CN109826024A - A kind of colouring method of the natural pigment based on cation-modified sodolin - Google Patents
A kind of colouring method of the natural pigment based on cation-modified sodolin Download PDFInfo
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- CN109826024A CN109826024A CN201910183880.3A CN201910183880A CN109826024A CN 109826024 A CN109826024 A CN 109826024A CN 201910183880 A CN201910183880 A CN 201910183880A CN 109826024 A CN109826024 A CN 109826024A
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Abstract
A kind of colouring method of the natural pigment based on cation-modified sodolin, it is related to the colouring method of sodolin.It is to solve the problems, such as that there are tinctorial yields is low, color fastness is low when existing natural pigment is applied to Dyeing of Linen Fabric.This method: one, sodolin leaching is entered into cellulase solution and is pre-processed with cellulase solution；Two, secondary treatment is carried out to sodolin with cation-modified agent solution；Three, dye solution is prepared with natural pigment dyestuff；Four, the sodolin for completing secondary treatment is immersed in dye solution and is dyed, complete the dyeing of sodolin.The dyeing percentage of method of the invention reaches 25%~50%, and color fastness reaches 4~5 grades.Suitable for field of printing and dyeing.
Description
Technical field
The present invention relates to the colouring methods of sodolin.
Background technique
Flax fiber is extremely important raw material in entire production in light industry as a kind of natural reproducible resource.
Sodolin has good water imbibition, static electricity resistance, thermal conductivity and gas permeability, is widely used in various textile fabrics.Flax
The main composition of fiber is cellulose, and containing impurity such as more lignin and hemicellulose, due to its special structure group
At leading to primary flax fiber textile there are feels coarse, dyeability is poor, the shortcomings that easily decoloration after washing.Therefore it is promoted
Level of comfort that flax fiber is taken, the dyeability for improving sodolin and to improve fastness after its dyeing be that current flax is spun
Knit one of industry urgent problem to be solved.
In recent years, as the green and healthy idea of the public is constantly promoted, it has been found that the synthesis that textile industry largely uses
There is irremediable defects for dyestuff: toxic, carcinogenicity and environment harmfulness.Synthetic dyestuffs are substituted using natural pigment
It can solve above-mentioned problem.Vegatable tannin is that one kind is widely present in the intracorporal polyatomic phenol natural pigment of plant, and resource is rich
Richness, it is extremely stable in aqueous solution and environment friendly and pollution-free, but as natural pigment be applied to Dyeing of Linen Fabric when exist coloring
The problem that rate is low, color fastness is low, performance is unstable.
Summary of the invention
That there are tinctorial yields is low, color fastness is low when being applied to Dyeing of Linen Fabric the present invention is to solve existing natural pigment
The problem of, and a kind of colouring method of natural pigment based on cation-modified sodolin is provided.
The colouring method of natural pigment based on cation-modified sodolin of the invention, sequentially includes the following steps:
It one, is that configuration concentration is 10~20g/L's as solvent using the NaAc_HAc buffer solution that pH is 4.5~5.5
Cellulase solution；Sodolin leaching is entered in cellulase solution, bath raio is 1:(15~16), it is warming up to 45~55 DEG C
3~5h is kept, sodolin is taken out, is washed with water to neutrality, pretreatment is completed in drying；
Two, be 20g/L~40g/L by the concentration of cation modifier, the concentration of sodium hydroxide is 10g/L~15g/L, will
Cation modifier and sodium hydroxide are added to water, are uniformly mixed, obtain modifier solution；Wherein cation modifier is (3-
Chloro- 2- hydroxypropyl) trimethyl ammonium chloride (CHPTMAC)；It will complete pretreated sodolin to be immersed in modifier solution, bathe
Than for 1:(30~50), 65~75 DEG C of 50~70min of holding are warming up to, fabric is taken out, are washed with water to neutrality, drying completes two
Secondary processing；
Three, it is 20~40g/L of concentration of 10~40g/L, accelerant by the concentration of natural colouring substance, by dyestuff and promotees to contaminate
Agent is added in distilled water, stirs evenly, obtains dye solution；
Four, dye solution is warming up to 40~45 DEG C, it is molten that the sodolin for completing secondary treatment is then immersed in dyestuff
It is dyed in liquid, after dyeing, takes out sodolin, with soaping, then after being rinsed with water, the dyeing of sodolin is completed in drying.
The microstructure of flax fiber determines dyeing and finishing process engineering, and it is pre- that sodolin is first used cellulase by the present invention
Processing, is then reprocessed with CHPTMAC under alkaline condition again, and two-step method is cooperateed with glucose in flax fiber element
Ring is opened, and the active force between fiber macromolecular is weakened, and the structure between fiber macromolecular becomes loose, and fiber morphology changes
Become, surface generates den and stripping damage streak, increases the noncrystalline domain of flax fiber, to make to contaminate in subsequent dyeing course
Material is easily accessible, and improves accessibility and reactivity, achievees the purpose that improve dyeing percentage and color fastness.Method of the invention
For dyeing percentage up to 25%~50%, color fastness reaches 4~5 grades.Method of the invention can be used for field of printing and dyeing.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of sodolin before modified in embodiment 1；
Fig. 2 is the stereoscan photograph through the pretreated sodolin of step 1 in embodiment 1；
Fig. 3 is the stereoscan photograph of the sodolin in embodiment 1 after step 2 completes secondary treatment；
Fig. 4 is the energy spectrum diagram of unmodified sodolin in embodiment 1；
Fig. 5 is the energy spectrum diagram of the sodolin in embodiment 1 after step 2 completes secondary treatment；
Fig. 6 is the XRD spectra of the fabric and the sodolin after secondary treatment of unmodified flax in embodiment 1.
Specific embodiment
Specific embodiment 1: the dyeing side of the natural pigment based on cation-modified sodolin of present embodiment
Method sequentially includes the following steps:
It one, is that configuration concentration is 10~20g/L's as solvent using the NaAc_HAc buffer solution that pH is 4.5~5.5
Cellulase solution；Sodolin leaching is entered in cellulase solution, bath raio is 1:(15~16), it is warming up to 45~55 DEG C
3~5h is kept, sodolin is taken out, is washed with water to neutrality, pretreatment is completed in drying；
Two, be 20g/L~40g/L by the concentration of cation modifier, the concentration of sodium hydroxide is 10g/L~15g/L, will
Cation modifier and sodium hydroxide are added to water, are uniformly mixed, obtain modifier solution；Wherein cation modifier is (3-
Chloro- 2- hydroxypropyl) trimethyl ammonium chloride (CHPTMAC)；It will complete pretreated sodolin to be immersed in modifier solution, bathe
Than for 1:(30~50), 65~75 DEG C of 50~70min of holding are warming up to, fabric is taken out, are washed with water to neutrality, drying completes two
Secondary processing；
Three, it is 20~40g/L of concentration of 10~40g/L, accelerant by the concentration of natural colouring substance, by dyestuff and promotees to contaminate
Agent is added in distilled water, stirs evenly, obtains dye solution；
Four, dye solution is warming up to 40~45 DEG C, it is molten that the sodolin for completing secondary treatment is then immersed in dyestuff
It is dyed in liquid, after dyeing, takes out sodolin, with soaping, then after being rinsed with water, the dyeing of sodolin is completed in drying.
Specific embodiment 2: the present embodiment is different from the first embodiment in that accelerant described in step 3
For sodium chloride；It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that day described in step 4
Right colouring substance is rubber Bowl tannin or Baybery tannin；It is other the same as one or two specific embodiments.
Specific embodiment 4: being dyed in step 4 unlike one of present embodiment and specific embodiment one to three
When, bath raio is 1:(20~40)；It is other identical as one of specific embodiment one to three.
Specific embodiment 5: being dyed in step 4 unlike one of present embodiment and specific embodiment one to four
When, dye bath is warming up to 80~95 DEG C of 50~90min of holding with 2~5 DEG C/min；Other phases one of with specific embodiment one to four
Together.
Specific embodiment 6: being dyed in step 4 unlike one of present embodiment and specific embodiment one to four
When, dye bath is warming up to 90 DEG C of holding 70min with 3 DEG C/min；It is other identical as one of specific embodiment one to four.
With the following examples verifying this it is bright the utility model has the advantages that
Embodiment 1: the colouring method of the natural pigment based on cation-modified sodolin of the present embodiment, by following
Step carries out:
It one, be 4.5 using pH is NaAc_HAc buffer solution as solvent, configuration concentration is that the cellulase of 15g/L is molten
Liquid；Sodolin is immersed in cellulase solution, bath raio 1:15, is warming up to 45 DEG C of holding 3h, taken out fabric, be washed with water
It to neutrality, is dried 3 hours under conditions of temperature is 40 DEG C, completes pretreatment；
Two, be 30g/L by the concentration of cation modifier, the concentration of sodium hydroxide is 12.5g/L, by cation modifier
It is added to water with sodium hydroxide, is uniformly mixed, obtains modifier solution；Wherein cation modifier is (the chloro- 2- hydroxypropyl of 3-)
Trimethyl ammonium chloride (CHPTMAC)；It will complete pretreated sodolin to be immersed in modifier solution, bath raio 1:30, rise
Temperature is taken out fabric, is washed with water to neutrality, dry 3 hours under conditions of temperature is 40 DEG C, complete two to 70 DEG C of holding 60min
Secondary processing；
Three, it is the concentration 20g/L of 30g/L, sodium chloride by the concentration of dyestuff, dyestuff and accelerant is added in distilled water,
It stirs evenly, obtains dye solution；Wherein dyestuff is rubber Bowl tannin；
Four, dye solution is warming up to 40 DEG C, then pretreated sodolin is immersed in dye solution, bath raio
For 1:20, dye bath is warming up to 90 DEG C of holdings dyeing 70min with 3 DEG C/min, after dyeing, takes out sodolin, with soaping, then
After being rinsed with water, the dyeing of sodolin is completed in drying.
The stereoscan photograph of the unmodified sodolin of step 1 through step 1 as shown in Figure 1, complete pre- in embodiment 1
The stereoscan photograph of the sodolin of processing is as shown in Fig. 2, complete the scanning electricity of the sodolin of secondary treatment through step 2
Mirror photo is as shown in Figure 3.Can be seen that out untreated flax fiber surface from Fig. 1, Fig. 2 and Fig. 3 has fiber fines tightly
Attachment has burr, and feel is poor, and the comfort of dress is poor.After enzyme pretreatment, fiber surface is relatively smooth, fiber table
The fiber fines in face remove completely substantially, will not generate prodding and itching feeling again, improve the wearing comfort of sodolin；By secondary
The flax fiber surface of processing is with den and stripping damage streak.After pretreatment and secondary treatment, the intensive dyestuff of marshalling
Structure change has occurred in the low cellulose crystallite area of the accessibility being difficult to enter, and cellulose glucose ring is opened, and fiber divides greatly
Active force between son is weakened, and the structure between fiber macromolecular becomes loose, thus fiber morphology changes, and surface generates nest
Point and stripping damage streak, the noncrystalline domain of flax fiber increase.The surface topography of flax fiber is set to change by modification,
Den and stripping damage streak are produced, and then improves the dyeability of flax fiber.
In embodiment 1 in step 1 the energy spectrum diagram of unmodified sodolin as shown in figure 4, Elemental analysis data such as table 1
Shown, the energy spectrum diagram for completing the sodolin of secondary treatment through step 2 is led to as shown in figure 5, Elemental analysis data is as shown in table 2
The energy spectrum analysis to rear flax fiber before modified is crossed, it is found that the percentage composition of N element in modified flax fiber is 18.46%,
The percentage composition of N element is 16.30% in flax fiber before modified, and the N element content in modified flax fiber, which is higher than, to be modified
Preceding flax fiber, sodolin are handled through CHPTMAC under enzyme pretreatment and alkaline condition, and CHPTMAC forms band epoxy group
Quaternary ammonium salt cationic compound, and with cellulose macromolecule 6 on hydroxy combining, keep the crystallization of macromolecular cellulose broken
It is bad.
The Elemental analysis data of the unmodified sodolin of table 1
| Element | Wt% | At% |
| CK | 43.76 | 49.86 |
| NK | 16.68 | 16.30 |
| OK | 39.56 | 33.84 |
Table 2 completes the Elemental analysis data of the sodolin of secondary treatment through step 2
| Element t | Wt% | At At% |
| CK | 43.19 | 49.16 |
| NK | 18.91 | 18.46 |
| OK | 37.90 | 32.38 |
In embodiment 1 in step 1 the fabric of unmodified flax with through step 2 complete secondary treatment flax fabric
XRD spectra as shown in fig. 6, from fig. 6, it can be seen that flax fiber has sharp diffraction maximum, modified flax before modified
Fiber diffraction peak acuity reduces, and illustrates to destroy flax fiber when modifying agent is reacted with cellulose fibre to a certain extent
The ordered structure of middle cellulose arrangement, declines its crystallinity.This is because modifier molecules amount is small, cellulose chain can be penetrated
Gap between piece causes the hydrogen bond between chain piece to be broken, therefore crystallinity declines.It is possible thereby at inferring flax fiber by being modified
Noncrystalline domain is managed to increase.In noncrystalline domain, macromolecular arrangement is disorderly and unsystematic, there is more cavity and seam between molecule and molecule
Gap improves the accessibility of dyestuff, so that fiber has good dyeability.
Embodiment 2: the colouring method of the natural pigment based on cation-modified sodolin of the present embodiment, by following
Step carries out:
It one, be 4.5 using pH is NaAc_HAc buffer solution as solvent, configuration concentration is that the cellulase of 20g/L is molten
Liquid；Sodolin is immersed in cellulase solution, bath raio 1:15, is warming up to 45 DEG C of holding 3h, taken out fabric, be washed with water
It to neutrality, is dried 3 hours under conditions of temperature is 40 DEG C, completes pretreatment；
Two, be 40g/L by the concentration of cation modifier, the concentration of sodium hydroxide is 12.5g/L, by cation modifier
It is added to water with sodium hydroxide, is uniformly mixed, obtains modifier solution；Wherein cation modifier is (the chloro- 2- hydroxypropyl of 3-)
Trimethyl ammonium chloride (CHPTMAC)；It will complete pretreated sodolin to be immersed in modifier solution, bath raio 1:30, rise
Temperature is taken out fabric, is washed with water to neutrality, dry 3 hours under conditions of temperature is 40 DEG C, complete two to 72 DEG C of holding 70min
Secondary processing；
Three, it is the concentration 30g/L of 15g/L, accelerant by the concentration of dyestuff, dyestuff and accelerant is added in distilled water,
It stirs evenly, obtains dye solution；Wherein dyestuff is rubber Bowl tannin；Accelerant is sodium chloride；
Four, dye solution is warming up to 40 DEG C, then pretreated sodolin is immersed in dye solution, bath raio
For 1:20, dye bath is warming up to 85 DEG C of holdings dyeing 60min with 5 DEG C/min, after dyeing, takes out sodolin, with soaping, then
After being rinsed with water, the dyeing of sodolin is completed in drying.
Embodiment 3: the dyestuff in step 3 is Baybery tannin to the present embodiment unlike the first embodiment, other and implementation
Example 1 is identical.
Embodiment 4: the dyestuff in step 3 is Baybery tannin to the present embodiment as different from Example 2, other and implementation
Example 2 is identical.
The measurement that Lab value and dye-uptake are carried out to sodolin after the dyeing of Examples 1 to 4 preparation, as a result such as 3 institute of table
Show:
Sodolin carries out Lab value and dye-uptake result after the dyeing of 3 Examples 1 to 4 of table preparation
| Sample | Dyestuff | L* | a* | b* | Color difference | Dye-uptake (%) |
| Embodiment 1 | Rubber Bowl tannin | 37.58 | 7.52 | 33.79 | 70.92 | 34.87 |
| Embodiment 2 | Rubber Bowl tannin | 44.23 | 5.73 | 21.52 | 59.56 | 26.49 |
| Embodiment 3 | Baybery tannin | 50.16 | 15.47 | 24.54 | 57.24 | 49.96 |
| Embodiment 4 | Baybery tannin | 54.98 | 12.69 | 18.34 | 49.78 | 39.12 |
Fastness analysis is carried out to the dyeing sodolin of Examples 1 to 4 preparation, wherein the measurement of washing fastness is according to state
Sample is handled under the conditions of as defined in family standard GB/T14575-2009, after processing with " dyefastness fading sample card " or
" dyefastness grey scale for staining " is compared grading.Washing fastness is divided into 5 grades, and 1 grade worst, and 5 grades best.Fastness to rubbing is divided into
Dry fastness and two kinds of fastness to wet rubbing are tested enterprising in rubfastness test instrument according to standard GB/T/T14575-2009
Row, compares grading with " crock fastness staining gray scale ".Crock fastness is divided into 5 grades, and 1 grade worst, and 5 grades best.Light
Measurement be international standard AATCC Test Method 16-2004 according to american chemical textile association, with YG (B) 611-
After type III solarization weathering fastness machine illumination for 24 hours, light grade is obtained with " blue wool colorimetric card " comparison.Washing fastness
Measurement result it is as shown in table 4, the measurement result of fastness to rubbing and light is as shown in table 5.
4 washing fastness test result of table
From table 4, it can be seen that the washing fastness of the sodolin after Examples 1 to 4 dyeing all reaches industrial and wants
It asks.
The test result of 5 crock fastness of table and light
As can be seen from Table 5, the dry and wet crock fastness of the sodolin after Examples 1 to 4 dyeing belongs to light
Higher level meets industrial standard.Flax fiber dyer can be shortened to a certain extent by further relating to method of the invention
Skill process improves production efficiency.
Claims (6)
1. a kind of colouring method of the natural pigment based on cation-modified sodolin, it is characterised in that this method is by following
Step carries out:
It one, is that configuration concentration is the fiber of 10~20g/L as solvent using the NaAc_HAc buffer solution that pH is 4.5~5.5
Plain enzyme solutions；Sodolin leaching is entered in cellulase solution, bath raio is 1:(15~16), it is warming up to 45~55 DEG C of holdings
3~5h takes out sodolin, is washed with water to neutrality, pretreatment is completed in drying；
Two, be 20g/L~40g/L by the concentration of cation modifier, the concentration of sodium hydroxide is 10g/L~15g/L, by sun from
Sub- modifying agent and sodium hydroxide are added to water, are uniformly mixed, obtain modifier solution；Wherein cation modifier is (the chloro- 2- of 3-
Hydroxypropyl) trimethyl ammonium chloride；Pretreated sodolin will be completed to be immersed in modifier solution, bath raio be 1:(30~
50) 65~75 DEG C of 50~70min of holding, are warming up to, fabric is taken out, are washed with water to neutrality, secondary treatment is completed in drying；
Three, it is 20~40g/L of concentration of 10~40g/L, accelerant by the concentration of natural colouring substance, dyestuff and accelerant is added
Enter in distilled water, stir evenly, obtains dye solution；
Four, dye solution is warming up to 40~45 DEG C, then the sodolin for completing secondary treatment is immersed in dye solution
Dyeing after dyeing, takes out sodolin, and with soaping, then after being rinsed with water, the dyeing of sodolin is completed in drying.
2. a kind of colouring method of natural pigment based on cation-modified sodolin according to claim 1,
It is characterized in that accelerant described in step 3 is sodium chloride.
3. a kind of colouring method of natural pigment based on cation-modified sodolin according to claim 1 or 2,
It is characterized in that natural pigment dyestuff described in step 4 is rubber Bowl tannin or Baybery tannin.
4. a kind of colouring method of natural pigment based on cation-modified sodolin according to claim 1 or 2,
It is characterized in that bath raio is 1:(20~40 when dyeing in step 4).
5. a kind of colouring method of natural pigment based on cation-modified sodolin according to claim 1 or 2,
It is characterized in that dye bath is warming up to 80~95 DEG C of 50~90min of holding with 2~5 DEG C/min when dyeing in step 4.
6. a kind of colouring method of natural pigment based on cation-modified sodolin according to claim 1 or 2,
It is characterized in that dye bath is warming up to 90 DEG C of holding 70min with 3 DEG C/min when dyeing in step 4.
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| CN110629571A (en) * | 2019-08-26 | 2019-12-31 | 徐州锦业纺织科技有限公司 | Cleaning and dyeing process of rayon yarn |
| CN111705510A (en) * | 2020-06-11 | 2020-09-25 | 台州恒彩纺织科技有限公司 | Modified cellulose fiber and dyeing pretreatment method of knitted fabric woven by using same |
| CN114606783A (en) * | 2022-03-18 | 2022-06-10 | 德州学院 | Process for dyeing hemp by using dark plum |
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Application publication date: 20190531 |