US1793649A - Process for maintaining the composition of viscose precipitating baths containing magnesium sulphate - Google Patents
Process for maintaining the composition of viscose precipitating baths containing magnesium sulphate Download PDFInfo
- Publication number
- US1793649A US1793649A US322295A US32229528A US1793649A US 1793649 A US1793649 A US 1793649A US 322295 A US322295 A US 322295A US 32229528 A US32229528 A US 32229528A US 1793649 A US1793649 A US 1793649A
- Authority
- US
- United States
- Prior art keywords
- bath
- sulphate
- sodium sulphate
- magnesium sulphate
- per litre
- 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
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title description 72
- 235000019341 magnesium sulphate Nutrition 0.000 title description 36
- 229910052943 magnesium sulfate Inorganic materials 0.000 title description 28
- 238000000034 method Methods 0.000 title description 20
- 229920000297 Rayon Polymers 0.000 title description 8
- 239000000203 mixture Substances 0.000 title description 7
- 230000001376 precipitating effect Effects 0.000 title description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 69
- 229910052938 sodium sulfate Inorganic materials 0.000 description 34
- 235000011152 sodium sulphate Nutrition 0.000 description 34
- 239000000243 solution Substances 0.000 description 23
- 150000003839 salts Chemical class 0.000 description 16
- 238000009987 spinning Methods 0.000 description 15
- 238000001816 cooling Methods 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 239000001117 sulphuric acid Substances 0.000 description 10
- 235000011149 sulphuric acid Nutrition 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000012452 mother liquor Substances 0.000 description 6
- 229910021653 sulphate ion Inorganic materials 0.000 description 6
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 241001237728 Precis Species 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- D01F13/00—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
- D01F13/02—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of cellulose, cellulose derivatives or proteins
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Definitions
- sulphuric acid precipitating baths which, in addition to sodium sulphate, also contain magnesium sulphate.
- Durin use the amount of sulphuric acid contained in the teract dilution by the water, or in evaporatspinning bath becomes reduced, owing to its being neutralized by the alkali of the viscose, and the quantity of the'spinning bath decreases, because a portion of the liquid is carried away by the products, e. g., the threads, and passes into the washing Water.
- Thepresent invention hasfor its object the provision and elaboration of a regeneration process which can be used for spinning baths which are required to contain magnesium sulphate in addition to sulphuric acid or sul phuric acid and sodium sulphate. That with such baths the simple evaporating process does not achieve the desired object has been shown by experiments, both with the main bath and also with the so-called upper baths, washing baths and. the like. It has been found, as a matter of fact, that in the simple evaporation of bath solutions containing both salts simultaneously, the sodium sulphate content increases, disproportionately to the magnesium sulphate content, since fresh sodium sulphate is continuously being formed in the spinning bath.
- Glauber salts separates out in the form of Glauber salts and to the extent of more than 80 gr. of sodium sulphate per litre, so that, after the separation of the crystals, a final liquor remains which,
- the bath is of the same composition as in the Example 1. This time the bath solution is first diluted'by about 12% so thata bath with about 115 gr. H 80 per litre, 165 gr. MgSO per litre, 115 gr. Na SO per litre is obtained. This solution is now cooled down to about 5 deg. C. At this temperature sodium sulphate free from magnesium sulphate separates out in the form of Glauber salts and in such quantity that only about 47% of sodium sulphate per litre still remains dissolved. The remaining liquor is worked up and used as in Example 1. About the same degree of efliciency is obtained.
- T bird example The bath solution to be operated on is com osed of 130 gr. H SO per litre, 240 gr. MggO. per litre, 130 gr. Na SO per litre.
- magnesium sulphate content does not amount to more than about 170 gr. per litre, separation of the Glauber salts may be effected at once by simple cooling.
- magnesium sulphate content amounts to more than about 220 gr. per litre a portion of the magnesium separated out by a first cooling own to about 8 to 10 deg. C. and then, after suitable dilution, the main portion of the sodium sulphate can be caused to crystallize out by a further coolingldown to 5 deg. C., for example.
- magnesium sulphate content lies in the intermediate region between 17 0 and 220 gr. per'litre, the magnesium sulphate content must first be increased by addition. Then the procedure may be as above described. Instead the ma esium sulphate content may be diminishe to less than 170 gr. per litre, by suitable dilution, and then according to the first directions, the separation of the Glauber salts may be begun at once.
- the new process can be used partly for concentrating the main spmning bath and to free it from anexcess of sodium sulphate. It can also be used for the working up of so-called drop baths which drop from spells or rollers or of centrifuge baths which are slung ofi irom spinning centrifuges, or of upper baths wherein spun spools are subsequently fixed or leached out. Ina'ny case the baths to be treated or parts thereof are advantageously worked up according to the process and the concentrated final liquor,
- sulphate may be,
- magnesium sulphate per litre part of the magnesium sulphate practically pure form by cooling, separating out the crystalline masses, diluting the resulting liquor and separating out sodium sulphate in ractically pure orm by further lowering. t e temperature, concentrating the resulting mother liquor and adding it with a proportion of magnesium sulphate to the precipitating bath to be revivified.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US461845A US1863172A (en) | 1928-11-27 | 1930-06-17 | Process for maintaining the composition of viscose precipitating baths containing magnesium sulphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1793649X | 1927-12-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US1793649A true US1793649A (en) | 1931-02-24 |
Family
ID=7743552
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US18802D Expired USRE18802E (en) | 1927-12-15 | Process for maintaining the composition of viscose precipitating baths | |
| US322295A Expired - Lifetime US1793649A (en) | 1927-12-15 | 1928-11-27 | Process for maintaining the composition of viscose precipitating baths containing magnesium sulphate |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US18802D Expired USRE18802E (en) | 1927-12-15 | Process for maintaining the composition of viscose precipitating baths |
Country Status (3)
| Country | Link |
|---|---|
| US (2) | US1793649A (enrdf_load_stackoverflow) |
| FR (1) | FR665645A (enrdf_load_stackoverflow) |
| NL (1) | NL32407C (enrdf_load_stackoverflow) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2570237A (en) * | 1950-06-17 | 1951-10-09 | Ind Rayon Corp | Spinning of acrylonitrile polymers |
| US2570257A (en) * | 1950-06-17 | 1951-10-09 | Ind Rayon Corp | Spinning of acrylonitrile polymers |
| US2645561A (en) * | 1948-11-23 | 1953-07-14 | Ind Rayon Corp | Sodium sulfate recovery |
| US6147272A (en) * | 1994-12-29 | 2000-11-14 | Institut Francais Du Petrole | Process for separating paraxylene comprising at least two crystallization stages at high temperature |
-
0
- NL NL32407D patent/NL32407C/xx active
- US US18802D patent/USRE18802E/en not_active Expired
-
1928
- 1928-11-27 US US322295A patent/US1793649A/en not_active Expired - Lifetime
- 1928-12-13 FR FR665645D patent/FR665645A/fr not_active Expired
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2645561A (en) * | 1948-11-23 | 1953-07-14 | Ind Rayon Corp | Sodium sulfate recovery |
| US2570237A (en) * | 1950-06-17 | 1951-10-09 | Ind Rayon Corp | Spinning of acrylonitrile polymers |
| US2570257A (en) * | 1950-06-17 | 1951-10-09 | Ind Rayon Corp | Spinning of acrylonitrile polymers |
| US6147272A (en) * | 1994-12-29 | 2000-11-14 | Institut Francais Du Petrole | Process for separating paraxylene comprising at least two crystallization stages at high temperature |
Also Published As
| Publication number | Publication date |
|---|---|
| NL32407C (enrdf_load_stackoverflow) | 1900-01-01 |
| FR665645A (fr) | 1929-09-20 |
| USRE18802E (en) | 1933-04-25 |
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