CN101701423A - Phosphorus flame retardant for viscose fibers and production method and application thereof - Google Patents
Phosphorus flame retardant for viscose fibers and production method and application thereof Download PDFInfo
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- CN101701423A CN101701423A CN 200910217775 CN200910217775A CN101701423A CN 101701423 A CN101701423 A CN 101701423A CN 200910217775 CN200910217775 CN 200910217775 CN 200910217775 A CN200910217775 A CN 200910217775A CN 101701423 A CN101701423 A CN 101701423A
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- flame retardant
- phosphorus flame
- dithiothyldimaide
- retardant
- fire
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Abstract
The invention discloses a phosphorus flame retardant for viscose fibers, which has the following chemical structural formula and is named as N,N'-bis (diphenoxy thiophosphoryl) dithicoxamide. The flame retardant can be prepared into flame retardant emulsion with methylene dinaphthyl sodium sulfonate, sodium dodecyl benzene sulfonate and tween-80. The flame retardant of the invention is an additive flame retardant for viscose fibers, is a phosphorus flame retardant which contains phosphorus, sulfur and nitrogen for synergetic flame retarding, does not contain halogen elements and has little pollution to the environment during thermal decomposition, and the fabrics treated by the flame retardant have obvious advantages of good flame retardant effects, high durability, small strength reduction and the like.
Description
Technical field
The present invention relates to a kind of fire-retardant new material, particularly a kind of phosphorus flame retardant and manufacture method and purposes that is used for viscose.
Background technology
Fire preventing is an eternal theme of human society safety.The macromolecular material that extensively adopts in industrial or agricultural now and the people's lives, the overwhelming majority is flammable and inflammable in air, their limited oxygen index is lower than 20% more.Therefore, the fire that various countries took place in recent decades, a large portion is ignited by macromolecular material and is caused.And the synthesized polymer material in modern age is different with the composition of natural macromolecular material, and the former can produce the flue dust of poisonous in a large number and acrid gaseous products when thermal cracking and burning, thereby they cause consequence just more serious in fire.Given this, each developed country of the world all gives great attention to the flame treatment of macromolecular material at present, the comparatively advanced mainstream product of wherein production Fire resistant viscose fiber has: the Polynosic viscose that the Fire resistant viscose fiber of Austrian Lenzing company and Japanese Japan are spun, and its fire retardant is organophosphor or halogen organic compound; Greatly Japanese and spin HFG fiber, its fire retardant is a chlorinated phosphate; The Luo Napu Lang Ke TF-80 fiber of France and the PER viscose of the U.S., its fire retardant is an organosilane ester; The cellulose that the Kemiraoy company of Finland produces and the mixture of fibers Visil of poly-silicic acid, its fire retardant is waterglass (sodium metasilicate).With abroad compare, the research of domestic Fire resistant viscose fiber only has about ten years historical, has explored blending method, dip coating etc., used fire retardant is a pyrophosphate class organic compound.Dandong FCFC, Nanjing FCFC, Shanghai chemical fibre three factories, sequential trial or small lot batch manufacture the Fire resistant viscose fiber product.The STI-27 fire retardant that Baoding chemical fibre mill adopts Switzerland Sandoflam-5060 and Shanghai to spin the production of institute of section has carried out the experimental study of anti-flaming viscose silk.
The fire retardant major part that production both at home and abroad at present and research cellulose are used is a halogen containing flame-retardant, because halogen containing flame-retardant in the decomposes process, can produce a large amount of toxic gases, thereby can bring the serious environmental pollution problem.
Summary of the invention
The purpose of this invention is to provide a kind of phosphorus flame retardant and manufacture method and purposes that is used for viscose.This phosphorus flame retardant is not halogen-containing compound, does not also contain formaldehyde, has good flame retardation effect, and characteristics of high efficiency and low toxicity is a kind of environment friendly flame retardant.
This fire retardant is a phosphorus flame retardant, and its chemical structural formula is as follows:
Called after N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
The manufacture method of this fire retardant is as follows: with the ratio of quality is that 2: 1 two phenoxy group thiophosphoryl chlorides and dithiothyldimaide is dissolved in N, in N-dimethylacetylamide or the ortho-xylene solvent, the pyridine or the triethylamine that add two times of dithiothyldimaide quality are the aluminium chloride (AlCl of acid binding agent and dithiothyldimaide quality 0.2～0.5%
3) or magnesium chloride (MgCl
2) as catalyst, under 40～80 ℃ condition, reacted 4～6 hours, reaction after finishing is washed product; with the dimethyl sulfoxide (DMSO) recrystallization, oven dry can obtain fire retardant lurid, needle-like; be N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
The application of phosphorus flame retardant of the present invention is to be made into fire-retardant emulsion by following prescription:
Phosphorus flame retardant 150g
Sodium metnylene bis-naphthalene sulfonate (NNO) 5g
Neopelex (DBS) 15g
Tween-80 (T-80) 10g
Use the ball mill ball milling after 10～15 hours according to the above ratio, thin up to a liter promptly can be made into fire-retardant emulsion.
The invention has the beneficial effects as follows: the present invention is a kind of addition type viscose fire retardant, is the phosphorus flame retardant that contains phosphorus, sulphur, nitrogen cooperative flame retardant, does not contain halogen element, and during thermal decomposition, contaminated environment is little.The fabric that uses this fire retardant to handle has good flame retardation effect, the durability height, and intensity reduces outstanding advantage such as little grade.
The specific embodiment
The present invention's fire retardant is a phosphorus flame retardant, and its chemical structural formula is as follows:
Called after N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
The manufacture method of this fire retardant is as follows: with the ratio of quality is that 2: 1 two phenoxy group thiophosphoryl chlorides and dithiothyldimaide is dissolved in N, in N-dimethylacetylamide or the ortho-xylene solvent, the pyridine or the triethylamine that add two times of dithiothyldimaide quality are the aluminium chloride (AlCl of acid binding agent and dithiothyldimaide quality 0.2～0.5%
3) or magnesium chloride (MgCl
2) as catalyst, under 40～80 ℃ condition, reacted 4～6 hours, reaction after finishing is washed product; with the dimethyl sulfoxide (DMSO) recrystallization, oven dry can obtain fire retardant lurid, needle-like; be N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
The application of phosphorus flame retardant of the present invention is to be made into fire-retardant emulsion by following prescription:
Phosphorus flame retardant 150g
Sodium metnylene bis-naphthalene sulfonate (NNO) 5g
Neopelex (DBS) 15g
Tween-80 (T-80) 10g
After using ball mill ball milling 10～15h according to the above ratio, thin up to a liter promptly can be made into fire-retardant emulsion.
Concrete manufacturing embodiment of the present invention is:
In the four-hole boiling flask of the 500ml that agitator, reflux condensing tube, thermometer, peristaltic pump are housed, add two phenoxy group thiophosphoryl chlorides, 60ml ortho-xylene, the dithiothyldimaide of 6g (0.05mol) and the AlCl of 0.001～0.0025g of 28.87g (0.1mol)
3, slowly the triethylamine of 10.1g is joined in the four-hole boiling flask with peristaltic pump then.Because this reaction is heat release, reversible reaction, can drip the speed that triethylamine speed is controlled reaction by peristaltic pump control, make reaction temperature be controlled at 40～80 ℃.After being added dropwise to complete; continue reaction after 2～3 hours; total reaction time is 4～6 hours, stops reaction, and product is filtered, washes 3～5 times; be recrystallized with dimethyl sulfoxide (DMSO) again; with the drying box oven dry, can get the crystal of light yellow needle-like, fire retardant promptly of the present invention; title is: N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
Claims (3)
1. phosphorus flame retardant that is used for viscose, its chemical structural formula is as follows:
Called after N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
2. the manufacture method that is used for the phosphorus flame retardant of viscose as claimed in claim 1; this method is that the ratio with quality is that 2: 1 two phenoxy group thiophosphoryl chlorides and dithiothyldimaide is dissolved in N; in N-dimethylacetylamide or the ortho-xylene solvent; aluminium chloride that pyridine that adding dithiothyldimaide quality is two times or triethylamine are acid binding agent and dithiothyldimaide quality 0.2～0.5% or magnesium chloride are as catalyst; under 40～80 ℃ condition, reacted 4～6 hours; reaction after finishing is washed product; be recrystallized with dimethyl sulfoxide (DMSO); oven dry; can obtain lurid; the fire retardant of needle-like; be N, N '-two (two phenoxy group thiophosphoryl bases) dithiothyldimaide.
3. the purposes that is used for the phosphorus flame retardant of viscose as claimed in claim 1 is that phosphorus flame retardant is made into fire-retardant emulsion by following prescription:
Phosphorus flame retardant 150g
Sodium metnylene bis-naphthalene sulfonate 5g
Neopelex 15g
Tween-80 10g
Use the ball mill ball milling after 10～15 hours according to the above ratio, thin up to a liter promptly can be made into fire-retardant emulsion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102177753A CN101701423B (en) | 2009-10-28 | 2009-10-28 | Phosphorus flame retardant for viscose fibers and production method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102177753A CN101701423B (en) | 2009-10-28 | 2009-10-28 | Phosphorus flame retardant for viscose fibers and production method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101701423A true CN101701423A (en) | 2010-05-05 |
| CN101701423B CN101701423B (en) | 2011-06-08 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102177753A Expired - Fee Related CN101701423B (en) | 2009-10-28 | 2009-10-28 | Phosphorus flame retardant for viscose fibers and production method and application thereof |
Country Status (1)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392314A (en) * | 2011-08-30 | 2012-03-28 | 成都丽雅纤维股份有限公司 | Halogen-free environment-friendly composite flame-retardant viscose fiber spinning solution and preparation method thereof |
| CN102561031A (en) * | 2012-02-03 | 2012-07-11 | 上海韬鸿化工科技有限公司 | Flame retardant viscose fiber and preparation method thereof |
| CN102816185A (en) * | 2012-09-14 | 2012-12-12 | 中国民用航空总局第二研究所 | Reaction type phosphorus-nitrogen fire retardant and preparation method thereof |
| CN103284368A (en) * | 2013-05-13 | 2013-09-11 | 上海特安纶纤维有限公司 | Blended flame-retardant fabric and flame-retardant protecting clothes |
| CN103614795A (en) * | 2013-11-25 | 2014-03-05 | 常熟市金羽纤维制品厂 | Flame-retardant viscose fiber |
| CN103981704A (en) * | 2014-05-23 | 2014-08-13 | 约克夏染料（中山）有限公司 | Multifunctional fabric fire retardant as well as preparation method and application of fabric fire retardant |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1642219A1 (en) * | 1967-03-18 | 1971-04-22 | Basf Ag | Pest repellants |
| US3658900A (en) * | 1970-08-03 | 1972-04-25 | Monsanto Co | N n'-dicyclopropyl dithiooxamide |
| DE10216736A1 (en) * | 2002-04-16 | 2004-02-05 | Bayer Ag | Flame retardants for polymers containing a mixture of two different aryl phosphates, their preparation and their use |
| CN100415758C (en) * | 2004-03-23 | 2008-09-03 | 天津工业大学 | Fire retardant in use for cellulose and fabricating method |
| CN101086136A (en) * | 2007-07-17 | 2007-12-12 | 中国石油化工股份有限公司 | Flame-resistant agent and its preparing process and usage |
| CN101498103A (en) * | 2009-02-16 | 2009-08-05 | 长春工业大学 | Non-formaldehyde flame retardant for viscose fiber |
-
2009
- 2009-10-28 CN CN2009102177753A patent/CN101701423B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392314A (en) * | 2011-08-30 | 2012-03-28 | 成都丽雅纤维股份有限公司 | Halogen-free environment-friendly composite flame-retardant viscose fiber spinning solution and preparation method thereof |
| CN102392314B (en) * | 2011-08-30 | 2013-12-25 | 成都丽雅纤维股份有限公司 | Halogen-free environment-friendly composite flame-retardant viscose fiber spinning solution and preparation method thereof |
| CN102561031A (en) * | 2012-02-03 | 2012-07-11 | 上海韬鸿化工科技有限公司 | Flame retardant viscose fiber and preparation method thereof |
| CN102561031B (en) * | 2012-02-03 | 2013-10-09 | 上海韬鸿化工科技有限公司 | Flame retardant viscose fiber and preparation method thereof |
| CN102816185A (en) * | 2012-09-14 | 2012-12-12 | 中国民用航空总局第二研究所 | Reaction type phosphorus-nitrogen fire retardant and preparation method thereof |
| CN102816185B (en) * | 2012-09-14 | 2015-01-28 | 中国民用航空总局第二研究所 | Reaction type phosphorus-nitrogen fire retardant and preparation method thereof |
| CN103284368A (en) * | 2013-05-13 | 2013-09-11 | 上海特安纶纤维有限公司 | Blended flame-retardant fabric and flame-retardant protecting clothes |
| CN103614795A (en) * | 2013-11-25 | 2014-03-05 | 常熟市金羽纤维制品厂 | Flame-retardant viscose fiber |
| CN103981704A (en) * | 2014-05-23 | 2014-08-13 | 约克夏染料（中山）有限公司 | Multifunctional fabric fire retardant as well as preparation method and application of fabric fire retardant |
| CN103981704B (en) * | 2014-05-23 | 2015-12-30 | 约克夏染料（中山）有限公司 | A kind of multifunctional fabric fire retardant and its preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101701423B (en) | 2011-06-08 |
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