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CN112452264B - Preparation method and application of melanoid microcapsules in red wolfberry - Google Patents

Preparation method and application of melanoid microcapsules in red wolfberry Download PDF

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Publication number
CN112452264B
CN112452264B CN202110008633.7A CN202110008633A CN112452264B CN 112452264 B CN112452264 B CN 112452264B CN 202110008633 A CN202110008633 A CN 202110008633A CN 112452264 B CN112452264 B CN 112452264B
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melanoid
red
dyeing
microcapsules
emulsion
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CN112452264A (en
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王雪梅
郭潇涵
易帆
洪国英
杨亮
陈莉萍
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Lanzhou University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/36—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using mordant dyes ; using metallisable dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02—Material containing basic nitrogen
    • D06P3/04—Material containing basic nitrogen containing amide groups
    • D06P3/14—Wool
    • D06P3/20—Wool using mordant dyes using metallisable dyes

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Cosmetics (AREA)
  • Coloring (AREA)

Abstract

The invention discloses a preparation method and application of melanoid microcapsules in red wolfberry, wherein the preparation method comprises the following steps: s1, dissolving 1 g of a mixture obtained by mixing soybean lecithin, phosphatidylcholine and cholesterol according to a mass ratio of 3:3:2 in an ether organic solvent with a certain volume to form a mixed organic liquid; s2, adding a PBS buffer solution in which melanoid extracted after red medlar is cured is dissolved into the mixed organic liquid, and placing the mixed organic liquid in an ultrasonic cleaner for ultrasonic treatment until a uniform W/O emulsion is formed; s3, adding another 10ml of PBS buffer solution into the flask of the uniform W/O emulsion formed in the step S2, continuing to perform ultrasonic treatment on the ultrasonic cleaning instrument for 5min until W/O/W multiple emulsion is formed, connecting the flask to a rotary evaporator, and performing reduced pressure distillation to remove the organic solvent to obtain the microcapsule suspension.

Description

Preparation method and application of melanoid microcapsules in red wolfberry fruits
Technical Field
The invention relates to the field of natural coloring agents, and in particular relates to a preparation method and application of melanoid microcapsules in red wolfberry.
Background
Melanoidins (melanoids) are brown macromolecular substances formed in the later stage of the Maillard reaction, are main products of non-enzymatic browning reaction, have natural color and relatively stable chemical properties, do not produce adverse reaction, have stronger biological activity and health-care function, and are environment-friendly natural pigments. The melanoid biological activity mainly shows antioxidant activity, antibacterial activity, anticancer activity, antihypertensive activity, dietary fiber-like function, flavor-substance combination and other biological activities. The melanoid is applied to the industries of textile, food, cosmetics and the like by combining various bioactive properties and excellent coloring property of melanoid, and compared with synthetic pigments, the melanoid has the advantages of simple and convenient operation process, safety, no pollution, natural bioactive property of coloring products, complete biodegradation and the like.
At present, the chemical components and active substances of the medlar, the drying and preservation process of the medlar and the processing and utilization aspects of the medlar are researched at home and abroad. A series of reactions occurring in the drying process of the medlar also have research on the influence of the medlar active substances. However, the study of Maillard reaction and the study of using the efficacy of Maillard reaction products are still deficient in the aspect of functional action in the wolfberry drying process, the study of applying melanoid to the field of textile printing and dyeing is rarely reported, only Ohe T and the like directly carry out Maillard reaction on nylon fibers and xylose which is one of reducing sugar, and the fibers after the reaction have strong antibacterial activity on gram-positive bacteria, gram-negative bacteria such as staphylococcus aureus, escherichia coli and the like. The melanoid can also endow the textile with biological functional characteristics, so the melanoid can be applied to the textile printing and dyeing field to improve the added value of the product.
Dyeing and finishing processing is an indispensable link in the finishing of wool products, not only a large amount of water resources are consumed, but also more serious water pollution is caused. At present, the annual discharge amount of textile printing and dyeing wastewater in China is about 16 billion cubic meters, the recovery rate of the wastewater is only 15 percent, and the wastewater which is not recycled becomes industrial sewage. Although many wool textile printing and dyeing enterprises can treat dyeing wastewater, the dyeing wastewater has complex components and many substances which are difficult to degrade, and complicated and tedious treatment procedures are required. In addition, the development and application of more dyeing processes and raw materials further aggravate the complexity and treatment difficulty of dyeing wastewater. Although various policies are set in China to aim at the discharge of wool spinning dyeing wastewater, the pollution degree of the dyeing wastewater in the current wool spinning industry, especially in centralized areas of the wool spinning industry, is quite serious. For this reason, many dyeing workers have conducted a lot of research on the problem of clean production and developed various environmentally friendly dyes, auxiliaries and dyeing processes, but the current dyeing wastewater treatment situation of wool spinning enterprises is still not optimistic due to technical defects and limitations of methods.
Among various environment-friendly dyeing processes, research on microcapsule dyeing technology is relatively mature, but the microcapsule dyeing technology is mainly researched and used for products such as terylene and chinlon at present, research on wool product dyeing is relatively less, and chemical dyes are prepared into microcapsules and applied to wool product dyeing, so that the dyeing temperature and dyeing wastewater pollution can be reduced, but the problem of wastewater pollution cannot be completely avoided.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method and application of melanoid microcapsules in red wolfberry.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the melanoid microcapsule in the red medlar comprises the following steps:
s1, dissolving 1 g of a mixture obtained by mixing soybean lecithin, phosphatidylcholine and cholesterol according to a mass ratio of 3:3:2 in an ether organic solvent with a certain volume to form a mixed organic liquid;
s2, adding a PBS buffer solution in which melanoid extracted after red medlar is cured is dissolved into the mixed organic liquid, and placing the mixed organic liquid in an ultrasonic cleaner for ultrasonic treatment until a uniform W/O emulsion is formed;
s3, adding another 10ml of PBS buffer solution into the flask of the uniform W/O emulsion formed in the step S2, continuing to perform ultrasonic treatment on the ultrasonic cleaning instrument for 5min until W/O/W multiple emulsion is formed, connecting the flask to a rotary evaporator, and performing reduced pressure distillation to remove the organic solvent to obtain the microcapsule suspension.
Further, in the step S1, the amount of the ether organic solvent used is 30 mL.
Further, in the step S2, the wall-core ratio is 25: 1.
The melanoid microcapsule in the red wolfberry can be used for dyeing wool fabrics, and further, a post mordant dyeing mode is selected, pomegranate bark is used as a natural medium, and the bath ratio is 33: 1. the pH was 3.5 and the temperature 77 ℃.
The invention has the following beneficial effects:
the research results provide theoretical basis and technical guidance for fully utilizing and processing Chinese wolfberry resources in our province (Gansu) and even western regions and for scientific development and comprehensive profit of the Chinese wolfberry resources; the melanoid-like lipid microcapsule is applied to dyeing of pure wool fabrics, the catalysis and promotion effects of a natural mordant dye fixing agent are involved, the natural mordant dye fixing agent such as gum arabic, pomegranate rind, gallnut, laccase and guava rind is used, the problem of environmental pollution caused by the conventional metal ion mordant dye fixing agent containing copper, iron, aluminum, chromium and the like can be avoided, the dyeing temperature is reduced to be below 80 ℃, a new way is opened up for the application of natural pigments in the field of textile printing and dyeing, the low-temperature dyeing process of wool with the advantages of environmental protection, energy saving and emission reduction is explored, and a green and healthy wool product is developed. The research result can also be applied to the preparation of microcapsules of other natural pigments and even microcapsule dyeing of other fiber products, and has higher economic and social significance for improving and popularizing the application technology and field of the natural pigments in the textile printing and dyeing industry of China, reducing the gap with foreign products, enhancing the competitiveness, developing low-consumption and environment-friendly green textiles which are beneficial to health.
Drawings
FIG. 1 shows the results of a single-factor test for extracting melanoid by microwave;
in the figure: (a) influence of ultrasound time on melanoid absorbance; (b) influence of the amount of diethyl ether on the absorbance of melanoids; (c) influence of wall-core ratio on melanoid absorbance; (d) the effect of the mass ratio of phosphatidylcholine, soy lecithin, cholesterol on the absorbance of melanoid.
FIG. 2 results of a class melanin microcapsule staining single factor test;
in the figure: (a) the effect of bath ratio on the color difference value Δ E of the wool fabric; (b) influence of pH on the colour difference value Δ E of wool fabrics; (c) influence of temperature on the color difference value Δ E of the wool fabric; (d) influence of a mordant dyeing mode on a color difference value delta E of the wool fabric; (e) the effect of natural mordants on the colour difference value Δ E of wool fabrics.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Examples of the experiments
Preparation of class 1 melanin microcapsule (multiple emulsion method)
Firstly, a mixture of soybean lecithin, phosphatidylcholine and cholesterol in a certain proportion (three kinds of the mixture are 1.000g in total) is dissolved in a certain volume of ether organic solvent to form a mixed organic liquid. Adding PBS buffer solution dissolved with melanoid extracted after aging red medlar into the mixed organic solution, placing the mixed organic solution in an ultrasonic cleaning instrument for ultrasonic treatment until uniform W/O emulsion is formed, adding 10ml of PBS buffer solution into the flask of the uniform W/O emulsion formed, and continuously performing ultrasonic treatment on the ultrasonic cleaning instrument for 5min until W/O/W compound emulsion is formed. Finally, the flask was connected to a rotary evaporator for distillation under reduced pressure to remove the organic solvent to obtain a microcapsule suspension, and each experiment was repeated 3 times.
Single factor experiment
TABLE 1 Melanin-like microcapsule one-factor test
Factor (I) Horizontal range Other conditions
Ultrasonic time/min 3、4、5、6、7 25ml、20:1、3:3:2
Amount of diethyl ether/ml 20、25、30、35、40 5min、20:1、3:3:2
Wall-core ratio g/g 15:1、20:1、25:1、30:1、35:1 30ml、5min、3:3:2
Phosphatidylcholine: soybean lecithin: cholesterol/g 1:1:1、3:3:2、3:1:1、2:2:1、1:3:1 30ml、25:1、5min
As can be seen from fig. 1, with the increase of the ultrasonic time, the absorbance of the melanoid firstly decreases and then slowly increases, and reaches the minimum in 5 min; with the increase of the use amount of the ether, the absorbance of the melanoid is in a descending trend, the effect is not obvious after the absorbance is more than 30ml, and 30ml is selected as an experimental result from the consideration of saving cost; along with the increase of the wall-core ratio, the melanoid absorbance is in a descending trend, the effect is not obvious after the wall-core ratio is more than 25:1, and 25:1 is selected as an experimental result from the consideration of saving cost; the proportion of the materials contained in the wall material is different, the absorbance of the melanoid is different, when the dosage of the phosphatidylcholine is large, the melanoid cannot be completely dissolved into the ether solvent, when the dosage of the phosphatidylcholine is small, the absorbance of the melanoid is slightly high, and 3:3:2 is selected as an experimental result.
Melanoid microcapsule dyeing
The dyeing time is 2 h. Respectively exploring the bath ratio, the pH value, the temperature, the mordant dyeing mode and the influence of a natural mordant on melanoid dyeing of wool fabrics, dyeing the wool fabrics under different conditions, washing the wool fabrics for 2-3 times by tap water, naturally drying the wool fabrics, taking the undyed wool fabrics as a standard sample, and measuring the color difference value delta E of the wool fabrics by using an NS800 spectrophotometer.
Single factor experiment
TABLE 2 Melanin staining single factor test
Factor (I) Horizontal range Other conditions
Bath ratio 20:1、25:1、30:1、35:1、40:1 One-bath dyeing, 5, 80。C. Laccase enzymes
pH
3、4、5、6、7 One-bath dyeing, 35:1, 80。C. Laccase enzymes
Enzymolysis temperature-。 C 60、70、80、90、100 One-bath dyeing, 35:1, 4, laccase
Mordant dyeing mode Mordant-free dyeing, front mordant dyeing, back mordant dyeing and one-bath dyeing 4、35:1、80。C. Laccase enzymes
Natural mordant Arabic gum, pericarpium Granati, Galla chinensis, laccase, and pericarpium Psidii Guajavae After mordant dyeing, 35:1, 80。C、4
As can be seen from fig. 2, with the increase of the bath ratio, the color difference value Δ E of the wool fabric firstly rises and then falls, reaches the maximum value at 35:1, and selects 30:1, 35:1 and 40:1 as 3 levels of response surface optimization analysis; with the increase of the pH value, the color difference value delta E of the wool fabric firstly rises and then falls, the maximum value is reached when the pH =4, and 3, 4 and 5 are selected as 3 levels of response surface optimization analysis; with the increase of the temperature, the color difference value delta E of the wool fabric firstly rises and then falls, the maximum value is reached at 80 ℃, and the temperature of 70 ℃, 80 ℃ and 90 ℃ are selected as 3 levels of response surface optimization analysis; different mordant dyeing modes and different color difference values delta E of the wool fabric, wherein the after mordant dyeing effect is the best; the color difference value delta E of the wool fabric is different according to different natural mordants, wherein the pomegranate rind has the best effect. The dosage of the five natural mordants is 5 g/L.
Response surface optimization (after mordanting method)
TABLE 3 Melanin dyeing response surface optimization experiment factor horizon
Factors of the fact Bath ratio of A B pH C temperature (C。C）
-1 30 3 70
0 35 4 80
1 40 5 90
TABLE 4 Box-Behnken test design and results
Numbering Bath ratio of A B pH C temperature (C。C） Color difference value Delta E
1 1 0 -1 8.72
2 0 0 0 15.46
3 0 0 0 15.46
4 0 -1 1 11.13
5 -1 0 -1 10.93
6 1 1 0 11.6
7 -1 1 0 13.27
8 -1 0 1 13.16
9 0 1 -1 10.12
10 0 0 0 15.46
11 -1 -1 0 11.51
12 0 0 0 15.46
13 1 0 1 11.49
14 0 0 0 15.46
15 1 -1 0 9.84
16 0 -1 -1 8.36
17 0 1 1 12.89
TABLE 5 regression model analysis of variance results
Sources of variance Sum of squares Degree of freedom Mean square F value P value Significance of
Model (model) 95.96 9 10.66 1023.77 < 0.0001 ***
A 6.52 1 6.52 625.68 < 0.0001 ***
B 6.20 1 6.20 594.88 < 0.0001 ***
C 13.89 1 13.89 1333.40 < 0.0001 ***
AB 0.000 1 0.000 0.000 1.0000
AC 0.073 1 0.073 7.00 0.0331 **
BC 0.000 1 0.000 0.000 1.0000
A2 12.57 1 12.57 1206.54 < 0.0001 ***
B2 19.96 1 19.96 1917.00 < 0.0001 ***
C2 29.74 1 29.74 2855.31 < 0.0001 ***
Residual error 0.073 7 0.010
Missimilitude term 0.073 3 0.024
Pure error 0.000 4 0.000
Sum of 96.03 16
Note: indicates extremely significant (P less than 0.0001), indicates extremely significant (P less than 0.01), and indicates significant (P less than 0.05).
As shown in Table 5, the theoretically optimal process for melanoid staining obtained by Design-Expert 10.0.4 software is as follows: the bath ratio is 33.065: 1. the pH value is 3.525, the temperature is 76.92 ℃, and the color difference value delta E of the wool fabric is 14.001. In order to facilitate practical operation, the optimal process parameters for correcting the melanoid dyeing are as follows: the bath ratio is 33: 1. the 3-group average value of the color difference value Delta E of the wool fabric measured at a pH of 3.5 and a temperature of 77 ℃ was 14.523. The model is basically consistent with the theoretical predicted value 14.001, so that the model is more truly fitted with the actual situation and has practical value.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.

Claims (5)

1. The preparation method of the melanoid microcapsule in the red medlar is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving 1 g of a mixture obtained by mixing soybean lecithin, phosphatidylcholine and cholesterol according to a mass ratio of 3:3:2 in an ether organic solvent with a certain volume to form a mixed organic liquid;
s2, adding a PBS buffer solution in which melanoid extracted after red medlar is cured is dissolved into the mixed organic liquid, and placing the mixed organic liquid in an ultrasonic cleaner for ultrasonic treatment until a uniform W/O emulsion is formed;
s3, adding another 10ml of PBS buffer solution into the flask of the uniform W/O emulsion formed in the step S2, continuing to perform ultrasonic treatment on the ultrasonic cleaning instrument for 5min until W/O/W multiple emulsion is formed, connecting the flask to a rotary evaporator, and performing reduced pressure distillation to remove the organic solvent to obtain the microcapsule suspension.
2. The method of preparing melanoid microcapsules in red wolfberry of claim 1, wherein: in the step S1, the dosage of the ether organic solvent is 30 mL.
3. The method of preparing melanoid microcapsules in red wolfberry of claim 1, wherein: in step S2, the wall-to-core ratio is 25: 1.
4. The use of the red wolfberry melanoid microcapsules according to any one of claims 1 to 3 in the preparation of red wolfberry melanoid microcapsules, wherein: can be used for dyeing wool fabrics.
5. The use of claim 4, wherein: the method selects a post mordant dyeing mode, takes pomegranate rind as a natural medium, and has a bath ratio of 33: 1. the pH was 3.5 and the temperature 77 ℃.
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