CN102250489B - Preparation method of lychee seed natural dye and application thereof as fabric coloring agent - Google Patents
Preparation method of lychee seed natural dye and application thereof as fabric coloring agent Download PDFInfo
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- CN102250489B CN102250489B CN 201110129168 CN201110129168A CN102250489B CN 102250489 B CN102250489 B CN 102250489B CN 201110129168 CN201110129168 CN 201110129168 CN 201110129168 A CN201110129168 A CN 201110129168A CN 102250489 B CN102250489 B CN 102250489B
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Abstract
The invention discloses a preparation method of a lychee seed natural dye and application thereof as a fabric coloring agent. The preparation method of the lychee seed natural dye comprises the following steps of: cleaning, air-drying and mechanically crushing lychee seeds; adding the crushed lychee seeds to an ethanol water solution containing 10-15g/L sodium hydroxide; reflowing and extracting at a temperature of 70-90DEG C for 1-2h to obtain an extraction solution; then filtering, and distilling the extraction solution at a reduced pressure to obtain the concentrated lychee seed natural dye, wherein the volume percent concentration of the ethanol water solution is 10-20 percent, the mass ratio of the crushed lychee seeds to an ethanol water solution 1:(10-30), and the volume of the concentrated lychee seed natural dye is 1/6-1/2 of that of the ethanol water solution. The preparation method disclosed by the invention adopts a simple process and has high extraction rate of effective components. The obtained dye has favorable compatibility with the ecological environment and can be biologically degraded. According to the preparation method disclosed by the invention, the natural dye is prepared by using the lychee seeds, thus the prices is low, resources of natural world are fully utilized and the market prospect is very wide.
Description
Technical field
The present invention relates to natural dyestuff and Application Areas thereof, particularly relate to a kind of preparation method of Semen Litchi natural dyestuff, and as the application of textile dyeing agent.
Background technology
Natural dyestuff refers to extract root, leaf, bark, shell, flower or animal secretions, the mineral substance from plant, can not cause environmental pollution in the preparation process, and can be by environment degradable.The part natural dyestuff also has the function of medicinal health-care except dyeing.Constantly strengthen and advocate under the tide of green consumption product in the mankind's environmental consciousness, natural dyestuff is at the high grade true silk goods, health-care underclothes, and home textile product has a wide range of applications in the adornment field.
Lichee is Sapindaceae lichee platymiscium, and aiphyllium produces areas such as southwest China, south and Guangdong, the southeast, Guangxi, Fujian, Sichuan, Taiwan, Yunnan.Lichee is good fruit variety, and lichee is nutritious, carries according to Compendium of Material Medica: lichee can " quench the thirst, beneficial people's color, logical god, intelligence development, strong gas, control scrofula, knurl is gone to live in the household of one's in-laws on getting married ... " etc.Litchi fruits is except edible, and nuclear is used as medicine and is the convergence pain killer, controls motive pain and hernia.Timber is solid, dark red brown, and texture grace, corrosion resistant always are first-class name material.Spending manyly, be rich in nectary, is important nectariferous plant.Contain flavones, phenolic acid compound in the Semen Litchi, the pigment content height, moreover, Semen Litchi extract has stronger bactericidal antiphlogistic effect, and the effect of assisting therapy may be arranged tetter.
Find that by prior art documents Chen Jie studies extraction and the stability of Semen Litchi brown pigments in Ji'nan University's master thesis " Semen Litchi The Chemical Constituents (I)-pigment extracts and determined amino acid " (in June, 2006) literary composition; (P:18-20), its extracting method all is to carry out in ethanolic soln to Wang Haiyan for " guizhou chemical industry ", 2003 the 28th volumes, and extraction efficiency is relatively poor at " extraction of Semen Litchi brown pigments and stability study ".
At present, for the research of Semen Litchi, only be used for Chinese medicine and food dye aspect on a small quantity, about preparation method and the application art research of Semen Litchi natural dyestuff, not seeing both at home and abroad has report.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of Semen Litchi natural dyestuff and as the application of textile dyeing agent.
Studies show that through the contriver, Semen Litchi extract is bright-coloured reddish-brown, its maximum absorption wavelength is at 400～420nm, protein fibre and fabric had good dyeing behavior, can obtain distinct colors by different mordant processing, and colour fastness is good, is an excellent property natural plant dye.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of this Semen Litchi natural dyestuff may further comprise the steps:
With Semen Litchi clean, dry, after the mechanical disintegration, the Semen Litchi crushed material is joined in the aqueous ethanolic solution that contains sodium hydroxide 10～15g/L, obtain extracting solution at 70～90 ℃ of following refluxing extraction 1～2h, then described extracting solution is filtered the Semen Litchi natural dyestuff that also underpressure distillation obtains concentrating; The concentration of volume percent of described aqueous ethanolic solution is 10～20%, and the mass ratio of described Semen Litchi crushed material and aqueous ethanolic solution is 1:10～30, and the volume of described concentrated Semen Litchi natural dyestuff is 1/6～1/2 of described aqueous ethanolic solution volume.
The application of Semen Litchi natural dyestuff of the present invention is: described Semen Litchi natural dyestuff is as the coloration of textile materials agent.
Utilize Semen Litchi natural dyestuff of the present invention that a kind of method that fabric dyes be may further comprise the steps:
1) fabric is carried out pre-mordant dyeing and handle, take out fabric after pre-mordant dyeing disposes and clean, extract; The condition that described pre-mordant dyeing is handled is: contain ferrous ion and/or aluminum ion in the used mordant solution, the weight of mordant be described fabric weight 1～5%, bath raio is 1:10～50, temperature is 60～80 ℃, the time is 30～45min;
2) will put in the dye liquor through the fabric that pre-mordant dyeing is handled and dye, after dyeing finishes with fabric washing, oven dry; Described dye liquor is formulated by the Semen Litchi natural dyestuff and the water that concentrate, and the pH value of described dye liquor is 4～6, wherein the quality of the Semen Litchi natural dyestuff of Nong Suoing account for dye liquor quality 5～25%; The condition of controlling during dyeing is: bath raio is 1:10～50, and temperature is 80～100 ℃, and the time is 45～75min.
Utilize Semen Litchi natural dyestuff of the present invention that the another kind of method that fabric dyes be may further comprise the steps:
1) fabric dropped in the dye liquor dye, after dyeing finishes with fabric washing, oven dry; Described dye liquor is formulated by the Semen Litchi natural dyestuff and the water that concentrate, and the pH value of described dye liquor is 4～6, wherein the quality of the Semen Litchi natural dyestuff of Nong Suoing account for described dye liquor quality 5～25%; The condition of controlling during dyeing is: bath raio is 1:10～50, and temperature is 80～100 ℃, and the time is 45～75min;
2) fabric that has dyeed is carried out the back mordant dyeing and handle, take out fabric after back mordant dyeing disposes and clean, extract; The condition that the mordant dyeing of described back is handled is: contain ferrous ion and/or aluminum ion in the used mordant solution, mordant weight be described fabric weight 1～5%, bath raio is 1:10～50, temperature is 60～80 ℃, the time is 30～45min.
Beneficial effect of the present invention is:
The present invention adopts ethanol-alkaline solution circumfluence method to extract brown natural dyestuff from Semen Litchi, extraction process is simple, extracts active ingredients efficient apparently higher than additive methods such as alcohol refluxs (through simultaneous test as can be known, ethanol-alkaline solution circumfluence method pigment extraction efficiency is 5～9 times of alcohol reflux efficient), can not cause environmental pollution in the leaching process; Extract is good to the protein fibre dyefastness; The dyeing back uses the environmental protection mordant to handle can increase chromatogram; Dyeing back fabric color is soft, and that dress safety does not have is carcinogenic, teratogenesis or cause allergic reaction; Good, biodegradable with the ecotope consistency; And utilize Semen Litchi to prepare the natural dyestuff low price, and having taken full advantage of natural resource, market outlook are very wide.
Embodiment
Embodiment 1:
Semen Litchi is cleaned, dried, after the mechanical disintegration, take by weighing 1 kilogram of Semen Litchi crushed material and join in 10 kilograms of aqueous ethanolic solutions that contain sodium hydroxide, and obtain extracting solution at 90 ℃ of following lixiviate 120min.Wherein, the concentration of volume percent of aqueous ethanolic solution is 10%, contains sodium hydroxide 10g in every liter of aqueous ethanolic solution.The back to extracting solution filter, centrifugal and underpressure distillation is concentrated into 5 liters, the Semen Litchi natural dyestuff that obtains concentrating.
Embodiment 2:
Semen Litchi is cleaned, dried, after the mechanical disintegration, take by weighing 1 kilogram of Semen Litchi crushed material and join in 20 kilograms of aqueous ethanolic solutions that contain sodium hydroxide, and obtain extracting solution at 80 ℃ of following lixiviate 90min.Wherein, the concentration of volume percent of aqueous ethanolic solution is 15%, contains sodium hydroxide 12.5g in every liter of aqueous ethanolic solution.Then earlier extracting solution is filtered, after more centrifugal and underpressure distillation be concentrated into 5 liters, namely get concentrated Semen Litchi natural dyestuff.
Embodiment 3:
Semen Litchi is cleaned, dried, after the mechanical disintegration, take by weighing 1 kilogram of Semen Litchi crushed material and join 30 kilograms of aqueous ethanolic solutions that contain sodium hydroxide, and obtain extracting solution at 70 ℃ of following lixiviate 60min.Wherein, the concentration of volume percent of aqueous ethanolic solution is 20%, contains sodium hydroxide 15g in every liter of aqueous ethanolic solution.Then earlier extracting solution is filtered, after more centrifugal and underpressure distillation be concentrated into 5 liters, the Semen Litchi natural dyestuff that is concentratedly.Embodiment 4:
1) real silk fabric is joined in the ferrous sulfate aqueous solution, under 60 ℃, carry out pre-mordant dyeing and handle 45min; Wherein, the weight of ferrous sulfate is 1% of the real silk fabric weight that adds, and bath raio is 1:50.The back taking-up fabric that disposes is cleaned, and extracts.
2) Semen Litchi natural dyestuff and the water that concentrates is made into dye liquor.In the dye liquor, the mass percent concentration of the Semen Litchi natural dyestuff that concentrates is 25%, and the pH value of dye liquor is 4, and bath raio is 1:30, and the real silk fabric that the pre-mordant dyeing of above-mentioned warp is handled immerses in the dye liquor, and in 80 ℃ of dyeing 75min.Dye finish after with the real silk fabric washing, oven dry gets the brown real silk fabric.
3) real silk fabric after the dyeing as calculated machine color measurement and color match instrument to record the K/S value be 8.23.
Embodiment 5:
1) wool fabric is joined in the ferrous sulfate aqueous solution, under 70 ℃, carry out pre-mordant dyeing and handle 30min.Wherein, the weight of ferrous sulfate is 3% of the wool fabric weight that adds, and bath raio is 1:30.The back taking-up fabric that disposes is cleaned, and extracts.
2) Semen Litchi natural dyestuff and the water that concentrates is made into dye liquor.In the dye liquor, the mass percent concentration of the Semen Litchi natural dyestuff that concentrates is 15%, and the pH value of dye liquor is 5, bath raio 1:50, and the wool fabric that the pre-mordant dyeing of above-mentioned warp is handled immerses in the dye liquor, and in 90 ℃ of dyeing 60min.Dye finish after with the wool fabric washing, oven dry gets the brown wool fabric.
3) wool fabric after the dyeing as calculated machine color measurement and color match instrument to record the K/S value be 5.78.
Embodiment 6:
1) wool fabric is joined in the alum solution, under 80 ℃, carry out pre-mordant dyeing and handle 38min.Wherein, the weight of alum is 5% of the wool fabric weight that adds, and bath raio is 1:10.Disposing, it is clean to take out fabric, extracts.
2) Semen Litchi natural dyestuff and the water that concentrates is made into dye liquor.In the dye liquor, the mass percent concentration of the Semen Litchi natural dyestuff that concentrates is 5%, and the pH value of dye liquor is 6, bath raio 1:10, and the wool fabric that the pre-mordant dyeing of above-mentioned warp is handled immerses in the dye liquor, and in 100 ℃ of dyeing 45min.Dye and finish the wool fabric washing, oven dry gets the yellowish brown wool fabric.
3) wool fabric after the dyeing as calculated machine color measurement and color match instrument to record the K/S value be 3.58.
Embodiment 7:
1) real silk fabric is immersed in the water, makes it fully wetting, after extract stand-by.
2) Semen Litchi natural dyestuff and the water that concentrates is made into dye liquor.In the dye liquor, the mass percent concentration of the Semen Litchi natural dyestuff that concentrates is 15%, and the pH value of dye liquor is 5, and bath raio is that 1:30 immerses above-mentioned real silk fabric in the dye liquor, and in 90 ℃ of dyeing 60min.Dye and finish the real silk fabric washing, extract.
3) real silk fabric after will dyeing joins in the alum solution, carries out the back mordant dyeing in 80 ℃ and handles 30min.Wherein, the weight of alum is 5% of the real silk fabric weight that adds, and bath raio is 1:30.Disposing, it is clean to take out fabric, and oven dry gets the olive brown real silk fabric.
Real silk fabric after the dyeing as calculated machine color measurement and color match instrument to record its K/S value be 7.25.
Embodiment 8:
1) real silk fabric is immersed in the water, makes it fully wetting, after extract stand-by.
2) Semen Litchi natural dyestuff and the water that concentrates is made into dye liquor.In the dye liquor, the mass percent concentration of the Semen Litchi natural dyestuff that concentrates is 25%, and the pH value of dye liquor is 4, and bath raio 1:50 immerses above-mentioned real silk fabric in the dye liquor, and in 80 ℃ of dyeing 75min.Dye and finish the real silk fabric washing, extract.
3) real silk fabric after will dyeing joins in the ferrous sulfate aqueous solution, carries out the back mordant dyeing in 70 ℃ and handles 45min.Wherein, the weight of ferrous sulfate is 1% of the real silk fabric weight that adds, and bath raio is 1:10.Dispose and take out clean, the oven dry of fabric, get the brown real silk fabric.
4) real silk fabric after the dyeing as calculated machine color measurement and color match instrument to record the K/S value be 9.25.
Embodiment 9:
1) wool fabric is immersed in the water, makes it fully wetting, after extract stand-by.
2) Semen Litchi natural dyestuff and the water that concentrates is made into dye liquor.In the dye liquor of preparing, the mass percent concentration of the Semen Litchi natural dyestuff that concentrates is 5%, and the pH value of dye liquor is 6, and bath raio 1:10 immerses above-mentioned wool fabric in the dye liquor, and in 100 ℃ of dyeing 45min.Dye and finish wool fabric washing, oven dry.
3) wool fabric after will dyeing joins in the ferrous sulfate aqueous solution, carries out the back mordant dyeing in 60 ℃ and handles 30min.Wherein, the weight of ferrous sulfate is 3% of the wool fabric weight that adds, and bath raio is 1:50.Dispose and take out clean, the oven dry of fabric, get the brown wool fabric.
4) wool fabric after the dyeing as calculated machine color measurement and color match instrument to record the K/S value be 5.94.
Claims (4)
1. the preparation method of a Semen Litchi natural dyestuff is characterized in that, may further comprise the steps:
With Semen Litchi clean, dry, after the mechanical disintegration, the Semen Litchi crushed material is joined in the aqueous ethanolic solution that contains sodium hydroxide 10 ~ 15g/L, obtain extracting solution at 70 ~ 90 ℃ of following refluxing extraction 1 ~ 2h, then described extracting solution is filtered the Semen Litchi natural dyestuff that also underpressure distillation obtains concentrating; The concentration of volume percent of described aqueous ethanolic solution is 10 ~ 20%, and the mass ratio of described Semen Litchi crushed material and aqueous ethanolic solution is 1:10 ~ 30, and the volume of described concentrated Semen Litchi natural dyestuff is 1/6 ~ 1/2 of described aqueous ethanolic solution volume.
2. the application of the Semen Litchi natural dyestuff that obtains of a preparation method according to claim 1, it is characterized in that: described Semen Litchi natural dyestuff is as the coloration of textile materials agent.
3. one kind is utilized Semen Litchi natural dyestuff that the described preparation method of claim 1 obtains to the method that fabric dyes, and it is characterized in that, may further comprise the steps:
1) fabric is carried out pre-mordant dyeing and handle, take out fabric after pre-mordant dyeing disposes and clean, extract; The condition that described pre-mordant dyeing is handled is: contain ferrous ion and/or aluminum ion in the used mordant solution, the weight of mordant be described fabric weight 1 ~ 5%, bath raio is 1:10 ~ 50, temperature is 60 ~ 80 ℃, the time is 30 ~ 45min;
2) will put in the dye liquor through the fabric that pre-mordant dyeing is handled and dye, after dyeing finishes with fabric washing, oven dry; Described dye liquor is formulated by the Semen Litchi natural dyestuff and the water that concentrate, and the pH value of described dye liquor is 4 ~ 6, wherein the quality of the Semen Litchi natural dyestuff of Nong Suoing account for dye liquor quality 5 ~ 25%; The condition of controlling during dyeing is: bath raio is 1:10 ~ 50, and temperature is 80 ~ 100 ℃, and the time is 45 ~ 75min.
4. one kind is utilized Semen Litchi natural dyestuff that the described preparation method of claim 1 obtains to the method that fabric dyes, and it is characterized in that, may further comprise the steps:
1) fabric dropped in the dye liquor dye, after dyeing finishes with fabric washing, oven dry; Described dye liquor is formulated by the Semen Litchi natural dyestuff and the water that concentrate, and the pH value of described dye liquor is 4 ~ 6, wherein the quality of the Semen Litchi natural dyestuff of Nong Suoing account for described dye liquor quality 5 ~ 25%; The condition of controlling during dyeing is: bath raio is 1:10 ~ 50, and temperature is 80 ~ 100 ℃, and the time is 45 ~ 75min;
2) fabric that has dyeed is carried out the back mordant dyeing and handle, take out fabric after back mordant dyeing disposes and clean, extract; The condition that the mordant dyeing of described back is handled is: contain ferrous ion and/or aluminum ion in the used mordant solution, mordant weight be described fabric weight 1 ~ 5%, bath raio is 1:10 ~ 50, temperature is 60 ~ 80 ℃, the time is 30 ~ 45min.
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| CN106147289A (en) * | 2016-06-29 | 2016-11-23 | 珠海无用文化创意有限公司 | The preparation method of lichee branches and leaves liquid plant dye liquor and the application as coloring agent |
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Application publication date: 20111123 Assignee: Zhejiang Sci-Tech University Shangyu Industrial Technology Research Institute Co., Ltd. Assignor: Zhejiang University of Technology Contract record no.: X2019330000038 Denomination of invention: Preparation method of lychee seed natural dye and application thereof as fabric coloring agent Granted publication date: 20130925 License type: Common License Record date: 20191108 |