CN110054648A - A kind of preparation method of cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant - Google Patents
A kind of preparation method of cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant Download PDFInfo
- Publication number
- CN110054648A CN110054648A CN201910450001.9A CN201910450001A CN110054648A CN 110054648 A CN110054648 A CN 110054648A CN 201910450001 A CN201910450001 A CN 201910450001A CN 110054648 A CN110054648 A CN 110054648A
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- CN
- China
- Prior art keywords
- flame retardant
- nitrogen
- response type
- necked flask
- cotton
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6515—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having three nitrogen atoms as the only ring hetero atoms
- C07F9/6521—Six-membered rings
-
- 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
- D06M13/322—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 nitrogen
- D06M13/44—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 nitrogen containing nitrogen and phosphorus
- D06M13/447—Phosphonates or phosphinates containing nitrogen atoms
-
- 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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- 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 present invention relates to a kind of cotton preparation methods of response type phosphorus-nitrogen-sulphur synergistic flame retardant, dichloro s-triazine base sodium sulfanilate salt is added in three-necked flask, pour into suitable distillation water as solvent, after mixing evenly, three-necked flask is fixed in the tepidarium of heat-collecting magnetic stirring device with iron stand, then methylol dimethylphosphite aqueous solution is added dropwise in above-mentioned three-necked flask, 4 h of reaction are stirred continuously under the conditions of certain temperature and pH, product is after condensation drying further isolates and purifies, obtaining product is response type phosphorus-nitrogen-sulphur synergistic flame retardant of the invention, it can be applied to the finishing functions of pure cotton fabric, the excellent flame retardant property of providing cotton fabric, it is a kind of novel function additive.
Description
Technical field
The present invention relates to a kind of cotton preparation methods of response type phosphorus-nitrogen-sulphur synergistic flame retardant, belong to novel dyeing and finishing and help
The development technique field of agent, can be used for the finishing functions of cotton fabric, reacts to form Covalent bonding together with cotton fabric, to assign cotton
Fabrics flame resistance function.
Background technique
The wearability outstanding that cotton fiber as natural fiber there are various chemical fibres not have, such as hydrophily,
Biocompatibility, degradability etc..People also increasingly tend to this kind of natural fabrics using cotton fabric etc..With each
Class weaving and the development of finishing technique, the purposes of cotton fabric is more and more extensive, not only can be made the underwear contacted with skin and produces
Product, moreover it is possible to make various decorations, the product taken outside.But the extremely incendive performance of cotton fabric affects it in the hair of more areas
Exhibition, while the potential security of the lives and property can be also brought to consumer, so the flame retardant treatment of cotton fabric just becomes increasingly to weigh
It wants.Researcher also develops some cotton fabric fire retardants, wherein the dosage of organophosphorous fire retardant Pyrovatex CP etc.
Larger, the thermal cracking products of organophosphorous fire retardant have very strong dehydration, promote charing when cotton fabric is heated, promote
Into the formation of charring layer, so that final carbon left surplus ratio increases, good fire retardation is played, the fabric being organized is made
With excellent flame retardant property.But Pyrovatex CP etc., which has to pass through high temperature, to be baked, fire retardant could occur with cotton fiber
Covalent cross-linking, since it contains N- methylol, leads to the cotton after arranging although improving washability of the fire retardant on cotton fabric
There is Form aldehyde release in fabric, and formaldehyde is determined as suspicious carcinogenic and teratogenesis toxic gas by the World Health Organization.Cause
This, the exploitation of novel high-efficiency environment friendly fire retardant is more and more of interest by researcher.The invention reside in prepare it is a kind of can and cotton fabric
Phosphorus-nitrogen-sulphur synergistic cotton flame retardant of covalent reaction occurs, which contains phosphorus, nitrogen, element sulphur, cotton fabric can occur
Cooperative flame retardant effect, while having and can improve the resistance to of fire retardant on cotton fabric with the active group of cotton fiber covalent reaction
Long property, the auxiliary agent can be such that fabric sufficiently reacts with fire retardant and reach good fire-retardant effect under the premise of not using crosslinking agent
Fruit does not influence the properties such as whiteness, the strength of fabric again while so that it is obtained good flame retardant property.
Currently, to have not been reported cotton of the present invention fire-retardant with response type phosphorus-nitrogen-sulphur synergistic for patent both domestic and external and document
The preparation method of agent, this function additive in terms of finishing functions of textile fabrics with good application prospect and practical value.
Summary of the invention
The invention reside in a kind of novel dyeing and finishing auxiliaries are synthesized, it is fire-retardant with response type phosphorus-nitrogen-sulphur synergistic to provide a kind of cotton
The preparation method of agent, the auxiliary agent can be with cotton fibers with the flame retardant property of Covalent bonding together providing cotton fabric excellent durability.
The synthetic method of cotton of the invention response type phosphorus-nitrogen-sulphur synergistic flame retardant operates as follows:
(1) the dichloro s-triazine base sodium sulfanilate salt of homemade 1 times of mole is added in three-necked flask, pours into appropriate
Distillation water as solvent three-necked flask is fixed in the tepidarium of heat-collecting magnetic stirring device with iron stand after mixing evenly,
Then the methylol dimethylphosphite of 1 times of mole is dissolved in appropriate distilled water, at 55 DEG C by methylol by temperature setting
The aqueous solution of dimethylphosphite is added dropwise in above-mentioned three-necked flask, is stirred continuously reaction at 55 DEG C, with 20% sodium carbonate
Solution adjusting pH=7-8, makes reaction carry out 4 h again after dripping off, product obtains white after condensation drying further isolates and purifies
Color solid powder, primary product are response type phosphorus-nitrogen-sulphur synergistic flame retardant, and key reaction equation is as follows:
Final product is cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant.
The method of the present invention is mainly used for the flame-proof treatment of cotton fabric.
Specific embodiment
Embodiment 1:
(1) Cyanuric Chloride of 9.22g (0.05mol) is added in three-necked flask, proper amount of acetone is added as solvent, by 11.56g
(0.05mol) sodium sulfanilate salt is dissolved in appropriate distilled water, will fill three mouthfuls of Cyanuric Chloride solution with iron stand
Flask is fixed in ice-water bath, and sodium sulfanilate solution is added dropwise in three-necked flask, is maintained at 0 DEG C and is stirred continuously
Reaction adjusts pH=5-6 with 20% aqueous sodium carbonate, and reaction carries out 1h, and primary product is dichloro s-triazine base p-aminophenyl
Sodium sulfonate (product A).
(2) 17.12g product A is added in three-necked flask, with distillation water as solvent, after mixing evenly, with iron stand by three
Mouth flask is fixed in the tepidarium of heat-collecting magnetic stirring device, and temperature setting is at 55 DEG C, then by 7.00g(0.05mol) hydroxyl
Methylisothiouronium methylphosphite dimethyl ester is dissolved in appropriate distilled water, the aqueous solution of methylol dimethylphosphite is added dropwise to above-mentioned
In three-necked flask, be stirred continuously reaction at 55 DEG C, adjust pH=7-8 with 20% aqueous sodium carbonate, make to react again after dripping off into
4 h of row, product obtain white solid powder after condensation drying further isolates and purifies, and primary product is cotton response type
Phosphorus-nitrogen-sulphur synergistic flame retardant (product B).
(3) 3.96 g of pure cotton fabric is cut, fire retardant 16.55g and 75.24 mL that the primary product of synthesis is B are distilled
Water, which is warming up to 60 DEG C and is uniformly mixed, is made finishing fluid, and cotton fabric is immersed in finishing fluid and is stirred continuously with glass bar, after 15 min
Sodium chloride (40 g/L) 3.01g is added, the reaction was continued, and 15 min react cotton fiber sufficiently with fire retardant, then heat to 90
DEG C, sodium carbonate (10 g/L) 0.75 g is added and is stirred continuously, sample, washing, drying are taken out after 1 h.
(4) it " is spun according to GB/T5454-1997 " textile combustion performance test oxygen index method ", GB/T 5455-2014
Fabric combustibility vertical direction char length, the measurement glowed with after flame time " test finish fabric limit oxygen index,
After flame time, smoldering time, char length.
Flame retardant property test:
| Finish fabric | Pure cotton blank fabric | |
| LOI | 30.5% | 18% |
| After flame time (s) | 0 | — |
| Smoldering time (s) | 0 | — |
| Char length (cm) | 7.2 | After-flame |
According to GB/T5454-1997, when the nonflammable material that belongs to of LOI≤26%, the limit oxygen index LOI of fabric after arrangement=
30.5%, illustrate after handling cotton fabric using auxiliary agent of the present invention, cotton fabric anti-flammability with higher.
Embodiment 2:
(1) Cyanuric Chloride of 5.53g (0.03mol) is added in three-necked flask, proper amount of acetone is added as solvent, by 6.94g
(0.03mol) sodium sulfanilate salt is dissolved in appropriate distilled water, will fill three mouthfuls of Cyanuric Chloride solution with iron stand
Flask is fixed in ice-water bath, and sodium sulfanilate solution is added dropwise in three-necked flask, is maintained at 0 DEG C and is stirred continuously
Reaction adjusts pH=5-6 with 20% aqueous sodium carbonate, and reaction carries out 1h, and primary product is dichloro s-triazine base p-aminophenyl
Sodium sulfonate (product A).
(2) 10.27g product A is added in three-necked flask, with distillation water as solvent, after mixing evenly, with iron stand by three
Mouth flask is fixed in the tepidarium of heat-collecting magnetic stirring device, and temperature setting is at 55 DEG C, then by 4.20(0.03mol) hydroxyl first
Base dimethylphosphite is dissolved in appropriate distilled water, and the aqueous solution of methylol dimethylphosphite is added dropwise to above-mentioned three
In mouth flask, it is stirred continuously reaction at 55 DEG C, pH=7-8 is adjusted with 20% aqueous sodium carbonate, reaction is made to carry out 4 after dripping off again
H, product obtain white solid powder after condensation drying further isolates and purifies, and primary product is cotton response type phosphorus-
Nitrogen-sulphur synergistic flame retardant (product B).
(3) 4.36 g of pure cotton fabric is cut, fire retardant 18.22g and 82.84 mL that the primary product of synthesis is B are distilled
Water, which is warming up to 60 DEG C and is uniformly mixed, is made finishing fluid, and cotton fabric is immersed in finishing fluid and is stirred continuously with glass bar, after 15 min
Sodium chloride (40 g/L) 3.13g is added, the reaction was continued, and 15 min react cotton fiber sufficiently with fire retardant, then heat to 90
DEG C, sodium carbonate (10 g/L) 0.83 g is added and is stirred continuously, sample, washing, drying are taken out after 1 h.
(4) it " is spun according to GB/T5454-1997 " textile combustion performance test oxygen index method ", GB/T 5455-2014
Fabric combustibility vertical direction char length, the measurement glowed with after flame time " test finish fabric limit oxygen index,
After flame time, smoldering time, char length.
Flame retardant property test:
| Finish fabric | Pure cotton blank fabric | |
| LOI | 29.7% | 18% |
| After flame time (s) | 0 | — |
| Smoldering time (s) | 0 | — |
| Char length (cm) | 8.6 | After-flame |
According to GB/T5454-1997, when the nonflammable material that belongs to of LOI≤26%, the limit oxygen index LOI of fabric after arrangement=
29.7%, illustrate after handling cotton fabric using auxiliary agent of the present invention, cotton fabric anti-flammability with higher.
Claims (1)
1. a kind of cotton preparation method of response type phosphorus-nitrogen-sulphur synergistic flame retardant, it is characterised in that operate in accordance with the following steps:
The dichloro s-triazine base sodium sulfanilate salt of homemade 1 times of mole is added in three-necked flask, pours into suitable
Three-necked flask is fixed in the tepidarium of heat-collecting magnetic stirring device with iron stand by distillation water as solvent after mixing evenly, temperature
Degree is arranged at 55 DEG C, and then the methylol dimethylphosphite of 1 times of mole is dissolved in appropriate distilled water, by methylol Asia
The aqueous solution of dimethyl phosphate is added dropwise in above-mentioned three-necked flask, is stirred continuously reaction at 55 DEG C, water-soluble with 20% sodium carbonate
Liquid adjusting pH=7-8, makes reaction carry out 4 h again after dripping off, product obtains white after condensation drying further isolates and purifies
Solid powder, primary product are response type phosphorus-nitrogen-sulphur synergistic flame retardant, and key reaction equation is as follows:
Final product is cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910450001.9A CN110054648A (en) | 2019-05-28 | 2019-05-28 | A kind of preparation method of cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910450001.9A CN110054648A (en) | 2019-05-28 | 2019-05-28 | A kind of preparation method of cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant |
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| Publication Number | Publication Date |
|---|---|
| CN110054648A true CN110054648A (en) | 2019-07-26 |
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| CN201910450001.9A Pending CN110054648A (en) | 2019-05-28 | 2019-05-28 | A kind of preparation method of cotton response type phosphorus-nitrogen-sulphur synergistic flame retardant |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024815A (en) * | 2021-04-09 | 2021-06-25 | 苏州大学 | Phosphorus/nitrogen/silica sol flame-retardant liquid and application thereof in flame-retardant finishing of protein fiber products |
| CN113089319A (en) * | 2021-04-09 | 2021-07-09 | 苏州大学 | Phosphorus/nitrogen/sulfur synergistic flame retardant and application thereof in flame retardant finishing of protein fiber products |
| CN115557740A (en) * | 2022-11-03 | 2023-01-03 | 深圳知本建筑节能材料有限公司 | Heat insulation material |
Citations (3)
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| CN103882698A (en) * | 2014-03-07 | 2014-06-25 | 浙江理工大学 | Symtriazine-type flame retardant, preparation method and application of symtriazine-type flame retardant |
| CN103980315A (en) * | 2014-05-27 | 2014-08-13 | 中北大学 | Triazine ring-containing phosphorus-nitrogen-silicon compound and preparation method thereof |
| CN104846639A (en) * | 2015-05-26 | 2015-08-19 | 中北大学 | Flame-retardant finishing method of reactive expansion flame retardants on cotton fabrics |
-
2019
- 2019-05-28 CN CN201910450001.9A patent/CN110054648A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882698A (en) * | 2014-03-07 | 2014-06-25 | 浙江理工大学 | Symtriazine-type flame retardant, preparation method and application of symtriazine-type flame retardant |
| CN103980315A (en) * | 2014-05-27 | 2014-08-13 | 中北大学 | Triazine ring-containing phosphorus-nitrogen-silicon compound and preparation method thereof |
| CN104846639A (en) * | 2015-05-26 | 2015-08-19 | 中北大学 | Flame-retardant finishing method of reactive expansion flame retardants on cotton fabrics |
Non-Patent Citations (1)
| Title |
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| SUN, FUYU ET AL.: "Synthesis, characterization, and DFT of a novel reactive phosphorus flame retardant", 《 ADVANCED MATERIALS RESEARCH》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024815A (en) * | 2021-04-09 | 2021-06-25 | 苏州大学 | Phosphorus/nitrogen/silica sol flame-retardant liquid and application thereof in flame-retardant finishing of protein fiber products |
| CN113089319A (en) * | 2021-04-09 | 2021-07-09 | 苏州大学 | Phosphorus/nitrogen/sulfur synergistic flame retardant and application thereof in flame retardant finishing of protein fiber products |
| CN113089319B (en) * | 2021-04-09 | 2022-03-11 | 苏州大学 | Phosphorus/nitrogen/sulfur synergistic flame retardant and application thereof in flame retardant finishing of protein fiber products |
| CN113024815B (en) * | 2021-04-09 | 2022-04-01 | 苏州大学 | Phosphorus/nitrogen/silica sol flame-retardant liquid and application thereof in flame-retardant finishing of protein fiber products |
| CN115557740A (en) * | 2022-11-03 | 2023-01-03 | 深圳知本建筑节能材料有限公司 | Heat insulation material |
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Application publication date: 20190726 |