CN101922059A - Production process of colored flat acrylic fiber and production line thereof - Google Patents
Production process of colored flat acrylic fiber and production line thereof Download PDFInfo
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Abstract
The invention relates to a production process of colored flat acrylic fiber and a production line thereof, which are a production process and a production line thereof for producing the colored flat acrylic fiber in a plurality of color systems with vivid colors, little chromatic aberration and great flatness by adopting a cationic dye, in particular to a spinning production line for producing the colored flat acrylic fiber by adopting a ternary aqueous suspension polymerization and sodium sulfocyanate wet method. In the invention, a long-strip arc dye liquor spray head is used for dying, and the long-strip arc dye liquor spray head is an arc spray head which comprises a spray head seat, a spray head cover and a dye liquor inlet pipe and has a hollow T-shaped cross section, wherein the spray head is a long-strip semi-cylindrical surface, and a plurality of penetrative spraying holes are arranged on the spray head cover in a staggered way. The invention overcomes the defects of stripy and uneven dyeing, great chromatic aberration, large volume of colored wastewater, long product processing period, and the like commonly existing in a production process and a production line thereof for producing white flat acrylic fiber by adopting a traditional dyeing mode of steaming loose fibers at a high temperature.
Description
Technical field
The present invention relates to a kind ofly to adopt cation dyes, produce polychrome system, the production technology and the production line thereof of bright-colored, aberration is little and flatness is big colored flat acrylic fiber fiber, be particularly related to and adopt ternary aqueous suspension polymerization and sodium sulfocyanate wet spinning to produce route production colored flat acrylic fiber fiber, to remedy the production technology and the production line thereof of shortcomings such as the look that generally occurs when white flat acrylic fiber fiber adopts bulk fibre high temperature decatize traditional dyeing mode is spent, dyeing is inhomogeneous, aberration is big, coloured sewage quantity big, the product process-cycle is long.
Background technology
Because flat acrylic fiber is the important source material of Fake Furs, the fibre section is similar to animal hair, and the imitation animal hair sense is strong, and the resilience excellence has special gloss, good bulkiness and anti-pilling.Thick dawn flat acrylic fiber fiber constitutes velvet, and thin denier flat shape acrylic fiber is a under hair then, the style of the peltry likelihood skin of making thus, and it is strong to have the feel of wool, and gloss is true to nature, and is soft, comfortable and easy to wear, the characteristics that warmth retention property is good.Its traditional dyeing method adopts bulk fibre high temperature decatize mode to dye.
At present, adopt the profile spinneret of non-circular pass,, can produce the flat acrylic fiber fiber of white through spinning technique optimization and improvement.The patent JP59094611 that delivers as Japanese Mitsubishi Rayon KK Co., Ltd. has illustrated a kind of dry-spinning method abnormity acrylic fibers technology of preparing, and the flatness of finished fiber is 5: 1.It is solvent that the patent EP0051189 that Germany Bayer AG company delivers has studied with DMF, adopts the dry-spinning method to make profiled filament.It is the wet method spinning making method of the 3.33dtex flat acrylic of solvent with organic solvent dimethylacetylamide (DMAC) that China Patent No. CN101445967A discloses a kind of.Manufacturer can only provide white flat acrylic fiber fiber for a long time, again by the needs of fur manufacturing producer according to fur colour, selects printing and dyeing company that the flat acrylic fiber fiber of white is dyeed.Have various problems thus: the glass transition temperature of acrylic fibers under humid tropical condition is 70～80 ℃, and the intensification when therefore dyeing must strictly be controlled, and needs to add accelerant or retarding agents according to dying shade.And the production technology difference of fiber (dry-spinning, wet spinning, comonomer form), dyestuff kind (performance) difference need be selected different dyeings for use.It is improper to control slightly, and very easily specking appears in the look flower.The aberration desired value (DEcmc) that characterizes colored fibre level-dyeing property and repeatability is usually greater than 1.5.In addition, after spin dyeing and need carry out in batches, unavoidable between each batch product in the difference of aspects such as color and luster, feel or outward appearance.Energy consumption height and coloured sewage quantity are big simultaneously, have also prolonged the process-cycle of product.All factors have all caused the fibre loss rate to improve, and have increased the cost of fur manufacturing.It also is a great problem in the fur manufacturing process so far.
At present, the method for conventional color acrylic fibre fiber production has endless tow continuous dyeing method, original liquid coloring method, gel staining method.Wherein endless tow continuous dyeing method is consistent with back spinning short fiber dyeing mechanism, and the finished product tow is carried out high temperature pad dyeing, aberration between only having solved batch, and other problems still exists, and only is fit to small lot batch manufacture.The original liquid coloring method is before spinning spinning solution to be mixed with pigment, makes coloured spinning solution, directly carries out spinning production.The original liquid coloring method of CN117004C, CN1523161, CN1465758A explanation exists pigment to grind, and the granules of pigments particle diameter is bigger in coloured stoste, and the spinning difficulty increases, and chromatogram is few.Gel staining method is with liquid dyes the as-spun fibre that is under the gel state to be dyeed in the acrylic fibre wet spinning process.The dyestuff allotment is flexible, so colour system is many, chromatogram is wide.4 kinds of representative in the world acrylic Fibre Gel Dyeing process routes have been introduced in " Kingsoft oiling fibre " the 4th phase of calendar year 2001 " application of gel-colored technology in acrylic fibers NaSCN two-step process ", domestic also have acrylic fibers company to introduce wherein Solutia, Sterling technology to produce conventional color acrylic fibre, as " Kingsoft oiling fibre " the 1st phase in 2004 " gel-colored technical optimization ".But it is solvent that Solutia company, Courtaulds company and Snia company adopt DMAC, NaSCN and DMF respectively, all is in stretching or the stretching poststaining, and dyeing time is short, and difficulty is dyed dark color.And after stretched, the amorphous region degree of orientation of fiber improves, and internal capillary is elongated and attenuates simultaneously, influences the infiltration of dyestuff, level-dyeing property variation, Yi Sehua.Especially DMAC and DMF are organic solvent, the spinning solution concentration of this process route adopts the NaSCN method of inorganic solvent to double above, so fibre structure is finer and close during spinning technique, the fibrous inside voidage is little, the cavity is little, dyestuff penetration is slow during dyeing, and dyeing and ventilative time will be grown, and level-dyeing property is poor than the NaSCN method.Sterling company is solvent with NaSCN, and to spray dyeing before the conventional acrylic fibers employing stretching of circular cross-section, shower is in the relative arranged vertical in tow two sides.Shortcoming is that dyeing time is grown (＞30 seconds), and for dye liquor is penetrated in the tow as much as possible, spray pressure is big, has the gel monofilament phenomenon that is thrust.Especially the wet spinning flat acrylic adopts and accelerates the solidification forming mode, and fiber weakness is big relatively, easier thrusting.Road hot-stretch after the gelatine silk that is thrust can't be finished, coloured light is different from the fiber that stretched, thereby produces aberration, and the powder height.In addition, for guaranteeing higher spray pressure, the shower top nozzle distributes less, and spacing is bigger, and nozzle is easily stifled, so it is higher dyeing striped probability to occur, even whiting is arranged.The DEcmc fluctuation is bigger, sometimes greater than 1.0, even 1.2.
In sum, the wet spinning flat acrylic is because its each side physical and mechanical properties and dyeability are different from conventional acrylic fibers, so need more the improvement to satisfy the woven requirement of fur on the preparation method, to disclose a kind of be production technology and the production line that the wet method of solvent is spun coloured flat acrylic with NaSCN and also still there is not document now.
Summary of the invention
Technical problem to be solved by this invention is at the above-mentioned state of the art, and a kind of production technology and production line thereof that dyeing can be directly used in coloured flat fiber of the woven polychrome of fur system, bright-colored and even dyeing that spin after not needing is provided.Relate to NaSCN is spin solvent, adopt spinnerets of the present invention, dye liquor injector head and spinning technique route to produce the colored flat acrylic fiber fiber, both can obtain satisfied flatness (length-width ratio of fiber cross section), the fiber flatness was greater than 9: 1, avoided difficult dyeing quality defective of dying dark color, look flower, striped even fiber whiting again, DEcmc≤0.25, more conventional gel staining method aberration reduction rate＞83% is than bulk fibre high temperature decatize decoration method aberration reduction rate＞89%.And simplified processing process reduces cost, and shortens the process-cycle, and the Fake Furs of making is beautiful in colour and have a skin emulation effect true to nature.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
The production technology of a kind of colored flat acrylic fiber of the present invention may further comprise the steps successively:
A, to adopt with water be the ternary aqueous suspension polymerization of medium, and promptly three kinds of comonomers by the redox system initiated polymerization, and are regulated molecular weight by chain-transferring agent under the water condition.
In the polymerisation, acrylonitrile is first comonomer, and the mass percent that accounts for all comonomers is 90%～92%;
Second comonomer is a kind of in methyl acrylate, methyl methacrylate or the vinyl acetate, and the mass percent that accounts for all comonomers is 7.7%～9.6%;
The 3rd comonomer is a kind of in methylpropene sodium sulfonate, sodium vinyl sulfonate, Sodium styrene sulfonate or the 2-acrylamido-2-methyl propane sulfonic acid, and the mass percent that accounts for all comonomers is 0.3%～0.4%;
The input concentration of total polymerization monomer is 33～35wt%, and reaction temperature is 53～56 ℃, and the reaction time is 53～57 minutes;
Water miscible redox initiation system is adopted in reaction, and oxidant is ammonium persulfate, potassium peroxydisulfate or sodium chlorate; Reductant is sodium pyrosulfite, sodium hydrogensulfite or sodium sulfite; The oxidant consumption is 0.5～0.6% of all monomer gross masses, and the mol ratio of reductant and oxidant is 1.45～1.55: 1;
The chain-transferring agent that is used to regulate molecular weight is a β hydroxyl ethyl mercaptan;
B, take off single and washing;
Polymer slurries is to remove unreacted monomer under 52～57kPa condition in vacuum; Slurry enters vacuum and rotates through filter after taking off singly, washes under 55～60kPa vacuum, 50～53 ℃ of temperature; Wash the back polymer and be diluted to 34～35wt% concentration, send into the polymer storage tank;
C, dissolving, deaeration and filtration;
High polymer slurry and sodium sulfocyanate are subjected to high speed shear, grinding and dissolve in dissolving machine; The thick stoste in dissolving back is 5～10kPa in vacuum, removes bubble under 20～22 ℃ of conditions of the temperature difference, and filters the back for spinning by plate and frame type filter-press.
D, spinning solidification forming;
To filter the resulting acrylonitrile compolymer body in back and make spinning solution through the sodium thiocyanate solution dissolving, the spinning solution after the heating is extruded from the rectangular opening of spinnerets, forms as-spun fibre through double diffusion in coagulating bath; Wherein, the weight percentage of acrylonitrile compolymer body is 11～12% in the described spinning solution; Described coagulating bath is for containing 14～15.5wt% sodium thiocyanate water solution, 1～4 ℃ of coagulation bath temperature, and draw ratio 1.7～1.9 is born in coagulating bath; Described spinnerets hole shape is a rectangle, and the length-width ratio of described rectangular opening is 12.93～16.67: 1, preferred 14.76: 1～16.25: 1, and hole count 7200～8500 holes of described spinnerets;
E, preliminary draft and washing;
2～2.5 times of as-spun fibre preliminary drafts behind the coagulation forming; 50～60 ℃ of washing temperature;
F, dyeing;
By the dyeing of strip arc dye liquor injector head spray, dye mother solution is added flow at 50～80L/hr to washing back fiber, 42～50 ℃ of dyeing temperatures in dyeing machine;
Described strip arc dye liquor injector head is by nozzle boss, nozzle cap and dye liquor inlet tube constitute, cross section is the "T"-shaped strip of hollow arc shower nozzle, nozzle cap is the semi-cylindrical of strip, the be staggered spray orifice of some perforations of described nozzle cap;
G, hot drawing-off;
Finish 4～4.5 times of the drawing-offs in 98～99 ℃ hot water of fiber after the dyeing;
H, densification;
Tow carries out densification at first drying machine after the drawing-off, and wet-bulb temperature is controlled at 65～80 ℃ in the drying machine;
I. curl and typing;
Adopt hot bath or decatize mode preheating tow to carry out machine crimp, curling pressure is 0.03～0.05MPa, and the fiber after curling carries out the saturated vapor HEAT SETTING to be handled, and heat setting temperature is 105～115 ℃;
J, oil and dry;
Fiber floods and oils after the heat treatment, and oil groove concentration is 1.5～2.5%, and afterwards, oven dry relaxes in second drying machine;
K, cut-out and packing;
Oven dry back fiber cuts off according to customer requirement, makes the staple fibre product of different length.
As optimized technical scheme:
The production technology of aforesaid a kind of colored flat acrylic fiber, described dyestuff is cation dyes, is cyanines class, heterocycle azo class, naphthalene lactam, azo class or anthraquinone dyes.
The production technology of aforesaid a kind of colored flat acrylic fiber, in the staining procedure, the spray orifice of described dye liquor injector head is the wicker leaf shape spray orifice, also can be ellipse spray orifice, rectangle spray orifice and circular spray orifice; There is the longitudinal fluting of the spray orifice of connection on same straight line on the surface of described nozzle cap.
The production technology of aforesaid a kind of colored flat acrylic fiber, described longitudinal fluting are " V " connected in star, and " V " shape opening is outside; The angle theta of described " V " shape is 60 °.Also can be " U " shape groove, " U " shape opening be outside; Or dovetail groove, the long limit of trapezoidal parallel edges is a notch.When groove was " U " shape groove, described " U " trench bottom aperture widths was not more than 1/3 of U-lag mouth width.When groove was dovetail groove, the bottom land width of described dovetail groove was 1/3 of a width of rebate.
The production technology of aforesaid a kind of colored flat acrylic fiber, in the staining procedure, the spray orifice of described dye liquor injector head is vertically lined up three rows, and every round is equally spaced; Also can arrange the pore size distribution that is staggered front to back arbitrarily according to injector head and spray orifice size.Described nozzle cap is a face of cylinder part, is of a size of: length * arc is wide=and 100mm * 50mm, face of cylinder diameter is 180mm; The major parameter of spray orifice satisfies following relational expression:
The willow leaf of single wicker leaf shape spray orifice is long to be 2k mm,
Willow leaf is wide to be 2k/3mm,
Total hole count n satisfies: n=23-3k, wherein, k=1～6, preferred k=3 or 4.
The present invention also provides a kind of production line of colored flat acrylic fiber, comprises successively: polymeric kettle, demonomerization tower, vacuum rotate through filter, polymer storage tank, high-shear dissolution machine, deaeration tower, stoste filter press, spinning machine, preliminary draft machine, tow rinsing maching, dyeing machine, hot drawing machine, first drying machine, crimping machine, setting machine, oiling machine, second drying machine, cutting machine and baling press;
Wherein, dyeing machine is provided with some strip arc dye liquor injector heads, described strip arc dye liquor injector head is by nozzle boss, nozzle cap and dye liquor inlet tube constitute, cross section is the "T"-shaped strip of hollow arc shower nozzle, nozzle cap is the semi-cylindrical of strip, the be staggered spray orifice of some perforations of described nozzle cap.
The production line of aforesaid a kind of colored flat acrylic fiber, wherein, described spray orifice is the wicker leaf shape spray orifice, also can be ellipse spray orifice, rectangle spray orifice and circular spray orifice; There is the longitudinal fluting of the spray orifice of connection on same straight line on the surface of described nozzle cap.
The production line of aforesaid a kind of colored flat acrylic fiber, wherein, described longitudinal fluting is " V " connected in star, " V " shape opening is outside; The angle theta of described " V " shape is 60 °; Also can be " U " shape groove, " U " shape opening be outside; Or dovetail groove, the long limit of trapezoidal parallel edges is a notch; When groove was " U " shape groove, described " U " trench bottom aperture widths was not more than 1/3 of U-lag mouth width; When groove was dovetail groove, the bottom land width of described dovetail groove was 1/3 of a width of rebate.。Described spray orifice is vertically lined up three rows, and every round is equally spaced; Also can arrange the pore size distribution that is staggered front to back arbitrarily according to injector head and spray orifice size.The cylindrical of described dye liquor inlet tube has screw thread; Described nozzle boss connects with welding manner with nozzle cap.
The production line of aforesaid a kind of colored flat acrylic fiber, wherein, described nozzle cap is a face of cylinder part, is of a size of: length * arc is wide=100mm * 50mm, face of cylinder diameter is 180mm; The major parameter of spray orifice satisfies following relational expression:
The willow leaf of single wicker leaf shape spray orifice is long to be 2k mm,
Willow leaf is wide to be 2k/3mm,
Total hole count n satisfies: n=23-3k, wherein, k=1～6, preferred k=3 or 4.
The used dye liquor injector head of dyeing of the present invention adopts the semi-cylindrical arc shower nozzle of strip, and arc length * wide is 100 * 50mm, and is distributed on the shower with 100～120mm spacing.Each ejection face is a face of cylinder part, face of cylinder diameter is 180mm, each nozzle surface has 3 60 ° of grooves at length direction, a plurality of wicker leaf shape spray orifices that are staggered front to back arrangement distribute, every round is equally spaced, the length of single hole (2k) mm (k=1～6), wide is (2k/3) mm, hole count is that n (individual) satisfies: n=23-3k.Preferred k=3,4, i.e. single hole hole length=6mm, 8mm, the hole is wide=2mm, 2.7mm, hole count n=14,11.Shower nozzle is apart from tow 20～25mm.Thus, jetting fluid wide coverage and intersection need not bigger spray pressure, and gelatine silk can not thrust, and are particularly useful for adopt accelerating the solidification forming mode, fiber weakness is big relatively, the wet spinning flat acrylic of more not easy-to-use high pressure nozzle spray staining method.And interlock because spray nozzle is arranged, stop up the hidden danger that influences local tow colouring because of indivedual spray orifices when having eliminated single tube nozzle spray, the fiber whiting does not take place, fiber colour is even, and aberration is minimum.In addition, easy to operate, single injector head has been realized the effect of many single mouth showers, shortens dyeing time greatly, and color is switched flexibly, and the transitional fibre of generation is few, the quality problems of avoiding fiber, yarn or fabric to bring in road, back dyeing process.Adopt colored flat acrylic fiber fiber color that the present invention produces can according to after spin needs and carry out the dyestuff color matching, aberration desired value≤0.25, more conventional gel staining method aberration reduction rate＞83% is than bulk fibre high temperature decatize decoration method aberration reduction rate＞89%.As application extension, this arc shower nozzle can be adjusted size and radian, can be hemispherical or spherical shower nozzle, satisfies the needs of different spray occasions.
The gel-colored process of the colored flat acrylic fiber fiber that the present invention relates to is after as-spun fibre goes out non-circular spinneret orifice, dyes between washing and hot drafting process.The present invention's dyestuff applicatory is cation dyes, comprises cyanines class, heterocycle azo class, naphthalene lactam, azo class and anthraquinone dyes.
Beneficial effect
Compared with prior art, the invention has the advantages that: adopt autocratic spinnerets, improve stoste from the spinnerets extruded velocity, the fiber flatness was greater than 9: 1.And on the flat acrylic process route, set up online dyeing apparatus, and utilizing the distinctive square-section of flat acrylic, opening character is splendid, inadherent characteristics between fiber, especially by special-purpose arcwall face dyeing shower nozzle, has solved the problem of spinning uneven dyeing behind the flat acrylic.In whole spinning technique, to solidification forming condition, drafting multiple distribution, compacting by drying and curl, the typing condition all need adjust, to satisfy the needs of coloured flat acrylic performance.
Description of drawings
Fig. 1 constitutes schematic diagram for production line of the present invention
Fig. 2 is the vertical view of a kind of dye liquor injector head of the present invention
Fig. 3 is the A-A cross-sectional view of a kind of dye liquor injector head of the present invention
Wherein 1 is nozzle boss; The 2nd, the dye liquor inlet tube; The 3rd, spray orifice; The 4th, groove; The 5th, screw thread; The 6th, nozzle cap
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
The production technology of a kind of colored flat acrylic fiber of the present invention may further comprise the steps successively:
A, employing are the ternary aqueous suspension polymerization of medium with water; Promptly three kinds of comonomers by the redox system initiated polymerization, and are regulated molecular weight by chain-transferring agent under the water condition.
In the polymerisation, acrylonitrile is first comonomer, and the mass percent that accounts for all comonomers is 90%～92%;
Second comonomer is a kind of in methyl acrylate, methyl methacrylate or the vinyl acetate, and the mass percent that accounts for all comonomers is 7.7%～9.6%;
The 3rd comonomer is a kind of in methylpropene sodium sulfonate, sodium vinyl sulfonate, Sodium styrene sulfonate or the 2-acrylamido-2-methyl propane sulfonic acid, and the mass percent that accounts for all comonomers is 0.3%～0.4%;
The input concentration of total polymerization monomer is 33～35wt%, and reaction temperature is 53～56 ℃, and the reaction time is 53～57 minutes;
Water miscible redox initiation system is adopted in reaction, and oxidant is ammonium persulfate, potassium peroxydisulfate or sodium chlorate; Reductant is sodium pyrosulfite, sodium hydrogensulfite, sodium sulfite; The oxidant consumption is 0.5～0.6% of all monomer gross masses, and the mol ratio of reductant and oxidant is 1.45～1.55: 1;
The chain-transferring agent that is used to regulate molecular weight is a β hydroxyl ethyl mercaptan;
B, take off single and washing;
Polymer slurries is to remove unreacted monomer under 52～57kPa condition in vacuum; Slurry enters vacuum and rotates through filter after taking off singly, washes under 55～60kPa vacuum, 50～53 ℃ of temperature; Wash the back polymer and be diluted to 34～35wt% concentration, send into the polymer storage tank;
C, dissolving, deaeration and filtration;
High polymer slurry and sodium sulfocyanate are subjected to high speed shear, grinding and dissolve in dissolving machine; The thick stoste in dissolving back is 5～10kPa in vacuum, removes bubble under 20～22 ℃ of conditions of the temperature difference, and filters the back for spinning by plate and frame type filter-press.
D, spinning solidification forming;
To filter the resulting acrylonitrile compolymer body in back and make spinning solution through the sodium thiocyanate solution dissolving, the spinning solution after the heating is extruded from the rectangular opening of spinnerets, forms as-spun fibre through double diffusion in coagulating bath; Wherein, the weight percentage of acrylonitrile compolymer body is 11～12% in the described spinning solution; Described coagulating bath is for containing 14～15.5wt% sodium thiocyanate water solution, 1～4 ℃ of coagulation bath temperature, and draw ratio 1.7～1.9 is born in coagulating bath; Described spinnerets hole shape is a rectangle, and the length-width ratio of described rectangular opening is 12.93～16.67: 1, preferred 14.76: 1～16.25: 1, and hole count 7200～8500 holes of described spinnerets;
E, preliminary draft and washing;
2～2.5 times of as-spun fibre preliminary drafts behind the coagulation forming; 50～60 ℃ of washing temperature;
F, dyeing;
By the dyeing of strip arc dye liquor injector head spray, dye mother solution is added flow at 50～80L/hr to washing back fiber, 42～50 ℃ of dyeing temperatures in dyeing machine;
Described strip arc dye liquor injector head is the arc shower nozzle of the "T"-shaped strip of hollow by nozzle boss (1), nozzle cap (6) and dye liquor inlet tube (2) formation, cross section, nozzle cap (6) is the semi-cylindrical of strip, described nozzle cap (6) the some spray orifices (3) that are staggered are shown in Fig. 2 and 3;
G, hot drawing-off;
H, densification;
Tow carries out densification at first drying machine after the drawing-off, and wet-bulb temperature is controlled at 65～80 ℃ in the drying machine;
I. curl and typing;
Adopt hot bath or decatize mode preheating tow to carry out machine crimp, curling pressure is 0.03～0.05MPa, and the fiber after curling carries out the saturated vapor HEAT SETTING to be handled, and heat setting temperature is 105～115 ℃;
J, oil and dry;
Fiber floods and oils after the heat treatment, and oil groove concentration is 1.5～2.5%, and afterwards, oven dry relaxes in second drying machine;
K, cut-out and packing;
Oven dry back fiber cuts off according to customer requirement, makes the staple fibre product of different length.
The production technology of a kind of colored flat acrylic fiber of the present invention, each polymerization single polymerization monomer enters polymeric kettle and carries out polymerisation, gained high polymer slurry enters the demonomerization tower and removes unreacted monomer, and polymerisation slurry rotates through filter through vacuum and finishes the polymer washing afterwards, and the polymer storage tank is delivered in dilution.The condensate slurry of sending from the polymer storage tank enters the high-shear dissolution machine through high speed shear, grinding with dense sodium sulfocyanate and dissolves, and the thick stoste that dissolving obtains enters the deaeration tower and removes bubble, and filters the back for spinning by the stoste filter press.Extrude solidification forming pancake as-spun fibre for spinning stock solution by spinning machine abnormity spinneret orifice, through the drawing-off of preliminary draft machine low power, entering online dyeing machine behind the sodium sulfocyanate of tow rinsing maching flush away remnants carries out dying on the cation dyes, flat acrylic after the dyeing is at hot drawing machine high drafting, after finishing densification by first drying machine, enter crimping machine and carry out machine crimp, heat treatment in setting machine, after the oiling machine dipping oils, dry through second drying machine, be cut into user's Len req at cutting machine, wind is delivered to the baling press packing.
Wherein, the production technology of aforesaid a kind of colored flat acrylic fiber, described dyestuff is cation dyes, is cyanines class, heterocycle azo class, naphthalene lactam, azo class or anthraquinone dyes.
The production technology of aforesaid a kind of colored flat acrylic fiber, in the staining procedure, the spray orifice of described dye liquor injector head (3) is the wicker leaf shape spray orifice, also can be ellipse spray orifice, rectangle spray orifice and circular spray orifice; There is the longitudinal fluting (4) of the spray orifice (3) of connection on same straight line on the surface of described nozzle cap (6).
The production technology of aforesaid a kind of colored flat acrylic fiber, described longitudinal fluting (4) are " V " connected in star, and " V " shape opening is outside; The angle theta of described " V " shape is 60 °.Also can be " U " shape groove, " U " shape opening be outside; Or dovetail groove, the long limit of trapezoidal parallel edges is a notch.When groove was " U " shape groove, described " U " trench bottom aperture widths was not more than 1/3 of U-lag mouth width.When groove was dovetail groove, the bottom land width of described dovetail groove was 1/3 of a width of rebate.
The production technology of aforesaid a kind of colored flat acrylic fiber, in the staining procedure, the spray orifice of described dye liquor injector head (3) is vertically lined up three rows, and every round is equally spaced; Also can arrange the pore size distribution that is staggered front to back arbitrarily according to injector head and spray orifice (3) size.Described nozzle cap (6) is a face of cylinder part, is of a size of: length * arc is wide=and 100mm * 50mm, face of cylinder diameter is 180mm; The major parameter of spray orifice (3) satisfies following relational expression:
The willow leaf of single wicker leaf shape spray orifice is long to be 2k mm,
Willow leaf is wide to be 2k/3mm,
Total hole count n satisfies: n=23-3k, wherein, k=1～6, preferred k=3 or 4.
The present invention also provides a kind of production line of colored flat acrylic fiber, as shown in Figure 1, comprise successively: polymeric kettle, demonomerization tower, vacuum rotate through filter, polymer storage tank, high-shear dissolution machine, deaeration tower, stoste filter press, spinning machine, preliminary draft machine, tow rinsing maching, dyeing machine, hot drawing machine, first drying machine, crimping machine, setting machine, oiling machine, second drying machine, cutting machine and baling press;
Wherein, dyeing machine is provided with some strip arc dye liquor injector heads, shown in Fig. 2 and 3, described strip arc dye liquor injector head is the arc shower nozzle of the "T"-shaped strip of hollow by nozzle boss (1), nozzle cap (6) and dye liquor inlet tube (2) formation, cross section, nozzle cap (6) is the semi-cylindrical of strip, described nozzle cap (6) the some spray orifices (3) that are staggered.
The production line of aforesaid a kind of colored flat acrylic fiber, wherein, described spray orifice (3) is the wicker leaf shape spray orifice, also can be ellipse spray orifice, rectangle spray orifice and circular spray orifice; There is the longitudinal fluting (4) of the spray orifice (3) of connection on same straight line on the surface of described nozzle cap (6).
The production line of aforesaid a kind of colored flat acrylic fiber, wherein, described longitudinal fluting (4) is " V " connected in star, " V " shape opening is outside; The angle theta of described " V " shape is 60 °; Also can be " U " shape groove, " U " shape opening be outside; Or dovetail groove, the long limit of trapezoidal parallel edges is a notch; When groove was " U " shape groove, described " U " trench bottom aperture widths was not more than 1/3 of U-lag mouth width; When groove was dovetail groove, the bottom land width of described dovetail groove was 1/3 of a width of rebate.Described spray orifice (3) is vertically lined up three rows, and every round is equally spaced; Also can arrange the pore size distribution that is staggered front to back arbitrarily according to injector head and spray orifice size.The cylindrical of described dye liquor inlet tube (2) has screw thread (5), and described screw thread adopts 60 ° of fastening connections of closely-pitched angular thread of common metric system, also the dye liquor injector head can be connected with shower by flange.Described nozzle boss (1) connects with welding manner with nozzle cap (6).
The production line of aforesaid a kind of colored flat acrylic fiber, wherein, described nozzle cap (6) is a face of cylinder part, is of a size of: length * arc is wide=100mm * 50mm, face of cylinder diameter is 180mm; The major parameter of spray orifice (3) satisfies following relational expression:
The willow leaf of single wicker leaf shape spray orifice is long to be 2k mm,
Willow leaf is wide to be 2k/3mm,
Total hole count n satisfies: n=23-3k, wherein, k=1～6, preferred k=3 or 4.
Aforesaid a kind of dye liquor injector head, described longitudinal fluting (4) degree of depth is k mm.
A kind of dye liquor injector head of the present invention is distributed on the shower with 100～120mm spacing, and the dye liquor injector head is connected on the shower by screw thread (5).Each nozzle cap (6) is a face of cylinder part, face of cylinder diameter is 180mm, each nozzle cap (6) has 3 60 ° grooves (4) at length direction, a plurality of wicker leaf shape spray orifices (3) that are staggered front to back arrangement distribute, every round is equally spaced, willow leaf length=6mm, the 8mm of single spray orifice, willow leaf is wide=2mm, 2.7mm, hole count n=14,11.Dye liquor enters by spray orifice from dye liquor inlet tube (2) and penetrates, and shower nozzle is apart from tow 20～25mm.Thus, jetting fluid wide coverage and intersection need not bigger spray pressure, and gelatine silk can not thrust, and are particularly useful for powerful little, not impact-resistant fiber.And interlock because spray nozzle is arranged, stop up the hidden danger that influences local tow colouring because of indivedual spray orifices when having eliminated single tube nozzle spray, the fiber whiting does not take place, fiber colour is even, and aberration is minimum.In addition, easy to operate, single injector head has been realized the effect of many single mouth showers, shortens dyeing time greatly, and color is switched flexibly, and the transitional fibre of generation is few, the quality problems of avoiding fiber, yarn or fabric to bring in road, back dyeing process.
The percentage and the umber that are adopted in the production technology of described colored flat acrylic fiber: embodiment and the comparative example are except that indicating, all by weight.
The acrylonitrile compolymer body of forming by acrylonitrile, methyl acrylate and Sodium styrene sulfonate, the comonomer proportioning consists of acrylonitrile: methyl acrylate: Sodium styrene sulfonate=90.0: 9.6: 0.4, total polymerization monomer feed concentration is 33%, reaction temperature is 56 ℃, in 53 minutes reaction time, oxidant is a sodium chlorate, and consumption is total single 0.5wt%, reductant is a sodium pyrosulfite, and reductant and oxidant mol ratio are 1.45.Slurry takes off list after the polymerisation under 57Kpa vacuum, after washing under 55kPa vacuum, the 50 ℃ of temperature, is diluted to 35% concentration.Is 8kPa with NaSCN solution dissolving back in vacuum, removes bubble under 22 ℃ of conditions of the temperature difference, and filters that to obtain always be 12% spinning solution admittedly.The spinnerets of this spinning solution by the special requirement size is that 14.0wt%, temperature are that solidification forming is an as-spun fibre in 1.0 ℃ the coagulating bath in sodium sulfocyanate concentration, negative draw ratio 1.9.As-spun fibre enters the preliminary draft machine and stretches 2.5 times.After 50 ℃ of water washings, in dyeing machine, finish dyeing with cation dyes, the dyestuff additional amount is 50L/hr, 42 ℃ of dyeing temperatures.Tow 4.0 times of drawing-offs in 98 ℃ of hot water in dyeing back are respectively densification in 80 ℃, 74 ℃, 70 ℃ first drying machine at wet-bulb temperature, curl under 0.03MPa curls pressure, and finish typing successively, oil and dry.Heat setting temperature is 105 ℃, and last oil concentration is controlled to be 1.5%.Oven dry back fiber cuts off according to customer requirement, makes the colored flat acrylic fiber staple fibre product of different length.
The acrylonitrile compolymer body of forming by acrylonitrile, methyl methacrylate and sodium vinyl sulfonate, the comonomer proportioning consists of acrylonitrile: methyl acrylate: sodium vinyl sulfonate=90.8: 8.8: 0.4, total polymerization monomer feed concentration is 34%, reaction temperature is 55 ℃, in 54 minutes reaction time, oxidant is a potassium peroxydisulfate, and consumption is total single 0.6wt%, reductant is a sodium hydrogensulfite, and reductant and oxidant mol ratio are 1.55.Slurry takes off list after the polymerisation under 55Kpa vacuum, after washing under 60kPa vacuum, the 51 ℃ of temperature, is diluted to 34.7% concentration.Is 7kPa with NaSCN solution dissolving back in vacuum, removes bubble under 21 ℃ of conditions of the temperature difference, and filters that to obtain always be 11.8% spinning solution admittedly.The spinnerets of this spinning solution by the special requirement size is that 14.5wt%, temperature are that solidification forming is an as-spun fibre in 2.0 ℃ the coagulating bath in sodium sulfocyanate concentration, negative draw ratio 1.8.As-spun fibre enters the preliminary draft machine and stretches 2.3 times.After 55 ℃ of water washings, in dyeing machine, finish dyeing with cation dyes, the dyestuff additional amount is 60L/hr, 45 ℃ of dyeing temperatures.Tow 4.4 times of drawing-offs in 98.5 ℃ of hot water in dyeing back are respectively densification in 73 ℃, 70 ℃, 67 ℃ first drying machine at wet-bulb temperature, curl under 0.04MPa curls pressure, and finish typing successively, oil and dry.Heat setting temperature is 108 ℃, and last oil concentration is controlled to be 1.85%.Oven dry back fiber cuts off according to customer requirement, makes the colored flat acrylic fiber staple fibre product of different length.
Embodiment 7～9:
The acrylonitrile compolymer body of forming by acrylonitrile, vinyl acetate and methylpropene sodium sulfonate, the comonomer proportioning consists of acrylonitrile: vinyl acetate: methylpropene sodium sulfonate=92.0: 7.7: 0.3, total polymerization monomer feed concentration is 35%, reaction temperature is 54 ℃, in 56 minutes reaction time, oxidant is an ammonium persulfate, and consumption is total single 0.55wt%, reductant is a sodium hydrogensulfite, and reductant and oxidant mol ratio are 1.5.。Slurry takes off list after the polymerisation under 52Kpa vacuum, after washing under 58kPa vacuum, the 53 ℃ of temperature, is diluted to 34.0% concentration.Is 5kPa with NaSCN solution dissolving back in vacuum, removes bubble under 20 ℃ of conditions of the temperature difference, and filters that to obtain always be 11% spinning solution admittedly.The spinnerets of this spinning solution by the special requirement size is that 15.0wt%, temperature are that solidification forming is an as-spun fibre in 3.0 ℃ the coagulating bath in sodium sulfocyanate concentration, negative draw ratio 1.7.As-spun fibre enters the preliminary draft machine and stretches 2.0 times.After 60 ℃ of water washings, in dyeing machine, finish dyeing with cation dyes, the dyestuff additional amount is 80L/hr, 50 ℃ of dyeing temperatures.Tow 4.5 times of drawing-offs in 99.0 ℃ of hot water in dyeing back are respectively densification in 75 ℃, 71 ℃, 67 ℃ first drying machine at wet-bulb temperature, curl under 0.05MPa curls pressure, and finish typing successively, oil and dry.The temperature of HEAT SETTING is 110 ℃, and last oil concentration is controlled to be 2.0%.Oven dry back fiber cuts off according to customer requirement, makes the colored flat acrylic fiber staple fibre product of different length.
Embodiment 10～12:
By the acrylonitrile compolymer body that acrylonitrile, methyl acrylate and 2-acrylamido-2-metering system sulfonic acid is formed, the comonomer proportioning consists of acrylonitrile: methyl acrylate: 2-acrylamido-2-metering system sulfonic acid=91.2: 8.5: 0.3, total polymerization monomer feed concentration is 34%, reaction temperature is 53 ℃, in 57 minutes reaction time, oxidant is a sodium chlorate, and consumption is 0.52% of total list, reductant is a sodium sulfite, and reductant and oxidant mol ratio are 1.52.Slurry takes off list after the polymerisation under 56Kpa vacuum, after washing under 57kPa vacuum, the 52 ℃ of temperature, is diluted to 34.5% concentration.Is 10kPa with NaSCN solution dissolving back in vacuum, removes bubble under 21.5 ℃ of conditions of the temperature difference, and filters that to obtain always be 11.6% spinning solution admittedly.The spinnerets of this spinning solution by the special requirement size is that 15.5wt%, temperature are that solidification forming is an as-spun fibre in 4.0 ℃ the coagulating bath in sodium sulfocyanate concentration, negative draw ratio 1.85.As-spun fibre enters the preliminary draft machine and stretches 2.1 times.After 57 ℃ of water washings, in dyeing machine, finish dyeing with cation dyes, the dyestuff additional amount is 70L/hr, 48 ℃ of dyeing temperatures.Tow 4.3 times of hot drawing-offs in 98.5 ℃ of hot water in dyeing back are respectively densification in 71 ℃, 69 ℃, 65 ℃ first drying machine at wet-bulb temperature, curl under 0.03MPa curls pressure, and finish typing successively, oil and dry.Heat setting temperature is 115 ℃, and last oil concentration is controlled to be 2.5%.Oven dry back fiber cuts off according to customer requirement, makes the colored flat acrylic fiber staple fibre product of different length.
The employed spinnerets of embodiment, dyeing shower nozzle specification and dyestuff title, proportioning see Table 1, and the value of chromatism of measuring coloured flat acrylic fiber sees Table 2.
After producing white flat acrylic fiber under identical polymerization, the spinning condition, select identical dye species and dyeing recipe for use, adopt bulk fibre high temperature decatize traditional dyeing mode that white flat acrylic fiber is carried out the dyeing of identical colour system, measure the value of chromatism of fiber, see Table 2.
Under identical polymerization, adopt conventional nozzle spray gel staining method, all the other spinning, dyeing condition are identical with embodiment 1～12 respectively, the coloured flat acrylic that obtains, the value of chromatism of mensuration fiber sees Table 2.
Table 1 spinnerets, dyeing shower nozzle specification and dyestuff title, proportioning
Table 2 fiber key property index
Annotate: aberration I is the value of chromatism of coloured flat acrylic fiber of employing the art of this patent route production.Aberration II is under identical polymerization, adopts conventional nozzle spray gel staining method, the coloured flat acrylic that obtains, the value of chromatism of mensuration fiber.Aberration III is under identical polymerization, spinning process condition, adopts bulk fibre high temperature decatize traditional dyeing mode that white flat acrylic fiber is carried out the dyeing of identical colour system, measures the value of chromatism of fiber.Aberration II reduction rate (%)=[(aberration II-aberration I)/aberration II] * 100%; Aberration III reduction rate (%)=[(aberration III-aberration I)/aberration III] * 100%.
Claims (9)
1. the production technology of a colored flat acrylic fiber is characterized in that may further comprise the steps successively:
A, to adopt with water be the ternary aqueous suspension polymerization of medium, and promptly three kinds of comonomers by the redox system initiated polymerization, and are regulated molecular weight by chain-transferring agent under the water condition;
In the polymerisation, acrylonitrile is first comonomer, and the mass percent that accounts for all comonomers is 90%～92%;
Second comonomer is a kind of in methyl acrylate, methyl methacrylate or the vinyl acetate, and the mass percent that accounts for all comonomers is 7.7%～9.6%;
The 3rd comonomer is a kind of in methylpropene sodium sulfonate, sodium vinyl sulfonate, Sodium styrene sulfonate or the 2-acrylamido-2-methyl propane sulfonic acid, and the mass percent that accounts for all comonomers is 0.3%～0.4%;
The input concentration of total polymerization monomer is 33～35wt%, and reaction temperature is 53～56 ℃, and the reaction time is 53～57 minutes;
Water miscible redox initiation system is adopted in reaction, and oxidant is ammonium persulfate, potassium peroxydisulfate or sodium chlorate; Reductant is sodium pyrosulfite, sodium hydrogensulfite or sodium sulfite; The oxidant consumption is 0.5～0.6% of all monomer gross masses, and the mol ratio of reductant and oxidant is 1.45～1.55: 1;
Described chain-transferring agent is a β hydroxyl ethyl mercaptan;
B, take off single and washing;
C, dissolving, deaeration and filtration;
D, spinning solidification forming;
To filter the resulting acrylonitrile compolymer body in back and make spinning solution in the sodium thiocyanate solution dissolving, the spinning solution after the heating is extruded from the rectangular opening of spinnerets, forms as-spun fibre through double diffusion in coagulating bath; Wherein, the content of acrylonitrile compolymer body is 11～12wt% in the described spinning solution; Described coagulating bath is for containing 14～15.5wt% sodium thiocyanate water solution, 1～4 ℃ of coagulation bath temperature, and draw ratio 1.7～1.9 is born in coagulating bath; Described spinnerets hole shape is a rectangle, and the length-width ratio of described rectangular opening is 12.93～16.67: 1, preferred 14.76: 1～16.25: 1, and hole count 7200～8500 holes of described spinnerets;
E, preliminary draft and washing;
F, dyeing;
By the dyeing of strip arc dye liquor injector head spray, dye mother solution is added flow at 50～80L/hr to washing back fiber, 42～50 ℃ of dyeing temperatures in dyeing machine;
Described strip arc dye liquor injector head is the arc shower nozzle of the "T"-shaped strip of hollow by nozzle boss (1), nozzle cap (6) and dye liquor inlet tube (2) formation, cross section, nozzle cap (6) is the semi-cylindrical of strip, the be staggered spray orifice (3) of some perforations of described nozzle cap (6);
G, hot drawing-off;
H, densification;
I. curl and typing;
J, oil and dry;
K, cut-out and packing.
2. the production technology of a kind of colored flat acrylic fiber according to claim 1 is characterized in that, in the staining procedure, described dyestuff is cation dyes, is cyanines class, heterocycle azo class, naphthalene lactam, azo class or anthraquinone dyes.
3. the production technology of a kind of colored flat acrylic fiber according to claim 1 is characterized in that, in the staining procedure, the spray orifice of described dye liquor injector head (3) is the wicker leaf shape spray orifice; There is the longitudinal fluting (4) of the spray orifice (3) of connection on same straight line on the surface of described nozzle cap (6).
4. the production technology of a kind of colored flat acrylic fiber according to claim 4 is characterized in that, described longitudinal fluting (4) is " V " connected in star, and " V " shape opening is outside; The angle theta of described " V " shape is 60 °.
5. the production technology of a kind of colored flat acrylic fiber according to claim 1 is characterized in that, in the staining procedure, the spray orifice of described dye liquor injector head (3) is vertically lined up three rows, and every round is equally spaced; Described nozzle cap (6) is a face of cylinder part, is of a size of: length * arc is wide=and 100mm * 50mm, face of cylinder diameter is 180mm; The major parameter of spray orifice (3) satisfies following relational expression:
The willow leaf of single wicker leaf shape spray orifice is long to be 2k mm,
Willow leaf is wide to be 2k/3mm,
Total hole count n satisfies: n=23-3k, wherein, k=1～6, preferred k=3 or 4.
6. the production line of a colored flat acrylic fiber, it is characterized in that comprising successively: polymeric kettle, demonomerization tower, vacuum rotate through filter, polymer storage tank, high-shear dissolution machine, deaeration tower, stoste filter press, spinning machine, preliminary draft machine, tow rinsing maching, dyeing machine, hot drawing machine, first drying machine, crimping machine, setting machine, oiling machine, second drying machine, cutting machine and baling press;
Wherein, dyeing machine is provided with some strip arc dye liquor injector heads, described strip arc dye liquor injector head is the arc shower nozzle of the "T"-shaped strip of hollow by nozzle boss (1), nozzle cap (6) and dye liquor inlet tube (2) formation, cross section, nozzle cap (6) is the semi-cylindrical of strip, the be staggered spray orifice (3) of some perforations of described nozzle cap (6).
7. the production line of a kind of colored flat acrylic fiber according to claim 7 is characterized in that, described spray orifice (3) is the wicker leaf shape spray orifice; There is the longitudinal fluting (4) of the spray orifice (3) of connection on same straight line on the surface of described nozzle cap (6).
8. the production line of a kind of colored flat acrylic fiber according to claim 7 is characterized in that, described longitudinal fluting (4) is " V " connected in star, and " V " shape opening is outside; The angle theta of described " V " shape is 60 °; Described spray orifice (3) is vertically lined up three rows, and every round is equally spaced; The cylindrical of described dye liquor inlet tube (2) has screw thread (5); Described nozzle boss (1) connects with welding manner with nozzle cap (6).
9. the production line of a kind of colored flat acrylic fiber according to claim 7 is characterized in that, described nozzle cap (6) is a face of cylinder part, is of a size of: length * arc is wide=and 100mm * 50mm, face of cylinder diameter is 180mm; The major parameter of spray orifice (3) satisfies following relational expression:
The willow leaf of single wicker leaf shape spray orifice is long to be 2k mm,
Willow leaf is wide to be 2k/3mm,
Total hole count n satisfies: n=23-3k, wherein, k=1～6, preferred k=3 or 4.
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