US2602739A - Sizing compositions and their preparation and use in paper - Google Patents

Sizing compositions and their preparation and use in paper Download PDF

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Publication number
US2602739A
US2602739A US764241A US76424147A US2602739A US 2602739 A US2602739 A US 2602739A US 764241 A US764241 A US 764241A US 76424147 A US76424147 A US 76424147A US 2602739 A US2602739 A US 2602739A
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United States
Prior art keywords
paper
parts
water
extract
weight
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US764241A
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English (en)
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Tadema Harco Jacob
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Shell Development Co
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Shell Development Co
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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/04—Hydrocarbons
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating 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
    • D06M15/17—Natural resins, resinous alcohols, resinous acids, or derivatives thereof
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20—Macromolecular organic compounds
    • D21H17/33—Synthetic macromolecular compounds
    • D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H17/35—Polyalkenes, e.g. polystyrene
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/60—Waxes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP 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
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/62—Rosin; Derivatives thereof

Definitions

  • compositions have been used; for the sizing'of .fibrousmaterials' ofdifierent types. Rosin or'colophony, for .exampleyiscommonly employed for paper sizingbut man'yother resins-waxes, bituminous. or' asphaltic materials, tars,- etc. have been-proposedfor such use.
  • the usual practice is tozapply an aqueoussolution or suspension .offthe sizirigagentato thefibers. to be sized-and precipitate the size-in the fibers by:
  • compositions comprise aqueous emulsions containing. -controlled proportions of colophony with the predominantly cyclic extracts obtainable rom m n al-1.01 artie ilar1 p t m. s- FOr best-resultsitis desirable not only toregulate.
  • the proportion of colophony to I cyclic extract in I the mixture but alsoto control the character of the .emulsion, particularly with respect to fine ness ofthe dispersion.
  • L 4 Accordingto ;the invention, improved; sizing compositions are produced by. emulsifying together with water? to about 30 parts byweightof, coloph'o ny; withl'95 to 70 parts by weight .of. the chosen cyclicextract, preferably 10 to tainable by ⁇ extracting petroleum or related oils, including hydrogenation products of coal and the like, with solvents, which are selective for nonparaffinic constituents.
  • polar solvents may be used for the preparation of such extracts, liquid .sulfurdioxide, phenol, cresylic acid, furfural, beta,betadichlorethyl ether, nitrobenzene the sulfolanes and sulfolenes, and the like beingtypical examples of suitable solvents.
  • Extracts of heavier petroleum oils such as the lubricating oils and residual stocks are especially usefulin thenew sizing compositions of the inpart'sof Icolophony wi h 90 to 80 partsof the ex;
  • l'Thecyclicextracts used in thenew compositionsflof the invention arethe products of predominantly aromatic and naphthenic nature obvention, but other fractions of petroleum or re';
  • lated hydrocarbon products can also be used successfully as sources of the extracts The extracts.
  • lubricantdistillates or bright oils or cylinder stocks which may, for instance, range in gravity from 15.to 8 API at F. They maybe obtained from any mixed type petroleum oil such as Mid-Continent or Coastal or California crudes or, in lower yields, from Pennsylvania type oils.
  • extracts boiling above 300; C. at 760 mm. Hg pressure'are preferred, and-most preferably extracts'boiling from about C. to 300 C. at 1 mm. Hg pressure are used. Extracts obtained from narrow fractions as described in U. S. Patent No. 2,115,960 may be advantageously employed. It is often sizing judged by permeability to water of sized,
  • the melting point of the mixture preferably a temperature between the melting point and about 10 C. higher is used. If-the temperature is too low the emulsification isfunfavorably affected due to insuflicient saponification of the rosin,
  • the transition point for the change in the type of emulsion generally is at about 40% to about 50% water in theemulsion.
  • Y I i As previously pointed out, at least 5%, and more preferably at least by weight of rosin based on the total amount of rosin and extract used should be employed, and the quantity of alkali 'should'be from about one-half to about twicethat required for saponifying the resinic acids present in the colophony, the alkali being supplied in the form of an aqueous solution of about 5% to about concentration, most preferably about 8% to'15% concentration It is advantageouswherehighly stable emulsions are desirable to use not more than the equivalent amount of alkalifor saponifying the rosin, most preferably about 90% to 100% of the equivalent amount. I
  • the most favorable results are obtained when the melted mixture of colophony and extract is vigorously stirred during the addition of the caustic solution.
  • the-particle size of the emulsion was inversely proportional to the rate of stirring in the. first stage of emulsification.
  • the rate'of stirring has little influence in the second emulsification stage, very good oil-in-w'ater type emulsion being obtained in some cases on simply pouring the initial water-in-oil paste into water.
  • the addition of the caustic in the first stage is preferably slow and gradual. The further dilution withwater may be carried out relatively rapidly.
  • temperature may be allowed to fall to about 40 C. at completion of the alkali addition and then may be reduced further by subsequent dilution.
  • the initially'formed water-in-oil type emulsion is particularly suitable for shipment and storage, and'maybeused with or without dilution for v the gluing together of fibers of imitation leather.
  • sizing of paper or cardboard it may be added directly to the fiber pulp in the Holland beater where it is dilutedand converted to an oil-in-water type emulsion.
  • The" diluted emulsion is also preferable'for treating textile threads and'fabrics to make them water-repellent.
  • the initially formed water-in-oil type of emulsions are usually 'dark' brown 'in color but dilution'to produce the oil-in-water type converts them to emulsions which are yellowish green by incident light' and reddish by transmitted light. Lighter colored sizes may-be obtained by suitable decolorization of the extract before emulsification; I
  • the Iproducts of. the invention can be ,used in much more concentrated form.
  • the manufacture of paper and cardboard they may be employed.asi20% to 50%"emulsions of the oil-'in-water type .quite successfully, and when so used, hydrationof the pulp is promoted making possible short'er'time's in'th'e beaters, but lower concentrations can also be employed.
  • the new sizes of 'the invention may be used without any other change in the paper-making process. They may-be precipitated on the fiber with aluminum sulfate or thelike. AjpH of about 4.5 -to 6, depending on the type of pulp, is desirable during precipitation; -If necessary, the pH may be controlled by adding dilute acid in the beater. About 2 5 1 grams of aluminum sulfate-perkilogram of dry stuif in the beater gives satisfactory precipitation. Too much alu minum in the paper should be avoided as it adversely affects the permeability to water.
  • Ijh e emulsi ons of rosin andlubricating oil extractprepared according to the invention are highly stable.
  • ,no flocculation was produced in a 0.04% emulsion with a particle size of 0.12 micron on addition of hydrogen chlorideto 1/40 normal or of aluminum sulfate to 1/80 normal.
  • the base in this emulsion had a normality of only 0.00013, so a hundred-fold excess of the acid or "aluminum sulfate did not result in'coagulation; However, in the presence of sulfite pulp a five-fold quantity. of aluminum sulfate calculated on the base present was sufficient for'complete precipitation.
  • the emulsions do not readily coagulate, they occaemulsions are prepared at a pH below 9.5, preferably at aboutii to. 9, and if the initial emulsion is too alkaline it can be given" the desired pH by adding aweak acid. Addition of small amounts of protective: colloids,' such' ascasein and gums, may be used to ensure the unlimited stability of the new emulsions. 1
  • a water-permeability test showed that the water had permeatedthe paper after 15 seconds.
  • the distillation residue of the same extract (the higher boiling 24%)- required only 0.63% size for normal sizing.
  • the %-75% fraction ofthe'di-stillation required 1. 50% for normalsiz ing andgave 'avery light colored-"size.
  • Example IV I Incomparative tests of sizing Kraft pulp with emulsions. prepared on the'one hand from colo-' phony alone and onthe other hand froma mixe turiefof. 20 parts of .fc'olophony and-80. partsof the gasoline extract ofan Edeleanu extract of 111-. bricating oil using the. emulsification method. of
  • Example I'I the permeability of papers contain? ing 3% size was as follows: w
  • a water-in-oil emulsion was obtained which, after being cooled to 40 C., was mixed while stirring with such an amount of water of normal temperature as to produce a 40% oil-in-water emulsion.
  • the emulsion thus obtained in spite of its high concentration, was still thinly liquid and had a green color with incident light.
  • the aver- I age particle size amounted to 68 millimicrons.
  • a Kraft-cellulose paper was manufactured
  • 2,41'01357 may be'used along with the new sizes of the inVentionQAlso; other acid-acting rtecipitating agents may .be used. instead iof. aluminum sulfate for sizing according to the inven'- tion. Still other variations are possible in the invention which is not intended to be limited to the specific procedures shown by way of exam-, ple, nor by any theory proposed in explanation of theimproved results which are obtained.
  • A- paper sizing composition consisting essentially of an aqueous emulsion having a pH of 8 a to 9 of 10 to 20,parts of colophony saponified to the extent of about to and 90 to 80 parts of an Edeleanu extract of higher boiling petroleumhydrocarbons I wherein. the .particles have anaverage sizeof less thanl micron.
  • An aqueous emulsionof the oil-in-water' typ'e suitable for sizing fibrous materials which comprises a stable dispersion in water of to 30 parts by weight of substantially'saponified colophony and 9'5 to 70 parts by weight of an extract of petroleum consisting largely of naphthenic and aromatic hydrocarbons, the water content of the mixture being at least 60% based upon the total weight of said dispersed components and wate v 3.- ,,An-emulsion oi the water-in-oiltype con sisting essentially of water and a mixture of 10 to -parts by weight of colophony, at least half of which is saponified, and 90 to 80 parts-by weightof a hydrocarbon mixture having a boiling point above"300 C.
  • a process of sizing cellulose fibers which comprises intimately contacting an aqueous slurry of the fibers with an aqueous dispersion of a mixture of 5 to parts by weight of cold-j phonyand 95 to 70 parts of an extract of petroe leum consisting largely of naphthenic and aro-. matic hydrocarbons, which mixture has been emulsified with sufiicient of an alkali solution oi 5% to 30% concentration to saponifyat least half of said colophony, and precipitating said dispersed mixture from an emulsion of the oilin-water type onto said fibers with an acid-acting compound.
  • a paper product comprising cellulose. fibers sized with a mixture of 10 to 20 parts of 0010- phony by weight and 90 to 80 parts by weight of a raflinate from extraction with gasoline of, an E'deleanu extract of lubricating oil.
  • theim-v provement which comprises precipitating onto the fibers suspendedparticles of about 0.1 micron diameter from an emulsion of the oil-in 'w'ater type of 5 to 30 parts by weight of colophony,-and 95 to parts by weight of the hydrocarbon extract of high boiling'petroleum hydrocarbons, whichextract is soluble in a solvent having a preferential solubility for aromatic hydrocarbons inthe presence of paraffins, whichemulsion con; tainsat least 60% of water based upon the total weight of colophony, hydrocarbon extract and water and is formed by reacting said colophony and hydrocarbon extract with a 5% to 30% aqueous solution of an inorganicbase selected from the groupconsisting of the hydroxides, carbonates, and bicarbonates of the alkali metals and of ammonia, andthe hydroxides of calcium and magnesium; HARCO JACOB REFERENCES

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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US764241A 1943-04-14 1947-07-28 Sizing compositions and their preparation and use in paper Expired - Lifetime US2602739A (en)

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DE (1) DE870462C (de)
FR (1) FR902441A (de)
NL (1) NL59736C (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2705205A (en) * 1951-08-23 1955-03-29 Shell Dev Sizing compositions and method of using the same
US2954313A (en) * 1955-10-17 1960-09-27 Kerr Mc Gee Oil Ind Inc Sizing fibrous cellulosic materials
FR2335643A1 (fr) * 1975-12-19 1977-07-15 Bayer Ag Emulsions d'isocyanates d'acides resiniques en tant qu'agents d'appretage pour papier

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2837439A (en) * 1953-10-27 1958-06-03 Sinclair Refining Co Paper size
US7476809B2 (en) 2005-03-28 2009-01-13 Rockbestos Surprenant Cable Corp. Method and apparatus for a sensor wire

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US568518A (en) * 1896-09-29 Process of manufacturing fiber-ware
US1806474A (en) * 1928-06-08 1931-05-19 Lecocq Ernest Process for sizing paper
US1833038A (en) * 1922-10-17 1931-11-24 Dispersions Process Inc Process of producing aqueous dispersions of water immiscible bodies
US1943975A (en) * 1930-11-06 1934-01-16 Celotex Company Water repellent size for fiber products
US2068299A (en) * 1931-06-24 1937-01-19 Nathaniel L Foster Paper article and method of making same
US2117256A (en) * 1933-11-18 1938-05-10 Raffold Process Corp Paper manufacture
US2285028A (en) * 1940-09-16 1942-06-02 Hercules Powder Co Ltd Rosin size emulsion
US2301298A (en) * 1940-11-28 1942-11-10 American Cyanamid Co Rosin size composition and method of preparing same
US2383933A (en) * 1942-12-10 1945-09-04 Monsanto Chemicals Preparation of resinous dispersions
US2415408A (en) * 1941-08-18 1947-02-11 Bergier Jacques Sizing and dressing means

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US568518A (en) * 1896-09-29 Process of manufacturing fiber-ware
US1833038A (en) * 1922-10-17 1931-11-24 Dispersions Process Inc Process of producing aqueous dispersions of water immiscible bodies
US1806474A (en) * 1928-06-08 1931-05-19 Lecocq Ernest Process for sizing paper
US1943975A (en) * 1930-11-06 1934-01-16 Celotex Company Water repellent size for fiber products
US2068299A (en) * 1931-06-24 1937-01-19 Nathaniel L Foster Paper article and method of making same
US2117256A (en) * 1933-11-18 1938-05-10 Raffold Process Corp Paper manufacture
US2285028A (en) * 1940-09-16 1942-06-02 Hercules Powder Co Ltd Rosin size emulsion
US2301298A (en) * 1940-11-28 1942-11-10 American Cyanamid Co Rosin size composition and method of preparing same
US2415408A (en) * 1941-08-18 1947-02-11 Bergier Jacques Sizing and dressing means
US2383933A (en) * 1942-12-10 1945-09-04 Monsanto Chemicals Preparation of resinous dispersions

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2705205A (en) * 1951-08-23 1955-03-29 Shell Dev Sizing compositions and method of using the same
US2954313A (en) * 1955-10-17 1960-09-27 Kerr Mc Gee Oil Ind Inc Sizing fibrous cellulosic materials
FR2335643A1 (fr) * 1975-12-19 1977-07-15 Bayer Ag Emulsions d'isocyanates d'acides resiniques en tant qu'agents d'appretage pour papier

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Publication number Publication date
FR902441A (fr) 1945-08-30
DE870462C (de) 1953-03-12
NL59736C (de)

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