CN104831386A - Spinning forming method of non-dyed flame-retardant viscose colored filament - Google Patents

Spinning forming method of non-dyed flame-retardant viscose colored filament Download PDF

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Publication number
CN104831386A
CN104831386A CN201510258077.3A CN201510258077A CN104831386A CN 104831386 A CN104831386 A CN 104831386A CN 201510258077 A CN201510258077 A CN 201510258077A CN 104831386 A CN104831386 A CN 104831386A
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spinning
mill base
pigment
acid bath
forming method
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CN201510258077.3A
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CN104831386B (en
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刘承修
毕慎平
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Blue Fire Resistance Fibre Of Beijing Sail Co Ltd
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Blue Fire Resistance Fibre Of Beijing Sail Co Ltd
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Priority to PCT/CN2016/082486 priority patent/WO2016184390A1/en
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Abstract

The invention relates to a spinning forming method of non-dyed flame-retardant viscose colored filaments. The spinning forming method comprises the following steps: providing spinning mixed liquid prepared by mixing a silicon-nitrogen flame retardant, color paste and alpha cellulose glue; providing a spinning acid bath prepared by mixing sulfuric acid, zinc sulfate and sodium sulfate; deforming and filtering the spinning mixed liquid, feeding the spinning mixed liquid into the spinning acid bath by virtue of a metering pump and a spinning nozzle, and carrying out solidification forming and spinning drafting so as to obtain colored continuous filaments; providing a curing treatment liquid containing positive ions Ti<4+> and Ca<2+>; curing the colored continuous filaments; and respectively carrying out water washing, drying and packaging on the cured filaments, so as to obtain the finished colored filaments. According to the spinning forming method, a downstream dyeing procedure is omitted, so that the environmental pollution caused by spinning printing and dyeing wastewater as well as the injury caused by dyed products to human bodies are maximally reduced or avoided.

Description

A kind of spinning technique method without the flame-retardant viscose fiber colored long filament of dye
Technical field
The present invention relates to wet spinning forming technology.
Background technology
No matter the equal easy firing of synthetic fiber, viscose or natural cotton fiber catches fire causes fire, and fire resistance fibre can address these problems, especially in viscose, add the Fire resistant viscose fiber that fire retardant is produced, the easily ignitable characteristic of fiber can be improved, avoid fire, reduce property and life injury, also maintain the special performance comfortable and easy to wear that viscose is original.
Due to can produce when mill base and fire retardant coexist in spinning mixture all impacts (such as painted insecure, fire retardant solidification effect is not good and acid bath coagulability difference etc. problem), the fire resistance fibre of current production and sales is all colourless (primary colors) base fibers, carries out dyestuff as required again and (dye) look after being woven into cloth.In this case dyeing waste water and dyeing and printing products unavoidably produce to environment and to health and endanger.
Summary of the invention
The object of this invention is to provide a kind of without the dye spinning technique technique of flame-retardant viscose fiber colored long filament or method, its applicable industrialization and environmental.
Spinning technique method without the flame-retardant viscose fiber colored long filament of dye according to the present invention comprises:
The spinning mixture be mixed with by the fine viscose glue of silicon nitrogen combustion inhibitor, mill base and first is provided, wherein mill base is the suspension dispersible pigment color paste of diameter≤0.4 μm, and the weight ratio of contained first fibre is 36-45% in the fine viscose glue of silicon nitrogen combustion inhibitor and first, contained by mill base and first fibre viscose glue, the weight ratio of first fibre is 0.7-2%;
The spinning acid bath be mixed with by sulfuric acid, zinc sulfate and sodium sulphate is provided, wherein sulfuric acid concentration is 85-115g/L, zinc sulfate concentration is 9-12g/L, sodium sulfate concentration is 222-268g/L;
By spinning mixture deaeration, filter after to be sent in spinning acid bath by measuring pump and spinning head and carry out coagulation forming and spinning drawing spins on dish to obtain coloured continuous filament yarn and to be wrapped in, wherein spinning acid bath temperature is 38-48 DEG C, spinning speed is 75-80m/min, and spinneret draft amount is 10-15%, spins that dish drawing-off amount is 20-25%, rear road drawing-off amount is 5-10%;
There is provided containing Ti 4+, Ca 2+the solidification treatment fluid of cation complex solution;
By coloured continuous filament yarn through washing and centrifugal treating to form spinning cake shape long filament;
Spinning cake shape long filament is sent into solidification treatment fluid and be cured process, wherein solidifying treatment fluid temperature is 75-90 DEG C; And
Process is washed, dries and packed to long filament after solidification process respectively again to obtain finished product coloured yarn.
In one particular embodiment of the present invention, spinning mixture viscosity (falling ball method) is preferably 19-36 second, and degree of ripeness is preferably 9-16ml (10%NH 4cL solution).Above-mentioned viscosity and degree of ripeness are demarcated unit and are known in the art.
In a preferred embodiment of the invention, spinneret draft amount is set to 13%, spin that dish drawing-off amount is 25%, rear road drawing-off amount is 5%.Each drawing-off amount above-mentioned is well known to the skilled person and usual.
In one particular embodiment of the present invention, mill base is preferably as follows preparation:
Be particle diameter≤0.4 μm by natural pigment or Prof. Du Yucang pigment grind;
There is provided polyvinylpyrrolidone as suspension dispersive agent; And
Added by pigment after above-mentioned grinding to form aqueous suspension mill base in suspension dispersive agent and water, wherein specific gravity of pigment is 35-50%, and polyvinylpyrrolidone proportion is 3-8%, and surplus is water.
In this embodiment, can also use colloid mill to preparation aqueous suspension mill base or the further grinding distribution 2-4 of colloid mill base hour to improve the colloidal dispersions uniformity.
In the fine viscose glue of the first 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 adopt Sail blue fire resistance fibre Co., Ltd in Beijing to produce and sell 802 #prepared by curing agent, concentration (curing agent weight content) is preferably 30-60%, is more preferably 32%-35%, most preferably is 33%.
The silicon nitrogen combustion inhibitor used in the present invention can adopt organosilan to be hydrolyzed dispersion liquid, and its chemical formula is [Me 2onSiO 2]+[--CONH], wherein Me representation metal ion, SiO 2content is 9.23-53%; Acid amides [--CONH] content is 4.3-27%.About silicon nitrogen combustion inhibitor, can see patent application CN104032401A and CN103789858A before applicant, at this respectively to introduce the full contents of these two applications see mode.In a preferred embodiment of the invention, silicon nitrogen combustion inhibitor adopts Sail blue fire resistance fibre Co., Ltd in Beijing to produce and sell 801 #silicon nitrogen combustion inhibitor.
Prepared according to the methods of the invention long filament specification can within the pole wide region of 70D-500D (the tow weight of representation unit length) and 15-60F (representing the monofilament quantity forming every beam filament).
In a preferred embodiment of the invention, spinning mixture can also comprise alkali and dispersant.Alkali can be NaOH or potassium hydroxide, and the concentration in spinning mixture is 7-8%.Dispersant then can preferably use Sail blue fire resistance fibre Co., Ltd in Beijing to produce and sell 803 #dispersant.
In a preferred embodiment of the invention, the water temperature of each washing process can be 60-80 DEG C.
In other embodiments of the invention, oiling treatment (the preferred 0.8-1.5g/L of Spinning Oil Concentration) can also be comprised after solidification process.In addition, the process of conventional one-tenth cylinder can also be comprised between oven dry and packaging process.
According to spinning technique technique of the present invention, owing to have employed unique spinning mixture, coordinate selected spinning acid bath and/or solidification treatment fluid, and well-designed process conditions, thus achieve suitability for industrialized production coloured yarn and there is the good advantage of firm coloration, fire retardant solidification effect and acid bath coagulation result.
In addition, the present invention also has the following advantages:
Owing to have employed nitrogen silicon series environmental protection fire retarding agent, thus fiber has environmental protection performance, meets national energy-saving environmental protection policy; And
Owing to have employed, mill base is effectively mixed in anti-flaming viscose the technique producing fire-retardant coloured yarn, not only eliminates the dyeing process in downstream, and amplitude peak can reduce or avoid textile printing and dyeing wastewater to the pollution of environment and dyeing product to the harm of human body.
Detailed description of the invention
(1) spinning mixture is mixed with by fire retardant and mill base and the fine viscose glue of first
Fire-retardant agent liquid, mill base are respectively 36-45%, 0.7-2% to the fine addition of the first in viscose glue according to weight ratio.After interpolation, strong agitation makes it to become all consistent colloid mixture; Then deaeration and filtration is carried out.Spinning mixture viscosity is 19-36 second, and degree of ripeness is 16-19ml (10%NH 4cL solution).Fire retardant adopts nitrogen silicon system environmental protection fire retarding agent.Mill base is the suspension dispersible pigment color paste of diameter≤0.4 μm, makes suspension dispersive agent by polyvinylpyrrolidone, colloid mill grinding distribution 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 reacted with acid bath by measuring pump and spinning head in spinning machine acid bath groove, coagulation forming, spinning speed 75-80m/min, spinneret draft amount is 10-15%, spin that dish drawing-off amount is 20-25%, rear road drawing-off amount is 5-10%.
(4) washing, centrifugal and curing process process
Flame-retardant viscose fiber colored long filament after drawing-off enters drip washing with spinning cake form or compresses and washes flow process and be cured process at this after washing and centrifugal treating.Described solidification treatment fluid temperature is 75-90 DEG C, and the curative concentration of employing is 30-60%.Described curing agent is for containing Ti 4+, Ca 2+etc. cationic complex solution.
(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 Fire resistant viscose fiber red filaments 250D/60F
Prepare mill base: get red pigment, through extra-fine grinding to particle diameter≤0.4 μm.Pigment 30% after above-mentioned process, polyvinylpyrrolidone 6%, pure water 64%, adds colloid mill grinding 3h, cools for subsequent use.
Fire-retardant agent liquid, red mill base and viscose glue contact according to certain weight ratio and mix; Join glue ratio: IIF glue is (containing first fibre 8.2%; Equally can purchased from the blue fire resistance fibre Co., Ltd of Beijing Sail) 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.Then carry out mixed processing mechanically, make it to become all consistent colloid mixture; Again deaeration and filtration are carried out to it, under dynamic action, (pump or compressed air) is sent to spinning by pipeline, be frozen into first growing filament in acid bath after, through drawing-off, spinning speed 80m/min, spinneret draft amount 10%, spins that 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 upper wet goods, dehydration post-drying and one-tenth 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%, upper oil concentration 1g gram/L.
embodiment 2: without the blue long filament 75D/32F of dye Fire resistant viscose fiber
Prepare mill base: get blue pigment, through extra-fine grinding to particle diameter≤0.4 μm.Pigment 35% after above-mentioned process, polyvinylpyrrolidone 4%, pure water 61%, adds colloid mill grinding 3h, cools for subsequent use.
Fire-retardant agent liquid, blue mill base and viscose glue contact according to certain weight ratio and mix; 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.Then carry out mixed processing mechanically, make it to become all consistent colloid mixture; Again deaeration and filtration are carried out to it, under dynamic action, (pump or compressed air) is sent to spinning by pipeline, be frozen into first growing filament in acid bath after, through drawing-off, spinning speed 80m/min, spinneret draft amount 15%, spins that dish drawing-off amount is 20%, rear road drawing-off amount is 10%, after carry out washing, be centrifuged into spinning cake, solidify, compress and wash/drip washing and upper wet goods, dehydration post-drying and one-tenth 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%, upper 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 is just not used to be limited to play explanation object of the present invention.Therefore these steps there is no inevitable precedence, also not indispensable.The present invention is only specifically limited by each claim.

Claims (3)

1., without a spinning technique method for the flame-retardant viscose fiber colored long filament of dye, comprising:
The spinning mixture be mixed with by the fine viscose glue of silicon nitrogen combustion inhibitor, mill base and first is provided, wherein mill base is the suspension dispersible pigment color paste of diameter≤0.4 μm, and the weight ratio of contained first fibre is 36-45% in the fine viscose glue of silicon nitrogen combustion inhibitor and first, contained by mill base and first fibre viscose glue, the weight ratio of first fibre is 0.7-2%;
The spinning acid bath be mixed with by sulfuric acid, zinc sulfate and sodium sulphate is provided, wherein sulfuric acid concentration is 85-115g/L, zinc sulfate concentration is 9-12g/L, sodium sulfate concentration is 222-268g/L;
By spinning mixture deaeration, filter after to be sent in spinning acid bath by measuring pump and spinning head and carry out coagulation forming and spinning drawing spins on dish to obtain coloured continuous filament yarn and to be wrapped in, wherein spinning acid bath temperature is 38-48 DEG C, spinning speed is 75-80m/min, and spinneret draft amount is 10-15%, spins that dish drawing-off amount is 20-25%, rear road drawing-off amount is 5-10%;
There is provided containing Ti 4+, Ca 2+the solidification treatment fluid of cation complex solution;
By coloured continuous filament yarn through washing and centrifugal treating to form spinning cake shape long filament;
Spinning cake shape long filament is sent into solidification treatment fluid and be cured process, wherein solidifying treatment fluid temperature is 75-90 DEG C; And
Process is washed, dries and packed to long filament after solidification process respectively again to obtain finished product coloured yarn.
2. method according to claim 1, wherein spinning mixture viscosity is 19-36 second, and degree of ripeness is 16-19ml (10%NH 4cL solution).
3. method according to claim 1, being wherein prepared as follows of mill base:
Be particle diameter≤0.4 μm by natural pigment or Prof. Du Yucang pigment grind;
There is provided polyvinylpyrrolidone as suspension dispersive agent; And
Added by pigment after above-mentioned grinding to form aqueous suspension mill base in suspension dispersive agent and water, wherein specific gravity of pigment is 35-50%, and polyvinylpyrrolidone proportion is 3-8%, and surplus is water.
CN201510258077.3A 2015-05-20 2015-05-20 A kind of spinning technique method without contaminating flame-retardant viscose fiber colored long filament Expired - Fee Related CN104831386B (en)

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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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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106012151A (en) * 2016-07-26 2016-10-12 北京赛欧兰阻燃纤维有限公司 Anti-flaming staple fiber yarn blended from silicon-nitrogen anti-flaming viscose staple fibers and polysulfonamide
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
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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CN1740412A (en) * 2005-09-23 2006-03-01 陈惠敏 Making process and product of addition type functional viscose fiber
US20070205402A1 (en) * 2006-03-03 2007-09-06 Birla Research Institute For Applied Sciences Flame retardant and glow resistant zinc free cellulose product
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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
CN101724926A (en) * 2009-11-18 2010-06-09 马晓宁 Spinning process of environment-friendly flame retarding flat viscose yarn
CN103789858A (en) * 2014-01-27 2014-05-14 刘承修 Environment-friendly high-temperature-resistant durable flame retardant fibers and preparation method thereof
CN104032401A (en) * 2014-06-27 2014-09-10 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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Publication number Priority date Publication date Assignee Title
CN1740412A (en) * 2005-09-23 2006-03-01 陈惠敏 Making process and product of addition type functional viscose fiber
US20070205402A1 (en) * 2006-03-03 2007-09-06 Birla Research Institute For Applied Sciences Flame retardant and glow resistant zinc free cellulose product
CN101070633A (en) * 2007-05-17 2007-11-14 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
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106012151A (en) * 2016-07-26 2016-10-12 北京赛欧兰阻燃纤维有限公司 Anti-flaming staple fiber yarn blended from silicon-nitrogen anti-flaming viscose staple fibers and polysulfonamide
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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