CN108018715A - A kind of preparation method of antiflaming finishing agent and fire-retardant regenerated cellulose fiber - Google Patents
A kind of preparation method of antiflaming finishing agent and fire-retardant regenerated cellulose fiber Download PDFInfo
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- CN108018715A CN108018715A CN201711302531.6A CN201711302531A CN108018715A CN 108018715 A CN108018715 A CN 108018715A CN 201711302531 A CN201711302531 A CN 201711302531A CN 108018715 A CN108018715 A CN 108018715A
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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
- 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
- D06M13/453—Phosphates or phosphites 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
- 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
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
-
- 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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses the preparation method of a kind of antiflaming finishing agent and fire-retardant regenerated cellulose fiber, this method is related to organic synthesis and textile engineering technical field.The preparation process of antiflaming finishing agent and fire-retardant regenerated cellulose fiber is in the present invention:First with polyalcohol such as ethylene glycol, glycerine, pentaerythrite etc., or polyhydric alcohol amine such as monoethanolamine, diethanol amine, triethanolamine etc., the i.e. polynary phosphate of the antiflaming finishing agent is prepared with phosphatase reaction, secondly polynary phosphate is dissolved in N, in N dimethylformamides, and add a certain amount of urea and be configured to fire retarding treating liquid, regenerated celulose fibre is immersed in dressing liquid, flame retardant treatment is carried out at a certain temperature, is finally dried in vacuo up to fire-retardant regenerated cellulose fiber.Fire retardant preparation process of the present invention is simple, cost is low, yield is high, environmentally protective, high temperature drying and the process of hot setting need not be used by preparing fire resistance fibre, on the basis of the excellent fire resistance of regenerated celulose fibre and good wash durability is assigned, its mechanical property and dyeability are not influenced, and there are great market prospects in application aspect.
Description
Technical field
The present invention relates to organic synthesis and textile engineering technical field, and in particular to a kind of antiflaming finishing agent and fire-retardant
The preparation method of regenerated celulose fibre.
Background technology
Regenerated celulose fibre is the fiber prepared using native cellulose as raw material, have excellent hygroscopicity, gas permeability,
The advantages that snugness of fit, pure can both spin, can also be blended with other textile fabrics, be suitable for manufacturing coat, underwear and various
Adornment.However, regenerated celulose fibre category flammable fiber, the textile being made from it easily burn and trigger fire, because
This, has been devoted to the fire-retardant research of fire-retardant regenerated cellulose fiber both at home and abroad, and production flame retardant textiles become and can not neglect
Depending on social concern, be progressively valued by people.
At present, the flame retardant cellulose fiber of industrialization mainly uses halogenated flame retardant and phosphorus flame retardant, such as Proban/ ammonia
Smoked technique, generates preshrunk body, the subsequent preshrunk body oozes in a manner of padding drying using tetra methylol phosphonium chloride and urea reaction
Entering into the amorphous area and gap of regenerated celulose fibre, then handled by ammonia cure, the methylol and ammonia for making preshrunk body are crosslinked,
Fabric forms after non-soluble polymer and obtains rock-steady structure through hydrogen peroxide oxidation, obtains excellent flame-proof cotton fabric, but
This method complex process, production cycle length, while formaldehyde can be discharged.The flame-proof finishing process that another kind is widely used is
Pyrovatex CP techniques, using N- methylols -3- (dimethoxy phosphono) propionamides and crosslinking agent under acid catalysis with fibre
Dimension element crosslinks reaction, prepares durable flame-retardant cotton fabric, but its application can release formaldehyde with combustion process.Chinese patent
CN104975497A is used as crosslinking agent pair using melamine pregnancy fork phosphoric acid and the fire retardant of urea reaction generation using dicyandiamide
Fiber is arranged, and obtains durable flame-retardant fiber, but the preparation process of fire retardant needs to use formaldehyde.Meanwhile above-mentioned arrangement
Process uses pad-dry-cure technique, and curing process needs to implement at very high temperatures.
In conclusion the present invention devises the preparation method of a kind of antiflaming finishing agent and fire-retardant regenerated cellulose fiber.
The content of the invention
In view of the shortcomings of the prior art, the present invention seeks to be to provide a kind of antiflaming finishing agent and fire-retardant regeneration
The preparation method of cellulose fibre, antiflaming finishing agent preparation process is simple, yield is high, environmentally protective, the preparation of fire resistance fibre
Journey need not use pad-dry-cure technique, react certain time after only being mixed by fire retardant with regenerated celulose fibre
Fire resistance fibre is can be prepared by, fire-retardant regenerated celulose fibre fire resistance is good, durability is good.
To achieve these goals, the present invention is to realize by the following technical solutions:A kind of system of antiflaming finishing agent
Preparation Method, comprises the following steps:By polyalcohol or polyhydric alcohol amine with phosphoric acid when reaction 1~3 is small at a temperature of 100 DEG C~130 DEG C
The polynary phosphate of the antiflaming finishing agent is synthesized, wherein, the molar ratio of polyalcohol and phosphoric acid is 1:2~4, polyhydric alcohol amine and phosphorus
The molar ratio of acid is 1:1~3.
The polyalcohol is diethanol, one kind in glycerine, pentaerythrite.
The polyhydric alcohol amine is monoethanolamine, one kind in diethanol amine, triethanolamine.
A kind of preparation method of fire-retardant regenerated cellulose fiber, comprises the following steps:First by 5~10 grams of polynary phosphates
It is dissolved in 10~30 milliliters of n,N-Dimethylformamide, then adds 6~12 grams of urea and be configured to fire retarding treating liquid, will
0.2~0.4 gram of regenerated celulose fibre is immersed in fire retarding treating liquid, finally will again when reaction 1~3 is small at 130~150 DEG C
Raw cellulose fibre is washed to neutrality, up to fire-retardant regenerated cellulose fiber when 30~50 DEG C of vacuum drying 1~12 are small.
The regenerated celulose fibre for viscose rayon, Lyocell fiber, Modal fibers, copper ammonia fiber cellulose fiber,
Cellulose carbamate fibre, ionic liquid spin one kind in cellulose fibre.
Beneficial effects of the present invention:Fire retardant preparation process provided by the invention is simple, yield is high, environmentally protective, fire-retardant
Fiber need not use pad-dry-cure technique, and a timing is reacted after only being mixed by fire retardant with regenerated celulose fibre
Between can be prepared by fire resistance fibre, fire-retardant regenerated celulose fibre fire resistance is good, and water-wash resistance is good.
Embodiment
To make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, with reference to
Embodiment, the present invention is further explained.
Present embodiment uses following technical scheme:A kind of preparation method of antiflaming finishing agent, comprises the following steps:
It is more that polyalcohol or polyhydric alcohol amine with phosphoric acid when reaction 1~3 is small at a temperature of 100 DEG C~130 DEG C are synthesized into the antiflaming finishing agent
First phosphate, wherein, the molar ratio of polyalcohol and phosphoric acid is 1:2~4, the molar ratio of polyhydric alcohol amine and phosphoric acid is 1:1~
3。
The polyalcohol is diethanol, one kind in glycerine, pentaerythrite.
The polyhydric alcohol amine is monoethanolamine, one kind in diethanol amine, triethanolamine.
A kind of preparation method of fire-retardant regenerated cellulose fiber, comprises the following steps:First by 5~10 grams of polynary phosphates
It is dissolved in 10~30 milliliters of n,N-Dimethylformamide, then adds 6~12 grams of urea and be configured to fire retarding treating liquid, will
0.2~0.4 gram of regenerated celulose fibre is immersed in fire retarding treating liquid, finally will again when reaction 1~3 is small at 130~150 DEG C
Raw cellulose fibre is washed to neutrality, up to fire-retardant regenerated cellulose fiber when 30~50 DEG C of vacuum drying 1~12 are small.
The regenerated celulose fibre for viscose rayon, Lyocell fiber, Modal fibers, copper ammonia fiber cellulose fiber,
Cellulose carbamate fibre, ionic liquid spin one kind in cellulose fibre.
Present embodiment fire retardant preparation process is simple, cost is low, yield is high, environmentally protective, prepares fire resistance fibre
High temperature drying and the process of hot setting need not be used, in the excellent fire resistance of imparting regenerated celulose fibre and well
On the basis of wash durability, its mechanical property and dyeability are not influenced, and there are great market prospects in application aspect.
Embodiment 1:The preparation of flame-retardant Lyocell fiber
1st, the synthesis of antiflaming finishing agent 1,2- diphosphonic acid ethyl ester:3.103 grams of ethylene glycol and 9.8 grams of phosphoric acid are added
To being equipped with 50 milliliters of flasks of reflux condensing tube, blender, 100 DEG C are warming up under nitrogen protection, keeps the temperature anti-
Answer 2 it is small when, product is water white transparency thick liquid i.e. 1,2- diphosphonic acid ethyl esters;
2nd, the preparation of flame-retardant Lyocell fiber:6.66 grams of 1,2- diphosphonic acid ethyl esters are dissolved in 30 milliliters of N, N- diformazans
In base formamide, then add 5.41 grams of urea and be configured to fire retarding treating liquid, 0.3 gram of Lyocell fiber is immersed fire-retardant
In dressing liquid, when reaction 1 is small at 150 DEG C, regenerated celulose fibre is finally washed to neutrality, when 40 DEG C of vacuum drying 12 are small
Up to flame-retardant Lyocell fiber.
Embodiment 2:The preparation of flame retardant viscose fiber
1st, the synthesis of antiflaming finishing agent 1,2,3- triphosphoric acids propyl diester:4.61 grams of glycerine is added with 14.7 grams of phosphoric acid
Enter to being equipped with 50 milliliters of flask of reflux condensing tube, blender, be warming up to 130 DEG C under nitrogen protection, keep the temperature
When degree reaction 1 is small, product is water white transparency thick liquid i.e. 1,2,3- triphosphoric acid propyl diesters;
2nd, the preparation of flame retardant viscose fiber:9.963 grams of 1,2,3- triphosphoric acid propyl diesters are dissolved in 30 milliliters of N, N- diformazans
In base formamide, then add 5.41 grams of urea and be configured to fire retarding treating liquid, 0.3 gram of viscose rayon is immersed into flame-proof treatment
In liquid, when reaction 2 is small at 150 DEG C, regenerated celulose fibre is finally washed to neutrality, when 40 DEG C of vacuum drying 6 are small to obtain the final product
Flame retardant viscose fiber.
Embodiment 3:The preparation of fire-retardant copper ammonia fiber cellulose fiber
1st, the synthesis of antiflaming finishing agent 2,2- diphosphonic acid monoethanolamine base ester:By 5.257 grams of diethanol amine and 9.8 grams of phosphorus
Acid, which is added to, to be equipped with 50 milliliters of flask of reflux condensing tube, blender, is warming up to 130 DEG C under nitrogen protection, is kept
When the thermotonus 2 is small, product is water white transparency thick liquid i.e. 2,2- diphosphonic acid monoethanolamine base esters;
2nd, the preparation of fire-retardant copper ammonia fiber cellulose fiber:8.36 grams of 2,2- diphosphonic acid monoethanolamine base esters are dissolved in 30 milliliters of N,
In dinethylformamide, then add 12.01 grams of urea and be configured to fire retarding treating liquid, will be plain by 0.4 gram of copper ammonia fiber
Fiber is immersed in fire retarding treating liquid, when reaction 3 is small at 130 DEG C, regenerated celulose fibre finally is washed to neutrality, 40 DEG C true
Up to fire-retardant copper ammonia fiber cellulose fiber when sky dry 1 is small.
Embodiment 4:The preparation of flame-retardant Lyocell fiber
1st, the synthesis of antiflaming finishing agent 2,2- diphosphonic acid monoethanolamine base ester:By 525.7 grams of diethanol amine and 989 grams of phosphorus
Acid, which is added to, to be equipped with 5 liters of reaction kettle of reflux condensing tube, blender, is warming up to 130 DEG C under nitrogen protection, and keeping should
When thermotonus 1.5 is small, product is water white transparency thick liquid i.e. 2,2- diphosphonic acid monoethanolamine base esters;
2nd, the preparation of flame-retardant Lyocell fiber:836 grams of 2,2- diphosphonic acid monoethanolamine base esters are dissolved in 3 liters of N, N- diformazans
In base formamide, then add 1201 grams of urea and be configured to fire retarding treating liquid, 30 grams of Lyocell fiber is immersed fire-retardant whole
Manage in liquid, when reaction 2 is small at 130 DEG C, regenerated celulose fibre is finally washed to neutrality, when 40 DEG C of vacuum drying 6 are small
Obtain flame-retardant Lyocell fiber.
Embodiment 5:The preparation of flame-retardant Lyocell fiber
1st, the synthesis of antiflaming finishing agent 2,2- diphosphonic acid monoethanolamine base ester:By 2.1 kilograms of diethanol amine and 3.92 kilograms
Phosphoric acid be added to and be equipped with 5 liters of reaction kettle of reflux condensing tube, blender, be warming up to 130 DEG C under nitrogen protection, protect
Hold the thermotonus 2 it is small when, product is water white transparency thick liquid i.e. 2,2- diphosphonic acid monoethanolamine base esters;
2nd, the preparation of flame-retardant Lyocell fiber:16.7 kilograms of 2,2- diphosphonic acid monoethanolamine base esters are dissolved in 60 liters of N, N-
In dimethylformamide, then add 24 kilograms of urea and be configured to fire retarding treating liquid, 600 grams of Lyocell fiber is immersed
In fire retarding treating liquid, when reaction 2 is small at 140 DEG C, regenerated celulose fibre is finally washed to neutrality, 40 DEG C of vacuum drying 10
Hour is up to flame-retardant Lyocell fiber.
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (5)
1. a kind of preparation method of antiflaming finishing agent, comprises the following steps:By polyalcohol or polyhydric alcohol amine and phosphoric acid 100 DEG C~
The polynary phosphate of the antiflaming finishing agent is synthesized when reaction 1~3 is small at a temperature of 130 DEG C, wherein, the molar ratio of polyalcohol and phosphoric acid
Example is 1:2~4, the molar ratio of polyhydric alcohol amine and phosphoric acid is 1:1~3.
2. the preparation method of a kind of antiflaming finishing agent according to claim 1, it is characterised in that the polyalcohol is two
One kind in ethanol, glycerine, pentaerythrite.
3. the preparation method of a kind of antiflaming finishing agent according to claim 1, it is characterised in that the polyhydric alcohol amine is
One kind in monoethanolamine, diethanol amine, triethanolamine.
4. a kind of preparation method of fire-retardant regenerated cellulose fiber, comprises the following steps:It is first that 5~10 grams of polynary phosphates are molten
In 10~30 milliliters of n,N-Dimethylformamide, then add 6~12 grams of urea and be configured to fire retarding treating liquid, by 0.2
~0.4 gram of regenerated celulose fibre is immersed in fire retarding treating liquid, finally will regeneration fibre when reaction 1~3 is small at 130~150 DEG C
Cellulose fiber is washed to neutrality, up to fire-retardant regenerated cellulose fiber when 30~50 DEG C of vacuum drying 1~12 are small.
5. a kind of preparation method of fire-retardant regenerated cellulose fiber according to claim 4, comprises the following steps:Described
Regenerated celulose fibre is viscose rayon, Lyocell fiber, Modal fibers, copper ammonia fiber cellulose fiber, cellulose carbamic acid
Ester fiber, ionic liquid spin one kind in cellulose fibre.
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Cited By (7)
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CN109537285A (en) * | 2018-11-03 | 2019-03-29 | 阜宁澳洋科技有限责任公司 | A kind of manufacturing method of flame retardant viscose fiber |
CN110273295A (en) * | 2019-06-20 | 2019-09-24 | 南通大学 | A kind of cellulose fiber Wesy flame-proof antibiotic phytic acid ammonium finishing agent and its method for sorting |
CN111592566A (en) * | 2019-02-21 | 2020-08-28 | 中国科学院理化技术研究所 | Preparation method of halogen-free flame retardant |
WO2020173101A1 (en) * | 2019-02-26 | 2020-09-03 | 东华大学 | Method for preparing flame-retardant cellulose fibre |
CN112442895A (en) * | 2019-09-03 | 2021-03-05 | 天津工业大学 | Chelate coordination type phosphorus-boron-nitrogen synergistic flame retardant and preparation method thereof |
CN112680963A (en) * | 2020-12-15 | 2021-04-20 | 南京金羚生物基纤维有限公司 | Preparation method of novel flame-retardant Lyocell fiber |
CN115650201A (en) * | 2022-12-26 | 2023-01-31 | 山东海科创新研究院有限公司 | Preparation method of lithium difluorophosphate |
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CN109537285B (en) * | 2018-11-03 | 2021-12-17 | 赛得利(盐城)纤维有限公司 | Method for manufacturing flame-retardant viscose fibers |
CN111592566B (en) * | 2019-02-21 | 2023-04-25 | 中国科学院理化技术研究所 | Preparation method of halogen-free flame retardant |
CN111592566A (en) * | 2019-02-21 | 2020-08-28 | 中国科学院理化技术研究所 | Preparation method of halogen-free flame retardant |
US11124900B2 (en) | 2019-02-26 | 2021-09-21 | Donghua University | Method for preparing flame-retardant cellulosic fibers |
WO2020173101A1 (en) * | 2019-02-26 | 2020-09-03 | 东华大学 | Method for preparing flame-retardant cellulose fibre |
CN110273295B (en) * | 2019-06-20 | 2022-01-14 | 南通大学 | Flame-retardant antibacterial ammonium phytate finishing agent for cellulose fibers and finishing method thereof |
CN110273295A (en) * | 2019-06-20 | 2019-09-24 | 南通大学 | A kind of cellulose fiber Wesy flame-proof antibiotic phytic acid ammonium finishing agent and its method for sorting |
CN112442895A (en) * | 2019-09-03 | 2021-03-05 | 天津工业大学 | Chelate coordination type phosphorus-boron-nitrogen synergistic flame retardant and preparation method thereof |
CN112442895B (en) * | 2019-09-03 | 2024-01-12 | 天津工业大学 | Chelate coordination type phosphorus-boron-nitrogen synergistic flame retardant and preparation method thereof |
CN112680963A (en) * | 2020-12-15 | 2021-04-20 | 南京金羚生物基纤维有限公司 | Preparation method of novel flame-retardant Lyocell fiber |
CN115650201A (en) * | 2022-12-26 | 2023-01-31 | 山东海科创新研究院有限公司 | Preparation method of lithium difluorophosphate |
WO2024008206A1 (en) * | 2022-12-26 | 2024-01-11 | 山东海科创新研究院有限公司 | Preparation method for lithium difluorophosphate |
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