US3794558A - Loading of paper furnishes with gelatinizable material - Google Patents

Loading of paper furnishes with gelatinizable material Download PDF

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US3794558A
US3794558A US00834790A US3794558DA US3794558A US 3794558 A US3794558 A US 3794558A US 00834790 A US00834790 A US 00834790A US 3794558D A US3794558D A US 3794558DA US 3794558 A US3794558 A US 3794558A
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pulp
starch
paper
refiner
refining
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S Back
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James River Corp of Nevada
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Crown Zellerbach Corp
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    • 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
    • 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
    • D21H17/24—Polysaccharides
    • D21H17/28—Starch
    • D21H17/29—Starch cationic

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  • Certain properties of paper products such as strength, internal bond, holdout, etc. are enhanced by the loading of the pulps from which they are prepared with a gelatinizable material such as starch.
  • a gelatinizable material such as starch.
  • One method in which such material is introduced into a pulp is by adding the material to the pulp as a cooked dispersion, i.e., a dispersion of the material where such has been heated above the gelatinization temperature of the material whereby the material has been converted into a gel.
  • the cooked material and the cellulosic fibers in the pulp are then intimately mixed, and the furnish produced is directed to a paper machine for conversion into paper.
  • an object of this invention is to provide an improved process for incorporating a gelatinizable material with a cellulosic pulp, which has been found to produce dramatic improvements in both the way that the pulp may be handled during its conversion into paper, and the physical characteristics obtainable in paper by reason of the inclusion of the material.
  • Another more specific object of the invention is to provide a process for preparing a paper-making pulp or furnish, which permits a far higher loading of the pulp with gelatinizable material to be attained without the difliculties normally associated with such loading.
  • Another object of the invention is to provide an improved pulp and process for preparing it, where such is loaded with a gelatinizable material, and such material contributes more etiectively to desirable properties in the final paper product.
  • Yet another object is to provide novel and improved paper products exhibiting exceptional properties such as strength, improved internal bond, holding endurance, toughness, etc., and to provide novel special type papers such as grease-proof papers, offset printing papers, etc., of a superior type.
  • the improved strength characteristics obtainable following the invention are particularly important with papers loaded with fillers, where properties such as internal bond customarily are deleteriously affected by such fillers.
  • Yet another object of the invention is to provide a novel process for preparing pulp and paper therefrom, which makes possible greater efiiciency in the retention of fillers and fines incorporated with the pulp.
  • a cellulosic fiber is formed of many layers of fibrils bound together and surrounded by an outer lignin lamella.
  • defibering In the production of paper, it is common to separate the cellulosic fibers in wood chips or other fiber agglomerates, either mechanically or chemically, and this physical separation of the fibers is known as defibering.
  • Defibered pulp i.e., a pulp made up of separated fibers may be further refined to produce freeing of the fibrils in the fiber, in a refining process which is known as fibrillation.
  • fibrillation In a fibrillated pulp, the fibrils in a fiber are loosened or partially freed, whereby they project as hairlike strands from the fiber body in which they originally were tightly bound.
  • fibrillation processes including fibrillation carried out at relatively low consistencies, where the pulp which includes the fibers contains sufiicient water to constitute a pumpable and flowable material, as well as fibrillation at relatively high consistencies, where the pulp generally is of a nonfluid or semisolid nature and of a nonpumpable character.
  • a gelatinizable material such as starch
  • water and subsequently cooked i.e., raised in temperature above the gelatinization temperature of the starch
  • swells and becomes converted into a gel with molecular chains in a starch particle becoming loosened, thence to extend in disassociated expanses in the water in which the starch is dispersed.
  • the starch is cooked before its introduction into the pulp
  • the material is introduced to the pulp as a gel, and any association which takes place between the starch with the fibers in the pulp is one which is attained through mixing of the already gelatinized material with the pulp fibers.
  • This invention is based on the discovery that unexpected results are obtained if the gelatinizable material is incorporated with the defibered pulp in a substantially uncooked condition, i.e., in a substantially nongelatinized state, and if this addition of the gelatinizable material is made prior to or simultaneously with the introduction of the pulp to a refiner producing fibrillation of the fibers in the pulp. Further, it is important according to this invention that the conditions be such that during the refining to produce fibrillation there is simultaneous cooking of the gelatinizable material whereby it converts into its gelatinized state. Under these conditions, the gelatinizable material swells into a gel simultaneously with loosening of the fiber fibrils, and apparently far greater sorption between the material and the fibers results.
  • high consistency refining techniques are particularly appropriate.
  • fibrillation is performed on pulp which is of a semisolid or nonflowable nature (the usual high consistency pulp has a consistency, i.e., a percent by weight of fiber on a dry basis, of or more), and fibril loosening is the result of interfiber friction produced by fibers rubbing against each other.
  • Temperatures are produced as a result of such fiber friction which are above the gelatinization or cooking temperature of the starch (about 150 F.), such temperatures normally ranging from about 170 F. to well above boiling temperature (temperatures as high as 260 F. have been observed).
  • the temperature condition needed to produce cooking is produced automatically and without the need of external heating.
  • a paper product may be produced that provides an excellent substrate for grease proofing.
  • new and improved grease-proof papers are possible.
  • Papers of exceptional strength can be produced, with a starch loading substantially exceeding that normally practiced in the past.
  • properties may be introduced into paper, such as stiffness, that make the paper available for special uses, such as for tab cards, etc.
  • the gelatinizable materials that may be utilized according to this invention include both the natural starches and starches that constitute derivatives of such natural starches, such as the so-called cationic starches of the type discussed in US. Pat. 2,813,093.
  • cationic starches of the type discussed in US. Pat. 2,813,093.
  • Starch comprises essentially amylopectin and amylose, the various types of starches being a major part amylose or amylopectin, depending upon their origin.
  • Starches high in either amylose or amylopectin are usable with the invention, with those high in amylopectin having certain advantages in that the more highly branched amylopectin starch molecule apparently produces a cross-linking action among the fibrils of the fibers not producible with the more linear amylose molecules.
  • Particle size does not seem to be too critical with respect to the retention obtained in the pulp, particularly when high consistency refining techniques are employed for incorporating the starch, possibly because of the shearing action generated during the fibrillation at high consistency which causes the starch to be broken down. However, as a practical matter, best retention seems most probably to be obtained with a particular size (wet mill-ed) of 30 microns or less.
  • Cellulosic material which is suitable for use as a starting material in accordance with this invention may be derived from any species of coniferous pulpwood, such as spruce, hemlock, fir, pine, and others; deciduous pulpwood, such as poplar, birch, cottonwood, alder, and others; as Well as from fibrous, nonwoody plants suitable for paper-making, such as cereal straws, bagasse, cornstalks, grasses, and the like, and also the usual waste cellulosic sources.
  • coniferous pulpwood such as spruce, hemlock, fir, pine, and others
  • deciduous pulpwood such as poplar, birch, cottonwood, alder, and others
  • fibrous, nonwoody plants suitable for paper-making such as cereal straws, bagasse, cornstalks, grasses, and the like, and also the usual waste cellulosic sources.
  • the pulp When high consistency refining is employed in the fibrillation of the pulp fibers, such is performed with the pulp having a consistency of between 10% and 60%, and preferably between 20% to 45%.
  • the pulp may be metered as by a screw conveyer into the refining apparatus, such as a conventional single-disk refiner, a double-disk refiner, or a conical-type refiner adapted for handling high consistency pulp. All of the above machines have two op posed surfaces which are spaced apart and more relative to one another, defining between them a Working space.
  • the surfaces should operate at a relative tangential velocity of no less than about 1,000 feet per minute and the rotation should be about a fixed axis to obviate relative gyratory movement which results in balling of the fiber.
  • the relative tangential velocity of the surfaces should preferably be at least 5,000 feet per minute, and in the case where both surfaces are moving in opposite directions, relative tangential velocity of at least 15,000 feet per minute is preferred.
  • the velocity should be sufiiciently great for any given spacing between the refining surfaces as to impart suflicient energy to the fibers to effect attrition therebetween and the fibrillation essential by the interfiber friction, and at the same time provide sufiicient energy to move the fibers through the refiner.
  • the two surfaces between which the pulp is treated may be roughened by having a set of ducts, grooves, indentations or other projections of such character as to engage the high consistency pulp.
  • the refining of high consistency pulp in order to effect fibrillation thereof is more fully discussed in US. Pat. 3,382,140.
  • Residence time within the refiner of the pulp being processed will vary somewhat, depending upon operating conditions. Usually, such will be less than about sec onds, with a residence time of from 0.3 to 3 seconds being typical.
  • a double-disk Bauer 411 refiner was used in the refining to effect fibrillation.
  • the plate clearance in the refiner was adjusted to between 0.02 and 0.04 inch.
  • Feed rate of pulp into the refiner was maintained between about three to four tons per hour.
  • EXAMPLE 1 A softwood (Western Hemlock) sulfite pulp, bleached to a brightness of 80% G.E.R.S. (General Electric Recording Spectrophotometer) was dewatered in a Sweco screen and pressed to a consistency of 35% through a Zenith press. Such pulp was then metered into the center or eye of the Bauer 411 refiner, to produce fibrillation of the fibers in the pump. Simultaneously with the feeding of the pulp, a mixed slurry of titanium dioxide pigment and an uncooked cationic cornstarch derivative of high amylose content was injected into the eye of the refiner.
  • G.E.R.S. General Electric Recording Spectrophotometer
  • the slurry of starch and pigment was made in cold water, with a pigment to starch ratio of 10 to 4, and the concentration of slurry solids in the slurry was 25%.
  • the pigment Du Ponts Ti-Pure LW, having an average micron size of 0.4, was first dispersed in water at room temperature, and the uncooked starch then added to the pigment slurry with mixing.
  • the starch utilized was a tertiary amino alkyl starch ether derivative, with a degree of substitution of about 4 amino alkyl groups per 100 anhydroglucose units.
  • the starch contained 70% amylose, and was obtained from National Starch and Chemical Company as National Starch 77-1405.
  • the starch had a particle size of microns.
  • the slurry was fed into the refiner at a rate to obtain a starch addition of about 3.3% based on the oven dry weight of fiber.
  • the power input to the refiner was approximately 5 horsepower day/ dry ton of fiber.
  • the freeness of the pulp was reduced from about 680 to 470 cc. 'CSF (Canadian Standard Freeness).
  • the pulp and slurry was fed into the refiner at approximate room temperature.
  • the residence time of the pulp and slurry, on making a single pass through the refiner, was approximately one second.
  • the temperature of the pulp and slurry was raised within the refiner, by interfiber friction, to approximately 235 F.
  • the pulp mixture or stock immediately on leaving the Bauer refiner was diluted with cold water to a consistency of 3.5%, such dilution lowering the temperature of the stock to 70 F.
  • the stock was then further refined using a conventional Jordan, low consistency refiner, to reduce its freeness to 220 cc. CSF.
  • the stock or furnish was then directed to a paper-making machine for conversion into paper.
  • the paper produced, without any size press treatment, exhibited the following properties:
  • the Scott internal bond property is indicated above as 500+, as the internal bond measured exceeded the measuring calibrations of the testing machine.
  • EXAMPLE 2 Softwood sulfite pulp of the type used in Example 1 was refined to produce fiber fibrillation as in Example 1, with the exception that in this instance, the mixed slurry of titanium dioxide pigment and uncooked starch was not introduced into the Bauer refiner with the pulp. Instead, the pulp was diluted on being discharged from the refiner to a consistency of about 3.5%, and the pigment and starch slurry was then added at this stage. The pulp mixture resulting was then further refined, as in Example 1, to reduce the -freeness of the stock to 200 cc. CSF. The stock or furnish was then fed to a paper machine to be converted into paper.
  • Paper produced from the furnish where the starch was added uncooked was given a starch size press treatment, to upgrade the finished paper, as is usual in the making of a business bond grade paper.
  • a coating composition is applied to both sides of the paper which is then metered off by reason of the paper passing between the nip of opposed rolls.
  • the coating composition used contained about 15% solids, and comprised in addition to water a mixture of parts ethylated starch (Penford Gum 260 by Pennick & Ford), 3 parts carboxylated styrene maleic anhydride resin copolymer (Scripset 500 produced by Monsanto), and 12.5 parts titanium dioxide (Ra42 by National Lead).
  • the composition was applied at a rate to obtain a distribution of solids on the paper of about one pound per 3,000 square feet. Physical propfrties noted in this size press treated paper were as folows:
  • EXAMPLE 3 A blend was prepared comprising 60% softwood sulfite pulp of the type set forth in Example 1 and 40% of a bleached birch kraft, bleached to a brightness of 85% G.E.R.S. This blend was dewatered and pressed to produce a pulp of 37% consistency. To produce fibrillation of the pulp, the pulp was fed into a Bauer refiner at this consistency simultaneously with the feeding into the refiner of a slurry comprising uncooked natural cornstarch (20 microns average particle size) dispersed in cold water, and with a slurry solids of 35%.
  • the pulp was refined with a power input of about 7 horsepower day/ dry ton of fiber.
  • the uncooked cornstarch slurry was fed at a rate to obtain a loading of starch, based on the dry weight of fiber.
  • the temperature of the pulp and starch slurry additive reached approximately 230 F. on making a single pass through the refiner, and the freeness of the stock on leaving the refiner was 385 cc. CSF. Residence time in the refiner was determined to be about 1.5 seconds.
  • Paper was prepared from stock or furnish so produced, and such paper (without any size press treatment) possessed the following physical properties:
  • WMD 1946 CMD 1351 Scott internal bond, ft.-lbs./in. 1000 483 *Cross machine direction.
  • the following example illustrates the use of a starch which is relatively high in amylopectin, in the preparation of a stock or furnish which is free of any pigment addition.
  • EXAMPLE 4 A blend of softwood sulfite pulp and bleached birch kraft, as used in Example 3, was processed as in Example 3 save that the slurry used to load the pulp was an aqueous slurry (30% solids) of a cationic cornstarch derivative containing about 75% amylopectin.
  • the starch was a tertiary amino alkyl starch ether derivative, having an average particle size of less than 20 micron, obtained from the National Starch and Chemical Company as Cato-Kote 1378.
  • the starch slurry was fed into the refiner together with the pulp at a rate to obtain a loading of 4%, based on the dry weight of fiber.
  • Residence time in the refiner was noted to be about 1.5 seconds and the temperature of the stock within the refiner was raised to about 240 F.
  • the Stock On leaving the refiners was diluted with cold water as in Example 3, and further refined at low consistency to obtain a headbox freeness of 200 cc. CSF.
  • EXAMPLE 5 A series of runs were performed to demonstrate the superior pigment retention obtainable when a pulp is loaded with starch and pigment in the manner contemplated by the invention. In these runs, paper products were prepared from various types of furnishes.
  • Furnishes were prepared from various pulp mixtures by injecting them into a Bauer refiner concurrently with continuously feeding into the refiner a mixed slurry of uncooked starch (of the type set forth in Example 1) and pigment, with the pigment to starch ratio in said slurry being 10 to 4.
  • the consistency of the pulp entering the refiner was approximately 35% and the pulp feed rate was approximately 3.4 tons per hour.
  • the refining power employed was 7-8 horsepower day/dry ton of fiber.
  • the freeness of the pulp coming from the Bauer refiner was in the range of 400 to 500 cc. CSF, and after additional refining in a Jordan refiner and at the headbox the freeness of the furnish was in the range of 200 to 250 cc. CSF.
  • the starch slurry was added at a rate sufiicient to produce a loading of 4% starch, based on the dry weight of fiber.
  • Residence time in the Bauer refiner ranged from one to three seconds, and temperatures in the refining ranging from 200 to 250 F. were noted.
  • Ratio of TiOz to extender in additive was 3:1.
  • the following example illustrates the preparation of a furnish, and paper from such furnish, where a very high loading of starch was employed in such furnish.
  • EXAMPLE 6 A pulp blend of the type utilized in Example 3 was passed through a Bauer refiner to obtain fiber fibrillation, the power input to the refiner during such fibrillation being approximately 10 horsepower day/dry ton of fiber.
  • the pulp on leaving the refiner was diluted to 3.5% consistency and further refined to a final headbox freeness of about 200 cc. CSF.
  • Residence time in the refiner was approximately two seconds and the temperature of the pulp in the refiner was raised to approximately 240 F.
  • Furnish so prepared was converted into paper on a paper-making machine. No problems were encountered in running the furnish on the machine.
  • the paper produced had a very fine erasable surface, with a surface strength comparable to the surface strength of the best erasable rag furnish tracing paper available commercially.
  • the surface strength when measured showed the maximum rating of 32.
  • the paper when measured for internal bond strength demonstrated an internal bond exceeding 500.
  • the following example illustrates the production of a paper having a high stiffness factor, such as may be employed in tab cards and other business form papers.
  • EXAMPLE 7 A blend of pulp of the type utilized in Example 3 was dewatered as in Example 3 to about 35% consistency and refined in a Bauer refiner to produce fiber fibrillation. A power input of about 8 horsepower day/dry ton of fiber was used. Simultaneously with the feeding of the pulp, a 30% slurry of uncooked starch (Cota-Kote 1448) was injected into the refiner. The residence time within the refiner was about three seconds and the temperature of the pulp mixture in the refiner was raised to approximately 240 F. The addition of the starch slurry was such as to produce a loading of 11% starch based on the dry weight of fiber. After leaving the Bauer refiner the pulp was diluted to 3.5% consistency and further refined in conventional Jordan refiner to about 230 cc. CSF.
  • EXAMPLE 8 Furnishes were prepared resembling the one prepared in Example 7, but differing in the amount of starch loading they contained. Papers prepared from such furnishes were given a size press treatment, to obtain grease resistance.
  • a size press composition was used consisting of an aqueous mixture of 100 parts Penford Gum 280 (Penick & Fords ethylated starch), 25 parts urea, and 1.25 parts Fe 806 (fluorocarbon, by Minnesota Mining and Manufacturing).
  • the size press coating composition contained 15% solids. In the size press treatment, the composition was applied at a rate to obtain a distribution of solids of about 1.75 to 2.0 pounds per 3000 square feet of paper.
  • the following table illustrates the grease holdout rating of the various papers produced.
  • the rating was determined by a procedure devised by Minnesota Mining and Manufacturing, wherein a drop of testing solution is placed on the surface of the sheet, and the rating given is related to the type of solution that will stand on the surface for 15 seconds in the form of a drop without failing.
  • the testing solutions used comprise a mixture of castor oil, heptane and toluene, with lower numbered solutions being high in castor oil, and the highest numbered solution (12) having no castor oil.
  • a coating composition comprising parts latex (carboxylated styrene-butadiene copolymer) and 33 parts alpha protein, in sufiicient water to make a 17% solids mixture. Paper so prepared exhibited good grease holdout properties com parable to the holdout properties.
  • FIGS. 1 and 2 are reproductions of two of such photomicrographs. It will be noted that the refining of the pulp at high consistency and with a temperature condition produced in the pulp above the gelation temperature of the starch were effective to produce cooking of the starch particles with such swelling to form gels. It Will further be noted that fibrillation occurred in the fibers by reason of such refining, as demonstrated by the hairlike strands which project out from the fiber bodies.
  • the photomicrographs reveal a high degree of sorption of the cooked starch, as evidenced by the gelatinized starch ap pearing as globular masses sorbed against the cellulosic fiber bodies, with the fibrils of such bodies projecting through and encompassed by such globular masses.
  • Furnish prepared according to the invention ordinarily is subjected to a finish refining at low consistency, after the fibrillation by refining at high consistency, which has the effect of further reducing the freeness of the pulp.
  • High consistency refining has been noted to introduce some balling and entangling of the fibers.
  • the finish refining serves to untangle these fibers, which results in a more uniform paper product being obtained.
  • a method of loading a pulp of cellulosic fibers with starch which in aqueous solution and at a temperature above gelatinization temperature cooks to form a gel comprising providing an aqueous pulp mixture of defibered cellulosic fibers, incorporating the starch with such in a nongelatinized state with the defibered pulp mixture, refining the pulp mixture together with such starch to effect fibrillation of the fibers with loosening of fiber fibrils, and concurrently with the refining and fibrillation of the fibers and with the pulp mixture raised to a. temperature which is above said gelatinization temperature cooking said starch to form a gel with such gel during such fibrillation becoming sorbed by the fibers in the pulp mixture and the fibrils which become loosened from the fibers.
  • a method of preparing a paper-making pulp with a starch loading of from 3 to 30% comprising an aqueous pulp mixture of defibered cellulosic fibers, refining the pulp mixture in a high consistency refiner to effect fibrillation of the fibers in pulp with loosening of the fibrils, introducing the starch in an uncooked state to the refiner together with the pulp mixture, the pulp mixture in the refiner and during the refining having a consistency exceeding about 10%, concurrently with the refining and by interfiber friction raising the temperature of the pulp mixture including starch within the refiner to above the cooking temperature of the starch to effect cooking of the starch with such forming a gel which becomes sorbed by the fibers in the pulp mixture and the fibrils which become loosened on the fiber, after refining lowering the consistency of the refined pulp mixture to one which is fiowable, and further refining this pulp mixture at such fiowable consistency to further reduce the freeness thereof.
  • a method of making a paper product having improved holdout and other properties comprising providing an aqueous pulp mixture of defibered cellulosic fibers, refining the pulp mixture in a high consistency refiner to effect fibrillation of the fibers in the mixture with loosening of the fiber fibrils, introducing starch in an uncooked state into the refiner together with the pulp mixture with the starch addition being within the range of 3 to 30% based on dry fiber weight, the pulp mixture during refining having a consistency exceeding about 10%, concurrently With the refining and by interfiber friction raising the temperature of the pulp mixture including the starch in the refiner to above the cooking temperature of the starch to effect cooking of the starch with such forming a gel which becomes sorbed by the fibers in the pulp mixture, after refining lowering the consistency of the pulp mixture to one which is fiowable and further refining the mixture to reduce the freeness thereof, converting the pulp mixture into paper, and size press treating such paper with a grease-resistant formulation.

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DE2023499C3 (de) 1975-06-19
GB1290972A (ja) 1972-09-27
FR2052618A5 (ja) 1971-04-09
NL7009025A (ja) 1970-12-22
JPS4944001B1 (ja) 1974-11-26
BE752229A (fr) 1970-12-01
DE2023499B2 (de) 1974-10-31
DE2023499A1 (de) 1971-01-07
CA919864A (en) 1973-01-30
NL148126B (nl) 1975-12-15
SE364745B (ja) 1974-03-04

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