CN107604483A - The fire resistance fibre for producing the method for fire resistance fibre and obtaining - Google Patents
The fire resistance fibre for producing the method for fire resistance fibre and obtaining Download PDFInfo
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Abstract
The present invention relates to a kind of method for producing fire resistance fibre and the fire resistance fibre obtained, methods described comprises the following steps：A) polyvinyl alcohol raw material spinning is used, obtains vinal；B) vinal obtained in step a) is immersed in the aqueous solution of tetra methylol phosphorus species, obtains soaking fiber；C) make the soaking fiber predrainage obtained in step b), obtain the fiber through predrainage；D) fiber through predrainage obtained in drying steps c), is obtained through dry fiber；E) make to obtain in step d) carries out ammonia cure through dry fiber, obtains the fiber through ammonia cure；F) fiber through ammonia cure for making to obtain in step e) is aoxidized, and obtains fire resistance fibre.
Description
Technical field
The present invention relates to the method for production fire resistance fibre and the fire resistance fibre obtained, more particularly it relates to use four
The fire resistance fibre that methylol phosphorus species substitute the method for Formaldehyde Production fire resistance fibre and obtained completely or partially.
Background technology
The raw material resources of polyvinyl alcohol (PVA) are extensive, can use the production of the resources such as natural gas, calcium carbide, oil.PVA is fine
Dimension is produced using wet spinning process, and the technical requirements of process equipment are relatively low, processing cost relative moderate.Prepared in conventional polyvinyl
In method, PVA fibers carry out acetalation through formaldehyde and two neighboring hydroxyl reaction, reduce fibre after being blocked to great amount of hydroxy group
Hydroxy radical content in dimension, obtained polyvinyl (also known as vinylon) fiber after acetalation is set to be resistant to the high temperature in dyeing and finishing processing
Hygrometric state condition, and its product has that intensity is high, wearability is good, acid-fast alkali-proof performance is good, good weatherability, can dyeing and printing, wear
The advantages of comfortableness is good.The characteristics of sun-proof performance of its special high-strength wearable is good, especially adapt to frock and army's People's Armed Police's BDU
Fabric uses.The intensity of common polyvinyl reaches 4.2cN/dtex or so；Using the high strength vinylon for adding boron wet method and acetalation to process
Intensity up to more than 8cN/dtex, use add boron wet spinning but fibre strength without acetalation up to 12cN/dtex with
On.The intensity of opposite cotton fiber is relatively low, and in 2.6~4.3cN/dtex or so, the dry strength of viscose rayon is 2.5~2.7cN/
Dtex, wet strength are only half of dry strength or so；The intensity of solvent method regenerated celulose fibre Lyocell fiber reaches
4cN/dtex or so, the good fibre strength of these comfortablenesses are not so good as polyvinyl, therefore, have impact on these fibers and are protected in frock etc.
Application on clothes.
Common polyvinyl and high strength vinylon carry out acetalation processing to the hydroxyl of PVA fibers using formaldehyde and are made, and use first
Aldehyde blocks to the hydroxyl in PVA fibers, considerably reduces the hydroxy radical content in fiber, so as to solve PVA fibers appearance
The problem of swelling, adhesion and dissolution phenomena easily occurs.But use formaldehyde to carry out hydroxy-end capped processing, hydroformylation process equipment be present
Air-tightness require the problem of high, also pollute the environment even if there is trace formaldehyde leakage, injury brought to staff.In environmental protection
Realize the today increasingly improved, the method using formaldehyde as control hydroxy radical content, not applied to current environmental protection will
Ask.
Thermal-flame can cause lethal accident of causing injury to army and police fire fighter and factories and miness occupational staff, and general resident also can be because
Textile is inflammable and causes small burning things which may cause a fire disaster sprawling to cause disaster and cause personal injury and property loss.Therefore to professional frock and household textile
Product carry out flame-retarded processing, are especially important and urgent social reality demands.
But present existing fire resistance fibre both at home and abroad, it is some because directly using intrinsically flame retarded high polymer material (as gathered
Mpd-i, polyimides, polyamide-imides, aromatic polysulfonamide, polyarylate, Ju Fang oxadiazoles etc.) it is made
Meta-aramid, P84, Kermel, PSA fiber, Vectra, the fiber such as Powerleader synthetic fibre, exist price it is high, as clothes and home textile
Comfortableness is poor during fabric use, can not dye or the problems such as poor color fastness.
Using the thermoplastic synthetic fibers such as the flame-resistant terylene of copolymerization or blending and modifying, fire-retardant polyamide fibre, flame-retardant polypropylene, processing side
Just it is, cheap, but melting drippage, contraction, easy the problem of scalding people can occur in the presence of chance fire.
The fire-retardant regenerated cellulose fiber of blending fire retardant will not occur to melt drippage problem, but low intensity is (domestic fire-retardant viscous
Glue fiber intensity about 1.9~2.0cN/dtex；The Austrian Lenzin company for reaching international highest level is based on high wet modulus viscosity glue
The FR fibre strengths of blending phosphorus flame retardant reach 2.4~2.7cN/dtex, wherein the intensity externally announced is 2.4cN/dtex；
The price of this FR fibers reaches 100,000 yuan/ton or so).Although there is researcher to solvent method regenerated celulose fibre (Lyocell
Fiber) carry out flame-retarded research, it is intended to prepared using the high strength characteristics (intensity reaches 4cN/dtex or so) of Lyocell fiber high-strength
Spend fire-retardant regenerated cellulose fiber, but because in the solvent NMMO systems of Lyocell fiber easily because of the presence of trace metal ion
And cause to explode, therefore not yet obtain being engineered process technology so far.
The flame-retarded research of polyvinyl has had kinds of schemes, including PVA and polychloroethylene blended spinning, blending bromine antimony synergistic
Halogen flame, blending phosphorus system or phosphorus nitrogen synergistic fire retardant the methods of.But because polyvinyl to be subjected in process compared with
Strong acid and alkaline processing environment, and up to 230 DEG C or so of high-temperature shaping environment, it is amenable to environment above and with good
The fire retardant of spinnability and fire resistance is seldom；The performances such as the form and aspect of obtained Flame Vinylon, fineness, feel still it is difficult meet it is multi-party
The needs in face；And even if high-strength fire-retarding polyvinyl not yet reaches desirable level, but current price is also up to 80,000 yuan/ton or so.Cause
This, research and development high performance-price ratio, high-strength fire-retarding polyvinyl and regenerated celulose fibre without molten drop, has important social demand.
It is the conventional flame-retardant finishing method of bafta that bafta Proban, which arranges (general Shandong benzene arranges), is to use tetra methylol
The low molecule aqueous solution such as sulfuric acid phosphorus, THPC pads in fabric and controls appropriate active constituent content, allows phosphorus
Based compound is penetrated into the amorphous area and gap of cotton fiber, and controls its moisture content, then by the quantitative stifling of ammonia, is made
NH3It is crosslinked with the methylol in phosphorus system preshrunk body, forms fire-retardant condensate in fibrous inside, and establish the fire-retardant association of phosphorus nitrogen synergistic
Same effect；The oxidized three valent phosphors made in fiber in fire retardant are changed into pentavalent phosphorus again, make the immobilization of fire retardant in the fibre
Further stabilized.Through as above arranging the bafta of processing, after thermal-flame is run into, phosphorus-containing compound decomposes first
Not volatile phosphoric acid or polyphosphoric acid acid anhydride are produced, dehydration occurs with the hydroxyl of cellulose, carbonizes fiber, so as to reach resistance
Fuel efficiency fruit.Fabrics feel soft, fire resistance after the processing of Proban methods is durable, can bear 50 times (or even 200 times) washing,
And remain to keep good fire resistance and the comfortableness of fabric, be suitable for makeing all kinds of protective garments, bedding, adornment with
And fire-retardant nightwear of children etc., be current durable bafta flame-proof treatment important method.But the disadvantage that general Shandong benzene arranges is
Fabric breaking strength after arrangement declines notable, it will usually reach 20% drop it is strong；Particularly tearing strength has significantly
Reduce.Therefore the application of such fire-retardant process technology is had a strong impact on.
Therefore, there is an urgent need to a kind of improved fire resistance fibre preparation side for the disadvantages mentioned above that can overcome prior art at present
Method.
The above-mentioned statement to background technology is merely for convenience (technological means that uses, to be solved to technical solution of the present invention
Technical problem and caused technique effect etc.) deep understanding, and be not construed as recognizing or in any form
Imply information structure prior art known to those skilled in the art.
The content of the invention
It is an object of the invention to provide a kind of improved fire resistance fibre preparation method, methods described is reduced or need not made completely
With the required virose formaldehyde of tool in conventional polyvinyl preparation technology, technological operation is safe and simple, and obtained fire resistance fibre has
High intensity, low cost, without molten drop, wear-resisting, weather-proof, sun-proof, acid and alkali-resistance；Additionally by using tetra methylol phosphorus species and ammonia
Smoked combination processing, makes tetra methylol phosphorus species enter the aggregated structure of fiber, causes the aggregated structure of fiber to become
In loose, the accessibility of dyestuff can be improved, so as to improve the dyeability of fiber.
It can be seen from previous Background, polyvinyl generally use formaldehyde is reacted the adjacent hydroxyl groups in PVA macromoleculars,
Realizing hydroxy-end capped, so as to prevent polyvinyl from producing because great amount of hydroxy group be present swelling adhesion or even the phenomenon dissolved, making through acetal
Change the damp and hot processing of high temperature that the polyvinyl of processing can be subjected in dyeing and finishing processing, but the technology is deposited using having virose formaldehyde
Necessarily limiting to.The present inventor has found by research, if using it is a kind of can be with PVA fibers or the PVA through acetalation
The compound is stably grafted on PVA macromoleculars by the compound that the hydroxyl in fiber reacts, the hydroxyl on PVA after reacting
On, the effect for eliminating hydroxyl in PVA can be equally played, if the compound connected by being reacted with the hydroxyl on PVA
It is fire retardant, then there can be anti-flaming function while PVA fiber resistant against high temperatures high humidity environments are made.Selection has in addition
Fire resistance and the fire retardant that molecular size range is suitable, steric hindrance size is appropriate, and learn and connect with the hydroxyl generating unit differentiation in fiber
Connect, then can control the infiltration quantity of fire retardant, and the regularity of the aggregated structure of PVA macromoleculars can be controlled, so as to control
Dyeability processed.
An aspect of of the present present invention is related to a kind of method for producing fire resistance fibre, it is characterised in that methods described includes as follows
Step：A) polyvinyl alcohol raw material spinning is used, obtains vinal；B) vinal obtained in step a) is soaked
Bubble obtains soaking fiber in the aqueous solution of tetra methylol phosphorus species；C) the soaking of the middle acquisitions of step b) is made
Fiber predrainage, obtain the fiber through predrainage；D) fiber through predrainage obtained in drying steps c), is obtained through dry
Fiber；E) make to obtain in step d) carries out ammonia cure through dry fiber, obtains the fiber through ammonia cure；F) make to obtain in step e)
The fiber through ammonia cure aoxidized, obtain fire resistance fibre.
In one embodiment, step a) and b) between optionally carry out acetalation including the use of formaldehyde so as to reaching not super
The step of crossing 35% acetalizing degree.
In another embodiment, the tetra methylol phosphorus species used in step b) are selected from tetra methylol chlorination
Phosphorus, tetrakis hydroxymetyl phosphonium sulfuric, THPC-urea condensate, tetrakis hydroxymetyl phosphonium sulfuric-urea condensate or its mixing
Thing.
In another embodiment, the concentration of the aqueous solution of the tetra methylol phosphorus species used in step b) is
25-45 weight %, preferably 30-40 weight %, soak time are 10-25 minutes, preferably 15-20 minutes.
In another embodiment, the fiber through predrainage obtained in step c) has 80-150 weight %, preferably
125-130 weight % liquid holdup.
In another embodiment, the drying in step d) carries out 10- at a temperature of 60-80 DEG C, preferably 70-75 DEG C
15 minutes, there is 10-30 weight %, preferably 15-25 weight % moisture content through dry fiber.
In another embodiment, during step e) ammonia cure, selection 90-100 volumes % ammonia concentration,
The ammonia cure temperature of 50-70 DEG C (preferably 60-65 DEG C) and the ammonia cure time of 15-20 minutes.
In another embodiment, in step f) oxidizing process, hydrogen peroxide of the concentration for 10-15 weight % is selected
The aqueous solution is as oxidant, and oxidizing temperature is 50-70 DEG C, and preferably 60-65 DEG C, oxidization time is 5-15 minutes, and preferably 8-10 divides
Clock.
In another embodiment, the method according to the invention also includes washing after step e), oils and dry
Step.
Another aspect of the present invention is related to the fire resistance fibre obtained by the method according to the invention.
The fire resistance fibre 28-34% obtained according to the present invention limited oxygen index, 108-115 DEG C of softening point in water,
3.8-7.5cN/dtex intensity.
Embodiment
The inventive concept of the present invention includes multiple specific embodiments, and different embodiments respectively has technically or applied
On stress, different embodiments, to meet different application scenarios, can solve different application demands with combination collocation.
Therefore, following descriptions to specific embodiment should not be construed as to this invention is intended to the restriction of the technical scheme of protection.
Embodiment 1：
Will through plus boron wet spinning process obtained by, that the high-strength polyvinyl alcohol endless tow without hydroformylation is submerged into 25 weight % is dense
The THPC aqueous solution soaking of degree 20 minutes；Then dressing liquid unnecessary in tow is dried by ironer, rolled
Remaining rate control is in 120 weight %；Fibre bundle after drying toasts 12 minutes in tow dryer at 60 DEG C, makes hygrometric state tow
Moisture control between 15-20 weight %；The tow of drying is sent into ammonia cure equipment progress ammonia and fumigated, and ammonia concentration >=
90 volume %, ammonia cure temperature 70 C, 20 minutes ammonia cure time；Then tow ammonia cure crossed is submerged into 65 DEG C, 10 weight %
Aqueous hydrogen peroxide solution carries out oxidation processes 5 minutes；The tow that oxidation processes finish removes surface impurity through water washing, then through oiling
Fire-retardant high-strength fiber product is arranged with Proban is obtained after drying.Fiber linear density 1.7dtex, intensity 7.4cN/dtex, fracture
Elongation 14.5%, limited oxygen index 32%, 112 DEG C of softening point in water.
Embodiment 2：
Will be dense through adding the high-strength polyvinyl alcohol endless tow without hydroformylation obtained by boron wet spinning process to be submerged into 30 weight %
The tetrakis hydroxymetyl phosphonium sulfuric aqueous solution soaking of degree 20 minutes；Then dressing liquid unnecessary in tow is dried by ironer, rolled
Remaining rate control is in 125 weight %；Fibre bundle after drying toasts 12 minutes in tow dryer at 65 DEG C, makes hygrometric state tow
Moisture control between 15-20 weight %；The tow of drying is sent into ammonia cure equipment progress ammonia and fumigated, and ammonia concentration >=
90 volume %, ammonia cure temperature 70 C, 20 minutes ammonia cure time；Then tow ammonia cure crossed is submerged into 65 DEG C, 10 weight %
Aqueous hydrogen peroxide solution carries out oxidation processes 8 minutes；The tow that oxidation processes finish removes surface impurity through water washing, then through oiling
Fire-retardant high-strength fiber product is arranged with Proban is obtained after drying.Fiber linear density 1.75dtex, intensity 7.5cN/dtex, fracture
Elongation 14.4%, limited oxygen index 33%, 114 DEG C of softening point in water.
Embodiment 3：
By through adding obtained by boron wet spinning process, acetalizing degree 15% high strength vinylon endless tow to be submerged into 40 weight % concentration
THPC-urea condensate aqueous solution soaking 10 minutes；Then by ironer by arrangement unnecessary in tow
Liquid is dried, and pick-up is controlled in 120 weight %；Fibre bundle after drying toasts 15 minutes in tow dryer at 70 DEG C,
Make the moisture control of hygrometric state tow between 15-25 weight %；The tow of drying is sent into ammonia cure equipment progress ammonia and fumigated,
The volume % of ammonia concentration >=90, ammonia cure temperature 50 C, 20 minutes ammonia cure time；Then tow ammonia cure crossed be submerged into 60 DEG C,
10 weight % aqueous hydrogen peroxide solution carries out oxidation processes 5 minutes；The tow that oxidation processes finish is miscellaneous through water washing removal surface
Matter, then obtain Proban after oiling and drying and arrange fire-retardant high-strength fiber product.Fiber linear density 1.8dtex, intensity
6.5cN/dtex, extension at break 13.4%, limited oxygen index 28%, 108 DEG C of softening point in water.
Embodiment 4：
Will be dense through adding obtained by boron wet spinning process, acetalizing degree 21% high strength vinylon chopped strand to be submerged into 30 weight %
The tetrakis hydroxymetyl phosphonium sulfuric of degree-urea condensate aqueous solution soaking 20 minutes；Then will be unnecessary in chopped strand by centrifuge
Arrangement fluid dewatering throw away, after dehydration in chopped strand liquid holdup control in 130 weight %；Fibre bundle after dehydration exists
Toasted 15 minutes at 75 DEG C in short fine carrier bar dryer, make the moisture control of hygrometric state chopped fiber between 10-30 weight %；Through
The chopped fiber of drying, which is sent into ammonia cure equipment and carries out ammonia, fumigates, the volume % of ammonia concentration >=90, ammonia cure temperature 60 C, the ammonia cure time
20 minutes；Then chopped fiber ammonia cure crossed is submerged into 70 DEG C, 10 weight % aqueous hydrogen peroxide solution carries out oxidation processes 10 and divide
Clock；The chopped fiber that oxidation processes finish scrubbed removal surface impurity, and centrifugal dehydration again again after centrifuge takes off liquid, then
Proban is obtained after oiling and drying and arranges fire-retardant high-strength chopped fiber product.Fiber linear density 1.9dtex, intensity 5.8cN/
Dtex, extension at break 14.8%, limited oxygen index 29%, 110 DEG C of softening point in water.
Embodiment 5：
45 weight % concentration will be submerged into through the polyvinyl alcohol filaments without hydroformylation obtained by saltcake wet spinning process
THPC-urea condensate aqueous solution soaking 15 minutes；Then by ironer by dressing liquid unnecessary in tow
Dry, pick-up is controlled in 120 weight %；Fibre bundle after drying toasts 12 minutes in tow dryer at 70 DEG C, makes
The moisture control of hygrometric state tow is between 10-20 weight %；The tow of drying is sent into ammonia cure equipment progress ammonia and fumigated, ammonia
The volume % of gas concentration >=90, ammonia cure temperature 60 C, 20 minutes ammonia cure time；Then tow ammonia cure crossed be submerged into 50 DEG C, 15
Weight % aqueous hydrogen peroxide solution carries out oxidation processes 8 minutes；The tow that oxidation processes finish removes surface impurity through water washing,
Proban is obtained after oiling and drying again and arranges fire resistance fibre product.Fiber linear density 2.1dtex, intensity 4.5cN/dtex,
Extension at break 18.9%, limited oxygen index 32%, 113 DEG C of softening point in water.
Embodiment 6：
Polyvinyl chopped strand through the acetalizing degree 35% obtained by saltcake wet spinning is submerged into the four of 30 weight % concentration
Methylol sulfuric acid phosphorus-urea condensate aqueous solution soaking 25 minutes；Then by centrifuge by arrangement unnecessary in chopped strand
Fluid dewatering is thrown away, and liquid holdup is controlled in 150 weight % in chopped strand after dehydration；Fibre bundle after dehydration is in short fine chain
Toasted 10 minutes at 80 DEG C in plate dryer, make the moisture control of hygrometric state chopped fiber between 15-30 weight %；Drying
Chopped fiber, which is sent into ammonia cure equipment and carries out ammonia, fumigates, and the volume % of ammonia concentration >=90,65 DEG C of ammonia cure temperature, the ammonia cure time 15 divides
Clock；Then chopped fiber ammonia cure crossed be submerged into 50 DEG C, 15 weight % aqueous hydrogen peroxide solution carry out oxidation processes 15 minutes；Oxygen
Change the chopped fiber being disposed scrubbed removal surface impurity, and centrifugal dehydration again again after centrifuge takes off liquid, then through upper
Proban, which is obtained, after oily and dry arranges fire retardant staple length fibers product.Fiber linear density 2.2dtex, intensity 3.8cN/dtex, fracture
Elongation 21.2%, limited oxygen index 34%, 115 DEG C of softening point in water.
Comparative example 1：
Cotton fiber is submerged into the THPC aqueous solution soaking 20 minutes of 25 weight % concentration；Then by from
Scheming throws away arrangement fluid dewatering unnecessary in cotton fiber, and liquid holdup is controlled in 120 weight % in cotton fiber after dehydration；It is de-
Cotton fiber after water toasts 12 minutes in dryer at 60 DEG C, makes the moisture control of hygrometric state cotton fiber in 15-20 weight %
Between；The cotton fiber of drying, which is sent into ammonia cure equipment and carries out ammonia, to be fumigated, the volume % of ammonia concentration >=90, ammonia cure temperature 70 C,
10 minutes ammonia cure time；Then cotton fiber ammonia cure crossed is submerged into 65 DEG C, 10 weight % aqueous hydrogen peroxide solution aoxidized
Processing 5 minutes；The cotton fiber that oxidation processes finish scrubbed removal surface impurity, and centrifugation is de- again again after centrifuge takes off liquid
Water, Proban is then obtained after oiling and drying and arranges cotton fiber product.Fiber linear density 1.43dtex (about 7000 public branch),
Intensity is reduced to 2.7cN/dtex, extension at break 3.1%, limited oxygen index 20.1% from initial 3.4cN/dtex.
Comparative example 2：
Using usual manner, hydroformylation is carried out to common polyvinyl or the high strength vinylon for adding boron wet spinning to produce in hydroformylation case
Processing, the formula of hydroformylation liquid is formaldehyde 25-35g/L, H2SO4220-320g/L、NaSO470-200g/L, hydroformylation temperature are 65-
80 DEG C, the hydroformylation time is 2-10 minutes.The polyvinyl through hydroformylation obtained can be subjected to the damp and hot processing of dyeing and finishing, but not have anti-flammability
Can, oxygen index (OI) is only 20% or so.
By contrasting the result of above-described embodiment and comparative example, for cotton fiber, due to whole by general Shandong benzene
Fabric feeling is hardened after reason, extensibility and deformability decline, and causes intensity to have 20% decline.Conversely pass through the side of the present invention
Fire resistance fibre intensity based on polyvinyl alcohol prepared by method significantly overcomes general Shandong benzene finishing technique up to 3.8-7.5cN/dtex
The problem of strong, drops in middle cotton fiber.
In addition, the limited oxygen index listed in embodiment is fire resistance.Those skilled in the art are generally by limit oxygen
Fiber of the index higher than 24% is classified as fire resistance fibre, fiber of the limited oxygen index higher than 27% is divided into flame retardant fibre, incited somebody to action
Fiber of the limited oxygen index higher than 30% is divided into fireproof fibre.It can be seen from the data of embodiment, the cotton that general Shandong benzene arranges is fine
Polyvinyl only has 20% or so limited oxygen index made from the processing of peacekeeping conventional hydroformylation, belongs to flammable fiber, and passes through this hair
Fire resistance fibre prepared by bright method has 28-34% limited oxygen index, reaches the grade of flame retardant fibre or fireproof fibre, has
Preferable flame retardant effect.
For dyeability, by taking the high reducing dye of color fastness as an example, for adding the production of boron wet spinning process
The common polyvinyl that high strength vinylon and saltcake wet spinning obtain, under the conditions of identical reducing dye dyeing, high strength vinylon
Color depth is lower than common polyvinyl half grade to 1 grade, and bright-coloured degree is also poor；Replaced using tetra methylol phosphorus type flame retardant
Formaldehyde blocks to hydroxyl in PVA, and the fire retardant for accounting for fibre weight about 20% is entered fiber amorphous region or other skies
At gap structure, make the structure of fiber become loose, add the accessibility of dyestuff, therefore under identical dyeing condition, obtain color depth and reach
The effect of common polyvinyl is arrived, bright-coloured degree has also reached the effect of common polyvinyl.Use tetra methylol phosphorus type flame retardant generation
For aldehyde reaction, half grade -1 grade of color depth can be improved to obtain.
The method according to the invention can apply to the vinal without acetalation or have already passed through acetalation
Vinylon fibre, it is however noted that, when applied to vinal without acetalation, obtained fire resistance and
Intensity is superior to have already passed through the vinylon fibre of acetalation.
The description that foregoing exemplary embodiment is presented is merely illustrative of the technical solution of the present invention, and is not intended to turn into
Milli exhaustively, is also not intended to limit the invention to described precise forms.Obviously, one of ordinary skill in the art's root
It is all possible to make many changes and change according to above-mentioned teaching.It is to explain to select illustrative embodiments and be described
The certain principles and its practical application of the present invention, so that others skilled in the art are readily appreciated, realized and utilized
The various illustrative embodiments and its various selection forms and modification of the present invention.Protection scope of the present invention is intended to by institute
Attached claims and its equivalents are limited.
Claims (10)
- A kind of 1. method for producing fire resistance fibre, it is characterised in that methods described comprises the following steps：A) polyvinyl alcohol raw material spinning is used, obtains vinal；B) vinal obtained in step a) is immersed in the aqueous solution of tetra methylol phosphorus species, obtained through leaching The fiber of bubble；C) make the soaking fiber predrainage obtained in step b), obtain the fiber through predrainage；D) fiber through predrainage obtained in drying steps c), is obtained through dry fiber；E) make to obtain in step d) carries out ammonia cure through dry fiber, obtains the fiber through ammonia cure；F) fiber through ammonia cure for making to obtain in step e) is aoxidized, and obtains fire resistance fibre.
- 2. it is according to claim 1 production fire resistance fibre method, it is characterised in that step a) and b) between optionally include Acetalation is carried out using formaldehyde so as to reach the step of being no more than 35% acetalizing degree.
- 3. the method for production fire resistance fibre according to claim 1, it is characterised in that the tetra methylol used in step b) Phosphorus species are selected from THPC, tetrakis hydroxymetyl phosphonium sulfuric, THPC-urea condensate, four hydroxyl first Base sulfuric acid phosphorus-urea condensate or its mixture.
- 4. the method for production fire resistance fibre according to claim 1, it is characterised in that the tetra methylol used in step b) The concentration of the aqueous solution of phosphorus species is 25-45 weight %, and soak time is 10-25 minutes.
- 5. the method for production fire resistance fibre according to claim 1, it is characterised in that obtain in step c) through predrainage Fiber there is 80-150 weight % liquid holdup.
- 6. the method for production fire resistance fibre according to claim 1, it is characterised in that the drying in step d) is in 60-80 10-15 minutes are carried out at a temperature of DEG C, the moisture content through dry fiber with 10-30 weight %.
- 7. the method for production fire resistance fibre according to claim 1, it is characterised in that during step e) ammonia cure, Select 90-100 volumes % ammonia concentration, 50-70 DEG C of ammonia cure temperature and the ammonia cure time of 15-20 minutes.
- 8. the method for production fire resistance fibre according to claim 1, it is characterised in that in step f) oxidizing process, Selecting the aqueous hydrogen peroxide solution that concentration is 10-15 weight %, oxidizing temperature is 50-70 DEG C, oxidization time 5- as oxidant 15 minutes.
- 9. the fire resistance fibre obtained by the method for the production fire resistance fibre according to claim any one of 1-8.
- 10. fire resistance fibre according to claim 9, it is characterised in that the fire resistance fibre has 28-34% limit oxygen Index, 108-115 DEG C of softening point in water, 3.8-7.5cN/dtex intensity.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110952320A (en) * | 2019-12-10 | 2020-04-03 | 山东芦氏阻燃纤维科技有限公司 | Continuous processing method of flame-retardant cellulose short fiber and flame-retardant cellulose short fiber obtained by same |
| CN110952224A (en) * | 2019-11-13 | 2020-04-03 | 华南理工大学 | Modified polyvinyl alcohol fiber composite material and preparation method and application thereof |
| CN111005220A (en) * | 2019-12-10 | 2020-04-14 | 山东芦氏阻燃纤维科技有限公司 | Intermittent processing method of flame-retardant cellulose short fiber and flame-retardant cellulose short fiber obtained by intermittent processing method |
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| CN110952224A (en) * | 2019-11-13 | 2020-04-03 | 华南理工大学 | Modified polyvinyl alcohol fiber composite material and preparation method and application thereof |
| CN110952224B (en) * | 2019-11-13 | 2022-02-15 | 华南理工大学 | Modified polyvinyl alcohol fiber composite material and preparation method and application thereof |
| CN110952320A (en) * | 2019-12-10 | 2020-04-03 | 山东芦氏阻燃纤维科技有限公司 | Continuous processing method of flame-retardant cellulose short fiber and flame-retardant cellulose short fiber obtained by same |
| CN111005220A (en) * | 2019-12-10 | 2020-04-14 | 山东芦氏阻燃纤维科技有限公司 | Intermittent processing method of flame-retardant cellulose short fiber and flame-retardant cellulose short fiber obtained by intermittent processing method |
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