CN102153882A - Method for extracting and dyeing reddish-brown natural dye of oil-tea camellia shells - Google Patents
Method for extracting and dyeing reddish-brown natural dye of oil-tea camellia shells Download PDFInfo
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Abstract
The invention discloses a method for extracting and dyeing reddish-brown natural dye of oil-tea camellia shells. After cleaned and air-dried, the oil-tea camellia shell is smashed and leached with taking sodium carbonate aqueous solution as solvent. Filtered filter residues are repeatedly leached with the sodium carbonate aqueous solution. Filtrate is combined to obtain natural dye concentrate of the oil-tea camellia shell by pressure reduction, distillation and concentration. The obtained concentrate is subjected to pectin removal, filtration, pressure reduction, distillation, concentration, spray and drying to obtain the powder natural dye of the oil-tea camellia shell. Pretreated pure cotton fabric can be dyed with the natural dye of the oil-tea camellia shell to obtain fabric which is uniform in gloss. The method for extracting and dyeing the natural dye of the oil-tea camellia shell is safe and environment-friendly by taking the oil-tea camellia shell as a raw material so as to effectively utilize natural waste. The fabric dyed by the method can be made into clothing that is safe, free of carcinogenic and deforming action or causing skin sensibility, good in compatibility with ecological environment and available for biodegradation.
Description
Technical field
The present invention relates to a kind of extraction and dyeing process of reddish-brown natural dyestuff, relate to the reddish brown natural dyestuff of a kind of oil-tea camellia husks more specifically and extract and dyeing process.
Technical background
The natural pigment safety non-toxic particularly is subjected to liking of people.Advocate today of health, back to nature and promotion environment protection in the whole world; synthetic dyestuff more and more are subjected to people's attention to the nocuity of human body with to the shortcomings such as pollution of environment; and the herbal medicine natural dyestuff extracts from organism, has good Environmental compatibility and biological degradability.And modern study shows, the herbal medicine natural dyestuff is in dyeing course, its drug activity composition, aromatising flavour composition and natural pigment are absorbed by fabric together, make the fabric after the dyeing have special medicinal health-care function, as antibiotic, anti-inflammatory, insect protected, antianaphylaxis, antitumor, anti-oxidant, radioprotective, step-down, stimulate circulation or the like.Therefore, herbal medicine be raw material natural dyestuff research and use the favor more and more be subjected to people.
Oil tea is that the whole world four is big woody one of with oil plants, is the advantageous natural resources of China, and according to statistics, there are oil tea 36.67 ten thousand mm in China
2, annual produce oil 1,500,000,000 kg, this will bring the oil-tea camellia husks of more than 100 hundred million kg.Oil-tea camellia husks has very high comprehensive utilization value, because the content of xylogen and pentosan is higher in the oil-tea camellia husks, therefore the utilization research at oil-tea camellia husks also concentrates in the preparation of furfural, gac, tea saponin and Xylitol at present, and the pigment composition that oil-tea camellia husks contains is developed as yet effectively.
Chinese patent application, application number are 201010221929.9, and name is called: " a kind of method of extracting brown pigments from oil-tea camellia husks ", it has introduced a kind of method of extracting brown pigments from the oil tea fruit.Liu Xiaogeng (" composition analysis of oil tea byproduct and utilization research ", grain and fodder industry, 1993 (4): 47-51) composition analysis of having reported the oil tea byproduct with utilize research, experiment utilizes microwave exposure heating and the optimum extraction process by orthogonal test research oil-tea camellia husks brown pigments, study the stability of pigment simultaneously, for the comprehensive development and utilization of oil-tea camellia husks provides reference.Ling Chengde etc. (" homemade edible natural pigment oil-tea camellia husks brown pigments toxicity test ", Chinese Journal of Preventive Medicine, 1985,19 (1): 16) reported homemade edible natural pigment tea fruit shell brown pigment toxicity test, pointed out that the oil-tea camellia husks brown pigments is a kind of safe natural food colour.Extraction and the stable report that study of people to oil tea fruit pigment do not arranged at present as yet.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of extract from oil-tea camellia husks reddish-brown natural dyestuff method and dyeing thereof are provided.It is raw material with the oil-tea camellia husks, effectively utilizes natural waste, safety and environmental protection, and the clothes safety that DYED FABRICS makes does not have carcinogenic, teratogenesis or causes skin allergy, and is good, biodegradable with the ecotope consistency.
The technical scheme that the present invention is adopted for its technical problem of solution is: the extracting method of the reddish brown natural dyestuff of a kind of oil-tea camellia husks has following processing step:
(1) raw material pre-treatment: clean oil-tea camellia husks with hot water, after airing or the oven dry oil-tea camellia husks is smashed.Adopt hot water to clean oil-tea camellia husks, can effectively remove the oil-tea camellia husks surface contaminants fast, it is cleaner to clean the back oil-tea camellia husks, can improve the purity of natural dyestuff like this, and oil-tea camellia husks is pulverized, and can increase the contact area of material and liquid, accelerates extraction rate.
(2) lixiviate separates: with the oil-tea camellia husks that crushes aqueous sodium carbonate lixiviate, the pH of the aqueous solution is 8-12, extracts 2-4 hour down at temperature 40-80 ℃, and solid-liquid ratio is volume ratio 1: 5-20, filters then, must contain the filtrate and the filter residue of natural dyestuff;
(3) concentrated removing photoresist: with the extracting solution concentrating under reduced pressure, evaporate the wherein moisture of 60wt%-80wt%, the pH value that will concentrate the back vat liquor again adopts the aqueous hydrochloric acid of 5wt%-10wt% to transfer to 2-6, add ethanol with the pectin Impurity removal in the concentrated solution, regulate the alcoholic acid volume fraction to 60%-90%; After having filtered pectin impurity at last, adopt the aqueous sodium hydroxide solution of 20wt%-30wt% to transfer to 8-12 the pH value of cleaner liquid, stir to leave standstill after 4-8 hour and extract supernatant liquid, in that being inserted in the vacuum concentration pot, the supernatant liquor that extracts concentrates, keep temperature be 40-80 ℃ until the ethanol removal that will add wherein, reclaim ethanol, obtain the concentrated solution of natural dyestuff.
Adopt aforesaid method, can reduce alcoholic acid consumption, the natural dyestuff solution concentration of extracting is removed photoresist, can improve the purity of oil-tea camellia husks natural dyestuff.
(4) be dried to powder: adopt the aqueous acetic acid of 10wt%-20wt% to transfer to 6-8 the concentrated solution pH value of natural dyestuff, the concentrated solution with natural dyestuff is heated to 40-80 ℃ of after-filtration then, and drying makes the Powdered natural dyestuff of reddish-brown.The right dyestuff of oil tea fruit Nan Tian is dried to powder, can reaches the stable purpose of depositing of oil-tea camellia husks natural dyestuff.
As preferably, the extracting method of the reddish brown natural dyestuff of described oil-tea camellia husks has following processing step:
(1) raw material pre-treatment: clean oil-tea camellia husks with 30-60 ℃ hot water, behind the natural air drying tea fruit shell smashed order to 30-70;
(2) lixiviate separates: with the oil-tea camellia husks that crushes aqueous sodium carbonate lixiviate, the pH of the aqueous solution is 8-12, extracts 2-4 hour down at temperature 40-80 ℃, and solid-liquid ratio is volume ratio 1: 5-20, filters then, must contain the filtrate and the filter residue of natural dyestuff; In order to realize efficient rapid extraction oil-tea camellia husks natural dyestuff, can adopt the multiple extraction filter residue of aforesaid method, extraction time is 2-4 time;
(3) concentrated removing photoresist: with the extracting solution concentrating under reduced pressure, evaporate the wherein moisture of 60wt%-80wt%, the pH value that will concentrate the back vat liquor again adopts the aqueous hydrochloric acid of 5wt%-10wt% to transfer to 2-6, add ethanol with the pectin Impurity removal in the concentrated solution, regulate the alcoholic acid volume fraction to 60%-90%; The pH value of having filtered at last behind the pectin impurity cleaner liquid adopts the aqueous sodium hydroxide solution of 20wt%-30wt% to transfer to 8-12, stir to leave standstill after 4-8 hour and extract supernatant liquid, in that being inserted in the vacuum concentration pot, the supernatant liquor that extracts concentrates, keep temperature be 40-80 ℃ until the ethanol removal that will add wherein, reclaim ethanol, obtain the concentrated solution of natural dyestuff;
(4) be dried to powder: adopt the aqueous acetic acid of 10wt%-20wt% to transfer to 6-8 the concentrated solution pH value of natural dyestuff, the concentrated solution with natural dyestuff is heated to 40-80 ℃ of after-filtration then, and drying makes the Powdered natural dyestuff of reddish-brown.
As preferably, the extracting method of the reddish brown natural dyestuff of described oil-tea camellia husks has following processing step:
(1) raw material pre-treatment: adopt 40-50 ℃ hot water to clean oil-tea camellia husks, behind the natural air drying tea fruit shell smashed order to 50-60;
(2) lixiviate separates: with the oil-tea camellia husks that crushes aqueous sodium carbonate lixiviate, the pH of the aqueous solution is 9-10, extracts 3 hours down at temperature 50-60 ℃, and solid-liquid ratio is volume ratio 1: 10-15, filters then, must contain the filtrate and the filter residue of natural dyestuff; In order to realize efficient rapid extraction oil-tea camellia husks natural dyestuff, adopt the multiple extraction filter residue of aforesaid method, extraction time is 3 times;
(3) concentrated removing photoresist: with the extracting solution concentrating under reduced pressure, evaporate the wherein moisture of 70wt%-75wt% number, the pH value that will concentrate the back vat liquor again adopts the aqueous hydrochloric acid of 5wt%-10wt% to transfer to 3-5, add ethanol with the pectin Impurity removal in the concentrated solution, regulate the alcoholic acid volume fraction to 70%-85%; The pH value of having filtered at last behind the pectin impurity cleaner liquid adopts the aqueous sodium hydroxide solution of 20wt%-30wt% to transfer to 9-10, stir to leave standstill after 5-6 hour and extract supernatant liquid, in that being inserted in the vacuum concentration pot, the supernatant liquor that extracts concentrates, keep temperature be 50-70 ℃ until the ethanol removal that will add wherein, reclaim ethanol, obtain the concentrated solution of natural dyestuff;
(4) be dried to powder: adopt the aqueous acetic acid pH value of 10wt%-20wt% to transfer to 7 the concentrated solution of natural dyestuff, the concentrated solution with natural dyestuff is heated to 50-70 ℃ of after-filtration then, and drying makes the Powdered natural dyestuff of reddish-brown.
The dry spray-drying process that adopts of the concentrated solution of natural dyestuff, its inlet temperature is 160-220 ℃, temperature out is 80-90 ℃.
As preferably, its inlet temperature is 170-190 ℃, and temperature out is 83-85 ℃.
The pure cotton dyeing method of the reddish brown natural dyestuff of the prepared oil-tea camellia husks of the extracting method of aforesaid oil-tea camellia husks natural dyestuff, the pre-treatment and the pure cotton dyeing two procedures that comprise cotton fabric, the pre-treatment of cotton fabric mainly are in order to overcome the problem of natural dyestuff and colour fastness difference low at the pure cotton fabric dye uptake.The pre-treating process of cotton fabric is the preparation 2-8 grams per liter cation modifier aqueous solution, puts into wherein after pure cotton fabric is cleaned, and room temperature dipping 2-10 minute pads 75-90 ℃ of oven dry; The dyestuff quality is the 0.5-8% of fabric quality in the pure cotton dyeing technology, and bath raio 1: 10-40 contaminated 30-90 minute down at 50-80 ℃, and taking-up fabric, acidity are soaped, clean, dried.Adopt above-mentioned processing condition that pure cotton fabric is dyeed, can make the oil-tea camellia husks natural dyestuff on the pure cotton fabric after the processing, obtain high dye uptake.
As preferably, the pre-treating process of cotton fabric is the preparation 5-6 grams per liter cation modifier aqueous solution, put into wherein after will pure cotton fabric cleaning, and room temperature dipping 4-6 minute, two soak two rolls, 80-85 ℃ of oven dry; The dyestuff quality is the 3-4% of fabric quality in the pure cotton dyeing technology, and bath raio 1: 20-30 contaminated 50-70 minute down at 60-70 ℃, and taking-up fabric, acidity are soaped, clean, dried.
In order to guarantee the quality of oil-tea camellia husks natural dye dying pure cotton fabric, improve its washing fastness, described acidity is soaped to acid scouring agent oil-tea camellia husks natural dye dying pure cotton fabric being cleaned, acid scouring agent is the solution that 1-5: 1-3: 5-15: 77-93 forms with the weight ratio by side chain Soxylat A 25-7, the water of sodium polyacrylate, polypyrrole alkane ketone, C13, and its pH value is 5-7.
The dyeing pure cotton fabric color and luster that makes as stated above is even, and value of chromatism Δ E is less than 0.20, and dye uptake reaches more than 80%.
The invention has the beneficial effects as follows that the present invention had both met environmental protection concept, satisfied consumers in general's demand simultaneously again.Effectively utilize natural waste, its extraction process is simple, the processing condition gentleness, and preparation cycle is short, and facility investment is few, and waste water reusable edible, waste material also can be made fodder additives, are fit to serialization, extensive chemical industry production.The clothes safety that DYED FABRICS makes does not have carcinogenic, teratogenesis or causes skin allergy, and has effects such as sterilization, and is good with the ecotope consistency, biodegradable.
Embodiment
To help to understand the present invention by following actually operating and embodiment, but not limit content of the present invention.
Embodiment one
Adopt 30 ℃ of warm water to clean oil-tea camellia husks, behind the natural air drying, take by weighing 100 grams, mechanical disintegration to 30 order, add aqueous sodium carbonate and carry out lixiviate, the pH of the aqueous solution is 8, extracts 2 hours down for 40 ℃ in temperature, solid-liquid ratio is 1: 5, filters then, must contain natural dyestuff filtrate and filter residue.Adopt the multiple extraction filter residue of aforesaid method, extraction time is 2 times.To the extracting solution concentrating under reduced pressure, evaporation is 60% moisture wherein, and the pH value that will concentrate the back vat liquor again transfers to 2 with the aqueous hydrochloric acid that adopts 5wt%, adds ethanol with the pectin Impurity removal in the concentrated solution, regulates alcoholic acid volume fraction to 60%.The pH value of having filtered at last behind the pectin impurity cleaner liquid transfers to 8 with the 20wt% sodium hydroxide lye, stir to leave standstill after 4 hours and extract supernatant liquid, concentrate in that the supernatant liquor that extracts is inserted in the vacuum concentration pot, keep temperature to be 40 ℃ and remove recovery ethanol until the ethanol that will add wherein.At first concentrated solution pH value is transferred to 6 with the aqueous acetic acid of 10wt%, then concentrated solution is heated to 40 ℃ of after-filtration, carry out spraying drying again, inlet temperature is 160 ℃, and temperature out is 80 ℃, makes the Powdered natural dyestuff of reddish-brown.
The pure cotton dyeing method of the reddish brown natural dyestuff of the prepared oil-tea camellia husks of the extracting method of oil-tea camellia husks natural dyestuff, the pre-treatment and the pure cotton dyeing two procedures that comprise cotton fabric, the pre-treating process of cotton fabric is the preparation 2 grams per liter cation modifier aqueous solution, to put into wherein after the pure cotton fabric cleaning, room temperature dipping 2 minutes, two soak two rolls, 75 ℃ of oven dry; The HS-PY that the cation modifier aqueous solution adopts Hansi Chemical Article Co., Ltd., Changzhou to produce.
To carrying out the pure cotton fabric dyeing of pre-treatment, the dyeing condition is: dye strength 2%, and bath raio 1: 10 was contaminated 30 minutes down at 50 ℃, and taking-up fabric, acidity are soaped, clean, are dried.The dyeing pure cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.15, and dye uptake reaches 80%.
Acidity is soaped and is adopted acid scouring agent that oil-tea camellia husks natural dye dying pure cotton fabric is cleaned, acid scouring agent is 1: 1: 5 by side chain Soxylat A 25-7, the water of sodium polyacrylate, polypyrrole alkane ketone, C13 with weight ratio: 93 solution of forming, its pH value is 5.
Embodiment two
Adopt 40 ℃ of warm water to clean oil-tea camellia husks, behind the natural air drying, take by weighing 100 grams, mechanical disintegration to 50 order, add aqueous sodium carbonate and carry out lixiviate, the pH of the aqueous solution is 9, extracts 3 hours down for 50 ℃ in temperature, solid-liquid ratio is 1: 10, filters then, must contain natural dyestuff filtrate and filter residue.Adopt the multiple extraction filter residue of aforesaid method, extraction time is 3 times.To the extracting solution concentrating under reduced pressure, evaporation is 70% moisture wherein, and the pH value of vat liquor transfers to 3 with the aqueous hydrochloric acid of 7wt% after will concentrating again, adds ethanol with the pectin Impurity removal in the concentrated solution, regulates alcoholic acid volume fraction to 70%.The pH value of having filtered at last behind the pectin impurity cleaner liquid transfers to 10 with the 25wt% sodium hydroxide lye, stir to leave standstill after 5 hours and extract supernatant liquid, concentrate in that the supernatant liquor that extracts is inserted in the vacuum concentration pot, keep temperature to be 50 ℃ and remove recovery ethanol until the ethanol that will add wherein.At first concentrated solution pH value is transferred to 7 with the aqueous acetic acid of 15wt%, then concentrated solution is heated to 50 ℃ of after-filtration, carry out spraying drying again, inlet temperature is 170 ℃, and temperature out is 90 ℃, makes the Powdered natural dyestuff of reddish-brown.
The pure cotton dyeing method of the reddish brown natural dyestuff of the prepared oil-tea camellia husks of the extracting method of oil-tea camellia husks natural dyestuff, the pre-treatment and the pure cotton dyeing two procedures that comprise cotton fabric, the pre-treating process of cotton fabric is the preparation 5 grams per liter cation modifier aqueous solution, to put into wherein after the pure cotton fabric cleaning, room temperature dipping 4 minutes, two soak two rolls, 80 ℃ of oven dry; The HS-PY that the cation modifier aqueous solution adopts Hansi Chemical Article Co., Ltd., Changzhou to produce.
To carrying out the pure cotton fabric dyeing of pre-treatment, the dyeing condition is: dye strength 3%, and bath raio 1: 20 was contaminated 50 minutes down at 60 ℃, and taking-up fabric, acidity are soaped, clean, are dried.The dyeing pure cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.20, and dye uptake reaches 82%.
Acidity is soaped and is adopted acid scouring agent that oil-tea camellia husks natural dye dying pure cotton fabric is cleaned, acid scouring agent is 2: 2: 10 by side chain Soxylat A 25-7, the water of sodium polyacrylate, polypyrrole alkane ketone, C13 with weight ratio: 86 solution of forming, its pH value is 6.
Embodiment three
Adopt 50 ℃ of warm water to clean oil-tea camellia husks, behind the natural air drying, take by weighing 100 grams, mechanical disintegration to 60 order, add aqueous sodium carbonate and carry out lixiviate, the pH of the aqueous solution is 10, extracts 4 hours down for 60 ℃ in temperature, solid-liquid ratio is 1: 15, filters then, must contain natural dyestuff filtrate and filter residue.Adopt the multiple extraction filter residue of aforesaid method, extraction time is 4 times.To the extracting solution concentrating under reduced pressure, evaporation is 75% moisture wherein, and the pH value of vat liquor transfers to 5 with the aqueous solution of 10wt% after will concentrating again, adds ethanol with the pectin Impurity removal in the concentrated solution, regulates alcoholic acid volume fraction to 85%.The pH value of having filtered at last behind the pectin impurity cleaner liquid transfers to 9 with the 28wt% sodium hydroxide lye, stir to leave standstill after 6 hours and extract supernatant liquid, concentrate in that the supernatant liquor that extracts is inserted in the vacuum concentration pot, keep temperature to be 70 ℃ and remove recovery ethanol until the ethanol that will add wherein.At first concentrated solution pH value is transferred to 8 with the acetum of 20wt%, then concentrated solution is heated to 70 ℃ of after-filtration, carry out spraying drying again, inlet temperature is 190 ℃, and temperature out is 85 ℃, makes the Powdered natural dyestuff of reddish-brown.
The pre-treating process of cotton fabric is the preparation 6 grams per liter cation modifier aqueous solution, after being cleaned, puts into wherein pure cotton fabric, and room temperature dipping 6 minutes, two soak two rolls, 85 ℃ of oven dry; The HS-PY that the cation modifier aqueous solution adopts Hansi Chemical Article Co., Ltd., Changzhou to produce.
To carrying out the pure cotton fabric dyeing of pre-treatment, the dyeing condition is: dye strength 4%, and bath raio 1: 30 was contaminated 70 minutes down at 70 ℃, and taking-up fabric, acidity are soaped, clean, are dried.The dyeing pure cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.18, and dye uptake reaches 85%.
Acidity is soaped and is adopted acid scouring agent that oil-tea camellia husks natural dye dying pure cotton fabric is cleaned, acid scouring agent is 5: 3: 15 by side chain Soxylat A 25-7, the water of sodium polyacrylate, polypyrrole alkane ketone, C13 with weight ratio: 77 solution of forming, its pH value is 7.
Embodiment four
Adopt 60 ℃ of hot water to clean oil-tea camellia husks, behind the natural air drying, take by weighing 100 grams, mechanical disintegration to 70 order, add aqueous sodium carbonate and carry out lixiviate, the pH of the aqueous solution is 12, extracts 4 hours down for 80 ℃ in temperature, solid-liquid ratio is 1: 20, filters then, must contain natural dyestuff filtrate and filter residue.Adopt the multiple extraction filter residue of aforesaid method, extraction time is 4 times.To the extracting solution concentrating under reduced pressure, evaporation is 80% moisture wherein, and the acetum that will concentrate the pH value 6wt% of back vat liquor again transfers to 6, adds ethanol with the pectin Impurity removal in the concentrated solution, regulates alcoholic acid volume fraction to 90%.The pH value of having filtered at last behind the pectin impurity cleaner liquid transfers to 12 with the 30wt% sodium hydroxide lye, stir to leave standstill after 8 hours and extract supernatant liquid, concentrate in that the supernatant liquor that extracts is inserted in the vacuum concentration pot, keep temperature to be 80 ℃ and remove recovery ethanol until the ethanol that will add wherein.At first the acetum with concentrated solution pH value 18wt% transfers to 8, then concentrated solution is heated to 80 ℃ of after-filtration, carries out spraying drying again, and inlet temperature is 220 ℃, and temperature out is 83 ℃, makes the Powdered natural dyestuff of reddish-brown.
The pre-treating process of cotton fabric is the preparation 8 grams per liter cation modifier aqueous solution, after being cleaned, puts into wherein pure cotton fabric, and room temperature dipping 10 minutes, two soak two rolls, 90 ℃ of oven dry; The HS-PY that the cation modifier aqueous solution adopts Hansi Chemical Article Co., Ltd., Changzhou to produce.
To carrying out the pure cotton fabric dyeing of pre-treatment, the dyeing condition is: dye strength 6%, and bath raio 1: 40 was contaminated 90 minutes down at 80 ℃, and taking-up fabric, acidity are soaped, clean, are dried.The dyeing pure cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.10, and dye uptake reaches 88%.
Acidity is soaped and is adopted acid scouring agent that oil-tea camellia husks natural dye dying pure cotton fabric is cleaned, acid scouring agent is 4: 2: 12 by side chain Soxylat A 25-7, the water of sodium polyacrylate, polypyrrole alkane ketone, C13 with weight ratio: 82 solution of forming, its pH value is 6.
Claims (8)
1. the extracting method of the reddish brown natural dyestuff of oil-tea camellia husks is characterized in that having following processing step:
(1) raw material pre-treatment: clean oil-tea camellia husks with hot water, after airing or the oven dry oil-tea camellia husks is smashed;
(2) lixiviate separates: with the oil-tea camellia husks that crushes aqueous sodium carbonate lixiviate, the pH of the aqueous solution is 8-12, extracts 2-4 hour down at temperature 40-80 ℃, and solid-liquid ratio is volume ratio 1: 5-20, filters then, must contain natural dyestuff filtrate and filter residue;
(3) concentrated removing photoresist: with the extracting solution concentrating under reduced pressure, evaporate the wherein moisture of 60wt%-80wt%, the pH value that will concentrate the back vat liquor again adopts the hydrochloric acid soln of 5wt%-10wt% to transfer to 2-6, adds ethanol with the pectin Impurity removal in the concentrated solution, regulates the alcoholic acid volume fraction to 60%-90%; After having filtered pectin impurity at last, adopt the sodium hydroxide solution of 20wt%-30wt% to transfer to 8-12 the pH value of cleaner liquid, stir to leave standstill after 4-8 hour and extract supernatant liquid, in that being inserted in the vacuum concentration pot, the supernatant liquor that extracts concentrates, keep temperature be 40-80 ℃ until the ethanol removal that will add wherein, reclaim ethanol, obtain the concentrated solution of natural dyestuff;
(4) be dried to powder: adopt the aqueous acetic acid of 10wt%-20wt% to transfer to 6-8 the concentrated solution pH value of natural dyestuff, the concentrated solution with natural dyestuff is heated to 40-80 ℃ of after-filtration then, and drying makes the Powdered natural dyestuff of reddish-brown.
2. the extracting method of the reddish brown natural dyestuff of oil-tea camellia husks according to claim 1 is characterized in that having following steps:
(1) raw material pre-treatment: clean oil-tea camellia husks with 30-60 ℃ hot water, behind the natural air drying tea fruit shell smashed order to 30-70;
(2) lixiviate separates: with the oil-tea camellia husks that crushes aqueous sodium carbonate lixiviate, the pH of the aqueous solution is 8-12, extracts 2-4 hour down at temperature 40-80 ℃, and solid-liquid ratio is volume ratio 1: 5-20, filters then, must contain the filtrate and the filter residue of natural dyestuff; Adopt the multiple extraction filter residue of aforesaid method, extraction time is 2-4 time;
(3) concentrated removing photoresist: with the extracting solution concentrating under reduced pressure, evaporate the wherein moisture of 60wt%-80wt%, the pH value that will concentrate the back vat liquor again adopts the aqueous hydrochloric acid of 5wt%-10wt% to transfer to 2-6, add ethanol with the pectin Impurity removal in the concentrated solution, regulate the alcoholic acid volume fraction to 60%-90%; The pH value of having filtered at last behind the pectin impurity cleaner liquid adopts the aqueous sodium hydroxide solution of 20wt%-30wt% to transfer to 8-12, stir to leave standstill after 4-8 hour and extract supernatant liquid, in that being inserted in the vacuum concentration pot, the supernatant liquor that extracts concentrates, keep temperature be 40-80 ℃ until the ethanol removal that will add wherein, reclaim ethanol, obtain the concentrated solution of natural dyestuff;
(4) be dried to powder: adopt the aqueous acetic acid of 10wt%-20wt% to transfer to 6-8 the concentrated solution pH value of natural dyestuff, the concentrated solution with natural dyestuff is heated to 40-80 ℃ of after-filtration then, and drying makes the Powdered natural dyestuff of reddish-brown.
3. as the extracting method of the reddish brown natural dyestuff of oil-tea camellia husks as described in the claim 2, it is characterized in that having following steps:
(1) raw material pre-treatment: adopt 40-50 ℃ hot water to clean oil-tea camellia husks, behind the natural air drying tea fruit shell smashed order to 50-60;
(2) lixiviate separates: with the oil-tea camellia husks that crushes aqueous sodium carbonate lixiviate, the pH of the aqueous solution is 9-10, extracts 3 hours down at temperature 50-60 ℃, and solid-liquid ratio is volume ratio 1: 10-15, filters then, must contain the filtrate and the filter residue of natural dyestuff; Adopt the multiple extraction filter residue of aforesaid method, extraction time is 3 times;
(3) concentrated removing photoresist: with the extracting solution concentrating under reduced pressure, evaporate the wherein moisture of 70wt%-75wt%, the pH value that will concentrate the back vat liquor again adopts the aqueous hydrochloric acid of 5wt%-10wt% to transfer to 3-5, add ethanol with the pectin Impurity removal in the concentrated solution, regulate the alcoholic acid volume fraction to 70%-85%; The pH value of having filtered at last behind the pectin impurity cleaner liquid adopts the aqueous sodium carbonate of 10wt%-20wt% to transfer to 9-10, stir to leave standstill after 5-6 hour and extract supernatant liquid, in that being inserted in the vacuum concentration pot, the supernatant liquor that extracts concentrates, keep temperature be 50-70 ℃ until the ethanol removal that will add wherein, reclaim ethanol, obtain the concentrated solution of natural dyestuff;
(4) be dried to powder: adopt the aqueous acetic acid of 10wt%-20wt% to transfer to 7 the concentrated solution pH value of natural dyestuff, the concentrated solution with natural dyestuff is heated to 50-70 ℃ of after-filtration then, and drying makes the Powdered natural dyestuff of reddish-brown.
4. as the extracting method of claim 1 to 3 reddish brown natural dyestuff of oil-tea camellia husks as described in each, it is characterized in that: the dry spray-drying process that adopts of the concentrated solution of natural dyestuff, its inlet temperature is 160-220 ℃, temperature out is 80-90 ℃.
5. as the extracting method of the reddish brown natural dyestuff of oil-tea camellia husks as described in the claim 4, it is characterized in that: its inlet temperature is 170-190 ℃, and temperature out is 83-85 ℃.
6. as the pure cotton dyeing method of the reddish brown natural dyestuff of the prepared oil-tea camellia husks of extracting method of each described oil-tea camellia husks natural dyestuff of claim 1 to 5, it is characterized in that: the pre-treatment and the pure cotton dyeing two procedures that comprise cotton fabric, the pre-treating process of cotton fabric is the preparation 2-8 grams per liter cation modifier aqueous solution, to put into wherein after the pure cotton fabric cleaning, room temperature dipping 2-10 minute, pad 75-90 ℃ of oven dry; The dyestuff quality is the 0.5-8% of fabric quality in the pure cotton dyeing technology, and bath raio 1: 10-40 contaminated 30-90 minute down at 50-80 ℃, and taking-up fabric, acidity are soaped, clean, dried.
7. oil-tea camellia husks natural dyestuff pure cotton dyeing method as claimed in claim 6, it is characterized in that: the pre-treating process of cotton fabric is the preparation 5-6 grams per liter cation modifier aqueous solution, puts into wherein room temperature dipping 4-6 minute after pure cotton fabric is cleaned, two soak two rolls, 80-85 ℃ of oven dry; The dyestuff quality is the 3-4% of fabric quality in the pure cotton dyeing technology, and bath raio 1: 20-30 contaminated 50-70 minute down at 60-70 ℃, and taking-up fabric, acidity are soaped, clean, dried.
8. as claim 6 or 7 described oil-tea camellia husks natural dyestuff pure cotton dyeing methods, it is characterized in that: described acidity is soaped to acid scouring agent oil-tea camellia husks natural dye dying pure cotton fabric being cleaned, acid scouring agent is the solution that 1-5: 1-3: 5-15: 77-93 forms with the weight ratio by side chain Soxylat A 25-7, the water of sodium polyacrylate, polypyrrole alkane ketone, C13, and its pH value is 5-7.
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| CN105088821A (en) * | 2015-09-08 | 2015-11-25 | 湖州吉昌丝绸有限公司 | Method for dyeing pure cotton fabric through lycopene |
| CN113622206A (en) * | 2021-08-16 | 2021-11-09 | 韵万千(长沙)服饰文化有限公司 | Plant coloring agent for cotton and linen dip-dyeing and preparation method thereof |
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| CN101775234A (en) * | 2010-02-05 | 2010-07-14 | 江苏工业学院 | Method for extracting natural dye of gordon euryale seed shell and application in pure cotton dyeing |
| CN101885925A (en) * | 2010-07-01 | 2010-11-17 | 韩山师范学院 | Method for extracting brown pigment from oil-tea camellia husks |
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| CN105088821A (en) * | 2015-09-08 | 2015-11-25 | 湖州吉昌丝绸有限公司 | Method for dyeing pure cotton fabric through lycopene |
| CN113622206A (en) * | 2021-08-16 | 2021-11-09 | 韵万千(长沙)服饰文化有限公司 | Plant coloring agent for cotton and linen dip-dyeing and preparation method thereof |
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