CN104594026B - A kind of fire resistance fibre and preparation method thereof - Google Patents
A kind of fire resistance fibre and preparation method thereof Download PDFInfo
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Abstract
The invention discloses fire resistance fibre of carbonization after a kind of burning and preparation method thereof, the fire resistance fibre is using the fiber of the fiber of phosphinylidyne-containing amine group and/or nitrile group as base material, through being obtained using the material of amido-containing group and/or oh group as cross-linked modifier is modified, its preparation method is as follows：The fiber base material is impregnated in the aqueous solution of the modifying agent and reacted under inert gas conditions, modified fiber is obtained.In order that modified fiber has more excellent fire resistance, methods described also includes being reacted the aqueous solution of alkali compounds and the aqueous solution of metal salt compound with the modified fiber, and product is washed with water to neutrality after terminating for reaction, is produced.Fire resistance fibre prepared by this method has excellent anti-flammability, and oxidation index is more than 28, and molten drop, does not shrink, free from extraneous odour, is the product of great use value.
Description
Technical field
The invention belongs to fire resistance fibre preparing technical field, and in particular to the fire resistance fibre and its system carbonized after a kind of burning
Preparation Method.
Background technology
Fire resistance fibre is the important kind of fiber art, and it plays vital work in the production of people, sphere of life
With in public places, the vehicles, sea-freight ships, the field such as Aero-Space be widely used.Fire resistance fibre is divided into two
Major class：Natural fire resistance fibre (such as wool, cashmere), artificial fire resistance fibre (chemical fibre).But natural fire resistance fibre is present using by season
Section influence (such as wool or cashmere are only suitable to use in winter), the shortcomings of snugness of fit is limited；It is fire-retardant in artificial fire resistance fibre to wash
There is molten drop phenomenon in synthetic fibre, flame-retardant acrylic fibre has high-temperature shrinkage and smoke neighbour suffocates；FRC low intensity, flame-retarding characteristic
Limited the shortcomings of, preferable flame retardant effect is not all reached.At present, countries in the world scientific and technical personnel have done substantial amounts of grind to fire resistance fibre
Study carefully work.Try hard to find the fire resistance fibre production method that fiber can be made directly to carbonize after burning, it is to avoid melt, go out after fiber burning
Now burn and scald phenomenon, its explore path see introductions repeatly, so far there are no maturation production technology and use achievement.
The content of the invention
For prior art and the deficiency of product, after a kind of excellent fireproof performance and burning
The fire resistance fibre directly carbonized.
Fire resistance fibre provided by the present invention is the warp using the fiber of phosphinylidyne-containing amine group and/or nitrile group as fiber base material
Obtained after modifier modification；Wherein, the modifying agent is the material containing amino and/or hydroxyl.
The fiber base material is chosen in particular from following at least one：Nylon (Fypro) and polyacrylonitrile fibre.
The modifying agent is selected from following at least one：The compound of amido-containing group and the compound of hydroxyl group.
The compound of the amido-containing group is chosen in particular from following at least one：Ammoniacal liquor, ethylenediamine, propane diamine, butanediamine,
Defend diamines, diamines, dicyandiamide, dimethylamine, N- (2- amino-ethyls) -1,2- ethylenediamines (DETA), triethylene tetramine (TETA)
Deng, the amino group number for 1 and more than.
The compound of the hydroxyl group is chosen in particular from following at least one：Ethanol, ethylene glycol, hexylene glycol, propyl alcohol, third
Glycol, glycerine and two amine alcohols etc., the number of the oh group for 1 and more than.
Fire resistance fibre provided by the present invention with charing combustion characteristics is prepared by following preparation methods.
It is another object of the present invention to provide a kind of preparation method of the fire resistance fibre directly carbonized after burning, including
Following steps：In an inert atmosphere, the fiber base material is impregnated in the aqueous solution of the modifying agent and reacted, changed
Fiber after property.
In above-mentioned preparation method, the gas in the inert atmosphere is nitrogen or carbon dioxide.
The line density of the fiber base material is 0.8dtex~5.5dtex.
The mass fraction of modifying agent is 5%~50%, preferably 15%~25% in the aqueous solution of the modifying agent.
The pH value of the aqueous solution of the modifying agent is 9~14, preferably 10~14, and the size of pH value is for modified effect shadow
Ring very big, the high modified effect of pH value is good, but can reduce fibre strength.The pH value of the aqueous solution of modifying agent is by improving modifying agent
Consumption reach.
The reaction is carried out in a kettle., and pressure is 0.1Mpa~0.5Mpa in the kettle of the reactor.
The temperature of the reaction is 80 DEG C~100 DEG C, and specially 90 DEG C~98 DEG C, the time is 2h~6h.
In addition, in order to accelerate reaction speed, the preparation method also includes adding into the reaction system before reaction triggering
The step of agent.
The initiator is peroxide, and the peroxide is chosen in particular from following at least one：Benzoyl peroxide and
Ammonium persulfate.
The peroxide is (0.1~1) with the mass ratio of the fiber base material：2500.
In order that modified fiber has more excellent fire resistance, the preparation method also includes to described modified
Fiber carry out following processing the step of：First reacted with the aqueous solution and the modified fiber of strongly alkaline compound,
Reaction product is obtained, then the aqueous solution of the reaction product and metal salt compound is reacted, after reaction terminates, by institute
Thing is obtained to be washed with water to neutral step.
The alkali compounds and metal salt compound, which rise, makes the modified fiber base material continue cross-linked graft
Act on, so that modified fiber base material has sufficient carboxylate groups, the fire-retardant work(of the modified fiber base material of enhancing
Energy.
The alkali compounds is chosen in particular from following at least one：NaOH, potassium hydroxide and magnesium hydroxide.
The mass fraction of strongly alkaline compound is 1%~10% in the aqueous solution of the alkali compounds.
The aqueous solution of the alkali compounds is 80 DEG C~98 with the reaction temperature that the modified fiber is reacted
DEG C, the reaction time is 2~3h.
The metal salt compound is chosen in particular from following at least one：Sodium carbonate, sodium acid carbonate, sodium sulphate, sulfurous acid
Hydrogen sodium and copper sulphate.
The mass fraction of metal salt compound is 1%~10% in the aqueous solution of the metal salt compound.
The reaction temperature that the aqueous solution of the reaction product and metal salt compound is reacted is 85 DEG C~100 DEG C,
Reaction time is 1~3h.
The aqueous solution of the alkali compounds is described anti-to impregnate with the addition of the aqueous solution of metal salt compound
The fiber base material in kettle is answered to be defined.
The number of times of the washing is 2~3 times.
The preparation-obtained fire resistance fibre of the present invention not only maintains fiber and had the special feature that in itself completely, has burning again
The characteristic carbonized afterwards, the fire resistance fibre has excellent anti-flammability, and limited oxygen index is more than 28, and molten drop, does not shrink, nothing
Peculiar smell, is the product of great use value.
Embodiment
The method of the present invention is illustrated below by specific embodiment, but the invention is not limited in this, it is all at this
Any modification, equivalent and improvement made within the spirit and principle of invention etc., should be included in the protection model of the present invention
Within enclosing.
Experimental method described in following embodiments, unless otherwise specified, is conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
The number of spent material is mass parts in following examples.The product test method of following examples is：Oxygen index (OI)
Carried out with combustion characteristic with reference to G3/T5454-1997.
Embodiment one：Prepare the fire resistance fibre directly carbonized after burning and its performance test
(1) fire resistance fibre directly carbonized after burning is prepared：
1st, the ㎏ of polyacrylonitrile fibre 500 that line density is 1.5dtex is weighed.
2nd, take two amine alcohol 600kg and pure water to be made into the aqueous solution that mass fraction is 15%, add in dyeing and finishing kettle, take 100
Gram benzoyl peroxide is added in dyeing and finishing kettle, and the pH value for keeping whole system is 10.
3rd, the polypropylene fibre in step 1 is added in the dyeing and finishing kettle in step 2, is fully warming up to 105 degree after submergence,
Start circulating pump.
4th, be filled with dyeing and finishing kettle nitrogen keep dyeing and finishing kettle in pressure in 0.1Mpa.
5th, circulate 5 hours, release raffinate.
6th, solid content is prepared to add in dyeing and finishing kettle for 5% sodium hydrate aqueous solution, not have fiber to be defined, 80 degree of circulations
3 hours, raffinate is released, is washed 3 times.
7th, the sodium bicarbonate solution that solid content is 5% is prepared, is added in dyeing and finishing kettle not have fiber to be defined, in 90 degree of circulations
2 hours, raffinate is released, 2 times is washed to neutral, discharges and produce required product.
(2) performance test：
The oxygen index (OI) for measuring the fire resistance fibre directly carbonized after burning using the methods of G3/T5454-1997 is 30, fire-retardant fibre
Carbonized completely after dimension burning, fire resistance fibre not molten drop, does not shrink in combustion process, free from extraneous odour is produced.
Embodiment two：Prepare the fire resistance fibre directly carbonized after burning and its performance test
(1) fire resistance fibre directly carbonized after burning is prepared：
1st, the ㎏ of nylon fiber 500 that line density is 1.5dtex is weighed.
2nd, take the ㎏ of triethylene tetramine 800 and pure water to be made into the solution that mass fraction is 20%, add in dyeing and finishing kettle, take 20
Gram ammonium persulfate is added in dyeing and finishing kettle, and the pH value for keeping whole system is 10.
3rd, the nylon fiber in step 1 is added in the dyeing and finishing kettle in step 2, fully protection is warming up to 90 after submergence
Degree, starts circulating pump.
4th, be filled with dyeing and finishing kettle nitrogen keep dyeing and finishing kettle in pressure in 0.2Mpa.
5th, circulate 5 hours, release raffinate.
6th, the potassium hydroxide aqueous solution for preparing solid content 10% is added in dyeing and finishing kettle, not have fiber to be defined, is followed at 95 degree
Ring 2 hours, releases raffinate, washes 2 times.
7th, the sodium sulfite solution that solid content is 10% is prepared, adds in dyeing and finishing kettle not have fiber to be defined, is followed at 85 degree
Ring 1 hour, releases raffinate, washes 2 times to neutral, discharges and produce required product.
(2) performance test：
The oxygen index (OI) for measuring the fire resistance fibre directly carbonized after burning using the methods of G3/T5454-1997 is 29, fire-retardant fibre
Carbonized completely after dimension burning, fire resistance fibre not molten drop, does not shrink in combustion process, free from extraneous odour is produced.
Embodiment three：Prepare the fire resistance fibre directly carbonized after burning and its performance test
(1) fire resistance fibre directly carbonized after burning is prepared：
1st, the ㎏ of polyacrylonitrile fibre 500 that line density is 1.5dtex is weighed.
2nd, take the ㎏ of diamines 800 and pure water to be made into the solution that mass fraction is 25%, add in dyeing and finishing kettle, take 200 grams
Potassium peroxydisulfate is added in dyeing and finishing kettle, and the pH value for keeping whole system is 13.
3rd, the polypropylene fibre in step 1 is added in the dyeing and finishing kettle in step 2, fully protects and be warming up to after submergence
102 degree, start circulating pump.
4th, be filled with dyeing and finishing kettle nitrogen keep dyeing and finishing kettle in pressure in 0.3Mpa.
5th, circulate 6 hours, release raffinate.
6th, the magnesium hydroxide aqueous solution for preparing solid content 8% is added in dyeing and finishing kettle, not have fiber to be defined, in 92 degree of circulations
2 hours, raffinate is released, is washed 3 times.
7th, the solution of sodium bisulfite that solid content is 9% is prepared, is added in dyeing and finishing kettle not have fiber to be defined, 85 degree of circulations
1 hour, raffinate is released, 2 times is washed to neutral, discharges and produce required product.
(2) performance test：
The oxygen index (OI) for measuring the fire resistance fibre directly carbonized after burning using the methods of G3/T5454-1997 is 34, fire-retardant fibre
Carbonized completely after dimension burning, fire resistance fibre not molten drop, does not shrink in combustion process, free from extraneous odour is produced.
Example IV：Prepare the fire resistance fibre directly carbonized after burning and its performance test
(1) fire resistance fibre with charing combustion characteristics is prepared：
1st, the ㎏ of polyacrylonitrile fibre 500 that line density is 1.5dtex is weighed.
2nd, take the ㎏ of hexylene glycol 200, the ㎏ of ethylenediamine 600 and pure water to be made into the solution that mass fraction is 25%, add dyeing and finishing
In kettle, 120 grams of potassium peroxydisulfates are taken to add in dyeing and finishing kettle, the pH value for keeping whole system is 11.
3rd, the polypropylene fibre in step 1 is added in the dyeing and finishing kettle in step 2, fully protects and be warming up to after submergence
108 degree, start circulating pump.
4th, be filled with dyeing and finishing kettle nitrogen keep dyeing and finishing kettle in pressure in 0.2Mpa.
5th, circulate 6 hours, release raffinate.
6th, the sodium hydrate aqueous solution for preparing solid content 5% is added in dyeing and finishing kettle, not have fiber to be defined, in 90 degree of circulations
2 hours, raffinate is released, is washed 2 times.
7th, the solution of sodium bisulfite that solid content is 4% is prepared, is added in dyeing and finishing kettle not have fiber to be defined, 95 degree of circulations
2 hours, raffinate is released, 3 times is washed to neutral, discharges and produce required product.
(2) performance test：
The oxygen index (OI) for measuring the fire resistance fibre directly carbonized after burning using the methods of G3/T5454-1997 is 30, fire-retardant fibre
Carbonized completely after dimension burning, fire resistance fibre not molten drop, does not shrink in combustion process, free from extraneous odour is produced.
Embodiment five：Prepare the fire resistance fibre with charing combustion characteristics and its performance test
(1) fire resistance fibre with charing combustion characteristics is prepared：
1st, the ㎏ of polyacrylonitrile fibre 500 that line density is 1.5dtex is weighed.
2nd, take the ㎏ of propyl alcohol 100, the ㎏ of dicyandiamide 600 and pure water to be made into the solution that mass fraction is 20%, add dyeing and finishing kettle
In, take 80 grams of benzoyl peroxides to add in dyeing and finishing kettle, the pH value for keeping whole system is 12.
3rd, the polypropylene fibre in step 1 is added in the dyeing and finishing kettle in step 2, fully protection is warming up to 95 after submergence
Degree, starts circulating pump.
4th, be filled with dyeing and finishing kettle nitrogen keep dyeing and finishing kettle in pressure in 0.2Mpa.
5th, circulate 3 hours, release raffinate.
6th, the magnesium hydroxide aqueous solution for preparing solid content 6% is added in dyeing and finishing kettle, not have fiber to be defined, in 90 degree of circulations
3 hours, raffinate is released, is washed 3 times.
7th, the copper-bath that solid content is 10% is prepared, is added in dyeing and finishing kettle not have fiber to be defined, 90 degree of circulations 1 are small
When, raffinate is released, 2 times is washed to neutral, discharges and produce required product.
(2) performance test：
The oxygen index (OI) for measuring the fire resistance fibre directly carbonized after burning using the methods of G3/T5454-1997 is 32, fire-retardant fibre
Carbonized completely after dimension burning, fire resistance fibre not molten drop, does not shrink in combustion process, free from extraneous odour is produced.
Embodiment six：Prepare the fire resistance fibre directly carbonized after burning and its performance test
(1) fire resistance fibre directly carbonized after burning is prepared：
1st, the ㎏ of nylon fiber 500 that line density is 1.5dtex is weighed.
2nd, take the ㎏ of dimethylamine 800 and pure water to be made into the solution that mass fraction is 15%, add in dyeing and finishing kettle, take 100 grams
Potassium peroxydisulfate is added in dyeing and finishing kettle, and the pH value for keeping whole system is 14.
3rd, the nylon fiber in step 1 is added in the dyeing and finishing kettle in step 2, fully protection is warming up to 100 after submergence
Degree, starts circulating pump.
4th, be filled with dyeing and finishing kettle nitrogen keep dyeing and finishing kettle in pressure in 0.3Mpa.
5th, circulate 6 hours, release raffinate.
6th, the potassium hydroxide aqueous solution for preparing solid content 2% is added in dyeing and finishing kettle, not have fiber to be defined, in 93 degree of circulations
3 hours, raffinate is released, is washed 3 times.
7th, the solution of sodium bisulfite that solid content is 10% is prepared, is added in dyeing and finishing kettle not have fiber to be defined, 90 degree are followed
Ring 3 hours, releases raffinate, washes 2 times to neutral, discharges and produce required product.
(2) performance test：
The oxygen index (OI) for measuring the fire resistance fibre directly carbonized after burning using the methods of G3/T5454-1997 is 36, fire-retardant fibre
Carbonized completely after dimension burning, fire resistance fibre not molten drop, does not shrink in combustion process, free from extraneous odour is produced.
Claims (7)
1. a kind of preparation method of fire resistance fibre, comprises the following steps：In an inert atmosphere, with phosphinylidyne-containing amine group and/or itrile group
The fiber of group is fiber base material, and the fiber base material is impregnated in the aqueous solution of modifying agent reacted, and obtains fire-retardant
Fiber；
The modifying agent be selected from it is following 1) or 2)：
1) compound of amido-containing group；
2) compound of the compound of amido-containing group and hydroxyl group；
The compound of the amido-containing group is selected from following at least one：Ammoniacal liquor, ethylenediamine, propane diamine, butanediamine, defend diamines,
Diamines, dicyandiamide, dimethylamine, N- (2- amino-ethyls) -1,2- ethylenediamines, triethylene tetramine and triethylene amine；
The compound of the hydroxyl group is selected from following at least one：Ethanol, ethylene glycol, hexylene glycol, propyl alcohol, propane diols, third
Triol and two amine alcohols；
The reaction is carried out in a kettle., and pressure is 0.1Mpa~0.5Mpa in the kettle of the reactor；
The temperature of the reaction is 80 DEG C~100 DEG C, and the time is 2h~6h；
The step of methods described also includes carrying out following processing to the modified fiber：First use the aqueous solution of alkali compounds
Reacted with the modified fiber, obtain reaction product, then by the water of the reaction product and metal salt compound
Solution is reacted, after reaction terminates, and gains are washed with water to neutral step；
The alkali compounds is selected from following at least one：NaOH and potassium hydroxide；
The percent concentration of the aqueous solution neutral and alkali compound of the alkali compounds is 1%~10%；
The metal salt compound is selected from following at least one：Sodium carbonate, sodium acid carbonate, sodium sulphate, sodium hydrogensulfite and sulphur
Sour copper；
The percent concentration of metal salt compound is 1%~10% in the aqueous solution of the metal salt compound.
2. preparation method according to claim 1, it is characterised in that：Gas in the inert atmosphere is nitrogen；
The fiber base material is selected from following at least one：Fypro and polyacrylonitrile fibre；
The line density of the fiber base material is 0.8dtex~5.5dtex.
3. preparation method according to claim 1 or 2, it is characterised in that：Modifying agent in the aqueous solution of the modifying agent
Mass fraction is 5%~50%；
The pH value of the aqueous solution of the modifying agent is 9~14, but does not include 9.
4. preparation method according to claim 1 or 2, it is characterised in that：The preparation method also includes to before reaction
The step of initiator being added in reaction system；
The initiator is peroxide, and the peroxide is selected from following at least one：Benzoyl peroxide and ammonium persulfate；
The peroxide is (0.1~1) with the mass ratio of the fiber base material：2500.
5. preparation method according to claim 1, it is characterised in that：The aqueous solution of the alkali compounds and the modification
The reaction temperature that fiber afterwards is reacted is 80 DEG C~100 DEG C, and the reaction time is 2~3h.
6. preparation method according to claim 1, it is characterised in that：The water of the reaction product and metal salt compound
The reaction temperature that solution is reacted is 85 DEG C~100 DEG C, and the reaction time is 1~4h；
The number of times of the washing is 2~3 times.
7. the fire resistance fibre that the preparation method any one of claim 1-6 is prepared.
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| CN105386292B (en) * | 2015-12-16 | 2017-06-09 | 湖南科技大学 | A kind of method of modifying of collagenous fibres |
| EP3417006B1 (en) * | 2016-02-19 | 2024-11-27 | Metis Technologies Pty Ltd | Flame-retardant acrylonitrile polymer for fibre manufacture |
| CN105780187A (en) * | 2016-04-01 | 2016-07-20 | 吴江市林旺纺织厂 | Method for preparing waterproof flame-retardant textile fiber |
| CN109537131A (en) * | 2018-11-26 | 2019-03-29 | 福建凤竹纺织科技股份有限公司 | A kind of flame-retardant complex fiber fabric and preparation method thereof |
| CN112301465A (en) * | 2019-08-02 | 2021-02-02 | 上海美纤智能科技有限公司 | White carbon fiber pre-oxidized (silk) fiber |
| CN112301740A (en) * | 2019-08-02 | 2021-02-02 | 上海美纤智能科技有限公司 | High-performance fiber |
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| CN101023212A (en) * | 2004-09-07 | 2007-08-22 | 日本爱克兰工业株式会社 | Highly flame-retardant and hygroscopic fiber and fiber structure |
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| JP3754132B2 (en) * | 1996-07-09 | 2006-03-08 | 日本板硝子株式会社 | Fiber treatment agent for reinforcing rubber, reinforcing fiber, and rubber reinforcement |
| CN101935946A (en) * | 2010-09-02 | 2011-01-05 | 荣盛石化股份有限公司 | Method for preparing flame-retardant fibers |
| CN103361978A (en) * | 2012-04-02 | 2013-10-23 | 中国人民解放军总后勤部军需装备研究所 | Method for preparing anti-melting polyester fiber or fabric |
| CN103173997B (en) * | 2013-03-25 | 2015-05-13 | 中国人民解放军总后勤部军需装备研究所 | Flame-retardant and anti-fusion fiber or fabric and preparation method thereof |
| CN103952916B (en) * | 2014-04-28 | 2016-01-20 | 绍兴文理学院 | A kind of preparation method of flame-retardant acrylic fibre |
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| CN101023212A (en) * | 2004-09-07 | 2007-08-22 | 日本爱克兰工业株式会社 | Highly flame-retardant and hygroscopic fiber and fiber structure |
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