CN102051063A - Camphor tree dye, extracting method thereof and use thereof - Google Patents
Camphor tree dye, extracting method thereof and use thereof Download PDFInfo
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Abstract
The invention discloses a camphor tree dye, an extracting method thereof and use thereof. Primary extraction is carried out for 80 minutes at the temperature of 100 DEG C by using 0.3mol/L solution of sodium hydroxide as an extractant, wherein the ratio of solid to liquid is 1: 30. The extracted camphor tree dye can be used as a coloring agent for pure silk. The camphor tree dye is convenient to extract, more color components can be extracted from the plants by adopting alkaline water solution, and the prepared dye has a good dyeing effect on the pure silk.
Description
Technical field
The present invention relates to a kind of dyestuff and extracting method thereof and purposes.
Background technology
Existing dye species is a lot, but is generally chemical dye, pollute greatly, and common dyestuff, the effect in silk dyeing is unsatisfactory.
Natural dyestuff be meant from plant or Animal resources, obtain, seldom or not pass through the dyestuff of chemical process, it has good Environmental compatibility and medicinal health-care function.Camphor tree is the aiphyllium plant that Lauraceae belongs to, and is that China's special product preciousness is used material and economic forest seeds, also is one of main composition seeds of China's subtropical evergreen broad-leaf forest, is described as south of the River Bao Shu.Camphor tree distributes wide in China, area is big, contains at most, and kind is complete.Contain aromaticity volatile oil, camphor etc. in the Leaf of Camphortree, nature and flavor hardship, Xin Wen, have dispel the wind, the effect of dehumidifying, pain relieving, desinsection, can adopt the whole year.The Leaf of Camphortree increment is big, is again reproducible resource, therefore is subject to people's attention in recent years.
Summary of the invention
The object of the present invention is to provide a kind of effective Leaf of Camphortree dye well extracting method and purposes to silk dyeing.
Technical solution of the present invention is:
A kind of Leaf of Camphortree dyestuff is characterized in that: be to extract the dyestuff that obtains from Leaf of Camphortree, its preparation method is: adopting the sodium hydroxide solution of 0.3mol/L is extraction agent, once extract, the temperature of extracting is 100 ℃, and the time of extraction is 80 minutes, and solid-liquid ratio is 1: 30 (g: mL).
A kind of extracting method of Leaf of Camphortree dyestuff is characterized in that: adopting the sodium hydroxide solution of 0.3mol/L is extraction agent, once extracts, and the temperature of extraction is 100 ℃, and the time of extraction is 80 minutes, and solid-liquid ratio is 1: 30, extract the Leaf of Camphortree dyestuff.
A kind of Leaf of Camphortree dyestuff is characterized in that in the application as the silk broadcloth dying agent: the Leaf of Camphortree dyestuff is made into the dye liquor that concentration is 10g/L, and the pH value of regulating dye liquor is 3～3.5; Silk broadcloth after wetting is dropped into dye liquor, and dyeing temperature is 90 ℃, and dyeing time is 60 minutes, and bath raio is 50: 1 (mL: g).
Described Leaf of Camphortree dyestuff is characterized in that in the application as the silk broadcloth dying agent: also carry out mordant dyeing and handle.
The present invention extracts conveniently, adopts alkaline 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 embodiment.
Fig. 1 is the Leaf of Camphortree extracting solution absorption spectrum curve figure that the present invention adopts different extraction agents.
Fig. 2 is the influence figure of extraction time to extraction effect.
Fig. 3 is the ph stability figure of Leaf of Camphortree extracting solution.
Fig. 4 is the stability diagram of Leaf of Camphortree extracting solution to light and time.
Embodiment
A kind of extracting method of Leaf of Camphortree dyestuff, adopting the sodium hydroxide solution of 0.3mol/L is extraction agent, once extracts, the temperature of extracting is 100 ℃, and the time of extraction is 80 minutes, and solid-liquid ratio is 1: 30 (g: mL), extract product (the Leaf of Camphortree dyestuff is also referred to as the Leaf of Camphortree extracting solution).
A kind of Leaf of Camphortree dyestuff is characterized in that in the application as the silk broadcloth dying agent: the Leaf of Camphortree dyestuff is made into the dye liquor that concentration is 10g/L, and the pH value of regulating dye liquor is 3～3.5 (regulating pH with 2mol/L hydrochloric acid); Silk broadcloth after wetting is dropped into dye liquor, and dyeing temperature is 90 ℃, and dyeing time is 60 minutes, and bath raio is 50: 1 (mL: g).
Described Leaf of Camphortree dyestuff is characterized in that in the application as the silk broadcloth dying agent: also carry out mordant dyeing and handle.
Test portion
1.1 test materials, medicine and instrument
Test materials commercially available 02 authentic silk is practiced white crepe de Chine.
Test drug sodium hydroxide, yellow soda ash, hydrochloric acid, anhydrous sodium sulphate, copper sulfate, potassium aluminium sulfate, ferrous sulfate, tin protochloride, zinc chloride, etc., being analytical pure, Leaf of Camphortree picks up from young East Road, Nantong City, Jiangsu Province in August, 2009.
The accurate pH meter of instrument and equipment PHS-3C, Shanghai Precision Scientific Apparatus Co., Ltd; Color-Eye3100 type color measurement and color match instrument is managed precious science equipment company limited; TU-1901 twin-beam ultraviolet-visible pectrophotometer, the general universal apparatus company limited of analysing in Beijing; GYROWASH415 washing/dry-cleaning colour fastness machine, Britain; Y (B) 571-II type presetting system colour fastness frictiograph, Wenzhou Daiei textile standard instrument plant; SHA-C constant temperature water bath vibrator, the permanent rich instrument plant in Jintan City.
1.2 test method
1.2.1 the extraction of Leaf of Camphortree natural dyestuff
Take by weighing the Leaf of Camphortree of cleaning oven dry and pulverizing, add required extraction agent, under specified temperature, extract certain hour, cool off, filter stand-by.
1.2.2 the Leaf of Camphortree extracting solution is to the substantive dyeing of silk broadcloth
Leaf of Camphortree extracting solution 10g/L, dye liquor pH value 2.00～7.00, sodium sulfate 0～50g/L, 40～100 ℃ of dyeing temperatures, dyeing time 15～120min, bath raio 50: 1.Prepare dye liquor on request, regulate dye liquor pH value, fully wetting silk broadcloth room temperature is dropped into dye liquor, be warming up to specified temperature, the continuous 30min that dyes adds sodium sulfate, renews under this temperature and dyes the regular hour, and the cooling washing is dried.
1.2.3 silk broadcloth mordant dying
Pre-mordant dyeing look contains the silk broadcloth input in the solution of mordant earlier, handles the regular hour under the certain temperature condition, takes out cloth specimen and puts in the Leaf of Camphortree dye liquor again, dyes according to the substantive dyeing technology of optimizing, and the cooling washing is dried.
Directly the silk broadcloth input is immersed the dye liquor that contains mordant and Leaf of Camphortree dyestuff with the mordant dyeing look, dye by the substantive dyeing technology of optimizing, the cooling washing is dried.
Back mordant dyeing look is put into silk broadcloth in the Leaf of Camphortree dye liquor earlier, dyes by the substantive dyeing technology of optimizing, and takes out to drop into to contain in the solution of mordant, handles the regular hour under the certain temperature condition, and the cooling washing is dried.
1.3 performance test
1.3.1 the mensuration of Leaf of Camphortree extracting solution absorbancy: measure with TU-1800SPC ultraviolet/visible spectrophotometer.
1.3.2 the K/S value of dyeing of real silk silk fabric, L
*, a
*, b
*, C
*, h ° value mensuration: the dyeing of real silk silk fabric is built up eight layers, on Color-Eye3100 type color measurement and color match instrument, measures, the L of record dyeing of real silk silk fabric
*, a
*, b
*, C
*, h ° value and maximum reflection wavelength place the K/S value.
1.3.3 the test of dyefastness: crock fastness is pressed GB/T3920-1997 " textile color stability test colour fastness to rubbing " and is measured.
Fastness to washing is pressed GB/T3921.1-1997 " textile color stability test colour fastness to washing: test 1 " and is measured.
2 results and discussion
2.1 Leaf of Camphortree natural dyestuff extraction process factor analysis
2.1.1 different extraction agents are to the influence of Leaf of Camphortree extraction effect
Other conditions of fixed extraction, water, 1% hydrochloric acid, 1% yellow soda ash and 1% sodium hydroxide are as extraction agent respectively, and the extracting solution absorption spectrum curve is seen Fig. 1.Wherein solid-liquid ratio is 1: 40, extracts 80 ℃ of temperature, extraction time 40min, and temperature is 100 ℃ when using water as extraction agent.
As seen from Figure 1, be extraction agent with water, hydrochloric acid soln and sodium carbonate solution, the absorbancy of extracting solution is less; Make extraction agent with sodium hydroxide solution, the absorbancy maximum of extracting solution illustrates that Leaf of Camphortree is better with the sodium hydroxide solution extraction effect.Therefore, select sodium hydroxide solution as extraction agent.
2.1.2 optimization of orthogonal test extraction process
Select sodium hydroxide concentration, extract temperature, extraction time, four factors of solid-liquid ratio, each factor is chosen three levels and is carried out L
9(3
4) orthogonal test.Absorbancy of orthogonal test scheme, extracting solution (400nm) and interpretation of result see Table 1.
Table 1L
9(3
4) orthogonal test scheme, result and analysis
As can be seen from Table 1, extracting temperature to the having the greatest impact of extraction effect, secondly is sodium hydroxide concentration, and extraction time, solid-liquid ratio are less to the influence of extraction effect.Extract temperature with level 3 extraction effect the bests, extraction time and solid-liquid ratio are all with level 2 the bests, and sodium hydroxide concentration level 2 is more or less the same with the result of level 3.Take all factors into consideration, the Leaf of Camphortree natural dyestuff extracts the technology of optimizing and is: sodium hydroxide 0.3mol/L, extract 100 ℃ of temperature, extraction time 80min, solid-liquid ratio 1: 30.
2.1.3 extraction time is to the influence of extraction effect
Fixedly sodium hydroxide 0.3mol/L extracts 100 ℃ of temperature, time 80min, and solid-liquid ratio 1: 30 carries out parallel extraction 3 times to Leaf of Camphortree, the results are shown in Figure 2.
As seen from Figure 2, the absorbancy of the Leaf of Camphortree extracting solution first time is far longer than and reaches the absorbancy of extracting solution for the third time for the second time, this explanation Leaf of Camphortree extracts for the first time and has extracted most pigments, carry out the second time again and extract for the third time having little significance, therefore Leaf of Camphortree is adopted the method for once extracting.
2.2 Leaf of Camphortree extracting solution stability study
2.2.1 extracting solution is to the stability of soda acid
The pH value of regulating the Leaf of Camphortree extracting solution is respectively 3.02,5.03,6.98,9.01 and reaches and do not regulate the pH value, measures its absorbancy, the results are shown in Figure 3.
As seen from Figure 3, in the pH value scope of adjusting, the maximum absorption wavelength of Leaf of Camphortree extracting solution changes little; And along with the decline of extracting liquid pH value, the long corresponding down absorbancy of its maximum absorption descends to some extent, and this shows when pH value is hanged down, the stability decreases of extracting solution.
2.2.2 extracting solution is to the stability of light and time
The Leaf of Camphortree extracting solution is put in sunlight and dark place respectively, and the absorbancy of extracting solution the results are shown in Figure 4 after the mensuration placement different number of days.
As seen from Figure 4, along with the extracting solution prolongation of storage period, its absorbancy constantly reduces, and the absorbancy that is positioned over sunlight place extracting solution descends manyly than the absorbancy that is positioned over dark place extracting solution.Visible light have destruction according to checking colors, and may cause the destruction of pigment in the Leaf of Camphortree extracting solution, and therefore, after Leaf of Camphortree extracted, its extracting solution in time used proper.
2.3 silk broadcloth substantive dyeing technological factor is analyzed
2.3.1 dyeing pH is to the influence of Color
Fixing painted other conditions are regulated dye liquor pH value and are respectively 2.02,3.01,3.51,3.99,4.52,5.03,5.49,6.01,6.52,7.02, K/S, the L of Leaf of Camphortree extracting solution dyeing of real silk silk fabric
*, a
*, b
*, C
*And h ° of value sees Table 2.
Table 2 dyeing pH value is to the influence of Color
Annotate: Leaf of Camphortree extracting solution 10g/L, sodium sulfate 0g/L, 90 ℃ of dyeing temperatures, dyeing time 60min, bath raio 50: 1.
As can be seen from Table 2, dyeing pH value is lower, and the K/S value of dyeing of real silk silk fabric is bigger, with ruddiness and gold-tinted heavier; And dyeing pH value is bigger, the K/S value of dyeing of real silk silk fabric and with ruddiness and gold-tinted all less; With the increase of tinction pH value, the K/S value of dyeing of real silk silk fabric and with ruddiness and gold-tinted reduce gradually, lightness increases gradually, the vividness of color descends gradually, hue angle increases gradually.Because dyeing pH value is too little, may bigger damage be arranged to silk broadcloth, and uneven dyeing easily, therefore to take all factors into consideration, dyeing pH value selects 3.00～3.50 left and right sides proper.
2.3.2 dyeing temperature is to the influence of Color
The K/S of dyeing of real silk silk fabric, L under the coloured differently temperature
*, a
*, b
*, C
*And h ° of value sees Table 3.
Table 3 dyeing temperature is to the influence of Color
Annotate: dyeing pH3.02, all the other conditions are with table 2.
As can be seen from Table 3, increase along with dyeing temperature, the K/S value of dyeing of real silk silk fabric increases gradually, lightness, with gold-tinted, bright-colored degree and hue angle reduce gradually, and with ruddiness increase gradually, when 90 ℃ of dyeing temperatures, the K/S value of dyeing of real silk silk fabric reaches maximum value, along with the increase of dye liquor temperature, the K/S value of dyeing of real silk silk fabric slightly reduces afterwards.Therefore, 90 ℃ of dyeing temperature selections are more suitable.
2.3.3 dyeing time is to the influence of Color
Dyeing time sees Table 4 to the influence of silk broadcloth dying effect.
Table 4 dyeing time is to the influence of Color
Annotate: dyeing pH3.04, all the other conditions are with table 2.
As can be seen from Table 4, increase along with dyeing time, the K/S value of dyeing of real silk silk fabric, the ruddiness that has increase, lightness, with gold-tinted, bright-colored degree and color hue angle reduce gradually, when the time is 60min, the K/S value of dyeing of real silk silk fabric reaches maximum value substantially, and along with the increase of dyeing time, the K/S value increasing degree of dyeing of real silk silk fabric is little afterwards.Therefore, dyeing time selects 60min more suitable.
2.3.4 the sodium sulfate consumption is to the influence of Color
During dyeing 30min, in dye liquor, add the sodium sulfate of different amounts, K/S, the L of extracting solution dyeing of real silk silk fabric
*, a
*, b
*, C
*And h ° of value sees Table 5.
As can be seen from Table 5, add sodium sulfate in the dye liquor, the K/S of dyeing of real silk silk fabric, lightness, the ruddiness that has, gold-tinted, bright-colored degree and hue angle value change little, whether add sodium sulfate when promptly dyeing to almost not influence of dyeing.
Table 5 sodium sulfate consumption is to the influence of Color
Annotate: dyeing pH3.01, all the other conditions are with table 2.
2.2.5 optimization of orthogonal test normal dyeing technology
On the basis of single factor experiment, adopt L
9(3
3) orthogonal test method, select dye liquor pH value, dyeing temperature, three of dyeing times Color to be influenced bigger factor carry out orthogonal test.The level of each factor of orthogonal test is respectively: dyeing pH value 3.01,3.52,4.02,80 ℃, 90 ℃, 100 ℃ of dyeing temperatures, dyeing time 45min, 60min, 75min.Orthogonal experiments is carried out range analysis, and in conjunction with monofactorial analysis, draw the Leaf of Camphortree extracting solution technology of silk broadcloth substantive dyeing is dyeing: dyeing pH value 3.00～3.50,90 ℃ of dyeing temperatures, dyeing time are 60min, bath raio 50: 1.
2.4 mordant dyeing is to the influence of silk broadcloth dying effect
Respectively with potassium aluminium sulfate, ferrous sulfate, copper sulfate, tin protochloride, zinc chloride to silk broadcloth carry out pre-mordant dyeing, with mordant dyeing and back mordant dyeing, the K/S of dyeing of real silk silk fabric, L
*, a
*, b
*, C
*And h ° of value sees Table 6.
Table 6 mordant dyeing method is to the influence of Color
Annotate: the normal dyeing technology of dyeing process for optimizing;
The mordant dyeing condition is as follows respectively:
Potassium aluminium sulfate 5g/L, 60 ℃ of mordant dyeing temperature, mordant dyeing time 15min, bath raio 50: 1.
Copper sulfate 5g/L, the mordant dyeing temperature is 70 ℃, the mordant dyeing time is 60min, bath raio 50: 1.
Ferrous sulfate 5g/L, the mordant dyeing temperature is 70 ℃, the mordant dyeing time is 45min, bath raio 50: 1.
Tin protochloride 3g/L, 60 ℃ of mordant dyeing temperature, mordant dyeing time 15min, bath raio 50: 1.
Zinc chloride 5g/L, 40 ℃ of mordant dyeing temperature, mordant dyeing time 60min, bath raio 50: 1.
As can be seen from Table 6, different mordant dyeing agent, different mordant dyeing method have different influences to the Color of dyeing of real silk silk fabric.For the potassium aluminium sulfate mordant dyeing, pre-matchmaker and back matchmaker increase the K/S value of dyeing of real silk silk fabric, and lightness descends, and with the matchmaker K/S value of dyeing of real silk silk fabric are descended, and lightness increases, mordant dyeing to ruddiness, gold-tinted, bright-colored degree and hue angle influence not quite.For the ferrous sulfate mordant dyeing, the K/S value of mordant dying silk broadcloth obviously improves, and lightness descends, wherein the back matchmaker descends more, with ruddiness, gold-tinted, bright-colored degree obviously descend, it is more wherein to descend with matchmaker and back matchmaker gold-tinted, hue angle increases and the back mordant dyeing increases at most.For the copper sulfate mordant dyeing, matchmaker and back matchmaker descend K/S increase, the lightness of dyeing of real silk silk fabric in advance, with the matchmaker decline of K/S value, the lightness of dyeing of real silk silk fabric are increased; Pre-matchmaker and the ruddiness that the dyeing of real silk silk ribbon is had with the matchmaker increase, and then the matchmaker slightly descends; Gold-tinted, bright-colored degree and hue angle that mordant dyeing has the dyeing of real silk silk ribbon slightly descend, and it is apparent in view that wherein back mordant dyeing makes that yellow degree, bright-colored degree descend, and it is more with mordant dyeing the color hue angle to be descended.For the tin protochloride mordant dyeing, back matchmaker is little to the K/S value of dyeing of real silk silk fabric, lightness, the ruddiness influence that has, but the gold-tinted that has, bright-colored degree and hue angle slightly descend; Pre-matchmaker and the K/S value of dyeing of real silk silk fabric is descended and more obvious with the matchmaker with the matchmaker, the gold-tinted that has, bright-colored degree and hue angle increase and make the hue angle increase more obvious with the matchmaker, the ruddiness decline that the dyeing of real silk silk ribbon is had with the matchmaker.
For the zinc chloride mordant dyeing, pre-matchmaker and make with the matchmaker that the K/S value of dyeing of real silk silk fabric descends, the lightness increase; It is little that back matchmaker changes the K/S value of dyeing of real silk silk fabric, and lightness descends; The ruddiness, gold-tinted and the bright-colored degree that the dyeing of real silk silk ribbon are had with the matchmaker slightly increase, and back matchmaker slightly descends, and pre-matchmaker changes not quite; Mordant dyeing descends the hue angle of dyeing of real silk silk fabric.
2.5 the dyefastness of dyeing of real silk silk fabric
Stained cloth is measured the dyefastness of dyeing of real silk silk fabric with 2.4, the results are shown in Table 7.
The colour fastness of table 7 dyeing of real silk silk fabric
As can be seen from Table 7, the different mordant dyeing agent, different mordant dyeing has different influences to the washable and crocking resistance of dyeing of real silk silk fabric, compares with mordant dying silk broadcloth not, and mordant dyeing makes the washable and crocking resistance of dyeing of real silk silk fabric that in various degree raising all be arranged.The potassium aluminium sulfate mordant dyeing, dyeing of real silk silk fabric fastness to washing and fastness to rubbing effect are not significantly improved; The ferrous sulfate mordant dyeing, dyeing of real silk silk fabric fastness to washing significantly improves, and its fastness to rubbing slightly descends, with fastness the best of mordant dyeing look silk broadcloth; Copper sulfate mordant dyeing, dyeing of real silk silk fabric fastness to washing and fastness to rubbing all slightly improve; The tin protochloride mordant dyeing, dyeing of real silk silk fabric fastness to washing is significantly improved; The zinc chloride mordant dyeing, the fastness to rubbing of dyeing of real silk silk fabric increases, and mordant dyeing best results after the fastness to washing.
3 conclusions
3.1 draw the optimization technology of Leaf of Camphortree natural dyestuff extraction by experiment be: sodium hydroxide 0.3mol/L, extract 100 ℃ of temperature, time 80min, solid-liquid ratio 1: 30 once extracts.The Leaf of Camphortree extracting solution to the optimization technology of silk broadcloth substantive dyeing is: dyeing pH value 3.00～3.50,90 ℃ of dyeing temperatures, time 60min, bath raio 50: 1.
3.2 different mordants, different mordant dyeing methods, the coloured light that obtains the dyeing of real silk silk fabric is different, ferrous sulfate mordant dying silk broadcloth changes of shade maximum wherein, potassium aluminium sulfate mordant dying silk broadcloth changes of shade minimum.
3.3 different mordants, different mordant dyeing methods has different influences to the washable and fastness to rubbing of dyeing of real silk silk fabric, and after the mordant dyeing, the washable and fastness to rubbing of dyeing of real silk silk fabric has raising in various degree.
3.4 Leaf of Camphortree extracting solution dyeing of real silk silk fabric has certain fragrant.
Above-mentioned test portion: K/S represents the surperficial color depth value of DYED FABRICS, is worth big more expression color dark more (dense); L
*Representative luminance value or brightness value are meant the Strong degree of color light and shade, are worth highly more, and the dye uptake of dyestuff is low more; a
*And b
*Represent tone, a
*For big more on the occasion of expression DYED FABRICS band ruddiness and value, the ruddiness of expression band is many more, a
*Represent DYED FABRICS band green glow for negative value, its absolute value is big more, and the green glow of expression band is many more; b
*For big more on the occasion of expression DYED FABRICS band gold-tinted and value, the gold-tinted of band is many more, b
*Represent DYED FABRICS band blue light for negative value, its absolute value is big more, and the blue light of expression band is many more; C
*The purity of representing colourity or color is the bright-coloured degree of color, is worth big more bright-coloured more; The form and aspect of h ° of representative color.
Claims (4)
1. Leaf of Camphortree dyestuff is characterized in that: be to extract the dyestuff that obtains from Leaf of Camphortree, its preparation method is: adopting the sodium hydroxide solution of 0.3mol/L is extraction agent, once extract, the temperature of extracting is 100 ℃, and the time of extraction is 80 minutes, and solid-liquid ratio is 1:30.
2. the extracting method of the described Leaf of Camphortree dyestuff of claim 1 is characterized in that: adopting the sodium hydroxide solution of 0.3mol/L is extraction agent, once extracts, and the temperature of extraction is 100 ℃, and the time of extraction is 80 minutes, and solid-liquid ratio is 1:30.
3. the described Leaf of Camphortree dyestuff of claim 1 is characterized in that in the application as the silk broadcloth dying agent: the Leaf of Camphortree dyestuff is made into the dye liquor that concentration is 10g/L, and the pH value of regulating dye liquor is 3 ~ 3.5; Silk broadcloth after wetting is dropped into dye liquor, and dyeing temperature is 90 ℃, and dyeing time is 60 minutes, and bath raio is 50:1.
4. Leaf of Camphortree dyestuff according to claim 3 is characterized in that in the application as the silk broadcloth dying agent: also carry out mordant dyeing and handle.
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| CN106192461A (en) * | 2016-07-20 | 2016-12-07 | 珠海无用文化创意有限公司 | Natural Camphor Tree Seeds is applied to the method on Nature Fibre Textile product as vegetable colour |
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