EP1846456A1 - Method for shaping cellulose ethers - Google Patents
Method for shaping cellulose ethersInfo
- Publication number
- EP1846456A1 EP1846456A1 EP06703567A EP06703567A EP1846456A1 EP 1846456 A1 EP1846456 A1 EP 1846456A1 EP 06703567 A EP06703567 A EP 06703567A EP 06703567 A EP06703567 A EP 06703567A EP 1846456 A1 EP1846456 A1 EP 1846456A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cellulose ethers
- cellulose ether
- holes
- product
- cellulose
- 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.)
- Withdrawn
Links
- 229920003086 cellulose ether Polymers 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000007493 shaping process Methods 0.000 title description 4
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 claims description 3
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 3
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 3
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 3
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229920000896 Ethulose Polymers 0.000 claims description 2
- 239000001859 Ethyl hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 2
- 235000019326 ethyl hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 2
- 229920000609 methyl cellulose Polymers 0.000 claims description 2
- 239000001923 methylcellulose Substances 0.000 claims description 2
- 235000010981 methylcellulose Nutrition 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 description 4
- 239000008188 pellet Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/20—Post-etherification treatments of chemical or physical type, e.g. mixed etherification in two steps, including purification
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
Definitions
- the present invention relates to a process for the preparation of cellulose ethers having a higher bulk density and a narrower particle size distribution compared to known cellulose ethers, by forcing the cellulose ethers through a perforated plate.
- the shaping step represents an important process step for influencing the properties of the product.
- quality parameters such as the grading curve and bulk density are influenced in this step.
- This process step is usually carried out after product washing and before drying and grinding.
- shaping takes place by the buildup agglomeration in horizontal litter mixers, in which the moist product is agglomerated, compacted and compacted (see, for example, DE 20 28 310, DE 33 08 420 A1).
- the cellulose ether is passed into an apparatus in which an axis is arranged vertically.
- a fixed plate On the axis of a fixed plate (plate), which has holes with a defined ratio of diameter to length attached.
- On this plate run roles (Koller, wheels, rollers), which press the cellulose ether in the holes, whereby this is forced promoted.
- Below the plate the cellulose ether is separated by rotating scrapers and thereby divided into small pellets.
- a further embodiment of the invention in a flat die press, in which the circumferential Koller (wheels), based on a comparison with holes provided for die (plate) run, the cellulose ether is forced through the holes of the die. Underneath the die is a shearing device to bring the pellets to the desired length. At least one Koller runs in the pug mill. Usual are two Koller; but it can also be more than two Koller. This depends on the size of the unit and the diameter of the Koller.
- the cellulose ether is compressed as it passes through the holes.
- About the geometry of the holes can be set the degree of compression. This regulates the necessary energy for the compression process.
- the cross-sectional shape of the moldings is determined by the shape of the hole cross-section.
- the consistency of the densified cellulose ether depends on circular holes from the press ratio P from.
- P is defined as the ratio of the length of the hole to the diameter of the hole in the die.
- the pressing ratio P should be between 0.5 and 5.0, preferably between 2 and 4.0.
- the holes have a square, rectangular, oval or irregular shaped cross-section.
- the number of holes per unit area of the plate depends on the stability of the plate.
- Suitable cellulose ethers for carrying out the process according to the invention are, for example, ionic and nonionic cellulose ethers.
- ionic are, for example, to call
- Carboxymethylcellulose hydroxyethylcarboxymethylcellulose, carboxymethylsulfoethylcellulose and sulfoethylcellulose, preferably carboxymethylcellulose.
- examples which may be mentioned as nonionic are hydroxyethylmethylcellulose, hydroxypropylmethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, ethylhydroxyethylcellulose, methylcellulose, preferably hydroxyethylmethylcellulose and hydroxypropylmethylcellulose.
- the cellulose ethers compacted by the process according to the invention have a higher bulk density with otherwise identical properties and form more stable granules than according to the prior art the art-treated cellulose ether.
- Typical bulk densities for the commercially valuable cellulose ethers compacted by the process according to the invention are from 400 g / l to 800 g / l.
- Typical particle size distributions of these cellulose ethers are from 125 ⁇ m to 1000 ⁇ m with an average particle size of 500 ⁇ m.
- the uncompressed material is added to the muller thread via a dosing device (eg screw, belt). It is also possible to render the pug mill inert, for example with nitrogen or carbon dioxide.
- a dosing device eg screw, belt
- the pug mill inert for example with nitrogen or carbon dioxide.
- Product CMC CRT 40000 (degree of substitution (DS) 0.9, product moisture 42%, viscosity of a 2% aqueous solution 40000 mP-s) is introduced as the fibrous, de-alcoholized drive in a horizontal mixer and continuously granulated.
- the granulate obtained is dried and subsequently milled in a batch apparatus' in a hammer mill with a screen basket to the required fineness.
- the product is screened off above 1 mm.
- Example 1 (according to the invention):
- Bulk density 711 g / l; Proportions less than 0.125 mm: 14% by weight, K 0.995
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Crushing And Grinding (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102005004893A DE102005004893B4 (en) | 2005-02-03 | 2005-02-03 | Process for shaping cellulose ethers |
| PCT/EP2006/000528 WO2006081955A1 (en) | 2005-02-03 | 2006-01-21 | Method for shaping cellulose ethers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP1846456A1 true EP1846456A1 (en) | 2007-10-24 |
Family
ID=36061388
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP06703567A Withdrawn EP1846456A1 (en) | 2005-02-03 | 2006-01-21 | Method for shaping cellulose ethers |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US20060205935A1 (en) |
| EP (1) | EP1846456A1 (en) |
| JP (1) | JP2008528773A (en) |
| KR (1) | KR20070101236A (en) |
| CN (1) | CN101039961B (en) |
| BR (1) | BRPI0605928A2 (en) |
| DE (1) | DE102005004893B4 (en) |
| WO (1) | WO2006081955A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2010234844A1 (en) * | 2009-03-31 | 2011-09-08 | Dow Global Technologies Llc | Carboxymethyl cellulose with improved properties |
| MX377527B (en) * | 2015-10-27 | 2025-03-10 | Shinetsu Chemical Co | NON-IONIC POROUS CELLULOSE ETHER SOLUBLE IN WATER THAT HAS EXCELLENT SOLUBILITY AND METHOD FOR PRODUCING THE SAME. |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3054705A (en) * | 1960-11-07 | 1962-09-18 | Rayonier Inc | Hydroxyethylcellulose pellets and process |
| DE2038310C3 (en) * | 1970-08-01 | 1982-04-01 | Henkel KGaA, 4000 Düsseldorf | Process and device for the continuous production of pure and dry carboxymethyl cellulose |
| DE2410789C2 (en) * | 1974-03-07 | 1980-08-07 | Hoechst Ag, 6000 Frankfurt | Process for cold grinding of cellulose derivatives |
| DE3038001A1 (en) * | 1980-10-08 | 1982-05-06 | Henkel KGaA, 4000 Düsseldorf | METHOD FOR PRODUCING MICROPOWDER FROM CELLULOSEETHER OR CELLULOSE |
| DE3308420A1 (en) * | 1983-03-09 | 1984-09-13 | Wolff Walsrode Ag, 3030 Walsrode | METHOD FOR CONTINUOUS GRANULATION OF CARBOXYMETHYLCELLULOSE |
| DE3843195A1 (en) * | 1988-12-22 | 1990-06-28 | Hoechst Ag | METHOD FOR PRODUCING STORAGE-STABLE, EASILY SOLUBLE BLEACHING ACTIVATOR GRANULES |
| US5488104A (en) * | 1994-06-30 | 1996-01-30 | The Dow Chemical Company | Process for comminuting cellulose ethers |
| DE19637082A1 (en) * | 1996-09-12 | 1998-03-19 | Boehringer Mannheim Gmbh | Rapidly disintegrating pellets |
| DE19909230A1 (en) * | 1999-03-03 | 2000-09-07 | Wolff Walsrode Ag | Process for the production of compressed free-flowing paint raw materials |
| DE10009409A1 (en) * | 2000-02-28 | 2001-08-30 | Wolff Walsrode Ag | Process for the preparation of powdery water-soluble cellulose derivatives |
-
2005
- 2005-02-03 DE DE102005004893A patent/DE102005004893B4/en not_active Revoked
-
2006
- 2006-01-21 BR BRPI0605928-7A patent/BRPI0605928A2/en not_active IP Right Cessation
- 2006-01-21 JP JP2007553497A patent/JP2008528773A/en active Pending
- 2006-01-21 WO PCT/EP2006/000528 patent/WO2006081955A1/en active Application Filing
- 2006-01-21 CN CN2006800010257A patent/CN101039961B/en not_active Expired - Fee Related
- 2006-01-21 KR KR1020077009371A patent/KR20070101236A/en not_active Ceased
- 2006-01-21 EP EP06703567A patent/EP1846456A1/en not_active Withdrawn
- 2006-01-30 US US11/342,992 patent/US20060205935A1/en not_active Abandoned
Non-Patent Citations (1)
| Title |
|---|
| See references of WO2006081955A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| US20060205935A1 (en) | 2006-09-14 |
| JP2008528773A (en) | 2008-07-31 |
| DE102005004893B4 (en) | 2011-02-10 |
| BRPI0605928A2 (en) | 2009-05-26 |
| DE102005004893A1 (en) | 2006-08-10 |
| WO2006081955A1 (en) | 2006-08-10 |
| CN101039961A (en) | 2007-09-19 |
| KR20070101236A (en) | 2007-10-16 |
| CN101039961B (en) | 2010-08-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| 17P | Request for examination filed |
Effective date: 20070903 |
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| AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC NL PL PT RO SE SI SK TR |
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| R17P | Request for examination filed (corrected) |
Effective date: 20070903 |
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| RBV | Designated contracting states (corrected) |
Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC NL PL PT RO SE SI SK TR |
|
| RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: DOW WOLFF CELLULOSICS GMBH |
|
| DAX | Request for extension of the european patent (deleted) | ||
| RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: DOW GLOBAL TECHNOLOGIES INC. |
|
| 17Q | First examination report despatched |
Effective date: 20090916 |
|
| RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: DOW GLOBAL TECHNOLOGIES LLC |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 20130801 |