CN103360784A - Broadbean pericarp dye and extraction method and application thereof - Google Patents
Broadbean pericarp dye and extraction method and application thereof Download PDFInfo
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- CN103360784A CN103360784A CN2013102962834A CN201310296283A CN103360784A CN 103360784 A CN103360784 A CN 103360784A CN 2013102962834 A CN2013102962834 A CN 2013102962834A CN 201310296283 A CN201310296283 A CN 201310296283A CN 103360784 A CN103360784 A CN 103360784A
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Abstract
The invention discloses a broadbean pericarp dye and an extraction method and application thereof. The dye is extracted from broadbean pericarp. A preparation method of the dye comprises the following steps of: weighing, cleaning and smashing the broadbean pericarp, adding water, extracting the broadbean pericarp once under the conditions that the temperature is 80-100 DEG C, the extraction time is 50-70min and the mass ratio of the broadbean pericarp to the water is 1:10-1:30, thus obtaining the broadbean pericarp dye. The broadbean pericarp dye is convenient to extract; by adoption of aqueous solution, more colorful components can be extracted from plants; the manufactured dye has a good dyeing effect on silk broadcloth.
Description
Technical field
The present invention relates to a kind of pod of Broadbean dyestuff and extracting method and purposes.
Background technology
Pod of Broadbean is the pod shell of leguminous plants broad bean, and summer, the broad bean fruit maturation was chocolate, and during the prematurity of broad bean fruit, after getting blue or green pod shell and drying, can obtain equally the pod of Broadbean of black.The pod of Broadbean source is very wide, and general rural area results broad bean can obtain a large amount of pod of Broadbean wastes, and processing mode then is landfill or burning; In the city, behind the edible blue or green broad bean, its pod of Broadbean also abandons as waste in addition, and this not only wastes but also environmental aspect is also had certain impact.Pod of Broadbean has the part pharmaceutical use, can treat all hemorrhagic symptoms.Because the pod of Broadbean after drying is chocolate, adopts certain method therefrom the chocolate pigment to be extracted, and be used for the dyeing of textiles, not only environmental protection, and can be salvaged.
Summary of the invention
The object of the present invention is to provide a kind of effective pod of Broadbean dyestuff and extracting method and purposes to silk dyeing.
Technical solution of the present invention is:
A kind of pod of Broadbean dyestuff, it is characterized in that: be from pod of Broadbean, to extract the dyestuff that obtains, its preparation method is: take by weighing the pod of Broadbean of cleaning and pulverizing, add entry, under for the condition of 1:10~1:30, extract 1 time with quality at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean, get product.
A kind of extracting method of pod of Broadbean dyestuff is characterized in that: take by weighing the pod of Broadbean of cleaning and pulverizing, add entry, extract 1 time under for the condition of 1:10~1:30 with quality at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean, get product.
A kind of pod of Broadbean dyestuff is as the application of silk broadcloth dying agent, it is characterized in that: the pod of Broadbean dyestuff is made into the dye liquor that concentration is 5~30g/L, dye liquor pH value 2.00~5.00, wetting silk broadcloth is dropped into dye liquor, 5~90min dyes under 40~100 ℃ condition; bath raio 50:1, cooling, and taking-up is washed and is dried.
Before with the pod of Broadbean dyeing, with in the pod of Broadbean dyeing or after with the pod of Broadbean dyeing, also carry out mordant dyeing with mordant and process.
Before with the pod of Broadbean dyeing or after with the pod of Broadbean dyeing, also carry out mordant dyeing with the mordant ferrous sulfate and process.
The present invention extracts conveniently, adopts the aqueous solution can extract more colored component from plant, and the dyestuff that makes is effective to silk broadcloth dying.
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is pod of Broadbean extracting solution absorption spectrum curve figure.
Fig. 2 is that dyeing pH value is on the schematic diagram that affects of silk broadcloth dying effect.
Fig. 3 is that dyeing temperature is on the schematic diagram that affects of the thick Color of real silk.
Fig. 4 is that dyeing time is on the schematic diagram that affects of silk broadcloth dying effect.
Fig. 5 is that sodium sulfate quality concentration is on the schematic diagram that affects of silk broadcloth dying effect.
Fig. 6 is that the pod of Broadbean mass concentration is on the schematic diagram that affects of silk broadcloth dying effect.
Embodiment
A kind of pod of Broadbean dyestuff, be to extract the dyestuff that obtains from pod of Broadbean, its preparation method is: take by weighing the pod of Broadbean of cleaning and pulverizing, add entry, under for the condition of 1:10~1:30, extract 1 time with quality at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean, get product.
A kind of extracting method of pod of Broadbean dyestuff takes by weighing the pod of Broadbean of cleaning and pulverizing, and adds entry, extracts 1 time under for the condition of 1:10~1:30 with quality at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean, gets product.
A kind of pod of Broadbean dyestuff is as the application of silk broadcloth dying agent, the pod of Broadbean dyestuff is made into the dye liquor that concentration is 5~30g/L, dye liquor pH value 2.00~5.00, wetting silk broadcloth is dropped into dye liquor, 5~the 90min that under 40~100 ℃ condition, dyes, bath raio 50:1(dye liquor: silk broadcloth, weight ratio), cooling, taking-up is washed and is dried.
Before with the pod of Broadbean dyeing, with in the pod of Broadbean dyeing or after with the pod of Broadbean dyeing, also carry out mordant dyeing with mordant and process.
Before with the pod of Broadbean dyeing or after with the pod of Broadbean dyeing, also carry out mordant dyeing with the mordant ferrous sulfate and process.
1 test portion
1.1 test materials, medicine and instrument
Test materials commercially available 12102 authentic silks are practiced white crepe de Chine.
Test drug hydrochloric acid, anhydrous sodium sulphate, ferrous sulfate, copper sulfate, etc., be analytical pure, available from Nantong Merck ﹠ Co., Inc.; Pod of Broadbean is to select from Dongcheng town, Rugao City, Jiangsu 2012 early summer.
The accurate pH meter of instrument and equipment PHS-3C, Color-Eye3100 type color measurement and color match instrument, TU-1901 twin-beam ultraviolet-visible pectrophotometer, GYROWASH415 washes/dry-cleans the colour fastness machine, Y (B) 571-II type presetting system colour fastness frictiograph, Y (GB)-611-II type solarization climate test instrument.
1.2 test method
1.2.1 the extraction of pod of Broadbean natural dyestuff
Taking by weighing the pod of Broadbean of cleaning and pulverizing, add entry, is to extract 1 time under 1: 10~1: 30 the condition at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean and quality ratio, and cooling is filtered.
1.2.2 the pod of Broadbean extracting solution is to real silk fabric substantive dyeing technique
Pod of Broadbean mass concentration 5~30g/L, dye liquor pH value 2.00~5.00, wetting silk broadcloth, room temperature enters to dye, the 5~90min that under 40~100 ℃ condition, dyes, bath raio (dye liquor: fabric) 50: 1, cooling, taking-up is washed and is dried.
2.2.3 the mordant dying of silk broadcloth
Pre-matchmaker's method dyeing drops into wetting silk broadcloth room temperature and contains in the solution of 3g/L mordant, and mordant dyeing 45min under 50 ℃ of conditions takes out after washing, then uses the pod of Broadbean dye liquor by the substantive dyeing dyeing of selecting, and the cooling washing is dried.
Add the 3g/L mordant with the dyeing of matchmaker's method in the pod of Broadbean dye liquor, fully drop into wetting silk broadcloth after the dissolving, by the substantive dyeing dyeing of selecting, the cooling washing is dried.
Back dyeing is pressed the substantive dyeing dyeing of selecting with wetting silk broadcloth first with the pod of Broadbean dye liquor, take out washing, and then with the mordanting bath mordant dyeing 45min under 50 ℃ condition that contains the 3g/L mordant, the washing of lowering the temperature is dried.
1.3 test
1.3.1 the mensuration of pod of Broadbean extracting solution absorbancy
Measure with TU-1901 twin-beam ultraviolet-visible pectrophotometer.
1.3.2 the mensuration of silk broadcloth dying effect
The silk broadcloth of dyeing is folded 8 layers, measure at Color-Eye3100 type color measurement and color match instrument.
1.3.3 the mensuration of dyeing of real silk silk fabric dyefastness performance
Fastness to soaping is pressed GB/T3921-2008 " textile color stability test fastness to soaping " method A (1) and is measured, colour fastness to rubbing is pressed GB/T3920-1997 " textile color stability test colour fastness to rubbing " and is measured, and color fastness to daylight is measured by GB/T8427-2008 " textile color stability is tested the colour fastness of anti-the artificial light: xenon arc " method (3).
2 results and discussion
2.1 pod of Broadbean extraction process factor analysis
2.1.1 determining of pod of Broadbean extracting solution maximum absorption wavelength
Water is cooked extraction agent, and pod of Broadbean is extracted 40min under 100 ℃ condition, and the mass ratio of pod of Broadbean and water is 1: 40, and the absorption spectrum curve of extracting solution is seen Fig. 1.
As can be seen from Figure 1, the pod of Broadbean extracting solution does not have absorption peak in visible-range, and two absorption peaks are arranged in the ultraviolet region, is respectively 271nm and 202nm, therefore judges the extraction effect of pod of Broadbean with the absorbancy size at this two place.
2.1.2 the extraction process of optimization of orthogonal test pod of Broadbean
Three factors of the mass ratio of selective extraction temperature, extraction time, pod of Broadbean and water, each factor is chosen three levels, carries out L
9(3
3) orthogonal test, orthogonal test scheme, test-results and interpretation of result see Table 1.
Table 1 pod of Broadbean extracts L
9(3
3) orthogonal test scheme, test-results and analysis of results table
As can be seen from Table 1, affecting the pod of Broadbean extraction effect by main to inferior order is: the mass ratio that extracts temperature, extraction time, pod of Broadbean and water.When the extraction temperature was 100 ℃, the extracting solution absorbancy was maximum; During extraction time 60min, the extracting solution absorbancy is maximum; The mass ratio of pod of Broadbean and water is 1: 30 o'clock, and the extracting solution absorbancy is maximum.Analysis-by-synthesis, the Optimization Technology that obtains the extraction of pod of Broadbean natural dyestuff is: the mass ratio that extracts 100 ℃ of temperature, extraction time 60min, pod of Broadbean and water is 1: 30, extracts 1 time.
2.2 the stability study of pod of Broadbean extracting solution
2.2.1 the pod of Broadbean extracting solution is to the stability of pH value
The pH value of regulating pod of Broadbean extracting solution (the pod of Broadbean mass concentration is 10g/L) is respectively 1.02,3.02,5.00,7.03,8.99,11.01 and extraction stoste, then dilute certain multiple, measure absorbancy with ultra-violet and visible spectrophotometer, the results are shown in Table 2.
The stability of the different pH values of table 2 pod of Broadbean extracting solution
As shown in Table 2, in the pH value scope of adjusting, the maximum absorption wavelength of pod of Broadbean extracting solution is without considerable change, and the absorbancy of the long lower correspondence of maximum absorption is along with the variation of pH value slightly has fluctuation, and this shows that the pod of Broadbean extracting solution has certain stability to acid, alkali.
2.2.2 the pod of Broadbean extracting solution is to the stability of light and time
Pod of Broadbean extracting solution (the pod of Broadbean mass concentration is 10g/L) is put in respectively sunlight and dark place, measures the absorbancy of placing the different number of days extracting solution after the dilution, the results are shown in Table 3.
Table 3 extracting solution is to the stability of light and time
As can be seen from Table 3, along with the increase of placing fate, the maximum absorption wavelength of pod of Broadbean extracting solution does not change, the maximum absorbance value is along with the increase of storage period slightly changes, and place the where there is light with open in dark place more approaching, this explanation pod of Broadbean extracting solution is to the stability of light and storage period better.
3.2.3 the temperature stability of pod of Broadbean extracting solution
Pod of Broadbean extracting solution (the pod of Broadbean mass concentration is 10g/L) is processed 60min under differing temps, measure again its absorbancy after the dilution, the results are shown in Table 4.
Table 4 pod of Broadbean extracting solution is to temperature stability
As can be seen from Table 4, the pod of Broadbean extracting solution is processed in condition of different temperatures, its maximum absorption wavelength does not change, corresponding absorbancy is along with the increase for the treatment of temp slightly increases on the contrary, reach maximum value when temperature is 90 ℃, this explanation pod of Broadbean extracting solution is better to the stability of temperature.
2.3 the pod of Broadbean extracting solution is analyzed silk broadcloth substantive dyeing technological factor
2.3.1 dyeing pH value is on the impact of silk broadcloth dying effect
Fixing pod of Broadbean mass concentration 20g/L, 90 ℃ of dyeing temperatures, dyeing time 60min, bath raio 50: 1(dye liquor: fabric), the coloration result of silk broadcloth is seen Fig. 2 under the coloured differently pH value condition.
As can be seen from Figure 2, with the increase of tinction pH value, the K/S value of dyeing of real silk silk fabric descends gradually, and the pH value is in 2.00~3.00 scopes, fall is less, but dyeing pH value was greater than 3 o'clock, and dyeing pH value increases, and the thick K/S value of dyeing of real silk declines by a big margin, because pH is too little in dyeing, may bring certain damage to silk broadcloth, cause the feel of dyeing of real silk silk fabric relatively poor, the pH value that therefore dyes selects 3.00 left and right sides proper.
2.3.2 dyeing temperature is on the impact of silk broadcloth dying effect
Fixing pod of Broadbean mass concentration 20g/L, dyeing pH value 3.00, dyeing time 60min, bath raio 50: 1, dyeing temperature is seen Fig. 3 to the impact of the Color of silk broadcloth.
As seen from Figure 3, rising along with dyeing temperature, the K/S value of dyeing of real silk silk fabric increases gradually, when dyeing temperature reaches 90 ℃, the K/S value of dyeing of real silk silk fabric is maximum, and dyeing temperature increases afterwards, and the K/S value of dyeing of real silk silk fabric slightly descends, therefore, it is proper that dyeing temperature is selected 90 ℃ of optimum dyeing temperature.
2.3.3 dyeing time is on the impact of Color
Fixing pod of Broadbean mass concentration 20g/L, dyeing pH value 3.00,90 ℃ of dyeing temperatures, bath raio 50: 1, dyeing time is seen Fig. 4 to the impact of silk broadcloth dying effect.
As seen from Figure 4, dyeing time is shorter, prolongation along with dyeing time, the K/S value of dyeing of real silk silk fabric increases obviously, after dyeing time reached 45min, the K/S value rangeability of dyeing of real silk silk fabric was less, considers that dyeing time is shorter, the silk broadcloth even dyeing effect is relatively poor, so dyeing time is selected 60min.
2.3.4 sodium sulfate quality concentration is on the impact of silk broadcloth dying effect
Fixing pod of Broadbean mass concentration 20g/L, dyeing pH is 3.00, and 90 ℃ of dyeing temperatures, dyeing time are 60min, and bath raio 50: 1 adds the sodium sulfate of different mass concentration in dye liquor, and the coloration result of silk broadcloth is seen Fig. 5.
As seen from Figure 5, add sodium sulfate during dyeing, the K/S value of dyeing of real silk silk fabric descends, this be because the iso-electric point of silk broadcloth in the scope of pH value 3.5~5.2, and the pH value that dyes is about 3.00, iso-electric point less than silk broadcloth, sodium sulfate has certain slow effect of dying to dying on the dyestuff, it can also be seen that from Fig. 5 in addition, and the mass concentration of sodium sulfate increases, the K/S value of dyeing of real silk silk fabric (surperficial color depth value) descends, and can select as required whether to add the amount of sodium sulfate and adding when therefore dyeing.
2.3.5 the pod of Broadbean mass concentration is on the impact of Color
Fixing dyeing pH is 3.00, and 90 ℃ of dyeing temperatures, dyeing time are 60min, and bath raio 50: 1 only changes the mass concentration of pod of Broadbean, and the coloration result of silk broadcloth is seen Fig. 6.
As seen from Figure 6, along with the increase of pod of Broadbean mass concentration, the increase that almost is in line of the K/S value of dyeing of real silk silk fabric, this explanation pod of Broadbean extracting solution has preferably improving performance, therefore can select as required the consumption of corresponding pod of Broadbean.
3.3.6 optimization of orthogonal test pod of Broadbean extracting solution is to the technique of silk broadcloth substantive dyeing
Selective staining temperature, dyeing time, pod of Broadbean mass concentration, four factors of dyeing pH value are carried out L
9(3
4) orthogonal test, each factor is chosen three levels.Orthogonal test scheme, test-results and interpretation of result see Table 5.
Table 5 pod of Broadbean extracting solution is to silk broadcloth substantive dyeing L
9(3
4) orthogonal test scheme, test-results and analysis of results table
As can be seen from Table 2, four factors on the impact of dyeing of real silk silk fabric K/S value by main to inferior order are: dyeing pH value, pod of Broadbean mass concentration, dyeing temperature, dyeing time.In the dyeing pH value, the pH value is that 2.50 o'clock K/S values are maximum, but dyeing pH value is too little, and the damage of silk broadcloth is larger, and the pH value that therefore dyes selection 3.00 is proper; In the pod of Broadbean mass concentration, the K/S value was maximum when mass concentration was 25g/L; In dyeing temperature and the dyeing time, the K/S value of three levels is all more approaching.Analysis-by-synthesis, the pod of Broadbean extracting solution that obtains to the Optimization Technology of silk broadcloth dying is: dyeing pH value about 3.00, dyeing temperature are 90 ℃, dyeing time 60min, select as required the consumption of pod of Broadbean.
2.4 mordant dyeing is on the impact of silk broadcloth dying effect
Select ferrous sulfate and copper sulfate respectively to silk broadcloth carry out pre-mordant dyeing, with mordant dyeing and rear mordant dyeing, the Color of silk broadcloth sees Table 7.
Table 6 mordant dyeing is on the impact of silk broadcloth dying effect
As can be seen from Table 3, compare with mordant dyeing substantive dyeing silk broadcloth not, ferrous sulfate mordant dyeing, mordant dyeing obviously increase the K/S value of dyeing of real silk silk fabric, wherein increase less with mordant dyeing; Mordant dyeing makes the lightness L of dyeing of real silk silk fabric
*It is more and less with mordant dyeing decline that value descends and rear mordant dyeing descends; Mordant dyeing makes the ruddiness a of dyeing of real silk silk fabric
*Value, gold-tinted b
*Value and colorimetric purity c
*Value descend and all after mordant dyeing descend more and pre-mordant dyeing descends lessly, it is more that mordant dyeing has increased hue angle h ° of the dyeing of real silk silk fabric and rear mordant dyeing increase.
The copper sulfate mordant dyeing, the K/S value of rear mordant dying silk broadcloth slightly rises, and pre-mordant dyeing reaches with mordant dyeing decline and descends apparent in view with mordant dyeing; Pre-mordant dyeing reaches the lightness L that makes the dyeing of real silk silk fabric with mordant dyeing
*Value rises then, and mordant dyeing descends to some extent; Mordant dyeing makes the ruddiness a of dyeing of real silk silk fabric
*Value descends and rear mordant dyeing descends more; Pre-matchmaker and make the gold-tinted b of dyeing of real silk silk fabric with the matchmaker
*Value and colorimetric purity c
*The value then mordant dyeing of rising descends; Mordant dyeing is so that the hue angle h of dyeing of real silk silk fabric ° of all to some extent increase.
2.5 the dyefastness of dyeing of real silk silk fabric
Sample is measured its dyefastness with 2.4, the results are shown in Table 7.
The dyefastness of table 7 dyeing of real silk silk fabric
As can be seen from Table 4, mordant dyeing substantive dyeing silk broadcloth does not have preferably dyefastness.The ferrous sulfate mordant dyeing, pre-mordant dyeing and rear mordant dyeing have improved the color fastness to daylight of dyeing of real silk silk fabric, but slightly influential to colour fastness to rubbing, have suitably improved fastness to soaping with mordant dyeing.Copper sulfate mordant dyeing, mordant dyeing have improved fastness to soaping and the color fastness to daylight of dyeing of real silk silk fabric, on not obviously impact of colour fastness to rubbing.
3 conclusions
(1) by analyzing, the Optimization Technology that obtains the pod of Broadbean extraction is: the mass ratio that extracts 100 ℃ of temperature, extraction time 60min, pod of Broadbean and water is 1: 30.
(2) the pod of Broadbean extracting solution has preferably acid and alkali-resistance, temperature, fast light and the time is stable.
(3) by analyzing, optimization pod of Broadbean extracting solution to the technique of silk broadcloth substantive dyeing is: dyeing pH value about 3.00,90 ℃ of dyeing temperatures, dyeing time 60min, bath raio 50: 1, pod of Broadbean consumption can be selected as required.
(4) select ferrous sulfate and copper sulfate that silk broadcloth is carried out mordant dyeing, can obviously affect the color of dyeing of real silk silk fabric.
(5) mordant dyeing substantive dyeing silk broadcloth does not have the colour fastness that dyes preferably, and ferrous sulfate and copper sulfate mordant dyeing can improve fastness to soaping and the color fastness to daylight of dyeing of real silk silk fabric.
Claims (5)
1. pod of Broadbean dyestuff, it is characterized in that: be from pod of Broadbean, to extract the dyestuff that obtains, its preparation method is: take by weighing the pod of Broadbean of cleaning and pulverizing, add entry, under for the condition of 1:10~1:30, extract 1 time with quality at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean, get product.
2. the extracting method of a pod of Broadbean dyestuff is characterized in that: take by weighing the pod of Broadbean of cleaning and pulverizing, add entry, extract 1 time under for the condition of 1:10~1:30 with quality at 80~100 ℃ of temperature, time 50~70min, pod of Broadbean, get product.
3. a pod of Broadbean dyestuff is as the application of silk broadcloth dying agent, it is characterized in that: the pod of Broadbean dyestuff is made into the dye liquor that concentration is 5 ~ 30g/L, dye liquor pH value 2.00~5.00, wetting silk broadcloth is dropped into dye liquor, 5~90min dyes under 40~100 ℃ condition; bath raio 50:1, cooling, and taking-up is washed and is dried.
4. pod of Broadbean dyestuff according to claim 1 is as the application of silk broadcloth dying agent, it is characterized in that: before with the pod of Broadbean dyeing, with in the pod of Broadbean dyeing or after with the pod of Broadbean dyeing, also carry out mordant dyeing with mordant and process.
5. pod of Broadbean dyestuff according to claim 4 is characterized in that as the application of silk broadcloth dying agent: before with the pod of Broadbean dyeing or after with the pod of Broadbean dyeing, also carry out mordant dyeing with the mordant ferrous sulfate and process.
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Cited By (1)
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CN107805955A (en) * | 2017-11-15 | 2018-03-16 | 南通大学 | A kind of diaphragma juglandis dyeing method |
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CN1876671A (en) * | 2006-07-17 | 2006-12-13 | 北京宝泰宁堂生物技术有限公司 | Soybean isoflavone extract, its preparation process and pharmaceutical compositions containing same |
CN101280525A (en) * | 2008-06-05 | 2008-10-08 | 重庆市农业科学院 | Natural staining agent, preparation thereof and application thereof to silk dyeing |
CN101709152A (en) * | 2009-12-02 | 2010-05-19 | 中国农业科学院植物保护研究所 | Natural plant dye, preparation method and application thereof |
CN102911517A (en) * | 2012-10-30 | 2013-02-06 | 中国农业科学院茶叶研究所 | Preparation method and usage of special tea dye for silk |
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CN1031549A (en) * | 1987-08-18 | 1989-03-08 | 蔡传英 | The extracting method of polyphenol edible natural pigment |
JPH0319985A (en) * | 1989-06-13 | 1991-01-29 | Nishizaki Orimono Senshoku:Kk | Method for dyeing with 'go-ishi-cha' |
CN1876671A (en) * | 2006-07-17 | 2006-12-13 | 北京宝泰宁堂生物技术有限公司 | Soybean isoflavone extract, its preparation process and pharmaceutical compositions containing same |
CN101280525A (en) * | 2008-06-05 | 2008-10-08 | 重庆市农业科学院 | Natural staining agent, preparation thereof and application thereof to silk dyeing |
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