CN109371670A - Flame-retardant silk and its preparation method and application - Google Patents
Flame-retardant silk and its preparation method and application Download PDFInfo
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- CN109371670A CN109371670A CN201811270793.3A CN201811270793A CN109371670A CN 109371670 A CN109371670 A CN 109371670A CN 201811270793 A CN201811270793 A CN 201811270793A CN 109371670 A CN109371670 A CN 109371670A
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- silk
- flame
- retardant
- dye yam
- polyporpyleneimine
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Abstract
The invention discloses a kind of methods for preparing flame-retardant silk, comprising the following steps: the condensed tannin in the dye yam extracting solution is adsorbed on silk fabric using dipping absorption method, obtains the modified silk fabric of dye yam extract by preparation dye yam extracting solution；Under the conditions of weakly alkaline, dipping absorption method is recycled to be adsorbed in polyporpyleneimine dendrimer through obtaining flame-retardant silk on the modified silk fabric of dye yam extract.Cross-linking reaction of the present invention using the condensed tannin and polyporpyleneimine dendrimer in dye yam extract on silk fabric under weak basic condition, the flame retardant property for effectively promoting silk fabric has the flame retarding function of good durability with the silk fabric that the method for the present invention arranges.
Description
Technical field
The present invention relates to textile finishing technical fields, and in particular to a kind of method, fire-retardant for improving silk inflaming retarding performance
Silk and its application.
Background technique
The fire for having nearly half in the world is drawn as caused by the burning of textile, and by textile and upholstery
The fire fatality accident risen ranks first.Silk belongs to natural protein fibre, smooth, soft glossy ventilative with moisture absorption, soft,
The features such as graceful magnificent, comfortable and easy to wear, thus it is deeply welcomed by the people and like.Silk fiber is often widely used for making high-grade bed
Upper textile, indoor decorative fabric, carpet, curtain, wall paper and textile art product etc., these silk products have certain resistance
Combustion requires.Although silk, compared with cellulose fibre, itself has certain anti-flammability, its limit oxygen index is generally only
It is 23% or so, the standard of flame retardant textiles is also far not achieved, it is also difficult to it is growing to flame-retardant silk product meets people
Consumption demand.In order to improve the flame retardant property of silk product, need to carry out flame-proof treatment to it.
Fire retardant applied to protein fibre (mainly silk and wool) product is broadly divided into inorganic fire retardants and has
Machine fire retardant two major classes.Commercialized inorganic fire retardants is mainly the metallic compound of zirconium and titanium, is usually applied to the resistance of wool
Combustion arranges, and it is not good enough to be applied to its washing durability when silk.Organic fire-retardant almost can be suitably used for the fire-retardant whole of all textiles
Reason, occupy the main market share, have used include with organic fire-retardant currently in use bromine, chlorine, phosphorus and nitrogen chemical combination
Object.Although many commercialized organic fire-retardants can impart silk inflaming retarding function, wherein being much not meet environmental protection to want
It asks, it is even toxic.For example, halogen compounds can generate a large amount of toxic gas in combustion, and exists and hold
A series of serious problems such as long property, bioconcentration and environmental toxicity, thus it is disabled in textile industry.Organic phosphorus resistance
Combustion agent has been widely used as the substitute of halogen flame.However, the fire-retardant spinning arranged using organophosphorous fire retardant
Fabric using and washing process in, due to containing phosphorus series compound in the waste liquid of discharge, will lead to the eutrophication of water body, and
And methylol contained by many phosphorus flame retardants can cause Form aldehyde release problem.It is at present industrially still using organic phosphorus fire-retardant
Agent, zirconium and titanium metal compound carry out flame-proof treatment to silk product.For to fire retardant harm and environment sustainable development
Understanding, research and development ecological, environmental protective, efficient new flame retardant have become fire retardant and its fire-retardant whole to substitute traditional flame-retardant compound
The developing direction of reason technology.
Chinese invention patent CN201710161634.9, which is disclosed, a kind of carries out dyeing and finishing processing to protein fibre with phytic acid
Method, dyeing accelerant and the antiflaming finishing agent of environment-friendly type, handled protein are used as using natural products phytic acid simultaneously
Fiber has good flame retardant property, and (limit oxygen index is up to 30%, and char length when vertical combustion is less than 15cm, is able to satisfy
B1 grades of flame retardant property requirements in China's " flame-retardant decorative fabric "), but individually using the resistance of the protein fibre product of phytic acid processing
Fire washing durability not good enough (Xibiao Zhang, Xian-You Zhou, the Xian-Wei Cheng, Ren-Cheng of function
Tang.Phytic acid as an eco-friendly flame retardant for silk/wool blend:A
comparative study with fluorotitanate and fluorozirconate.Journal of Cleaner
Production,2018,198:1044-1052).Chinese invention patent 201710568421.8 is disclosed using dye yam flooding
The method for taking object, citric acid, sodium citrate, sodium formate mixed liquor to carry out durable flame-retardant arrangement to silk fabric, it is mixed using this
It closes liquid to impregnate, then after baking through squezzing, drying, high temperature, wash, dry, obtains durable flame-retardant silk fabric, flame-retardant silk is knitted
The limit oxygen index of object can reach 27~28%, and char length is less than 15cm when vertical combustion, and after 20 repeated washings,
Char length is still less than 15cm when the limit oxygen index of flame-retardant silk fabric remains to reach 27~28%, vertical combustion；With it is not whole
Reason silk fabric is compared, and the limit oxygen index promotion amplitude of flame-retardant silk fabric is still limited, cannot reach 30%.The above problem is
The problem of this field urgent need to resolve.
Summary of the invention
Combined the technical problem to be solved in the present invention is to provide a kind of using dye yam extract and polyporpyleneimine dendrimer
The method that processing improves a kind of raising silk inflaming retarding performance of silk fabric flame retardant property.
In order to solve the above technical problem, the present invention provides scheme be: the method for preparing flame-retardant silk, feature exist
In, comprising the following steps:
S1, silk is immersed in the dye yam extracting solution, is heated to 75-90 DEG C and is handled, is obtained through condensed tannin
Modified silk fabric；
S2, the silk fabric modified through condensed tannin is immersed in pH value as 8-9.5, concentration is the poly- of 5-15g/L
In propyleneimine tree solution, it is heated to 55-70 DEG C and is handled, obtain flame-retardant silk.
The application using in dye yam extract condensed tannin and polyporpyleneimine dendrimer on silk fabric in weak base
Property under the conditions of cross-linking reaction, assign the good durability of silk fabric flame retarding function.
Further, the step S1 further includes preparing the dye yam extracting solution, comprising the following steps: by dye yam stem tuber
It is placed in water mashing by weight for 15/100-30/100, the pH value of slurries is adjusted to 8, is heated to 85-95 DEG C of processing 50-
Dye yam extracting solution is obtained by filtration in 80min.
Further, the time heated in the step S1 is 70-120min.
Further, the time of the heat treatment is 30-40min in the step S2.
Further, polyporpyleneimine dendrimer used is two generation polyporpyleneimine dendrimers or three generations's polypropyleneimine
Tree.
Further, polyporpyleneimine dendrimer used is two generation polyporpyleneimine dendrimers or three generations's polypropyleneimine
Tree.
The application further provides a kind of flame-retardant silk prepared by the above method.
The application further provides the application by above-mentioned flame-retardant silk in weaving.
Beneficial effects of the present invention: the dye yam extract that the present invention uses is safe and non-toxic, polyporpyleneimine dendrimer reaction
Active site is more, and the condensed tannin in dye yam extract can be quickly condensed with polyporpyleneimine dendrimer under weak basic condition
Cross-linking reaction, cross-linking products can occur good combination with silk fiber, ensure that the washing durability of flame retarding function；Condensation is single
Rather with the cross-linking products of polyporpyleneimine dendrimer with good high-temperature stability and at carbon ability, so that silk fabric is firing
There is stronger char forming ability when burning；Present invention process is simple, operation is convenient, and the silk fabric flame retardant effect arranged is excellent,
And durability is good.
Specific embodiment
The present invention is further explained in the light of specific embodiments, so that those skilled in the art can be preferably
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
S1, it prepares dye yam extracting solution and silk fabric is modified using dye yam extract:
Dye yam stem tuber is cleaned, peeling, chopping.The dye yam stem tuber of 150g chopping is weighed, 500mL water is added, is mechanically pulverized
Mashing adjusts slurry pH value to 8 with soda ash, is heated to 85 DEG C, impregnates 80min, be then allowed to stand, cool down, filter；In filtrate,
It is diluted with water, stirs evenly, and be settled to 1L to get dye yam extracting solution.Through the above steps, the tannin in dye yam can be extracted
Condensation is that tannin condensation is dissolved in water.
The amount of above-mentioned dye yam extracting solution and silk is configured according to bath raio 1:50.Silk is immersed in dye yam extracting solution, from
30 DEG C start to process, and are gradually heated to 90 DEG C with the heating rate of 2 DEG C/min, isothermal holding 70min.After immersion treatment, take out
Silk after washing, obtains the silk fabric modified through dye yam extract.
S2, it is handled using the polyporpyleneimine dendrimer silk fabric modified to dye yam extract:
Configuration concentration is three generations's polyporpyleneimine dendrimer (molecular weight 1687g/mol) solution of 5g/L, with acetic acid and
The solution ph is adjusted to 9.5 by soda ash, obtains polyporpyleneimine dendrimer solution.
Silk and polyporpyleneimine dendrimer solution are configured according to bath raio 1:50.The modified silk fabric of dye yam is immersed
It in polyporpyleneimine dendrimer solution, is started to process from 30 DEG C, is gradually heated to 55 DEG C with the heating rate of 2 DEG C/min, heat preservation
Handle 40min.It is disposed, takes out silk, squezzing, 80 DEG C of drying obtain flame-retardant silk fabric.
Embodiment 2
S1, dye yam stem tuber is cleaned, peeling, chopping.The dye yam stem tuber of 75g chopping is weighed, 500mL water, mechanical powder is added
Broken mashing adjusts slurry pH value to 8 with soda ash, is heated to 95 DEG C, impregnates 50min, be then allowed to stand, cool down, filter；In filtrate
In, it is diluted with water, stirs evenly, and be settled to 1L to get dye yam extracting solution.Above-mentioned dye yam extracting solution is configured according to bath raio 1:50
With the amount of silk.Silk is immersed in dye yam extracting solution, is started to process from 30 DEG C, is gradually risen with the heating rate of 2 DEG C/min
Temperature is to 75 DEG C, isothermal holding 120min.After immersion treatment, silk is taken out, after washing, obtains the silk modified through dye yam extract
Fabric.
S2, two generation polyporpyleneimine dendrimer (molecular weight 777g/mol) solution that configuration concentration is 10g/L, use acetic acid
The solution ph is adjusted to 8 with soda ash, obtains polyporpyleneimine dendrimer solution.Silk and poly- third is configured according to bath raio 1:50
Alkene imines tree solution.The modified silk fabric of dye yam is immersed in polyporpyleneimine dendrimer solution, 30 DEG C of beginnings
Reason, is gradually heated to 70 DEG C with the heating rate of 2 DEG C/min, isothermal holding 30min.It is disposed, takes out silk, squezzing, 80
DEG C drying, obtain flame-retardant silk fabric.
Embodiment 3
S1, dye yam stem tuber is cleaned, peeling, chopping.The dye yam stem tuber of 125g chopping is weighed, 500mL water, mechanical powder is added
Slurry pH value is adjusted to 8 with soda ash by broken mashing, is heated to 90 DEG C, is impregnated 65min, is then allowed to stand, cools down, filters；In filtrate
In, it is diluted with water, stirs evenly, and be settled to 1L to get dye yam extracting solution.Silk is configured according to bath raio 1:50 and polypropylene is sub-
Amine tree solution.Silk is immersed in dye yam extracting solution, 30 DEG C start to process, and are gradually risen with the heating rate of 2 DEG C/min
Temperature is to 85 DEG C, isothermal holding 90min.After immersion treatment, silk is taken out, after washing, obtains the silk modified through dye yam extract
Fabric.
S2, two generation polyporpyleneimine dendrimer (molecular weight 777g/mol) solution for configuring 15g/L, with acetic acid and soda ash
Adjusting the solution ph is 8.5, obtains polyporpyleneimine dendrimer solution.Polyporpyleneimine dendrimer is configured according to bath raio 1:50
The amount of solution and silk.The modified silk fabric of dye yam is immersed in polyporpyleneimine dendrimer solution, 30 DEG C start to process,
60 DEG C are gradually heated to the heating rate of 2 DEG C/min, isothermal holding 30min.It is disposed, takes out silk, squezzing, 80 DEG C of bakings
It is dry, obtain flame-retardant silk fabric.
Flame retardant property is carried out to flame-retardant silk fabric obtained in above-described embodiment 1 to embodiment 3 and wash durability is surveyed
Examination.
Wherein, flame retardant property limit oxygen index and char length evaluation when vertical combustion；The limit oxygen index of fabric
Char length by GB/T 5454-1997 " textile combustion performance test oxygen index method " standard test, when fabric vertical combustion
By GB/T 5455-2014 " measurement that textile combustion performance vertical direction char length glows with after flame time " standard test；
The combustibility of fabric is according to GB/T 17591-2006 " flame-retardant textile " standard rating.The method for washing of flame-retardant textile is referring to GB/
T 3921-2008 " textile color stability test fastness to soaping " standard carries out, using detergent for silk and wool 2g/L, bath raio 1:
Washing 30min is primary at 50,40 DEG C, and repetition is washed to required washing times.
For the ease of comparing, the application is additionally provided with following control sample；
Control sample 1: untreated silk fabric is used.
Control sample 2: individually with the silk fabric of 70 DEG C of the two generation polyporpyleneimine dendrimers processing 30min of 10g/L.
Control sample 3: the silk fabric individually handled with dye yam extract, it is specific for using in embodiment 1 merely through
Step S1 treated silk fabric.
Final testing result is as shown in table 1.
The flame retardant property of 1 silk fabric of table
As can be seen from Table 1, the limit oxygen index of the silk fabric without any processing is 24.5%, in vertical combustion mistake
Completely burned in journey, char length 30cm belong to not fire-retardant fabric.The silk individually handled with polyporpyleneimine dendrimer
Fabric, limit oxygen index are improved to some extent, but are also completely burned in vertical combustion, and char length 30cm belongs to
In not fire-retardant fabric.The limit oxygen index of the silk fabric individually handled with dye yam extract is 27.0%, when vertical combustion
Char length be 12.5cm, required although also meeting in China " flame-retardant decorative fabric " B1 grade flame retardant properties, limit oxygen
Index is still relatively low.And the limit oxygen index of the silk fabric through dye yam extract and polyporpyleneimine dendrimer Combined Treatment is up to
30.6-30.8%, char length when vertical combustion are 9.5-11.0cm, are all satisfied in China " flame-retardant decorative fabric " and hinder for B1 grade
Performance requirement is fired, and limit oxygen index is higher, there is better flame resistance；In addition, even if through 20 times repeated washing after,
Char length of the limit oxygen index still at 30% or more, vertical combustion is still less than 11cm, and being still able to satisfy China, " flame-retardant decorative is knitted
Object " in the requirement of B1 grades of flame retardant properties, the washing of the flame retarding function of flame-retardant silk fabric prepared by explanation the method for the present invention is durable
Property is fine.
The above case study on implementation illustrates have using dye yam extract and the silk fabric of polyporpyleneimine dendrimer Combined Treatment
There is the flame retarding function of good durability.
The principle of the application is: using dipping absorption method, the condensed tannin in dye yam extract being made to be adsorbed in silk fabric
On, recycle dipping absorption method to be adsorbed in polyporpyleneimine dendrimer on silk fabric, in certain temperature and weak basic condition
Under, condensation cross-linking reaction occurs on silk fabric for condensed tannin and polyporpyleneimine dendrimer, is insoluble in water to be formed
3 D stereo reticular structure.The presence of this cross-linked structure, so that silk fabric has stronger char forming ability, institute in burning
At carbon play the role of it is heat-insulated, oxygen-impermeable, to improve the flame retardant property of silk fabric.
The dye yam extract that the present invention uses is safe and non-toxic, and polyporpyleneimine dendrimer reaction active sites are more, and dye yam is extracted
Condensed tannin in object can quickly occur condensation cross-linking with polyporpyleneimine dendrimer under weak basic condition and react, cross-linking products
Good combination can occur with silk fiber, ensure that the washing durability of flame retarding function；Condensed tannin and polypropyleneimine tree
The cross-linking products of shape object have good high-temperature stability and at carbon abilities so that silk fabric have in burning it is stronger at
Charcoal ability；Present invention process is simple, operation is convenient, and the silk fabric flame retardant effect arranged is excellent, and durability is good, in addition also
It is able to achieve the one-step method processing of dyeing and flame-proof treatment.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (7)
1. the method for preparing flame-retardant silk, which comprises the following steps:
S1, silk is immersed in the dye yam extracting solution, is heated to 75-90 DEG C and is handled, obtained modified through condensed tannin
Silk fabric；
S2, the silk fabric modified through condensed tannin is immersed in pH value as 8-9.5, concentration is the polypropylene of 5-15g/L
In imines tree solution, it is heated to 55-70 DEG C and is handled, obtain flame-retardant silk.
2. the method for preparing flame-retardant silk as described in claim 1, which is characterized in that the step S1 further includes described in preparation
Dye yam extracting solution, comprising the following steps: by dye yam stem tuber be by weight that 15/100-30/100 is placed in water mashing, by slurries
PH value be adjusted to 8, be heated to 85-95 DEG C of processing 50-80min, dye yam extracting solution be obtained by filtration.
3. as described in claim 1 prepare flame-retardant silk method, which is characterized in that heat in the step S1 when
Between be 70-120min.
4. the method for preparing flame-retardant silk as described in claim 1, which is characterized in that in the step S2, at the heating
The time of reason is 30-40min.
5. the method for preparing flame-retardant silk as described in claim 1, which is characterized in that polyporpyleneimine dendrimer used is two
For polyporpyleneimine dendrimer or three generations's polyporpyleneimine dendrimer.
6. according to claim 1 to flame-retardant silk prepared by any one of 5.
7. application of the flame-retardant silk as claimed in claim 6 in weaving.
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| CN109457470A (en) * | 2018-11-16 | 2019-03-12 | 南通纺织丝绸产业技术研究院 | The flame-retardant silk and its preparation method and application prepared using flavones and metal salt |
| CN114657779A (en) * | 2022-04-06 | 2022-06-24 | 苏州大学 | Durable intumescent flame-retardant protein fiber product and preparation method thereof |
| CN114657779B (en) * | 2022-04-06 | 2022-12-30 | 苏州大学 | Durable intumescent flame-retardant protein fiber product and preparation method thereof |
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