CN107938010A - High-strength fine-denier flame-retardant viscose fiber and production process thereof - Google Patents
High-strength fine-denier flame-retardant viscose fiber and production process thereof Download PDFInfo
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- CN107938010A CN107938010A CN201711034334.0A CN201711034334A CN107938010A CN 107938010 A CN107938010 A CN 107938010A CN 201711034334 A CN201711034334 A CN 201711034334A CN 107938010 A CN107938010 A CN 107938010A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 156
- 239000000835 fiber Substances 0.000 title claims abstract description 119
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229920000297 Rayon Polymers 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000009987 spinning Methods 0.000 claims abstract description 82
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims description 72
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 57
- 229920002678 cellulose Polymers 0.000 claims description 37
- 239000001913 cellulose Substances 0.000 claims description 37
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 36
- 238000007792 addition Methods 0.000 claims description 29
- 239000003513 alkali Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 23
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 22
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 20
- 230000001112 coagulating effect Effects 0.000 claims description 19
- 238000006477 desulfuration reaction Methods 0.000 claims description 19
- 230000023556 desulfurization Effects 0.000 claims description 19
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000003398 denaturant Substances 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000003431 cross linking reagent Substances 0.000 claims description 14
- 239000003921 oil Substances 0.000 claims description 13
- 238000004061 bleaching Methods 0.000 claims description 12
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 claims description 11
- 229920000609 methyl cellulose Polymers 0.000 claims description 11
- 239000001923 methylcellulose Substances 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 10
- 229960001763 zinc sulfate Drugs 0.000 claims description 10
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 7
- 239000007844 bleaching agent Substances 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- 230000003009 desulfurizing effect Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 230000035800 maturation Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000004925 denaturation Methods 0.000 claims description 3
- 230000036425 denaturation Effects 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 229920003043 Cellulose fiber Polymers 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- -1 Sulphonic acid ester Chemical class 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000004627 regenerated cellulose Substances 0.000 description 2
- 238000009955 starching Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a high-strength fine-denier flame-retardant viscose fiber and a production process thereof, wherein the viscose fiber is prepared by adding a flame retardant into a dispersing agent, grinding the mixture into flame retardant slurry, adding the flame retardant slurry into spinning solution, and carrying out spinning, drafting and post-treatment on the mixture to obtain the fiber with the following performance indexes: the dry breaking strength is more than or equal to 2.7cn/dtex, the dry breaking elongation is 13-20%, the fineness of the product is more than or equal to 0.8D, the limiting oxygen index is more than or equal to 30%, the after-burning time is less than or equal to 3 seconds, and the smoldering time is less than or equal to 3 seconds. The flame-retardant viscose fiber has high strength and excellent flame retardance, the fiber number can reach 0.8D, and the blank of fine denier flame-retardant fiber in China is filled.
Description
Technical field
The present invention relates to viscose rayon technical field, more particularly to a kind of high-intensity fine denier flame retardant viscose fiber and its production
Technique.
Background technology
Fire retardant is divided into organic phosphorus or halogen system organic compound, inorganic combustion inhibitor two used by flame retardant cellulose fiber
Major class.Inorganic based flame retardant forms the fiber being uniformly mixed in spinning process with cellulose and consolidates compound, can obtain good
Flame retardant effect, it is cheap, but its acidproof alkaline stability is poor, when carrying out the final finishing such as dyeing after the fabric that spins, flame retardant effect
Can disappear totally, can be only applied to that the disposable application places for the final finishing such as dyeing need not be carried out, as mattress liner, sofa,
The various fillers such as toy filler and non-woven fabrics field.Organic based flame retardant generally the knot such as crosslinks with cellulosic structure body
The change of structure, therefore obtained flame retardant effect has possessing property, acidproof alkaline stability, can be applied to field of textiles.But at present
There are fire retardant to come off seriously for the fire resistance fibre developed of the country, reaches standard required value, it is necessary to largely use fire retardant, fire-retardant
There are problems with for the increase of agent：1 cause spinning solution can anti-property be greatly lowered, spinning efficiency is low, strand shaping it is poor；It is fire-retardant
Agent influences spinning solution quality after adding, and causes fire-retardant cellulose intensity low, intensity is in 2.0-2.4cn/dtex, resultant yarn spinnability
Difference；3rd, because the addition of fire retardant, can not spin to obtain fine-denier fire resistance fibre, product fiber number is all in more than 1.5D；4th, currently on the market
Fire resistance fibre not wash resistant；5th, spinning efficiency is low so that production cost is high, and product price is high；Fine-denier fire resistance fibre does not have.With
Upper problem limitation fire resistance fibre promotes the use, and constrains the development of flame retardant cellulose fiber.
One Publication No. CN102965751A discloses entitled high wet modulus fire-retardant regenerated cellulose fiber and its system
The patent of Preparation Method, the high wet modulus flame retardant viscose fiber are to be added pyrophosphate based flame retardant using the method for blending addition
To for spinning in spinning solution, the percentage by weight of wherein pyrophosphate based flame retardant is 15-25%.Step：Prepare former for spinning spinning
Liquid, fire retardant allotment and addition, spinning, drawing-off and post processing.High-temperature modulus fire-retardant regenerated cellulose fiber possesses natural fiber
Cellulose fiber feel and skin-friendly, have good anti-flammability, without secondary burn hazard, good spinnability；Fire retardant loss is small, possesses
Rate is up to 98%；Resistance to acid and alkali is good, can be applied to the textile industries such as textile garment fabric, underwear.This method is although a degree of to be carried
The high intensity of fiber, but also exist its fiber number greatly, it is not washable the problems such as.
The content of the invention
Present invention seek to address that in the prior art because additions of fire retardant cause to produce obtained fire resistance fibre fiber number it is big
In 1.5D, intensity is low, not washable, and spinning solution spinnability is poor, and spinning efficiency is low, and production cost is high, and it is not patient to obtain product
Problem, there is provided a kind of high-intensity fine denier flame retardant viscose fiber and its production technology, the flame retardant viscose fiber intensity is high, fibre number
Up to 0.8D, the blank of having filled up domestic fine-denier fire resistance fibre.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions：
A kind of high-intensity fine denier flame retardant viscose fiber, the viscose rayon are that fire retardant addition dispersant is ground into fire retardant
It is added to after slurry in spinning solution and obtains the fiber with following performance indicators through spinning, drawing-off and post processing：Dry fracture strength
>=2.7cn/dtex, dry elongation at break 13-20%, product fiber number >=0.8D, limited oxygen index >=30%, after flame time≤3 second, it is cloudy
Fire time≤3 second.
The addition of the flame retardant paste is 15~25% of methylcellulose weight in spinning solution.
The fire retardant includes nitrogen phosphorus flame retardant, silicone flame retardant.Wherein, the nitrogen phosphorus flame retardant includes
The fire retardants such as the nitrogen phosphorus system KD12 of Clariant Corporation, the silicone flame retardant include the silicon-type KG22 of Clariant Corporation
Deng.
The dispersant includes the TM15 of Italy V51/41, LEVACO company.
A kind of production technology of high-intensity fine denier flame retardant viscose fiber, comprises the following steps
A：Pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process, and alkali cellulose is sent to rubbing
The rubbing of stranding machine is processed into the slurry congee that concentration is 30~40%；
B, send after the slurry congee that step A is obtained is mixed with the sodium hydroxide solution of 140~200g/l of concentration to having excluded air
Drop in poly- reactor, add 2~10% pure oxygen of reactor volume, orientation drop poly- 30~60min obtain the degree of polymerization for 400~
600th, first fibre purity is 98.0~98.5% alkali cellulose；
C, obtained alkali cellulose obtains spinning solution after yellow, dissolving, filtering, deaeration, maturation in step B；During the yellow
Denaturant is added, the addition of denaturant is the 0.1-1.0 ‰ of first fibre weight；
D, flame retardant paste is prepared：Any one in nitrogen phosphorus flame retardant, silicone flame retardant is taken, dispersant is added and grinds
Grind solid content is 20-40%, the flame retardant paste of D95 particle diameter≤1 μm；
E, fire retardant made from 15~25% step D of methylcellulose weight in spinning solution is added to the obtained spinning solutions of step C
Slurry, is uniformly mixed, and obtains for spinning spinning solution；
F, step E is obtained being sent into spinning-drawing machine for spinning spinning solution, the thread extruded by the spinning head of spinning-drawing machine enters a bath and solidifies
Form tow, the coagulating bath that uses of a bath include the sulfuric acid of 90~120g/L, the sodium sulphate of 220~280g/L and 8~
The zinc sulfate of 15g/L, temperature are 40~50 DEG C；
G：Tow after a bath is sent into two baths by one of drafting machine, and the coagulating bath that two bath uses includes 18~22g/L's
Sulfuric acid, temperature are 80~90 DEG C, and the degree of draft of one of drafting machine is 50~100%；Three bath temperatures are 80~90 DEG C；
H：Tow after two baths is sent into three baths by two drafting machines, and it is 1~3 that the coagulating bath that three bath uses, which includes pH value,
Sulfuric acid, temperature are 80~90 DEG C, and the degree of draft of two drafting machine is 40~60%；
I：Tow after three baths is sent out after three drafting machine drawing-offs, and the degree of draft of three drafting machine is 5~15%；
J, tri- drafting machines of step I send out tow it is refined, drying obtain high-intensity fine denier flame retardant viscose fiber, in the essence
Concentration 2-5g/l is added during refining, crosslinking agent and the silk speed of 50-60 DEG C of temperature carry out cross-linking reaction 90-120 seconds.
In the step A, the lye is the sodium hydroxide solution of 110~240g/L of concentration, steeping liquor
Temperature is 30~60 DEG C, and dip time is 50~90min；The grinder is arranged on the pipeline of connection treating tank and squeezer
It is interior；The temperature of the slurry congee is 30~60 DEG C, and the milling time of the grinder is 10~40s；The temperature of the squeezing is 57
~63 DEG C, squeezing multiple be 2.2~2.8；The degree of grinding of the crushing is 120~180g/L.
In the step C, the yellow is to add carbon disulfide in xanthating machine to carry out yellow reaction, the Huang
Change reaction time control in 45~50min, yellow reaction temperature is 20~30 DEG C, and the addition of carbon disulfide is made for step A
Alkali cellulose in first fibre content 35~37%；The dissolving is that the cellulose sulfonate that yellow obtains is added solvent to mix
Close stirring and grinding obtains the cellulose sulfonate solution that concentration is 9.0~10.0%, it is 25~45 that the solvent, which includes concentration,
G/L sodium hydroxide solutions aqueous solution and the sodium sulfite aqueous solution that concentration is 5~10 g/L；The solution temperature is 10~20
DEG C, dissolution time is 30~50min.
In step C, the denaturant for the production of Aksu company denaturation A M-6510, it is described in step D,
The dispersant includes the TM15 of Italy V51/41, LEVACO company, and in step J, the crosslinking agent is given birth to for Clariant
The crosslinking agent KJK325 of production.
In step J, the refining includes the desulfurization of the tow progress formed to spinning drawing, bleaches and oil, institute
The sodium carbonate that vulcanized sodium and concentration that desulfurizing agent that desulfurization uses is 4~8g/L by concentration are 1~4g/L is stated to form；The bleaching
The bleaching agent used is the hydrogen peroxide of 0.3~0.6g/L of concentration；The oil agent addition used that oils is 7~9g/L, is oiled
The pH value of tow is 6.5~7 afterwards, and the drying is that the tow that refining obtains is used drying machine drying, drying temperature 75
~115 DEG C.
The desulfurization temperature is 50~55 DEG C, and desulfurization time is 2~3min；The bleaching temperature is 50~55 DEG C,
Bleaching time is 1~2min；The temperature of the finish is 50~55 DEG C.
The invention has the advantages that：
Existing fire resistance fibre performance indicator：General strength is low, and most of is 2.0-2.4cn/dtex, and without the fire-retardant of fine-denier
Fiber, its fiber number is mostly in more than 1.5D.The present invention provides a kind of high-strength anti-flaming viscose rayon, and it is strong which does fracture
Degree >=2.7cn/dtex, product fiber number >=0.8D, limited oxygen index >=30%, filled up in current fire resistance fibre do not have it is high-strength thin
The blank of denier fiber.
The present invention is in technique prepared by existing conventional flame retardant fiber, by long-term practical studies, by specifically spinning
Silk liquid preparing process simultaneously specifically adds denaturant in yellow, the intensity of fiber can be improved to greatest extent, in spinning solution
Adding flame retardant paste prepared by ad hoc approach is blended spinning solution and fire retardant, can so make fire retardant fully, uniformly with
Spinning solution mixes so that for spinning spinning solution homogeneity before spinning or during spinning, fire retardant is good with spinning solution associativity and can protect
The spinnability of spinning solution is demonstrate,proved, so as to ensure spinning spinnability and the anti-flammability of obtained fiber, nor affects on what is obtained through spinning
The intensity of silk speed；Crosslinking agent is added when silk speed refines, fire retardant combines after being blended with spinning solution through crosslinking agent and silk speed crosslinking,
So that fire retardant is linked to, silk speed is upper so that manufactured silk speed is remaining to keep the anti-flammability of fiber after post processing；It is existing
Fire resistance fibre is simply by spinning after spinning solution and fire retardant blending, and the fiber that this method obtains is because pass through final finishing（Bag
Rubbing method is included, pads and bakes）So that fiber fire resistance after soda acid several times, water washing substantially reduces, and pass through this hair
The specific operation order and technique of bright blending post-crosslinking so that fiber acid and alkali-resistance and water washing performance provide, in this way, passing through
Final finishing and padding still can keep the anti-flammability of fiber after baking, extend fiber service life.
Fire retardant is added in spinning solution and carries out spinning by the prior art, and there are spinnability is poor, fibre number and intensity are low
Problem, it is 20-40% to wait the present invention that grinding of fire retardant specifically is made solid content, the flame retardant paste of D95 particle diameter≤1 μm；
By the flame retardant paste and then in spinning solution is added to, getable uniformity it is good for spinning spinning, this for spin spinning solution with
The preparation process of specific spinning solution of the invention（Sent including slurry congee after dipping, grinder grinding, squeezing, crushing and crushing to
In the poly- reactor of drop for excluding air, addition pure oxygen orientation drop is poly-, alkali cellulose adds denaturant yellow, dissolving etc.）It is and specific
Spinning process（Coagulating bath component and temperature, degree of draft process combine）So as to which the high fine-denier fire resistance fibre of intensity be made.
The acid bath in spinning of existing fire resistance fibre is combined using high zinc sulfate, low sodium sulphate, and high zinc sulfate can water guide weight
Metallic pollution is serious, and low sodium sulphate can then cause its acid bath evaporation to crystallize high energy consumption.Again compatibility acid bath forms the present invention, such as
One bath uses sulfuric acid 90-120g/L, and zinc sulfate 8-15g/L, sodium sulphate 220-280g/L composition, are ensureing the same of acid bath effect
When, high zinc sulfate, the constituent of low sodium sulphate of traditional acid bath have been overturned completely, avoid heavy metal pollution of water body and acid bath
The problem of evaporative crystallization.
Brief description of the drawings
Fig. 1 is the anti-flammability testing result figure of embodiment 10.
Embodiment
It is noted that described further below be all exemplary, it is intended to which the required present invention is provided further
Bright, unless otherwise indicated, all technical and scientific terms used herein has the common skill with the technical field of the invention
The normally understood identical meanings of art personnel.
In each desired value of following embodiments of the present invention, fracture strength is done by GB/T14463-2008 standard detections, dry fracture
Degree of stretching by GB/T14463-2008 standard detections, product fiber number by GB/T14463-2008 standard detections, limited oxygen index by
GB/T5454 standard detections %, after flame time press GB/T5445-2014 standard detections, and smoldering time is marked by GB/T5445-2014
Quasi- detection.
The fire resistance of fire resistance fibre is also embodied by well the good flame resistance in the reuse in later stage, makes in the repetition in later stage
In, fire resistance fibre can pass through substantial amounts of washing and be used under acid or alkaline environment, GB/T5445-2014 detection methods
Principle be by fire resistance fibre after certain number of washes, then detect the glowing of fire resistance fibre, after flame time, glow, afterflame
Time, the washability of fiber is judged according to its anti-flammability.
Embodiment 1
A kind of high-intensity fine denier flame retardant viscose fiber, the viscose rayon are that fire retardant addition dispersant is ground into fire retardant
It is added to after slurry in spinning solution and is obtained through spinning, drawing-off and post processing, obtained fiber has the fiber of following performance indicators：
Dry fracture strength 2.7cn/dtex, dry elongation at break 18%, product fiber number 1.05D, limited oxygen index 30%, after flame time 3 seconds are cloudy
Fire 3 seconds time.
In the present embodiment, the addition of the fire retardant is 15% of methylcellulose weight in spinning solution.The fire retardant is
Nitrogen phosphorus flame retardant, specific is the nitrogen phosphorus flame retardant KD12 of Clariant Corporation.
The dispersant is Italy V51/41.
In the present embodiment, what spinning solution preparation, drawing-off processing, post processing included is refining, drying according in the prior art
Prepared by conventional method, prepared by specific spinning solution：Pulp material through soda-dip, squeeze, obtain alkali cellulose, at alkali cellulose
Manage into slurry congee；Then sodium hydroxide solution is added, progress air drop is poly- to obtain alkali cellulose；Alkali cellulose through yellow, dissolving,
Spinning solution is obtained after filtering, deaeration, maturation；
In the present embodiment prepared by flame retardant paste：Nitrogen phosphorus flame retardant KD12 is taken, adds dispersant, grinding obtained solid content is
20% slurry, after testing, D95 particle diameter≤1 μm of flame retardant paste；
Embodiment 2
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 2.82cn/
Dtex, dry elongation at break 18%, product fiber number 0.91D, limited oxygen index 32%, after flame time 2 seconds, smoldering time 2 seconds；
Preparing the high-intensity fine denier anti-flaming viscose of These parameters system in short-term, the present embodiment and embodiment 1 difference lies in：This
In embodiment, the addition of the fire retardant is 20% of methylcellulose weight in spinning solution.The fire retardant is nitrogen phosphorous flame-retardant
Agent, the specific nitrogen phosphorus flame retardant KD12 using Clariant Corporation production.The dispersant is the TM15 of LEVACO companies.
In the present embodiment prepared by flame retardant paste：Nitrogen phosphorus flame retardant KD12 is taken, adds dispersant, grinds and solid content is made
For 25% slurry, after testing, D95 particle diameter≤1 μm of flame retardant paste；
Embodiment 3
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 2.7cn/
Dtex, dry elongation at break 16%, product fiber number 1.02D, limited oxygen index 34%, after flame time 3 seconds, smoldering time 3 seconds；
Preparing the high-intensity fine denier anti-flaming viscose of These parameters system in short-term, the present embodiment and embodiment 1 difference lies in：Institute
The addition for stating flame retardant paste is 25% of methylcellulose weight in spinning solution.The fire retardant is silicone flame retardant, tool
The silicone flame retardant KG22 produced using Clariant Corporation of body.The dispersant is Italy V51/41.
In the present embodiment prepared by flame retardant paste：Machine silicon-series five-retardant KG22 is taken, dispersant grinding is added and solid content is made
For 30% flame retardant paste, D95 particle diameter≤1 μm of obtained flame retardant paste.
Embodiment 4
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 2.94cn/
Dtex, dry elongation at break 18%, product fiber number 0.86D, limited oxygen index 32%, after flame time 3 seconds, smoldering time 3 seconds；
The high-intensity fine denier flame retardant viscose fiber of the present embodiment is prepared as follows：
A：Pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process, and alkali cellulose is sent to rubbing
The rubbing of stranding machine is processed into the slurry congee that concentration is 30-40%；
B：Send to the drop for having excluded air and gather instead after the slurry congee that step A is obtained is mixed with the sodium hydroxide solution of concentration 200g/l
Answer in device, add 2% pure oxygen of reactor volume, orientation drop poly- 60min obtain the degree of polymerization be 400~600, first fibre purity be
98.0~98.5% alkali cellulose；
C：Obtained alkali cellulose obtains spinning solution after yellow, dissolving, filtering, deaeration, maturation in step B；Added during yellow
0.1 ‰ denaturant of first fibre content, denaturant use the denaturation A M-6510 of Aksu company production.
D：Prepare flame retardant paste：Take nitrogen phosphorus flame retardant（Clariant Corporation, nitrogen phosphorus flame retardant KD12）, add scattered
Agent Italy V51/41, grinds the flame retardant paste for being made that solid content is 35%, D95 particle diameter≤1 μm of slurry；
E, fire retardant made from 15% step D of methylcellulose weight in spinning solution is added to the obtained spinning solutions of step C, mixed
Close uniformly, obtain for spinning spinning solution；
F, step E is obtained being sent into spinning-drawing machine for spinning spinning solution, the thread extruded by the spinning head of spinning-drawing machine enters a bath and solidifies
Tow is formed, the coagulating bath that a bath uses includes sulfuric acid, the sodium sulphate of 220g/L and the zinc sulfate of 8g/L of 90g/L；
G：Tow after a bath is sent into two baths by one of drafting machine, and the coagulating bath that two bath uses includes the sulfuric acid of 18g/L,
The degree of draft of one of drafting machine is 50%；
H：Tow after two baths is sent into three baths by two drafting machines, and the coagulating bath that three bath uses includes the sulphur that pH value is 1
Acid, the degree of draft of two drafting machine is 40%；
I：Tow after three baths is sent out after three drafting machine drawing-offs, and the degree of draft of three drafting machine is 5%；
J, tri- drafting machines of step I send out tow it is refined, drying obtain high-intensity fine denier flame retardant viscose fiber, refining
When, concentration 5g/l is added in the refining, crosslinking agent and the silk speed of temperature 60 C carry out cross-linking reaction 90 seconds.
Embodiment 5
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 2.8cn/
Dtex, dry elongation at break 15%, product fiber number 0.8D, limited oxygen index 32%, after flame time 2 seconds, smoldering time 2 seconds；
When preparing the high-intensity fine denier flame retardant viscose fiber of These parameters system, the present embodiment and embodiment 4 difference lies in：
In the present embodiment, in step A, alkali cellulose send to kneading machine rubbing and is processed into the slurry congee that concentration is 35%；
In step B, sent after the slurry congee that step A is obtained is mixed with the sodium hydroxide solution of concentration 140g/l to having excluded air
Drop in poly- reactor, add 5% pure oxygen of reactor volume, orientation drops poly- 30min and obtains the degree of polymerization as 400~600, first fibre
Purity is 98.0~98.5% alkali cellulose；
In step C, during yellow, the addition of denaturant is 0.5 ‰；
In step D, prepare flame retardant paste：Silicone flame retardant KG22 is taken, the TM15 for adding dispersant LEVACO companies is ground
Grind solid content for 40%, the flame retardant paste of D95 particle diameter≤1 μm；
In step E, the addition of fire retardant is 22% of methylcellulose weight in spinning solution；
In step F, the coagulating bath that a bath uses includes sulfuric acid, the sodium sulphate of 260g/L and the zinc sulfate of 15g/L of 120g/L；
In step G, the coagulating bath that two baths use includes the sulfuric acid of 22g/L, and the degree of draft of one of drafting machine is 50~100%；
In step H, the coagulating bath that three baths use includes the sulfuric acid that pH value is 3, and the degree of draft of two drafting machine is 60%；
In step I：The degree of draft of three drafting machines is 15%.
In step J, concentration 4g/l is added in the refining, crosslinking agent and the silk speed of temperature 50 C carry out cross-linking reaction
120 seconds.
Embodiment 6
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 3.0cn/
Dtex, dry elongation at break 16%, product fiber number 0.9D, limited oxygen index 32%, after flame time 1 second, smoldering time 1 second；
When preparing the high-intensity fine denier flame retardant viscose fiber of These parameters system, the present embodiment and embodiment 5 difference lies in：
In the present embodiment, in step A, alkali cellulose send to kneading machine rubbing and is processed into the slurry congee that concentration is 30-40%；
In step B, sent after the slurry congee that step A is obtained is mixed with the sodium hydroxide solution of concentration 200g/l to having excluded air
Drop in poly- reactor, add 2% pure oxygen of reactor volume, orientation drops poly- 30min and obtains the degree of polymerization as 400~600, first fibre
Purity is 98.0~98.5% alkali cellulose；
In step C, the addition of yellow time variation agent is 1.0 ‰；
In step D, prepare flame retardant paste：Silicone flame retardant KG22 is taken, the TM15 for adding dispersant LEVACO companies is ground
Grind solid content for 20%, the flame retardant paste of D95 particle diameter≤1 μm；
In step E, the 20% of methylcellulose weight in the addition spinning solution of fire retardant；
In step F, the coagulating bath that a bath uses includes sulfuric acid, the sodium sulphate of 240g/L and the zinc sulfate of 12g/L of 115g/L；
In step G, the coagulating bath that two baths use includes the sulfuric acid of 22g/L, and the degree of draft of one of drafting machine is 80%；
In step H, three coagulating baths that use of bath include the sulfuric acid that pH value is 2, the degree of draft of two drafting machine for 40~
60%；
In step I：The degree of draft of three drafting machines is 10%.
In step J, concentration 2g/l is added in the refining, the crosslinking agent that 55 DEG C of temperature carries out cross-linking reaction with silk speed
110 seconds.
Embodiment 7
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 3.02cn/
Dtex, dry elongation at break 16%, product fiber number 0.82D, limited oxygen index 32%, after flame time 2 seconds, smoldering time 2 seconds；
When preparing the high-intensity fine denier flame retardant viscose fiber of These parameters system, the present embodiment and embodiment 6 difference lies in：
In the present embodiment, in step A, alkali cellulose send to kneading machine rubbing and is processed into the slurry congee that concentration is 30-40%；
In step B, sent after the slurry congee that step A is obtained is mixed with the sodium hydroxide solution of concentration 160g/l to having excluded air
Drop in poly- reactor, add 10% pure oxygen of reactor volume, orientation drops poly- 30min and obtains the degree of polymerization as 400~600, first fibre
Purity is 98.0~98.5% alkali cellulose；
In step C, the addition of yellow time variation agent is 1.0 ‰
In step D, prepare flame retardant paste：Nitrogen phosphorus flame retardant is taken, adds the TM15 of dispersant LEVACO companies, grinding is made
Solid content is the flame retardant paste of 28%, D95 particle diameter≤1 μm；
In step E, the 25% of methylcellulose weight in the addition spinning solution of fire retardant；
In step F, the coagulating bath that a bath uses includes sulfuric acid, the sodium sulphate of 280g/L and the zinc sulfate of 15g/L of 120g/L；
In step G, the coagulating bath that two baths use includes the sulfuric acid of 20g/L, and the degree of draft of one of drafting machine is 100%；
In step H, the coagulating bath that three baths use includes the sulfuric acid that pH value is 3, and the degree of draft of two drafting machine is 50%；
In step I：The degree of draft of three drafting machines is 15%.
In step J, concentration 5g/l is added in the refining, crosslinking agent and the silk speed of temperature 60 C carry out cross-linking reaction
100 seconds.
Embodiment 8
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 3.11cn/
Dtex, dry elongation at break 18%, product fiber number 0.8D, limited oxygen index 32%, after flame time 2 seconds, smoldering time 2 seconds；
When preparing the high-intensity fine denier flame retardant viscose fiber of These parameters system, the present embodiment is on the basis of embodiment 7, also
With following differences：In step, the lye is the sodium hydroxide solution of concentration 110g/L, and the temperature of steeping liquor is
60 DEG C, dip time 90min；The grinder is arranged in the pipeline of connection treating tank and squeezer；The temperature of the slurry congee
Spend for 30 DEG C, the milling time of the grinder is 10s；The temperature of the squeezing is 57~63 DEG C, squeezing multiple is 2.2；Institute
The degree of grinding for stating crushing is 120g/L.
In the step C, during the yellow, carbon disulfide is added in xanthating machine and carries out yellow reaction, it is described
For the control of yellow reaction time in 45min, yellow reaction temperature is 20 DEG C, and the addition of carbon disulfide is that alkali made from step A is fine
The 35% of first fibre content in dimension element；The dissolving is that the cellulose sulfonate that yellow obtains is added solvent to be mixed and grind
Mill obtains the cellulose sulfonate solution that concentration is 9.0~10.0%, and it is molten for 25 g/L sodium hydroxides that the solvent includes concentration
Liquid aqueous solution and the sodium sulfite aqueous solution that concentration is 5 g/L；The solution temperature is 10 DEG C, dissolution time 30min.
One bath temperature is 40 DEG C, two bath temperatures are 80 DEG C, three bath temperatures are 80 DEG C.
In step J, the refining includes the desulfurization of the tow progress formed to spinning drawing, bleaches and oil, institute
The sodium carbonate that vulcanized sodium and concentration that desulfurizing agent that desulfurization uses is 4g/L by concentration are 1g/L is stated to form；It is described to bleach what is used
Bleaching agent is the hydrogen peroxide of concentration 0.3g/L；The oil agent addition used that oils is 7g/L, and the pH value of tow is after oiling
6.5, the drying is that the tow that refining obtains is used drying machine drying, and drying temperature is 75 DEG C.
The desulfurization temperature is 50 DEG C, desulfurization time 2min；The bleaching temperature is 50 DEG C, and bleaching time is
1min；The temperature of the finish is 50 DEG C.
Embodiment 9
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 3.0cn/
Dtex, dry elongation at break 17%, product fiber number 0.8D, limited oxygen index 32%, after flame time 0 second, smoldering time 0 second；
When preparing the high-intensity fine denier flame retardant viscose fiber of These parameters system, the present embodiment and embodiment 8 difference lies in：
In step, the lye is the sodium hydroxide solution of concentration 240g/L, and the temperature of steeping liquor is 30 DEG C, dipping
Time is 50min；The temperature for starching congee is 30 DEG C, and the milling time of grinder is 40s；The temperature of squeezing is 63 DEG C, squeezing multiple
For 2.8；The degree of grinding of crushing is 180g/L.
In the step C, yellow reaction time control is in 50min, and yellow reaction temperature is 30 DEG C, two sulphur
The addition for changing carbon is 37% of first fibre content in alkali cellulose made from step A；The cellulose that the dissolving control obtains
Sulphonic acid ester solution concentration is 9.0~10.0%, and the solvent includes concentration for 45 g/L sodium hydroxide solutions aqueous solutions and dense
Spend for the sodium sulfite aqueous solution of 10 g/L；The solution temperature is 20 DEG C, dissolution time 50min.
In step（D）In, the dispersant is V51/41.In step J, desulfurization that the desulfurization uses
The sodium carbonate that the vulcanized sodium and concentration that agent is 8g/L by concentration are 4g/L forms；The bleaching agent used of bleaching is concentration
The hydrogen peroxide of 0.6g/L；The oil agent addition used that oils is 9g/L, and the pH value of tow is 7 after oiling, the drying
It is that the tow that refining obtains is used into drying machine drying, drying temperature is 115 DEG C.The desulfurization temperature is 55 DEG C, during desulfurization
Between be 3min；The bleaching temperature is 55 DEG C, bleaching time 2min；The temperature of the finish is 55 DEG C.
Embodiment 10
High-intensity fine denier flame retardant viscose fiber provided in this embodiment has following index systems：Dry fracture strength 3.14cn/
Dtex, dry elongation at break 18%, product fiber number 0.8D, limited oxygen index 34%, after flame time 0 second, smoldering time 0 second.
When preparing the high-intensity fine denier flame retardant viscose fiber of These parameters system, the difference with the technique of embodiment 8 exists
In：
In step, the lye is the sodium hydroxide solution of concentration 180g/L, and the temperature of steeping liquor is 45 DEG C, dipping
Time is 70min；The temperature for starching congee is 50 DEG C, and the milling time of grinder is 25s；The temperature of squeezing is 60 DEG C, squeezing multiple
For 2.4；The degree of grinding of crushing is 150g/L.
In the step C, yellow reaction time control is in 42min, and yellow reaction temperature is 25 DEG C, two sulphur
The addition for changing carbon is 36% of first fibre content in alkali cellulose made from step A；The cellulose that the dissolving control obtains
Sulphonic acid ester solution concentration is 9.0~10.0%, and the solvent includes concentration for 32g/L sodium hydroxide solutions aqueous solution and dense
Spend for the sodium sulfite aqueous solution of 8 g/L；The solution temperature is 15 DEG C, dissolution time 40min.
In step J, carbon that vulcanized sodium and concentration that desulfurizing agent that the desulfurization uses is 6g/L by concentration are 2.5g/L
Sour sodium composition；The hydrogen peroxide bleached the bleaching agent used and be concentration 0.5g/L；The oil agent addition used that oils is
8g/L, the pH value of tow is 6.5~7 after oiling, and the drying is that the tow that refining obtains is used drying machine drying, is dried
Temperature is 95 DEG C.The desulfurization temperature is 52 DEG C, desulfurization time 3min；The bleaching temperature is 55 DEG C, bleaching time
For 1min；The temperature of the finish is 50 DEG C.
Therefore, in order to better illustrate flame retardant viscose fiber of the present invention, will be prepared into using 10 method of the embodiment of the present invention
To viscose rayon send national clothes and household textile products Quality Supervision and Inspection Center（Chongqing）Detect its anti-flammability, test side
Method is GB/T5455-2014, and the results are shown in Figure 1 for its anti-flammability, its directly to, laterally continue the right time be 0 second, its directly to, laterally
Smoldering time is 0 second.It is consistent with our company test result, it is seen then that flame retardant viscose fiber of the present invention is according to GB/T5455-2014
After test method test, remain to keep preferable anti-flammability.
In order to better illustrate the performance of fire resistance fibre of the present invention, the present invention sets control group,
Control group 1：The control group is prepared with reference to the method for embodiment 5, its difference is only：In step C, when yellow, is added without change
Property agent；
Control group 2：The control group is prepared with reference to the method for embodiment 5, its difference is only：In step C, when yellow, is added without change
Property agent；Without the preparation of flame retardant paste, fire retardant is directly added into；
Control group 3：The control group is prepared with reference to the method for embodiment 5, its difference is only：Without the preparation of flame retardant paste,
It is directly added into fire retardant；
Control group:4：The control group is prepared with reference to the method for embodiment 5, its difference is only：In step C, when yellow, is added without
Denaturant；Without the preparation of flame retardant paste, fire retardant is directly added into, in step J, is added without crosslinking agent；
Control group 5：The control group is prepared with reference to the method for embodiment 10, its difference is only：In step C, when yellow, is added without
Denaturant；
Control group 6：The control group is prepared with reference to the method for embodiment 10, its difference is only：In step C, when yellow, is added without
Denaturant；Without the preparation of flame retardant paste, fire retardant is directly added into；
Control group 7：The control group is prepared with reference to the method for embodiment 10, its difference is only：Without the preparation of flame retardant paste,
It is directly added into fire retardant；
Control group 8：The control group is prepared with reference to the method for embodiment 10, its difference is only：In step C, when yellow, is added without
Denaturant；Without the preparation of flame retardant paste, fire retardant is directly added into, in step J, is added without crosslinking agent.
By the index of correlation of embodiment 5,10 and the fire resistance fibre of control group 1-8 and by GB/T5455-2014 test sides
The anti-flammability result statistics of method test is in table 1 below；
Table 1
From 1 data of upper table, each step of technique of the invention is the entirety of a mutual response, is particularly added in yellow
The specific preparation of denaturant and cooperation flame retardant paste and the specific operation that crosslinking agent is specifically added in refining, they are mutual
Influence, mutually restrict, have impact on the intensity, fiber number and anti-flammability of fire resistance fibre on the whole.
Claims (10)
- A kind of 1. high-intensity fine denier flame retardant viscose fiber, it is characterised in that：The viscose rayon is to add fire retardant to disperse Agent is ground into after flame retardant paste to be added in spinning solution obtains the fibre with following performance indicators through spinning, drawing-off and post processing Dimension：It is dry fracture strength >=2.7cn/dtex, dry elongation at break 13-20%, product fiber number >=0.8D, limited oxygen index >=30%, continuous Fire time≤3 second, smoldering time≤3 second.
- 2. high-intensity fine denier flame retardant viscose fiber according to claim 1, it is characterised in that：The flame retardant paste adds Enter amount for 15~25% of methylcellulose weight in spinning solution.
- 3. high-intensity fine denier flame retardant viscose fiber according to claim 1, it is characterised in that：The fire retardant includes nitrogen phosphorus Flame retardant, silicone flame retardant.
- 4. high-intensity fine denier flame retardant viscose fiber according to claim 1, it is characterised in that：It is big that the dispersant includes meaning The TM15 of sharp V51/41, LEVACO company.
- A kind of 5. production technology of high-intensity fine denier flame retardant viscose fiber as claimed in claim 1, it is characterised in that：The work Skill comprises the following steps：A：Pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process, and alkali cellulose is sent to rubbing The rubbing of stranding machine is processed into the slurry congee that concentration is 30~40%；B, send after the slurry congee that step A is obtained is mixed with the sodium hydroxide solution of 140~200g/l of concentration to having excluded air Drop in poly- reactor, add 2~10% pure oxygen of reactor volume, orientation drop poly- 30~60min obtain the degree of polymerization for 400~ 600th, first fibre purity is 98.0~98.5% alkali cellulose；C, obtained alkali cellulose obtains spinning solution after yellow, dissolving, filtering, deaeration, maturation in step B；During the yellow Denaturant is added, the addition of denaturant is the 0.1-1.0 ‰ of first fibre weight；D, flame retardant paste is prepared：Any one in nitrogen phosphorus flame retardant, silicone flame retardant is taken, dispersant is added and grinds Grind solid content is 20-40%, the flame retardant paste of D95 particle diameter≤1 μm；E, fire retardant made from 15~25% step D of methylcellulose weight in spinning solution is added to the obtained spinning solutions of step C Slurry, is uniformly mixed, and obtains for spinning spinning solution；F, step E is obtained being sent into spinning-drawing machine for spinning spinning solution, the thread extruded by the spinning head of spinning-drawing machine enters a bath and solidifies Form tow, the coagulating bath that uses of a bath include the sulfuric acid of 90~120g/L, the sodium sulphate of 220~280g/L and 8~ The zinc sulfate of 15g/L, temperature are 40~50 DEG C；G：Tow after a bath is sent into two baths by one of drafting machine, and the coagulating bath that two bath uses includes 18~22g/L's Sulfuric acid, temperature are 80~90 DEG C, and the degree of draft of one of drafting machine is 50~100%；Three bath temperatures are 80~90 DEG C；H：Tow after two baths is sent into three baths by two drafting machines, and it is 1~3 that the coagulating bath that three bath uses, which includes pH value, Sulfuric acid, temperature are 80~90 DEG C, and the degree of draft of two drafting machine is 40~60%；I：Tow after three baths is sent out after three drafting machine drawing-offs, and the degree of draft of three drafting machine is 5~15%；J, tri- drafting machines of step I send out silk it is refined, drying obtain high-intensity fine denier flame retardant viscose fiber, in the refining When add concentration 2-5g/l, the crosslinking agent of 50-60 DEG C of temperature carries out cross-linking reaction 90-120 seconds with silk.
- A kind of 6. production technology of high-intensity fine denier flame retardant viscose fiber according to claim 5, it is characterised in that：Institute In the step A stated, the lye is the sodium hydroxide solution of 110~240g/L of concentration, and the temperature of steeping liquor is 30~60 DEG C, dip time is 50~90min；The grinder is arranged in the pipeline of connection treating tank and squeezer；The slurry congee Temperature is 30~60 DEG C, and the milling time of the grinder is 10~40s；The temperature of the squeezing is 57~63 DEG C, squeezing times Number is 2.2~2.8；The degree of grinding of the crushing is 120~180g/L.
- A kind of 7. production technology of high-intensity fine denier flame retardant viscose fiber according to claim 5, it is characterised in that：Institute In the step C stated, the yellow is to add carbon disulfide in xanthating machine to carry out yellow reaction, yellow reaction time control For system in 45~50min, yellow reaction temperature is 20~30 DEG C, and the addition of carbon disulfide is in alkali cellulose made from step A The 35~37% of first fibre content；The dissolving is that the cellulose sulfonate for obtaining yellow adds solvent mixing and grinding The cellulose sulfonate solution that concentration is 9.0~10.0% is obtained, the solvent is 25~45 g/L sodium hydroxides including concentration Solution aqueous solution and the sodium sulfite aqueous solution that concentration is 5~10 g/L；The solution temperature is 10~20 DEG C, dissolution time For 30~50min.
- A kind of 8. production technology of high-intensity fine denier flame retardant viscose fiber according to claim 5, it is characterised in that：In step In rapid C, the denaturant for the production of Aksu company denaturation A M-6510, it is described in step D, the dispersant bag The TM15 of Italian V51/41, LEVACO company is included, in step J, the crosslinking agent is KJK325.
- A kind of 9. production technology of high-intensity fine denier flame retardant viscose fiber according to claim 5, it is characterised in that：In step In rapid J, the refining includes the desulfurization of the tow progress formed to spinning drawing, bleaches and oil, what the desulfurization used The sodium carbonate that the vulcanized sodium and concentration that desulfurizing agent is 4~8g/L by concentration are 1~4g/L forms；It is described to bleach the bleaching agent used For the hydrogen peroxide of 0.3~0.6g/L of concentration；The oil agent addition used that oils is 7~9g/L, the pH value of tow after oiling For 6.5~7, the drying is will to refine obtained tow use drying machine drying, and drying temperature is 75~115 DEG C.
- A kind of 10. production technology of high-intensity fine denier flame retardant viscose fiber according to claim 9, it is characterised in that：Institute The desulfurization temperature stated is 50~55 DEG C, and desulfurization time is 2~3min；The bleaching temperature is 50~55 DEG C, bleaching time 1 ~2min；The temperature of the finish is 50~55 DEG C.
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