阅读说明：本技术 一种亚临界法制备板栗壳植物染料的方法及其染色方法 (Method for preparing chestnut shell vegetable dye by subcritical method and dyeing method thereof ) 是由 祝洪哲 于 2021-07-07 设计创作，主要内容包括：一种亚临界法制备板栗壳植物染料的方法及其染色方法,制备方法包括：1)将板栗壳和纯净水加入到亚临界不锈钢设备中,并向亚临界不锈钢设备中加入高温碱性缓冲剂AH,然后加热至亚临界温度,提取板栗壳天然色素,过滤出料；2)在步骤1)过滤后得到的提取液中加入天然染色助剂FA,制成板栗壳植物染料。本发明采用亚临界法制备的板栗壳植物染料,经同浴低温分段染色法,可得到较高的上染率和色牢度,使农林废弃资源可到重新循环利用,改善了环境,也使植物染色后的纺织品更安全、环保。(A method for preparing plant dye of chestnut shell by subcritical method and dyeing method thereof, the preparation method comprises: 1) adding chestnut shells and purified water into subcritical stainless steel equipment, adding a high-temperature alkaline buffer AH into the subcritical stainless steel equipment, heating to subcritical temperature, extracting natural pigments of the chestnut shells, filtering and discharging; 2) adding a natural dyeing auxiliary agent FA into the extracting solution obtained after filtering in the step 1) to prepare the chestnut shell vegetable dye. The chestnut shell vegetable dye prepared by the subcritical method can obtain higher dye-uptake and color fastness by a one-bath low-temperature sectional dyeing method, so that agricultural and forestry waste resources can be recycled, the environment is improved, and the textile dyed by the plant is safer and more environment-friendly.)

1. A method for preparing chestnut shell plant dye by a subcritical method is characterized by comprising the following steps:

1) adding chestnut shells and purified water into subcritical stainless steel equipment, adding a high-temperature alkaline buffer AH into the subcritical stainless steel equipment, heating to subcritical temperature, extracting natural pigments of the chestnut shells, filtering and discharging;

2) adding a natural dyeing auxiliary agent FA into the extracting solution obtained after filtering in the step 1) to prepare the chestnut shell vegetable dye.

2. The method for preparing the chestnut shell plant dye by the subcritical method according to claim 1, wherein the weight ratio of the chestnut shells to the purified water in the step 1) is 1: 5-10, and the added high-temperature alkaline buffer AH accounts for 0.3-2% of the total weight of the purified water.

3. The method for preparing the plant dye for the chestnut shells by the subcritical method according to claim 1, wherein the subcritical temperature in the step 1) is 120-135 ℃, the extraction time is 20-50 minutes, the temperature is reduced to below 60 ℃ after the extraction, and the material is filtered and discharged.

4. The subcritical method for preparing chestnut shell vegetable dye according to claim 1, wherein the dosage of the natural dyeing auxiliary agent FA accounts for 0.5-10% of the total weight of the extracting solution, the natural dyeing auxiliary agent FA is added under stirring, the stirring is carried out for 20-30 minutes to prepare the chestnut shell vegetable dye, and the filtering and discharging are carried out.

5. The method for preparing chestnut shell vegetable dye by subcritical process according to claim 1, characterized in that chestnut shells are selected which are peeled by mechanical peeling machine.

6. A dyeing method for preparing chestnut shell vegetable dye by a subcritical method is characterized in that the adopted chestnut shell vegetable dye is prepared by the method for preparing chestnut shell vegetable dye by the subcritical method according to any one of claims 1 to 5, and specifically comprises the following steps: the method comprises the steps of dyeing the chestnut shell plant dye at a low temperature of below 90 ℃ for 50-80 minutes, adding a natural dyeing auxiliary agent AE in a same bath for further dyeing for 20-35 minutes, washing the dyed chestnut shell plant dye with water at 75-90 ℃, and fixing the chestnut shell plant dye with a natural fixing agent LG at 75-90 ℃ for 20-30 minutes.

7. The dyeing method for preparing the plant dye for the chestnut shells by the subcritical method according to claim 6, wherein the bath ratio of dyeing is 1: 6-20, the bath ratio of washing after dyeing is 1: 6-20, and the fixing bath ratio after dyeing is 1: 6-20.

8. The dyeing method for preparing the chestnut shell vegetable dye by the subcritical method according to claim 6, wherein the dosage of the chestnut shell vegetable dye is 5-25% of the weight of the dyed textile.

9. The dyeing method for preparing the chestnut shell vegetable dye by the subcritical method according to claim 6, wherein the natural dyeing auxiliary AE accounts for 5-30% of the weight of the dyed textile; the dosage of the natural color fixing agent LG is 1-3% of the weight of the dyed textile.

Technical Field

The invention relates to the field of natural plant dye research and development and production, in particular to a method for preparing a chestnut shell plant dye by a subcritical method and a dyeing method thereof.

Background

The Chinese chestnut originates from China, is distributed in 26 provinces in China, is rich in starch, sugar and various vitamins, is a delicacy on a dining table and a fruit which people like to eat during leisure, and has the functions of tonifying the kidney and strengthening the bones and muscles. The Chinese chestnut in south area has no peeling for three days, and the kernel becomes black and rotten. The inner skin peeling machine for Chinese chestnut is used in factory to peel the outer shell of raw or cooked Chinese chestnut.

The bracts outside the chestnuts contain more tannin substances and can be used for plant dyeing, but the bracts are generally extracted in time in the harvest season, so that the seasonality is strong, and more residues are generated. The invention does not use the bract on the outer layer of the chestnut shell, directly adopts the chestnut shell peeling machine, can peel off the raw chestnut shell and the cooked chestnut shell, has the advantages of difficult decay and long shelf life, can be used for extraction and processing all the year round, has less residue after pigment extraction of the chestnut shell, solves the problem of field, can be used for preparing the active carbon by using the extracted chestnut shell, and has better adsorption performance of the prepared active carbon.

Subcritical Water Extraction (Subcritical Water Extraction) is a green and environment-friendly Extraction technology, Water is gradually changed from strong polarity to weak polarity or nonpolar in a Subcritical state, hydrogen bonds of Subcritical Water are opened or weakened, the dissolving capacity of Subcritical Water on fat-soluble components is similar to that of an organic solvent, and supercritical fluid (supercritical CO) is adopted₂Mainly) can be applied to the Extraction of substances with strong polarity and higher relative molecular mass in traditional Chinese medicinal materials, and just compensates CO₂The deficiency of supercritical fluid extraction. The chestnut shells are extracted with pigments in a subcritical manner to prepare the vegetable dye, so that the use of conventional flammable and explosive solvents such as ethanol and the like is avoided, and the extraction process is safer and more environment-friendly. The subcritical high-temperature and high-pressure extraction of the pigment also plays a role in sterilization, and the shelf life of the chestnut shell pigment is prolonged.

Disclosure of Invention

The invention aims to provide a method for preparing chestnut shell vegetable dye by a subcritical method and a dyeing method thereof.

In order to achieve the purpose, the invention adopts the following technical scheme:

a method for preparing chestnut shell plant dye by a subcritical method comprises the following specific steps:

1) adding chestnut shells and purified water into subcritical stainless steel equipment, adding a high-temperature alkaline buffer AH into the subcritical stainless steel equipment, heating to subcritical temperature, extracting natural pigments of the chestnut shells, filtering and discharging; taking out the extracted chestnut shells after extraction, naturally airing, and preparing the chestnut shells into biofuel or active carbon.

2) Adding a natural dyeing auxiliary agent FA into the extracting solution obtained after filtering in the step 1) to prepare the chestnut shell vegetable dye.

The weight ratio of chestnut shells to the purified water in the step 1) is 1: 5-10, and the added high-temperature alkaline buffer AH accounts for 0.3-2% of the total weight of the purified water.

The subcritical temperature in the step 1) is 120-.

The dosage of the natural dyeing auxiliary agent FA accounts for 0.5-10% of the total weight of the extracting solution, a stirrer is started, the natural dyeing auxiliary agent FA is added under the stirring state, the stirring is carried out for 20-30 minutes, and the chestnut shell vegetable dye is prepared, filtered and discharged.

Selecting clean chestnut shells which are not mildewed and are peeled by a mechanical peeling machine.

A dyeing method for preparing chestnut shell vegetable dye by a subcritical method is characterized in that the adopted chestnut shell vegetable dye is prepared by the method for preparing chestnut shell vegetable dye by the subcritical method, and specifically comprises the following steps: the method comprises the steps of adopting a low-temperature one-bath sectional dyeing method, dyeing for 50-80 minutes by adopting a chestnut shell plant dye at a low temperature below 90 ℃, then adding a natural dyeing auxiliary agent AE in one bath for further dyeing for 20-35 minutes, washing with water at 75-90 ℃ once after dyeing, and then fixing the color for 20-30 minutes at 75-90 ℃ by using a natural color fixing agent LG.

The bath ratio of dyeing is 1: 6-20, the bath ratio of washing after dyeing is 1: 6-20, and the fixing bath ratio after dyeing is 1: 6-20.

The dosage of the chestnut shell vegetable dye is 5 to 25 percent of the weight of the dyed textile.

The dosage of the natural dyeing auxiliary AE is 5-30% of the weight of the dyed textile; the dosage of the natural color fixing agent LG is 1-3% of the weight of the dyed textile.

Compared with the prior art, the invention has the beneficial effects that:

the invention adopts subcritical water extraction method, avoids using flammable and explosive organic solvent, and makes the extraction process safer and more environment-friendly. Subcritical high temperature and high pressure change the polarity of water, and improve permeability. The chestnut shell is a shell mainly made of lignin, pigments are contained in a three-dimensional grid of the lignin, and the lignin is a firm organism and is difficult to degrade. Partial nodes of the lignin three-dimensional grid can be effectively opened by adopting subcritical high temperature and high pressure, and pigment dissolution is facilitated. The subcritical extraction of the pigment also has the sterilization effect, and the shelf life of the chestnut shell pigment is prolonged. Partial pigment is converted in a subcritical state, the color value is improved, and the high-temperature-stability high-light-fastness-light-fastness-light-does not only have a little.

The subcritical water extraction method adopted by the invention does not simply use pure water as dissolution, but adds a high-temperature alkaline buffer with eutectic property, so that the antibacterial property of the chestnut shell pigment is maintained after extraction, and the chestnut shell pigment can effectively inhibit staphylococcus aureus, candida albicans, escherichia coli, bacillus subtilis and the like. The subcritical water extraction method has short production period and controllable production quality, is a clean and environment-friendly production mode suitable for large-scale production, does not discharge waste water in the whole production process, has high resource utilization rate and does not pollute the environment. Can replace partial chemical dye, and avoid the harm to human body and environmental pollution in the production process of the chemical dye.

The chestnut shell plant dye prepared by the subcritical method adopts a one-bath low-temperature sectional dyeing method, the dye uptake is higher than that of a traditional direct dyeing method, a pre-mordant dyeing method, a same-mordant dyeing method, a post-mordant dyeing method and the like by more than 30%, and the color fastness is improved by 0.5-1 level. The dyed textile meets all requirements of A class in the national basic safety technical specification GB 18401-.

The chestnut shell vegetable dye prepared by the subcritical method can be used for plant dyeing of fibers, yarns, fabrics and clothes such as cotton, hemp, tencel, modal, wool, silk and the like, so that agricultural and forestry waste resources can be recycled, the environment is improved, and the textile dyed by the plants is safer and more environment-friendly.

Detailed Description

The present invention will be described in detail with reference to examples, but the scope of the present invention is not limited to the examples described below.

The first embodiment is as follows:

1. the subcritical method for preparing the chestnut shell plant dye comprises the following steps:

selecting clean chestnut shells which are not mildewed and are peeled by a mechanical peeling machine, adding the chestnut shells and purified water into subcritical stainless steel equipment, wherein the weight ratio of the chestnut shells to the purified water is 1:6, and adding a high-temperature alkaline buffer AH into the subcritical stainless steel equipment, wherein the added high-temperature alkaline buffer AH accounts for 1% of the total weight of the purified water. Then heating to the subcritical extraction temperature of 125 ℃, extracting for 35 minutes, cooling to below 60 ℃ after extraction, filtering and discharging.

Taking out the extracted chestnut shells after extraction, naturally airing, and preparing the chestnut shells into biofuel or active carbon. Adding natural dyeing auxiliary agent FA into the extractive solution with a dosage of 6% (relative to the total weight of the subcritical extractive solution of chestnut shell), starting a stirrer, adding natural dyeing auxiliary agent FA under stirring, stirring for 30 min to obtain chestnut shell vegetable dye, filtering, and discharging.

2. The dyeing method for preparing the chestnut shell plant dye by the subcritical method comprises the following steps:

the chestnut shell vegetable dye is adopted, the dyeing bath ratio (the weight ratio of dyed cotton, hemp, silk, wool, tencel, modal, viscose and other textiles to dyeing water) is 1:12, the dosage of the chestnut shell vegetable dye is 10% of the weight of the dyed textiles, the dyed textiles are dyed for 70 minutes at the low temperature below 75 ℃, then a natural dyeing auxiliary agent AE is added in the same bath at the 15% of the weight of the dyed textiles, the dyeing is continued for 30 minutes, the dyed textiles are washed once by water at the temperature of 75 ℃, then the color is fixed for 25 minutes at the temperature of 75 ℃ by using the natural color fixing agent LG at the dosage of 2% of the weight of the dyed textiles.

The chestnut shell vegetable dye prepared by the subcritical method adopts a one-bath low-temperature sectional dyeing method, the dye uptake is higher than that of the traditional direct dyeing method, pre-mordant dyeing method, same mordant dyeing method, post-mordant dyeing method and the like by more than 30%, and the color fastness is improved by 1 level. The dyed textile meets all requirements of A class in the national basic safety technical specification GB 18401-.

The dyed textile is soaped for 30 minutes at 40 ℃ by 5g/l (proportion of total liquid amount) of standard soap chips, and the soaping fastness is measured to be more than 4 grade.

Example two:

1. the method for preparing the chestnut shell plant dye by the subcritical method comprises the following steps:

selecting clean chestnut shells which are not mildewed and are peeled by a mechanical peeling machine, adding the chestnut shells and purified water into subcritical stainless steel equipment, wherein the weight ratio of the chestnut shells to the purified water is 1:10, and adding a high-temperature alkaline buffer AH into the subcritical stainless steel equipment, wherein the added high-temperature alkaline buffer AH accounts for 2% of the total weight of the purified water. Then heating to 120 ℃ of subcritical extraction temperature, extracting for 50 minutes, cooling to below 60 ℃ after extraction, filtering and discharging.

Taking out the extracted chestnut shells after extraction, naturally airing, and preparing the chestnut shells into biofuel or active carbon. Adding natural dyeing auxiliary agent FA into the extractive solution with a dosage of 4% (relative to the total weight of the subcritical extractive solution of chestnut shell), starting a stirrer, adding natural dyeing auxiliary agent FA under stirring, stirring for 30 min to obtain chestnut shell vegetable dye, filtering, and discharging.

2. The dyeing method for preparing the chestnut shell plant dye by the subcritical method comprises the following steps:

the method is characterized in that chestnut shell vegetable dye is adopted, the ratio of dyeing baths (the weight ratio of dyed cotton, hemp, silk, wool, tencel, modal, viscose and other textiles to dyeing water) is 1:12, the dosage of the chestnut shell vegetable dye is 20% of the weight of the dyed textiles, the dyed textiles are dyed for 70 minutes at the low temperature below 75 ℃, then natural dyeing auxiliary agents AE is added in the same bath at the dosage of 10% of the weight of the dyed textiles, the dyeing is continued for 30 minutes, the dyed textiles are washed once at the low temperature of 75 ℃, then the dyed textiles are fixed for 25 minutes at the temperature of 75 ℃ by using the natural color fixing agent LG at the dosage of 1.5% of the weight of the dyed textiles.

After the dyed textile is soaped for 30 minutes at 40 ℃ by 5g/l (proportion of total liquid amount) of standard soap chips, the soaping fastness is measured to be more than 4 grade

Example three:

1. the method for preparing the chestnut shell plant dye by the subcritical method comprises the following steps:

selecting clean chestnut shells which are not mildewed and are peeled by a mechanical peeling machine, adding the chestnut shells and purified water into subcritical stainless steel equipment, wherein the weight ratio of the chestnut shells to the purified water is 1:6, and adding a high-temperature alkaline buffer AH into the subcritical stainless steel equipment, wherein the added high-temperature alkaline buffer AH accounts for 4% of the total weight of the purified water. Then heating to 130 ℃ of subcritical extraction temperature, extracting for 20 minutes, cooling to below 60 ℃ after extraction, filtering and discharging.

Taking out the extracted chestnut shells after extraction, naturally airing, and preparing the chestnut shells into biofuel or active carbon. Adding natural dyeing auxiliary agent FA into the extractive solution with an amount of 8% (relative to the total weight of the subcritical extractive solution of chestnut shell), starting a stirrer, adding natural dyeing auxiliary agent FA under stirring, stirring for 30 min to obtain chestnut shell vegetable dye, filtering, and discharging.

2. The dyeing method for preparing the chestnut shell plant dye by the subcritical method comprises the following steps:

the method is characterized in that chestnut shell vegetable dye is adopted, the ratio of dyeing baths (the weight ratio of dyed cotton, hemp, silk, wool, tencel, modal, viscose and other textiles to dyeing water) is 1:12, the dosage of the chestnut shell vegetable dye is 15% of the weight of the dyed textiles, the dyed textiles are dyed for 70 minutes at the low temperature below 75 ℃, then natural dyeing auxiliary agents AE is added in the same bath at the dosage of 20% of the weight of the dyed textiles, the dyeing is continued for 30 minutes, the dyed textiles are washed once at the low temperature of 75 ℃, then the dyed textiles are fixed for 25 minutes at the temperature of 75 ℃ by using natural color fixing agents LG at the dosage of 2.5% of the weight of the dyed textiles.

The chestnut shell vegetable dye prepared by the subcritical method adopts a one-bath low-temperature sectional dyeing method, the dye uptake is higher than that of the traditional direct dyeing method, pre-mordant dyeing method, same mordant dyeing method, post-mordant dyeing method and the like by more than 30%, and the color fastness is improved by 1 level. The dyed textile meets all requirements of A class in the national basic safety technical specification GB 18401-.