US3389428A - Apparatus for the wet extrusion of solutions of polymers of vinyl chloride exhibiting a high degree of syndiotacticity - Google Patents
Apparatus for the wet extrusion of solutions of polymers of vinyl chloride exhibiting a high degree of syndiotacticity Download PDFInfo
- Publication number
- US3389428A US3389428A US310992A US31099263A US3389428A US 3389428 A US3389428 A US 3389428A US 310992 A US310992 A US 310992A US 31099263 A US31099263 A US 31099263A US 3389428 A US3389428 A US 3389428A
- Authority
- US
- United States
- Prior art keywords
- spinneret
- spinning
- side wall
- syndiotacticity
- vinyl chloride
- 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.)
- Expired - Lifetime
Links
- 229920000642 polymer Polymers 0.000 title claims description 20
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 title claims description 12
- 230000001747 exhibiting effect Effects 0.000 title description 6
- 238000001125 extrusion Methods 0.000 title description 4
- 238000009987 spinning Methods 0.000 claims description 31
- 238000002166 wet spinning Methods 0.000 claims description 8
- 239000013529 heat transfer fluid Substances 0.000 claims description 2
- 239000000499 gel Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/08—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons
- D01F6/10—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons from polyvinyl chloride or polyvinylidene chloride
Definitions
- the present invention relates to apparatus for the wet spinning of polymer solutions, and in particular apparatus which does not require the spinning device to be dipped into the coagulum bath.
- the invention relates to an apparatus for wet spinning vinyl polymer solutions which may be successfully used where it is necessary, for example, to maintain the spinning device separate from the coagulum bath, to maintain the temperature of the solution higher than that of the coagulum bath, or to prevent the material forming the spinneret holder being attached by the coagulum bath.
- One of the principal applications of this invention is the wet spinning of solutions of vinyl chloride polymers exhibiting a high degree of syndiotacticity, in which cases it is necessary to maintain the spinning solution at high temperature, at least over 80 C. e.g., in the range of about 90 to 150 C. while maintaining the temperature of the coagulum bath considerably lower, e.g., in the range of about 30 to 80 C. and usually less than 60 C.
- polymers of vinyl chloride exhibiting a high degree of syndiotactieity should be understood to embrace homopolymers of vinyl chloride having a syndiotacticity degree greater than 2 (the degree of syndiotacticity determined by the absorption bands ratio LR. D635 and D692 cmr see Burleigh ].A.C.S., 82 page 7494960), as well as its copolymers and their mixtures comprising at least 85% vinyl chloride by weight.
- the equipment usually employed in wet spinning of polymer solutions consists of a spinning device mounted to suitable spinner holders, the entire combination being adaptable for complete immersion into the coagulum bath.
- the dope is fed to each spinning device by means of a spin-metering pump connected to the main duet through which the dope flows from the storage tanks. It is readily observable that this type of spinning device is quite unsuitable where the spinning device should be maintained separate from the coagulum bath.
- spinning devices of this type are unsuitable for Wet spinning of vinyl chloride polymers having a high degree of syndiotacticity, which require a coagulum bath maintained at a temperature definitely lower than that of the dope; as matter of fact it is known that soluions of vinyl chloride polymers exhibiting a high degree of syndiotacticity have the tendency to gel at fairly high temperatures, therefore during the passage in a coagulum bath maintained at low temperature as above said, the solutions gel immediately.
- the gel temperature is strictly related to the stereo regularity of the product, hence to the polymerization temperature and quantity of polymer present in the solution.
- a solution having 18% polymer and a syndiotacticity degree of about 2.2, and an intrinsic viscosity of 1.3 abruptly gels at about 90-95 C., while a solution at 20% of the same polymer gels at 105-110 C.
- coaguluant mixtures which prove more effective in the spinning of vinyl chloride polymers having a high degree of syndiotacticity, comprise rather volatile compounds, which must be maintained at temperatures in the range of about 3080 C. in order to avoid excessive evaporation of the same with a consequent increased cost of the finished product, which would render the process commercially uneconomic. Furthermore it has been experimentally proved, in cases in which non volatile compounds have been employed as coagulant mixtures, that the coagulum is better and brighter and more compact fibers are obtained, if the coagulation is carried out at temperatures lower than 50-60 C.
- an apparatus and method for spinning of polymer solution in which the surface contact between the spinning device, hence dope to be spun, and the coagulum bath is extremely limited, that is, limited strictly to the external surface of the spinneret.
- the spinning apparatus of this invention allows the spinning of polymer solutions requiring the maintainance of high temperatures until the moment of extrusion, and a coagulum bath at considerably lower temperatures.
- Another advantage derived from apparatus of this invention lies in the improved filterability of the solution because the solution is more fluid, being the temperature maintained high, which in turn makes it possible to use very thin filters, avoiding thereby, clogging of the spinneret holes, and improving the evenness and final characteristics of the obtained fibres.
- FIGURE 1 is a diagrammatic perspective view showing a wet spinning apparatus according to this invention.
- FIGURE 2 is a sectional view of a spinning head suitable for use in this invention.
- the spinning solution coming from tank by means of general duct 1 passes into the metering pump 2, and after filtering into the filter 3, it goes to the spinning de vice 4, which is screwed, flanged or coupled by means of a system which assures a perfect sealing to the spinneret holder 5 directly coupled to tank 6, which contains the coagulum bath. In such a manner, the contact between the spinning solution and the coagulum bath is limited .to the external surface of the spinneret.
- Tank 6 is provided at the lower part with a discharge valve 12, which allows the discharge of the coagulum bath every time it calls for a cleaning or a checking of the spinning device.
- the yarns 10, coming from the spinning device, are coagulated in a suitable bath deviated from roller 11 and are subjected to appropriate treatment.
- FIGURE 1 shows a sectional view of the spinning head, object of this invention.
- the dope coming from tube 13 is filtered under heat in a plug filter 14 and is then filtered in a disk-filter 15, which is supported by plate 116, finally being extruded through spinneret 17.
- the whole block is kept heated by sleeve 18, wherein vapor or hot oil is circulating entering at 18' and coming out at 18".
- Sleeve 18 is fixed to wall 19 of the coagulation tank by means of bolts 20 and 26', while tightness of the coagulation tank is ensured by a toroidal gasket 21.
- This gasket 21 is pressed against wall 19 by a cylindrical body 19, which is pushed by a threaded rod 22 which in its turn is engaged on the tilting bracket 23 mounted in a turning way on pivot 23.
- Apparatus for forming fibres, filaments and yarns by wet-spinning of solutions of polymers of vinyl chloride having a degree of syndiotacticity greater than 2, wherein the polymer solution must be maintained at a temperature higher than that of the coagulum bath comprising a tank for holding the coagulum bath provided with an opening in its side wall; a sleeve fixed to said tank side Wall and having an end in registry with the opening in said side wall; a metering pump for the spinning solution, a filter and a spinneret connected in sequence and enclosed by said sleeve with the spinneret directed to deliver the spinning solution through said opening in the tank side wall; means securing the spinncret in the end of said sleeve and in relation to the opening in the tank side Wall so that the surface contact between the spinneret and coagulum bath is limited only to the external frontal surface of the spin neret; and means for circulating a heat transfer fluid through said sleeve in heat transfer
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IT2753162 | 1962-09-27 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3389428A true US3389428A (en) | 1968-06-25 |
Family
ID=11221840
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US310992A Expired - Lifetime US3389428A (en) | 1962-09-27 | 1963-09-24 | Apparatus for the wet extrusion of solutions of polymers of vinyl chloride exhibiting a high degree of syndiotacticity |
Country Status (6)
Country | Link |
---|---|
US (1) | US3389428A (en, 2012) |
BE (1) | BE637676A (en, 2012) |
DE (1) | DE1435324C3 (en, 2012) |
GB (1) | GB1064494A (en, 2012) |
NL (1) | NL298105A (en, 2012) |
SE (1) | SE304348B (en, 2012) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3879506A (en) * | 1970-06-01 | 1975-04-22 | Chatillon Societa & 0 Anonima | Process for producing chloro-vinyl fibers having modified light reflection |
CN101899719A (zh) * | 2009-05-25 | 2010-12-01 | 上海启鹏化工有限公司 | 一种新型纺丝组件 |
US20140141111A1 (en) * | 2011-06-15 | 2014-05-22 | Trützschler Nonwovens Gmbh | Spinning bath vat |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19949399A1 (de) | 1999-10-13 | 2001-05-10 | Fraunhofer Ges Forschung | Spinndüsenvorrichtung einer Nassspinneinrichtung |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
USRE20080E (en) * | 1933-01-25 | 1936-08-25 | Process for making films and the | |
US2367493A (en) * | 1940-12-19 | 1945-01-16 | Eastman Kodak Co | Cellulose derivative extrusion process |
US2984593A (en) * | 1959-08-31 | 1961-05-16 | Monsanto Chemicals | Uniaxially oriented polyvinyl chloride |
US3011859A (en) * | 1958-08-18 | 1961-12-05 | Chemstrand Corp | Manufacture of polymeric shaped objects by wet spinning |
US3044115A (en) * | 1958-11-21 | 1962-07-17 | American Viscose Corp | Method and apparatus for producing films |
US3206529A (en) * | 1961-11-30 | 1965-09-14 | American Enka Corp | Extrusion process and apparatus |
US3222317A (en) * | 1961-10-30 | 1965-12-07 | Argus Chem | Polyvinyl chloride stabilized with a combination of organotin compounds and aromatic nitrogen compounds |
-
0
- BE BE637676D patent/BE637676A/xx unknown
- NL NL298105D patent/NL298105A/xx unknown
-
1963
- 1963-09-19 GB GB36893/65A patent/GB1064494A/en not_active Expired
- 1963-09-21 DE DE1435324A patent/DE1435324C3/de not_active Expired
- 1963-09-24 US US310992A patent/US3389428A/en not_active Expired - Lifetime
- 1963-09-27 SE SE10610/63A patent/SE304348B/xx unknown
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
USRE20080E (en) * | 1933-01-25 | 1936-08-25 | Process for making films and the | |
US2367493A (en) * | 1940-12-19 | 1945-01-16 | Eastman Kodak Co | Cellulose derivative extrusion process |
US3011859A (en) * | 1958-08-18 | 1961-12-05 | Chemstrand Corp | Manufacture of polymeric shaped objects by wet spinning |
US3044115A (en) * | 1958-11-21 | 1962-07-17 | American Viscose Corp | Method and apparatus for producing films |
US2984593A (en) * | 1959-08-31 | 1961-05-16 | Monsanto Chemicals | Uniaxially oriented polyvinyl chloride |
US3222317A (en) * | 1961-10-30 | 1965-12-07 | Argus Chem | Polyvinyl chloride stabilized with a combination of organotin compounds and aromatic nitrogen compounds |
US3206529A (en) * | 1961-11-30 | 1965-09-14 | American Enka Corp | Extrusion process and apparatus |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3879506A (en) * | 1970-06-01 | 1975-04-22 | Chatillon Societa & 0 Anonima | Process for producing chloro-vinyl fibers having modified light reflection |
CN101899719A (zh) * | 2009-05-25 | 2010-12-01 | 上海启鹏化工有限公司 | 一种新型纺丝组件 |
US20140141111A1 (en) * | 2011-06-15 | 2014-05-22 | Trützschler Nonwovens Gmbh | Spinning bath vat |
US9334585B2 (en) * | 2011-06-15 | 2016-05-10 | Truetzschler Nonwovens Gmbh | Spinning bath vat |
Also Published As
Publication number | Publication date |
---|---|
DE1435324C3 (de) | 1974-03-07 |
DE1435324B2 (de) | 1973-08-02 |
DE1435324A1 (de) | 1969-03-20 |
GB1064494A (en) | 1967-04-05 |
SE304348B (en, 2012) | 1968-09-23 |
NL298105A (en, 2012) | |
BE637676A (en, 2012) |
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