阅读说明：本技术 一种大麻二酚整理液及大麻二酚功能面料的整理工艺 (Cannabidiol finishing liquid and finishing process of cannabidiol functional fabric ) 是由 陈义亮 周绚丽 韩翠翠 刘慧� 解晓明 于 2021-09-23 设计创作，主要内容包括：本申请涉及一种大麻二酚整理液及大麻二酚功能面料的整理工艺,属于功能性面料整理技术的领域,大麻二酚整理液包括以下组分：CBD微胶囊、交联剂、渗透剂和水,其中,CBD微胶囊从内向外依次为CBD芯材、内包覆层和外包覆层。上述大麻二酚整理液用于大麻二酚功能面料的整理工艺包括以下步骤：S1、整理液配置；S2、整理；S3、后处理。本申请中的大麻二酚具有活性成分CBD稳定性高的效果。(The application relates to a cannabidiol finishing liquid and a finishing process of cannabidiol functional fabric, belonging to the field of functional fabric finishing technology, wherein the cannabidiol finishing liquid comprises the following components: the CBD core material comprises CBD microcapsules, a cross-linking agent, a penetrating agent and water, wherein the CBD microcapsules sequentially comprise a CBD core material, an inner coating layer and an outer coating layer from inside to outside. The finishing process of the cannabidiol finishing liquid for the cannabidiol functional fabric comprises the following steps: s1, preparing finishing liquid; s2, finishing; and S3, post-processing. The cannabidiol in the application has the effect of high stability of the active ingredient CBD.)

1. A cannabidiol finishing liquid is characterized in that: the composite material comprises the following components in percentage by mass:

5-8% of CBD microcapsules;

1.5-2% of a cross-linking agent;

0.2 to 0.5 percent of penetrating agent;

supplementing water to 100%;

the CBD microcapsule comprises a CBD core material, an inner coating layer and an outer coating layer from inside to outside in sequence.

2. A cannabidiol finishing liquor according to claim 1, characterised in that: the CBD core material at least comprises the following raw materials in parts by mass:

3. a cannabidiol finishing liquor according to claim 2, characterised in that: the reducing agent is a mixture of polyethylene glycol and zinc pyrrolidone carboxylate, and the mass ratio of the polyethylene glycol: zinc pyrrolidone carboxylate is (10-12): (0.2-0.4).

4. A cannabidiol finishing liquor according to claim 3, characterised in that: the polyethylene glycol is PEG-1000 and PEG-1500 according to the mass ratio of 1: (0.37-0.40).

5. A cannabidiol finishing liquor according to any one of claims 2 to 4, characterised in that: the inner coating layer at least comprises the following raw materials in parts by mass:

6. a cannabidiol finishing liquor according to claim 5, characterised in that: the outer coating layer at least comprises the following raw materials in parts by mass:

100 portions of 2wt percent chitosan solution and 110 portions;

200 portions and 210 portions of 0.25wt percent fucoidan solution;

0.5-1 part of crosslinking component.

7. A cannabidiol finishing liquor according to claim 6, characterised in that: the crosslinking component is a mixture of tannic acid and citric acid, and the mass ratio of tannic acid: citric acid is 1: 1.

8. a cannabidiol finishing liquor according to claim 7, characterised in that: the CBD microcapsule is prepared by the following process:

a1, preparing a CBD core material, adding CBD and a reducing agent into water according to a ratio, performing ultrasonic dispersion, performing homogeneous dispersion, adding lysine after the homogeneous dispersion, and further performing the homogeneous dispersion to obtain the CBD core material;

a2, preparing an inner coating layer, namely putting fucoidan, glycerol and gelatin into water according to the proportion, heating and stirring to completely dissolve the materials to obtain an inner membrane liquid, then mixing the inner membrane liquid with the CBD core material obtained in the step A1, performing ultrasonic dispersion, performing homogeneous dispersion, and obtaining a crude product after the homogeneous dispersion;

a3, preparing an outer coating layer, mixing a chitosan solution and an algin solution according to a ratio, stirring and dispersing after mixing, dripping a crosslinking component after uniform dispersion, further stirring and dispersing to obtain an outer membrane solution, immediately adding the outer membrane solution into the crude product obtained in the step A2, then homogenizing and dispersing to obtain a microcapsule emulsion;

and A4, spray drying, namely spray drying the microcapsule emulsion obtained in the step A3 to obtain the CBD microcapsule.

9. A cannabidiol finishing liquor according to claim 1, characterised in that: the cross-linking agent is a mixture of dopamine hydrochloride and zinc acetylacetonate in equal mass ratio.

10. A finishing process of a cannabidiol functional fabric is characterized in that: the method comprises the following process steps:

s1, preparing a finishing liquid, dissolving the CBD microcapsules, the cross-linking agent and the penetrating agent into water according to the proportion of any one of claims 1 to 9, and uniformly stirring to obtain the cannabidiol finishing liquid;

s2, finishing, namely putting the combed cotton fabric into the cannabidiol finishing liquid obtained in the step S1, and vibrating at the temperature of 80-85 ℃ to obtain finished grey cloth;

and S3, post-processing, namely washing and drying the finished grey cloth obtained in the step S2 in sequence to obtain the cannabidiol functional fabric.

Technical Field

The application relates to the field of functional fabric finishing, in particular to a cannabidiol finishing liquid and a cannabidiol functional fabric finishing process.

Background

Hemp has been planted in China for over five thousand years and is one of the earliest crops. Cannabis sativa contains Tetrahydrocannabinol (THC) as an active ingredient which can cause addiction to humans, and is classified as one of three drug source plants. However, not all cannabis is narcotic cannabis, and depending on the THC content of addictive components in the cannabis plant, cannabis with THC contents higher than 0.3% are called narcotic cannabis, while cannabis with THC contents lower than 0.3% are generally called industrial cannabis, also called hemp and cannabis.

China-hemp is the earliest natural fiber used for fabrics by human beings, cellulose has the reputation of 'the king of natural fiber', and China-hemp fabrics have the advantages of moisture absorption, air permeability, comfort, heat dissipation, mildew resistance, bacteriostasis, radiation resistance, ultraviolet resistance, sound absorption and the like. However, the hemp fabric is similar to flax fiber, has poor skin-friendly property and higher hardness, and is comparatively prickled, so the hemp fabric is not suitable for being used as underwear and bedding fabrics. Due to the characteristics of the fibrilia, the skin-friendly effect of the pure cotton fabric is difficult to achieve even if the treatments such as softening finishing and the like are carried out. Therefore, how to combine the advantages of the hemp fabric with the advantages of the pure cotton fabric, or how to make the pure cotton fabric have the advantages of the hemp fabric, is the next grinding heating point.

Due to the intrinsic defect of the fibrilia, the fabric obtained by blending even if the cotton fiber and the fibrilia are blended often cannot achieve good skin-friendly performance, so that the more suitable method is to arrange the active ingredients in the fibrilia on the pure cotton fabric, so that the pure cotton fabric has the excellent performance of the fibrilia, and the problem of poor skin-friendly performance of the fibrilia is solved.

The hemp contains various active ingredients, wherein the high content of Cannabidiol (CBD) and THC. Unlike THC, CBD has no addiction, and CBD has good anti-inflammatory, antibacterial and antioxidant effects usually possessed by general plant components, and also has a soothing and tranquilizing effect which is usually not possessed by general plant components, so that CBD has good relieving and sleep-helping effects.

Recent studies have found that the side effects of improving sleep through the human body's own endocannabinoid system are almost negligible compared to general hypnotic drugs. Cannabinoid receptors are widely distributed in various organs and tissues of the human body, and can combine with endogenous cannabinoids produced in the body to play a role in helping sleep. CBD is easy to be absorbed by human cannabinoid receptors, so that the transdermal absorption rate is higher, and the CBD can play a good role in helping sleep. Therefore, a new sleep-aiding idea is provided for sleep-aiding bedding, sleep-aiding pajamas and the like.

However, CBD is easily deactivated by oxidation, acid, alkali, etc. and is not easily soluble in water, which makes it difficult to prepare CBD directly into a finishing liquor for cotton fabric, and the market is still blank for how to prepare CBD into a finishing liquor with higher stability.

Disclosure of Invention

In order to overcome the defect that the CBD is not easy to prepare and obtain the finishing liquid with high stability, the application provides the cannabidiol finishing liquid and the finishing process of the cannabidiol functional fabric.

The technical scheme adopted by the application is as follows:

in a first aspect, the application provides a cannabidiol finishing liquid, which adopts the following technical scheme:

the cannabidiol finishing liquid comprises the following components in percentage by mass:

5-8% of CBD microcapsules;

1.5-2% of a cross-linking agent;

0.2 to 0.5 percent of penetrating agent;

supplementing water to 100%;

the CBD microcapsule comprises a CBD core material, an inner coating layer and an outer coating layer from inside to outside in sequence.

By adopting the technical scheme, the cannabidiol (namely CBD) is not acid-resistant, alkali-resistant and oxidation-resistant, if the CBD is directly prepared into finishing liquor, the CBD fails in the finishing process due to various reasons, and the CBD cannot exert corresponding effects even if being finished on the fabric. Specifically, the CBD is prepared into a double-layer coated microcapsule, so that the possibility of CBD inactivation can be remarkably reduced.

Compared with common single-layer and three-layer or more microcapsules, the double-layer microcapsules are more suitable for being used as bedding or pajamas in terms of strength, toughness, tightness and other properties. If the microcapsule wall is too thin, the microcapsule wall is easy to break in the finishing process, so that the loss of CBD is caused, and even if the single-layer microcapsule is finished on the fabric, the damage of the microcapsule wall is easily caused in the processes of garment making and transportation of the fabric, so that the loss of CBD is caused. If the wall of the microcapsule is too thick, the overall strength of the microcapsule is too high and the microcapsule is not easy to break and CBD is not easy to release and take effect when a consumer actually uses the fabric finished with the microcapsule.

Optionally, the CBD core material at least comprises the following raw materials in parts by mass:

by adopting the technical scheme, because the CBD is not oxidation-resistant, the reducing agent is added into the CBD core material, so that the possibility that the CBD is oxidized by dissolved oxygen in the material and oxygen in the air in the microcapsule preparation process can be reduced. Lysine is a basic amino acid that is positively charged due to its two primary amine groups, whereas the CBD has two phenol groups, somewhat negatively charged. In the emulsification process of the CBD core material, lysine can be attracted by the micro-emulsion droplets with certain negative charges and attached to the surfaces of the micro-emulsion droplets, so that the surfaces of the micro-emulsion droplets are provided with certain positive charges, and adjacent micro-emulsion droplets repel each other due to the positive charges, so that emulsion breaking and aggregation are not easy to occur, and the stability of a system is improved.

Optionally, the reducing agent is a mixture of polyethylene glycol and zinc pyrrolidone carboxylate, and the mass ratio of polyethylene glycol: zinc pyrrolidone carboxylate is (10-12): (0.2-0.4).

By adopting the technical scheme, no matter polyethylene glycol or zinc pyrrolidone carboxylate has certain reducibility, and the possibility of oxidation of CBD can be reduced.

Furthermore, polyethylene glycol is a good thickening agent and can play a role in stabilizing suspension of the whole system, so that the stability of the whole system is improved. In addition, the polyethylene glycol is a good phase-change material, the CBD core material is solid at room temperature only by controlling the molecular weight of the polyethylene glycol, and the CBD core material can be liquid only when the temperature of the microcapsule rises when the CBD core material is attached to a human body. Therefore, even if the capsule wall of the CBD microcapsule is ruptured during the process of clothing, transportation, etc., the CBD core material remains substantially solid and is not easily lost when the outside temperature is not high.

Furthermore, pyrrolidone carboxylic acid ions in the zinc pyrrolidone carboxylate are substances naturally existing in human skin, are easily absorbed by the skin, have good moisture retention property, and can enhance the flexibility and elasticity of the skin to enable the skin to be rich in luster. The zinc ions not only have good antibacterial effect, but also can relieve the skin and relieve skin inflammation, acne and the like.

Optionally, the polyethylene glycol is PEG-1000 and PEG-1500 according to a mass ratio of 1: (0.37-0.40).

By adopting the technical scheme, if the molecular weight of the polyethylene glycol is too large, the phase transition temperature of the polyethylene glycol is too high, the polyethylene glycol is difficult to reach the liquefaction temperature even being attached to a human body, and when the molecular weight of the polyethylene glycol is too small, the polyethylene glycol is too low in phase transition temperature and is liquefied at a lower temperature, so that unnecessary loss of the active ingredient CBD is easily caused.

It is noted that the most frequent point of movement of the bedding product is often when the consumer is just asleep, and when the capsule wall of the microcapsules is most likely to rupture. However, consumers of the time node are still excited, and even if the CBD is released at the time, the sleep-aiding effect is poor. This makes the releasing node of the CBD be a period of time after the consumer sleeps in, at the moment, the emotion of the consumer is calmer and relaxed, and the releasing CBD has better sleep-assisting effect.

Through a large number of experiments, the inventor finds that the phase transition temperature of the PEG mixture prepared according to the proportion as the core material of the double-layer microcapsule is about 30-32 ℃, the optimum temperature in the quilt during sleeping is about 32-34 ℃, and the phase transition temperature of the CBD core material is slightly lower than the optimum temperature in the quilt. Therefore, when the temperature in the quilt reaches the optimum temperature, the CBD core material can continuously absorb heat and be liquefied and released, so that the effect of long-time slow release of CBD to help sleep is achieved. And because the CBD core material has the heat absorption effect, the temperature in the quilt can be adjusted to a certain extent.

And because the optimum temperature of the quilt is gradually increased, even if the quilt is moved to cause the capsule wall of the CBD microcapsule to be broken when sleeping, the temperature of the quilt is lower, and the CBD core material is approximately solid and is not easy to release. Along with the extension of the sleeping time of a consumer, the temperature of the quilt is gradually increased, the CBD core material is gradually liquefied at the moment, the CBD is released, the emotion of the consumer at the moment is more relaxed, and therefore the releasing node of the CBD can be controlled by specifically selecting and controlling the components and the proportion of the CBD core material, and the sleeping aid effect of the CBD is better.

Optionally, the inner coating layer at least comprises the following raw materials in parts by mass:

by adopting the technical scheme, the gelatin is a material which is rich in source and degradable, is a good film-forming material, but has poor mechanical property, is brittle and is easily corroded by bacteria. The additional addition of glycerol can improve the toughness of the inner coating layer to a certain extent, improve the film forming property of the gelatin and reduce the possibility of brittle fracture of the gelatin film. The fucoidin additionally added is a good film forming material, has good antibacterial and antibacterial effects, and can complement the defect that gelatin is easy to be corroded by bacteria.

Optionally, the outer coating layer at least comprises the following raw materials in parts by mass:

100 portions of 2wt percent chitosan solution and 110 portions;

200 portions and 210 portions of 0.25wt percent fucoidan solution;

0.5-1 part of crosslinking component.

By adopting the technical scheme, the chitosan molecule contains a large amount of primary amino and carboxyl, wherein the primary amino has positive charges, and the carboxyl has negative charges. Through electrostatic interaction, primary amino and carboxyl carry out complex reaction to form the polyelectrolyte composite membrane. Fucoidan is an acidic sulfated polysaccharide, the main chain of which is composed of fucose, and a large number of sulfate groups are contained in the fucose, and the sulfate groups have negative charges. When the chitosan and the fucoidan are mixed, the sulfate group on the fucoidan and the primary amino group on the chitosan are mutually attracted and generate a complex reaction through electrostatic interaction, and the chitosan-fucoidan polyelectrolyte composite membrane is formed under the action of a crosslinking component.

Optionally, the crosslinking component is a mixture of tannic acid and citric acid, and the mass ratio of tannic acid: citric acid is 1: 1.

by adopting the technical scheme, compared with common aldehyde crosslinking agents such as glutaraldehyde and formaldehyde, the tannin and citric acid have higher safety. However, citric acid is easy to yellow under high temperature conditions, and the color of the fabric is affected, so that the mixture of tannic acid and citric acid is selected as a crosslinking component to reduce the generation of yellow stain. In addition, tannic acid has an amphiphilic structure, which results in better dispersion of the microcapsules after crosslinking with tannic acid.

In addition, the inventor unexpectedly finds that compared with glutaraldehyde as a crosslinking component, tannin and citric acid as the crosslinking components greatly prolong the service life of the microcapsule on the premise of hardly influencing the sleeping-aiding effect of CBD, and the microcapsule can still release CBD after long-term use.

This is probably due to the fact that after the microcapsules are broken, the CBD core material with the polyethylene glycol and zinc pyrrolidone carboxylate flows out, while the outer coating layer contains tannic acid, which can form hydrogen bond complexes with polyethylene glycol, which can be deposited as a film in sodium chloride solution.

The zinc pyrrolidone carboxylate in the CBD core material has very good hygroscopicity, so that sweat on the surface of human skin can be absorbed after the zinc pyrrolidone carboxylate in the CBD core material is released, and the sweat contains sodium chloride with a certain concentration, so that a hydrogen bond complex formed by tannic acid and polyethylene glycol can form a stable and insoluble film and repair a broken capsule wall after meeting the sweat of the human body, and the hydrogen bond of the cured hydrogen bond complex is enhanced and has good adhesion and oxidation resistance. This prevents the CBD core material from continuing to flow out and from being oxidized.

Since this hydrogen bonding complex is only deposited as a film upon contact with sweat, this indicates that the relatively high temperatures within the quilt have been reached and the consumer has slept longer. Thus, the CBD released prior to repair of the ruptured capsule wall is already sufficiently hypnotic. After the broken capsule wall is repaired by the hydrogen bond compound, part of the CBD core material in the microcapsule does not flow out, and the action of a consumer after sleeping is usually small, so that the microcapsule is not easy to break. Thus, the repaired microcapsules can be ruptured the next time they sleep to release the remaining CBD core material to provide a sleep aid effect.

Namely, the microcapsule capable of self-repairing greatly reduces the possibility of waste caused by excessive release of the CBD core material, changes the current situation that the core material can only be completely released once the capsule wall of the common microcapsule is broken, and prolongs the service life of the microcapsule.

Optionally, the CBD microcapsule is prepared by the following process:

a1, preparing a CBD core material, adding CBD and a reducing agent into water according to a ratio, performing ultrasonic dispersion, performing homogeneous dispersion, adding lysine after the homogeneous dispersion, and further performing the homogeneous dispersion to obtain the CBD core material;

a2, preparing an inner coating layer, namely putting fucoidan, glycerol and gelatin into water according to the proportion, heating and stirring to completely dissolve the materials to obtain an inner membrane liquid, then mixing the inner membrane liquid with the CBD core material obtained in the step A1, performing ultrasonic dispersion, performing homogeneous dispersion, and obtaining a crude product after the homogeneous dispersion;

a3, preparing an outer coating layer, mixing a chitosan solution and an algin solution according to a ratio, stirring and dispersing after mixing, dripping a crosslinking component after uniform dispersion, further stirring and dispersing to obtain an outer membrane solution, immediately adding the outer membrane solution into the crude product obtained in the step A2, then homogenizing and dispersing to obtain a microcapsule emulsion;

and A4, spray drying, namely spray drying the microcapsule emulsion obtained in the step A3 to obtain the CBD microcapsule.

By adopting the technical scheme, substances with positive charges such as lysine and the like are added into the CBD core material, fucoidan and the like in the inner coating layer have negative charges, and chitosan in the outer coating layer has positive charges. Therefore, according to the sequence, the inner coating layer and the outer coating layer can be alternately deposited on the surface of the CBD core material under the action of electrostatic adsorption, so that a multilayer emulsion is formed, and finally, after spray drying, the double-layer coated CBD microcapsule is obtained.

Optionally, the cross-linking agent is a mixture of dopamine hydrochloride and zinc acetylacetonate in equal mass ratio.

By adopting the technical scheme, the dopamine is easy to carry out self-polymerization reaction, and an adhesive layer is formed on the surface of the fabric, and the adhesive layer has active functional groups such as catechol and amino with good adhesive property, can form covalent bonds with the surface of the fabric, and is stably attached to the surface of the fabric. The zinc acetylacetonate is a cross-linking agent and can react with amino groups and other groups, and under the action of the zinc acetylacetonate, components such as chitosan and fucoidan on the surface of the CBD microcapsule react with the polydopamine, so that the CBD microcapsule is stably deposited on the fabric through the polydopamine.

The inventor unexpectedly finds that the service life of the microcapsule can be further prolonged by selecting dopamine hydrochloride and zinc acetylacetonate as a cross-linking agent, probably because the CBD microcapsule is attached to the surface of polydopamine, the surface of the polydopamine has catechol group and catechol group, the catechol group and the catechol group have good effect of complexing metal ions, zinc ions can be complexed with the polydopamine to form hydrogel after the zinc pyrrolidone carboxylate in the CBD core material is released, and the microcapsule can be repaired after the hydrogel is dried to form a film, so that the service life of the microcapsule can be prolonged.

In addition, due to the characteristic of polyhydroxy of the tannic acid, the tannic acid has good light absorption performance and a certain sun-blocking effect, zinc acetylacetonate is easy to convert into brown under the action of light, and the light absorption characteristic of the tannic acid can reduce the browning of the zinc acetylacetonate.

In a second aspect, the application provides a finishing process of a cannabidiol functional fabric, which adopts the following technical scheme:

a finishing process of a cannabidiol functional fabric comprises the following process steps:

s1, preparing a finishing liquid, dissolving the CBD microcapsules, the cross-linking agent and the penetrating agent into water according to the proportion, and uniformly stirring to obtain the cannabidiol finishing liquid;

s2, finishing, namely putting the combed cotton fabric into the cannabidiol finishing liquid obtained in the step S1, and vibrating at the temperature of 80-85 ℃ to obtain finished grey cloth;

and S3, post-processing, namely washing and drying the finished grey cloth obtained in the step S2 in sequence to obtain the cannabidiol functional fabric.

By adopting the technical scheme, the inventor finds that if a conventional padding process (such as two-padding and two-rolling) is adopted in the step S2, the antibacterial performance of the finally prepared cannabidiol functional fabric is relatively general, and when a vibration treatment finishing process is specially adopted, the antibacterial performance of the finally prepared cannabidiol is relatively obviously improved. The reason is probably that zinc acetylacetonate in the cross-linking agent can react with primary amine under the condition of oscillation, the microcapsule is inevitably broken in the finishing process, the CBD core material is released, lysine exists in the CBD core material, and the lysine has two primary amine groups, so that the zinc acetylacetonate and the lysine react to generate a substance with good bactericidal activity, and the finished cannabidiol functional fabric has good antibacterial performance.

In summary, the present application includes at least one of the following beneficial technical effects:

1. the CBD is prepared into the double-layer coated microcapsule, so that the possibility of CBD inactivation can be reduced, and the specific double-layer coating mode not only reduces the possibility of CBD loss caused by too thin capsule wall in the processes of finishing, conveying and the like, but also reduces the possibility that the microcapsule is not easy to break and CBD cannot be released and take effect in the actual use process because the capsule wall is too thick;

2. the reducing agent has the functions of improving the skin moisture retention and adjusting the releasing time node of the CBD core material by specially limiting the components and the proportion of the reducing agent, and the sleeping aid effect of the CBD is greatly improved as the releasing node of the CBD is more in line with the sleeping habits of consumers;

3. the composition and the proportion of the outer coating layer are specially limited, if citric acid and tannic acid are specially selected as crosslinking components of the outer coating layer, the crosslinking effect can be promoted, and the tannin can also be used for repairing broken microcapsules together with polyethylene glycol and zinc pyrrolidone carboxylate in the CBD core material, so that the service life of the microcapsules is prolonged;

4. by specially limiting the composition and the proportion of the cross-linking agent in the finishing liquid, the microcapsule can be firmly attached to the fabric, and the microcapsule can be repaired by the cooperation of polydopamine in the cross-linking agent and zinc pyrrolidone carboxylate in a CBD core material, so that the service life of the microcapsule is further prolonged;

5. the zinc acetylacetonate in the cross-linking agent has a good effect of promoting cross-linking, and the tannic acid in the outer coating layer has the effect of relieving the browning of the zinc acetylacetonate;

6. zinc acetylacetonate in the cross-linking agent and lysine in the CBD core material can react to form beta-enaminone substances with good bactericidal activity under a specific finishing process, so that the finally prepared fabric has good antibacterial property.

Detailed Description

The present application is described in further detail below with reference to preparation examples and examples.

The raw material sources in the various preparations and examples are given in the following table:

raw material	Performance parameters/brands	Source
			CBD	CBD≥99.5％	Yunnan Hansu bio-technology Co.,Ltd.
Fucoidan	LF0902	Shenzhen Lefu Biotech Co Ltd
			Gelatin	The content of effective substances is more than or equal to 99 percent	Shandong Nuanju Biotech Co Ltd
Chitosan	Degree of deacetylation 95%	ZHEJIANG GOLDEN-SHELL BIOCHEMICAL Co.,Ltd.
			Dopamine hydrochloride	98.5％	Shanghai-derived leaf organisms Ltd

Except for the raw materials in the table above, the other raw materials are all conventionally sold on the market except for special description.

Preparation example 1

The CBD microcapsule comprises a CBD core material, an inner coating layer and an outer coating layer from inside to outside in sequence.

Wherein, each prepared CBD core material comprises the following components in parts by mass:

the reducing agent is PEG-1000.

Wherein, each prepared inner coating layer raw material comprises the following components in parts by mass:

wherein, each prepared outer coating layer raw material comprises the following components in parts by mass:

100g of 2 wt% chitosan solution;

200g of 0.25 wt% fucoidan solution;

0.5g of a crosslinking component;

the crosslinking component is citric acid;

the 2 wt% chitosan solution refers to a solution obtained by dissolving chitosan in 1 wt% acetic acid solution according to a ratio.

The 0.25 wt% fucoidan solution refers to a solution obtained by dissolving fucoidan in deionized water according to a ratio.

The CBD microcapsule is prepared by the following process:

a1, preparing a CBD core material, adding CBD and a reducing agent into water according to a ratio, ultrasonically dispersing for 15min at a power of 60W, and then uniformly dispersing for 5min at a rotating speed of 8000 r/min. And after the homogeneous dispersion is finished, adding lysine, wherein the stirring speed is 500r/min in the adding process, and after the lysine is added, carrying out the homogeneous dispersion for 3min at the rotating speed of 8000r/min to obtain the CBD core material.

A2, preparing an inner coating layer, namely, putting fucoidin, glycerol and gelatin into water according to the proportion, heating to 80 ℃, and stirring at the speed of 500r/min until the raw materials are completely dissolved to obtain the inner membrane liquid. And then mixing the obtained internal membrane liquid with the CBD core material obtained in the step A1, wherein the mass ratio of the internal membrane liquid is as follows: CBD core material 1: 1. and ultrasonically dispersing for 10min at the power of 60W after mixing, then carrying out uniform dispersion for 5min at the rotating speed of 8000r/min, and obtaining a crude product after the uniform dispersion is finished.

A3, preparing an outer coating layer, mixing the chitosan solution and the fucoidin solution according to a ratio, stirring for 30min at a speed of 1000r/min after mixing to uniformly mix the chitosan solution and the fucoidin solution, then dripping the crosslinking component at a stirring speed of 500r/min during dripping, and dispersing for 5min at a speed of 5000r/min after finishing dripping to obtain the outer coating liquid. Immediately adding the membrane solution into the crude product obtained in the step A2, wherein the mass ratio of the membrane solution is as follows: crude product 1: and 1, after the addition is finished, homogenizing and dispersing for 5min at the rotating speed of 8000r/min to obtain the microcapsule emulsion.

And A4, spray drying, namely spray drying in a spray dryer at the air inlet temperature of 120 +/-2 ℃, and spray drying to obtain the CBD microcapsule.

Preparation example 2

The difference between preparation example 2 and preparation example 1 is that the following components in parts by mass are required for each part of CBD core material:

the reducing agent is PEG-1000.

Preparation example 3

Preparation example 3 differs from preparation example 1 in that the following components in parts by mass are required for each configuration of one CBD core material:

the reducing agent is PEG-1000.

Preparation example 4

Preparation 4 differs from preparation 1 in that 10.2g of the reducing agent was obtained by mixing 10g of PEG-1000 and 0.2g of zinc pyrrolidone carboxylate.

Preparation example 5

Preparation example 5 differs from preparation example 3 in that 12.4g of a reducing agent was obtained by mixing 12g of PEG-1000 and 0.4g of zinc pyrrolidone carboxylate.

Preparation example 6

Preparation 6 differs from preparation 5 in that 12.4g of a reducing agent was obtained by mixing 8.76g of PEG-1000 and 3.24g of PEG-1500, and 0.4g of zinc pyrrolidone carboxylate. That is, in the present production example, PEG-1000: PEG-1500 ═ 1: 0.37.

preparation example 7

Preparation example 7 differs from preparation example 6 in that 12.4g of a reducing agent was obtained by mixing 8.57g of PEG-1000 and 3.43g of PEG-1500, and 0.4g of zinc pyrrolidone carboxylate. That is, in the present production example, PEG-1000: PEG-1500 ═ 1: 0.40.

preparation example 8

Preparation example 8 is different from preparation example 7 in that the following components in parts by mass are required for each preparation of one part of raw material for the inner coating layer:

preparation example 9

Preparation example 9 differs from preparation example 7 in that the following components in parts by mass are required for each prepared portion of the outer cladding raw material:

110g of 2 wt% chitosan solution;

210g of 0.25 wt% fucoidan solution;

1g of a crosslinking component;

the crosslinking component is citric acid.

Preparation example 10

Preparation example 10 differs from preparation example 9 in that 1g of a crosslinking component was obtained by mixing 0.5g of tannic acid and 0.5g of citric acid.

Preparation example 11

Preparation 11 differs from preparation 10 in that 12.4g of a reducing agent was obtained by mixing 8.86g of PEG-1000 and 3.54g of PEG-1500. That is, in the present production example, PEG-1000: PEG-1500 ═ 1: 0.40, and no zinc pyrrolidone carboxylate was added.

Preparation example 12

Preparation example 12 is different from preparation example 10 in that equal masses of CBD in the CBD core material are replaced with glycerin.

Examples

Example 1

The embodiment of the application firstly discloses a cannabidiol finishing liquid, wherein each prepared cannabidiol finishing liquid comprises the following components in parts by mass:

wherein, the CBD microcapsule prepared in the preparation example 1 is selected as the CBD microcapsule.

Wherein the cross-linking agent is dopamine hydrochloride.

Wherein the penetrating agent is JFC-4 penetrating agent.

The technology for using the cannabidiol finishing liquid for finishing the cannabidiol functional fabric is as follows:

s1, preparing a finishing liquid, dissolving the CBD microcapsules, the cross-linking agent and the penetrating agent in water according to the proportion, and uniformly stirring to obtain the cannabidiol finishing liquid.

S2, finishing, namely, padding the combed cotton fabric into the cannabidiol finishing liquid obtained in the step S1, wherein a two-padding and two-rolling process is adopted, the padding rate is 100%, and the padding temperature is 60 ℃, so that finished gray fabric is obtained.

And S3, post-processing, namely washing the finished grey cloth obtained in the step S2 with water twice in sequence, and drying the washed grey cloth at the temperature of 80 ℃ to obtain the cannabidiol functional fabric.

Example 2

Example 2 differs from example 1 in that each configuration of one part of cannabidiol finishing liquor comprises the following components in parts by mass:

example 3

Example 3 differs from example 1 in that each portion of cannabidiol finishing liquor is prepared with the following components in parts by mass:

example 4

Example 4 differs from example 2 in that 18g of cross-linking agent was obtained by mixing 9g of dopamine hydrochloride and 9g of zinc acetylacetonate.

Example 5

The difference between the embodiment 5 and the embodiment 4 is that the technology of the cannabidiol finishing liquid used for finishing the cannabidiol functional fabric is as follows:

s1, preparing a finishing liquid, dissolving the CBD microcapsules, the cross-linking agent and the penetrating agent in water according to the proportion, and uniformly stirring to obtain the cannabidiol finishing liquid.

And S2, finishing, namely putting the finishing liquid obtained in the step S1 into a constant-temperature oscillation dyeing machine, putting combed cotton fabric into the constant-temperature oscillation dyeing machine, and performing oscillation finishing for 1 hour at the temperature of 80 ℃ to obtain finished gray fabric.

And S3, post-processing, namely washing the finished grey cloth obtained in the step S2 with water twice in sequence, and drying the washed grey cloth at the temperature of 80 ℃ to obtain the cannabidiol functional fabric.

Example 6

Example 6 is different from example 5 in that the shaking finishing temperature in step S2 was 85 ℃.

Example 7-example 15 differed from example 5 only in that the source of the CBD microcapsules used in step S1 was different, and the source of the CBD microcapsules for each example is represented in the following table:

examples	CBD microcapsule source
		Examples 1 to 6	Preparation example 1
Example 7	Preparation example 2
		Example 8	Preparation example 3
Example 9	Preparation example 4
		Example 10	Preparation example 5
Example 11	Preparation example 6
		Example 12	Preparation example 7
Example 13	Preparation example 8
		Example 14	Preparation example 9
Example 15	Preparation example 10
		Example 16	Preparation example 11

Comparative example

Comparative example 1

Comparative example 1 is a blank control, i.e. no treatment of the combed cotton face.

Comparative example 2

Comparative example 2 is different from example 5 in that the CBD microcapsule used in step S1 is the CBD microcapsule prepared in preparation example 12.

Performance detection

1. Detection of antibacterial Properties

The fabric antibacterial performance is subjected to antibacterial test on the prepared cannabidiol functional fabric according to the method in AATCC100-2012 'evaluation of textile material antibacterial finishing agent', and the experimental strains adopt staphylococcus aureus (gram-positive bacteria ATCC6538) and bacillus pneumoniae (gram-negative bacteria ATCC 4352). It should be noted that in this experiment, the antibacterial property of the fabric sample is detected after the fabric sample is kneaded for 5min before the experiment.

The percent reduction of bacteria is calculated as:

R＝(B－A)/B×100％

wherein R is the percentage of bacteria reduction; a is the number of bacteria recovered after the antibacterial finished sample is in contact with the bacteria and cultured for 24 hours; b is the number of bacteria recovered immediately after inoculation ("0" contact time) of the antimicrobial finish sample with the bacteria. The higher the percentage reduction of bacteria, the better the antibacterial effect.

Wherein the percentage reduction of bacteria in Staphylococcus aureus is denoted as R_{Gold (Au)}(ii) a The percent reduction of bacteria in the genus Klebsiella was recorded as R_{Lung (lung)}。

2. Sleep aid effect detection

The sleep aid effect evaluation is mainly evaluated according to a Pittsburgh Sleep Quality Index (PSQI), and the sleep aid effect evaluation is composed of 19 self-evaluation items and 5 other evaluation items, wherein the 19 th self-evaluation item and the 5 other evaluation items are not scored. That is, the scored items are 18 self-rated items and are divided into 7 dimensions: sleep quality, time to sleep, sleep time, sleep efficiency, sleep disturbance, hypnotics, and daytime dysfunction. The score of each item is 0-3, and the scores of all the items are accumulated to obtain the PSQI total score. A higher score indicates a poorer sleep quality. When the total score is less than or equal to 7 minutes, the sleep quality is better, and when the total score is more than 7 minutes, the sleep quality is poorer.

18 volunteers were recruited this time and all had some sleep disturbance, with 8 males and 10 females aged between 18-35 years.

The hempsediol functional fabric prepared in each example or comparative example is used for preparing the quilt, and the quilt must be used closely. The whole experiment period is one year, the initial PSQI value, the PSQI value at 1 day, the PSQI value at 100 days, the PSQI value at 200 days, the PSQI value after 300 days and the PSQI value after 365 days are respectively recorded, and cotton quilt is uniformly recovered, washed and dried after the PSQI values are recorded every time.

The test results are shown in the following table:

conclusion

By comparing the antibacterial data of the embodiment 4, the embodiment 5 and the embodiment 6, it can be shown that the finally prepared cannabidiol functional fabric has a better antibacterial effect by adopting the vibration finishing process. This is probably because the zinc acetylacetonate in the crosslinking agent and the primary amine group on the lysine in the CBD core material do not react under the padding process condition, and react under the shock finishing process condition to generate β -enaminone compounds, which have good antibacterial activity. Therefore, compared with example 4, the antibacterial properties of the cannabidiol functional fabrics prepared in examples 5 and 6 are significantly improved.

By comparing the antibacterial property data of example 15 and example 16, it can be shown that the zinc pyrrolidone carboxylate added to the CBD core material has a certain antibacterial activity, and the antibacterial property of the finally prepared cannabidiol functional fabric can be improved.

By comparing the antibacterial property data of example 5 and comparative example 2, it can be seen that CBD has a stronger antibacterial activity and can exert a stronger antibacterial effect than glycerin.

By comparing the sleep-aid effect data of comparative examples 1, 2 and example 5, it can be concluded that the PSQI score of the volunteer is significantly decreased, that is, CBD can exert a significant sleep-aid effect (the PSQI score is more decreased). Compared with the comparative example 1, the PSQI score of the volunteer in the comparative example 2 also decreases relatively stably, which is probably because the finally obtained fabric has the effect of adjusting the temperature although no CBD sleep-assisting component exists, and the sleep comfort level is improved to a certain extent.

By comparing the sleep-aiding effect data of examples 1 to 8, it can be shown that within 100 days, the hemp two phenol functional fabric has a good sleep-aiding effect and a large reduction in PSQI. However, the sleep-aiding effect of the cannabidiol functional fabric is remarkably reduced in 200 days, which is probably caused by that the sleep-aiding effect is reduced due to insufficient concentration of subsequently released CBD (conjugated diene) caused by excessive rupture of CBD microcapsules on the cannabidiol functional fabric. At 300 and 365 days, the sleep-aiding effect of the cannabidiol functional fabric basically disappears, which is probably because the CBD microcapsules on the cannabidiol functional fabric are basically broken, and the CBD cannot be continuously released to aid sleep.

By comparing the sleep-aiding effect data of the embodiment 8 and the embodiment 9, it can be obtained that the cannabidiol functional fabric prepared in the embodiment 9 still has a relatively obvious sleep-aiding effect at 200 days, which is obviously superior to the sleep-aiding effect of the cannabidiol functional fabric prepared in the embodiment 8 at 200 days. The reason is probably that zinc pyrrolidone carboxylate is added into the reducing agent, and the zinc pyrrolidone carboxylate is complexed with polydopamine after being released, so that a certain self-repairing effect is achieved.

By comparing the sleep-aiding effect data of examples 10 to 12, it can be seen that the cannabidiol functional fabrics prepared in examples 11 and 12 have more excellent sleep-aiding effect than the hemp functional fabrics prepared in example 10. This is probably superior to that the phase transition temperature of the CBD microcapsules in examples 11 and 12 is more reasonable, and compared with the simple PEG-1000, the PEG-1000 and PEG-1500 have more suitable phase transition temperature after mixing, so that the release node of the CBD is more suitable, and the sleep-aiding effect of the CBD is better.

By comparing the sleep-aid effect data of example 14 and example 15, it can be seen that the cannabidiol functional fabric prepared in example 15 can maintain a very good sleep-aid effect even at 365 days. This shows that the cannabidiol functional fabric of example 15 has a significantly longer life compared to the cannabidiol functional fabric of example 14. This is probably due to the fact that after release of the polyethylene glycol from the CBD core material, hydrogen bonding complexes can form with tannic acid on the outer coating layer, which upon encountering sweat adsorbed by zinc pyrrolidone carboxylate form a stable and insoluble film to repair the capsule wall of the CBD microcapsules. Therefore, the cannabidiol functional fabric only releases enough CBD for helping sleep during sleeping every time, so that the waste of the CBD is avoided to a great extent, and the service life of the cannabidiol functional fabric is prolonged.

By comparing the sleep-aid effect data of example 15 and example 16, it can be seen that the sleep-aid effects of both are not very different (PSQI score decreases by 7 or 8 points) at the beginning, but the sleep-aid effect of example 16 significantly decreases after 300 days. This is probably because zinc pyrrolidone carboxylate is not added to the CBD microcapsules in preparation example 11, which reduces the moisture absorption effect of the CBD microcapsules after rupture, and thus cannot well adsorb sweat on human body, and even though the polyethylene glycol in the CBD core material and the tannic acid in the outer coating layer are mixed, the CBD microcapsules are not easily formed into a film without sodium chloride, and thus, the self-repairing effect of the CBD microcapsules is poor, and the life of the cannabidiol functional fabric is significantly reduced.

The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.