CN101747662B - Method for preparing hematoxylin powder dyes - Google Patents
Method for preparing hematoxylin powder dyes Download PDFInfo
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- CN101747662B CN101747662B CN 200910264655 CN200910264655A CN101747662B CN 101747662 B CN101747662 B CN 101747662B CN 200910264655 CN200910264655 CN 200910264655 CN 200910264655 A CN200910264655 A CN 200910264655A CN 101747662 B CN101747662 B CN 101747662B
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Abstract
The invention relates to a method using a membrane separation technology to prepare hematoxylin powder dyes, comprising the following six steps: (1) adding water with the weight of 20-30 times in a crushed hematoxylin core material, and heating to 80-100 DEG C for extracting for 1-1.5 h and 2-3 times; (2) adopting a screen with 120-200 meshes for rough filtration; (3) filter paper sucking filtration; (4) adopting a polyvinylidene fluoride (PVDF) microfiltration membrane with a pore size of 0.1-0.4mum for removing impurities and bacterium; (5) adopting a hydrophobic polysulfone ultrafiltration membrane with intercepted molecular weight of 1000-5000 for concentrating extract liquid, concentrating to the solid content of retain liquid, namely pigment concentration liquid of 5-10%, and recycling permeation liquid with low-content hematoxylin power to extract hematoxylin pigment; (6) and spraying and drying to prepare the high-purity hematoxylin powder dyes. The method can reduce energy and water consumption in the preparation process of the hematoxylin dyes, and reduces the preparation cost and the dye impurity rate. The hematoxylin dyes can be used for developing green-feature textiles and can also be used for preparing hair dyes.
Description
(1) technical field
The present invention relates to a kind of preparation method of vegetable dye, especially relate to a kind of method that adopts membrane separation technique to prepare hematoxylin powder dyes.The preparing technical field of platymiscium dyestuff.
(2) background technology
Bush (Sappanwood) is the dry core of leguminous plants bush (Caesalpinia Sappan L.), is a kind of traditional Chinese medicine material, and aboundresources is of many uses.Domestic bush resource mainly is distributed in the ground such as Yunnan, Guizhou, Sichuan, Guangdong and Guangxi Provinces, Fujian and Taiwan.On traditional Chinese medicine, bush has capable blood and dissolving stasis, and the multiple efficacies such as swelling and pain relieving are used on the tcm clinical practice through closing stomachache, postpartum stasis blocking, chest ventral spine pain, wound swell and ache etc.In recent years, take water as solvent, adopt traditional circumfluence method and decocting method technique to extract hemartine extract, and study the great attention that its pharmacology, drug effect and development and use have been subject to people.Studies show that aqueous extract of lignum sappan has maincenter inhibition, anti-inflammatory, lipidemia effect; Have obvious immunosuppressive action, anti-heart transplant rejection etc.Bush is except medicinal, and its water extract presents red-violet colour, is a kind of vegetable dye, adopts the harmless metal salt mordants such as aluminium, iron can dye the colors such as red, brown.Research thinks that brazilwood dye can be used for the dyeing of wool, silk, soybean fiber, cotton fibre and fabric thereof.In addition, hematoxylin can also be developed botanical hair dye.The brazilwood dyeing textiles is bright in colour, has antibiotic biological activity and nourishing function, belongs to simultaneously Green Textiles.
The hematoxylin chemical ingredients mainly contains brazilin (Brazilin) and phenodin (Hematoxylin).Brazilin is the amber yellow crystal, easily is oxidized to especially red brasilein at the aqueous solution in basic solution.And phenodin is white crystals, is oxidized to rapidly the hematoxylein of reddish-brown in air.Because these two kinds of pigment compositions all contain great amount of hydroxy group, therefore soluble in water, used water is done the solvent extraction bush.Traditional brazilwood dye preparation method comprises following technical process: bush → and take water or water/alcohol as solvent extraction hematoxylin → filtration → concentrating under reduced pressure → spraying drying → powder brazilwood dye.Wherein, concentrating under reduced pressure is to adopt the method for decompression, moisture vaporization with the moisture in the extracting solution and pigment separated, reaches the purpose of concentrated pigment, and the method energy consumption is large, and water consumption is large.
In recent years, the membrane sepn scientific and technological development is very fast.In membrane sepn, according to the difference of membrane pore size, 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 0.1-1 μ m 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.For ultra-filtration membrane, the characteristic of holding back of film is so that the organic molecular weight cut-off of standard is characterized, and the molecular weight cut-off scope is at 1000-300000 usually.The membrane sepn process is a kind of pure physical process, without phase change, need not add auxiliary agent.
(3) summary of the invention
The object of the invention is to the superiority based on the affluent resources of bush and extensive use, membrane separation technique, be intended to adopt the concentrated hematoxylin extracting solution of membrane separation technique with preparation powder brazilwood dye, invent a kind of method that the energy, water-saving employing membrane separation technique prepare hematoxylin powder dyes of saving.
The object of the present invention is achieved like this: a kind of method that adopts membrane separation technique to prepare hematoxylin powder dyes is characterized in that described method comprises following processing step:
Step 1, hot water extraction hematoxylin
Under the normal temperature, the bush core is added in the 20-30 times of weight water, be heated to temperature 80-100 ℃ and extract hematoxylin, extract 1-1.5h at every turn, extract 2-3 time.
Step 2, employing sieve
Adopt the 120-200 eye mesh screen while hot the bush extracting solution to be carried out coarse filtration, with the removal filter residue, and with the merging of each time filtrate, make reddish yellow hematoxylin extracting solution.
Step 3, filter paper suction filtration
Middling speed or fast quantification or qualitative filter paper are placed on the Büchner funnel, utilize vacuum pump that reddish yellow hematoxylin extracting solution is carried out suction filtration.
Step 4, micro-filtrate membrane filtration removal of impurities degerming
Adopt recycle pump, will be that the feed liquid below 35 ℃ is passed through the microfiltration membrane fluid inlet through the temperature of filter paper, and carry out membrane separation for removing impurities.Used microfiltration membrane material be polyvinylidene difluoride (PVDF) (PVDF), aperture at 0.1-0.4 μ m, external-compression type, regulating the membrane sepn working pressure is 0.02-0.07MPa, sees through liquid and still is back to former liquid container.Collect respectively clarification bright see through liquid and contain impurity do not see through liquid.
Step 5, the concentrated bush extracting solution of ultra-filtration membrane
Adopt ultra-filtration membrane that the bright feed liquid of clarification that sees through microfiltration membrane is concentrated.Each chemical ingredients of hematoxylin is wetting ability, and molecular weight is about about 400.Selecting the stronger polysulfones material of hydrophobicity, molecular weight cut-off is the ultra-filtration membrane of 1000-5000, simultaneously, and the membrane operations pressure range 0.02-0.04MPa of selection of small.Under such film condition, the hematoxylin more than 80% is difficult to see through ultra-filtration membrane, and the trapped fluid that does not see through ultra-filtration membrane is the hematoxylin concentrated solution, when the concentrated solution solid content is 5-10%, and the stopper film concentration process.The hematoxylin concentrated solution carries out the drying process with atomizing in lower step, and the very low liquid that sees through of hematoxylin content recycles the extraction hematoxylin.
Step 6, spraying drying
Adopt spray-drier, with the evaporation of the moisture in the hematoxylin concentrated solution, make hematoxylin powder dyes.
Brazilwood dye of the present invention can be used for dying hair, silk, cotton, flaxen fiber, yarn and fabric, and can be used for allocating the bush cream rinse.
The inventive method can reduce the energy and the water consumption in the hematoxylin powder dyes preparation process, reduces preparation cost and dye impurity rate.
(5) embodiment
Embodiment 1: hematoxylin powder dyes preparation method and step
Step 1, hot water extraction hematoxylin
Under the normal temperature, the bush core of pulverizing is added in 20 times of weight water, be heated to 90 ℃, extract 1h, extract altogether 3 times.
Step 2, employing sieve
Adopt 180 order steel-wire screens while hot bush feed liquid, material slag mixture to be carried out coarse filtration, with separation bush feed liquid and material slag, and merge each time filtrate, make reddish yellow hematoxylin extracting solution.
Step 3, filter paper suction filtration
Fast qualitative filter paper is placed on the Büchner funnel, utilize vacuum pump to vacuumize (vacuum tightness is 0.098MPa) feed liquid is carried out suction filtration.
Step 4, micro-filtrate membrane filtration removal of impurities degerming
The employing recycle pump will be that the feed liquid below 35 ℃ is passed through the microfiltration membrane fluid inlet through the temperature of filter paper, entering material is that polyvinylidene difluoride (PVDF) (PVDF), aperture are 0.2 μ m external-compression type microfiltration membrane, Adjustment operation pressure is 0.04MPa, do not see through liquid and still be back to former liquid container, repeatedly move to through liquid and substantially do not flow out, collect respectively clarification bright see through liquid and contain impurity do not see through liquid.
Step 5, the concentrated hematoxylin solution of employing ultra-filtration membrane
The employing molecular weight cut-off is 3000 hydrophobicity polysulphones hyperfiltration membrane, and the bright feed liquid of clarification that sees through microfiltration membrane is concentrated, and being concentrated into the feed liquid solid content is 5%.In the micro-filtration membrane concentration process, regulating membrane operations pressure is 0.02MPa.The trapped fluid that sees through ultra-filtration membrane is the hematoxylin concentrated solution, and concentrated solution carries out the drying process with atomizing in lower step, and very low through hematoxylin content in the liquid, recycles the extraction hematoxylin.
Step 6, spraying drying
Adopt spray-drier, with the evaporation of the moisture in the hematoxylin concentrated solution, make the high hematoxylin powder dyes of effective pigment composition content.
Embodiment 2: hematoxylin powder dyes preparation method and step
Step 1: the recycle ultrafiltration membrane permeate liquid prepares method and the step of hematoxylin powder dyes
Under the normal temperature, the bush core of pulverizing is added in 30 times of weight ultrafiltration membrane permeate liquid, be heated to 90 ℃, extract 1.5h, extract 3 times.
Step 2: sieve
Adopt 120 order steel-wire screens to carry out coarse filtration, with separation bush feed liquid and material slag, and merge each time extraction filtrate.
Step 3: filter paper suction filtration
With the step 3 among the embodiment 1.
Step 4: adopt the further clear filtrate of microfiltration membrane
Adopt recycle pump will be through the temperature of filter paper feed liquid below 35 ℃ to enter material by fluid inlet be polyvinylidene difluoride (PVDF) (PVDF), aperture 0.1 μ m external-compression type microfiltration membrane, regulating membrane operations pressure is 0.05MPa, still is back to former liquid container through liquid.Collect respectively bright the seeing through liquid and contain the more polymictic liquid that do not see through of clarification.
Step 5, the concentrated hematoxylin solution of employing ultra-filtration membrane
The employing molecular weight cut-off is 2000 PS ultra-filtration membrane, and the bright feed liquid of clarification that sees through microfiltration membrane is concentrated, and being concentrated into the feed liquid solid content is 5%.In the membrane concentration process, regulating membrane operations pressure is 0.04MPa.The trapped fluid that sees through ultra-filtration membrane is the hematoxylin concentrated solution, and concentrated solution carries out the drying process with atomizing in lower step, and very low through hematoxylin content in the liquid, again recycles the extraction hematoxylin.
Step 6: spraying drying
With embodiment 1 step 6.
Claims (1)
1. method that adopts membrane separation technique to prepare hematoxylin powder dyes, it is characterized in that: described method comprises following processing step:
Step 1, hot water extraction hematoxylin
Under the normal temperature, the bush core of pulverizing is added in the 20-30 times of weight water, be heated to temperature 80-100 ℃, extract 1-1.5h, extract 2-3 time;
Step 2, employing sieve
Adopt 120-200 order metallic sieve while hot hematoxylin solution, material slag mixture to be carried out coarse filtration and separate, expect slag to remove, and each time filtrate is merged, make reddish yellow hematoxylin extracting solution;
Step 3, filter paper suction filtration
Filter paper is placed on the Büchner funnel, utilize vacuum pump that described reddish yellow hematoxylin extracting solution is carried out suction filtration;
Step 4, micro-filtrate membrane filtration removal of impurities degerming
The employing recycle pump will be that the feed liquid below 35 ℃ is passed through the microfiltration membrane fluid inlet through the temperature of filter paper, described microfiltration membrane material is that polyvinylidene difluoride (PVDF) (PVDF), aperture are 0.1-0.4 μ m, external-compression type, regulating the microfiltration membrane working pressure is 0.02-0.07MPa, see through liquid and still be back to former liquid container, collect respectively clarification bright see through liquid and contain impurity do not see through liquid;
Step 5, the concentrated bush extracting solution of ultra-filtration membrane
Adopting molecular weight cut-off is the hydrophobicity polysulphones hyperfiltration membrane of 1000-5000, and the bright feed liquid of clarification that sees through microfiltration membrane is concentrated, and being concentrated into the feed liquid solid content is 5-10%; In the ultra-filtration membrane concentration process, regulating membrane operations pressure is 0.02-0.04MPa; The trapped fluid that sees through ultra-filtration membrane is the hematoxylin concentrated solution, and concentrated solution carries out the drying process with atomizing in lower step, and very low through hematoxylin content in the liquid, recycles the extraction hematoxylin;
Step 6, spraying drying
Adopt spray-drier, with the evaporation of the moisture in the described hematoxylin concentrated solution, make the higher hematoxylin powder dyes of purity.
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| CN 200910264655 CN101747662B (en) | 2009-12-25 | 2009-12-25 | Method for preparing hematoxylin powder dyes |
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| CN 200910264655 CN101747662B (en) | 2009-12-25 | 2009-12-25 | Method for preparing hematoxylin powder dyes |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983991A (en) * | 2010-07-26 | 2011-03-09 | 杭州集美印染有限公司 | Preparation method and dyeing method of sapelli wood natural dye |
| CN102329294A (en) * | 2011-07-26 | 2012-01-25 | 苏州宝泽堂医药科技有限公司 | Method for extracting brasilein |
| CN102433016B (en) * | 2011-10-14 | 2013-11-20 | 山西大学 | Method for preparing edible pigment from medicinal-component-extracted raffinate of sapanwood |
| CN103571227A (en) * | 2013-11-10 | 2014-02-12 | 哈尔滨市工艺美术有限责任公司 | Formula and production method for preparing silver red wheat straw dye |
| CN104480756A (en) * | 2014-12-22 | 2015-04-01 | 江南大学 | Method for dyeing cellulosic fiber fabric by sorghum husk pigment |
| CN108948782B (en) * | 2018-07-08 | 2020-04-03 | 杭州彩润科技有限公司 | Method for producing plant dye by adopting red wood chips |
Citations (2)
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| CN101077942A (en) * | 2007-04-27 | 2007-11-28 | 海澜集团有限公司 | Method for refining powdered catechu dye by film separation technique and dyeing method thereof |
| CN101555359A (en) * | 2009-05-27 | 2009-10-14 | 青岛鹏远天然色素研究所 | Grape skin red pigment preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077942A (en) * | 2007-04-27 | 2007-11-28 | 海澜集团有限公司 | Method for refining powdered catechu dye by film separation technique and dyeing method thereof |
| CN101555359A (en) * | 2009-05-27 | 2009-10-14 | 青岛鹏远天然色素研究所 | Grape skin red pigment preparation method |
Non-Patent Citations (1)
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Application publication date: 20100623 Assignee: Luolai Home Textile Co., Ltd. Assignor: Jiangnan University Contract record no.: 2015320010027 Denomination of invention: Method for preparing hematoxylin powder dyes Granted publication date: 20130313 License type: Exclusive License Record date: 20150401 |
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