CN109371660A - A kind of flame-retardant silk and its preparation method and application - Google Patents
A kind of flame-retardant silk and its preparation method and application Download PDFInfo
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- CN109371660A CN109371660A CN201811270759.6A CN201811270759A CN109371660A CN 109371660 A CN109371660 A CN 109371660A CN 201811270759 A CN201811270759 A CN 201811270759A CN 109371660 A CN109371660 A CN 109371660A
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- silk
- flame
- retardant
- tannic acid
- retardant silk
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Classifications
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
-
- 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
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
-
- 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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a kind of methods for preparing flame-retardant silk, comprising the following steps: immerses silk in the tannic acid solution that pH value is 3-4, is warming up to 80-90 DEG C of progress isothermal holding；Silk after treatment is immersed into the metal salt solution of 2-6g/L, and is warming up to 50-70 DEG C and is handled, obtains flame-retardant silk.Method of the invention assigns the good flame retardant property of silk in the case where not adding containing traditional nitrogen, phosphorus, halogen fire retardant, and can be avoided due to using conventional flame retardant bring in flame-retardant silk production and use process and and flame-retardant silk by nitrogen, phosphorus, halogen bring problem of environmental pollution after discarded.This method has the advantages that environmentally friendly, efficient, simple and easy.
Description
Technical field
The present invention relates to textile finishing technical fields, and in particular to a kind of method for preparing flame-retardant silk and using should
The flame-retardant silk of method preparation.
Background technique
Silk is one of most common natural protein fibre, because of its soft natural gloss, exclusive scrooping feel, good
Health and comfort and be loved by consumers.Silk textile is usually used in the high-grade clothes and ornament of production, silk
The daily clothes of ornament and part have higher requirement to flame retardant property.Silk cannot pass through as natural protein fibre
With the method for fire retardant co-blended spinning it is carried out flame-retardant modified, can only be processed by the final finishing of printing and dyeing and reach fire-retardant mesh
's.Good flame-proof treatment, other than it can provide flame retarding function, it is necessary to which nontoxicity, smoke is few, is resistant to a degree of washing
And dry-cleaning, and the original fine quality of silk is not interfered.
The flame-proof treatment of silk, in early days using stannic acid or boric acid-borax infusion process processing, although good flame retardation effect
Preferably, but intolerant to washing.Halogen flame was once applied to the flame-proof treatment of silk, but after it is disabled because of toxicity problem.Cotton
It was also once applied to the flame-proof treatment of silk with P-N type fire retardant, and the preferable flame retardant property of silk and water-wash resistance can be assigned
Can, however the disadvantage is that processing charges is high, technics comparing is complicated, and gained silk feel is hardened and yellowing, and exists free
Form aldehyde release problem.Currently, being widely used in " Zirpro " technique of wool flame-proof treatment, also there is certain answer on silk
With, which carries out flame-proof treatment to silk by metal complexes such as titanium, zirconiums, the flame retardant property of silk can be effectively promoted,
But the species of metal ion being applicable in is less, and price is relatively expensive, and the washability of flame retarding function is not good enough yet.Since P elements exist
It can cause eutrophication in water body, halogen fire retardant can discharge toxic gas in use to endanger environment and people
Body.Therefore, pay attention to environmental problem, exploitation green is friendly, economic and practical, the simple flame-retarded technology of technique for applying is that this field needs
It solves the problems, such as.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method is simple, good flame retardation effect it is a kind of prepare it is fire-retardant
The method of silk.
In order to solve the above technical problem, the present invention provides scheme be: a method of prepare flame-retardant silk, including with
Lower step:
S1, silk is immersed in the tannic acid solution that pH value is 3-4, is warming up to 80-90 DEG C of progress isothermal holding；
S2, will by step S1, treated that silk is immersed into the metal salt solution of 2-6g/L, and be warming up to 50-70 DEG C
It is handled, obtains flame-retardant silk.
Tannic acid can adsorb on silk from plant tissue containing carboxyl under mildly acidic conditions, and and silkworm
Silk occurs ionic bond and combines；After tannic acid adsorbs on silk, then through metal salt treatment, metal ion can with inhaled on silk
Complexing occurs for attached tannic acid and silk fiber, and then changes thermal degradation process when silk burns and play fire-retardant
Effect.Tannic acid and the silk of metal salt Combined Treatment have good flame retardant property and splendid washability.
Further, the time of isothermal holding is 45-75min in the step S1.
Further, the processing time in the step S2 at 50-70 DEG C is 20-40min.
Further, the dosage of tannic acid is the 10-30% to the relative weight of silk in the step S1.
Further, the metal salt is one of ferrous sulfate, ferric sulfate, titanium sulfate or calcium sulfate or more
Kind.
The present invention further provides a kind of flame-retardant silk being prepared according to the above method.
The present invention further provides a kind of application of the flame-retardant silk being prepared according to the above method in terms of weaving.
Beneficial effects of the present invention:
1, the tannic acid that the present invention uses is a kind of environmental-friendly native compound from plant tissue.
2, the flame-retardant finishing method that the present invention uses is a kind of completely new flame resistant method and technology, the operation of flame-proof treatment process
Simply, effect is obvious, and metal ion used is easy to get, is cheap.
3, in the case where not adding traditional nitrogen, phosphorus, halogen fire retardant, it can assign silk good flame retardant property,
And the durability of flame retarding function is splendid, and can be avoided bring due to using conventional flame retardant and produce and make in flame-retardant silk
With in the process and and flame-retardant silk by nitrogen, phosphorus, halogen bring problem of environmental pollution after discarded.This method has ring
It protects, efficient, simple and easy advantage.
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.
In following embodiment of the present invention, the flame retardant property of silk fabric is according to GB/T 5454-1997 " textile combustion
Oxygen index method can be tested " and GB/T 5455-2014 " textile combustion performance vertical direction char length glows and after flame time
Measurement " be measured.Referring to GB/T 3921-2008, " textile color stability tests resistance to soap to the method for washing of flame-retardant silk fabric
Wash color fastness " standard carries out, and using silk wool fabric special purpose detergent 2g/L, bath raio 1:50, washing 30min is primary at 40 DEG C.
Repetition is washed to required washing times.
Embodiment 1
It is S1, the tannic acid of 20% (to the relative weight of silk) is soluble in water, 10min is stirred under room temperature, uses lemon
PH value is adjusted to 4 by acid/disodium hydrogen phosphate buffer solution；Silk is immersed in above-mentioned tannic acid solution, is warming up to 90 DEG C, heat preservation
45min is handled, silk is taken out, is cleaned, drying.
S2, above-mentioned tannic acid treated silk is immersed in the ferrous sulfate or ferrum sulfuricum oxydatum solutum of 2g/L, at 70 DEG C
20min is managed, cleans, drying, obtains the silk of the flame retarding function of durability.
The limit oxygen index of silk through tannic acid and ferrous sulfate Combined Treatment is 27.5%, and char length is only
11.0cm；The limit oxygen index of silk through tannic acid and ferric sulfate Combined Treatment is 27.6%, and char length is only 11.1cm.
Silk through tannic acid and ferrous sulfate or ferric sulfate Combined Treatment is all satisfied in China GB/T17591-2006 " flame-retardant textile "
B1 grades of flame retardant properties require (char length is less than 15cm).
Embodiment 2
It is S1, the tannic acid of 20% (to the relative weight of silk) is soluble in water, 10min is stirred under room temperature, uses lemon
The pH value of above-mentioned solution is adjusted to 3 by acid/disodium hydrogen phosphate buffer solution；Silk is immersed in above-mentioned tannic acid solution, is heated up
To 80 DEG C, isothermal holding 75min, silk is taken out, is cleaned, drying.
S2, above-mentioned tannic acid treated silk is immersed in the calcium sulfate or titanium sulfate solution of 6g/L, is handled in 50 DEG C
40min cleans, drying, obtains the silk of the flame retarding function of durability.
The limit oxygen index of silk through tannic acid and calcium sulfate Combined Treatment is 27.5%, and char length is only
12.3cm；The limit oxygen index of silk through tannic acid and titanium sulfate Combined Treatment is 28.5%, and char length is only 10.0cm.
Silk through tannic acid and calcium sulfate or titanium sulfate Combined Treatment is all satisfied B1 in China GB/T17591-2006 " flame-retardant textile "
Grade flame retardant property requirement.
Embodiment 3
It is S1, respectively that 10%, 20% and 30% (to the relative weight of silk) tannic acid is soluble in water, it is stirred under room temperature
The pH value of above-mentioned solution is adjusted to 3 using citric acid/disodium hydrogen phosphate buffer solution by 10min；Silk is immersed respectively above-mentioned
In tannic acid solution, 90 DEG C, isothermal holding 60min are warming up to, takes out silk, is cleaned, drying.
S2, above-mentioned tannic acid treated silk is immersed in the ferrous sulfate solution of 2g/L, in 60 DEG C of processing 30min,
It cleans, drying, obtains the silk of the flame retarding function of durability.
As comparative example, ferrous sulfate is used alone and handles silk: silk fabric is dipped in the ferrous sulfate solution of 2g/L
In in 70 DEG C of processing 30min；Tannic acid is used alone and handles silk: silk fabric is dipped in 20% (to the relative weight of silk)
In 90 DEG C of processing 60min in tannic acid solution.
Flame retardant property test is carried out to untreated and processing silk fabric, the results are shown in Table 1.
The flame retardant property of 1 silk fabric of table
Table 1 shows: the limit oxygen index of the silk individually handled with ferrous sulfate is 25.1%, in vertical burn test
Completely burned, char length 30.0cm；The limit oxygen index of the silk individually handled with tannic acid is 26.1%, is vertically being fired
Char length is 19.5cm when burning；Individually China GB/T is not able to satisfy with the silk that ferrous sulfate or tannic acid are handled
B1 grades of flame retardant property requirements in 17591-2006 " flame-retardant textile ".Through 10%, 20% and 30% tannic acid solution and 2g/L sulfuric acid
The limit oxygen index of the silk of ferrous Combined Treatment is 26.9% to 27.9%, and in vertical combustion, char length is on the left side 11cm
The right side is all satisfied B1 grades of flame retardant property requirements in China GB/T 17591-2006 " flame-retardant textile ".
Embodiment 4
Flame retardant treatment is carried out to silk fabric according to 1 the method for embodiment, the silk of obtained flame-retardant function is carried out resistance to
The test of washing property, the results are shown in Table 2.
The washability of 2 silk fabric flame retardant property of table
Table 2 shows that after washing is repeated several times, the limit oxygen index of flame-retardant silk changes very little, and damages in vertical combustion
The flame retardant effect for ruining length still less than 15cm, explanation the method for the present invention silk prepared has splendid washability or washing
Durability.
Above embodiments explanation, using the method for preparing flame-retardant silk in the present invention, can assign silk good anti-flammability
Can, and the washing durability of flame retarding function is splendid.This method has the advantages that environmentally friendly, efficient, simple and easy.
It is good that method of the invention assigns silk in the case where not adding containing traditional nitrogen, phosphorus, halogen fire retardant
Flame retardant property, and can be avoided due to using conventional flame retardant bring in flame-retardant silk production and use process and
And flame-retardant silk is by discarded rear nitrogen, phosphorus, halogen bring problem of environmental pollution.This method has environmentally friendly, efficient, simple easy
Capable advantage.
Tannic acid can adsorb on silk from plant tissue containing carboxyl under mildly acidic conditions, and and silkworm
Silk occurs ionic bond and combines；After tannic acid adsorbs on silk, then through metal salt treatment, metal ion can with inhaled on silk
Complexing occurs for attached tannic acid and silk fiber, and then changes thermal degradation process when silk burns and play fire-retardant
Effect.Tannic acid and the silk of metal salt Combined Treatment have good flame retardant property and splendid washability.
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. a kind of method for preparing flame-retardant silk, which comprises the following steps:
S1, silk is immersed in the tannic acid solution that pH value is 3-4, is warming up to 80-90 DEG C of progress isothermal holding；
S2, will by step S1, treated that silk is immersed into the metal salt solution of 2-6g/L, and be warming up to 50-70 DEG C of progress
Processing, obtains flame-retardant silk.
2. as described in claim 1 prepare flame-retardant silk method, which is characterized in that in the step S1 isothermal holding when
Between be 45-75min.
3. the method for preparing flame-retardant silk as described in claim 1, which is characterized in that in the step S2 at 50-70 DEG C
The processing time be 20-40min.
4. the method for preparing flame-retardant silk as described in claim 1, which is characterized in that in the step S1, the use of tannic acid
Amount is the 10-30% to the relative weight of silk.
5. as described in claim 1 prepare flame-retardant silk method, which is characterized in that the metal salt be ferrous sulfate,
One of ferric sulfate, titanium sulfate or calcium sulfate are a variety of.
6. the flame-retardant silk that one kind is prepared to any one of 5 according to claim 1.
7. application of the flame-retardant silk that one kind is prepared to any one of 5 according to claim 1 in weaving.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811270759.6A CN109371660B (en) | 2018-10-29 | 2018-10-29 | Flame-retardant silk and preparation method and application thereof |
| PCT/CN2018/113686 WO2020087499A1 (en) | 2018-10-29 | 2018-11-02 | Flame retardant silk, preparation method therefor and use thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811270759.6A CN109371660B (en) | 2018-10-29 | 2018-10-29 | Flame-retardant silk and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN109371660A true CN109371660A (en) | 2019-02-22 |
| CN109371660B CN109371660B (en) | 2021-05-28 |
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| CN201811270759.6A Active CN109371660B (en) | 2018-10-29 | 2018-10-29 | Flame-retardant silk and preparation method and application thereof |
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| WO (1) | WO2020087499A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109371670A (en) * | 2018-10-29 | 2019-02-22 | 南通纺织丝绸产业技术研究院 | Flame-retardant silk and its preparation method and application |
| 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 |
| CN109837750A (en) * | 2019-03-06 | 2019-06-04 | 苏州大学 | Silk durable flame-retardant method for sorting and flame-retardant silk based on casein phosphopeptide |
| CN110172823A (en) * | 2019-06-27 | 2019-08-27 | 四川大学 | A kind of preparation method of formaldehydeless water-fastness flame-retardant textile |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109371670A (en) * | 2018-10-29 | 2019-02-22 | 南通纺织丝绸产业技术研究院 | Flame-retardant silk and its preparation method and application |
| 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 |
| CN109837750A (en) * | 2019-03-06 | 2019-06-04 | 苏州大学 | Silk durable flame-retardant method for sorting and flame-retardant silk based on casein phosphopeptide |
| CN109837750B (en) * | 2019-03-06 | 2021-05-18 | 苏州大学 | Casein phosphopeptide-based silk durability flame-retardant finishing method and flame-retardant silk |
| CN110172823A (en) * | 2019-06-27 | 2019-08-27 | 四川大学 | A kind of preparation method of formaldehydeless water-fastness flame-retardant textile |
| CN110172823B (en) * | 2019-06-27 | 2020-10-30 | 四川大学 | Preparation method of formaldehyde-free washable flame-retardant fabric |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2020087499A1 (en) | 2020-05-07 |
| CN109371660B (en) | 2021-05-28 |
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