CN107326647B - A kind of preparation method of fire-retardant dust-proof stephanoporate polyamide fibrous composite - Google Patents
A kind of preparation method of fire-retardant dust-proof stephanoporate polyamide fibrous composite Download PDFInfo
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- CN107326647B CN107326647B CN201710689005.3A CN201710689005A CN107326647B CN 107326647 B CN107326647 B CN 107326647B CN 201710689005 A CN201710689005 A CN 201710689005A CN 107326647 B CN107326647 B CN 107326647B
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- stephanoporate polyamide
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- stephanoporate
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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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/265—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from at least two different diamines or at least two different dicarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
-
- 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
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of preparation methods of fire-retardant dust-proof stephanoporate polyamide fibrous composite, polyethylene glycol is added in Fypro preparation process and forms porous structure, and porous graphene powder is added, it stirs evenly, it is then transferred into spinning in spinning machine and obtains Fypro, filtering is boiled into polyamide ethyl alcohol immersion, then is filtered through boiling pure water, stephanoporate polyamide fiber has been obtained；Gained stephanoporate polyamide fiber is immersed in super-hydrophobic automatic cleaning clear dope 5-10 minutes, it is then centrifuged for filter 23-10 minutes, it has been centrifugated the stephanoporate polyamide fiber of super-hydrophobic automatic cleaning clear dope, it is drying to obtain fire-retardant dust-proof stephanoporate polyamide fibrous composite, the dust-proof stephanoporate polyamide fibrous composite of obtained flame-retardant has good dust-proof, fire-retardant, insulative properties, can be used as multi-functional high quality cloth textile.
Description
Technical field
The present invention relates to a kind of preparation methods of fire-retardant dust-proof stephanoporate polyamide fibrous composite, belong to textile fabric skill
Art field.
Background technique
The synthetic fibers that Fypro is as a kind of good hand touch, wearability is good, color fastness is done are widely used in weaving row
Industry.With scientific and technological progress, higher and higher, such as heat insulation property, dust tightness, anti-is also required the multifunctionality of textile fabric at present
Fire, the performance of existing Fypro in these areas are unsatisfactory.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of fire-retardant dust-proof stephanoporate polyamide fibrous composite, in polyamides
Pore former and porous graphene are added in amine fiber, are obtained the stephanoporate polyamide fiber with flame-retarding characteristic, are then carried out super thin
Water is modified, changes the surface contact angle of stephanoporate polyamide fiber, it is made to have good dust tightness.
The present invention is realized by following technical proposals.A kind of fire-retardant dust-proof stephanoporate polyamide fibrous composite
Preparation method, its step are as follows:
(1) decamethylene diamine is added to dissolution in ethyl alcohol together with butanediamine and obtains solution A, decanedioic acid and itaconic acid are added
Into ethyl alcohol, dissolution obtains solution B, and solution A is mixed with solution B, and reaction 20 minutes, cooling knot are stirred at 50-60 DEG C
Brilliant, washing is dried to obtain amidic-salt；
(2) under nitrogen protection, be added to polyethylene glycol as pore former in dimethyl acetamide, after mixing plus
Enter into amidic-salt prepared by step (1), heating melting, sufficiently obtain copolyamide fluid after reaction, is then added more
Hole graphene powder, stirs evenly, and is then transferred into spinning in spinning machine and obtains Fypro, which is soaked with ethyl alcohol
Bubble boils filtering, then filters through boiling pure water, has dissolved polyethylene glycol in this way, has obtained stephanoporate polyamide fiber；
(3) stephanoporate polyamide fiber obtained by step (2) is immersed in super-hydrophobic automatic cleaning clear dope 5-10 minutes, so
Centrifugal filtration 3-10 minutes afterwards, it is centrifugated the stephanoporate polyamide fiber of super-hydrophobic automatic cleaning clear dope, then certainly
It so dries or 40-50 DEG C of drying is to get fire-retardant dust-proof stephanoporate polyamide fibrous composite.
Further, in step (3), super-hydrophobic automatic cleaning clear dope super-hydrophobic automatic cleaning clear dope is needed before use
Dispersed with ultrasonic wave, and in stephanoporate polyamide fiber soaking process, continual ultrasonic wavelength-division dissipate, allow coating molecule into
It in the gap for entering stephanoporate polyamide fiber, is preferably adsorbed on stephanoporate polyamide fiber, so that stephanoporate polyamide fiber has
High surface contact angle, has dirt exclusion capabilities.
Further, in the step (2), the additional amount of porous graphene powder is the 1- of copolyamide fluid mass
3%.
Technical effect of the invention: pore former and porous graphene are added in Fypro preparation process, is had
Have the stephanoporate polyamide fiber of flame-retarding characteristic, pore former added during preparing Fypro, then dissolution removal at
Hole agent, so that Fypro is in porous structure, porous graphene powder is added in Fypro, not only enhances fiber
Intensity and toughness, improve mechanical mechanics property, and it is with flame-retarding characteristic.Then modifying super hydrophobicity is carried out, is changed porous
The surface contact angle of Fypro makes it have good dust tightness, because Fypro is in porous structure, and mixes
Miscellaneous porous graphene powder also has porosity characteristic, so that fiber has good absorption to super-hydrophobic automatic cleaning clear dope
Property, and auxiliary ultrasonic is dispersed, and fiber surface is allowed to adhere to super-hydrophobic automatic cleaning clear dope, porous polyamides well
Amine fiber is immersed in super-hydrophobic automatic cleaning clear dope and is centrifugated, by adjusting the adjustable fiber surface of centrifugation time
Paint thickness.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
Embodiment 1
6kg decamethylene diamine and 4kg butanediamine are weighed, is dissolved to obtain solution A with ethyl alcohol；6k decanedioic acid and 4kg itaconic acid are weighed,
It is dissolved to obtain solution B with ethyl alcohol, solution A is mixed with solution B, reaction 20 minutes is stirred at 60 DEG C, crystallisation by cooling is washed
It washs and is dried to obtain amidic-salt；
Weigh polyethylene glycol, dimethyl acetamide, amidic-salt, polyethylene glycol, dimethyl acetamide, the molar ratio of amidic-salt
Be added to polyethylene glycol as pore former in dimethyl acetamide under nitrogen protection for 4:15:25, after mixing plus
Enter into amidic-salt, heating melting, reacted 5 hours at 200 DEG C, sufficiently reaction after obtain copolyamide fluid, then plus
Enter porous graphene powder, the additional amount of porous graphene powder is the 1% of copolyamide fluid mass, stirs evenly, drops
Temperature is then transferred into spinning in spinning machine and obtains Fypro, filtering is boiled in polyamide ethyl alcohol immersion, then through pure water
Filtering is boiled, has dissolved polyethylene glycol in this way, finally vacuum drying has obtained stephanoporate polyamide fiber；
Gained stephanoporate polyamide fiber is immersed in super-hydrophobic automatic cleaning clear dope 5 minutes, filter 23 point is then centrifuged for
Clock has been centrifugated the stephanoporate polyamide fiber of super-hydrophobic automatic cleaning clear dope, and then naturally dry is up to fire-retardant anti-
Dirt stephanoporate polyamide fibrous composite.Super-hydrophobic automatic cleaning clear dope can use commercially available product, can also be according to existing
There is the open source literature of technology to prepare.Super-hydrophobic automatic cleaning clear dope super-hydrophobic automatic cleaning clear dope is needed before use with ultrasound
Wavelength-division dissipates, and in stephanoporate polyamide fiber soaking process, and continual ultrasonic wavelength-division dissipates, and coating molecule is entered porous
It in the gap of Fypro, is preferably adsorbed on stephanoporate polyamide fiber, so that stephanoporate polyamide fiber has high surface
Contact angle has dirt exclusion capabilities.
Embodiment 2
5kg decamethylene diamine and 5kg butanediamine are weighed, is dissolved to obtain solution A with ethyl alcohol；5k decanedioic acid and 5kg itaconic acid are weighed,
It is dissolved to obtain solution B with ethyl alcohol, solution A is mixed with solution B, reaction 20 minutes is stirred at 50 DEG C, crystallisation by cooling is washed
It washs and is dried to obtain amidic-salt；
Weigh polyethylene glycol, dimethyl acetamide, amidic-salt, polyethylene glycol, dimethyl acetamide, the molar ratio of amidic-salt
Be added to polyethylene glycol as pore former in dimethyl acetamide under nitrogen protection for 5:12:20, after mixing plus
Enter into amidic-salt, heating melting, reacted 8 hours at 200 DEG C, sufficiently reaction after obtain copolyamide fluid, then plus
Enter porous graphene powder, the additional amount of porous graphene powder is the 2% of copolyamide fluid mass, stirs evenly, drops
Temperature is then transferred into spinning in spinning machine and obtains Fypro, filtering is boiled in polyamide ethyl alcohol immersion, then through pure water
Filtering is boiled, has dissolved polyethylene glycol in this way, finally vacuum drying has obtained stephanoporate polyamide fiber；
Gained stephanoporate polyamide fiber is immersed in super-hydrophobic automatic cleaning clear dope 10 minutes, filtering 5 is then centrifuged for
Minute, be centrifugated the stephanoporate polyamide fiber of super-hydrophobic automatic cleaning clear dope, then 50 DEG C it is obtained by drying fire-retardant
Dust-proof stephanoporate polyamide fibrous composite.
Embodiment 3
6kg decamethylene diamine and 4kg butanediamine are weighed, is dissolved to obtain solution A with ethyl alcohol；5k decanedioic acid and 5kg itaconic acid are weighed,
It is dissolved to obtain solution B with ethyl alcohol, solution A is mixed with solution B, reaction 20 minutes is stirred at 55 DEG C, crystallisation by cooling is washed
It washs and is dried to obtain amidic-salt；
Weigh polyethylene glycol, dimethyl acetamide, amidic-salt, polyethylene glycol, dimethyl acetamide, the molar ratio of amidic-salt
Be added to polyethylene glycol as pore former in dimethyl acetamide under nitrogen protection for 4:12:22, after mixing plus
Enter into amidic-salt, heating melting, reacted 5 hours at 200 DEG C, sufficiently reaction after obtain copolyamide fluid, then plus
Enter porous graphene powder, the additional amount of porous graphene powder is the 3% of copolyamide fluid mass, stirs evenly, drops
Temperature is then transferred into spinning in spinning machine and obtains Fypro, filtering is boiled in polyamide ethyl alcohol immersion, then through pure water
Filtering is boiled, has dissolved polyethylene glycol in this way, finally vacuum drying has obtained stephanoporate polyamide fiber；
Gained stephanoporate polyamide fiber is immersed in super-hydrophobic automatic cleaning clear dope 8 minutes, filtering 10 is then centrifuged for
Minute, be centrifugated the stephanoporate polyamide fiber of super-hydrophobic automatic cleaning clear dope, then 40 DEG C it is obtained by drying fire-retardant
Dust-proof stephanoporate polyamide fibrous composite.
Performance detection is made to the product of embodiment 1-3, as a result as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Combustion phenomena | Not molten drop | Not molten drop | Not molten drop |
| Porosity (%) | 32 | 27 | 31 |
| Thermal coefficient (W/m*k) | 0.18 | 0.17 | 0.20 |
| Tensile strength (MPa) | 45.3 | 44.1 | 46.1 |
| Surface contact angle | 150° | 153° | 146° |
As seen from the above table, the fire-retardant dust-proof stephanoporate polyamide fibrous composite anti-flammability prepared by the present invention is high, heat-insulated
Property it is good, tensile strength is high, and surface contact angle is big, and dustproof and waterproof is good, and dust-proof key is exactly surface contact angle, surface contact angle
More, dust dirt is more difficult to be adsorbed on above.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In details described herein.
Claims (3)
1. a kind of preparation method of fire-retardant dust-proof stephanoporate polyamide fibrous composite, it is characterized in that steps are as follows:
(1) decamethylene diamine is added to dissolution in ethyl alcohol together with butanediamine and obtains solution A, decanedioic acid and itaconic acid are added to second
Dissolution obtains solution B in alcohol, and solution A is mixed with solution B, is stirred and reacts 20 minutes at 50-60 DEG C, crystallisation by cooling,
Washing is dried to obtain amide；
(2) under nitrogen protection, it is added to polyethylene glycol as pore former in dimethyl acetamide, is added to after mixing
In amide prepared by step (1), heating melting sufficiently obtains copolyamide fluid after reaction, porous graphite is then added
Alkene powder, stirs evenly, and is then transferred into spinning in spinning machine and obtains Fypro, and polyamide ethyl alcohol immersion is boiled
Filtering, then filtered through boiling pure water, polyethylene glycol has been dissolved in this way, has obtained stephanoporate polyamide fiber；
(3) stephanoporate polyamide fiber obtained by step (2) is immersed in super-hydrophobic automatic cleaning clear dope 5-10 minutes, then from
Heart filter 23-10 minutes has been centrifugated the stephanoporate polyamide fiber of super-hydrophobic automatic cleaning clear dope, has then been dried in the air naturally
Dry or 40-50 DEG C of drying is to get fire-retardant dust-proof stephanoporate polyamide fibrous composite.
2. the preparation method of the fire-retardant dust-proof stephanoporate polyamide fibrous composite of one kind according to claim 1, feature
Be: in step (3), super-hydrophobic automatic cleaning clear dope needs to be dispersed with ultrasonic wave before use, and in stephanoporate polyamide fiber
In soaking process, continual ultrasonic wavelength-division dissipates.
3. the preparation method of the fire-retardant dust-proof stephanoporate polyamide fibrous composite of one kind according to claim 1, feature
Be: in the step (2), the additional amount of the porous graphene powder is the 1-3% of copolyamide fluid mass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710689005.3A CN107326647B (en) | 2017-08-13 | 2017-08-13 | A kind of preparation method of fire-retardant dust-proof stephanoporate polyamide fibrous composite |
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| CN201710689005.3A CN107326647B (en) | 2017-08-13 | 2017-08-13 | A kind of preparation method of fire-retardant dust-proof stephanoporate polyamide fibrous composite |
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| CN107326647B true CN107326647B (en) | 2019-06-18 |
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| CN110438586B (en) * | 2018-05-04 | 2020-11-17 | 浙江大学 | Preparation method of super-hydrophobic porous fiber with oriented pore structure, product and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981635A (en) * | 2014-05-09 | 2014-08-13 | 浙江省纺织测试研究院 | Preparation method of porous fiber non-woven fabric |
| CN104562276A (en) * | 2014-12-05 | 2015-04-29 | 淮安锦纶化纤有限公司 | Method for modifying chinlon 6 fibers and modified product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103981635A (en) * | 2014-05-09 | 2014-08-13 | 浙江省纺织测试研究院 | Preparation method of porous fiber non-woven fabric |
| CN104562276A (en) * | 2014-12-05 | 2015-04-29 | 淮安锦纶化纤有限公司 | Method for modifying chinlon 6 fibers and modified product |
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