# US 9,751,247 B2 · Extrusion method

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- Number: US 9,751,247 B2
- Document ID: US9751247B2
- Status: Granted
- Kind: B2
- Application number: 14/241,653
- Filed: 2012-09-03
- Published: 2014-12-18
- Granted: 2017-09-05
- Earliest claimed: 2011-09-02
- Assignees: Aurotec GmbH
- Applicants: Stefan Zikeli; Friedrich Ecker
- Inventors: Stefan Zikeli; Friedrich Ecker
- Web page: https://patentgrep.com/patent/US9751247B2

## CPC

- B29C 48/1472: {at the die nozzle exit zone}
- B29C 48/022: {characterised by the choice of material}
- B29C 48/05: Filamentary, e.g. strands
- B29C 48/08: flexible, e.g. films
- B29C 48/345: Extrusion nozzles comprising two or more adjacently arranged ports, for simultaneously extruding multiple strands, e.g. for pelletising
- B29C 48/865: {Heating}
- B29C 48/87: Cooling
- B29C 48/919: {using a bath, e.g. extruding into an open bath to coagulate or cool the material}
- B29C 48/92: Measuring, controlling or regulating
- C08J 3/096: {Nitrogen containing compounds}
- C08J 5/18: Manufacture of films or sheets
- D01D 5/06: Wet spinning methods {(D01D5/0046 takes precedence)}
- D01F 2/00: Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D04H 3/013: Regenerated cellulose series
- D04H 3/16: with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion
- B29C 48/142: {using force fields, e.g. gravity or electrical fields (B29C48/9165 takes precedence)}
- B29C 48/872: {characterised by differential heating or cooling}
- B29C 48/917: {by applying pressurised gas to the surface of the flat article}
- B29C 2948/92514: Pressure
- B29C 2948/92704: Temperature
- B29K 2001/00: Use of cellulose, modified cellulose or cellulose derivatives, e.g. viscose, as moulding material
- B29K 2105/0073: {Solution}
- B29L 2007/00: Flat articles, e.g. films or sheets (B29L2024/00 takes precedence)
- B29L 2031/726: {Fabrics (nets B29L2028/00)}
- B29L 2031/731: {Filamentary material, i.e. comprised of a single element, e.g. filaments, strands, threads, fibres (cables B29L2031/707)}
- C08J 2301/02: Cellulose; Modified cellulose
- D01D 5/084: Heating filaments, threads or the like, leaving the spinnerettes
- D01D 5/088: Cooling filaments, threads or the like, leaving the spinnerettes
- D01D 10/02: Heat treatment (heating for finishing D02J13/00)
- D01D 10/06: Washing or drying
- D10B 2201/22: made from cellulose solutions
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- D01D: MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D04H: MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL (weaving D03; knitting D04B; braiding D04C; net-making D04G; sewing D05B; tufting D05C; finishing non-woven fabrics D06); FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING {; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION}(non-woven fabrics having an intermediate or external layer of a different kind, e.g. of woven fabric, B32B)
- B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29L: INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- D10B: INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES

## Abstract

A method is provided for producing solid cellulose filaments or films from a solution of cellulose, NMMO (N-methylmorpholine-N-oxide) and water, including pressure-extruding the solution by one or more extrusion openings and by solidifying the filaments or films in a precipitation bath. The solution is guided between the extrusion opening and the precipitation bath by an air gap, the temperature of the solution on the extrusion opening being lower than 105° C. and the pressure difference in the air gap between the pressure of the solution immediately prior to extrusion and after extrusion is between 8 and 40 bar.

## Claims

### Claim 1

A method for producing solid cellulosic shaped articles, or films, from a solution of cellulose, NMMO (N-methylmorpholine N-oxide) and water, comprising:
extruding the solution through one or more extrusion openings under pressure and solidifying said articles, or films, in a collecting bath, wherein a length of the solution extends between the extrusion openings and the collecting bath; and
guiding the solution through an air gap with a gas flow between the extrusion openings and the collecting bath, the temperature of the solution at the extrusion openings is below 105° C. and the pressure difference between the pressure of the solution immediately before extrusion and after extrusion in the air gap is between 8 and 40 bar, wherein the gas flow is guided against the entire length of the solution extending between the extrusion openings and the collecting bath by a fan and an additional flow guide element.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the temperature of the solution is between 80° C. and 98° C.

### Claim 3 (depends on 1)

The method according to claim 1, wherein the pressure difference is between 16 bar and 38 bar.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the pressure immediately before extrusion is between 13 and 50 bar.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the pressure after extrusion in the air gap is between 0.5 bar and 3 bar.

### Claim 6 (depends on 1)

The method according to claim 1, further comprising guiding a lateral gas flow in the air gap.

### Claim 7 (depends on 6)

The method according to claim 6, wherein the gas flow is between 30 to 300 liters/h of gas per mm of length of the region of the extrusion openings in the gas flow direction or is between 0.15 and 20 liters/h of gas per mm3 of spinning field volume in the air gap.

### Claim 8 (depends on 6)

The method according to claim 6, wherein the region between the extrusion openings and the collecting bath is flushed substantially completely by the gas flow.

### Claim 9 (depends on 6)

The method according to claim 6, wherein the gas flow is laminar.

### Claim 10 (depends on 6)

The method according to claim 6, further comprising a plurality of extrusion openings provided in the direction of the gas flow.

### Claim 11 (depends on 6)

The method according to claim 6, wherein a partial flow of the gas flow is heated by one of an extrusion plate comprising the extrusion openings or by a heating element in the fan.

### Claim 12 (depends on 1)

The method according to claim 1, wherein said articles are selected from cellulose filaments, cellulose staple fibres, cellulose non-woven articles or cellulose films.

### Claim 13 (depends on 1)

The method according to claim 1, wherein one or more components solubilising the cellulose are separated from the extruded solution by the gas flow.

### Claim 14 (depends on 13)

The method according to claim 13, wherein the components separated by means of the gas flow are discharged from the spinning field on a flow-off side.

### Claim 15 (depends on 14)

The method according to claim 14, wherein the components discharged from the spinning field on the flow-off side are crystallised.

### Claim 16

A method for producing solid cellulosic shaped articles, or films, from a solution of cellulose, NMMO (N-methylmorpholine N-oxide) and water, comprising:
extruding the solution through one or more extrusion openings under pressure and solidifying said articles, or films, in a collecting bath, wherein a length of the solution extends between the extrusion openings and the collecting bath; and
guiding the solution through an air gap with a gas flow directed toward the entire length of the solution extending between the extrusion openings and the collecting bath by a fan and an additional flow guide element, the temperature of the solution at the extrusion openings is below 105° C. and the pressure difference between the pressure of the solution immediately before extrusion and after extrusion in the air gap is between 8 and 40 bar so that NMMO particle formation in the air gap is reduced.