CN107557890A - A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn - Google Patents

A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn Download PDF

Info

Publication number
CN107557890A
CN107557890A CN201710791197.9A CN201710791197A CN107557890A CN 107557890 A CN107557890 A CN 107557890A CN 201710791197 A CN201710791197 A CN 201710791197A CN 107557890 A CN107557890 A CN 107557890A
Authority
CN
China
Prior art keywords
spinning
retardant
viscose
solution
plate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710791197.9A
Other languages
Chinese (zh)
Other versions
CN107557890B (en
Inventor
唐金钟
夏长林
王云
邱林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yibin Grace Group Co Ltd
Yibin Haisite Fiber Co Ltd
Original Assignee
Yibin Grace Group Co Ltd
Yibin Haisite Fiber Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yibin Grace Group Co Ltd, Yibin Haisite Fiber Co Ltd filed Critical Yibin Grace Group Co Ltd
Priority to CN201710791197.9A priority Critical patent/CN107557890B/en
Publication of CN107557890A publication Critical patent/CN107557890A/en
Application granted granted Critical
Publication of CN107557890B publication Critical patent/CN107557890B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Artificial Filaments (AREA)

Abstract

The present invention provides a kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:A pulp materials obtain alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;B alkali cellulose carries out experienced, sulfonation, dissolving, deaeration, maturation processing;In maturation, nitrogen phosphorus flame retardant slurry is added into viscose solution makes the amount of fire retardant be 0.5~3% of first fibre content in viscose glue, then the amount of fire retardant is made to reach setting value adding nitrogen phosphorus flame retardant slurry after one KKF is filtered, in the viscose solution that is obtained after two plate-frame filterings, after three plate-frame filterings respectively, then the sheet frames of Jing Jin tetra- are filtrated to get for spinning spinning solution;C is extruded for spinning spinning solution by the spinning head of spinning-drawing machine, obtains tow through spinning bath solidification, drafting machine drawing-off, tow is refined, dries to obtain anti-flaming viscose long filament.The technique makes fire retardant good dispersion in viscose glue, with being well mixed for viscose glue, avoids impacting the intensity of fiber to greatest extent.

Description

A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn
Technical field
The present invention relates to the production of viscose filament yarn, is specifically related to a kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn.
Background technology
The semicontinuous spinning technique flow of viscose filament yarn is:Pulp material is through impregnating, squeezing, crushing, experienced, yellow, molten Solution, deaeration, maturation, spinning solution is filtrated to get, spinning solution is glued by measuring pump, spinning head, acid bath, drawing-off and postprocessing working procedures Glue long filament, at present, the semicontinuous spinning technique of viscose filament yarn is ripe, and yield is big, purposes pipe, but viscose filament yarn chance fire easily fires Burn, limit its use in the field such as life and industry, therefore, anti-flaming viscose long filament is largely developed, FRC Preparing can use blending method and post processing flame-retardant modified, and wherein blending method is related to the preparation technology of stoste, and technological transformation is complicated, needs High investment.And because Forming of Viscose Rayon process is complicated, therefore it is required that the fire retardant added can not be with viscose glue stoste and solidifying Gu some adverse effects occur for bath, and can not be separated out in spinning and last handling process, in addition, difficulty should not be caused to spinning. Especially, by the way that the FRC of production is blended, due to adding substantial amounts of fire retardant, the thing of fire resistance fibre has been had a strong impact on Mechanical performance is managed, and feel etc. takes new energy, limits its use in fields such as dress ornament, underwears.Viscose rayon post-processes Fire-retardant modification, finished fiber excellent flame retardancy, every physical index is good, while it is fine to solve existing anti-flaming viscose Low intensity is tieed up, is not easy to shape, it is difficult to carry out the deficiency of textile process.But the resistance in the prior art, prepared using post-processing technology Fiber is fired, there is that flame retardant effect is undesirable and the unabiding bottleneck problem of fire resistance again, and fibre whiteness after flame retardant treatment The problem of reduction, limit the popularization of this technology.Therefore, it is main at present that anti-flaming viscose fibre is prepared using blending production method Dimension, and according to the same of fire retardant species, fire resistance fibre common are nitrogen phosphorous flame-retardant fiber, silicon nitrogen system anti-flaming viscose etc.;Such as Wu Great waves,《The anti-flaming viscose long filament spinning experiment of silicon nitrogen system》, staple fibre, the 3rd phase in 2013, the technique by silicon nitrogenated flame retardant, help Agent, dispersant are deployed into uniform and stable solution, then are added to by a certain percentage under stirring after yellow in mixing of viscose, By being sufficiently mixed and disperseing, make itself and cellulose graft, disintegrating and regeneration reaction, generation anti-flaming viscose length are carried out by coagulating bath Silk, the experiment points out that the addition of fire retardant has a great influence to the physical and mechanical properties of viscose rayon, particularly dry fracture strength and Wet breaking strength has significant change, and comprehensive mechanical property declines, and in actual industrialization production, do fracture strength and wet fracture Intensity declines more.Therefore, intensity, the spinning of fiber how are ensured during FRC is prepared using blending method During spinnability, the washability of fiber and last anti-flammability this combination property get a promotion, technical staff takes Different measures, as CN102409420A patent document in provide a kind of composite silicon-based flame-retardant viscose fiber and its producer Method, belong to field of viscose fiber.Composite silicon-based flame-retardant viscose fiber provided by the invention is composed of the following components:Linear silicon systems resistance 52~82 parts of viscose before 13~28 parts of agent of combustion, 3~12 parts of auxiliary flame retardant, 2~8 parts of silane coupler, spinning, it is multiple by preparing Silicon-series five-retardant liquid, fire retardant liquid are closed with viscose blending before spinning and using conventional spinning, post processing, drying and is packed To composite silicon-based flame-retardant viscose fiber.The composite silicon-based flame-retardant viscose fiber of the present invention improves, improves FRC Mechanical property(It is dry to bring up between 2.03~2.21 by force), heat resistance, anti-flammability, preparation method solves FRC can The problem of property spun.The fire resistant fluid composition added in this method is too many, includes linear silicon-series five-retardant, auxiliary flame retardant etc., group Into complexity, higher requirement is possessed for mixing uniformity.And the technique fire retardant is the research to silicon-series five-retardant.Fire retardant It is fire-retardant compared to halogen system that the difference of species can influence index, the nitrogen phosphorus flame retardants such as the intensity of obtained fire resistance fibre, anti-flammability Fiber contamination is big, and market prospects are little, has pollution small, possesses the bigger market space and market potential, but at present using altogether Mixed method, which adds, has sub-wire broken end seriously when nitrogen phosphorus flame retardant is prepared into viscose rayon, the property spun is poor, and shower nozzle blocks serious, fiber number Serious unqualified, obtained fire-retardant yarn strength is far below the intensity of silicon-series five-retardant, only 1.0cn/dtex.Therefore, it is necessary to It is a kind of to solve the problems, such as the production technology for the nitrogen phosphorous flame-retardant fiber that above-mentioned nitrogen phosphorus fire resistance fibre is present.
The content of the invention
Present invention seek to address that existing nitrogen phosphorous flame-retardant viscose filament yarn filters before spinning is directly added into nitrogen phosphorus system in spinning solution Fire retardant causes sub-wire in spinning process to break end seriously, and the property spun is poor, and shower nozzle blocks seriously, and fiber number is seriously unqualified, obtained resistance Fire the problem of yarn strength is low, there is provided a kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, by carrying out composition point to mill base Analysis, uniformity processing, Study on dispersity allow fire retardant good dispersion in viscose glue, and particle is small and uniform, equal with the mixing of viscose glue It is even, avoid impacting the intensity of fiber to greatest extent.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions;
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 0.5~3% of first fibre content in viscose glue, after being well mixed, into one Road KKF is filtered, and adds nitrogen phosphorus flame retardant slurry again in the viscose solution being filtrated to get, the amount for making fire retardant is first fibre content 3~7%, well mixed to enter two plate-frame filterings, addition nitrogen phosphorus flame retardant in the viscose solution that two sheet frames are filtrated to get Slurry, the amount for making fire retardant is the 7~12% of first fibre content, well mixed to enter three plate-frame filterings, is obtained through three plate-frame filterings To viscose solution in add nitrogen phosphorus flame retardant slurry make fire retardant amount be first fibre content 12~25%, be well mixed into Enter four plate-frame filterings, obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
It is the 12~25% of first fibre content that four sheet frame, which is filtrated to get for spinning flame retardant agent content in spinning solution,.
The nitrogen phosphorus flame retardant slurry is that the dispersant that 0.1~2 % is added into fire retardant is ground and is prepared, Grain diameter≤0.327 μm of fire retardant in the nitrogen phosphorus flame retardant slurry.
The anti-flaming viscose long filament has following index systems:The cn/dtex of intensity 1.5~2.1, fiber number 60D~150D, Anti-flammability:Limited oxygen index >=30%, after flame time≤3 second, smoldering time≤3 second.
In step B, the filtering accuracy of one described of KKF filterings is 25~30 μm, two plate-frame filtering, three Road plate-frame filtering, the filtering accuracy of four plate-frame filterings are 8~15 μm.
In stepb, the dispersant is scattered chelating agent HA~AL.With stronger dispersive property, belong to a kind of table Face activating agent.The viscose glue that fire retardant spinning solution is used when configuring is controlled in strict accordance with big production viscose glue production technology.Such as it In involve dipping, grinding, squeezing, experienced, yellow etc..Sulfuric acid, sodium sulphate, zinc sulfate and acid bath temperature are tight in spinning bath Lattice perform according to big production, and temperature is 50~55 DEG C, 130~140g/l of sulfuric acid content, 240~255g/l of sodium sulphate content, sulphur Sour 10~12g/l of Zn content.
The invention has the advantages that:
1st, the content needs because of fire retardant in fire-retardant silk, which have reached more than 12%, just preferable flame retardant effect, and largely hinders If combustion agent is disposably added in viscose glue, because viscose glue viscosity itself is higher, in mixing, normal agitation is difficult to fire resistant fluid It is well mixed with viscose glue, produces a large amount of foamings but if increasing stirring dynamics and easily causing viscose glue again, influence spinnability, the present invention Respectively in maturation, after one of KKF filtering, after two plate-frame filterings, after three plate-frame filterings, add and hinder after four plate-frame filterings Flame retardant agent content in combustion agent slurry and the viscose glue that makes to obtain each time gradually increases, it is this in batches, it is laddering(Fire retardant Amount)Add and ensure that the nitrogen phosphorous flame-retardant liquid energy of addition enough being distributed in viscose solution evenly, ensure the resistance of viscose filament yarn Spinnability higher fire retardant spinning solution is formed while combustion property.It is proven, according to the specific viscose solution of the present invention Prepare, prepared and spinning process for spinning spinning solution, realize the sub-wire rate of viscose filament yarn in spinning process, end breakage rate, change spinneret Head rate is small, improves production efficiency, reduces production cost, and the intensity of obtained viscose filament yarn is intensity up to 1.5~2.1 cn/ Dtex, fiber number are 60~150D, solve the nitrogen phosphorous flame-retardant viscose filament yarn low intensity that prior art produces to obtain, and fiber number is big Problem;And find the nitrogen phosphorous flame-retardant viscose rayon of fiber that obtained viscose filament yarn is prepared compared with prior art more resistant to Wash, extend the service life of fiber.
2nd, it is the 20% of first fibre content that the present invention, which controls the flame retardant agent content in four sheet frames are filtrated to get for spinning spinning solution, It is further ensured that the spinnability of spinning solution and the anti-flammability of obtained viscose filament yarn.
3rd, nitrogen phosphorus flame retardant slurry of the invention is that the dispersant that 0.1~2 % is added into fire retardant is ground system It is standby to obtain, after grinding in nitrogen phosphorus flame retardant slurry fire retardant grain diameter≤0.327 μm, so, not only increase fire-retardant Dispersiveness of the agent in viscose solution, while fire-retardant particles particle diameter≤0.327 μm can effectively avoid spinning head in spinning process Blockage problem, improve production efficiency.
4th, of the invention, the filtering accuracy of one of KKF filtering is 25~30 μm, two plate-frame filterings, three plate-frame filterings, four The filtering accuracy of road plate-frame filtering is 8~15 μm.By the control of the filtering accuracy, make filtering while filter efficiency is ensured The flame retardant agent content in viscose glue afterwards reaches the scope of setting, so as to ensure that anti-flammability.
Embodiment
The present invention is described in detail with reference to specific embodiment.
Embodiment 1
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 0.5% of first fibre content in viscose glue, after being well mixed, into together KKF is filtered, and nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, and the amount for making fire retardant is first fibre content 3%, it is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, The amount for making fire retardant is the 12% of first fibre content, well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames Nitrogen phosphorus flame retardant slurry is added in solution makes the amount of fire retardant be the 12% of first fibre content, well mixed to enter four sheet frame mistakes Filter, obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
Embodiment 2
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 3% of first fibre content in viscose glue, after being well mixed, into one of KKF Filtering, nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, the amount for making fire retardant is the 7% of first fibre content, It is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, is made The amount of fire retardant is the 12% of first fibre content, and well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames is molten Nitrogen phosphorus flame retardant slurry is added in liquid makes the amount of fire retardant be the 25% of first fibre content, well mixed to enter four plate-frame filterings, Obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
Embodiment 3
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 1.5% of first fibre content in viscose glue, after being well mixed, into together KKF is filtered, and nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, and the amount for making fire retardant is first fibre content 5%, it is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, The amount for making fire retardant is the 10% of first fibre content, well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames Nitrogen phosphorus flame retardant slurry is added in solution makes the amount of fire retardant be the 20% of first fibre content, well mixed to enter four sheet frame mistakes Filter, obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
Embodiment 4
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 1.5% of first fibre content in viscose glue, after being well mixed, into together KKF is filtered, and nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, and the amount for making fire retardant is first fibre content 3%, it is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, The amount for making fire retardant is the 12% of first fibre content, well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames Nitrogen phosphorus flame retardant slurry is added in solution makes the amount of fire retardant be the 25% of first fibre content, well mixed to enter four sheet frame mistakes Filter, obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
The nitrogen phosphorus flame retardant slurry is that the dispersant that 0.1 % is added into fire retardant is ground and is prepared, institute State grain diameter≤0.327 μm of fire retardant in nitrogen phosphorus flame retardant slurry.
In step B, the filtering accuracy of one described of KKF filterings is 25 μm, two plate-frame filtering, three guidance tapes Frame filtering, the filtering accuracy of four plate-frame filterings are 8 μm.
In stepb, the dispersant is scattered chelating agent HA~AL.
Sulfuric acid, sodium sulphate, zinc sulfate and acid bath temperature perform in strict accordance with big production in spinning bath, the present embodiment temperature For 50~55 DEG C, 130~140g/l of sulfuric acid content, 240~255g/l of sodium sulphate content, 10~12g/l of zinc sulfate content.
Embodiment 5
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 2% of first fibre content in viscose glue, after being well mixed, into one of KKF Filtering, nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, the amount for making fire retardant is the 5% of first fibre content, It is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, is made The amount of fire retardant is the 12% of first fibre content, and well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames is molten Nitrogen phosphorus flame retardant slurry is added in liquid makes the amount of fire retardant be the 15% of first fibre content, well mixed to enter four plate-frame filterings, Obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
The nitrogen phosphorus flame retardant slurry is to add 2% dispersant into fire retardant to be ground and be prepared, the nitrogen Grain diameter≤0.327 μm of fire retardant in phosphorus flame retardant slurry.
In step B, the filtering accuracy of one described of KKF filterings is 30 μm, two plate-frame filtering, three guidance tapes Frame filtering, the filtering accuracy of four plate-frame filterings are 8 μm.
In stepb, the dispersant is scattered chelating agent HA~AL.Sulfuric acid in spinning bath, sodium sulphate, zinc sulfate and Acid bath temperature performs in strict accordance with big production, and temperature is 50~55 DEG C, 130~140g/l of sulfuric acid content, and sodium sulphate content 240~ 255g/l, 10~12g/l of zinc sulfate content.
Embodiment 6
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 1% of first fibre content in viscose glue, after being well mixed, into one of KKF Filtering, nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, the amount for making fire retardant is the 6% of first fibre content, It is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, is made The amount of fire retardant is the 10% of first fibre content, and well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames is molten Nitrogen phosphorus flame retardant slurry is added in liquid makes the amount of fire retardant be the 23% of first fibre content, well mixed to enter four plate-frame filterings, Obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
The nitrogen phosphorus flame retardant slurry is to add 0.8% dispersant into fire retardant to be ground and be prepared, described Grain diameter≤0.327 μm of fire retardant in nitrogen phosphorus flame retardant slurry.
In step B, the filtering accuracy of one described of KKF filterings is 28 μm, two plate-frame filtering, three guidance tapes Frame filtering, the filtering accuracy of four plate-frame filterings are 12 μm.
In stepb, the dispersant is scattered chelating agent HA~AL.Sulfuric acid in spinning bath, sodium sulphate, zinc sulfate and Acid bath temperature performs in strict accordance with big production, and temperature is 50~55 DEG C, 130~140g/l of sulfuric acid content, and sodium sulphate content 240~ 255g/l, 10~12g/l of zinc sulfate content.
Embodiment 7
A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn, comprises the steps:
A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 3% of first fibre content in viscose glue, after being well mixed, into one of KKF Filtering, nitrogen phosphorus flame retardant slurry is added again in the viscose solution being filtrated to get, the amount for making fire retardant is the 5% of first fibre content, It is well mixed to enter two plate-frame filterings, nitrogen phosphorus flame retardant slurry is added in the viscose solution that two sheet frames are filtrated to get, is made The amount of fire retardant is the 12% of first fibre content, and well mixed to enter three plate-frame filterings, the viscose glue being filtrated to get through three sheet frames is molten Nitrogen phosphorus flame retardant slurry is added in liquid makes the amount of fire retardant be the 18% of first fibre content, well mixed to enter four plate-frame filterings, Obtain for spinning spinning solution;
C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
The nitrogen phosphorus flame retardant slurry is to add 2% dispersant into fire retardant to be ground and be prepared, the nitrogen Grain diameter≤0.327 μm of fire retardant in phosphorus flame retardant slurry.
In step B, the filtering accuracy of one described of KKF filterings is 30 μm, two plate-frame filtering, three guidance tapes Frame filtering, the filtering accuracy of four plate-frame filterings are 10 μm.
In stepb, the dispersant is scattered chelating agent HA~AL.With stronger dispersive property, belong to a kind of table Face activating agent.The viscose glue that fire retardant spinning solution is used when configuring is controlled in strict accordance with big production viscose glue production technology.Such as it In involve dipping, grinding, squeezing, experienced, yellow etc..Sulfuric acid, sodium sulphate, zinc sulfate and acid bath temperature are tight in spinning bath Lattice perform according to big production, and temperature is 50~55 DEG C, 130~140g/l of sulfuric acid content, 240~255g/l of sodium sulphate content, sulphur Sour 10~12g/l of Zn content.
By the intensity of the viscose filament yarn obtained in above-described embodiment 1~7, fiber number, anti-flammability, change spinning head rate, strand breaks Head rate, sub-wire rate and washability, statistics are in table 1 below;
Meanwhile in order to better illustrate the present invention, the present invention provides a kind of life of the nitrogen phosphorous flame-retardant viscose filament yarn of prior art Production. art group as a comparison, its technique to prepare spinning solution, spinning identical with the present invention, fire retardant machine flame retardant paste prepare with The present invention is identical, and difference is, contrast groups disposably add the fire retardant of set amount in the spinning solution being prepared, then By one of plate-frame filtering, 12 μm of filtering accuracy is filtrated to get for spinning spinning solution.Contrast groups 1 are set respectively:Nitrogen phosphorus flame retardant Addition is 12%, contrast groups 2, and nitrogen phosphorus flame retardant addition is 15%, contrast groups 3, and nitrogen phosphorus flame retardant addition is 20%, Contrast groups 4, retardant load level 25%, above-mentioned flame retardant amount are the percentage of first fibre content in spinning solution.By above-mentioned contrast groups The correlated performance for the viscose filament yarn for producing to obtain in 1~4 is counted in table 1.
From upper table data, obtained very using the inventive method viscose filament yarn intensity that method produces to obtain compared with prior art Big raising, flame retardant-effective are guaranteed, and under the inventive method, in spinning process, it changes spinning head rate, strand breaks Frequently prior art is low for head rate, spinline breakage rate, effectively raises production efficiency.

Claims (6)

  1. A kind of 1. production technology of nitrogen phosphorous flame-retardant viscose filament yarn, it is characterised in that:Comprise the steps:
    A, pulp material obtains alkali cellulose through soda-dip, grinder grinding, squeezing, pulverization process;
    B, step A is obtained into alkali cellulose and carries out experienced, sulfonation, dissolving, deaeration, maturation processing, in maturation, to viscose solution The middle nitrogen phosphorus flame retardant slurry that adds makes the amount of fire retardant be 0.5~3% of first fibre content in viscose glue, after being well mixed, into one Road KKF is filtered, and adds nitrogen phosphorus flame retardant slurry again in the viscose solution being filtrated to get, the amount for making fire retardant is first fibre content 3~7%, well mixed to enter two plate-frame filterings, addition nitrogen phosphorus flame retardant in the viscose solution that two sheet frames are filtrated to get Slurry, the amount for making fire retardant is the 7~12% of first fibre content, well mixed to enter three plate-frame filterings, is obtained through three plate-frame filterings To viscose solution in add nitrogen phosphorus flame retardant slurry make fire retardant amount be first fibre content 12~25%, be well mixed into Enter four plate-frame filterings, obtain for spinning spinning solution;
    C, step B is obtained being sent into spinning-drawing machine for spinning spinning solution, solidified by the thread of the spinning head extrusion of spinning-drawing machine through spinning bath, Drafting machine drawing-off obtains tow, and tow is refined, drying obtains anti-flaming viscose long filament.
  2. A kind of 2. production technology of nitrogen phosphorous flame-retardant viscose filament yarn according to claim 1, it is characterised in that:Described four It is the 12~25% of first fibre content that plate-frame filtering, which is obtained for spinning flame retardant agent content in spinning solution,.
  3. A kind of 3. production technology of nitrogen phosphorous flame-retardant viscose filament yarn according to claim 1, it is characterised in that:The nitrogen phosphorus Flame retardant slurry is that the dispersant that 0.1~2 % is added into fire retardant is ground and is prepared, the nitrogen phosphorus flame retardant Grain diameter≤0.327 μm of fire retardant in slurry.
  4. A kind of 4. production technology of nitrogen phosphorous flame-retardant viscose filament yarn according to claim 1, it is characterised in that:It is described fire-retardant Viscose filament yarn has following index systems:1.5~2.1cn/dtex of intensity, fiber number 60D~150D, anti-flammability:Limited oxygen index >=30%, after flame time≤3 second, smoldering time≤3 second.
  5. A kind of 5. production technology of nitrogen phosphorous flame-retardant viscose filament yarn according to claim 1, it is characterised in that:In step B In, the filtering accuracy of one described of KKF filterings is 25~30 μm, two plate-frame filtering, three plate-frame filterings, four guidance tapes The filtering accuracy of frame filtering is 8~15 μm.
  6. A kind of 6. production technology of nitrogen phosphorous flame-retardant viscose filament yarn according to claim 3, it is characterised in that:It is described scattered Agent is scattered chelating agent HA-AL.
CN201710791197.9A 2017-09-05 2017-09-05 Production process of nitrogen-phosphorus flame-retardant viscose filament yarn Active CN107557890B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710791197.9A CN107557890B (en) 2017-09-05 2017-09-05 Production process of nitrogen-phosphorus flame-retardant viscose filament yarn

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710791197.9A CN107557890B (en) 2017-09-05 2017-09-05 Production process of nitrogen-phosphorus flame-retardant viscose filament yarn

Publications (2)

Publication Number Publication Date
CN107557890A true CN107557890A (en) 2018-01-09
CN107557890B CN107557890B (en) 2020-04-03

Family

ID=60979282

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710791197.9A Active CN107557890B (en) 2017-09-05 2017-09-05 Production process of nitrogen-phosphorus flame-retardant viscose filament yarn

Country Status (1)

Country Link
CN (1) CN107557890B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111304767A (en) * 2020-02-17 2020-06-19 河北吉藁化纤有限责任公司 Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber
CN112831852A (en) * 2020-12-31 2021-05-25 宜宾海丝特纤维有限责任公司 Production process for continuously spinning superfine filaments
CN116285013A (en) * 2023-03-15 2023-06-23 赛得利(江苏)纤维有限公司 Flame-retardant viscose production process

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1540047A (en) * 2003-10-29 2004-10-27 冷纯廷 Method for producing Nano fire resistant and fire retardant fiber
CN1847476A (en) * 2006-05-12 2006-10-18 山东海龙股份有限公司 Technological process of producing fire retardant antiflux fiber
CN1904156A (en) * 2006-07-31 2007-01-31 唐山三友集团化纤有限公司 Fire retardant viscose short filament and its production technology
CN101037812A (en) * 2007-04-06 2007-09-19 山东海龙股份有限公司 Melt-resistant flame-proof cellulose viscose and method for making same
CN102352539A (en) * 2011-07-27 2012-02-15 杭州奥通特种纤维技术有限公司 Manufacturing method of silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber
CN103789858A (en) * 2014-01-27 2014-05-14 刘承修 Environment-friendly high-temperature-resistant durable flame retardant fibers and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1540047A (en) * 2003-10-29 2004-10-27 冷纯廷 Method for producing Nano fire resistant and fire retardant fiber
CN1847476A (en) * 2006-05-12 2006-10-18 山东海龙股份有限公司 Technological process of producing fire retardant antiflux fiber
CN1904156A (en) * 2006-07-31 2007-01-31 唐山三友集团化纤有限公司 Fire retardant viscose short filament and its production technology
CN101037812A (en) * 2007-04-06 2007-09-19 山东海龙股份有限公司 Melt-resistant flame-proof cellulose viscose and method for making same
CN102352539A (en) * 2011-07-27 2012-02-15 杭州奥通特种纤维技术有限公司 Manufacturing method of silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber
CN103789858A (en) * 2014-01-27 2014-05-14 刘承修 Environment-friendly high-temperature-resistant durable flame retardant fibers and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111304767A (en) * 2020-02-17 2020-06-19 河北吉藁化纤有限责任公司 Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber
CN111304767B (en) * 2020-02-17 2022-10-04 河北吉藁化纤有限责任公司 Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber
CN112831852A (en) * 2020-12-31 2021-05-25 宜宾海丝特纤维有限责任公司 Production process for continuously spinning superfine filaments
CN116285013A (en) * 2023-03-15 2023-06-23 赛得利(江苏)纤维有限公司 Flame-retardant viscose production process
CN116285013B (en) * 2023-03-15 2024-05-03 赛得利(江苏)纤维有限公司 Flame-retardant viscose production process

Also Published As

Publication number Publication date
CN107557890B (en) 2020-04-03

Similar Documents

Publication Publication Date Title
CN103556260B (en) A kind of bamboo-carbon viscose fibre and preparation method thereof
CN105908282B (en) A kind of preparation method of the Manufacturing Pet Fine Filaments of 33dtex/144f
CN101314673B (en) Production method for full-dull nylon 6-slice
CN102560734B (en) Antioxidant toughening modified polyphenylene sulfide monofilament and preparation method thereof
CN107557890A (en) A kind of production technology of nitrogen phosphorous flame-retardant viscose filament yarn
CN101328626A (en) Method for continuously preparing regenerated cellulose fibre
CN102851776B (en) Production method of colored cotton, wood and bamboo composite pulp viscose
CN106633834A (en) Black masterbatch, nylon 6 fiber and preparation method of black masterbatch and nylon 6 fiber
CN107419354A (en) High cut resistant high-strength high-modulus polyethylene long filament and preparation method thereof
CN105544000B (en) High-temperature oxidation resistant composite Nano PPS/Ti SiOx chopped fibers and preparation method thereof
CN110791831A (en) Preparation method of plant modified viscose filament yarn
CN103184582B (en) Preparation method of PVA composite high-strength high-modulus cellulose fiber
CN102839432A (en) Preparation method of ultra-high-speed spinning polyester pre-oriented yarn
CN104480555A (en) Production process of high-elasticity-feature terylene pre-oriented fibers
CN104389039A (en) Method for producing temperature-regulating viscose fibers
CN103409835A (en) Fine denier polyphenylene sulfide short fiber production method
CN105586683A (en) Regenerated stock solution colored high-speed polyester staple fiber sewing thread and preparation method thereof
CN105401252A (en) Preparation method of flame-retardant PET fiber
CN101736428A (en) Method for preparing Chinese medicinal cellulose fiber by solvent method
CN101768790B (en) Sheath core composite fibre of chitin and cellulose and preparation method thereof
CN107502965A (en) A kind of nano barium sulfate viscose glue flat filament and preparation method thereof
CN112095171A (en) Polyamide fiber containing plant functional porous molecular nest and preparation method thereof
CN106319656A (en) Preparation method for two-component side-by-side composite fibres
CN106400131B (en) A kind of processing system reducing viscose glue population suitable for spinning technique
CN111691007A (en) Preparation process of bi-component superfine composite fiber

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant