CN108049173A - A kind of preparation method of phosphorus-nitrogen containing antiflaming finishing agent and flame retardant cellulose fiber fabric - Google Patents
A kind of preparation method of phosphorus-nitrogen containing antiflaming finishing agent and flame retardant cellulose fiber fabric Download PDFInfo
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- CN108049173A CN108049173A CN201711306962.XA CN201711306962A CN108049173A CN 108049173 A CN108049173 A CN 108049173A CN 201711306962 A CN201711306962 A CN 201711306962A CN 108049173 A CN108049173 A CN 108049173A
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- Prior art keywords
- finishing agent
- flame
- phytic acid
- phosphorus
- antiflaming finishing
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Classifications
-
- 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
- D06M13/244—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 sulfur or phosphorus
- D06M13/282—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 sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
-
- 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
Abstract
The invention discloses the preparation methods of a kind of phosphorus-nitrogen containing antiflaming finishing agent and flame retardant cellulose fiber fabric.The antiflaming finishing agent is phytic acid ammonium and urea, the mixed solution of dicyandiamide.The preparation method of the antiflaming finishing agent comprises the following steps:First using phytic acid and nitrogenous compound as Material synthesis fire retardant phytic acid ammonium;Secondly it is the fire retardant phytic acid ammonium of synthesis is soluble in water, add in a certain amount of urea, crosslinking agent is made into the antiflaming finishing agent of respective concentration;Finally, the flame-proof treatment for antiflaming finishing agent being baked finishing technique and being applied to cellulose fibre/fabric using drying is padded.Antiflaming finishing agent of the present invention is raw materials used environmentally protective, and finishing technique is simple to operation, and any substance done harm to human body and environmental toxic will not be generated during operating process and use.Cellulose fibre/fabric of collated mistake has excellent flame retardant property and good wash durability, has extensive market application foreground.
Description
Technical field
The present invention relates to organic syntheses and textile engineering technical field, and in particular to a kind of phosphorus-nitrogen containing antiflaming finishing agent
And the preparation method of flame retardant cellulose fiber fabric.
Background technology
Cellulose fibre (such as cotton fiber) is most common, the widest natural fiber in source.Cellulose fibre has good
Good sucting wet air permeability and comfortable and easy to wear and recyclability and be widely used in the fields such as clothes, decoration.However, fiber
The limit oxygen index of cellulose fiber only has 17%, belongs to combustible material.At present, many industries are proposed for the flame retardant rating of textile
Increasingly higher demands, in order to assign cellulose fibre good flame retardant property, widen its application field, both at home and abroad it is many specially
Family scholar has conducted intensive studies cellulose fibre/fabrics flame resistance.
Traditional halogenated flame retardant is considered as efficient cellulose fire retardant, but halogenated flame retardant is using process
The toxic and corrosive substance of middle release makes it gradually be used by limitation.Instead halogen-free flame retardants.Halogen-free flame retardants
Mainly comprising phosphate, phosphate, phosphorus-nitrogen compound, phosphorus silicon compound, nitrogen silicon compound, silicon boron compound etc..Wherein, phosphorus nitrogen
System fire retardant is most effective cellulose fire retardant.At present, the cellulose of industrialization is with phosphorus nitrogen flame-proof finishing process
Pyrovatex CP techniques, using N- methylols -3- (dimethoxy phosphono) propionamides and crosslinking agent under acid catalysis with
Cellulose crosslinks reaction, obtains durable flame-retardant cotton fabric.But it is collated after fabric during storage and use
Free formaldehyde can be released.To find a kind of nontoxic halogen-free flame retardants, Chinese patent CN1362413A utilizes melamine and phosphorus
Acid etc. prepares a kind of melamine phosphate fire retardant, among the high molecular materials such as various thermoplasticity and thermosetting property, obtains
Good durable flame-proof material, however solubility is minimum in water is unfavorable for native cellulose and regenerated cellulose for prepared product
Fire-retardant application.
In conclusion the present invention devises the preparation side of a kind of phosphorus-nitrogen containing antiflaming finishing agent and flame retardant cellulose fiber fabric
Method.
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 phosphorus-nitrogen containing antiflaming finishing agent and resistance
The preparation method of cellulose base fiber fabric is fired, antiflaming finishing agent preparation process is simple and feasible, during preparation process and use
Release without noxious material.Obtained flame retardant cellulose fiber/fabric, excellent fireproof performance, wash durability are good.This hair
Bright prepared antiflaming finishing agent can reach raising cellulose fibre/flame retardant property of fabric, wash durability, and green simultaneously
The requirement of environmental protection.
To achieve these goals, the present invention is to realize by the following technical solutions:A kind of phosphorus-nitrogen containing flame-proof treatment
Agent includes the raw material of following weight proportion:Flame-retardant composition 20%, crosslinking agent 6%, water 74%.
The flame-retardant composition is phytic acid ammonium and urea.
The crosslinking agent is dicyandiamide, the one or more in guanidine carbonate, urea, melamine.
The synthesis of phytic acid ammonium in the flame-retardant composition it is raw materials used for phosphorus-containing compound phytic acid with nitrogenous compound such as
Urea, ammonium hydroxide, thiocarbamide, hydrazine hydrate, thiosemicarbazides, two amido thiocarbamides, ethylenediamine, diethylenetriamine, triethylene tetramine, ethyl alcohol
One kind in amine, azanol, diethanol amine, dimethylaminoethanol.
The synthesis technology step and condition of phytic acid ammonium in the flame-retardant composition be:First phytic acid and nitrogenous compound are pressed
Molar ratio is 1:6~12 proportioning is added in reactor, under the conditions of 30~100 DEG C reaction 3~12 it is small when, be made it is fire-retardant into
Divide phytic acid ammonium.
A kind of cellulose base fiber fabric for cotton, fiber crops, bamboo fibre, viscose rayon, copper ammonia fiber cellulose fiber,
Lyocell fiber and ionic liquid spin one kind in cellulose fibre/fabric.
A kind of cellulose base fiber fabric flame-retardant finishing method, comprises the following steps:Flame-proof treatment, which uses, pads-does
Dry-baking, wherein padding in step, dressing liquid temperature is room temperature~70 DEG C, and soaking time is 10~120 minutes;It is described
In drying steps, drying temperature is 80~150 DEG C, and drying time is 5~15 minutes;Described to bake in step, baking temperature is
160~200 DEG C, the time is baked as 2~20 minutes.
Described pad in step soaks two roll process using two, and immersion liquid rate is 80~150%.
The invention has the advantages that:By the present invention in that it is prepared by the use of phytic acid as raw material with nitrogenous compound fire-retardant
Agent phytic acid ammonium, phytic acid are a kind of natural materials of high phosphorus content, and will not generate any has human body and environment in use
Noxious material, avoiding problems in widely used fire retardant processing procedure in the market discharge noxious material the defects of.In addition,
It is fine which solves many flame-proof treatments since the special construction of phytic acid and its ammonium salt makes it form chemical bond with cellulose fibre
The problem of dimension/fabric is not water-fastness solves the problems, such as flame retardant cellulose fiber/fabric durability.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, with reference to
Specific embodiment, the present invention is further explained.
Present embodiment uses following technical scheme:A kind of novel phosphorus-containing nitrogen antiflaming finishing agent, including following weight
The raw material of proportioning:Flame-retardant composition 20%, crosslinking agent 6%, water 74%.The flame-retardant composition is phytic acid ammonium and urea.Described
Crosslinking agent is dicyandiamide, guanidine carbonate, urea, melamine one kind therein.The synthesis institute of phytic acid ammonium in the flame-retardant composition
It is phosphorus-containing compound phytic acid and nitrogenous compound with raw material, such as urea, ammonium hydroxide, thiocarbamide, hydrazine hydrate, thiosemicarbazides, two amido sulphur
One kind in urea, ethylenediamine, diethylenetriamine, triethylene tetramine, ethanolamine, azanol, diethanol amine, dimethylaminoethanol.
The preparation method of the antiflaming finishing agent comprises the following steps:First using phytic acid and nitrogenous compound as Material synthesis
Fire retardant phytic acid ammonium;Secondly it is the fire retardant phytic acid ammonium of synthesis is soluble in water, add in a certain amount of urea, dicyandiamide is made into accordingly
The antiflaming finishing agent of concentration;Finally ,-dry-by antiflaming finishing agent using padding bake finishing technique be applied to cellulose fibre/
The flame-proof treatment of fabric.
Embodiment 1
In the present embodiment, the preparation of antiflaming finishing agent and the flame-proof treatment of cellulose base fiber fabric are as follows:
1st, 400 grams of the plant acid solution that mass fraction is 70% is weighed, is poured into 2 equipped with mechanical agitator and thermometer
It rises in reaction kettle;151 grams of urea is weighed to be poured slowly among reaction kettle;Start blender, automatically controlled heating, when temperature rises to 90 DEG C
When, to get fire retardant phytic acid ammonium when sustained response 5 is small;
2nd, the 150 grams and 50 grams urea of phytic acid ammonium obtained in step 1 are weighed, 50 grams of dicyandiamides are dissolved in 0.75 liter of water
In, it is sufficiently stirred and obtains antiflaming finishing agent;
3rd, 1 kilogram of Lyocell fiber fabric is impregnated in the fire retarding treating liquid described in step 2,90 points is impregnated at 50 DEG C
Clock afterwards suppresses Lyocell fiber fabric with double roll press, and two leachings two are rolled, and the pick-up rate for making Lyocell fiber fabric is
150%, it is then 15 minutes dry in 80 DEG C, 20 minutes are baked then at 160 DEG C to get to flame-retardant Lyocell fiber fabric.
Embodiment 2
In the present embodiment, the preparation of antiflaming finishing agent and the flame-proof treatment of cellulose fibre/fabric concretely comprise the following steps:
1st, 400 grams of the plant acid solution that mass fraction is 70% is weighed, is poured into 2 equipped with mechanical agitator and thermometer
It rises in reaction kettle;154 grams of the hydrazine hydrate that mass fraction is 80% is weighed to be poured slowly among reaction kettle;Blender is started, it is automatically controlled
Heating, when temperature rises to 50 DEG C, to get fire retardant phytic acid ammonium when sustained response 5 is small;
2nd, the 140 grams and 60 grams urea of phytic acid ammonium obtained in step 1 are weighed, 50 grams of dicyandiamides are dissolved in 0.75 liter of water
In, it is sufficiently stirred and obtains antiflaming finishing agent;
3rd, 1 kilogram of cotton fabric is impregnated in the fire retarding treating liquid described in step 2, is impregnated 60 minutes at 70 DEG C, it
Cotton fabric is suppressed with double roll press afterwards, two leachings two are rolled, and the pick-up rate for making cotton fabric is 120%, then in 100 DEG C
Dry 10 minutes, 5 minutes are baked then at 180 DEG C to get to flame-retardant cotton fiber fabric.
Embodiment 3
In the present embodiment, the preparation of antiflaming finishing agent and the flame-proof treatment of cellulose fibre/fabric concretely comprise the following steps:
1st, 400 grams of the plant acid solution that mass fraction is 70% is weighed, is poured into 2 equipped with mechanical agitator and thermometer
It rises in reaction kettle;352 grams of the ammonium hydroxide that mass fraction is 25% is weighed to be poured slowly among reaction kettle;Blender is started, it is automatically controlled to add
Heat, when temperature rises to 40 DEG C, to get fire retardant phytic acid ammonium when sustained response 2 is small;
2nd, the 160 grams and 40 grams urea of phytic acid ammonium obtained in step 1 are weighed, 50 grams of dicyandiamides are dissolved in 0.75 liter of water
In, it is sufficiently stirred and obtains antiflaming finishing agent;
3rd, 1 kilogram of viscose fiber fabric is impregnated in the fire retarding treating liquid described in step 2, is impregnated 120 minutes at 60 DEG C,
Viscose fiber fabric is suppressed with double roll press afterwards, two leachings two are rolled, and the pick-up rate for making viscose fiber fabric is 100%, then
It is 8 minutes dry in 120 DEG C, 2 minutes are baked then at 190 DEG C to get to flame retardant viscose fabric.
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 (8)
1. a kind of phosphorus-nitrogen containing antiflaming finishing agent, which is characterized in that include the raw material of following weight proportion:Flame-retardant composition 20% is handed over
Join agent 6%, water 74%.
2. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 1, which is characterized in that the flame-retardant composition is phytic acid
Ammonium and urea.
3. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 1, which is characterized in that the crosslinking agent is double cyanogen
One or more in amine, guanidine carbonate, urea, melamine.
4. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 1,2, which is characterized in that in the flame-retardant composition
The raw materials used synthesis of phytic acid ammonium is phosphorus-containing compound phytic acid and nitrogenous compound such as urea, ammonium hydroxide, thiocarbamide, hydrazine hydrate, amino
Thiocarbamide, two amido thiocarbamides, ethylenediamine, diethylenetriamine, triethylene tetramine, ethanolamine, azanol, diethanol amine, dimethylamino second
One kind in alcohol.
5. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 2, the synthesis technology step and item of the phytic acid ammonium
Part is:It is first 1 in molar ratio by phytic acid and nitrogenous compound:6~12 proportioning is added in reactor, in 30~100 DEG C of items
When reaction 3~12 is small under part, flame-retardant composition phytic acid ammonium is made.
6. a kind of cellulose base fiber fabric, which is characterized in that the cellulose base fiber fabric is cotton, fiber crops, bamboo fibre, viscose glue fibre
Dimension, copper ammonia fiber cellulose fiber, lyocell fiber and ionic liquid spin one kind in cellulose base fiber fabric.
7. a kind of cellulose base fiber fabric flame-retardant finishing method, which is characterized in that comprise the following steps:Flame-proof treatment is using leaching
- baking is rolled-dries, wherein padding in step, dressing liquid temperature is room temperature~70 DEG C, and soaking time is 10~120 minutes;
In the drying steps, drying temperature is 80~150 DEG C, and drying time is 5~15 minutes;It is described to bake in step, bake temperature
It spends for 160~200 DEG C, bakes the time as 2~20 minutes.
8. a kind of cellulose base fiber fabric flame-retardant finishing method according to claim 7, which is characterized in that described to pad step
Two roll process are soaked using two in rapid, immersion liquid rate is 80~150%.
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Cited By (21)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109183409A (en) * | 2018-08-16 | 2019-01-11 | 重庆消防安全技术研究服务有限责任公司 | The method and flame retardant viscose fiber of melamine grafting oxidation viscose rayon preparation flame retardant viscose fiber |
CN110016130A (en) * | 2019-04-01 | 2019-07-16 | 东华大学 | The preparation method of phosphorus, nitrogen type flame retardant and flame-retardant textile based on hyper-branched polyester |
CN110055755A (en) * | 2019-05-09 | 2019-07-26 | 盐城工学院 | A kind of method for sorting of providing cotton fabric flame-proof antibiotic effect |
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 |
CN111484647A (en) * | 2019-01-29 | 2020-08-04 | 马德里高等材料研究院 | Halogen-free phosphorus-containing flame retardant, preparation method thereof and bio-based halogen-free flame-retardant polylactic acid material prepared from halogen-free phosphorus-containing flame retardant |
CN111910432A (en) * | 2020-08-18 | 2020-11-10 | 上海婉静纺织科技有限公司 | Antibacterial fabric and preparation method thereof |
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 |
CN112553705A (en) * | 2020-12-09 | 2021-03-26 | 赛得利(福建)纤维有限公司 | Preparation method of flame-retardant viscose fibers |
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 |
CN112961253A (en) * | 2021-02-20 | 2021-06-15 | 南通纺织丝绸产业技术研究院 | Method for flame-retardant modification of microcrystalline cellulose by phytic acid |
CN113215859A (en) * | 2021-05-11 | 2021-08-06 | 安徽工程大学 | Simple, convenient, efficient and environment-friendly preparation method of flame-retardant office paper |
CN113322676A (en) * | 2021-05-27 | 2021-08-31 | 安徽工程大学 | Biomass-based environment-friendly washable flame retardant PD flame-retardant finished fabric and preparation method thereof |
CN113861298A (en) * | 2021-09-01 | 2021-12-31 | 青岛科技大学 | Phosphorus-nitrogen-containing cellulose bio-based flame retardant and preparation method thereof |
CN114293373A (en) * | 2022-01-13 | 2022-04-08 | 内蒙古工业大学 | Durable flame-retardant non-ironing finishing liquid and finishing method |
CN115573170A (en) * | 2022-12-09 | 2023-01-06 | 江苏恒力化纤股份有限公司 | Preparation method of flame-retardant polyester/cotton blended fabric |
CN115652642A (en) * | 2022-12-09 | 2023-01-31 | 江苏恒力化纤股份有限公司 | Preparation method of flame-retardant durable polyester/cotton blended fabric |
CN115897287A (en) * | 2022-10-11 | 2023-04-04 | 天津科技大学 | Washable flame-retardant material and preparation method and application thereof |
CN116283129A (en) * | 2023-02-10 | 2023-06-23 | 桐庐奔腾建材制品有限公司 | Composite fiber modified concrete and preparation method thereof |
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CN116641231A (en) * | 2023-05-19 | 2023-08-25 | 苏州大学 | Multi-active-group reactive flame retardant and application thereof to durable flame-retardant finishing of protein fiber products |
CN116905110A (en) * | 2023-07-19 | 2023-10-20 | 佛山市别藏科技发展有限公司 | Flame-retardant fabric and preparation method thereof |
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CN109183409A (en) * | 2018-08-16 | 2019-01-11 | 重庆消防安全技术研究服务有限责任公司 | The method and flame retardant viscose fiber of melamine grafting oxidation viscose rayon preparation flame retardant viscose fiber |
CN111484647A (en) * | 2019-01-29 | 2020-08-04 | 马德里高等材料研究院 | Halogen-free phosphorus-containing flame retardant, preparation method thereof and bio-based halogen-free flame-retardant polylactic acid material prepared from halogen-free phosphorus-containing flame retardant |
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CN110055755A (en) * | 2019-05-09 | 2019-07-26 | 盐城工学院 | A kind of method for sorting of providing cotton fabric flame-proof antibiotic effect |
CN110055755B (en) * | 2019-05-09 | 2021-11-12 | 盐城工学院 | Finishing method for endowing cotton fabric with flame-retardant and antibacterial effects |
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CN111910432B (en) * | 2020-08-18 | 2022-09-02 | 浙江跃嘉纺织科技有限公司 | Antibacterial fabric and preparation method thereof |
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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 |
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CN113215859B (en) * | 2021-05-11 | 2023-11-10 | 安徽工程大学 | Simple, efficient and environment-friendly preparation method of flame-retardant office paper |
CN113215859A (en) * | 2021-05-11 | 2021-08-06 | 安徽工程大学 | Simple, convenient, efficient and environment-friendly preparation method of flame-retardant office paper |
CN113322676A (en) * | 2021-05-27 | 2021-08-31 | 安徽工程大学 | Biomass-based environment-friendly washable flame retardant PD flame-retardant finished fabric and preparation method thereof |
CN113861298A (en) * | 2021-09-01 | 2021-12-31 | 青岛科技大学 | Phosphorus-nitrogen-containing cellulose bio-based flame retardant and preparation method thereof |
CN114293373A (en) * | 2022-01-13 | 2022-04-08 | 内蒙古工业大学 | Durable flame-retardant non-ironing finishing liquid and finishing method |
CN115897287A (en) * | 2022-10-11 | 2023-04-04 | 天津科技大学 | Washable flame-retardant material and preparation method and application thereof |
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