CN100591727C - Method for refining powdered catechu dye by film separation technique and dyeing method thereof - Google Patents
Method for refining powdered catechu dye by film separation technique and dyeing method thereof Download PDFInfo
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- CN100591727C CN100591727C CN200710022226A CN200710022226A CN100591727C CN 100591727 C CN100591727 C CN 100591727C CN 200710022226 A CN200710022226 A CN 200710022226A CN 200710022226 A CN200710022226 A CN 200710022226A CN 100591727 C CN100591727 C CN 100591727C
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Abstract
The present invention relates to membrane separating process for refining powdered catechu dye and its dyeing process. The catechu dye refining process includes the steps of: dissolving marketable catechu paste in boiling water, screen filtering, filter paper filtering, microfltering membrane separating to eliminate impurity and to obtain clear dye solution, concentrating the dye solution, and spray dying to obtain powdered catechu dye. The dyeing process with the powdered catechu dye includes: adding dye in 1-5 %(o.w.f), bath ratio of 1 to 20-40, dye bath pH of 5-8; starting dyeing at 20-40 deg.c, heating in the rate of 1-2 deg.c/min to the dyeing temperature of 90-100 deg.c; maintaining for 40-60min; washing the dyed fabric with detergent at 40-60 deg.c for 10-20min; washing in cold water and drying. The present invention is favorable to developing antibiotic fabric.
Description
Technical field
The present invention relates to a kind of preparation method of functional textile dyestuff, especially relate to a kind of method and dyeing process thereof of refining powdered catechu dye by film separation technique.The preparation of platymiscium dyestuff and textile dyeing and finishing technical field.
Background technology
The present invention is intended to adopt catechu Acacia catechu (L.f.) Willd. with anti-microbial effect as dyestuff, and exploitation has the textiles of antibacterial.According to the Compendium of Material Medica record, catechu has the effect of " heat on the clear diaphragm is acted as expectorant, and is coated with metal-inflicted wound, all sores, promoting granulation and relieving pain, hemostasis, hygroscopic "; According to " book on Chinese herbal medicine justice " record, catechu have " fall fire and promote the production of body fluid, aphtha larynx numbness is controlled in clear sputum cough, and dysphoria with smothery sensation is only quenched one's thirst; spit blood, bleeding from five sense organs or subcutaneous tissue is had blood in stool, hematuria, dysentery due to damp-heat blood and married woman are collapsed pouring, menses are more than; children's's infantile malnutrition due to digestive disturbances or intestinalparasites heat, aphthae in children, herpes simplex, wet mashed all sores are held back flesh and are put on flesh, and also kill parasites." experiment in vitro proves that the catechu water decoction all has certain restraining effect to streptococcus aureus, Pseudomonas aeruginosa, diphtheria corynebacterium, Bacillus proteus, dysentery bacterium, Corynebacterium diphtheriae, and tubercule bacillus is had obvious restraining effect, and influenza virus is had deactivation.Catechu water logging agent (1: 2) in vitro to trichophyton, Trichophyton concentricum, permitted dermatophytess such as blue achorion, Du's big belly microspore tinea bacterium difficult to understand, rust microspore's tinea bacterium, ulotrichy microspore's tinea bacterium, epidermophyton inguinale, epidermophyton rubrum, star-shaped nocardia in various degree restraining effect all arranged.In Yunnan, all there are distribution in Zhejiang Province, Fujian Province, Taiwan Province, Hainan Province, Guangdong Province, Guangxi autonomous region to catechu at Chinese main product.As dyestuff, the special textiles that exploitation has antibacterial meets the textiles developing direction, not only can further open up the Application Areas of catechu with catechu, and can solve the potential insecurity of mainly carrying silver particles production antibacterial fabric at present with inorganic nano.The catechu medicinal material is generally sold with CATECHU, CATECHU be with catechu branch, dried be raw material, remove crust, be chopped to bulk, boiling, concentrate, be drying to obtain.CATECHU is square bulk or irregular shape, and surface black or sorrel are level and smooth and little glossy, surperficial sometimes visible crack; With the surface black and slightly redly, glossy, the foaming of burning on fire, savory person be for good; The crisp easy fragmentation of matter, section is irregular, and pore is arranged, and is also glossy, inner red-brown.Mainly contain effectively impurity such as pigment composition and natural gum such as catechutannic acid (Catechu tannic acid), catechin (Catechin), epicatechin (Epicatechin), catechu red, Quercetin in the CATECHU.After the commodity CATECHU was dissolved in boiling water, clarity of solution was very low, and viscosity is big, contained simultaneously to adopt traditional screen to be difficult to filtering tiny wooden slag, was unsuitable for modern textile dyeing, needed further separating impurity; Simultaneously, in order to improve dye stability, convenient dye dosage and the examination dyestuff quality calculated need be carried out the Spray powder to the catechu dye liquor after refining, to make the powdery catechu dye.
In recent years, the development of membrane sepn science and technology is very fast, adopts membrane separation technique refined plant dyestuff not appear in the newspapers as yet, and the present invention is intended to adopt membrane separation technique to make with extra care catechu dye.The aperture of film is generally micron order, according to the difference in its aperture, film can be divided into microfiltration membrane, ultra-filtration membrane, nanofiltration membrane and reverse osmosis membrane.For microfiltration membrane, the characteristic of holding back of film is that aperture with film characterizes, and pore diameter range is at the 0.1-1 micron usually, so microfiltration membrane can be separated large diameter thalline, suspended solids, macromolecular natural gum etc., can be used as the clarification, degerming of feed liquid etc.Because the membrane sepn process is a kind of pure physical process, no phase change need not added auxiliary agent, and film is widely used in fermentation, pharmacy, chemical industry, water treatment process and the environmental protection industry (epi).
Summary of the invention
First purpose of the present invention is to provide a kind of method that adopts refining powdered catechu dye by film separation technique, to reduce the impurity in the catechu dye, improves the content of its effective pigment composition, improves the clarity of dye liquor, is suitable for modern dyeing and finishing industry.
Second purpose of the present invention is to provide a kind of catechu dye to be used to dye the method for hair, silk, cotton, flaxen fiber, yarn and fabric, to improve the dyeing behavior of catechu dye, comprise the utilization ratio that improves dyestuff, painted homogeneity and dyefastness, reduce the damage of dyeing fiber.
First purpose of the present invention is achieved in that a kind of method of refining powdered catechu dye by film separation technique, this method is the commodity CATECHU to be separated four one-step physical methods by boiling water dissolving, sieve, filter paper suction filtration, microfiltration membrane separate wherein impurity, to improve the effective pigment composition content in the dye liquor, obtain clarifying bright dye liquor, then dye liquor is concentrated, and spraying drying is a powder.The processing step of this method is:
Step 1: boiling water dissolving CATECHU
Under the normal temperature, CATECHU is added in the 30-60 times of water gaging, boil about 20-40min, CATECHU all is dissolved in the boiling water, make CATECHU solution.
Step 2: sieve
Adopt the 120-200 eye mesh screen that CATECHU solution is carried out coarse filtration,, discard the impurity of failing, filter the back feed liquid and continue following sepn process by filter screen to remove bulk impurity.
Step 3: filter paper suction filtration
Middling speed or fast quantification or qualitative filter paper are placed on the B, utilize vacuum pump that feed liquid is carried out suction filtration.Be to improve suction filtration speed, preferably take advantage of feed liquid suction filtration when hot, and slowly pour feed liquid into, with anti-clogging plug.
Step 4: micro-filtrate membrane filtration
The employing recycle pump will be that the feed liquid below 35 ℃ enters polyvinylidene difluoride (PVDF) (PVDF), aperture 0.2um-0.5um external-compression type microfiltration membrane by fluid inlet through the temperature of filter paper, the adjusting working pressure is 0.02-0.07MPa, do not see through liquid and still be back to former liquid container, move to repeatedly through liquid and do not flow out substantially, collect respectively clarification bright see through liquid and contain more impurity do not see through liquid.
Step 5: dye liquor concentrates
Adopt the concentrating under reduced pressure method, the bright feed liquid of clarification that sees through microfiltration membrane is concentrated, being concentrated into the feed liquid solid content is 5-10%.
Step 6: spraying drying
Adopt spray-drier, the moisture evaporation with concentrating in the catechu dye liquor makes the high refining powdered catechu dye of effective pigment composition content.
Second purpose of the present invention is achieved in that a kind of dyeing process of refining powdered catechu dye, and substantive dyeing and two kinds of dyeing processs of back mordant dying are arranged, and the substantive dyeing method is divided into dyeing and two steps of aftertreatment; Back mordant dying method was divided into for three steps, was respectively dyeing, mordant dyeing, three steps of aftertreatment.
First kind, substantive dyeing method
The first step: dyeing
Refining powdered catechu dye consumption 1-5% (o.w.f), bath raio 1: 20-1: 40, dye bath pH=5-8,20-40 ℃ is dyed, and temperature rise rate 1-2 ℃/min, is warming up to dyeing temperature 90-100 ℃, insulation 40-60min; Hair, silk, cotton, textile materialss such as bast-fibre, yarn, fabric all can dye, and hair, silk class textiles dye under solutions of weak acidity, and cotton, crudefiber crop textile materials dyes under weak basic condition.Dyeing is simple, and dyeing course and discharge of wastewater can not produce environment and pollute.
Second step: aftertreatment
With 0.5-2g/L 209 washing composition dyed textile material is cleaned earlier, cleaning is: bath raio 1: 20-1: 40, and normal temperature adds dyed textile material down, is warming up to 40-60 ℃ of insulation and cleans 10-20min.Then, clean with cold water again, and dry.
Second kind, back mordant dying method
The first step: dyeing
Technology is with the substantive dyeing method.
Second step: back mordant dyeing technology
Dyed textiles is carried out the back mordant dyeing, and mordant can be used Potassium aluminum sulfate dodecahydrate (KAl (SO
4)
2.12H
2O) or iron vitriol (FeSO
4.7H
2O), different mordant dyeing agent kind, different amounts all can change the color feature value of final dyed textiles, and slightly can improve the fastness to wet rubbing of dyed textiles.Mordant KAl (SO
4)
2.12H
2O mordant dyeing technology is: consumption 1-6% (o.w.f), bath raio 1: 20-1: add textiles in the time of 40,20 ℃-40 ℃, be warming up to 60-80 ℃, mordant dyeing 20-30min; Mordant FeSO
4.7H
2O mordant dyeing technology is: consumption 1-3% (o.w.f), bath raio 1: 20-1: add textiles in the time of 40,20 ℃-40 ℃, be warming up to 50 ℃-70 ℃, mordant dyeing 20-40min
The 3rd step: aftertreatment
Aftertreatment technology is with the substantive dyeing method.
The present invention is intended to adopt the catechu with anti-microbial effect as dyestuff, and exploitation has the textiles of antibacterial.The present invention adopts the method for refining powdered catechu dye by film separation technique, can reduce the impurity in the catechu dye, improves the content of its effective pigment composition, improves the clarity of dye liquor, is suitable for modern dyeing and finishing industry.
Catechu dye of the present invention is used to dye the method for hair, silk, cotton, flaxen fiber, yarn and fabric, can
Improve the dyeing behavior of catechu dye, comprise the utilization ratio that improves dyestuff, painted homogeneity and dyefastness, the reduction dyeing is to the damage of fiber etc.
Embodiment:
Embodiment 1: refining catechu dyestuff powder method
Step 1, boiling water dissolving CATECHU
Under the normal temperature, CATECHU is added in 40 times of water gagings, be heated to little 30min of boiling, CATECHU all is dissolved in the boiling water, make CATECHU solution.
Step 2, sieve
Adopt 180 order steel-wire screens that CATECHU solution is carried out coarse filtration.
Step 3, filter paper suction filtration
Fast qualitative filter paper is placed on the B, utilize vacuum pump (vacuum tightness is 0.098MPa) that feed liquid is carried out suction filtration.
Step 4, micro-filtrate membrane filtration
The employing recycle pump will be that the feed liquid below 35 ℃ enters polyvinylidene difluoride (PVDF) (PVDF), aperture 0.2um-0.5um external-compression type microfiltration membrane (because pressure by fluid inlet through the temperature of filter paper, effective small molecules pigment enters film inside from the film outside to dyeing, and macromolecular impurity can not enter film inside), the adjusting working pressure is 0.04MPa, do not see through liquid and still be back to former liquid container, move to repeatedly through liquid and do not flow out substantially, collect respectively clarification bright see through liquid and contain more impurity do not see through liquid.
Step 5, dye liquor concentrate
The bright dye liquor of clarification that sees through microfiltration membrane is carried out concentrating under reduced pressure, and being concentrated into the feed liquid solid content is 5-10%.
Step 6, spraying drying
Adopt spray-drier, the moisture evaporation with concentrating in the catechu dye liquor makes the high refining powdered catechu dye of effective pigment composition content.
Embodiment 2: adopt refining powdered catechu dye that wool fabric is carried out the substantive dyeing step
Step 1, dyeing
Refining powdered catechu dye consumption 3% (o.w.f), bath raio 1: 25, dye bath pH=6.5,40 ℃ are dyed, and 1 ℃/min of temperature rise rate is warming up to 100 ℃ of dyeing temperatures, insulation 60min.
Step 2, aftertreatment
With 209 washing composition dyed textile material is cleaned earlier, washing composition consumption 1g/L, bath raio 1: 25, normal temperature adds the dyeing wool fabric down, is warming up to 60 ℃ of insulations and cleans 10min.Then, clean oven dry again with cold water.
Embodiment 3: adopt refining powdered catechu dye that wool fabric is carried out back mordant dying step
Step 1, dyeing
Refining powdered catechu dye consumption 5% (o.w.f), bath raio 1: 25, dye bath pH=6.5,40 ℃ are dyed, and 1 ℃/min of temperature rise rate is warming up to 100 ℃ of dyeing temperatures, insulation 60min.
Second step: back mordant dyeing
The wool fabric that dyes is carried out the back mordant dyeing, mordant KAl (SO
4)
2.12H
2O, consumption 3% (o.w.f), bath raio 1: 25 adds wool fabric in the time of 40 ℃, be warming up to 80 ℃, mordant dyeing 30min.
Step 3, aftertreatment
Clean with 209 washing composition earlier, washing composition consumption 2g/L, bath raio 1: 25, normal temperature adds the dyeing wool fabric down, is warming up to 60 ℃ of insulations and cleans 10min.Then, clean oven dry again with cold water.
Embodiment 4: adopt refining powdered catechu dye that wool fabric is carried out back mordant dying step
The difference of present embodiment and embodiment 3 is: mordant adopts FeSO
4.7H
2O, all the other are all with embodiment 3.
Claims (2)
1, a kind of method that adopts refining powdered catechu dye by film separation technique, it is characterized in that this method is the commodity CATECHU to be separated four one-step physical methods by boiling water dissolving, sieve, filter paper suction filtration separate wherein impurity with microfiltration membrane, obtain clarifying bright dye liquor, then dye liquor is concentrated, and spraying drying is a powder.
2, a kind of method that adopts refining powdered catechu dye by film separation technique according to claim 1 is characterized in that the processing step of described method is:
Step 1: boiling water dissolving
Under the normal temperature, CATECHU is added in the 30-60 times of water gaging, boils 20-40min, CATECHU all is dissolved in the boiling water, make CATECHU solution,
Step 2: sieve
Adopt the 120-200 eye mesh screen that CATECHU solution is carried out coarse filtration,
Step 3: filter paper suction filtration
Middling speed or fast quantification or qualitative filter paper are placed on the B, utilize vacuum pump, the feed liquid after the coarse filtration is carried out suction filtration,
Step 4: micro-filtrate membrane filtration
The employing recycle pump will be that the feed liquid below 35 ℃ enters the polyvinylidene difluoride (PVDF) external-compression type microfiltration membrane that the aperture is 0.2um-0.5um by fluid inlet through the temperature of filter paper, the adjusting working pressure is 0.02-0.07MPa, do not see through liquid and still be back to former liquid container, move to repeatedly through liquid and do not flow out, collect respectively clarification bright see through liquid and contain more impurity do not see through liquid
Step 5: dye liquor concentrates
Adopt the concentrating under reduced pressure method, the feed liquid that sees through microfiltration membrane is concentrated, being concentrated into the feed liquid solid content is 5-10%,
Step 6: spraying drying
Adopt spray-drier, the moisture evaporation with concentrating in the catechu dye liquor makes refining powdered catechu dye.
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| CN200710022226A CN100591727C (en) | 2007-04-27 | 2007-04-27 | Method for refining powdered catechu dye by film separation technique and dyeing method thereof |
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|---|---|---|---|
| CN200710022226A CN100591727C (en) | 2007-04-27 | 2007-04-27 | Method for refining powdered catechu dye by film separation technique and dyeing method thereof |
Related Child Applications (2)
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|---|---|---|---|
| CN200910170830A Division CN101713152A (en) | 2007-04-27 | 2007-04-27 | Method of dyeing by using refined powder wadalee-gum-tree dye |
| CN2009101708312A Division CN101666045B (en) | 2007-04-27 | 2007-04-27 | Dyeing method of powdered catechu dye |
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| CN100591727C true CN100591727C (en) | 2010-02-24 |
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Cited By (1)
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| CN101747662B (en) * | 2009-12-25 | 2013-03-13 | 江南大学 | Method for preparing hematoxylin powder dyes |
| CN101956334B (en) * | 2010-09-10 | 2012-04-25 | 中国农业科学院茶叶研究所 | Method for dying cotton fiber by utilizing tea vegetable dye |
| CN102352127B (en) * | 2011-08-25 | 2014-03-26 | 郑州大学 | Active turquoise blue dye used in digital printing, and preparation method thereof |
| CN102924963B (en) * | 2012-10-08 | 2015-04-22 | 常州富思生物科技有限公司 | Method for preparing natural red jujube skin pigment and application of natural red jujube skin pigment |
| CN104480756A (en) * | 2014-12-22 | 2015-04-01 | 江南大学 | Method for dyeing cellulosic fiber fabric by sorghum husk pigment |
| CN105780526A (en) * | 2014-12-22 | 2016-07-20 | 常熟市虹桥印染有限公司 | Dye liquor for printing and dyeing of cotton cloth |
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Cited By (1)
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| WO2012065576A1 (en) | 2010-11-19 | 2012-05-24 | 浙江养生堂天然药物研究所有限公司 | Use of tea polyphenols and/or tea pigments as dyes and products thereof |
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| CN101077942A (en) | 2007-11-28 |
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