CN104831386B - A kind of spinning technique method without contaminating flame-retardant viscose fiber colored long filament - Google Patents
A kind of spinning technique method without contaminating flame-retardant viscose fiber colored long filament Download PDFInfo
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- CN104831386B CN104831386B CN201510258077.3A CN201510258077A CN104831386B CN 104831386 B CN104831386 B CN 104831386B CN 201510258077 A CN201510258077 A CN 201510258077A CN 104831386 B CN104831386 B CN 104831386B
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Abstract
A kind of spinning technique method without contaminating flame-retardant viscose fiber colored long filament, including: the spinning mixture being mixed with first fibre viscose glue by silicon nitrogen combustion inhibitor, mill base is provided;The spinning acid bath being mixed with sodium sulphate by sulfuric acid, zinc sulfate is provided;Coagulation forming and spinning drawing is carried out to obtain coloured continuous filament yarn by being sent in spinning acid bath by measuring pump and spinning head after spinning mixture deaeration, filtration;There is provided containing Ti4+、Ca2+The solidification treatment fluid of cation complex solution;Coloured continuous filament yarn is carried out solidification process;And the long filament after processing solidification washes, dries and packing processes is to obtain finished product coloured yarn.Present invention omits the dyeing process in downstream, amplitude peak has been reduced or avoided textile printing and dyeing wastewater to the pollution of environment and the dyeing product harm to human body.
Description
Technical field
The present invention relates to wet spinning forming technology.
Background technology
No matter synthetic fibers, viscose rayon or the equal easy firing of natural cotton fiber catches fire and causes fire
Calamity, and fire resistance fibre can solve these problems, especially adds fire retardant in viscose rayon raw
The FRC produced, can improve the easily ignitable characteristic of fiber, it is to avoid fire, reduces
Property and life injury, also maintain the special performance comfortable and easy to wear that viscose rayon is original.
Owing to all impacts can be produced (such as when mill base and fire retardant coexist in spinning mixture
Colour insecure, fire retardant solidification effect is the best and acid bath coagulability difference etc. problem), at present
The fire resistance fibre of production and sales is all colourless (primary colors) base fiber, is woven into after cloth according to need
To carry out dyestuff again and (dye) look.In this case dyeing waste water and dyeing and printing products are inevitable
Harm is produced to environment and to health.
Summary of the invention
It is an object of the invention to provide a kind of without contaminating being spun to of flame-retardant viscose fiber colored long filament
Shape technique or method, it is suitable for industrializing and environmental.
The spinning technique method without the flame-retardant viscose fiber colored long filament of dye according to the present invention includes:
The spinning mixture being mixed with first fibre viscose glue by silicon nitrogen combustion inhibitor, mill base is provided, its
Middle mill base is the suspension dispersible pigment color paste of diameter≤0.4 μm, and silicon nitrogen combustion inhibitor glues with first fibre
In glue, the weight ratio of contained first fibre is 36-45%, and mill base is the fine weight of contained first with first fibre viscose glue
Amount ratio is 0.7-2%;
Thering is provided the spinning acid bath being mixed with by sulfuric acid, zinc sulfate with sodium sulphate, wherein sulfuric acid is dense
Degree is 85-115g/L, zinc sulfate concentration is 9-12g/L, sodium sulfate concentration is 222-268g
/L;
Sent into after spinning mixture deaeration, filtration in spinning acid bath by measuring pump and spinning head
Carry out coagulation forming and spinning drawing to obtain coloured continuous filament yarn and to be wrapped in and spin on dish,
Wherein spinning acid bath temperature is 38-48 DEG C, and spinning speed is 75-80m/min, and spinning head
Drawing-off amount is 10-15%, spin dish drawing-off amount is 20-25%, rear road drawing-off amount is 5-10%;
There is provided containing Ti4+、Ca2+The solidification treatment fluid of cation complex solution;
By coloured continuous filament yarn through washing with centrifugal treating to form spinning cake shape long filament;
Spinning cake shape long filament being sent into solidification treatment fluid and carries out solidification process, wherein solidification processes liquid temperature
Degree is for 75-90 DEG C;And
Long filament after processing solidification is washed, is dried with packing processes to be become
Product coloured yarn.
In one particular embodiment of the present invention, spinning mixture viscosity (falling ball method) is preferred
For the 19-36 second, degree of ripeness is preferably 9-16ml (10%NH4CL solution).Above-mentioned viscosity and ripe
Become scale order position the most known in the art.
In a preferred embodiment of the invention, spinneret draft amount is set to 13%, spins dish drawing-off amount
Be 25%, rear road drawing-off amount be 5%.It is ripe that each drawing-off amount above-mentioned is those skilled in the art institute
Know and usual.
In one particular embodiment of the present invention, mill base is preferably as follows preparation:
It is particle diameter≤0.4 μm by natural pigment or Prof. Du Yucang pigment grind;
There is provided polyvinylpyrrolidone as suspension dispersive agent;And
Pigment after above-mentioned grinding is added in suspension dispersive agent and water to form aqueous suspension look
Slurry, wherein specific gravity of pigment is 35-50%, and polyvinylpyrrolidone proportion is 3-8%, and surplus is water.
In this embodiment, it is also possible to use the colloid mill aqueous suspension mill base to preparing or colloid
Mill base further grinding distribution 2-4 hour is to improve the colloidal dispersions uniformity.
In the first fibre viscose glue used in the present invention, " first is fine " (weight) content is preferably 8-10%.
The solidification treatment fluid used in the present invention can preferably employ Beijing Sail orchid fire resistance fibre
Co., Ltd produce and sell 802#Prepared by curing agent, concentration (curing agent weight content) is excellent
Elect 30-60% as, more preferably 32%-35%, most preferably 33%.
The silicon nitrogen combustion inhibitor used in the present invention can use organosilan to hydrolyze dispersion liquid, and it is changed
Formula is [Me2O·nSiO2]+[--CONH], wherein Me represents metal ion, SiO2Content
For 9.23-53%;Acid amides [--CONH] content is 4.3-27%.About silicon nitrogen combustion inhibitor, permissible
See patent application CN104032401A and CN103789858A before applicant, at this
Introduce the full content of the two application seeing mode respectively.A preferred reality in the present invention
Executing in example, silicon nitrogen combustion inhibitor uses Beijing Sail orchid fire resistance fibre Co., Ltd to produce and sell
801#Silicon nitrogen combustion inhibitor.
Prepared according to the methods of the invention long filament specification can be at 70D-500D (representation unit
The tow weight of length) and 15-60F (representing the monofilament quantity forming every beam filament)
Within the scope of the widest.
In a preferred embodiment of the invention, spinning mixture can also include alkali and dispersion
Agent.Alkali can be NaOH or potassium hydroxide, and the concentration in spinning mixture is 7-8%.
Dispersant then can be preferably used what Beijing Sail orchid fire resistance fibre Co., Ltd produced and sold
803#Dispersant.
In a preferred embodiment of the invention, the water temperature that each washing processes can be 60-80 DEG C.
In other embodiments of the invention, solidification can also include oiling treatment after processing
(the preferred 0.8-1.5g/L of Spinning Oil Concentration).It addition, drying between packing processes
Can also include that conventional one-tenth cylinder processes.
Spinning technique technique according to the present invention, owing to have employed the spinning mixture of uniqueness, joins
Close selected spinning acid bath and/or solidification treatment fluid, and well-designed process conditions, from
And achieve industrialized production coloured yarn and have firm coloration, fire retardant solidification effect with
And the advantage that acid bath coagulation result is good.
Additionally, it also have the advantage that
Owing to have employed nitrogen silicon series environmental protection fire retarding agent, thus fiber has environmental protection performance,
Meet national energy-saving environmental protection policy;And
Fire-retardant coloured yarn is produced owing to have employed mill base to be effectively mixed in anti-flaming viscose
Technique, not only eliminates the dyeing process in downstream, and can be reduced or avoided with amplitude peak and spin
Knit dyeing waste water to the pollution of environment and the dyeing product harm to human body.
Detailed description of the invention
(1) it is mixed with spinning mixture by fire retardant and mill base with first fibre viscose glue
First fibre addition in viscose glue is respectively by fire-retardant agent liquid, mill base according to weight ratio
36-45%, 0.7-2%.After interpolation, strong agitation makes the most consistent colloid mixture;
Then deaeration and filtration are carried out.Spinning mixture viscosity is the 19-36 second, and degree of ripeness is 16-19
Ml (10%NH4CL solution).Fire retardant uses nitrogen silicon system environmental protection fire retarding agent.Mill base is diameter≤0.4
The suspension dispersible pigment color paste of μm, is made suspension dispersive agent by polyvinylpyrrolidone, and colloid mill grinds
Disperse 2-4 hour and make 35-50% aqueous suspension mill base.
(2) preparation of spinning acid bath
Use pure water preparation spinning acid bath, wherein sulfuric acid 85-115g/L, zinc sulfate 9-12g
/ L, sodium sulphate 222-268g/L.Keep acid bath temperature 38-48 DEG C.
(3) spinning technique drawing-off
Spinning mixture is passed through measuring pump and spinning head anti-with acid bath in spinning-drawing machine acid bath groove
Should, coagulation forming, spinning speed 75-80m/min, spinneret draft amount is 10-15%, spins
Dish drawing-off amount is 20-25%, rear road drawing-off amount is 5-10%.
(4) wash, be centrifuged and curing process process
Flame-retardant viscose fiber colored long filament after drawing-off through washing and centrifugal treating after with
Spinning cake form enters drip washing or compresses and washes flow process and carry out solidification process at this.Described solidification processes
Liquid temp is 75-90 DEG C, and the curative concentration of employing is 30-60%.Described curing agent is for containing
Ti4+、Ca2+Complex solution Deng cation.
(5) again wash, oil, dry, the post processing such as packaging
Gained coloured yarn specification is 70D-500D and 15-60F.
Embodiment 1: without dye FRC red filaments 250D/60F
Prepare mill base: take red pigment, through extra-fine grinding to particle diameter≤0.4 μm.Above-mentioned process
After pigment 30%, polyvinylpyrrolidone 6%, pure water 64%, add colloid mill grind 3h,
Cool down standby.
Fire-retardant agent liquid, red mill base contact mixing with viscose glue according to certain weight ratio;Join glue
Ratio: IIF glue is (containing first fibre 8.2%;It is purchased from Beijing Sail limited public affairs of orchid fire resistance fibre equally
Department) 16OOOL;Silicon nitrogen combustion inhibitor 801#2360L;10% sodium hydroxide solution 1200L;
Dispersant 803#200L;Red mill base 300kg.Charging sequence is: II F glue---dispersant
803#---(alkali lye--fire retardant 801#)---mill base.Mix the most mechanically
Process, make the most consistent colloid mixture;Again it is carried out deaeration and filtration, dynamic
Under power effect, (pump or compressed air) is sent to spinning by pipeline, is frozen into just growth in acid bath
After Si, through drawing-off, spinning speed 80m/min, spinneret draft amount 10%, spins dish drawing-off
Amount is 25%, rear road drawing-off amount is 5%, after carry out washing, be centrifuged into spinning cake, solidify, compress and wash
/ drip washing and oiling, dehydration post-drying and become cylinder, packing is finished product.Wherein washing temperature
70 DEG C, solidification treatment fluid temperature is 75-90 DEG C, curing agent 802#Concentration is 33%, oils dense
Spend 1g gram/L.
Embodiment 2: without dye FRC blueness long filament 75D/32F
Prepare mill base: take blue pigment, through extra-fine grinding to particle diameter≤0.4 μm.Above-mentioned process
After pigment 35%, polyvinylpyrrolidone 4%, pure water 61%, add colloid mill grind 3h,
Cool down standby.
Fire-retardant agent liquid, blue mill base contact mixing with viscose glue according to certain weight ratio;Join glue
Ratio: IIF glue 16OOOL;Silicon nitrogen combustion inhibitor 801#2000L;10% potassium hydroxide solution
1000L;Dispersant 803#160L;Blue mill base 100kg.Charging sequence is: II F glue---
Dispersant 803#---(alkali lye--fire retardant 801#)---mill base.Enter the most mechanically
Row mixed processing, makes the most consistent colloid mixture;Again it is carried out deaeration and filtration,
Under dynamic action, (pump or compressed air) is sent to spinning by pipeline, at the beginning of being frozen in acid bath
After growing filament, through drawing-off, spinning speed 80m/min, spinneret draft amount 15%, spins dish
Drawing-off amount is 20%, rear road drawing-off amount is 10%, after carry out washing, be centrifuged into spinning cake, solidification,
Compressing and washing/drip washing and oiling, dehydration post-drying and become cylinder, packing is finished product.Wherein wash
Temperature 70 C, solidification treatment fluid temperature is 75-90 DEG C, curing agent 802#Concentration is 33%, on
Oil concentration 1g gram/L.
It will be understood by those skilled in the art that each method step successively listed in above-described embodiment
Suddenly it is intended merely to serve the purpose of illustrating the invention and be not used to be limited.Therefore these
Step there is no inevitable precedence, the most indispensable.The present invention is only by each claim
Specifically limit.
Claims (1)
1. without contaminating a spinning technique method for flame-retardant viscose fiber colored long filament, including:
The spinning mixture being mixed with first fibre viscose glue by silicon nitrogen combustion inhibitor, mill base is provided, wherein mill base is the suspension dispersible pigment color paste of diameter≤0.4 μm, in first fibre viscose glue, fine (weight) content of first is 8-10%, and the weight ratio of contained first fibre is 36-45% to silicon nitrogen combustion inhibitor with first fibre viscose glue, the weight ratio of contained first fibre is 0.7-2% to mill base with first fibre viscose glue;
The spinning acid bath that is mixed with sodium sulphate by sulfuric acid, zinc sulfate is provided, wherein sulfuric acid concentration be 85-115g/L, zinc sulfate concentration be 9-12g/L, sodium sulfate concentration be 222-268g/L;
By spinning mixture deaeration, filter after sent into by measuring pump and spinning head and spinning acid bath to carry out coagulation forming and spinning drawing to obtain coloured continuous filament yarn and to be wrapped in and spin on dish, wherein spinning acid bath temperature is 38-48 DEG C, spinning speed is 75-80m/min, and spinneret draft amount be 10-15%, to spin dish drawing-off amount be 20-25%, rear road drawing-off amount is 5-10%;
There is provided containing Ti4+、Ca2+The solidification treatment fluid of cation complex solution;
By coloured continuous filament yarn through washing with centrifugal treating to form spinning cake shape long filament;
Spinning cake shape long filament being sent into solidification treatment fluid and carries out solidification process, wherein solidification treatment fluid temperature is 75-90 DEG C;And
Long filament after processing solidification is washed, is dried and packing processes is to obtain finished product coloured yarn,
Wherein spinning mixture viscosity is the 19-36 second, and degree of ripeness is 16-19mL (10%NH4C
L solution),
Wherein mill base prepare as follows:
It is particle diameter≤0.4 μm by natural pigment or Prof. Du Yucang pigment grind;
There is provided polyvinylpyrrolidone as suspension dispersive agent;
Adding in suspension dispersive agent and water the pigment after above-mentioned grinding to form aqueous suspension mill base, wherein specific gravity of pigment is 35-50%, and polyvinylpyrrolidone proportion is 3-8%, and surplus is water;And
Use the colloid mill further grinding distribution of aqueous suspension mill base to preparing 2-4 hour.
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CN201510258077.3A CN104831386B (en) | 2015-05-20 | 2015-05-20 | A kind of spinning technique method without contaminating flame-retardant viscose fiber colored long filament |
PCT/CN2016/082486 WO2016184390A1 (en) | 2015-05-20 | 2016-05-18 | Spinning forming method for coloured flame-retardant viscose filaments and staple fibres without dyeing |
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CN201510258077.3A CN104831386B (en) | 2015-05-20 | 2015-05-20 | A kind of spinning technique method without contaminating flame-retardant viscose fiber colored long filament |
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CN104831386B true CN104831386B (en) | 2016-09-07 |
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Cited By (1)
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CN108754786A (en) * | 2018-07-16 | 2018-11-06 | 北京赛欧兰阻燃纤维有限公司 | A kind of multifunctional flame-proof blanket and preparation method thereof |
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WO2016184390A1 (en) * | 2015-05-20 | 2016-11-24 | 北京赛欧兰阻燃纤维有限公司 | Spinning forming method for coloured flame-retardant viscose filaments and staple fibres without dyeing |
CN106012151B (en) * | 2016-07-26 | 2018-05-01 | 北京赛欧兰阻燃纤维有限公司 | Silicon nitrogen fire retardant viscose short filament and the blended manufactured flame resistant spun staple yarns of PSA fiber |
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CN1740412B (en) * | 2005-09-23 | 2010-11-03 | 陈惠敏 | Making process and product of addition type functional viscose fiber |
US7651590B2 (en) * | 2006-03-03 | 2010-01-26 | Birla Research Institute For Applied Sciences | Flame retardant and glow resistant zinc free cellulose product |
CN100494524C (en) * | 2007-05-17 | 2009-06-03 | 山东海龙股份有限公司 | Method for preparing cellulose and silicon dioxide composite coloured fiber and coloured fiber made thereby |
CN101724926A (en) * | 2009-11-18 | 2010-06-09 | 马晓宁 | Spinning process of environment-friendly flame retarding flat viscose yarn |
CN101701362A (en) * | 2009-11-25 | 2010-05-05 | 河南海洋化纤集团有限公司 | Spinning forming technique of environment-friendly flame-retardant viscose fiber colored filament and staple |
CN103789858B (en) * | 2014-01-27 | 2015-12-30 | 刘承修 | A kind of environment-friendly type thermostable durable flame-retardant fiber and preparation method thereof |
CN104032401B (en) * | 2014-06-27 | 2015-05-20 | 北京赛欧兰阻燃纤维有限公司 | Environment-friendly type fire retardant as well as preparation method and application thereof |
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CN108754786A (en) * | 2018-07-16 | 2018-11-06 | 北京赛欧兰阻燃纤维有限公司 | A kind of multifunctional flame-proof blanket and preparation method thereof |
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