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United States Patent Office Patented Apr 3,180,787 United States Patent Office Patented Apr. 27, 1965 2 not suitable. In general, polyethylene polyamines having 3,180,787 PROCESS FOR MAKENGHGH FLEXURAL molecular weights in excess of 150 are satisfactory, and STRENGTH PAPER those ranging in molecular weight from 500 to 1000 are James W. Adams, Schofield, Wis, assignor to American preferred. Can Company, New York, N.Y., a corporation of New 5 Lignosulfonates satisfactory for use in my invention Jersey may be obtained by isolation from spent sulfite liquor by No Drawing. Filed May 20, 1959, Ser. No. 844,409 any of several means. For example, treatment of spent 2 Claims. (C.162-163) sulfite liquor with lime according to the Howard process described in the United States Patents Re. 18,268, Decem This invention relates to a method for increasing the 10 ber 1, 1931; 1,856,558, May 3, 1932 and 1,924,361, Au flexural strength of fibrous cellulosic products by incorpo gust 29, 1933, results in the recovery of lignin material as rating therein a polyethylene polyamine lignosulfonate basic calcium lignosulfonate. This water-insoluble ma and to the improved fibrous products obtained thereby. terial may be converted to the water-soluble lignosulfonic Stiffness, without accompanying brittleness, is a desir acid or soluble salt derivative such as the ammonium or able attribute of paperboard products such as cartons 5 alkali metal salt by known methods. These water solu used in the protective packaging of various commodities. ble compounds are suitable for use in our invention. Such cartons must have adequate stiffness to insure proper I have also found that separation of the lignosulfonate operation on packaging machinery, to retain the packaged fraction from spent sulfite liquor is not a necessary pre product without undue deformation of the package and requisite to its use in my invention, since the whole spent to give the customer a feeling of sturdiness and strength 20 sulfite liquor may be economically utilized in my proc of package rather than flimsiness and shoddiness. ess. Whole spent sulfite liquor may be added to a slurry Stiffness of paper and paperboard products may be in of cellulose pulp and, upon addition of a water solution creased by an increase in thickness of the sheet, but it is of the desired polyethylene polyamine, the lignosulfonate often desirable to increase stiffness without increasing content of the liquor is precipitated as an insoluble poly the caliper, or thickness, of the packaging material, both 25 ethylene polyamine lignosulfonate and becomes largely from the standpoint of economy and machine workability. occluded by the pulp fibers. On making paper from this Thus, the packaging industry desires high flexural strength pulp slurry, the soluble wood sugars, carbohydrates and in paperboard packaging materials. Flexural strength is hemicellulose present in the whole spent liquor are sepa a measure of stiffness independent of the thickness, or rated from the pulp on the paper machine wire and suc caliper, of the sheet material. 30 tion rolls and thereby pass off in the white water, leaving I have found that the flexural strength (i.e. stiffness only the desired insoluble polyethylene polyamine ligno per unit caliper) of paper and paperboard may be in sulfonate affixed to the fibers of the paper web. creased by the precipitation of insoluble polyethylene The degree of increase in flexural strength resulting polyamine salt of an anion such as the lignosulfonate, from the process of my invention is dependent both on alkyl aryl sulfonate or alkyl naphthalene sulfonate in 35 the amount of the polyethylene polyamine lignosulfonate, the presence of an aqueous slurry of cellulose fiber pulp alkyl aryl sulfonate or alkyl naphthalene sulfonate oc which occludes the freshly precipitated polyethylene poly cluded with a given weight of pulp and on the composi amine salt. Paper sheets made from pulp so treated have tion of the insoluble polyamine salt. I have found that greater stiffness per unit of thickness than paper made higher amounts of the salt result in greater flexural from untreated pulp. Polyethylene polyamine lignosul 40 strength up to a maximum which is obtained when be fonates are the preferred stiffening agents, although poly tween about 30% and 50% of polyethylene polyamine amine salts of other anions may also be used as will be lignosulfonate or similar insoluble polyethylene polyamine detailed later. salt based on the weight of the pulp fibers is present. The process of my invention, as illustrated by treatment Higher percentages fail to increase the flexural strength of cellulose pulp with polyethylene polyamine lignosul 45 further, and may even result in a decrease in flexural fonate, may be carried out as follows: An aqueous slurry strength due to the increased brittleness of the sheet. Fur of cellulose pulp obtained from wood, straw or similar thermore, the amount of flexural strength increase will fibrous material by any conventional digestive cooking vary depending on the ratio of polyethylene polyamine to process such as the sulfite process, the soda process, the lignosulfonate or other anion used in the preparation of sulfate process or other similar process is admixed with 50 the insoluble salt. Both polyethylene polyamines and an aqueous solution of lignosulfonic acid or a soluble lignesulfonic acid have a plurality of reactive salt-forming metal salt of lignosulfonic acid. To the pulp slurry is then groups so that these two reactants may be combined in added sufficient polyethylene polyamine to precipitate the varying ratios to form salts. In general, an increase in lignosulfonate present in the pulp slurry as a water-in the polyamine to lignosulfonate ratio results in increased soluble polyethylene polyamine lignosulfonate salt. The 55 flexural strength of the treated paperboard except when pulp slurry is then made into a paper sheet on conven both polyamine and lignosulfonate are added in relatively tional paper-making equipment. The insoluble polyamine large amounts. lignosulfonate becomes largely trapped or occluded by The data in the following Table I indicate the increase the pulp fibers and remains fixed on the fiber surface in flexural strength of paperboard obtained by precipitat throughout the paper-making process. When the paper 60 ing varying amounts of polyethylene polyamine lignosul web formed from the pulp on conventional equipment is fonate on pulp using a constant ratio of the amine and passed over the drying rolls, the precipitated polyethylene lignosulfonate reactants, whereby a constant composition polyamine lignosulfonate which is present fuses and then of the precipitated polyethylene polyamine lignosulfonate sets as a thermosetting resinous material under the in is obtained. The samples were prepared and tested as fluence of the drier heat and thereby contributes mark 65 follows: - edly to the flexural strength of the resulting paper sheet. Nine grams of sulfite cellulose pulp were dispersed in The polyethylene polyamines, in order to be satisfac 900 cc. of water. To a pulp slurry of this composition tory for my use, must be water soluble but also must form was added varying amounts of spent sulfite liquor and insoluble salts of lignosulfonate and other suitable anions. then polyethylene polyamine as indicated in Table I. The The lower molecular weight polyethylene polyamines such 70 spent liquor contained about 10gm. of organic solids of as ethylene diamine, diethylene triamine and triethylene which about 5gm. comprised lignosulfonates calculated as tetramine form soluble lignosulfonate salts and hence are lignoSulfonic acid per 100 cc. of liquor. The polyethylene 3,180,787 3. 4. polyamine had a molecular weight of about 650 and was TABLE I added as a 10% aqueous solution. The treated pulp was formed into a 9' x 9’ handsheet by conventional pro Flexural strength of handsheets from pulp treated with cedures, which included drying the sheet at a tempera polyethylene polyamine lignosulfonate ture (about 200 F.) sufficient to fuse the precipitated amine lignosulfonate on the fibers of the sheet, and the Flexural strength, p.s.i. flexural strength was obtained on this handsheet. Flexu ral strength is obtained by subjecting a strip of paperboard Parts polyamine 1. O 2 4. O A. 16 to sufficient longitudinal bending stress to fracture or Parts SSL Solids: separate a sufficient number of the fibers so that a crease O 50-------------- 2,340 3,000 3,350 3,710 3,270 4,140 forms across the width of the board. The force necessary 8-- - - 2,290 2,920 3,520 4,710 4,030 4, 210 O 2,320 2,850 4,550 5,030 4,060 5,110 to bend the board to its creasing or "breaking' point is O 2,100 2,320 3,320 4, 270 3,820 4,410 measured and flexural strength is calculated using this 220 1,530 1,620 2,960 3,800 3,770 4,790 280. -- 1,770 1,820 2,900 3,370 3,490 3,580 value. In the present case, a 1-inch wide strip of the 340------------- l, 125 -------- 1,620 2,740 4,090 2,320 handsheet about 4 inches long was positioned horizontally 5 400------------- 1,820 -------- 2,760 3,070 2,600 1,080 on two vertical supporting columns so as to span the 1/8 inch gap between the supports. Force was applied down 1 Parts per 100 parts oven dry pulp. ward on the test sample at the midpoint of the 1/8 inch it will be noted from the data in Table II that increas span by a steel knife 332 inch in thickness having a rounded ing the amount of polyethylene polyamine added with a edge. The force applied to the knife blade was measured 20 given amount of spent sulfite liquor (tabulated as spent by a strain gauge, the varying resistance of the gauge being sulfite solids) generally results in an increase in flexural read from a bridge amplifier meter calibrated in ounces.
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