DE1470825A1 - Process for the production of micro-cellulose crystallite aggregates - Google Patents

Process for the production of micro-cellulose crystallite aggregates

Info

Publication number
DE1470825A1
DE1470825A1 DE19641470825 DE1470825A DE1470825A1 DE 1470825 A1 DE1470825 A1 DE 1470825A1 DE 19641470825 DE19641470825 DE 19641470825 DE 1470825 A DE1470825 A DE 1470825A DE 1470825 A1 DE1470825 A1 DE 1470825A1
Authority
DE
Germany
Prior art keywords
cellulose
crystallite aggregates
micro
production
cellulose crystallite
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.)
Pending
Application number
DE19641470825
Other languages
German (de)
Inventor
Battista Orlando A
Smith Patricia A
Herald Carl R
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
FMC Corp
Original Assignee
FMC Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from US10072A external-priority patent/US3157518A/en
Application filed by FMC Corp filed Critical FMC Corp
Publication of DE1470825A1 publication Critical patent/DE1470825A1/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/018Dielectrics
    • H01G4/06Solid dielectrics
    • H01G4/14Organic dielectrics
    • H01G4/16Organic dielectrics of fibrous material, e.g. paper
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P20/00Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10Coating with edible coatings, e.g. with oils or fats
    • A23P20/105Coating with compositions containing vegetable or microbial fermentation gums, e.g. cellulose or derivatives; Coating with edible polymers, e.g. polyvinyalcohol
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P20/00Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/19Coating with non-edible coatings
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/02Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/08Fractionation of cellulose, e.g. separation of cellulose crystallites
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/02Cellulose; Modified cellulose
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/05Cellulose or derivatives thereof
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/10Coatings without pigments
    • D21H19/14Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • D21H19/34Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising cellulose or derivatives thereof

Description

Dr E Wetzel «οονοπ·««!. —19.sept.1968Dr E Wetzel «οονοπ ·« «!. -19 September 1968

LJt LJt m L·.. »»OlAUI Hetnereplatz3 Telefon0911/204081-83 m L · .. »» OlAUI Hetnereplatz3 Telephone 0911 / 204081-83

-^. . . r- T* _ Tel·* 08/22327 Telegramm· Patweto·! - ^. . . r- T * _ Tel * 08/22327 Telegram Patweto!

Dipl.-lng. E. Tergau U 7 O 8 2 5 °—-» ■- **·. ^- 3ββ«οDipl.-Ing. E. Tergau U 7 O 8 2 5 ° --- »■ - ** ·. ^ - 3ββ «ο

Stadteparkaiee Nürnberg 63835 Stadteparkaiee Nuremberg 63835

Patentanwälte potitch*eiiiioni0 Nürnb#rg 111β1 Patent attorneys potitch * eiiiioni0 Nürnb # rg 111β1

- unter Zeichen blue Immer engeben — - Always enter under the sign blue -

25/33 25/33

70 825.9 "70 825.9 "

PMC Corporation.Philadelphia.Pa/ USAPMC Corporation, Philadelphia, Pa / USA

Verfahren zur Gewinnung von Mikro-Cellulose-Krlstallit-AggregatenProcess for the production of micro-cellulose crystallite aggregates

Die Erfindung betrifft ein Verfahren zur Gewinnung von faserfreien Mikro-Cellulose-Kristalllt-Aggregaten in Pulverform aus Cellulose-Kristallit-Aggregaten. Zur epraohliohen Vereinfachung werden in den folgenden Ausführungen die Worte Cellulose-Kristallit-Aggregate duroh CKA und Mikro-Cellulose-Kristallit-Aggregate durch MCKA abgekürzt.The invention relates to a method for obtaining fiber-free micro-cellulose crystallite aggregates in powder form from cellulose crystallite aggregates. For the sake of simplicity, the following Execution the words cellulose crystallite aggregate duroh CKA and micro-cellulose crystallite aggregates by MCKA abbreviated.

Die Gewinnung von faserfreien CKA und MCKA kann als bekannt vorausgesetzt werden (franz.Patentschrift 1 194 486 und die hierin angegebenen Literaturstellen). Grundlage der Gewinnung der CKA ist die Behandlung von nativer oder regenerierter Cellulose duroh saure Hydrolyse unter Bedingungen, die zu einem im wesentlichen einheitlichen durchschnittlichen Polymerisationsgrad führen. Es werden hierbei die faserigen, amorphen Bestandteile herausgelöst. Die so erhaltene Cellulose liegt in Form von CKA vor, die duroh Waschen im wässerigen Medium von der Säure befreit werden. Um MCKA zu erhalten, werden die CKA mit oder ohne vorherige Trooknung in einem wässerigen Medium zerkleinert (vgl, auoh DAS 1 123 460 entsprechend Anmeldung A 28 768 ),The production of fiber-free CKA and MCKA can be assumed to be known (French patent specification 1 194 486 and the references cited herein). The basis for obtaining the CKA is the treatment of native or regenerated Cellulose duroh acid hydrolysis under conditions which lead to a substantially uniform average degree of polymerization. The fibrous, amorphous components dissolved out. The cellulose obtained in this way is in the form of CKA, which can be washed in water Medium to be freed from the acid. To get MCKA, the CKA are comminuted with or without prior drying in an aqueous medium (cf. also DAS 1 123 460 according to application A 28 768),

909813/1371909813/1371

(Art.) s ι ζ$$^Λ'ν*"^ llV.-f'i{'#!/!fÜS'ul'1'' * 4" J' (Art. ) S ι ζ $$ ^ Λ'ν * "^ ll V.-f'i {'#! / ! FÜS' ul ' 1 ''* 4 " J '

U70Q25U70Q25

Han kann jetzt den Feststoffanteil Im wässerigen Medium erhöhen und die Dispersion In ein Gel überführen. Mit steigendem Peststoffgehalt erhält man eine pastenartige Masse und schließlich eine Masse, die dem Gefühl nach trocken, jedoch nicht trocken im eigentlichen Sinn ist, da sie ja noch einen bestimmten Anteil des Dispersionsmittels enthält.Han can now increase the solids content in the aqueous medium and transfer the dispersion into a gel. With increasing pesticide content, a paste-like mass is obtained and Finally, a mass that feels dry, but not dry in the real sense, since it still has something else Contains a certain proportion of the dispersant.

Die Erfindung beschäftigt sich mit der Aufgabe, MCKA in einer Form zu erhalten, in der sie nicht nur trocken erscheinen, sondern tatsächlich ein trockenes Pulver sind. Der Bedarf nach einem solchen trockenen Pulver besteht insbesondere für die Verwendung in der Nahrungs- und Genußmittelindustrie als Füllmittel, da Cellulose vom menschlichen Körper nicht aufgenommen wird und infolgedessen nicht dick macht. Es hat sich nämlich gezeigt, daß die nur trocken erscheinende MCKA nur schwer hinreichend homogen in die Masse des Nahrungs- oder Genußmittels eingebracht werden können, so daß, wie gesagt, die Aufgabe entstand, die MCKA als tatsächlich trockenes Pulver zu erhalten. Man hätte an sich von getrocknetem CKA ausgehen und diese mechanisch zerkleinern können. Aber eine derartige Mikro-Mahlanlage ist teuer; der Mahlvorgang würde eine verhältnismäßig lange Zeit in Anspruch nehmen. Die Erfindung geht deshalb einen anderen Weg, nämlich den, den Zerkleinerungsvorgang zwar wie bisher in ein wässeriges Medium zu verlegen, aber dann anschließend die so gebildeten MCKA duroh Gefriertrocknung aus dem wässerigen Medium abzutrennen. Das angestrebte trockene Pulver wird also in zweiThe invention is concerned with the task of MCKA in a To obtain form in which they not only appear dry, but are actually a dry powder. The need after such a dry powder exists in particular for use in the food and beverage industry as Bulking agent, as cellulose is not absorbed by the human body and, as a result, does not make you fat. It has namely shown that the only dry appearing MCKA is difficult to integrate sufficiently homogeneously into the mass of the food or Stimulants can be introduced, so that, as I said, the task arose, the MCKA as an actually dry powder to obtain. One could have started from dried CKA and mechanically crushed it. But one such micro-grinding equipment is expensive; the grinding process would take a relatively long time. The invention therefore takes a different approach, namely, the comminution process, as before, in an aqueous one Medium to be laid, but then subsequently to separate the MCKA formed in this way duroh freeze-drying from the aqueous medium. So the desired dry powder is divided into two

909813/13 7 1909813/13 7 1

U70R25U70R25

Schritten gewonnen, in einem ersten Schritt, in dem die CKA im wässerigen Medium zu MCKA zerkleinert werden, und einem zweiten Schritt, in dem diese MCKA durch Gefriertrocknung aus dem wässerigen Medium in Pulverform abgeschieden werden·Steps gained, in a first step in which the CKA are comminuted in the aqueous medium to MCKA, and a second step in which these MCKA are separated from the aqueous medium in powder form by freeze-drying.

Es hat sich gezeigt, daß auf diese Weise mit geringem Mahl- und Zeitaufwand ein Pulver mit einem sehr geringen Schüttgewicht, etwa 0,157 g/ocm gewonnen werden kann, das weich und porös ist und ein angenehmes Mundgefühl erzeugt. Jedoch ist das Gebiet der Nahrungs- und Genuamittel nicht das einzige Anwendungsgebiet des Pulvers. Es gibt eine Reihe anderer Fälle, in denen Bedarf nach einem trocknen Pulver aus MCKA besteht. Dieses Pulver ist ein in der Cellulose-Technik neuartiges und wertvolles Produkt.It has been shown that in this way with little grinding and expenditure of time a powder with a very low bulk density, about 0.157 g / ocm, which is soft and is porous and creates a pleasant mouthfeel. However, the field of food and genetics is not the only one Application area of the powder. There are a number of other cases when there is a need for a dry powder of MCKA. This powder is a new and valuable product in cellulose technology.

909813/13 7909813/13 7

Claims (1)

U70825U70825 PatentanspruchClaim Verfahren zur Gewinnung von faserfreien Mikro-Cellulose-Kristallit-Aggregaten in Pulverform aus Cellulose-Kristallit-Aggregaten, die durch saure Hydrolyse von Cellulose unter Bedingungen gewonnen sind, die zu einem im wesentlichen einheitlichen Polymerisationsgrad führen, die nach der Hydrolyse durch Auswaschen von der Säure befreit und die anschließend in einem wässerigen Medium derafct zerkleinert sind, daß mindestens 1 % der Kristallit-Aggregate eine Teilchengröße von unter 1 μ aufweist, dadurch gekennzeichnet, daß die so gebildete Mikro-Cellulose-Kristallit-Aggregate durch ( an sich bekannte ). Gefriertrocknung als Pulver aus dem wässerigen Medium abgetrennt werden.Process for the production of fiber-free micro-cellulose crystallite aggregates in powder form from cellulose crystallite aggregates which are obtained by acid hydrolysis of cellulose under conditions which lead to an essentially uniform degree of polymerization which, after hydrolysis, is washed out by the acid are freed and then comminuted derafct in an aqueous medium, that at least 1% of the crystallite aggregates having a particle size of less than 1 μ, characterized in that the thus formed micro-cellulose crystallite aggregates by (known per se). Freeze drying can be separated as a powder from the aqueous medium. 909813/137909813/137
DE19641470825 1960-02-19 1964-09-03 Process for the production of micro-cellulose crystallite aggregates Pending DE1470825A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US969160A 1960-02-19 1960-02-19
US10072A US3157518A (en) 1960-02-23 1960-02-23 Coatings of cellulose crystallite aggregates
US3394160A 1960-06-06 1960-06-06

Publications (1)

Publication Number Publication Date
DE1470825A1 true DE1470825A1 (en) 1969-03-27

Family

ID=27358905

Family Applications (3)

Application Number Title Priority Date Filing Date
DE1960A0036064 Pending DE1567322B1 (en) 1960-02-19 1960-11-10 Process for making a moist stable comminuted cellulose
DE19641470825 Pending DE1470825A1 (en) 1960-02-19 1964-09-03 Process for the production of micro-cellulose crystallite aggregates
DE19641470824 Pending DE1470824A1 (en) 1960-02-19 1964-09-03 Process for the production of aqueous dispersions of crystalline cellulose

Family Applications Before (1)

Application Number Title Priority Date Filing Date
DE1960A0036064 Pending DE1567322B1 (en) 1960-02-19 1960-11-10 Process for making a moist stable comminuted cellulose

Family Applications After (1)

Application Number Title Priority Date Filing Date
DE19641470824 Pending DE1470824A1 (en) 1960-02-19 1964-09-03 Process for the production of aqueous dispersions of crystalline cellulose

Country Status (3)

Country Link
CH (1) CH395045A (en)
DE (3) DE1567322B1 (en)
GB (1) GB970111A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4474949A (en) * 1983-05-06 1984-10-02 Personal Products Company Freeze dried microfibrilar cellulose

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE564287A (en) * 1957-01-28

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4474949A (en) * 1983-05-06 1984-10-02 Personal Products Company Freeze dried microfibrilar cellulose

Also Published As

Publication number Publication date
DE1567322B1 (en) 1971-07-15
GB970111A (en) 1964-09-16
CH395045A (en) 1965-07-15
DE1470824A1 (en) 1969-03-27

Similar Documents

Publication Publication Date Title
DE1470825A1 (en) Process for the production of micro-cellulose crystallite aggregates
DE1470825C (en) Process for the production of fiber-free micro-cellulose crystallite aggregates in powder form
DE475114C (en) Process for making a dentifrice
DE1470825B (en) Process for the production of fiber-free micro cellulose crystallite aggregates in powder form
DE1692587A1 (en) Process for the treatment of plant tissues, or. Fabrics
DE815602C (en) Process for the treatment of cellulose-containing substances by means of ultrasonic waves, in particular for the production of paper pulp
Tarnóczy The speech-chorus method
DE702218C (en) Process for the decomposition of wet grains
DE535369C (en) Coatings made from dissolved cellulose esters for the dolls of electrical elements
AT144812B (en) Process for the production of easily disintegrating tablets.
DE835588C (en) Process for the production of yeast extract as a starting product for yeast components
DE601590C (en) Process for the production of a preparation intended for hemostatic purposes
DE747802C (en) Process for the production of solid spreadable agents for the preservation of green fodder
DE743246C (en) Means for producing practically unchangeable changes in the shape of the hair
DE124234C (en)
DE820950C (en) Process for extracting the ingredients of plant material
DE631954C (en) Process for obtaining long-life flour from the germs of plant seeds
DE949238C (en) Process for the transfer of urea solutions into solid, hard, uniform and storage-stable spheres
AT10113B (en) Process for converting raw, green or dried plant fibers (ramie, Chinese grass, etc.) into spinnable fibers.
DE885988C (en) Process for refining cellulose hydrate textiles
DE428004C (en) Process for the production of an adhesive
DE708741C (en) Process for the production of particulate filter media
DE1567322C (en) Process for producing a moist stable comminuted cellulose
DE742702C (en) Process for the production of dry pectin
DE916108C (en) Process for obtaining highly effective adrenal extracts

Legal Events

Date Code Title Description
E77 Valid patent as to the heymanns-index 1977