves the technical problems by the following technical scheme:
the invention relates to a preparation method of an intercalation modified montmorillonite/cassava starch composite film. The traditional Chinese medicine is prepared from the following raw materials in parts by weight: organic montmorillonite: 15-20 parts of a solvent; magnetic organic montmorillonite: 25-100 parts; distilled water: 100-150 parts; cassava starch: 5-10 parts of glycerol: 15-30 parts; absolutely dry montmorillonite: 15-100 parts; distilled water: 400-600 parts; dodecyl Trimethyl Ammonium Chloride (DTAC): 30-90 parts;
the preparation method comprises the following operation steps:
s1 drying: drying montmorillonite in 50 deg.C air-blast drying oven, and cooling in drying dish to obtain oven-dried montmorillonite
S2 preparation of montmorillonite suspension: weighing 15-100 parts of oven-dried montmorillonite, pouring into 400-600 parts of distilled water, and magnetically stirring to completely fuse with the water. Ultrasonically dispersing at room temperature, and magnetically stirring to obtain montmorillonite suspension.
Modification of S3: and (3) adding 30-90 parts of dodecyl trimethyl ammonium chloride into the montmorillonite suspension prepared in the step S2, fully and uniformly stirring the mixture until the medicine is dissolved, reacting the mixture under an ultrasonic condition, and then carrying out water bath magnetic stirring. After the solution was cooled to room temperature while stirring, the solution was again sonicated, and the precipitate in the solution was centrifuged. Washing the precipitate with ethanol solution until no Cl-, drying under a forced air drying oven, grinding the dried montmorillonite, and sieving with a 120-mesh sieve to obtain the modified dodecyl trimethyl ammonium chloride.
S4 preparation of organic montmorillonite suspension: placing dodecyl ammonium chloride obtained in the step of S3 modification into a three-neck flask, adding distilled water, stirring overnight, and stirring for 12h to form an organic montmorillonite suspension
S5, drying: ultrasonically dispersing the suspension obtained in the step of preparing the organic montmorillonite suspension from S4 for 30min, and adding FeCl3And FeCl2Dissolving in 100ml of water, quickly pouring the solution into a flask with air exhausted, uniformly stirring, adjusting the pH value of the mixed solution to 11 by using a NaOH solution, magnetically stirring in a water bath at 80 ℃, continuing to perform ultrasonic dispersion after stopping stirring, performing magnetic separation on the obtained product, cleaning black precipitate for multiple times, and drying the obtained precipitate in a vacuum drying oven at 50 ℃.
S6 preparation of magnetic montmorillonite suspension: and (3) placing 25-100 parts of the magnetic montmorillonite obtained in the step of drying S5 into a three-neck flask, adding 100-150 parts of distilled water, performing ultrasonic treatment, and mechanically stirring to form a magnetic organic montmorillonite suspension.
S7 film formation: adding 5-10 parts of cassava starch, 15-30 parts of glycerol and 100-150 parts of water into the montmorillonite suspension, uniformly stirring, heating in a water bath and mechanically stirring, stopping heating and continuously stirring to room temperature. And (4) performing ultrasonic treatment to obtain the magnetic starch montmorillonite film-forming solution. Pouring the film forming liquid into a square plastic culture dish, and drying the disordered material in a drying oven; the ordered material is naturally air-dried in parallel magnetic induction lines generated by strong magnetism, and is air-dried at 50 ℃.
The beneficial effects of the invention are as follows:
the invention carries out organic modification of the montmorillonite by changing the ultrasonic condition for the first time, and carries out intercalation reaction on the montmorillonite while carrying out the organic modification, thereby further exploring the barrier property of the composite film, wherein the montmorillonite has hydroxyl and absorbs water together with the water absorption hydroxyl of the starch film, so that the moisture permeability of the montmorillonite is increased, and the moisture permeability of the montmorillonite is gradually reduced along with the increase of the consumption of the montmorillonite. The moisture permeability of the composite film is slightly reduced along with the increase of the addition amount of the magnetic montmorillonite, and the magnetic montmorillonite has larger mass and is influenced by magnetism to form the montmorillonite starch film with a single direction, so that the path is infinite and tends to be optimal, the longest path is obtained, and the optimal barrier property of the montmorillonite starch film is obtained. Compared with the ordered starch film, the ordered magnetic montmorillonite material starch film has the advantages that the ordered starch film is faster and more stable to achieve a constant gas barrier effect, and the barrier property of the montmorillonite starch film can be effectively improved by introducing the Fe.
Drawings
FIG. 1 is a contact angle diagram of the intercalation modified montmorillonite/tapioca starch composite film of the invention
FIG. 2 is an XRD pattern of an intercalated modified montmorillonite/tapioca starch composite film
FIG. 3 is a graph showing the tendency of montmorillonite added in different amounts to affect the oxygen permeability of a starch film; the curves I, II and III are respectively organic montmorillonite (OMMT), iron ordered intercalated organic montmorillonite (Fe-OMMT-Y) and iron modified organic montmorillonite (Fe-OMMT).
FIG. 4 is a graph showing the influence of montmorillonite in different addition amounts on the moisture permeability of a starch film; the curves I, II and III are respectively organic montmorillonite (OMMT), iron ordered intercalated organic montmorillonite (Fe-OMMT-Y) and iron modified organic montmorillonite (Fe-OMMT).
The specific implementation mode is as follows:
in the raw materials prepared by the invention, cassava starch and montmorillonite are used as main materials, glycerol and Dodecyl Trimethyl Ammonium Chloride (DTAC) are used as auxiliary agents, and the main materials and the auxiliary agents are prepared from the following raw materials in parts by weight: organic montmorillonite: 15-20 parts of a solvent; magnetic organic montmorillonite: 25-100 parts; distilled water: 100-150 parts; cassava starch: 5-10 parts of glycerol: 15-30 parts; absolutely dry montmorillonite: 15-100 parts; distilled water: 400-600 parts; dodecyl trimethyl ammonium chloride: 30-90 parts;
the following are specific examples of the present invention
Example 1:
the required raw materials are as follows according to the weight portion: organic montmorillonite: 20 parts of magnetic organic montmorillonite: 25 parts of (1); distilled water: 150 parts; cassava starch: 5 parts, glycerol: 15 parts of (1); absolutely dry montmorillonite: 30 parts of (1); distilled water: 600 parts of water; dodecyl Trimethyl Ammonium Chloride (DTAC): 30 parts of (1);
s1 drying: drying montmorillonite in a forced air drying oven at 50 ℃ for 24h, placing the dried montmorillonite in a drying dish, and cooling to obtain absolutely dried montmorillonite S2 to prepare montmorillonite suspension: 30 parts of oven-dried montmorillonite prepared in the step S1 is weighed, poured into 600 parts of distilled water, and stirred for 1 hour by magnetic force to be completely fused with the water. Ultrasonically dispersing for 1h at room temperature, and magnetically stirring for 12h (500r/min) to obtain montmorillonite suspension for later use.
Modification of S3: and (3) adding 30 parts of dodecyl trimethyl ammonium chloride into the montmorillonite suspension prepared in the step (S2), fully stirring the mixture until the medicine is completely dissolved, reacting the mixture for 1 hour under the ultrasonic condition, and then carrying out magnetic stirring for 3 hours in a water bath at the temperature of 80 ℃. After cooling the solution to room temperature with stirring, sonication was again carried out for 1 hour, and the precipitate in the solution was centrifuged (7000rpm, 10 min). The precipitate was washed with 50% ethanol solution to Cl- (0.2 mol/LAgNO was used)3Detecting the solution until no precipitate exists), drying for 24h at 50 ℃ in an air drying oven, grinding the dried montmorillonite, and sieving with a 120-mesh sieve to obtain the modified dodecyl trimethyl ammonium chloride (1-1 DTAC).
S4 preparation of organic montmorillonite suspension: and (3) putting 20 parts of (1-2D) organic montmorillonite obtained after the S3 modification step into a three-neck flask, adding 200 parts of distilled water, stirring overnight and stirring for 12 hours to form an organic montmorillonite suspension.
S5, drying: ultrasonically dispersing the suspension obtained in the step S4 for 30min, introducing argon into the device, exhausting the air in the flask, and adding 0.01mol of FeCl3And 0.005mol FeCl2Dissolving in 100 parts of water, quickly pouring the solution into a flask with air exhausted, uniformly stirring, adjusting the pH value of the mixed solution to 11 by using 0.2mol/L NaOH solution, magnetically stirring for 1h in water bath at 80 ℃, continuing to perform ultrasonic dispersion for 30min after stopping stirring, performing magnetic separation on the obtained product, washing black precipitate with distilled water for multiple times, and drying the obtained precipitate for 24h at 50 ℃ in a vacuum drying oven.
S6 preparation of magnetic montmorillonite suspension: introducing argon into the three-neck flask to completely exhaust air in the three-neck flask, taking 25 parts of modified montmorillonite, placing the modified montmorillonite into the three-neck flask, adding 50 parts of distilled water, performing ultrasonic treatment for 1 hour, and mechanically stirring for 12 hours to form a magnetic organic montmorillonite suspension.
S7 film formation: adding 5 parts of cassava starch, 15 parts of glycerol and 100 parts of water into the montmorillonite suspension, uniformly stirring, heating in a water bath at 80 ℃, mechanically stirring for 30min, stopping heating, and continuously stirring to room temperature. And (5) performing ultrasonic treatment for 30min to obtain the magnetic starch montmorillonite film-forming solution. Pouring 48 parts of the film forming solution into a square plastic culture dish with the thickness of 12 x 12cm, and drying the disordered material in a drying oven at the temperature of 50 ℃ for 10 hours; the ordered material is naturally air-dried in parallel magnetic induction lines generated by strong magnetism for 24 hours, and is air-dried for 1 hour at 50 ℃.
Example 2:
the required raw materials are as follows according to the weight portion: organic montmorillonite: 20 parts of magnetic organic montmorillonite: 50 parts of a mixture; distilled water: 150 parts; cassava starch: 5 parts, glycerol: 15 parts of (1); absolutely dry montmorillonite: 30 parts of (1); distilled water: 600 parts of water; dodecyl Trimethyl Ammonium Chloride (DTAC): 60 parts;
s1 drying: drying montmorillonite in a forced air drying oven at 50 ℃ for 24h, placing the dried montmorillonite in a drying dish, and cooling to obtain absolutely dried montmorillonite S2 to prepare montmorillonite suspension: 30 parts of oven-dried montmorillonite prepared in the step S1 is weighed, poured into 600 parts of distilled water, and stirred for 1 hour by magnetic force to be completely fused with the water. Ultrasonically dispersing for 1h at room temperature, and magnetically stirring for 12h (500r/min) to obtain montmorillonite suspension for later use.
Modification of S3: and adding 60 parts of dodecyl trimethyl ammonium chloride into the montmorillonite suspension prepared in the step S2, fully stirring the mixture until the medicine is completely dissolved, reacting the mixture for 1 hour under the ultrasonic condition, and performing magnetic stirring for 3 hours in a water bath at the temperature of 80 ℃. After cooling the solution to room temperature with stirring, sonication was again carried out for 1 hour, and the precipitate in the solution was centrifuged (7000rpm, 10 min). The precipitate was washed with 50% ethanol solution to Cl- (0.2 mol/LAgNO was used)3Detecting the solution until no precipitate exists), drying for 24h at 50 ℃ in an air drying oven, grinding the dried montmorillonite, and sieving with a 120-mesh sieve to obtain the modified dodecyl trimethylAmmonium chloride (1-1 DTAC).
S4 preparation of organic montmorillonite suspension: and (3) putting 20 parts of (1-2D) organic montmorillonite obtained after the S3 modification step into a three-neck flask, adding 200 parts of distilled water, stirring overnight and stirring for 12 hours to form an organic montmorillonite suspension.
S5, drying: ultrasonically dispersing the suspension obtained in the step S4 for 30min, introducing argon into the device, exhausting the air in the flask, and adding 0.01mol of FeCl3And 0.005mol FeCl2Dissolving in 100 parts of water, quickly pouring the solution into a flask with air exhausted, uniformly stirring, adjusting the pH value of the mixed solution to 11 by using 0.2mol/L NaOH solution, magnetically stirring for 1h in water bath at 80 ℃, continuing to perform ultrasonic dispersion for 30min after stopping stirring, performing magnetic separation on the obtained product, washing black precipitate with distilled water for multiple times, and drying the obtained precipitate for 24h at 50 ℃ in a vacuum drying oven.
S6 preparation of magnetic montmorillonite suspension: introducing argon into the three-neck flask to completely exhaust air in the three-neck flask, taking 50 parts of modified montmorillonite, placing the modified montmorillonite into the three-neck flask, adding 50 parts of distilled water, performing ultrasonic treatment for 1 hour, and mechanically stirring for 12 hours to form a magnetic organic montmorillonite suspension.
S7 film formation: adding 5 parts of cassava starch, 15 parts of glycerol and 100 parts of water into the montmorillonite suspension, uniformly stirring, heating in a water bath at 80 ℃, mechanically stirring for 30min, stopping heating, and continuously stirring to room temperature. And (5) performing ultrasonic treatment for 30min to obtain the magnetic starch montmorillonite film-forming solution. Pouring 48 parts of the film forming solution into a square plastic culture dish with the thickness of 12 x 12cm, and drying the disordered material in a drying oven at the temperature of 50 ℃ for 10 hours; the ordered material is naturally air-dried in parallel magnetic induction lines generated by strong magnetism for 24 hours, and is air-dried for 1 hour at 50 ℃.
Example 3:
the required raw materials are as follows according to the weight portion: organic montmorillonite: 20 parts of magnetic organic montmorillonite: 75 parts of a mixture; distilled water: 150 parts; cassava starch: 5 parts, glycerol: 15 parts of (1); absolutely dry montmorillonite: 30 parts of (1); distilled water: 600 parts of water; dodecyl Trimethyl Ammonium Chloride (DTAC): 90 parts of a mixture;
s1 drying: drying montmorillonite in a forced air drying oven at 50 ℃ for 24h, placing the dried montmorillonite in a drying dish, and cooling to obtain absolutely dried montmorillonite S2 to prepare montmorillonite suspension: 30 parts of oven-dried montmorillonite prepared in the step S1 is weighed, poured into 600 parts of distilled water, and stirred for 1 hour by magnetic force to be completely fused with the water. Ultrasonically dispersing for 1h at room temperature, and magnetically stirring for 12h (500r/min) to obtain montmorillonite suspension for later use.
Modification of S3: and (3) adding 90 parts of dodecyl trimethyl ammonium chloride into the montmorillonite suspension prepared in the step (S2), fully stirring the mixture until the medicine is completely dissolved, reacting the mixture for 1 hour under the ultrasonic condition, and then carrying out magnetic stirring for 3 hours in a water bath at the temperature of 80 ℃. After cooling the solution to room temperature with stirring, sonication was again carried out for 1 hour, and the precipitate in the solution was centrifuged (7000rpm, 10 min). The precipitate was washed with 50% ethanol solution to Cl- (0.2 mol/LAgNO was used)3Detecting the solution until no precipitate exists), drying for 24h at 50 ℃ in an air drying oven, grinding the dried montmorillonite, and sieving with a 120-mesh sieve to obtain the modified dodecyl trimethyl ammonium chloride (1-1 DTAC).
S4 preparation of organic montmorillonite suspension: and (3) putting 75 parts of (1-2D) organic montmorillonite obtained in the S3 modification step into a three-neck flask, adding 200 parts of distilled water, stirring overnight, and stirring for 12 hours to form an organic montmorillonite suspension.
S5, drying: ultrasonically dispersing the suspension obtained in the step S4 for 30min, introducing argon into the device, exhausting the air in the flask, and adding 0.01mol of FeCl3And 0.005mol FeCl2Dissolving in 100 parts of water, quickly pouring the solution into a flask with air exhausted, uniformly stirring, adjusting the pH value of the mixed solution to 11 by using 0.2mol/L NaOH solution, magnetically stirring for 1h in water bath at 80 ℃, continuing to perform ultrasonic dispersion for 30min after stopping stirring, performing magnetic separation on the obtained product, washing black precipitate with distilled water for multiple times, and drying the obtained precipitate for 24h at 50 ℃ in a vacuum drying oven.
S6 preparation of magnetic montmorillonite suspension: introducing argon into the three-neck flask to completely exhaust air in the three-neck flask, taking 75 parts of modified montmorillonite, placing the modified montmorillonite into the three-neck flask, adding 50 parts of distilled water, performing ultrasonic treatment for 1 hour, and mechanically stirring for 12 hours to form a magnetic organic montmorillonite suspension.
S7 film formation: adding 5 parts of cassava starch, 15 parts of glycerol and 100 parts of water into the montmorillonite suspension, uniformly stirring, heating in a water bath at 80 ℃, mechanically stirring for 30min, stopping heating, and continuously stirring to room temperature. And (5) performing ultrasonic treatment for 30min to obtain the magnetic starch montmorillonite film-forming solution. Pouring 48 parts of the film forming solution into a square plastic culture dish with the thickness of 12 x 12cm, and drying the disordered material in a drying oven at the temperature of 50 ℃ for 10 hours; the ordered material is naturally air-dried in parallel magnetic induction lines generated by strong magnetism for 24 hours, and is air-dried for 1 hour at 50 ℃.
The above description should not be taken as limiting the invention to the embodiments, but rather, as will be apparent to those skilled in the art to which the invention pertains, numerous simplifications or substitutions may be made without departing from the spirit of the invention, which shall be deemed to fall within the scope of the invention as defined by the claims appended hereto.
Claims (5)
1. The preparation method of the intercalated modified montmorillonite/cassava starch composite film is characterized by comprising the following raw materials in parts by weight: organic montmorillonite: 15-20 parts of a solvent; magnetic organic montmorillonite: 25-100 parts; distilled water: 100-150 parts; cassava starch: 5-10 parts of glycerol: 15-30 parts; absolutely dry montmorillonite: 15-100 parts; distilled water: 400-600 parts; dodecyl trimethyl ammonium chloride: 30-90 parts;
the preparation method comprises the following operation steps:
s1 drying: drying montmorillonite in a forced air drying oven, and cooling in a drying dish to obtain oven-dried montmorillonite;
s2 preparation of montmorillonite suspension: weighing the oven-dried montmorillonite obtained in the step S1, pouring the oven-dried montmorillonite into distilled water, and magnetically stirring to completely fuse the montmorillonite with the water; carrying out ultrasonic dispersion and magnetic stirring at room temperature to obtain montmorillonite suspension;
modification of S3: adding dodecyl trimethyl ammonium chloride into the montmorillonite suspension obtained in the step S2, stirring at room temperature, performing ultrasonic dispersion, performing water bath stirring on the mixture, cooling to room temperature, performing ultrasonic dispersion again, and centrifuging precipitates in the solution; washing, drying, grinding and sieving the precipitate to obtain the organic modified montmorillonite;
s4 preparation of organic montmorillonite suspension: adding distilled water into the organic montmorillonite obtained in the step S3, and stirring to form an organic montmorillonite suspension;
s5, drying: ultrasonically dispersing the suspension prepared in the step S4, dissolving FeCl3 and FeCl2 in water, quickly pouring the solution into a flask with air exhausted, uniformly stirring, adjusting the pH value of the mixed solution by using a NaOH solution, and carrying out water bath; magnetic stirring, ultrasonic dispersing, magnetic separating, cleaning and drying the product;
s6 preparation of magnetic montmorillonite suspension: weighing the magnetic montmorillonite dried in the step S5, adding distilled water, and performing ultrasonic treatment; mechanically stirring; obtaining a suspension;
s7 film formation: adding cassava starch, glycerol and water into the magnetic montmorillonite suspension obtained in the step S6, uniformly stirring, carrying out water bath heating and mechanical stirring, carrying out ultrasonic treatment to obtain a film forming solution, pouring the film forming solution into a culture dish, and drying to obtain the composite film.
2. The method for preparing the intercalated modified montmorillonite/tapioca starch composite film according to claim 1, wherein the modification centrifugation in step S3 is 7000rpm/10min, and the washing is carried out by using 50% ethanol solution until no Cl is formed-。
3. The method for preparing an intercalated modified montmorillonite/tapioca starch composite film according to claim 1, wherein when preparing the organic montmorillonite in the step of S4, drying for 24h at 50 ℃ in a forced air drying oven, grinding the dried montmorillonite, and sieving with a 120-mesh sieve.
4. The preparation method of the intercalated modified montmorillonite/tapioca starch composite film according to claim 1, wherein the concentration of NaOH solution used in the S5 drying step is 0.2mol/L, and the pH is adjusted to 11.
5. The method for preparing the intercalated modified montmorillonite/tapioca starch composite film according to claim 1, wherein in the step of S7 film formation, water bath heating at 80 ℃ is required and mechanical stirring is required for 30min, and the culture dish is 12 x 12cm square plastic.
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| CN115448794A (en) * | 2022-09-20 | 2022-12-09 | 安徽司尔特化肥科技有限公司 | Preparation and coating method of controlled-release fertilizer coating material |
| EP4279469A1 (en) * | 2022-05-16 | 2023-11-22 | Mühl Engineering Systems GmbH | Mineral fabric |
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