阅读说明：本技术 一种牵牛花色素提取方法、牵牛花色素提取液及其应用 (Morning glory pigment extraction method, morning glory pigment extracting solution and application thereof ) 是由 林君 于 2021-07-30 设计创作，主要内容包括：本申请涉及色素提取技术领域,具体公开一种牵牛花色素提取方法、牵牛花色素提取液及其应用。该提取方法包括：将干燥的牵牛花进行粉碎处理后过筛网,得到牵牛花粉末,解决了新鲜的牵牛花的保存问题,且减少了细胞液的影响；将牵牛花粉末与蒸馏水按预设质量比混合得到的混合液进行加热；待加热后的混合液冷却后,超声提取得到超声提取液,使色素充分溶解于水中,提高色素析出；将超声提取液过滤得到的滤液进行离心分离,充分去除杂质；取离心分离得到的上清液调至第一预设pH之后,滴加硫酸镁溶液,得到较为稳定、易于保存、色素含量高,且杂质较少的牵牛花色素提取液。(The application relates to the technical field of pigment extraction, and particularly discloses a morning glory pigment extraction method, morning glory pigment extracting solution and application thereof. The extraction method comprises the following steps: the dried morning glory is crushed and screened to obtain morning glory powder, so that the storage problem of fresh morning glory is solved, and the influence of cell sap is reduced; heating mixed liquid obtained by mixing morning glory powder and distilled water according to a preset mass ratio; after the heated mixed solution is cooled, ultrasonic extraction is carried out to obtain an ultrasonic extracting solution, so that the pigment is fully dissolved in water, and the pigment precipitation is improved; performing centrifugal separation on filtrate obtained by filtering the ultrasonic extracting solution to fully remove impurities; and (3) regulating the supernatant obtained by centrifugal separation to a first preset pH value, and then dropwise adding a magnesium sulfate solution to obtain the morning glory pigment extracting solution which is stable, easy to store, high in pigment content and less in impurities.)

1. A method for extracting morning glory pigment is characterized by comprising the following steps:

crushing the dried morning glory, and then sieving the crushed morning glory through a screen to obtain morning glory powder;

heating mixed liquid obtained by mixing morning glory powder and distilled water according to a preset mass ratio;

after the heated mixed solution is cooled, carrying out ultrasonic extraction to obtain an ultrasonic extracting solution;

filtering the ultrasonic extracting solution to obtain filtrate, and performing centrifugal separation on the filtrate;

and (3) regulating the supernatant obtained by centrifugal separation to a first preset pH value, and then dropwise adding a magnesium sulfate solution to obtain the morning glory pigment extracting solution.

2. The method of claim 1, wherein the first predetermined pH is 9 to 10 and the concentration of the magnesium sulfate solution is 10%.

3. The method of claim 1, wherein adjusting the centrifuged supernatant to a first predetermined pH comprises:

adding sodium bicarbonate into the supernatant obtained by centrifugal separation to adjust the pH value to a first preset value.

4. The method of claim 1, wherein the screen is an 80-120 mesh screen.

5. The method according to claim 1, wherein the predetermined mass ratio is 1:23 to 1: 28.

6. The method according to claim 1, wherein the heating temperature is 80-85 ℃ and the heating time is 5-6 h.

7. The method of claim 1, wherein the frequency of the ultrasonic extraction is 35 to 40KHz, and the time of the ultrasonic extraction is 0.8 to 1.5 hours.

8. The method of claim 1, wherein the rotation speed of the centrifugal separation is 3500 to 4500r/min, and the time of the centrifugal separation is not less than 3 min.

9. A morning glory pigment extract liquid, which is produced by the method according to any one of claims 1 to 8.

10. The use of the morning glory pigment extract of claim 9, comprising the steps of:

adding a mordant into the morning glory pigment extracting solution to a second preset pH value to obtain a dyeing solution;

and (3) immersing the silk fiber into a dyeing solution for dyeing to obtain the dyed silk fiber.

Technical Field

The application relates to the technical field of pigment extraction, and particularly relates to a morning glory pigment extraction method, morning glory pigment extracting solution and application thereof.

Background

In the textile industry, textiles are dyed to a desired color by fixing dyes into the textile. Generally, artificial synthetic dyes are adopted for dyeing, so that serious pollution exists in the dyeing process, and dyed textiles can also cause damage to the skin. Therefore, how to prepare natural pigment extracts becomes a major concern.

Morning glory (also called trumpet flower) is a high-quality pigment raw material with gorgeous color and good water solubility. In the related technology, fresh morning glory is soaked in a solvent such as warm water for pigment extraction, and the morning glory pigment extracting solution is extracted.

However, the morning glory pigment extract obtained in the above manner cannot effectively precipitate morning glory pigment, and the obtained morning glory pigment extract has many impurities and a low pigment content.

Disclosure of Invention

The application provides a morning glory pigment extraction method, morning glory pigment extracting solution and application thereof, which are used for extracting and obtaining morning glory pigment extracting solution with less impurities and high pigment content.

In order to achieve the purpose, the application provides the following technical scheme:

in a first aspect, the present embodiments provide a method for extracting morning glory pigment, including:

crushing the dried morning glory, and then sieving the crushed morning glory through a screen to obtain morning glory powder;

heating mixed liquid obtained by mixing morning glory powder and distilled water according to a preset mass ratio;

after the heated mixed solution is cooled, carrying out ultrasonic extraction to obtain an ultrasonic extracting solution;

filtering the ultrasonic extracting solution to obtain filtrate, and performing centrifugal separation on the filtrate;

and (3) regulating the supernatant obtained by centrifugal separation to a first preset pH value, and then dropwise adding a magnesium sulfate solution to obtain the morning glory pigment extracting solution.

Further, the first preset pH value is 9-10, and the concentration of the magnesium sulfate solution is 10%.

Further, adjusting the supernatant obtained by centrifugation to a first predetermined pH, comprising:

adding sodium bicarbonate into the supernatant obtained by centrifugal separation to adjust the pH value to a first preset value.

Further, the screen is a screen of 80-120 meshes.

Further, the preset mass ratio is 1: 23-1: 28.

Further, the heating temperature is 80-85 ℃, and the heating time is 5-6 h.

Furthermore, the frequency of ultrasonic extraction is 35-40 KHz, and the time of ultrasonic extraction is 0.8-1.5 h.

Further, the rotating speed of centrifugal separation is 3500-4500 r/min, and the time of centrifugal separation is not less than 3 min.

Further, the water content of the dried morning glory is below 5%.

The method for extracting morning glory pigment provided by the embodiment of the application has the following beneficial effects:

1. since fresh morning glory is not easy to preserve and contains a large amount of cell sap, the cell sap can influence pigment extraction, so that the pigment extraction is carried out on the basis of the dried morning glory, the preservation problem of the fresh morning glory is solved, and the influence of the cell sap is reduced;

2. mixing the obtained morning glory powder with distilled water, heating, and performing ultrasonic extraction to fully dissolve the pigment in the water, thereby improving the pigment precipitation;

3. filtering the ultrasonic extracting solution, performing centrifugal separation, and fully removing impurities;

4. and taking the supernatant liquid which is separated out of a large amount of pigment and is fully removed of impurities, regulating the pH value, and dropwise adding a magnesium sulfate solution to obtain the morning glory pigment extracting solution which is stable, easy to store, high in pigment content and less in impurities.

In a second aspect, the present embodiments provide a morning glory pigment extract, which is prepared by the morning glory pigment extraction method according to any one of the first aspect.

The morning glory pigment extracting solution provided by the embodiment of the application has the following beneficial effects: the morning glory pigment extract is a natural pigment extract with stable property, easy storage, high pigment content and less impurities.

In a third aspect, the present application provides a use of the morning glory pigment extract solution as described in the second aspect, including the following steps:

adding a mordant into the morning glory pigment extracting solution to a second preset pH value to obtain a dyeing solution;

and (3) immersing the silk fiber into a dyeing solution for dyeing to obtain the dyed silk fiber.

Further, the mordant is an aluminum potassium sulfate dodecahydrate solution with the concentration of 9-11 g/100 mL; the second preset pH value is 2.9-3.1.

Further, immersing the silk fiber into a dyeing solution for dyeing to obtain the dyed silk fiber, comprising:

immersing the silk fiber into the dyeing solution, and dyeing for 0.8-1.2 h at 89-91 ℃ to obtain colored silk fiber;

it is right the silk fibre of coloring washes water, and the chromatic value of silk fibre's water through coloring is in predetermineeing the colourity within range up to, and the fibrous surface of silk of coloring does not have the flooding, obtains the silk fibre after the dyeing.

Further, after obtaining the dyed silk fiber, the method further comprises the following steps:

and soaking the dyed silk fiber in an acid solution or an alkaline solution to obtain the color-changed silk fiber.

Further, the silk fiber is silk satin fabric; soaking the dyed silk fiber in an acid solution or an alkaline solution to obtain the color-changed silk fiber, which comprises the following steps:

soaking the dyed silk fiber in an acid solution to obtain pink silk fiber; or soaking the dyed silk fiber in an alkaline solution to obtain green silk fiber.

Further, the silk fiber is silk loose fiber; soaking the dyed silk fiber in an acid solution or an alkaline solution to obtain the color-changed silk fiber, which comprises the following steps:

soaking the dyed silk fiber in an acid solution to obtain dark brown silk fiber; or soaking the dyed silk fiber in an alkaline solution to obtain green silk fiber.

Further, the acid solution is a citric acid solution with the pH value of 3.8-4.2; the alkaline solution is a sodium bicarbonate solution with the pH value of 8.8-9.2.

The application of the morning glory pigment extracting solution provided by the embodiment of the application has the following beneficial effects:

by adding a mordant into the morning glory pigment extracting solution and adopting a mordant dyeing method to dye, the dyeing fastness is improved; and (3) immersing the silk fiber into the dyeing solution for dyeing to obtain the silk fiber with high dyeing fastness and no formaldehyde.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.

Fig. 1 is a schematic flow chart of a method for extracting morning glory anthocyanidin according to the present embodiment;

fig. 2 is a schematic flow chart illustrating the application of a morning glory pigment extract solution provided in the present application;

fig. 3 is a schematic flow chart of another application of the morning glory pigment extract solution provided in the examples of the present application.

Detailed Description

The principles and spirit of the present application will be described with reference to a number of exemplary embodiments. It should be understood that these embodiments are given solely for the purpose of enabling those skilled in the art to better understand and to practice the present application, and are not intended to limit the scope of the present application in any way. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.

It should be noted that: in the present application, all embodiments and preferred methods mentioned herein can be combined with each other to form new solutions, if not specifically stated. In the present application, all the technical features mentioned herein as well as preferred features may be combined with each other to form new technical solutions, if not specifically stated.

In the present application, percentages (%) or parts refer to percent by weight or parts by weight relative to the composition, unless otherwise specified. In the present application, the components referred to or the preferred components thereof may be combined with each other to form new embodiments, if not specifically stated. In this application, unless otherwise stated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, a numerical range of "6 to 22" means that all real numbers between "6 to 22" have been listed herein, and "6 to 22" is simply a shorthand representation of the combination of these values. The "ranges" disclosed herein may be in the form of lower limits and upper limits, and may be one or more lower limits and one or more upper limits, respectively. In the present application, unless otherwise indicated, the individual reactions or process steps may or may not be performed in sequence. Preferably, the reaction processes herein are carried out sequentially.

Unless otherwise defined, technical and scientific terms used herein have the same meaning as is familiar to those skilled in the art. In addition, any methods or materials similar or equivalent to those described herein can also be used in the present application.

Morning glory (also called trumpet flower) is a high-quality pigment raw material with gorgeous color and good water solubility. However, since the pigment extraction is carried out by directly soaking fresh morning glory in a solvent such as warm water, the morning glory pigment cannot be efficiently separated out, and the obtained morning glory pigment extract has many impurities and a low pigment content.

In order to extract a morning glory pigment extract with less impurities and higher pigment content, the present example provides a method for extracting morning glory pigment, which is shown in fig. 1 and includes the following steps:

step S101: and (4) crushing the dried morning glory, and then sieving the crushed morning glory through a screen to obtain morning glory powder.

Fresh morning glory is easy to deteriorate and rot, and is not easy to transport, so that the morning glory is difficult to store for a long time.

In addition, the vacuole of fresh morning glory contains a large amount of cellular fluid, which is a bubble-like structure in cytoplasm, is wrapped by vacuole membrane, contains aqueous cellular fluid, and contains components such as salt, sugar, carbonic acid, etc. in the cellular fluid. The content of carbonic acid in different morning glory cell sap is different, namely the cell sap has different pH value, so that the color of fresh morning glory is unstable, and the subsequent pigment extraction is influenced.

Based on this, the present example was based on pigment extraction from dried morning glory, solving the preservation problem of fresh morning glory and reducing the influence of the cell sap.

The application does not limit the specific implementation manner of obtaining the dried morning glory, for example: the picked fresh morning glory can be placed in a sunny and ventilated place for airing, and the dried morning glory with lower water content can be obtained after the airing for a proper time.

In some optional embodiments, the dried morning glory has a water content of 5% or less (including 5%), and is dried for 7-9 hours as described above to obtain dried morning glory having a water content of 5% or less.

This application is not restricted to the concrete implementation who carries out shredding with dry morning glory, if smashes dry morning glory in placing rubbing crusher, obtains 30 ~ 300 mesh morning glory granules that differ in size, and wherein rubbing crusher's working parameter can refer to as follows:

the voltage is 200V/50-60 Hz; the power is 2000W; the rotation speed is 28000 r/min.

As described above, the morning glory granules obtained after the pulverization treatment are not uniform in size, and it is difficult for pigment to be precipitated from large morning glory granules. For this reason, dried morning glory is pulverized and sieved.

In some optional embodiments, a 80-120-mesh screen is adopted, and the morning glory particles after the crushing treatment are screened to obtain morning glory powder with uniform size.

Step S102: and heating mixed liquid obtained by mixing morning glory powder and distilled water according to a preset mass ratio.

In practice, if the morning glory powder is mixed with water, the morning glory powder is difficult to dissolve sufficiently in water, and the amount of pigment deposited is still small.

In this example, the morning glory powder was sufficiently dissolved in distilled water by mixing the morning glory powder with distilled water and heating, thereby increasing the amount of the pigment precipitated.

Because the heating temperature is lower, when the heating time is shorter, the pigment precipitation cannot be obviously improved; the pigment is decomposed when the heating temperature is high and the heating time is long. Therefore, the heating temperature cannot be too high or too low, and the heating time cannot be too short or too long.

In some optional embodiments, the heating temperature is 80-85 ℃, the heating time is 5-6 h, so that the heated morning glory powder is fully dissolved with distilled water, and the mixed solution contains more undecomposed pigment.

In addition, when the morning glory powder is mixed with distilled water, if the mass ratio of the morning glory powder to the distilled water is too large, the morning glory powder is difficult to be fully dissolved in the water; if the mass ratio of the two is too small, the pigment concentration is too low. Based on this, the mass ratio of the morning glory powder to the distilled water cannot be too large or too small, and in some alternative embodiments, the preset mass ratio between the morning glory powder and the distilled water is 1:23 to 1: 28.

Step S103: and after the heated mixed solution is cooled, carrying out ultrasonic extraction to obtain an ultrasonic extracting solution.

Since morning glory pigment exists in morning glory cells, complete pigment release cannot be guaranteed after morning glory powder is dissolved in distilled water. Based on the above, after the mixed solution is cooled, ultrasonic extraction is carried out, so that the release of intracellular pigment is accelerated, and the pigment extraction efficiency is improved.

In some optional embodiments, the frequency of ultrasonic extraction is 35 to 40KHz, and the time of ultrasonic extraction is 0.8 to 1.5 h.

Step S104: and filtering the ultrasonic extracting solution to obtain filtrate, and performing centrifugal separation on the filtrate.

In this embodiment, the morning glory pigment needs to be extracted, but the ultrasonic extracting solution contains more impurities, and large-particle impurities can be filtered out by filtering the ultrasonic extracting solution; and then through centrifugal separation, can filter out the tiny particle impurity, obtain the supernatant fluid that the pigment content is high and fully get rid of the impurity.

In the implementation, in order to sufficiently remove impurities, the rotation speed of centrifugal separation cannot be too low, and the time cannot be too short, in some optional embodiments, the rotation speed of centrifugal separation is 3500-4500 r/min, and the time of centrifugal separation is not less than 3min, so that the impurities in the ultrasonic extracting solution are sufficiently removed.

Step S105: and (3) regulating the supernatant obtained by centrifugal separation to a first preset pH value, and then dropwise adding a magnesium sulfate solution to obtain the morning glory pigment extracting solution.

The desired color can be obtained by adjusting the pH of the supernatant. The stability of the extract can be improved by adding a magnesium sulfate solution dropwise, such as: pigment in the extracting solution is more uniform, pigment layering is avoided, and then the extracting solution is used for dyeing, so that the condition of uneven dyeing is reduced. In addition, the magnesium sulfate solution is a salt solution, and the corrosion resistance of the extracting solution is also improved.

In some optional embodiments, the first predetermined pH is 9 to 10, and the purple supernatant is adjusted to blue;

the concentration of the magnesium sulfate solution is 10%, so that the stability of the extracting solution can be effectively improved.

In this embodiment, a specific implementation manner of adjusting the supernatant to the first preset pH is not limited, and optionally, the supernatant is adjusted to the first preset pH by adding sodium bicarbonate.

In this embodiment, the storage manner of the morning glory pigment extract is not particularly limited, and examples thereof include: it can be preserved at normal temperature; or put in a refrigerator for low-temperature refrigeration (4 ℃) for storage in order to prolong the storage life.

The extraction method of the present application will be described in further detail below with reference to specific examples and comparative examples.

Example 1

S1: pulverizing morning glory A1 with water content of 5%, and sieving with 120 mesh sieve to obtain morning glory powder B1;

s2: taking 50g of morning glory powder B1 and distilled water, mixing the mixture according to the mass ratio of 1:23 to obtain a mixed solution, and heating the mixed solution at 80 ℃ for 6 hours to obtain a heated mixed solution C1;

s3: after the heated mixed solution C1 is cooled, carrying out ultrasonic extraction for 1.5h at the frequency of 35KHz to obtain an ultrasonic extracting solution D1;

s4: filtering the ultrasonic extractive solution D1 to obtain filtrate, centrifuging at a rotation speed of 4500r/min for 3min to obtain supernatant E1;

s5: after the pH of the supernatant E1 was adjusted to 9, a 10% magnesium sulfate solution was added dropwise to obtain a morning glory pigment extract F1.

Example 2

S11: pulverizing morning glory A2 with water content of 0.5%, and sieving with 80 mesh sieve to obtain morning glory powder B2;

s12: taking 50g of morning glory powder B2 and distilled water, mixing the mixture according to the mass ratio of 1:28, and heating the mixture at 85 ℃ for 5 hours to obtain a heated mixture C2;

s13: cooling the heated mixed solution C2, and performing ultrasonic extraction for 0.8h at the frequency of 40KHz to obtain an ultrasonic extract D2;

s14: filtering the ultrasonic extract D2 to obtain filtrate, centrifuging at rotation speed of 3500r/min for 5min to obtain supernatant E2;

s15: after the pH of the supernatant E2 was adjusted to 10, a 10% magnesium sulfate solution was added dropwise to obtain a morning glory pigment extract F2.

Example 3

S21: pulverizing morning glory A3 with water content of 3%, and sieving with 100 mesh sieve to obtain morning glory powder B3;

s22: taking 50g of morning glory powder B3 and distilled water, mixing the mixture according to the mass ratio of 1:25, and heating the mixture at 83 ℃ for 5.5h to obtain heated mixture C3;

s23: after the heated mixed solution C3 is cooled, carrying out ultrasonic extraction for 1h at the frequency of 37KHz to obtain an ultrasonic extracting solution D3;

s24: filtering the ultrasonic extracting solution D3 to obtain filtrate, and centrifuging at the rotation speed of 4000r/min for 8min to obtain supernatant E3;

s25: after the pH of the supernatant E3 was adjusted to 9.5, a 10% magnesium sulfate solution was added dropwise to obtain a morning glory pigment extract F3.

Example 4

S31: pulverizing morning glory A4 with water content of 4%, and sieving with 110 mesh sieve to obtain morning glory powder B4;

s32: taking 50g of morning glory powder B4 and distilled water, mixing the mixture according to the mass ratio of 1:27 to obtain a mixed solution, and heating the mixed solution at 84 ℃ for 6 hours to obtain a heated mixed solution C4;

s33: after the heated mixed solution C4 is cooled, carrying out ultrasonic extraction for 1.3h at the frequency of 38KHz to obtain an ultrasonic extracting solution D4;

s34: filtering the ultrasonic extract D4 to obtain filtrate, centrifuging at a rotation speed of 3600r/min for 3min to obtain supernatant E4;

s35: after the pH of the supernatant E4 was adjusted to 9.3, a 10% magnesium sulfate solution was added dropwise to obtain a morning glory pigment extract F4.

Comparative example 1

Only differs from example 3 in that in step S21, fresh morning glory a5 was pulverized and sieved through a 100-mesh sieve to obtain morning glory powder B5; and performing steps S12-S15 based on the morning glory powder B5 to obtain morning glory pigment extract F5.

Comparative example 2

The only difference from example 3 is that, in step S22, the mixed solution is not subjected to the heat treatment. Comparative example 2 yielded a morning glory pigment extract F6.

Comparative example 3

The only difference from example 3 is that in step S22, heating was carried out at 100 ℃ for 5.5 h. Comparative example 3 yielded a morning glory pigment extract F7.

Comparative example 4

The only difference from example 3 is that ultrasonic extraction was not performed through step S23, resulting in a morning glory pigment extract F8.

Comparative example 5

The only difference from example 3 is that in step S23, at a frequency of 20KHz, ultrasonic extraction is performed for 0.2 h. Comparative example 5 yielded a morning glory pigment extract F9.

Comparative example 6

The only difference from example 3 is that the morning glory pigment extract F10 was obtained without filtration in step S24.

Comparative example 7

The only difference from example 3 is that the morning glory pigment extract F11 was obtained without centrifugation in step S24.

Comparative example 8

The only difference from example 3 is that the magnesium sulfate solution was not added dropwise in step S25, and the morning glory pigment extract F12 was obtained.

Comparative example 9

The only difference from example 3 is that in step S25, a 5% magnesium sulfate solution was added dropwise to obtain a morning glory pigment extract F13.

Comparative example 10

The only difference from example 3 is that in step S25, a 20% magnesium sulfate solution was added dropwise to obtain a morning glory pigment extract F14.

The comparison results of the morning glory pigment extract solutions F1 to F14 are shown in table 1:

TABLE 1

Comparing example 3 with comparative example 1, it can be seen that if pigment extraction is performed based on fresh morning glory, the pigment extraction is affected by the cell sap, and the color of the extraction liquid is lighter; the pigment extraction is carried out on the basis of the dried morning glory, so that the influence of cell sap is reduced;

comparing example 3 with comparative example 2, it can be seen that if the mixed solution is not heated, the precipitation amount of the pigment is not significantly increased, and the obtained extract has a lighter color; according to the embodiment of the application, the obtained mixed liquid is heated, so that the morning glory pollen powder is fully dissolved in the distilled water, and the precipitation amount of the pigment is increased;

comparing example 3 with comparative example 3, it can be seen that if the mixed solution is heated at a high temperature, the pigment is decomposed, and the obtained extract has a lighter color; the heating is carried out at the heating temperature adopted in the embodiment of the application, so that the decomposition of the pigment is reduced;

comparing example 3 with comparative examples 4 and 5, it can be seen that if the mixed solution is not subjected to ultrasonic extraction, a large amount of pigment cannot be released, the obtained extract has a lighter color, and the pigment release effect is also affected by the lower frequency and shorter time of ultrasonic extraction. The frequency of ultrasonic extraction is 35-40 KHz, the time of ultrasonic extraction is 0.8-1.5 h, the release of intracellular pigments is accelerated, and the pigment extraction efficiency is obviously improved;

comparing example 3 with comparative example 6, it can be seen that if the ultrasonic extraction solution is not filtered, more large-particle impurities exist in the obtained extraction solution; according to the embodiment of the application, the ultrasonic extracting solution is filtered, so that large-particle impurities can be filtered;

comparing example 3 with comparative example 7, it can be seen that if the filtrate is not centrifuged, the resulting extract has more small particle impurities; in the embodiment of the application, small particle impurities can be filtered out through centrifugal separation;

comparing example 3 with comparative examples 8 and 9, it can be seen that if magnesium sulfate solution or magnesium sulfate solution with lower concentration is not dripped, the obtained extract has poor stability, uneven color, obvious layering and poor corrosion resistance; comparing example 3 with comparative example 10, it can be seen that if the magnesium sulfate solution with too high concentration is added dropwise, the obtained extract has poor stability, uneven color and obvious layering. According to the embodiment of the application, the stability of the extracting solution can be effectively improved by dropwise adding the magnesium sulfate solution with the concentration of 10%.

This example provides the application of the morning glory pigment extract prepared by the above example, referring to fig. 2, including the following steps:

step S201: and adding a mordant into the morning glory pigment extracting solution to a second preset pH value to obtain a staining solution.

In the implementation, the morning glory pigment has good water solubility, and the morning glory pigment in the extracting solution can be directly fixed on the fiber, but has low dyeing fastness and is easy to fade. Based on the method, in order to improve the color fastness, mordant is added into the morning glory pigment extracting solution, and the dyeing is carried out by adopting a mordant dyeing method.

In some optional embodiments, the mordant is a solution of aluminum potassium sulfate dodecahydrate with a concentration of 9-11 g/100 mL; the second preset pH value is 2.9-3.1.

9-11 g/100mL of aluminum potassium sulfate dodecahydrate solution is added into the morning glory pigment extracting solution until the pH value is 2.9-3.1, so that the color fastness can be effectively improved.

Step S202: and (3) immersing the silk fiber into a dyeing solution for dyeing to obtain the dyed silk fiber.

If the temperature is too low and the dyeing time is too short during dyeing, the dyeing fastness is low; if the temperature is too high and the dyeing time is too long during dyeing, the coloring matter in the dyeing solution is decomposed, resulting in poor coloring. Therefore, the temperature at the time of dyeing cannot be excessively high or low, and the dyeing time cannot be excessively short or long.

In addition, the colored silk fiber is at the second preset pH value, which does not meet the fabric production requirements of the basic safety technical specification of the textile products in GB 18401-2010, and the surface of the colored silk fiber has loose color, so that the dyeing solution can be stained on the skin. Therefore, the colored silk fiber is also required to be washed with water.

In some optional embodiments, the silk fiber is immersed in the dyeing solution and dyed at 89-91 ℃ for 0.8-1.2 h to obtain the silk fiber with high dyeing fastness and better coloring; and then carry out the washing to the silk fibre of coloring, until satisfying following two conditions, obtain the silk fibre after the dyeing: 1. the chromatic value of the colored silk fiber water is within the preset chromatic range, the discharged water is clear and has no impurity color, the production requirement of the fabric specified by the national standard is met, and 2, the colored silk fiber surface has no floating color, and the dyeing liquid is prevented from being stained on the skin.

The specific implementation manner of the silk fiber is not limited in this embodiment, and based on the molecular structure of morning glory pigment, morning glory pigment is suitable for being fixed on the mulberry silk fiber, and in some specific implementation manners, mulberry silk fiber can be adopted. In addition, the silk fiber can be satin fabric or loose fiber.

The use of the extract liquid of morning glory anthocyanidin of the present application will be described in further detail with reference to specific examples and comparative examples.

Example 5

S41: adding 9G/100mL aluminum potassium sulfate dodecahydrate solution into the morning glory pigment extracting solution F3 to reach pH3.1 to obtain a dyeing solution G1;

s42: immersing the silk fiber H1 into a dyeing solution G1, and dyeing for 0.8H at 89 ℃ to obtain colored silk fiber I1;

s43: and (3) washing the colored silk fiber I1 until the colorimetric value of water of the colored silk fiber is within a preset colorimetric range and the surface of the colored silk fiber has no flooding color, so that the dyed silk fiber J1 is obtained.

Example 6

S51: adding 11G/100mL aluminum potassium sulfate dodecahydrate solution into the morning glory pigment extracting solution F3 to reach pH2.9, so as to obtain a dyeing solution G2;

s52: immersing silk fiber H1 in dyeing solution G2, and dyeing at 91 ℃ for 1.2H to obtain colored silk fiber I2;

s53: and (3) washing the colored silk fiber I2 until the colorimetric value of water of the colored silk fiber is within a preset colorimetric range and the surface of the colored silk fiber has no flooding color, so that the dyed silk fiber J2 is obtained.

Example 7

S61: adding 10G/100mL aluminum potassium sulfate dodecahydrate solution into the morning glory pigment extracting solution F3 to reach the pH of 3 to obtain a staining solution G3;

s62: immersing the silk fiber H1 into a dyeing solution G3, and dyeing for 1H at 90 ℃ to obtain colored silk fiber I3;

s63: and (3) washing the colored silk fiber I3 until the colorimetric value of water of the colored silk fiber is within a preset colorimetric range and the surface of the colored silk fiber has no flooding color, so that the dyed silk fiber J3 is obtained.

Comparative example 11

The only difference from example 7 was that dyed silk fiber J4 was obtained by using the morning glory pigment extract F3 as a dyeing liquid.

Comparative example 12

The only difference from example 7 is that in step S61, a solution of potassium aluminium sulphate dodecahydrate with a concentration of 2g/100mL is added dropwise to obtain dyed silk fibre J5.

Comparative example 13

The only difference from example 7 is that in step S62, the silk fiber H1 was immersed in the dyeing solution G3 and dyed at normal temperature for 1H, and comparative example 13 gave a dyed silk fiber J6.

Comparative example 14

The only difference from example 7 was that S63 was not performed, and the dyed silk fiber J3 was directly used as dyed silk fiber J7.

The comparison results of the dyed silk fibers J1 to J7 are shown in table 2:

TABLE 2

Comparing example 7 with comparative examples 11 and 12, it can be seen that in the example of the present application, a mordant with an appropriate concentration is added into the morning glory pigment extracting solution, and dyeing is performed by adopting a mordant dyeing method, so that the dyeing fastness can be significantly improved;

comparing example 7 with comparative example 13, it can be seen that the example improves the color fastness compared with the normal temperature dyeing by increasing the temperature during dyeing;

comparing example 7 with comparative example 14, it can be seen that the example of the present application avoids the surface flooding of the silk fibers by washing the colored silk fibers with water.

In addition, in the morning glory pigment extract solutions extracted from the natural morning glory used in the above examples 5 to 7 and comparative examples 11 to 14, no formaldehyde was detected in any of the silk fibers J1 to J7, and therefore, the morning glory pigment extract solution was suitably used for dyeing underwear, such as clothes and home textiles.

It will be appreciated that the dyed silk fibres which have been subjected to water washing are wet cloths which are dried (e.g. by drying at 105 ℃) prior to use.

This example provides another application of the morning glory pigment extract prepared by the above example, referring to fig. 3, including the following steps:

step S301: and adding a mordant into the morning glory pigment extracting solution to a second preset pH value to obtain a staining solution.

Step S302: and (3) immersing the silk fiber into a dyeing solution for dyeing to obtain the dyed silk fiber.

The specific implementation manner of steps S301 to S302 may refer to steps S201 to S202 described above, and will not be described herein again.

Step S303: and soaking the dyed silk fiber in an acid solution or an alkaline solution to obtain the color-changed silk fiber.

The morning glory pigment can present different colors in different acid-base environments, and therefore, the silk fibers with different colors can be obtained by soaking the dyed silk fibers in an acidic solution or an alkaline solution.

The color of the dyed silk fibres when soaked in acidic or alkaline solutions is dependent on the type of silk fibres, and is exemplified by:

1) the silk fiber is silk satin fabric;

soaking the dyed silk fiber in an acid solution to obtain pink silk fiber;

and soaking the dyed silk fiber in an alkaline solution to obtain green silk fiber.

In the implementation, the white silk satin fabric is dyed into brownish red, and the silk satin fabric dyed into the brownish red is soaked in an acid solution to be changed into pink silk satin fabric; the pink silk satin fabric is soaked in clear water for cleaning, and has no obvious fading; soaking the pink silk satin fabric in an alkaline solution to obtain a green silk satin fabric; soaking the silk satin fabric which is changed into green in an acid solution again to change the silk satin fabric into pink silk satin fabric;

dyeing white silk satin fabric into brownish red, and soaking the silk satin fabric dyed into brownish red in alkaline solution to obtain green silk satin fabric; the green silk satin fabric is soaked in clear water for cleaning, and no obvious fading occurs; soaking the green silk satin fabric in an acid solution to obtain pink silk satin fabric; soaking the silk satin fabric which is turned into pink in alkaline solution again to turn into green silk satin fabric;

through the exemplary mode, the silk satin fabric is repeatedly discolored, and a green silk satin fabric or a pink silk satin fabric is obtained according to actual needs.

2) The silk fiber is silk loose fiber;

soaking the dyed silk fiber in an acid solution to obtain dark brown silk fiber;

and soaking the dyed silk fiber in an alkaline solution to obtain green silk fiber.

In the implementation, the silk loose fibers are dyed to be light brown, and the silk loose fibers dyed to be light brown are soaked in an acid solution to be changed into dark brown silk loose fibers; the dark brown silk loose fiber is soaked in clear water for cleaning, and no obvious fading exists; soaking the dark brown silk loose fibers in an alkaline solution to obtain green silk loose fibers; soaking the silk loose fibers which are changed into green in an acid solution again to change the silk loose fibers into dark brown silk loose fibers;

dyeing the silk loose fibers to light brown, and soaking the silk loose fibers dyed to light brown in an alkaline solution to obtain green silk loose fibers; the green silk loose fibers are soaked in clear water for cleaning, and no obvious fading is caused; soaking the green silk loose fibers in an acid solution to obtain dark brown silk loose fibers; soaking the silk loose fibers which are turned into dark brown in the alkaline solution again to turn into green silk loose fibers;

through the exemplary mode, the silk loose fiber is repeatedly discolored, and green silk loose fiber or dark brown silk loose fiber can be obtained according to actual needs.

In this embodiment, the specific implementation manner of the acidic solution and the alkaline solution is not limited, for example, the acidic solution is a citric acid solution with a ph of 3.8-4.2, and the alkaline solution is a sodium bicarbonate solution with a ph of 8.8-9.2.

The dyed silk fibers are soaked in citric acid solution with the pH value of 3.8-4.2 or sodium bicarbonate solution with the pH value of 8.8-9.2, so that the silk fibers are obviously discolored.

The use of the extract liquid of morning glory anthocyanidin of the present application will be described in further detail with reference to specific examples and comparative examples.

Example 8

S71: soaking the white silk satin fabric into the dyeing solution G3, and dyeing for 1h at 90 ℃ to obtain colored silk fiber I4;

s72: and (3) washing the colored silk fiber I4 until the colorimetric value of water of the colored silk fiber is within a preset colorimetric range, and the surface of the colored silk fiber has no flooding color to obtain brownish red silk satin fabric J8.

S73: soaking the brownish red silk satin fabric J8 in a citric acid solution with the pH value of 3.8 to obtain pink silk satin fabric J9; the brownish red silk satin fabric J8 was soaked in sodium bicarbonate solution of pH9.2 to give a green silk satin fabric J10.

Example 9

Only differs from example 8 in that in S73, the brownish-red silk satin fabric J8 is soaked in a citric acid solution at ph4.2 to give a pink silk satin fabric J11; and soaking the brownish red silk satin fabric J8 in a sodium bicarbonate solution with the pH value of 8.8 to obtain a green silk satin fabric J12.

Example 10

Only differs from example 8 in that in S73, the brownish-red silk satin fabric J8 was soaked in a citric acid solution at pH4 to give a pink silk satin fabric J13; the brownish red silk satin fabric J8 was soaked in sodium bicarbonate solution at pH9 to give a green silk satin fabric J14.

Example 11

S81: immersing the silk loose fibers into the dyeing solution G3, and dyeing for 1h at 90 ℃ to obtain colored silk fibers I5;

s82: and (3) washing the colored silk fiber I5 until the colorimetric value of water of the colored silk fiber is within a preset colorimetric range and the surface of the colored silk fiber has no floating color, so as to obtain light brown silk loose fiber J15.

S83: soaking light brown silk loose fibers J15 in citric acid solution with pH of 4.2 to obtain dark brown silk loose fibers J16; light brown silk loose fibers J15 were soaked in sodium bicarbonate solution pH9.2 to obtain green silk loose fibers J17.

Example 12

Only differs from example 11 in that in S83 light brown silk loose fibres J15 are soaked in citric acid solution with ph3.8 to give dark brown silk loose fibres J18; light brown silk loose fibers J15 were soaked in sodium bicarbonate solution of pH8.8 to obtain green silk loose fibers J19.

Example 13

Only differs from example 11 in that in S83 light brown silk bulk fibres J15 were soaked in citric acid solution at pH4 to give dark brown silk bulk fibres J20; light brown silk loose fibres J15 were soaked in sodium bicarbonate solution pH9 to give green silk loose fibres J21.

Comparative example 15

Only the difference from example 8 is that in S73, the color of silk satin J8 did not change significantly when the red brown silk satin J8 was soaked in citric acid solution at pH 6; the brownish red silk satin fabric J8 is soaked in the sodium bicarbonate solution with the pH value of 7.5, and the color of the silk satin fabric J8 is not obviously changed.

Comparative example 16

The only difference from example 11 is that in S83, the color of the silk loose fibres J15 did not change significantly when light brown silk loose fibres J15 were soaked in citric acid solution at pH 6; the light brown silk loose fibers J15 were soaked in a pH7.5 sodium bicarbonate solution, and the color of the silk loose fibers J15 did not change significantly.

Comparing example 8 with comparative example 15, it can be seen that if the dyed silk satin is soaked in a less acidic solution (pH < 7, but close to 7) or in a less basic solution (pH > 7, but close to 7), the color of the silk satin does not change significantly.

Comparing example 11 with comparative example 16, it can be seen that if the dyed silk loose fibres are soaked in a less acidic (pH < 7, but close to 7) solution or in a less basic (pH > 7, but close to 7) solution, the colour of the silk loose fibres does not change significantly.

While the preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all alterations and modifications as fall within the scope of the application.

It will be apparent to those skilled in the art that various changes and modifications may be made in the embodiments of the present application without departing from the spirit and scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application is intended to include such modifications and variations as well.