Process for Preparing a Non-Woven Cellulosic Structure and the Non-Woven Cellulosic Structure Prepared Therefrom
The present invention relates to a process for preparing a non-woven cellulosic structure comprising the steps of extruding continuous filaments from a cellulosic solution; passing the extruded filaments through a regenerating liquid to attenuate the filaments and laying the attenuated filaments into a web and to the non-woven cellulosic structure prepared therefrom.
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This Application claims priority to Indian Application No. 999/MUM/2004 dated 17.09.2004.
BACKGROUND OF INVENTIONThe present invention relates to a process for preparing a non-woven cellulosic structure and the non-woven cellulosic structure prepared therefrom. Particularly, the present invention relates to a process for preparing a consolidated multiple/single layer, absorbent, durable or disposable composite non-woven cellulosic structure comprising of at least one layer that is made from bio-degradable, continuous cellulosic material.
More particularly, the present invention relates to a process for preparing a non-woven cellulosic structure comprising of continuous, randomized cellulosic fibers and the composite non-woven cellulosic structure prepared therefrom.
1. Introduction
Consolidated non-woven structure may comprise of Viscose Fibers, Lyocell Fibers, Cellulose acetate, and/or its blends with synthetic fibers. Lyocell fiber is a man made fiber based on dissolving non-derivatized cellulose directly in an organic solvent. Lyocell fibers are produced by regeneration of cellulosic fiber from a solution of cellulose in an organic solvent like N Methyl Morpholine N Oxide.
2. Prior Art
The process of manufacturing cellulosic fibers is known in the prior art. U.S. Pat. No. 3,600,379 discloses a process of manufacturing Viscose fibers wherein the wood pulp is utilized as a raw material. It is steeped either as sheets or slurry with 17-22 percent NaOH solution. The excess steeping liquor is removed by pressing. The alkali cellulose is shredded and aged. The aged alkali cellulose is xanthated with an amount of carbon disulphide. The xanthate is dissolved in NaOH solution forming Viscose solution. The viscose is ripened and filtered once or several times either during or after ripening. The viscose solution can then be spun through fine orifices in acidic spin bath to form regenerated cellulosic filaments/fibers/tow. Viscose/Rayon spinning is almost 100 years old technology and hence described in brief only. Similarly preparation of non-derivatized cellulose solution through solvent spinning route is also known.
Indian Patent No. 189773 mentions a process of preparing cellulose solution for spinning fibers/films. The process includes introducing cellulose material into an aqueous solution of tertiary amine oxide to prepare a suspension. Later the suspension is subjected to high shear equipment heating under reduced pressure.
U.S. Pat. Nos. 4,144,080 and 4,246,221 disclose a method of preparation of amine oxide solution by extruding ground tertiary Amine Oxide solution and Cellulose. Also disclosed is the method of producing fibers by spinning the solution through fine orifices in air, orienting the same by mechanical stretching and regenerating the cellulose from the solution bay allowing the spun filaments to pass through a bath of a nonsolvent.
Once filaments are formed either through Viscose process or by any other process, the tow is washed and fibers cut into staple length. Conventionally the staple fibres are dried and baled (if non-wovens are prepared at different location). The dried staple fiber bale is opened, blended if required and carded to form a fibrous mat. This mat is directly or after cross lapping bonded to form a non-woven material.
Methods cited in U.S. Pat. Nos. 3,833,438 and 3,906,130 explain a process to make non-woven and perforated textile fabrics from continuous cupramonium rayon, viscose rayon and the like fiber filaments. In this process primarily the continuous filaments are cast on a conveyor, which is caused to oscillate laterally along with forward motion. The spinning units describe respective parallel and sinusoidal curves. Later, consolidation is achieved by water jets. Cupramonium rayon is an expensive method to produce absorbent cellulosic non-woven. Method involves mechanical moving parts like cam/crank mechanisms, which are prone to breakdown/maintenance. The limiting oscillation speed (cycles/min) limits the filament feed velocity and hence the production rate.
U.S. Pat. Nos. 3,620,903 and 4,069,563 disclose a method to produce light weight, non patterned non-woven fabrics by treating fibrous sheet of materials with fine, essentially one or more columnar streams of liquid jetted from orifices, under high pressure. A layer of fiber web is supported on a surface and traversed with the streams to entangle the fibers in a manner which imparts strength and stability without the need for binder.
The aforesaid patents describe the processes wherein the cellulosic solution is spun using a solvent spun method. The cellulosic fibers are spun and cut into staple lengths. Subsequently, they are treated with water and/or other chemicals. These wet fibers are then dried. In order to manufacture a non-woven product, the mat is opened by use of an opener, carded and then hydro entangled to obtain a spun laced product. The said product is re-dried to achieve a cellulosic non-woven fiber. This is a conventional and well-accepted method to produce cellulosic non-woven fiber. However, the process involves drying the said fiber twice, thereby increasing the costs. Also strength of the said non-woven fiber is not high since it comprises of short (staple) length fibers.
SUMMARY OF PRESENT INVENTIONThe present invention discloses a process of manufacturing continuous cellulosic filaments obviating the aforesaid drawbacks.
The present invention relates to a process for preparing a non-woven cellulosic structure comprising the steps of extruding filaments from a cellulosic solution; passing the extruded filaments through a regenerating liquid to attenuate the filaments and laying the attenuated filaments into a web and to the non-woven cellulosic structure prepared therefrom.
The present invention will now be described with reference to the figures accompanying the specification, wherein the same numerals denote the same parts and wherein:
Referring to
Pulp preferred for use for making the solution is soft wood pulp having high alpha cellulose content (89-93%) and low semi-cellulose content. DP (Degree of Polymerization) of the pulp is in the range of 600 to 1100, preferred range would be 700 to 1000. Cellulose concentration to achieve a spin able solution can be in the range of 5% to 28%. Preferably 7% to 20%, most preferred values of the cellulose concentration are 10% to 15%. NMMO (N-Methyl Morpholine N-Oxide) as available in the market is of 50% concentration has to be pre-concentrated to 77% prior to dissolution of cellulose by conventional distillation process. Blending of small pieces of pulp with pre-concentrated solvent is carried out at about 100° C. in a double blade sigma mixer where in vacuum of 400 mm Hg is applied. After duration of 1.5 hours a homogeneous solution is obtained, which is allowed to cool down to solid condition. Other methods available for making cellulose solutions on a continuous basis are available like use of high shear blender, thin film device or a devolatalizing type counter rotating twin screw extruders. A method described in Indian Patent No. 189773 may also be followed.
A spinning die with multiple holes arranged in a rectangular configuration having aspect ratio of length to breadth around 1.2 to 200, which has spinning hole diameters ranging from 50 micron to 150 micron, preferably 55 to 100 microns, is utilized to extrude filaments. The above given aspect ratio allows for providing 10 to 60 rows of holes.
During spinning of Lyocell polymer at 90 to 110 deg C., adequate air gap and air flow in cross direction is provided. Depending upon the size of the spinneret and the stretch ratio, filaments from sub denier to 5 deniers can be spun.
Filaments coming out in the form of a curtain retain their rectangular configuration by the virtue of a special device, which contains the regeneration bath. Central portion of the box has a funnel type arrangement. The funnel may be perforated from the top and plain below a certain distance. Internal are so arranged such that a slit is provided at the bottom of the funnel, which serves as an outlet for the regeneration solution as well as outlet for spun filament. The funnel is sealed and isolated from the sides so that the regeneration liquid from the bottom of the box cannot enter the funnel. The inlet of the regeneration liquid is provided at the bottom. As the liquid fills the box and level is raised beyond the plain portion of the funnel, the liquid reaches to the perforated portion of the funnel. Liquid enters the funnel. Flow in the box is so adjusted that the outlet level matches with the inlet and always keeps the regeneration box full up to the brim. The velocity of the extruded filaments is 8 m/min to 80 m/min.
Flow of liquid inside a small width accelerates the filaments from the spinneret. The regeneration liquid is sent for solvent recovery process. Velocity of the regeneration liquid attained at the outlet of the spinning box is governed by the relation:
V2=2×g×h
h—height of regeneration liquid from funnel bottom opening in m
V—velocity of regeneration liquid in m/sec.
The velocity of the regenerating liquid is kept between 50 m/min to 250 m/min, preferably between 100 m/min to 200 m/min.
Flow rate of regeneration liquid required to maintain the level in the spinning box is governed by the relation:
Q=L×W×V
W—Opening of the funnel bottom in m
Q—Quantity of regeneration liquid required to maintain the level in m3/Hr.
From the above relations it can be observed that for a given width of spinneret, water flow depends mainly on 2 parameters, viz. the height and the funnel bottom opening. Trials conducted on various funnels showed that higher the liquid height, higher is the flow rate and higher is the drag (stretch) imparted to the filaments. On the other side of it, higher the water flow rate means higher water energy at the funnel outlet position. Higher the water energy higher is the disturbance imparted to filaments. Therefore while-designing a spinning box funnel one should keep both these factors into consideration. Examples cited show different funnel configurations.
When the extruded filaments are passed through the regenerating liquid, the filaments are attenuated.
The said filaments formed by the method described above are brought to the belt conveyor where filaments may get additionally randomized due to flow of regenerating liquid. As an alternative for belt conveyor, collection of web may be done on a rotary vacuum drum system. The feeding box may have a mechanically driven twin roll arrangement to draw the web and feed it below. The feeding box has a variable speed drive and is pivoted by a swing arrangement which lays down the web in folds on to the moving collecting belt. Step less adjustment of the swing amplitude and the swing speed can also be provided. Depending upon the coverage required the speed of the swing, the amplitude of the swing, the drop down rate and belt conveyor speed can be adjusted so as to get webs with coverage from 10 to 600 gsm. Filament mat can also be formed without swinging the feeding box also. Then the only variables would be the conveyor and the curtain drop down speed.
Yet another laying option is cross lapping. The method is similar to the one shown in
The un-bonded web then passes through consolidation step, which may include hydro-entanglement, chemical bonding, needle punching system, etc., which consolidates the mat fibers together to produce a bonded consolidated non-woven material.
Wet non-woven bonded material is thereafter treated for, bleaching, further washing, dyeing, soft finishing, etc. and then passed through a dryer that expels excess moisture. Subsequently the web is collected on the winder and rolled. The said web has a soft handle and good strength and may be used for many different applications of semi-durable or disposable segment.
Viscose Spinning Route:Properly aged, filtered, ripened and deaerated viscose is fed at right temperature to the spinning machine. Spinneret holder may remain same or needs to be modified suitable to the cluster plate which has circular precious metal eyes fitted and arranged in the form of a rectangular shape. Each eye is drilled with required number of spinning orifices following the conventional triangular pitch and configuration.
Spinneret is dipped in the spin bath maintained at desired temperature and concentration level in the bottom down position, i.e. the spinning orifices face downwards. The only difference between Lyocell route and Viscose route is that in Lyocell route, an air gap is maintained between the regeneration liquid and spinneret, while in case of Viscose route, spinneret is immersed in the regeneration bath, since Viscose spinning is a wet spinning process. Thus a viscose web is formed. Cross section of the cellulosic fibers may be altered by using different spinnerets to obtain tri-lobal, Y-shaped, or other shapes to impart specific properties to the structure. Subsequent steps are same as mentioned above for the solvent spinning route for the formation of a non-woven material. Only the hydro entanglement/consolidation operating parameters might differ for Viscose.
Understanding the filament behavior when they are laid down is necessary. Hence an analogy of a thread is considered. When a thread is laid down perpendicularly on to a moving belt, the laid down form taken by the thread is determined by the filament properties (linear density, bending rigidity and torsional rigidity, height of the feed point and feed to belt speed ratio). Further, important variables apart from the filament properties in the process of lay down are filament velocity, belt speed, water velocity, height of the spinning box from the belt, vacuum below the collecting belt and design of the spinning box.
Consolidation:Once the curtain of randomized/laid continuous cellulosic filaments is obtained, next process is to consolidate the curtain into a non-woven web. There are numerous options available (as shown in
Test procedures used to determine the properties of the consolidated non-woven structure and products made by the disclosed process are known to those well versed in the non-woven field.
Tensile Tests:A sample of 200 mm length and 2.5 cm wide can be stretched in an Instron equipment at a rate of 100 mm/min obtains the point at which the structure yields. This figure when represented in N/2.5 cm value describes the value of tensile strength of a non-woven. Values obtained are shown in the table No. 1.
Fiber Orientation Distribution:This test is a measure of randomization of filaments in a non-woven structure. Two example graphs as shown below: Graph: 1 represents a non-woven structure which has more number of filaments in a particular direction—representing a low degree of randomization, while Graph: 2 shows a non-woven structure with a higher degree of randomization. One can thus determine the amount of randomization of the web structure.
Other tests which are essential to understand the performance of the product are: Basis weight, Elongation at break, tear strength, web abrasion resistance test, drop absorbency test, absorbent capacity test, vertical wicking rate, drip capacity test, dry lint release test. Procedure for these tests can be obtained from any non-woven handbook.
EXAMPLES Example 112% cellulose Lyocell polymer solution was fed at the rate of 0.06 grams/hole/min through a rectangular spinneret having 20 rows of 80 micron diameter holes, giving an extrusion speed of 10 m/min. Below the spinneret the spinning box maintaining a regeneration liquid column of 510 mm was installed in such a way that the gap between top most water surface and spinneret bottom is between 15 to 25 mm. 5 mm gap was provided in the funnel bottom portion. Regeneration liquid flow rate of 10 to 15 m3/hr was sufficient to maintain full level in spinning box. The velocity of the liquid is kept at 190 m/min. Although the water velocity at the outlet of the funnel is much higher, the drag imparted to the filaments made them to attenuate at 40 to 60 m/min speed, thus giving a draw ratio of 4 to 6. (Draw ratio is the ratio of filament speed to extrusion speed.) Collection belt operating at 10 m/min below the spinning box maintained a distance of 120 mm between the spinning box. Vacuum of 400 mm of water column was provided below the laying portion. Web obtained on the belt was washed clear off the solvent and sent to multi layering device and then for bonding. Different samples were prepared by varying the number of layers to get non-woven samples of different coverage. Non-wovens obtained had good strength, were soft and absorbent. Samples were tested for coverage in grams/square metre (gsm), water absorbency measured in gram/gram and tensile tests as described above in machine direction (MD) and in cross direction (CD) both in dry and wet condition. Key test results are tabulated below:
11% cellulose Lyocell polymer solution was fed at the rate of 0.01 grams/hole/min through a rectangular spinneret having 20 rows of 80 micron diameter holes, giving an extrusion speed of 1.72 m/min. Spinning box was maintained at regeneration liquid column of 170 mm. 4 mm gap was provided in the funnel bottom portion. Regeneration liquid flow rate of 7 m3/hr was sufficient to maintain full level in spinning box. The velocity of the liquid is kept at 109 m/min. Although the water velocity at the outlet of the funnel is much higher, the drag imparted to the filaments made them to attenuate at 8 m/min speed, thus giving a draw ratio of 4.6. Web laying speed was kept at 1 to 3 m/min to obtain a uniform non-woven. Vacuum of 255 mm of water column was provided below the laying portion. Web obtained on the belt was washed clear off the solvent and sent to multi layering device and then for bonding. Different samples were prepared by varying the number of layers to get non-woven samples of different coverage. Results obtained were very similar to those disclosed above.
The present invention can also be worked on viscose to achieve similar comparative results.
Benefits of this Invention:a) For the same coverage, strength of the cellulosic non-woven fabric is higher by a factor of 1.5 to 2 as compared to staple fiber carded spun laced fabric and substantially higher as compared to Lyocell melt blown fabric. This means, keeping the material input same one can get a stronger fabric or for the same strength lower usage of material can serve the same purpose.
b) Process does not involve use of expensive high temperature air for spinning as done in Lyocell melt blowing. Entire process operates on lower temperatures, thus reduction in total energy consumed per Kg of fabric.
c) Attenuation of filaments does not need expensive high pressure air.
d) Randomization of filaments does not need injection of high pressure fluid and large vacuum levels. It uses low quantity and velocity of recyclable fluid.
e) Process from Viscose to Web or from Lyocell dope to Web involves only one step of drying (in the final stage after spun lacing), thus saving one complete step of drying as compared to non-woven webs made through staple fiber—carded spun laced route. This process also eliminates tow cutting, fiber opening and carding steps.
f) Once a randomized mat is produced, one can adopt other processes to consolidate the web, viz. needle punching, using binders, etc. without the use of additional equipments like cross lappers, etc.
g) Process uses only continuous fibers, hence no chances of short fibers resulting into linting, ideal for producing wipes for clean room application
Claims
1-17. (canceled)
18. A process for preparing a non-woven cellulosic structure comprising the steps of:
- a) extruding filaments from a cellulosic solution;
- b) passing said extruded filaments through a regenerating liquid, to attenuate and randomize said filaments; and
- c) laying said attenuated and randomized filaments into a web.
19. The process of claim 18, wherein said filaments are continuous.
20. The process of claim 19, wherein said structure is uniform.
21. The process of claim 20, wherein said non-woven cellulosic structure is consolidated.
22. The process of claim 18 wherein said regenerating liquid and said extruded filament are passed through a gap of from 3 mm to 7 mm.
23. The process of claim 22, wherein said regenerating liquid and said extruded filament are passed through a gap of from 4 mm to 6 mm.
24. The process of claim 18 wherein said regenerating liquid has a velocity of from 50 m/min to 330 m/min.
25. The process of claim 24 wherein said regenerating liquid has a velocity of from 200 m/min to 216 m/min.
26. The process of claim 24 wherein said velocity of said regenerating liquid is attained by a gravitational force.
27. The process of claim 18 wherein said filament is from 1 to 5 denier.
28. The process of claim 18 wherein a velocity of said extruded filament when it exits from said regenerating liquid is from 8 m/min to 80 m/min.
29. The process of claim 18 wherein a velocity of said extruded filament provides a maximum draw ratio of 6.
30. The process of claim 18 wherein said laying is carried out by a vacuum assisted process.
31. The process of claim 30 wherein said vacuum assisted process is achieved by a rotary vacuum drum system.
32. A non-woven cellulosic structure comprising:
- a plurality of extruded continuous filaments attenuated in a regenerating liquid and laid into a web.
33. The non-woven cellulosic structure of claim 32, wherein said plurality of filaments is formed of lyocell, viscose or a combination of lyocell and viscose.
34. A non-woven consolidated structure comprising:
- at least one layer of a non-woven cellulosic structure having a plurality of extruded continuous filaments attenuated in a regenerating liquid and laid into a web; and
- another layer of a cellulosic or synthetic non woven material.
Type: Application
Filed: Sep 16, 2005
Publication Date: Jan 31, 2008
Applicant:
Inventors: Jagrat M. Mankad (Mumbai), Parag D. Patil (Mumbai), Aditya N. Shrivastava (Nagda), Brij B. Koutu (Nagda), Raj K. Ojha (Nagda)
Application Number: 11/574,680
International Classification: D04H 3/02 (20060101); D01F 2/00 (20060101);