CN106189347A - A kind of technique extracting nanoscale stain from plant - Google Patents
A kind of technique extracting nanoscale stain from plant Download PDFInfo
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- CN106189347A CN106189347A CN201610554077.2A CN201610554077A CN106189347A CN 106189347 A CN106189347 A CN 106189347A CN 201610554077 A CN201610554077 A CN 201610554077A CN 106189347 A CN106189347 A CN 106189347A
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- plant
- stain
- supersound extraction
- nanoscale
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
Abstract
The invention discloses a kind of technique extracting nanoscale stain from plant, comprise the following steps: plant is pulverized by (1), it is then added in acid solution, described plant is (1 3) with the mass ratio of acid solution: (1 3), stir, place 30 90 minutes, filter, obtain acidolysis material；(2) acidolysis material is added to the water, supersound extraction is carried out after regulation pH to 3 10, described acidolysis material is 1:10 1:50 with the mass ratio of water, supersonic frequency is 10 80KHz, first with 38 42 DEG C of supersound extraction 15 25 minutes, then with 88 92 DEG C of supersound extraction 5 15 minutes, finally with 18 22 DEG C of supersound extraction 25 35 minutes, filter, collect filtrate；(3) filtrate is concentrated, lyophilization；(4) extra-fine grinding.The nanoscale stain extraction process of the present invention, low for equipment requirements, technique is simple, and extraction efficiency is high, extracts the stain pure natural obtained, safe to the human body, can be widely applied to textile dyeing, tattoo eyeline, the literary composition human body skin such as lip, tattooing lid margin dyeing.
Description
Technical field
The present invention relates to vegetable dyeing agent extractive technique field, be specifically related to a kind of extraction nanoscale stain from plant
Technique.
Background technology
The definition be given according to Britain's stain and association of dyeing man, " natural dyeing agent " refers to from plant, animal or ore deposit
Produce acquisition, the little or no stain through chemical process in resource.Vegetable dyeing agent is most important in natural dyeing agent
A class, nonhazardous wide with its source, of low pollution, insect protected sterilization are beneficial to the good characteristics such as preservation and take the course of its own.General plant
Leaf, skin, flower and root all contain a certain amount of pigment.
China is vast in territory, and vast territory and abundant resources, vegetable dyeing agent aboundresources.Stain floristics is a lot, has arbor, filling
Wood, also has draft, liana.Having plenty of the wild plant that hill is spontaneous, have plenty of the plant of rural area cultivation, type, the place of production are different,
Its pigment content is the most inconsistent.The traditional main stain plant of China has the most several:
(1) red
Red staining agent is present in nature not as Yellow colorant in a large number, and most red staining agent is hidden
In the body of root, bark or the lead insecticide of plant.Although the limited source of red staining agent, but they are a kind of plant
The a large amount of color base of middle existence, the most easily extracts, and relatively main and conventional natural red stain is Radix Rubiae and lac.
(2) yellow
Yellow is the most lively, is also stain the most sufficient in all form and aspect of nature existence.Yellow dye can be produced
The quantity of the plant of toner is more much more than the quantity of the plant producing other colors staining agent.Turmeric dyeing agent is spreading out of Rhizoma Curcumae Longae
Biology, is one of stain most notable and the most bright-coloured in natural origin Yellow colorant.
(3) blue
From ancient times to the present, one of always main and the most the most frequently used indigo blue dyeing agent, blue dyeing agent can with polygonum tinctorium ait.,
Isatis indigotica Fort., Folium et Caulis Indigoferae Tinctoriae, Acanthaceous indigo, spirulina extract.
(4) purple
Violet vegetable dyeing agent includes Radix Arnebiae (Radix Lithospermi), Lignum pterocarpi indici, wild Herba Amaranthi tricoloris, Herba basellae rubrae, auspicious wood, Folium Perillae etc..Radix Arnebiae (Radix Lithospermi) is modal purple
Colour system stain, Li Shizhen (1518-1593 A.D.) says: " this showy flowers of herbaceous plants Rhizoma Seu Herba Bergeniae is purple, can contaminate purple ".Radix Arnebiae (Radix Lithospermi) is invigorated blood circulation, eliminating inflammation and expelling toxin effect.
(5) Lycoperdon polymorphum Vitt and black
Element Pedicellus et Pericarpium Trapae, Galla Chinensis, Fructus rhois chinensis, Ke Shu, Folium Querci dentatae (if Mongolian oak), Ramulus et folium glochidionis eriocarpi (Folium Glochidii Eriocarpi), Herba Gelsemii Elegantis (Herba Gelsemii Elegantis), Platycarya strobilacea, Cortex Sapii Radicis, wild rice etc.
For Lycoperdon polymorphum Vitt and black plant black stain.Tannin vegetable dyeing agent is mainly utilized to generate ash, black system through mordant dyeing on fiber.
(6) green system
The plant of green system has Fructus rhamni (Rhamnus davurica Pall.) etc., and it is perennial defoliation small arbor or shrub, has another name called mountain Fructus Pruni salicinae, green son, freezes green,
The greenest etc..Stain pigment composition is present among tender fruit and base of leaf, is referred to as freezing green, is natural greens few in number in ancient times
One of stain is green also known as China in the world.
(7) the natural dyeing agent of other color
Orange natural dyeing agent can be extracted from plant, such as the flower of dahlia plant, or obtains from mineral origin
Arrive, such as the clay of a kind of redness.Brown system vegetable dyeing agent has Semen Fagopyri Esculenti, Semen sojae atricolor, prunus mume (sieb.) sieb.et zucc., tea, chestnut, birch etc..
Natural dyeing agent can meet mankind's regress into nature, pursue natural demand, shorter and shorter at synthetic colourant raw material
Lack, environmental pollution is increasingly severe, even have today of carcinogenesis to people, nontoxic, non-stimulated to human body, tone is unique,
The natural dyeing agent with ecological environment with excellent compatibility is undoubtedly focus of concern.
Summary of the invention
For above-mentioned deficiency present in prior art, the technical problem to be solved is to provide a kind of from plant
The technique of middle extraction nanoscale stain.
The present invention seeks to be achieved through the following technical solutions:
A kind of technique extracting nanoscale stain from plant, comprises the following steps:
(1) being pulverized by plant, be then added in acid solution, described plant is (1-3) with the mass ratio of acid solution: (1-3), stirs
Mix uniformly, place 30-90 minute, filter, obtain acidolysis material；
(2) acidolysis material is added to the water, after regulation pH to 3-10, carries out the mass ratio of supersound extraction, described acidolysis material and water
For 1:10-1:50, supersonic frequency is 10-80KHz, first with 38-42 DEG C of supersound extraction 15-25 minute, more ultrasonic carries with 88-92 DEG C
Take 5-15 minute, finally with 18-22 DEG C of supersound extraction 25-35 minute, filter, collect filtrate；
(3) filtrate is concentrated, lyophilization；
(4) extra-fine grinding.
Preferably, described plant is Pedicellus et Pericarpium Trapae, Galla Chinensis, Fructus rhois chinensis, Ke Shu, Folium Querci dentatae, Ramulus et folium glochidionis eriocarpi (Folium Glochidii Eriocarpi), Herba Gelsemii Elegantis, Platycarya strobilacea, crow
The mixture of one or more in Chinese tallow tree, wild rice.
Preferably, the temperature of the acid solution in described step (1) is 10-30 DEG C, is made up of the raw material of following mass percent:
Lactic acid 0.3-3%, hydrochloric acid 0.3-3%, acetic acid 0.3-3%, water 91-99%.
Concrete, in the present invention:
Lactic acid, No. CAS: 849585-22-4.
Hydrochloric acid, No. CAS: 7647-01-0.
Acetic acid, No. CAS: 64-19-7.
The vegetable dyeing agent extraction process of the present invention, low for equipment requirements, technique is simple, and extraction efficiency is high, and extraction obtains
Stain pure natural, safe to the human body, can be widely applied to textile dyeing, tattoo eyeline, the literary composition human body skin such as lip, tattooing lid margin dye
Color.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, the following stated, is only the preferable enforcement to the present invention
Example, not does the restriction of other forms to the present invention, and any those skilled in the art are possibly also with the disclosure above
Technology contents be changed to the Equivalent embodiments that changes on an equal basis.Every without departing from the present invention program content, according to the present invention
Technical spirit any simple modification that following example are done or equivalent variations, all fall within protection scope of the present invention.
Galla Chinensis, Classification system: Rhus chinensis Mill., have another name called hundred worm storehouses, Mass Galla chinesis et camelliae Fermentata, son, for Homoptera
The horned gall aphid of aphid section or the female worm of melaphis peitan Tsai et Tang parasitize Anacardiaceae plant " Fructus rhois chinensis " and belong to tender leaf or the leaf of other plant together
Handle, stabs and generates a kind of cryptomere consor thing insect gall, through drying a times dried gained.Galla Chinensis used by the embodiment of the present invention is bought certainly
Anshun, Anguo City reaches medical material row.
Embodiment 1
The technique extracting stain in nanoscale Galla Chinensis, comprises the following steps:
(1) gallnut extract being broken to 5 mesh, be then added in acid solution, described Galla Chinensis is 1:1 with the mass ratio of acid solution,
It is uniformly mixed, places 60 minutes, use 180 mesh filter-cloth filterings, obtain acidolysis material；
(2) acidolysis material is added to the water, uses the salt acid for adjusting pH of 1mol/L to carry out supersound extraction, described acidolysis after 5
Material and the mass ratio of water are 1:15, and supersonic frequency is 20KHz, first with 40 DEG C of supersound extraction 20 minutes, then with 90 DEG C of supersound extraction
10 minutes, finally with 20 DEG C of supersound extraction 30 minutes, use 180 mesh filter-cloth filterings, collect filtrate；
(3) reverse osmosis membrane that filtrate via hole diameter is 0.0002 μm being concentrated into density is 1.2g/cm3, then through-20 DEG C of lyophilizing
Cheng Fen.
(4) (super grinder is that Wuxi City flight song Machinery Co., Ltd. produces to use super grinder after being lyophilized into powder again
The super grinder that model is CXM) carry out extra-fine grinding to 500nm.Obtain nanoscale Galla Chinensis stain.
The temperature of the acid solution in described step (1) is 20 DEG C, is made up of the raw material of following mass percent: lactic acid 0.5%,
Hydrochloric acid 0.5%, acetic acid 0.5%, water 98.5%.It is added to the water to be uniformly mixed by lactic acid, hydrochloric acid, acetic acid and i.e. obtains acid solution.
Embodiment 2
Substantially the same manner as Example 1, differ only in: the temperature of the acid solution in described step (1) is 20 DEG C, by following
The raw material composition of mass percent: lactic acid 0.75%, acetic acid 0.75%, water 98.5%.Lactic acid, acetic acid are added to the water stirring and mix
Close and uniformly i.e. obtain acid solution.
Embodiment 3
Substantially the same manner as Example 1, differ only in: the temperature of the acid solution in described step (1) is 20 DEG C, by following
The raw material composition of mass percent: hydrochloric acid 0.75%, acetic acid 0.75%, water 98.5%.Hydrochloric acid, acetic acid are added to the water stirring and mix
Close and uniformly i.e. obtain acid solution.
Embodiment 4
Substantially the same manner as Example 1, differ only in: the temperature of the acid solution in described step (1) is 20 DEG C, by following
The raw material composition of mass percent: lactic acid 0.75%, hydrochloric acid 0.75%, water 98.5%.Lactic acid, hydrochloric acid are added to the water stirring and mix
Close and uniformly i.e. obtain acid solution.
Embodiment 5
Substantially the same manner as Example 1, differ only in, described step (2) is: be added to the water by acidolysis material, uses
The salt acid for adjusting pH of 1mol/L carries out supersound extraction after 5, and described acidolysis material is 1:15 with the mass ratio of water, and supersonic frequency is
20KHz, with 40 DEG C of supersound extraction 60 minutes, uses 180 mesh filter-cloth filterings, collects filtrate.
Embodiment 6
Substantially the same manner as Example 1, differ only in, described step (2) is: be added to the water by acidolysis material, uses
The salt acid for adjusting pH of 1mol/L carries out supersound extraction after 5, and described acidolysis material is 1:15 with the mass ratio of water, and supersonic frequency is
20KHz, with 90 DEG C of supersound extraction 60 minutes, uses 180 mesh filter-cloth filterings, collects filtrate.
Embodiment 7
Substantially the same manner as Example 1, differ only in, described step (2) is: be added to the water by acidolysis material, uses
The salt acid for adjusting pH of 1mol/L carries out supersound extraction after 5, and described acidolysis material is 1:15 with the mass ratio of water, and supersonic frequency is
20KHz, with 20 DEG C of supersound extraction 60 minutes, uses 180 mesh filter-cloth filterings, collects filtrate.
Embodiment 8
The technique extracting stain in nanoscale Radix Rubiae, comprises the following steps:
(1) Radix Rubiae being crushed to 5 mesh, be then added in acid solution, described Radix Rubiae is 1:1 with the mass ratio of acid solution, stirring
Mix homogeneously, places 60 minutes, uses 180 mesh filter-cloth filterings, obtain acidolysis material；
(2) acidolysis material is added to the water, uses the salt acid for adjusting pH of 1mol/L to carry out supersound extraction, described acidolysis after 5
Material and the mass ratio of water are 1:15, and supersonic frequency is 20KHz, first with 40 DEG C of supersound extraction 20 minutes, then with 90 DEG C of supersound extraction
10 minutes, finally with 20 DEG C of supersound extraction 30 minutes, use 180 mesh filter-cloth filterings, collect filtrate；
(3) reverse osmosis membrane that filtrate via hole diameter is 0.0002 μm being concentrated into density is 1.2g/cm3, then through-20 DEG C of lyophilizing
Cheng Fen.
(4) (super grinder is that Wuxi City flight song Machinery Co., Ltd. produces to use super grinder after being lyophilized into powder again
The super grinder that model is CXM) carry out extra-fine grinding to 500nm.Obtain nanoscale Radix Rubiae stain.
The temperature of the acid solution in described step (1) is 20 DEG C, is made up of the raw material of following mass percent: lactic acid 0.5%,
Hydrochloric acid 0.5%, acetic acid 0.5%, water 98.5%.It is added to the water to be uniformly mixed by lactic acid, hydrochloric acid, acetic acid and i.e. obtains acid solution.
Test case 1
Nanoscale Galla Chinensis stain yield embodiment 1-7 obtained is added up.Computational methods: yield (%)=five
Gall nut stain quality/Galla Chinensis quality × 100, concrete test result is shown in Table 1.
Table 1: survival rate result table
| Yield, % | |
| Embodiment 1 | 1.2 |
| Embodiment 2 | 0.7 |
| Embodiment 3 | 0.8 |
| Embodiment 4 | 0.8 |
| Embodiment 5 | 1.0 |
| Embodiment 6 | 0.9 |
| Embodiment 7 | 0.7 |
Comparing embodiment 1 and embodiment 2-4, embodiment 1 (lactic acid, hydrochloric acid, acetic acid are compounding) yield is apparently higher than embodiment
2-4 (in lactic acid, hydrochloric acid, acetic acid, arbitrarily the two is compounding).Comparing embodiment 1 and embodiment 5-7, embodiment 1 (used for three stages surpassed
Sound extracts) yield is apparently higher than in embodiment 5-7 (holding steady temperature).
Test case 2
The dyeability of nanoscale Galla Chinensis stain embodiment 1-7 obtained is tested.By Galla Chinensis stain
It is made into dye liquor for 1:20 in mass ratio with water, and its pH is all adjusted to 5, measure the dye liquor of same volume, to silk fabrics
(100wt% mulberry silk) dyes, dyeing temperature 100 DEG C, bath raio 1:25.Dyeability test result is shown in Table 2.
Table 2: dyeability test result table
| Degree of fixation (%) | Water-fastness color fastness | Colour fastness to rubbing | |
| Embodiment 1 | 96 | 5 grades | 5 grades |
| Embodiment 2 | 89 | 3 grades | 4 grades |
| Embodiment 3 | 92 | 4 grades | 4 grades |
| Embodiment 4 | 90 | 4 grades | 3 grades |
| Embodiment 5 | 88 | 4 grades | 4 grades |
| Embodiment 6 | 93 | 3 grades | 3 grades |
| Embodiment 7 | 92 | 4 grades | 4 grades |
Comparing embodiment 1 and embodiment 2-4, embodiment 1 (lactic acid, hydrochloric acid, acetic acid are compounding) dyeability is apparently higher than reality
Execute example 2-4 (in lactic acid, hydrochloric acid, acetic acid, arbitrarily the two is compounding).Comparing embodiment 1 and embodiment 5-7, embodiment 1 (uses three rank
Section supersound extraction) dyeability is apparently higher than in embodiment 5-7 (keep steady temperature supersound extraction).
Claims (3)
1. the technique extracting nanoscale stain from plant, it is characterised in that comprise the following steps:
(1) being pulverized by plant, be then added in acid solution, described plant is (1-3) with the mass ratio of acid solution: (1-3), and stirring is all
Even, place 30-90 minute, filter, obtain acidolysis material；
(2) being added to the water by acidolysis material, carry out supersound extraction after regulation pH to 3-10, described acidolysis material is 1 with the mass ratio of water:
10-1:50, supersonic frequency is 10-80KHz, first with 38-42 DEG C of supersound extraction 15-25 minute, then with 88-92 DEG C of supersound extraction 5-
15 minutes, finally with 18-22 DEG C of supersound extraction 25-35 minute, filter, collect filtrate；
(3) filtrate is concentrated, lyophilization；
(4) extra-fine grinding.
2. the technique extracting nanoscale stain from plant as claimed in claim 1, it is characterised in that: described plant is
The mixture of one or more in Pedicellus et Pericarpium Trapae, Galla Chinensis, Fructus rhois chinensis, Ke Shu, Folium Querci dentatae, Ramulus et folium glochidionis eriocarpi (Folium Glochidii Eriocarpi), Herba Gelsemii Elegantis, Platycarya strobilacea, Cortex Sapii Radicis, wild rice.
3. the technique extracting nanoscale stain from plant as claimed in claim 1, it is characterised in that: described step (1)
In the temperature of acid solution be 10-30 DEG C, be made up of the raw material of following mass percent: lactic acid 0.3-3%, hydrochloric acid 0.3-3%, second
Acid 0.3-3%, water 91-99%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107266933A (en) * | 2017-08-25 | 2017-10-20 | 中山市中广测协同创新中心 | Dyeing method on a kind of red sandalwood dyestuff and fabric |
| CN108047754A (en) * | 2017-11-29 | 2018-05-18 | 徐小毛 | A kind of extraction process of nanoscale coloring agent |
| CN108912731A (en) * | 2018-08-09 | 2018-11-30 | 界首市恒仁服饰有限公司 | A kind of preparation method of vegetable dyeing agent |
| CN109370251A (en) * | 2018-11-12 | 2019-02-22 | 苏州经贸职业技术学院 | A kind of high efficiency extraction technique of vegetable dyeing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107266933A (en) * | 2017-08-25 | 2017-10-20 | 中山市中广测协同创新中心 | Dyeing method on a kind of red sandalwood dyestuff and fabric |
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| CN109370251A (en) * | 2018-11-12 | 2019-02-22 | 苏州经贸职业技术学院 | A kind of high efficiency extraction technique of vegetable dyeing agent |
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