CN102102304A - Application of shaddock peel natural dye in cotton fabrics dyeing - Google Patents

Application of shaddock peel natural dye in cotton fabrics dyeing Download PDF

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Publication number
CN102102304A
CN102102304A CN2010106176127A CN201010617612A CN102102304A CN 102102304 A CN102102304 A CN 102102304A CN 2010106176127 A CN2010106176127 A CN 2010106176127A CN 201010617612 A CN201010617612 A CN 201010617612A CN 102102304 A CN102102304 A CN 102102304A
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natural dye
cotton fabrics
cotton fabric
dyeing
filtrate
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CN102102304B (en
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纪俊玲
王炜
朱美芳
李小琴
杨扬
汪媛
何叶丽
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SAINTYEAR HOLDING GROUP CO Ltd
Donghua University
Changzhou University
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SAINTYEAR HOLDING GROUP CO Ltd
Donghua University
Changzhou University
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Abstract

The invention relates to an application of shaddock peel natural dye in cotton fabrics dyeing, which comprises the following steps: 1) pre-treating raw materials; 2) soaking crushed shaddock peel powders in ethanol water at room temperature; 3) extracting by using an ultrasonic extraction method; 4) centrifuging the filtrate, removing the insoluble substances, reducing the pressure, and concentrating the filtrate so as to obtain an orange red color sizing; 5) adding little water into the orange red color sizing, suspending the mixture, and centrifugally separating the mixture so as to obtain a read pigment solution; 6) modifying the cotton fabrics; and 7) dyeing the cotton fabrics with the shaddock peel natural dye obtained in step 5), taking out the cotton fabrics, washing the cotton fabrics with water and finally drying the cotton fabrics. The application of shaddock peel natural dye in cotton fabrics dyeing has the advantages that the preparation process is simple, the raw materials are low in cost and are easily acquired, and the extraction efficiency is high. The fabrics which are dyed with the shaddock peel natural dye is safe and environment-friendly, has no chemical harm to human body, is biodegradable, has good pigment stability and wide application prospect.

Description

The application of shaddock skin natural dye in cotton fabric dyeing process
Technical field
The invention belongs to the Application Areas of natural dye, especially relate to the application of a kind of shaddock skin natural dye in cotton fabric dyeing process.
Background technology
Along with people's ecological, environmental protective consciousness strengthen gradually and to the growing interest of self health, increasing consumer favors the textiles in environmental protection, natural dye also day by day causes people's attention.With the fabric of natural dye dying, both satisfied environmental protection, ecological production demand, avoided the infringement of synthetic dyestuffs again to health, meet the clothes requirement of health, functionalization.
Shaddock claims the pomelo again, is the Rutaceae citrus fruit, and kind is many, and ground such as Sichuan, Hainan, Zhejiang, Shaanxi abound with, and sells and spreads all over all parts of the country.The traditional Chinese medical science thinks, shaddock ped has cough-relieving, reduces phlegm, regulates the flow of vital energy, anti-inflammatory, effect such as antipruritic.Therefore, extract natural dye and be applied to textile dyeing from the shaddock skin, for increasing natural dye kind and chromatogram, improve the surcharge of textiles, construction economizing type, friendly environment society have crucial meaning.
The natural colouring matter that contains two class different in kinds in the shaddock ped, a class are fat-soluble class carrot pigment, and another kind of is water miscible xanthein, and it is sweet etc. that xanthein mainly contains aurantiin, aurantiamarin and naringenin rue, and its composition is similar to the orange peel pigment.
About the existing a small amount of report of the extraction of shaddock skin natural colouring matter, and, have not yet to see relevant report about its application." extraction and the stability study of shaddock Beijing opera pigment " (Wenzhou normal academy's journal that Cao Yanping, Huo Wenlan deliver, 2002 the 6th phases) simply having introduced with 95% acidic ethanol is solvent, the refluxing extraction uranidin, this method recovery rate is low, cause the loss of mass efficient composition, be unfavorable for a large amount of productions; " technical study of natural colouring matter in the supercritical carbon dioxide extracting Changshan Hu shaddock exocarp " (Zhejiang Forestry Institute journal that Shi Haixiang, Zhong Shanmin etc. deliver, 2008 the 5th phases) adopt supercritical carbon dioxide extraction method to extract Changshan shaddock natural colouring matter recklessly, this method production cost height, operation is loaded down with trivial details also to be unfavorable for large-scale production.
Summary of the invention
Technical problem to be solved of the present invention provides the application of a kind of shaddock skin natural dye in cotton fabric dyeing process, and this preparation technology is simple, the extraction efficiency height; Gained DYED FABRICS safety and environmental protection, biodegradable, and pigment stability is good, has broad application prospects.
The extraction of a kind of shaddock skin natural dye of the present invention and the application in cotton fabric dyeing process comprise:
1) remove shaddock skin exocuticle afterwash, dry 24h of vacuum drying chamber or low temperature (40~60 ℃) are air-dry, are crushed to the 20-80 order;
2) the shaddock skin powder after will pulverizing is dipped in the ethanol water that volume fraction is 50-95%, and the feed liquid mass ratio is 1: 5-40, and soak at room temperature 3-5h makes the abundant swelling of shaddock skin powder, accelerates disengaging of dyestuff;
3) soak continues to extract with ultrasonic extraction, and ultrasonic power is 300-800W, after extracting 30-60min under the 40-60 ℃ of condition, filters, and must contain natural dye filtrate and filter residue;
4) filter residue is carried out the post bake refluxing extraction: extractant is the ethanol water of volume fraction 50-95%, and temperature is elected 50-80 ℃ as, and extraction time is 60-90min; The filtrate that merges twice gained, insoluble matter is removed in filtration, centrifugation.Concentrate recovery ethanol by reducing pressure and get orange red mill base;
5) orange red mill base is added the low amounts of water suspendible after centrifugation get red pigments liquid, water insoluble part is an orange pigment glue;
6) modification of COTTON FABRIC is handled, preparation contains dyeing finishing agent GRE (purchasing in Hansi Chemical Article Co., Ltd., Changzhou) 10-15g/L, and the caustic soda consumption is the aqueous solution of 3-10g/L, and bath raio is 1: 20-60, under 60-80 ℃, the pure cotton fabric after cleaning is put into above-mentioned solution react 30-60min;
7) COTTON FABRIC after under the normal temperature modification being handled is immersed in the shaddock skin natural dye, and dye strength is mass fraction 1-10%, bath raio 1: 10-40, be warming up to 50-80 ℃ of afterreaction 30-90min again after, take out COTTON FABRIC, washing, after the oven dry promptly.
Fat-soluble orange pigment need pass through emulsifying agent, dispersant processing changing into water colo(u)r just can be used for dyeing.This patent mainly uses water-soluble red pigments liquid to dye.
Beneficial effect
1, preparation technology of the present invention is simple, and raw material is cheap and easy to get, and the extraction efficiency height is fit to large-scale production.
2, fabric is handled with the dyeing finishing agent before dyeing, improved the dye-uptake of COTTON FABRIC, avoided improving the harm that dyeing efficient is brought to environment with mordant in the conventional method.
3, the DYED FABRICS safety and environmental protection that obtains of the present invention can not produce chemical hazard to human body, and is biodegradable, pollution-free, and pigment stability is good, has broad application prospects.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing and remove epidermis shaddock skin after the oven dry, be crushed to 20 orders, it is in 50% the ethanol water that shaddock skin powder is dipped in volume fraction, solid-liquid ratio is 1: 5, soak at room temperature 3h adopts ultrasonic extraction to continue to extract then, and ultrasonic power is 300W, after extracting 30min under 40 ℃, must contain natural dye filtrate and filter residue.With filter residue with the ethanol of volume fraction 90% behind 60 ℃ of following lixiviate 60min, merge the filtrate of twice gained, filter, centrifugation removes insoluble matter.Concentrate to reclaim ethanol by reducing pressure and get orange red mill base, rough orange red mill base is added the low amounts of water suspendible after centrifugation get red pigments liquid.
Preparation dyeing finish solution: 10g/L dyeing finishing agent, 3g/L NaOH, bath raio is 1: 30.Under 60 ℃, behind reaction 30min in the pure cotton fabric adding dyeing finish solution, washing, oven dry.
Pure cotton fabric after handling is dyeed, shaddock skin natural dye concentration (mass fraction) 1%, bath raio 1: 10, normal temperature is contaminated down, is warming up to 50 ℃ of after stain 30min with 2 ℃/min, washing, oven dry.The dyed cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.5, and dye-uptake reaches 75%.
Embodiment 2
Take by weighing and remove epidermis shaddock skin after the vacuumize, be crushed to 40 orders, shaddock skin powder is dipped in the ethanol water of volume fraction 60%, solid-liquid ratio is 1: 10 soak at room temperature 4h, adopt ultrasonic extraction to continue to extract then, ultrasonic power is 500W, after temperature is to extract 50min under 50 ℃ of conditions, must contain natural dye filtrate and filter residue.With filter residue with the ethanol water of volume fraction 80% behind 70 ℃ of following lixiviate 90min, merge the filtrate of twice gained, filter, centrifugation removes insoluble matter.Concentrate to reclaim ethanol by reducing pressure and get orange red mill base, with rough orange red mill base with the low amounts of water suspendible after centrifugation get red pigments liquid.
Preparation dyeing finish solution: 12g/L dyeing finishing agent, 5g/L NaOH, bath raio is 1: 20.Under 70 ℃, behind reaction 50min in the pure cotton fabric adding dyeing finish solution, washing, oven dry.
Pure cotton fabric after handling is dyeed, and shaddock skin natural dye concentration is mass fraction 4%, bath raio 1: 20, and normal temperature is contaminated down, is warming up to 60 ℃ of after stain 40min with 2 ℃/min, washing, oven dry.The dyed cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.35, and dye-uptake reaches 80%.
Embodiment 3
Take by weighing and remove epidermis shaddock skin after the oven dry, be crushed to 60 orders, shaddock skin powder is dipped in the ethanol water of volume fraction 70%, solid-liquid ratio 1: 20, soak at room temperature 5h adopts ultrasonic extraction to continue to extract then, and ultrasonic power is 600W, after temperature is to extract 60min under 60 ℃ of conditions, must contain natural dye filtrate and filter residue.With filter residue with the ethanol of volume fraction 70% behind 80 ℃ of following lixiviate 60min, merge the filtrate of twice gained, filter, centrifugation removes insoluble matter.Concentrate to reclaim ethanol by reducing pressure and get orange red mill base, with rough orange red mill base with the low amounts of water suspendible after centrifugation get red pigments liquid.
Preparation dyeing finish solution: 14g/L dyeing finishing agent, 6g/L NaOH, bath raio is 1: 30.Under 75 ℃, behind reaction 60min in the pure cotton fabric adding dyeing finish solution, washing, oven dry.
Pure cotton fabric after handling is dyeed, and shaddock skin natural dye concentration is mass fraction 6%, bath raio 1: 30, and normal temperature is contaminated down, is warming up to 70 ℃ of after stain 50min with 2 ℃/min, washing, oven dry.The dyed cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.3, and dye-uptake reaches 82%.
Embodiment 4
Take by weighing and remove epidermis shaddock skin after the oven dry, be crushed to 80 orders, shaddock skin powder is dipped in the ethanol water of volume fraction 95%, solid-liquid ratio 1: 40, soak at room temperature 5h adopts ultrasonic extraction to continue to extract then, and ultrasonic power is 800W, after temperature is to extract 60min under 60 ℃ of conditions, must contain natural dye filtrate and filter residue.With filter residue with the ethanol of volume fraction 50% behind 70 ℃ of following lixiviate 60min, merge the filtrate of twice gained, filter, centrifugation removes insoluble matter.Concentrate to reclaim ethanol by reducing pressure and get orange red mill base, with rough orange red mill base with the low amounts of water suspendible after centrifugation get red pigments liquid.
Preparation dyeing finish solution: 15g/L dyeing finishing agent, 10g/L NaOH, bath raio is 1: 60.Under 80 ℃, behind reaction 60min in the pure cotton fabric adding dyeing finish solution, washing, oven dry.
The pure cotton fabric of having handled is dyeed, and shaddock skin natural dye concentration is mass fraction 10%, bath raio 1: 40, and normal temperature is contaminated down, is warming up to 80 ℃ of after stain 90min with 2 ℃/min, washing, oven dry.The dyed cotton fabric color and luster that obtains is even, and value of chromatism Δ E is less than 0.3, and dye-uptake reaches 84.5%.

Claims (2)

1. the application of a shaddock skin natural dye in cotton fabric dyeing process comprises:
1) shaddock skin exocuticle is removed afterwash, dry or air-dry, be crushed to the 20-80 order;
2) the above-mentioned shaddock skin powder that crushes is dipped in the ethanol water that volume fraction is 50-95%, the feed liquid mass ratio is 1: 5-40, and soak at room temperature 3-5h makes the abundant swelling of shaddock skin powder, accelerates disengaging of dyestuff;
3) above-mentioned soak continues to extract with ultrasonic extraction, and ultrasonic power is 300-800W, after extracting 30-60min under the 40-60 ℃ of condition, filters, and must contain natural dye filtrate and filter residue;
4) with above-mentioned filtrate, insoluble matter is removed in filtration, centrifugation, concentrates recovery ethanol by reducing pressure and gets orange red mill base;
5) orange red mill base is added the low amounts of water suspendible after centrifugation get red pigments liquid;
6) modification of COTTON FABRIC is handled: preparation contains dyeing finishing agent 10-15g/L, and the caustic soda consumption is the aqueous solution of 3-10g/L, and bath raio is 1: 20-60, under 60-80 ℃, put into above-mentioned solution with the pure cotton fabric after cleaning and react 30-60min;
7) COTTON FABRIC after under the normal temperature above-mentioned modification being handled is immersed into 5) in the shaddock skin natural dye of gained, dye strength is mass fraction 1-10%, bath raio 1: 10-40 is warming up to 50-80 ℃ of afterreaction 30-90min again, takes out COTTON FABRIC, washing, after the oven dry promptly.
2. the application of a kind of shaddock skin natural dye according to claim 1 in cotton fabric dyeing process, it is characterized in that: gained filter residue in the step 3) is carried out the post bake refluxing extraction, extractant is the ethanol water of volume fraction 50-95%, temperature is elected 50-80 ℃ as, extraction time is 60-90min, filter, with gained filtrate and 3) merging of gained filtrate, more successively according to the step 4) in the claim 1,5), 6), 7) operate.
CN2010106176127A 2010-12-30 2010-12-30 Application of shaddock peel natural dye in cotton fabrics dyeing Expired - Fee Related CN102102304B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102888128A (en) * 2012-09-27 2013-01-23 河南牧翔动物药业有限公司 Extracting technology of viburnum sargenti fruit pigment
CN104278548A (en) * 2014-10-15 2015-01-14 嘉兴市梦迪织造有限公司 Digital ink-jet printing ink based on extract of stems and leaves of celosia cristata L.
CN105040484A (en) * 2015-09-08 2015-11-11 湖州宏鑫绸厂 Novel process for dyeing soybean protein fiber with aubergine red pigment
CN107401067A (en) * 2017-08-25 2017-11-28 陈值英 Colouring method of the one ganoid konjaku taro leaf dyestuff to bafta
CN109537316A (en) * 2018-11-30 2019-03-29 河南健锋帽业有限公司 A kind of coloring agent, preparation method and the application on fabric printing

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85102662A (en) * 1985-04-01 1986-09-24 四川大学 From citrus peel, obtain through refining the method for pectin coproduction simultaneously wine, oil, sauce, pigment and orange peel glucoside
CN1058224A (en) * 1990-07-12 1992-01-29 山东大学 From maize yellow-powder, extract the food dye maize
CN101210113A (en) * 2006-12-31 2008-07-02 福建农林大学 Method for preparing oil soluble citrus coloring matter
CN101469517A (en) * 2007-12-27 2009-07-01 恒源祥(集团)有限公司 Method for dyeing peony pigment on protein fibre fabric
CN101666044A (en) * 2008-09-03 2010-03-10 上海市长宁区少年科技指导站 Application of alkannin serving as dye

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85102662A (en) * 1985-04-01 1986-09-24 四川大学 From citrus peel, obtain through refining the method for pectin coproduction simultaneously wine, oil, sauce, pigment and orange peel glucoside
CN1058224A (en) * 1990-07-12 1992-01-29 山东大学 From maize yellow-powder, extract the food dye maize
CN101210113A (en) * 2006-12-31 2008-07-02 福建农林大学 Method for preparing oil soluble citrus coloring matter
CN101469517A (en) * 2007-12-27 2009-07-01 恒源祥(集团)有限公司 Method for dyeing peony pigment on protein fibre fabric
CN101666044A (en) * 2008-09-03 2010-03-10 上海市长宁区少年科技指导站 Application of alkannin serving as dye

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102888128A (en) * 2012-09-27 2013-01-23 河南牧翔动物药业有限公司 Extracting technology of viburnum sargenti fruit pigment
CN104278548A (en) * 2014-10-15 2015-01-14 嘉兴市梦迪织造有限公司 Digital ink-jet printing ink based on extract of stems and leaves of celosia cristata L.
CN104278548B (en) * 2014-10-15 2016-06-29 浙江梦迪针织有限公司 A kind of digital ink-jet printed ink based on Flos Celosiae Cristatae stem and leaf extract
CN105040484A (en) * 2015-09-08 2015-11-11 湖州宏鑫绸厂 Novel process for dyeing soybean protein fiber with aubergine red pigment
CN105040484B (en) * 2015-09-08 2017-12-15 盐城金大纺织机械制造有限公司 A kind of dyeing of aubergine red pigment to soybean fiber
CN107401067A (en) * 2017-08-25 2017-11-28 陈值英 Colouring method of the one ganoid konjaku taro leaf dyestuff to bafta
CN109537316A (en) * 2018-11-30 2019-03-29 河南健锋帽业有限公司 A kind of coloring agent, preparation method and the application on fabric printing

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