CN109440474A - A kind of low-gravity flame retardant viscose fiber and its manufacturing method - Google Patents
A kind of low-gravity flame retardant viscose fiber and its manufacturing method Download PDFInfo
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- CN109440474A CN109440474A CN201811304226.5A CN201811304226A CN109440474A CN 109440474 A CN109440474 A CN 109440474A CN 201811304226 A CN201811304226 A CN 201811304226A CN 109440474 A CN109440474 A CN 109440474A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
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- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
- D06M13/298—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof containing halogen atoms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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Abstract
The invention discloses a kind of low-gravity flame retardant viscose fiber and its manufacturing method, specific gravity≤1.20g/cm of the low-gravity flame retardant viscose fiber3, limit oxygen index >=32.5%.Manufacturing method includes preparing low-gravity viscose rayon and flame-proof treatment step: (1) preparing sour reactant solution and curing agent solution respectively, be blended before spinning with rayon spinning liquid, be frozen into as-spun fibre through spinning bath；Low-gravity viscose rayon is obtained after plasticizing, drawing-off, desulfurization and washing.(2) low-gravity viscose rayon is impregnated to 3~20s in the fire-retardant soak containing fire retardant and bleeding agent；Then solidification is carried out by fixation bath to oil, 10~30s is impregnated in the fixation bath；Last drying obtains the low-gravity flame retardant viscose fiber.Low-gravity flame retardant viscose fiber provided by the invention not only has good flame retardation effect, and flame retardant property is lasting, and has many advantages, such as that low-gravity, highly hygroscopic, antistatic, feel is fluffy, form is elegant.
Description
Technical field
The present invention relates to modified cellulose fibre technical fields, and in particular to a kind of flame retardant viscose fiber.
Background technique
Cellulose can be used for manufacturing fiber, plastics, film, film etc., grind in civilian, industrial, medicine, national defence and science
Study carefully etc. suffers from extensive purposes.The resource of cellulose be it is unlimited, make full use of this resource abundant to develop fibre
Dimension element industry, has long-range, important meaning, moreover, regenerated cellulose with native cellulose be equally it is environmental-friendly, can
With regeneration and natural degradation.
Viscose rayon is laid equal stress on fibre obtained from plastic fiber molecule using " wood " as raw material from extracting in natural lignose
Cellulose fiber.The hygroscopicity of viscose rayon meets the physiological requirement of human body, has smooth nice and cool, ventilative, antistatic, UV resistance
Line, lucuriant in design, the features such as dyefastness is preferable.Its essence with cotton, the quality of silk.It is genuine plant fiber, is derived from
It however better than natural.It is now widely used for the fields such as all kinds of underwears, weaving, clothes, nonwoven.
With social progress and development, the fire proofing market demand of weaving also increasingly increases, to textile and viscose glue
The requirement of the flame retardant property, multifunctionality, the feature of environmental protection and durability of fiber also increasingly improves.The intensity of viscose rayon, modulus compared with
It is low, it meets fire easily burning and causes fire, limit oxygen index only has 17% or so, to cause personal injury and property loss.It is low
Specific gravity flame retardant viscose fiber had not only guaranteed the excellent physical property of fiber, but realize low cigarette, nontoxic, nontoxic, free from extraneous odour, etc. spies
Property, application performance, security performance greatly improve, and can be widely applied to the fields such as civilian, industrial and military.
The preparation of existing flame retardant viscose fiber is mainly using the method being blended, such as patent document CN200710116512.4
Method for preparing flame-proof viscose fiber, CN200610069338.8 anti-flame fusion-resisting cellulose viscose and its production method,
A kind of flame retardant viscose fiber of CN201610343351.1 and preparation method thereof etc. discloses the preparation method of flame retardant viscose fiber.
But these preparation methods there are the problem of first is that fire retardant is expensive, cause production cost excessively high, seriously limit fire-retardant
The application range of product.Second is that due to being mixed into flame retardant constituent in production process, physical and mechanical property to fibrous finished product and
The stability of spinning production process makes a big impact.And it is modified obtained fire resistance fibre using fire-retardant immersion is post-processed, although
Its physical mechanical property is greatly improved, but fire-retardant persistence it is difficult to ensure that.
Summary of the invention
The first technical problem to be solved by the present invention is: in view of the deficienciess of the prior art, providing a kind of low ratio
Weight flame retardant viscose fiber, not only has good flame retardation effect, the advantage that flame retardant property is lasting and physical mechanical property is good, and have
Low-gravity, the advantages that highly hygroscopic, antistatic, feel is fluffy, form is elegant.
Second technical problem to be solved by this invention is: in view of the deficienciess of the prior art, providing a kind of low ratio
Weight flame retardant viscose fiber manufacturing method, the product being prepared have low-gravity, highly hygroscopic, antistatic, feel is fluffy, form
The advantages that elegant, and using post-process it is fire-retardant impregnate obtained viscose rayon good flame retardation effect, flame retardant property is persistently and physics
Good mechanical property.
In order to solve the first technical problem mentioned above, the technical scheme is that
A kind of low-gravity flame retardant viscose fiber, specific gravity≤1.20g/cm of the low-gravity flame retardant viscose fiber3, do disconnected
Resistance to spalling is 1.75~2.2CN/dtex, and wet breaking strength is 0.8~1.4CN/dtex, limit oxygen index >=32.5%.
To solve above-mentioned second technical problem, the technical scheme is that
A kind of manufacturing method of low-gravity flame retardant viscose fiber, including following prepare low-gravity viscose rayon and flame-proof treatment
Step:
(1) prepare low-gravity viscose rayon: preparing sour reactant solution and curing agent solution respectively, before spinning with viscose glue
Spinning solution is blended, and co-blended spinning liquid is frozen into as-spun fibre through spinning bath；By the as-spun fibre through plasticizing, drawing-off, desulfurization
With the low-gravity viscose rayon is obtained after washing.
(2) the low-gravity viscose rayon flame-proof treatment: is impregnated into 3~20s in fire-retardant soak；The fire-retardant immersion
Contain fire retardant and bleeding agent in liquid；The fire retardant is the combination of one or more of TCEP, DMMP, DEEP；The infiltration
Saturating agent is polyoxyethylene ether compound；Then solidification is carried out by fixation bath to oil, 10~30s is impregnated in the fixation bath；
Last drying obtains the low-gravity flame retardant viscose fiber.
As a kind of improved technical solution, it is described acid reactant solution the preparation method comprises the following steps: by sour reactant and soft water
It is uniformly dissolved according to the ratio of mass ratio 1:1~1.5, and carries out plate-frame filtering.
As a kind of improved technical solution, the curing agent solution the preparation method comprises the following steps: by curing agent and soft water according to
The ratio of 1:1~5 is diluted, and is uniformly mixed.
As a kind of preferred technical solution, the temperature of the acid reactant solution is 15~25 DEG C, and pH value is 9~12；
The temperature of the curing agent solution is 15~25 DEG C.
As a kind of preferred technical solution, the acid reactant is one of sodium carbonate, potassium carbonate, ammonium carbonate or several
Kind.
As a kind of preferred technical solution, the curing agent is isopropanol, in cyclohexanol, neopelex
It is one or more of.
As a kind of preferred technical solution, the adding proportion of the acid reactant be to the 10 of the amount of alpha-cellulose~
50wt%, the adding proportion of the curing agent are 1~10wt% to the amount of alpha-cellulose.
As a kind of preferred technical solution, the osmotic agent concentration in the fire-retardant soak is 3~10g/l, fire retardant
Concentration is 100~300g/l；The temperature of the fire-retardant soak is 40~60 DEG C.
As a kind of improved technical solution, the fire retardant and 2~8g/ containing 20~50g/l in the fixation bath
The finish of l；The temperature of the fixation bath is 20~60 DEG C.
As a kind of preferred technical solution, the polyoxyethylene ether compound is alkyl phenol polyoxyethylene ether, fatty alcohol
The combination of one or more of polyoxyethylene ether, aryl polyoxyethylene ether.
As a kind of improved technical solution, contain in the spinning bath: 100~150g/L of sulfuric acid, sodium sulphate 270~
350g/L, 10~40g/L of zinc sulfate, 10~50g/L of spinning stabilizer.
As a kind of preferred technical solution, the spinning stabilizer is dimethylene amino monoethanolamine, octadecyl
One or more of amine, sodium ethylenediamine tetramethylenephosphonate.
As a kind of improved technical solution, the temperature of the spinning bath is 45~55 DEG C；What the plasticizing process used
Contain 10~25g/L of sulfuric acid, 25~60g/L of sodium sulphate, 5~15g/L of zinc sulfate in plasticizing-bath.
As a kind of improved technical solution, the temperature of the plasticizing-bath is 95~100 DEG C.
As a kind of improved technical solution, the temperature of the low-gravity viscose rayon drying is 110~140 DEG C.
As a kind of preferred technical solution, the preparation of the rayon spinning liquid is the wood by the degree of polymerization 500~700
Pulp rayon spinning liquid made of dipping, squeezing, crushing, experienced, yellow, grinding, filtering, deaeration.
By adopting the above-described technical solution, the beneficial effects of the present invention are:
Sour reactant and curing agent has been blended when preparing low-gravity viscose rayon in the present invention in rayon spinning liquid, altogether
For blended ratio liquid in spinning bath when solidification forming, sour reactant and the sulfuric acid reaction in coagulating bath generate carbon dioxide gas,
As-spun fibre tow inner inflatable is overflowed after forming cavity structure, makes fibre structure fluffyization, and fiber specific gravity reduces.Viscose rayon tow warp
After the inflation extruding of reactant, with the evolution of gas, the cavity structure that original bulking effect is formed has substantial portion of contracting
It returns and collapses, can reduce after addition curing agent in rayon spinning liquid and slow down this retraction and collapse, be conducive to fluffy cavity
The holding and fixation of structure help the solidification for inflating the cavity structure of formation.It is viscous using this low-gravity with cavity structure
Glue fiber, when preparing fire resistance fibre using post-processing flame-proof treatment method, fire retardant is entered directly into the cavity structure of fiber, resistance
Combustion agent retention is high and can obtain permanent flame retardant effect.
The present inventor is devoted for years in the research of the especially flame-retardant modified viscose rayon of viscose rayon, discovery by TCEP,
The fire retardant that DMMP, DEEP etc. are originally intended to the fields such as plastics, foam, resin is used as the fire retardant of low-gravity flame retardant viscose fiber,
And when using polyoxyethylene ether compound as bleeding agent, both discoveries combine and have obtained the strong technology of unexpected penetration
Effect, the low-gravity flame retardant viscose fiber that fire-retardant immersion obtains after post treatment, good flame retardation effect, combustion limits oxygen index (OI) are up to
34% or more.
The present invention is in spinning moulding, cellulose sulfonate, the sour reactant being added while and sulfuric acid in spinning bath
Reaction, reaction severe degree are more violent than the spinning solution of no sour reactant, and therefore, spinning is added in the present invention in spinning bath
Stabilizer can be conducive to the formation of fine structure inside strand with slowed down reaction speed, guarantee the physical mechanics property that fiber is made
The improvement and raising of energy index, while improving the stability and spinnability of fibre solidification forming process.
The present invention is after fire-retardant immersion, and by the way of solidifying, oiling while carrying out, 20~50g/l is contained in fixation bath
The fire retardant and 2~8g/l finish, flame retardant effect is further strengthened, while oiling, has received better resistance
It fires and the effect that oils, it is especially more lasting by fire resistance fibre flame retardant effect processed in this way.
Present invention drying temperature for using in drying is dried at high temperature for 110~140 DEG C, further strengthen with surely
Determine flame retardant effect.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the fibre section figure of low-gravity flame retardant viscose fiber of the invention under the microscope.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is further explained.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
By Fig. 1, it can be seen that, low-gravity flame retardant viscose fiber of the invention is the fiber with many cavity structures,
When post-processing impregnates fire-retardant, fire retardant can enter in cavity to be retained for a long time.
Embodiment 1
A kind of low-gravity flame retardant viscose fiber, the specific gravity 1.12g/cm of the low-gravity flame retardant viscose fiber3, do fracture
Intensity is 1.89CN/dtex, wet breaking strength 1.05CN/dtex, limit oxygen index 33.1%.
Embodiment 2
A kind of low-gravity flame retardant viscose fiber, the specific gravity 1.10g/cm of the low-gravity flame retardant viscose fiber3, do fracture
Intensity is 1.76CN/dtex, wet breaking strength 0.95CN/dtex, limit oxygen index 33.6%.
Embodiment 3
(1) sour reactant sodium carbonate and soft water are uniformly dissolved according to the ratio of mass ratio 1:1.1, temperature is 20 DEG C, pH
Value is 10.5, carries out plate-frame filtering.
(2) curing agent isopropanol and soft water are diluted according to the ratio of 1:1.1, are uniformly mixed, temperature is 20 DEG C.
(3) sour reactant solution and curing agent solution are blended before spinning with rayon spinning liquid, co-blended spinning liquid is passed through
Spinning bath is frozen into as-spun fibre；The adding proportion of the acid reactant sodium carbonate is the 20wt% to the amount of alpha-cellulose, institute
The adding proportion of curing agent isopropanol is stated as the 2.5wt% of the amount to alpha-cellulose.In the spinning bath containing sulfuric acid 125g/L,
Sodium sulphate 310g/L, zinc sulfate 12.5g/L, dimethylene amino monoethanolamine 20g/L；Temperature is 51 DEG C.
(4) as-spun fibre is obtained into low-gravity viscose rayon after plasticizing, drawing-off, desulfurization and washing.
(5) the low-gravity viscose rayon is being contained into fire retardant TCEP200g/l and bleeding agent alkyl phenol polyoxyethylene ether
15s is impregnated in the fire-retardant soak of 4.5g/l；The temperature of the fire-retardant soak is 52 DEG C.
(6) then solidification is carried out in the fixation bath by the finish of fire retardant TCEP and 4.0g/l containing 35g/l to oil,
20s is impregnated in the fixation bath；The temperature of the fixation bath is 50 DEG C.
(7) it most dries to obtain the low-gravity flame retardant viscose fiber through 125 DEG C of temperature afterwards.
Embodiment 4
(1) sour reactant potassium carbonate and soft water are uniformly dissolved according to the ratio of mass ratio 1:1.2, temperature is 18 DEG C, pH
Value is 10, carries out plate-frame filtering.
(2) curing agent cyclohexanol and soft water are diluted according to the ratio of 1:2, are uniformly mixed, temperature is 18 DEG C.
(3) sour reactant solution and curing agent solution are blended before spinning with rayon spinning liquid, co-blended spinning liquid is passed through
Spinning bath is frozen into as-spun fibre；The adding proportion of the acid reactant potassium carbonate is the 30wt% to the amount of alpha-cellulose, institute
State curing agent isopropanol, cyclohexanol, neopelex adding proportion be 3wt% to the amount of alpha-cellulose.It is described
Contain sulfuric acid 130g/L, sodium sulphate 300g/L, zinc sulfate 12g/L, octadecylamine 20g/L in spinning bath；Temperature is 50 DEG C.
(4) as-spun fibre is obtained into low-gravity viscose rayon after plasticizing, drawing-off, desulfurization and washing.
(5) the low-gravity viscose rayon is being contained into fire retardant DMMP250g/l and bleeding agent fatty alcohol polyoxyethylene ether
18s is impregnated in the fire-retardant soak of 3.8g/l；The temperature of the fire-retardant soak is 52 DEG C.
(6) then solidification is carried out in the fixation bath by the finish of fire retardant DMMP and 4g/l containing 35g/l to oil,
16s is impregnated in the fixation bath；The temperature of the fixation bath is 40 DEG C.
(7) it most dries to obtain the low-gravity flame retardant viscose fiber through 130 DEG C of temperature afterwards.
Embodiment 5
(1) sour reactant ammonium carbonate and soft water are uniformly dissolved according to the ratio of mass ratio 1:1.3, temperature is 23 DEG C, pH
Value is 11, carries out plate-frame filtering.
(2) curing agent neopelex and soft water are diluted according to the ratio of 1:3, are uniformly mixed, temperature
It is 23 DEG C.
(3) sour reactant solution and curing agent solution are blended before spinning with rayon spinning liquid, co-blended spinning liquid is passed through
Spinning bath is frozen into as-spun fibre；The adding proportion of the acid reactant ammonium carbonate is the 40wt% to the amount of alpha-cellulose, institute
The adding proportion of curing agent neopelex is stated as the 5.0wt% of the amount to alpha-cellulose.Contain in the spinning bath
Sulfuric acid 130g/L, sodium sulphate 320g/L, zinc sulfate 15g/L, sodium ethylenediamine tetramethylenephosphonate 40g/L；Temperature is 52 DEG C.
(4) as-spun fibre is obtained into low-gravity viscose rayon after plasticizing, drawing-off, desulfurization and washing.
(5) the low-gravity viscose rayon is being contained into fire retardant DEEP250g/l and bleeding agent aryl polyoxyethylene ether
12s is impregnated in the fire-retardant soak of 4.5g/l；The temperature of the fire-retardant soak is 49 DEG C.
(6) then solidification is carried out in the fixation bath by the finish of fire retardant DEEP and 3.6g/l containing 33g/l to oil,
18s is impregnated in the fixation bath；The temperature of the fixation bath is 55 DEG C.
(7) it most dries to obtain the low-gravity flame retardant viscose fiber through 132 DEG C of temperature afterwards.
Embodiment 6
(1) sour reactant sodium carbonate and soft water are uniformly dissolved according to the ratio of mass ratio 1:1, temperature is 25 DEG C, pH value
It is 11, carries out plate-frame filtering.
(2) curing agent isopropanol and soft water are diluted according to the ratio of 1:1, are uniformly mixed, temperature is 25 DEG C.
(3) degree of polymerization is passed through into dipping, squeezing, crushing, experienced, yellow, grinding, filtering, deaeration system in 600 wood pulps
At rayon spinning liquid；Sour reactant solution and curing agent solution are blended before spinning with rayon spinning liquid, by co-blended spinning liquid
As-spun fibre is frozen into through spinning bath；The acid reactant sodium carbonate, potassium carbonate, ammonium carbonate adding proportion be to alpha-cellulose
Amount 20wt%, the adding proportion of the curing agent isopropanol is the 2.5wt% to the amount of alpha-cellulose.In the spinning bath
Contain sulfuric acid 130g/L, sodium sulphate 295g/L, zinc sulfate 12.5g/L, dimethylene amino monoethanolamine 22g/L；Temperature is 52
℃。
(4) as-spun fibre is passed through and contains sulfuric acid 18g/L, the plasticizing-bath plasticizing of sodium sulphate 35g/L, zinc sulfate 12g/L,
Low-gravity viscose rayon is obtained after drawing-off, desulfurization and washing；The temperature of plasticizing-bath is 100 DEG C.
(5) the low-gravity viscose rayon is being contained into fire retardant TCEP190g/l and bleeding agent alkyl phenol polyoxyethylene ether
8s is impregnated in the fire-retardant soak of 5.5g/l；The temperature of the fire-retardant soak is 58 DEG C.
(6) then solidification is carried out in the fixation bath by the finish of fire retardant TCEP and 3.5g/l containing 33g/l to oil,
18s is impregnated in the fixation bath；The temperature of the fixation bath is 55 DEG C.
(7) it most dries to obtain the low-gravity flame retardant viscose fiber through 128 DEG C of temperature afterwards.
Comparative experiments example 1
Comparative experiments example 1 is with the difference of embodiment 3, without step (1), (2), in step (3), does not add sour reaction
Agent and curing agent directly carry out spinning using rayon spinning liquid, do not contain spinning stabilizer in spinning solution, are prepared common viscous
Glue fiber, then going to step (5), (6), (7) impregnate, fire-retardant, solidification oils and drying obtains common fire resistance fibre.
Comparative experiments example 2
Comparative experiments example 1 is with the difference of embodiment 3, contains only finish in fixation bath in step (6), without containing fire-retardant
Agent.
Comparative experiments example 3
Comparative experiments example 2 is that solidification and the substep that oils are carried out in step (6) with the difference of embodiment 3, is first solidified
It is fire-retardant, 15s is respectively impregnated using the finish of the fire retardant TCEP and 4.0g/l of 35g/l respectively.
Comparative experiments example 4
Comparative experiments example 3 is that the drying temperature in step (7) is 105 DEG C with the difference of embodiment 3.
The physical mechanical property for the flame retardant viscose fiber that above embodiments 3-6 and comparative experiments example 1-4 are prepared refers to
It is marked with and flame retardant property see the table below 1.Wherein fire-retardant enduring quality is using electronic friction-bar to one Wan Cihou of fire resistance fibre friction
The limit oxygen index of measurement.
Table 1
As it can be seen that if using common viscose fiber, impregnated using post-processing of the invention it is flame-retardant modified, flame retardant property and
Persistence can not show a candle to using the low-gravity fiber for having cavity structure.When post-processing flame-proof treatment, if only used when oiling
Finish does not use fire retardant curing process, then seriously affects its flame retardant effect and fire-retardant persistence；If solidification and upper oil
Step carries out, then seriously affects its fire-retardant persistence；And when being dried after flame-proof treatment, if drying temperature is low also to will affect its resistance
Fire persistence.
Claims (10)
1. a kind of low-gravity flame retardant viscose fiber, it is characterised in that: the specific gravity of the low-gravity flame retardant viscose fiber≤
1.20g/cm3, doing breaking strength is 1.75~2.2CN/dtex, and wet breaking strength is 0.8~1.4CN/dtex, limit oxygen index
>=32.5%.
2. a kind of manufacturing method of low-gravity flame retardant viscose fiber, it is characterised in that including it is following prepare low-gravity viscose rayon and
Flame-proof treatment step:
(1) prepare low-gravity viscose rayon: preparing sour reactant solution and curing agent solution respectively, before spinning with rayon spinning
Liquid is blended, and co-blended spinning liquid is frozen into as-spun fibre through spinning bath；By the as-spun fibre through plasticizing, drawing-off, desulfurization and water
The low-gravity viscose rayon is obtained after washing；
(2) the low-gravity viscose rayon flame-proof treatment: is impregnated into 3~20s in fire-retardant soak；In the fire-retardant soak
Contain fire retardant and bleeding agent；The fire retardant is the combination of one or more of TCEP, DMMP, DEEP；The bleeding agent
For polyoxyethylene ether compound；Then solidification is carried out by fixation bath to oil, 10~30s is impregnated in the fixation bath；Finally
Drying obtains the low-gravity flame retardant viscose fiber.
3. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: the acid reactant is molten
The temperature of liquid is 15~25 DEG C, and pH value is 9~12；The temperature of the curing agent solution is 15~25 DEG C.
4. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: it is described acid reactant be
One or more of sodium carbonate, potassium carbonate, ammonium carbonate；The curing agent is isopropanol, cyclohexanol, neopelex
One or more of.
5. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: the acid reactant
Adding proportion is 10~50wt% to the amount of alpha-cellulose, and the adding proportion of the curing agent is 1 to the amount of alpha-cellulose
~10wt%.
6. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: the fire-retardant soak
In osmotic agent concentration be 3~10g/l, flame retardant concentration is 100~300g/l；The temperature of the fire-retardant soak is 40~60
℃。
7. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: contain in the fixation bath
There are the fire retardant of 20~50g/l and the finish of 2~8g/l；The temperature of the fixation bath is 20~60 DEG C.
8. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: the polyoxyethylene ether
Compound is the combination of one or more of alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, aryl polyoxyethylene ether.
9. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: contain in the spinning bath
Have: 100~150g/L of sulfuric acid, 270~350g/L of sodium sulphate, 10~40g/L of zinc sulfate, 10~50g/L of spinning stabilizer；It is described
Spinning stabilizer is one of dimethylene amino monoethanolamine, octadecylamine, sodium ethylenediamine tetramethylenephosphonate or several
Kind.
10. the manufacturing method of low-gravity flame retardant viscose fiber as claimed in claim 2, it is characterised in that: the low-gravity is viscous
The temperature of glue fiber drying is 110~140 DEG C.
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