Composite material capable of slowly releasing antibacterial ingredients, preparation method thereof and antibacterial slow release bag

文档序号：335924 发布日期：2021-12-03 浏览：19次中文

阅读说明：本技术 一种可缓释抗菌成分的复合材料及其制备方法与抗菌缓释袋 (Composite material capable of slowly releasing antibacterial ingredients, preparation method thereof and antibacterial slow release bag ) 是由林志丹熊子涵曹琳于 2021-10-19 设计创作，主要内容包括：本发明涉及抗菌薄膜材料制备技术领域,具体公开了一种可缓释抗菌成分的复合材料及其制备方法与抗菌缓释袋。所述的可缓释抗菌成分的复合材料的制备方法,其通过包含如下步骤的方法制备得到：S11.取多孔吸附材料与抗菌精油混合,得吸附有精油的多孔吸附材料；S12.将吸附有精油的多孔吸附材料与糊化后的淀粉混合,得抗菌缓释材料。由该方法制备得到的可缓释抗菌成分的复合材料可以持续4个月以上释放精油抗菌成分,最好的实施例中,精油抗菌成分的持续释放时间达9个月。进一步地,将本发明所述的可缓释抗菌成分的复合材料包裹在由PET、PE、PA或PP制成的透气薄膜袋中制成抗菌缓释袋,所述的抗菌缓释袋可以被广泛地应用于各种需要抗菌的环境中。(The invention relates to the technical field of preparation of antibacterial film materials, and particularly discloses a composite material capable of slowly releasing antibacterial components, a preparation method thereof and an antibacterial sustained-release bag. The preparation method of the composite material capable of slowly releasing the antibacterial component comprises the following steps: s11, mixing the porous adsorption material with antibacterial essential oil to obtain the porous adsorption material adsorbed with the essential oil; s12, mixing the porous adsorption material adsorbed with the essential oil with the gelatinized starch to obtain the antibacterial slow-release material. The composite material capable of slowly releasing the antibacterial component prepared by the method can release the antibacterial component of the essential oil for more than 4 months, and in the best embodiment, the sustained release time of the antibacterial component of the essential oil reaches 9 months. Furthermore, the composite material capable of slowly releasing the antibacterial component is wrapped in a breathable film bag made of PET, PE, PA or PP to form an antibacterial sustained-release bag, and the antibacterial sustained-release bag can be widely applied to various environments needing antibacterial.)

1. A preparation method of a composite material capable of slowly releasing an antibacterial component is characterized by comprising the following steps:

s11, mixing the porous adsorption material with antibacterial essential oil to obtain the porous adsorption material adsorbed with the essential oil;

s12, mixing the porous adsorption material adsorbed with the essential oil with the gelatinized starch to obtain the composite material capable of slowly releasing the antibacterial component.

2. The preparation method of the composite material capable of slowly releasing the antibacterial component according to claim 1, wherein the dosage ratio of the porous adsorption material to the antibacterial essential oil in the step S11 is 1g: 0.3-0.6 mL;

most preferably, the dosage ratio of the porous adsorption material to the antibacterial essential oil in the step S11 is 1g:0.5 mL;

the porous adsorption material in the step S11 is composed of zeolite powder and kaolin according to the weight ratio of 1-3: 1;

the essential oil in the step S11 is one or a mixture of garlic essential oil and mustard essential oil.

3. The method for preparing the composite material capable of slowly releasing the antibacterial component according to claim 1, wherein the weight ratio of the porous adsorbing material adsorbed with the essential oil to the gelatinized starch in the step S12 is 2-4: 1;

most preferably, the weight ratio of the porous adsorption material with adsorbed essential oil to the gelatinized starch in the step S12 is 3: 1.

4. The method for preparing a composite material capable of slowly releasing an antibacterial ingredient according to claim 1, wherein the gelatinized starch is prepared by the following method: adding corn starch into water, uniformly stirring, and gelatinizing at 70-80 ℃ for 25-40 min to obtain the gelatinized starch.

5. The method for preparing a composite material capable of slowly releasing an antibacterial ingredient according to claim 1, wherein carbon nanotubes are further added in step S12; and mixing the porous adsorption material adsorbed with the essential oil, the gelatinized starch and the carbon nano tubes to obtain the composite material capable of slowly releasing the antibacterial component.

6. The preparation method of the composite material capable of slowly releasing the antibacterial component according to claim 5, wherein the weight ratio of the porous adsorbing material adsorbed with the essential oil to the gelatinized starch and carbon nanotubes is 2-4: 1: 0.03-0.06;

most preferably, the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and the carbon nanotubes is 3:1: 0.05.

7. The method for preparing a composite material capable of slowly releasing an antibacterial component according to claim 6, wherein the carbon nanotubes are modified carbon nanotubes;

the modified carbon nanotube is prepared by the following method: soaking the carbon nano tube in a solution containing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane and 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid for 6-12 h, taking out and drying to obtain the modified carbon nano tube;

wherein the mass fractions of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane in the solution are respectively 3-6%; the mass fractions of the 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid in the solution are respectively 5-10%.

8. The method for preparing a composite material capable of slowly releasing an antibacterial ingredient according to claim 7, wherein the mass fractions of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane in the solution are 5% respectively; the mass fractions of 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid in the solution were 8%, respectively.

9. The composite material capable of slowly releasing the antibacterial component, which is prepared by the preparation method of the composite material capable of slowly releasing the antibacterial component according to any one of claims 1 to 8.

10. An antibacterial sustained-release bag, characterized in that the composite material capable of sustained-release of the antibacterial ingredient according to claim 9 is wrapped in a breathable film bag made of PET, PE, PA or PP or a mixture of two or more thereof.

Technical Field

The invention relates to the technical field of preparation of antibacterial sustained-release materials, in particular to a composite material capable of slowly releasing antibacterial components, a preparation method thereof and an antibacterial sustained-release bag.

Background

The polyethylene film refers to a film prepared from polyethylene resin; it is usually used as a packaging bag, such as a commonly used food bag, a garment bag, etc. The antibacterial film is prepared by adding a certain amount of antibacterial agent into a resin material for preparing the film; inorganic antibacterial agents such as nano silver and nano zinc oxide are usually added to achieve the antibacterial effect.

The garlic essential oil and mustard essential oil are natural products with antibacterial effect; the garlic essential oil or mustard essential oil serving as an antibacterial agent is added into the film material, so that the natural antibacterial effect can be realized, and the film material has a wide application prospect. But the antibacterial film material prepared by directly adding the antibacterial essential oil into the film resin is easy to volatilize quickly, so that the antibacterial effect is not durable; therefore, the technical problem that the antibacterial essential oil is easy to volatilize in the film material is urgently needed to be solved.

Disclosure of Invention

In order to overcome the technical problems in the prior art, the invention provides a composite material capable of slowly releasing an antibacterial component and a preparation method thereof.

The technical scheme of the invention is as follows:

a preparation method of a composite material capable of slowly releasing an antibacterial component is characterized by comprising the following steps:

s11, mixing the porous adsorption material with antibacterial essential oil to obtain the porous adsorption material adsorbed with the essential oil;

s12, mixing the porous adsorption material adsorbed with the essential oil with the gelatinized starch to obtain the composite material capable of slowly releasing the antibacterial component.

The invention adsorbs the antibacterial essential oil in the porous adsorption material for the first time, and then the release time of the essential oil can be effectively prolonged by starch plugging.

Preferably, the using amount ratio of the porous adsorption material to the antibacterial essential oil in the step S11 is 1g: 0.3-0.6 mL.

Most preferably, the dosage ratio of the porous adsorbing material to the antibacterial essential oil in the step S11 is 1g:0.5 mL.

Preferably, the porous adsorption material in the step S11 is composed of zeolite powder and kaolin according to a weight ratio of 1-3: 1.

Preferably, the essential oil in step S11 is selected from one or a mixture of garlic essential oil and mustard essential oil.

Preferably, the weight ratio of the porous adsorbing material with the adsorbed essential oil to the gelatinized starch in the step S12 is 2-4: 1.

Most preferably, the weight ratio of the porous adsorption material with adsorbed essential oil to the gelatinized starch in the step S12 is 3: 1.

Preferably, the gelatinized starch is prepared by the following method: adding corn starch into water, uniformly stirring, and gelatinizing at 70-80 ℃ for 25-40 min to obtain the gelatinized starch.

Preferably, carbon nanotubes are also added in step S12; and mixing the porous adsorption material adsorbed with the essential oil, the gelatinized starch and the carbon nano tubes to obtain the composite material capable of slowly releasing the antibacterial component.

Preferably, the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and carbon nanotubes is 2-4: 1: 0.03-0.06.

Most preferably, the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and the carbon nanotubes is 3:1: 0.05.

Preferably, the carbon nanotube is a modified carbon nanotube;

Preferably, the mass fraction of the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane in the solution is 5 percent respectively; the mass fractions of 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid in the solution were 8%, respectively.

The inventor further studies and finds that,

the antibacterial essential oil is absorbed in a porous absorption material consisting of zeolite powder and kaolin, and then is blocked by gelatinized starch, so that the release time of the essential oil can be effectively prolonged; but the gelatinized starch blocks micropores of the antibacterial slow-release material to a certain extent, so that the release of the antibacterial essential oil is prevented, the antibacterial essential oil cannot be completely released, and the release time of the essential oil cannot be fully prolonged. Based on the problem, the inventor surprisingly found through a large amount of research that: the carbon nano tube is added in the process of preparing the composite material capable of slowly releasing the antibacterial component, so that the release time of the essential oil can be further prolonged.

The invention also provides the composite material capable of slowly releasing the antibacterial component, which is prepared by the preparation method of the composite material capable of slowly releasing the antibacterial component.

The invention also provides an antibacterial sustained-release bag, which is prepared by wrapping the composite material capable of slowly releasing the antibacterial component in a breathable film bag made of PET, PE, PA or PP or a mixture of more than two of the PET, PE, PA and PP.

Has the advantages that: according to the invention, the antibacterial essential oil is adsorbed in the porous adsorption material for the first time, and then starch is used for plugging, so that the prepared composite material capable of slowly releasing the antibacterial component can effectively prolong the release time of the essential oil. Further research by the inventors shows that: the carbon nano tube is added in the process of preparing the composite material capable of slowly releasing the antibacterial component, so that the release time of the essential oil can be further prolonged. The tests of the examples show that the composite material capable of slowly releasing the antibacterial component prepared by the method can release the antibacterial component of the essential oil for more than 4 months, and in the best examples, the sustained release time of the antibacterial component of the essential oil reaches 9 months. Furthermore, the composite material capable of slowly releasing the antibacterial component is wrapped in a breathable film bag made of PET, PE, PA or PP to form an antibacterial sustained-release bag, and the antibacterial sustained-release bag can be widely applied to various environments needing antibacterial.

Detailed Description

The present invention is further explained below with reference to specific examples, which are not intended to limit the present invention in any way.

In the following examples, the carbon nanotubes are multiwalled carbon nanotubes (30-50 nm in diameter and 10-20um in length) produced by Beijing Deke island gold technologies, Inc. under the trade name of CNT 106; other raw materials without marked sources are all products which can be purchased by the technicians in the field through conventional purchasing approaches; the source of the above-mentioned raw materials does not limit the scope of the present invention.

Example 1

S11, mixing zeolite powder and kaolin according to a weight ratio of 2:1 to form a porous adsorption material, and then mixing the porous adsorption material with garlic essential oil to obtain the porous adsorption material adsorbed with the essential oil; the dosage ratio of the porous adsorption material to the antibacterial essential oil is 1g:0.5 mL;

s12, mixing the porous adsorption material adsorbed with the essential oil with the gelatinized starch to obtain a composite material capable of slowly releasing the antibacterial component;

wherein the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch is 3: 1;

in step S12, the gelatinized starch is prepared by the following method: adding corn starch into water, uniformly stirring, and gelatinizing at 75 ℃ for 30min to obtain gelatinized starch; wherein the dosage ratio of the corn starch to the water is 1g:3 mL.

Example 2

s12, mixing the porous adsorption material adsorbed with the essential oil with the gelatinized starch and the carbon nano tubes to obtain a composite material capable of slowly releasing the antibacterial component;

wherein the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and carbon nanotubes is 3:1: 0.05;

Example 2 is different from example 1 in that carbon nanotubes are added in the preparation of the composite material capable of slowly releasing the antibiotic component.

Example 3

s12, mixing the porous adsorption material adsorbed with the essential oil with the gelatinized starch and the modified carbon nano tubes to obtain a composite material capable of slowly releasing the antibacterial component;

wherein the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and the modified carbon nanotubes is 3:1: 0.05;

in step S12, the modified carbon nanotube is prepared by the following method: soaking the carbon nano tube in a DMSO solution containing 5% by mass of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane and 8% by mass of 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid for 8 hours, taking out and drying to obtain the modified carbon nano tube.

Example 3 is different from example 2 in that modified carbon nanotubes are added in the preparation of the composite material capable of slowly releasing the antibiotic component.

Comparative example 1

wherein the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and the modified carbon nanotubes is 3:1: 0.05;

in step S12, the modified carbon nanotube is prepared by the following method: soaking the carbon nano tube in a DMSO solution containing 13% of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane for 8 hours, taking out and drying to obtain the modified carbon nano tube.

Comparative example 1 is different from example 3 in that the modified carbon nanotube is prepared by a different method, and comparative example 1 prepares the modified carbon nanotube by merely soaking the carbon nanotube in a DMSO solution containing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane; in example 3, the carbon nanotubes were immersed in a DMSO solution containing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane and 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid to prepare modified carbon nanotubes.

Comparative example 2

wherein the weight ratio of the porous adsorption material adsorbed with the essential oil to the gelatinized starch and the modified carbon nanotubes is 3:1: 0.05;

s13, uniformly mixing the antibacterial slow-release material with low-density polyethylene resin, and then carrying out melt blending and extrusion by a double-screw extruder to obtain the film material capable of slowly releasing the antibacterial component; the weight ratio of the antibacterial slow-release material to the low-density polyethylene resin is 5: 100, respectively;

in step S12, the modified carbon nanotube is prepared by the following method: soaking the carbon nano tube in a DMSO solution containing 13% of 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid by mass for 8h, taking out and drying to obtain the modified carbon nano tube.

Comparative example 2 is different from example 3 in that the preparation method of the modified carbon nanotube is different, and comparative example 2 prepares the modified carbon nanotube by merely soaking the carbon nanotube in a DMSO solution containing 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid; in example 3, the carbon nanotubes were immersed in a DMSO solution containing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane and 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid to prepare modified carbon nanotubes.

Experimental examples, 100g of each of the composite materials capable of slowly releasing the antibacterial component prepared in examples 1 to 3 and comparative examples 1 to 2 was put into 5 beakers; checking whether each beaker has the smell of the garlic essential oil every 1 month and recording; the results are shown in Table 1.

TABLE 1 film material essential oil slow release time of the invention capable of slow releasing antibacterial component

	Time of slow release of essential oil
		EXAMPLE 1 film Material capable of Slow-Release of antibacterial component	4 months old
EXAMPLE 2 film Material capable of Slow-Release of antibacterial component	6 months old
		EXAMPLE 3 film Material capable of Slow-Release of antibacterial component	9 months old
Comparative example 1 film Material capable of slowly releasing antibacterial ingredient	6 months old
		Comparative example 2 film Material capable of slowly releasing antibacterial ingredient	6 months old

As can be seen from the experimental data in Table 1, the composite material capable of slowly releasing the antibacterial ingredient prepared in example 1 has a long essential oil release time of 4 months.

As can be seen from the experimental data in table 1, the composite material capable of slowly releasing antibacterial components prepared in example 2 has a release time of essential oil of 6 months, which is greatly improved compared with example 1, and this shows that: the carbon nano tube is added in the process of preparing the composite material capable of slowly releasing the antibacterial component, so that the release time of the essential oil can be effectively prolonged.

As can be seen from the experimental data in table 1, the release time of the essential oil of the composite material capable of slowly releasing the antibacterial component prepared in example 3 is 9 months, which is further greatly improved compared with example 2, which indicates that the release time of the essential oil can be further greatly prolonged compared with the addition of the unmodified carbon nanotube when the modified carbon nanotube prepared by the method of the present invention is added in the process of preparing the composite material capable of slowly releasing the antibacterial component.

As can be seen from the experimental data in Table 1, the composite materials capable of slowly releasing the antibacterial component prepared in comparative examples 2 and 3 have the essential oil release time of 6 months, which is equivalent to that of example 2 and is greatly smaller than that of example 3; this indicates that: the modification method of the modified carbon nanotube is very critical; the release time of the essential oil of the prepared composite material capable of slowly releasing the antibacterial component can be greatly prolonged only by soaking the carbon nano tube in a DMSO solution containing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane and 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid to prepare the modified carbon nano tube; the preparation of modified carbon nanotubes by merely soaking carbon nanotubes in a DMSO solution containing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane or 2-amino-3- (4-hydroxy-3-methoxyphenyl) propionic acid does not improve the release time of essential oil from the prepared composite material capable of slowly releasing the antibacterial component.

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Composite material capable of slowly releasing antibacterial ingredients, preparation method thereof and antibacterial slow release bag

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