some experiments in sodium sulfite !pulping

21
OREGON FOREST PRODUCTS LMORATOIR LIBRARY SOME EXPERIMENTS IN SODIUM SULFITE !PULPING August 1948 INFORMATION REV!EWtLI AND REAFFIRMED March 1956 No. 81728 UNITED STATES DEPARTMENT OF AGRICULTURE FOREST SERVICE FOREST PRODUCTS LABORATORY Madison 5, Wisconsin In Cooperation with the University of Wisconsin

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Page 1: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

OREGON FOREST PRODUCTS LMORATOIRLIBRARY

SOME EXPERIMENTS IN SODIUMSULFITE !PULPING

August 1948

INFORMATION REV!EWtLI

AND REAFFIRMED

March 1956

No. 81728

UNITED STATES DEPARTMENT OF AGRICULTUREFOREST SERVICE

FOREST PRODUCTS LABORATORYMadison 5, Wisconsin

In Cooperation with the University of Wisconsin

Page 2: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

CREGON FOREST PRODUCTS LABOKRTORILIBRARY

_

SOME EXPERIMENTS IN SODIUM SULFITE PULPING1-

By

J. N. McGOVERN, Chemical Engineer'and

E. L. KELLER, Chemist

Forest Products Laboratory,? Forest ServiceU. S. Department of Agriculture

Abstract

Pulping with sodium sulfite (Na2 SO ), one of the earliest-mentioned chemicalpulping processes, has not been ustd commercially to any extent despite the'high. quality of the pulp, mainly because-of chemical-recovery complications.Recently renewed interest in the process, due perhaps to the possibility ofemploying it for little-used wood species, has made timely the presentationof results of some experiments in sodium sulfite pulping at the Forest ProductsLaboratory, Madison 5, Wis. These experiments were as follows:

1. Black spruce chips were pulped with sodium sulfite buffered with sodiumsulfide, and the effects on pulp yield and on quality of variations in pulpingtime, temperature, and liquor concentration were determined.

2. The black spruce sodium sulfite pulps were compared with acid sulfite andsulfate pulps from the same kind of chips, and were found to be produced in15-percent-lower yield, to be nearly as bright as the acid sulfite pulps (un-bleached), to be as strong or stronger than the sulfate pulps, and to require25 percent more chemical on a sodium oxide base and much longer pulping timesthan the sulfate pulps.

3. Sodium sulfite pulps were also prepared from white spruce, Engelmann spruce,balsam fir, aspen, and black maple. The results from the softwood pulps wereall similar, whereas the hardwood pulps were produced in appreciably higheryields and brightnesses, but were considerably weaker than the softwood pulps.The hardwood sodium sulfite pulps, however, after some beater processing, com-pared favorably in strength with softwood acid sulfite pulp..

Presented at the annual meeting of the Technical Section, Canadian Pulp &Paper Assn., Montreal, Q., Jan. 28-30, 1948; published in Pulp & Paper Mag.of Canada, Aug. 1948.

2Maintained at Madison 5, Wis., in cooperation with the University of Wiscon-sin.

Report No. R1728 -1-

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4. Jack pine chips were pulped with sodium sulfite buffered with sodium bi-carbonate in producing paps in yields varying from 48'to 78 percent. Maxi...mums in bursting, tearing, and tensile strengths were obtained in pulps madein yields of 55 to 60 percent, but the decreases in these strengths up to 78percent yield were only 25 percent of the maximum values. The highest folding-endurance values were shown by the lowest ...yield pulp. A high-yield (56.5 per-cent) sulfate pulp from the same"chips had the same strengths as the neutralsodium sulfite pulp made in the same yield except for folding endurance,which was twice as high for the sulfate pulp.

Introduction

The idea of using sodium sulfite (Na 2S0) in the neutral or slightly alkalinecondition to produce a chemical pulp fr6m wood is credited to Cross in 1880

(8).2 In 1886 (9), Cross and Bevan published a "Classification of the Chemi-cal Processes of Disintegrating Wood," which included, as a specific process,pulping with "Water Together with Neutral Sulfites." A neutral pulpingprocess was apparently proposed by Cross to avoid the serious difficultiesfrom corrosion encountered in acid sulfite pulping; The high temperaturesand pressures required for neutral sulfite pulping, however, prohibited itsapplication in the digesters of the construction of that time. The subsequentdevelopment of acid-resistant digester linings removed the need for a neutralpulping agent.

Except for occasional patents relating to sodium sulfite pulping,` it wasnot until more than 40 years after Cross' invention that a definite interestin the process was again shown. By this time the limitations of digesterconstruction had largely been overcome; and the demand for pulps of higherand higher quality had turned the attention of the pulp industry to thepreviously recognized excellence of sodium sulfite pulps. These pulps weregenerally considered to equal sulfate pulps in strength and acid sulfite pulpsin unbleached brightness and bleachability (a satisfactory method for bleach-ing sulfate pulps was not available at that time): During the 1920's several.American mills started commercial pulping with sodium sulfite according to theKeebra process (2, 7), and Drewsen mentioned his work and application inthe same field (11). The procedures used, however, for recovering the largeamounts of chemical used in the process were somewhat complicated and notentirely satisfactory, and operation of the process was gradually

-Underlined figures in parentheses refer to Literature Cited on page 10 of thisreport.

LiBecause excellent reviews of the literature on sodium sulfite pulping havebeen given by Hausen (13), Rue (17), Haffner and Kobe (12), Sutermeister(19), and Schellhorn T8), and the general aspects of salium sulfite haverecently been considered by Wells (20) and Murdock (15), no attempt ismade to cover the literature in this report.

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discontinued. Further, the subsequent development of methods for bleachingsulfate pulps practically made sodium sulfite pulps unnecessary.

In the last few years an interest in sodium sulfite pulping has reappeared,possibly due to a desire to obtain greater pulp values from the little-usedspecies, such as the hardwoods and Douglas-fir, than seemingly can be ob-tained from pulps prepared by conventional methods (6, 12).

So far as the technology of sodium sulfite pulping is concerned, Cross (10)established the main principles involved, namely, that high temperatures andlarge amounts of chemicals are required, but gave few details of the process.Since that time there have been relatively few published studies giving basicdata needed for the successful application of the process, outside of theinformation to be found in patents and descriptive articles. The chief basicstudies appearing in the literature have been as follows:

1. Aspen and blackgum sawdusts have been pulped under certain variations oftemperature, time, and chemical concentration and compositions, and yieldsand chemical compositions of the pulps have been determined (1, 3, 4, 16).

2. White spruce, Western hemlock, and slash pine have been pulped withsodium sulfite and sodium bisulfite and mixtures thereof, and pulp yields andproperties have been determined (5).

3. Shortleaf pine has been pulped with sodium sulfite, buffered withvarious agents because wood acids formed during pulping, especially fromhardwoods, cause sodium sulfite liquors to become acid unless provisionis made to maintain the liquor in the neutral or slightly alkaline condi-tion, and the yield, bleachability, and strengths of the pulp have beendetermined (6). A sodium sulfide buffered liquor has been also applied tonumerous hardwoods and softwoods in determining its effects on pulp bleach-ability and strength (6).

4. Douglas-fir has been pulped, the pulp yield, bleachabilities, andstrengths have been determined under various conditions of temperature andratios of sodium oxide to sulfur dioxide in the cooking liquor and sodiumoxide to the wood in establishing the optimum conditions for pulping thisspecies. Southern pine, Western hemlock, cottonwood, and aspen have alsobeen pulped under the established conditions (12).

The semichemical pulping process'employing sodium sulfite buffered withsodium bicarbonate or carbonate, which started in the late 1920 1 s, has

shown a remarkable expansion in recent years. In semichemical pulping,wood chips are softened and partially delignified by cooking in the sodiumsulfite liquor, and the pulping is completed mechanically, usually in anattrition mill. Because of the relatively small amount of chemicals usedand the high pulp yields obtained, recovery of the chemicals has generallynot been necessary for economical operation. This process has been foundparticularly applicable to hardwood species.

Report Nos 81728 -3-

Page 5: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

5. The effect of the presence of sodium thiosulfate in the sodium sulfitecooking liquor on pulp properties has been determined in connection with theformation of this chemical in preparing the cooking liquor following certainproposed chemical-recovery processes (14, 18).

The experiments reported here were conducted at the Forest Products Laboratoryon certain variables of the sodium sulfite pulping process and on severalspecies in connection with developing pulps for special paper products. Theseexperiments included a study of the effects on pulp yield and properties oftime, temperature, and liquor concentration in pulping black spruce withsodium sulfite buffered with sodium sulfide and a study of the effect of pulpyield on properties of jack pine pulps made with sodium sulfite buffered withsodium bicarbonate. Also included in the report, are a comparison of blackspruce sodium sulfite, sulfate, and acid sulfite pulps and a comparison ofseveral hardwood and softwood pulps prepared by odium sulfite processes andconventional processes.

PULPING WITH SODIUM SULFITE BUFFERED WITH SODIUM SULFIDE

Varying Time, Temperature, and Liquor concentration

in Pulping Black Spruce

In these experiments typical black spruce (Picea mariana) from the AlgomaDistrict, Ontario, Canada, was pulped with a sodium sulfite liquor bufferedwith sodium sulfide. The effects of varying (a) pulping time, (b) pulpingtemperature, and (c) concentration of sodium sulfite in the pulping liquoron • pulp yield and properties were determined. The digestions of 5/8-inchchips were made in duplicate in a stainless-steel-lined, tumbling digesterequipped with a steam jacket and having a capacity of 13 cubic feet. Thecooking liquor was made by adding separately to the digester sodium sulfiteand sodium sulfide solutions prepared from technical-grade chemicals. Thecooking liquor at the start of the digestion had a pH value of approximately11.0. The pH value dropped to about 9.0, however, shortly after the start ofthe digestion and remained near this lower value to the end of the digestion.The digestion conditions employed are given in table 1. Upon completion ofthe digestions the pulps were discharged into a blowpit end washed. The pulpswere then screened over a flat diaphragm screen with 0.008-inch slots andlapped on a wet machine for the yield determination. The screening rejectswere dried directly. The pulps were tested for bleachability as measured,bypermanganate number, strength, and chemical composition, according to TAPPIstandard methods.

The digestions were all conducted with an excess of sodium sulfite in thecooking liquor. In the experiments on effect of pulping time and tempera-ture, nearly twice the chemicals required for pulping were present. In theexperiments on effect of liquor concentration, the excess varied roughlyfrom 50 to 100 percent of the actual chemical requirements.

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(a) Effect of Pulping Variables onPulp Yield and Chemical Composition

Pulping time (Series I table 1).--The general effects of increasing the totalpulping time from 7.25to 11.5 hours, other conditions being the same, were,of course, to decrease total yield, screenings, permanganate number, and pulplignin content, and to increase chemical consumption and the total and alphacellulose content of the pulps. The nature of some of these changes withinthe range of the experiments are shown in figure 1. The change in chemicalcomposition of the pulp with increasing pulping time is interesting. Thedelignification reaction proceeded at a uniform rate up to the point of about99 percent lignin removal, corresponding to about 0.5 percent lignin in thepulp, and then practically ceased. During the period of delignificationwithin the present experiments, only small amounts of total and alpha cellu-lose were removed and the contents of these constituents in the pulps in-creased at the expense of the lignin. When delignification virtually stopped,however, the rates of cellulose removal became appreciable and pulp yield de-creased at a faster rate than previously, which indicated overcooking anddegradation of the cellulose. During this period of degradation, the cellu-lose contents of the pulp increased somewhat, probably because hemicelluloseswere being removed at a faster rate than the cellulose. It should be statedthat nearly 37 percent of the total cellulose and 27 percent of the alphacellulose present in the wood had been removed in pulping to the highest yieldunder consideration in these experiments.

Pulping temperature (Series II, table 1).--The main effect of increasing thepulping temperature from 170° to 185° C., in pulping to the same permanganatenumber, was to reduce greatly the pulping time. Only 2.3 hours were requiredat a pulping temperature of 185° C., in comparison with 8 hours at 170° C., to

remove approximately 98 percent of the lignin in the wood. (The total diges-tion times were 7.3 and 13 hours, respectively,) The yield data were notsufficient to determine any definite effect. The chemical compositions ofthe pulps made at the different temperatures were practically the same, whichindicated that the relative rates of total and alpha cellulose and lignin solu-tion were the same at the various temperatures. Slightly less chemical wasconsumed in pulping at 185° C. in comparison with 170° C. This decrease mayhave meant that the pulping was somewhat more efficient at the higher tempera-ture.

Pulping liquor concentration (Series III, table 1).--The general effects of in-creasing the concentration of sodium sulfite in the pulping liquor from 98 to

177 grams per liter, in pulping to the same permanganate number, was to reduceappreciably the pulping time, to increase chemical consumption, and to decreasesomewhat (at the highest concentration) the total and alpha cellulose contentsof the pulp. The total digestion time at the highest concentration was 8.5

hours in comparison with 10.5 hours at the lowest concentration. The chemicalconsumption increased approximately 25 percent when pulping with the strongestas compared with the weakest, pulping liquor. The pulp made with the strongestpulping liquor appeared to have lower total and alpha cellulose contents thanthose made with weaker liquors, a fact that indicates a possibly more drasticaction on the pulp at high concentrations of cooking liquor than at lowerconcentrations.

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Page 7: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

(b) Effect of Pulping Variables on Pulp Strength

All of the black spruce sodium sulfite pulps were very strong, in whichrespect they were comparable to sulfate pulps . (as will be discussed later).Variations in the pulping conditions affected pulp strength only in a minorway, for the most part.

Pulping time (Series I, table 2).--The bursting and tensile strengths showed atendency toward maximum values at the medium pulping times in the medium tohard pulps (permanganate numbers of 11 to 16). The tearing strength appearedto increase somewhat with pulping time, and was highest in the softest pulp.The folding endurance of pulps did not change according to any trend withdegree of pulping.

Pulping temperature (Series. II, table 2).--There appeared to be no trend inpulp strength with temperature of pulping within the limits of the experi-ments.

Pulping liquor; concentration (Series table 2).--Although differences inpulp strength were found between pulps made with varying concentrations ofsodium sulfite in the pulping liquor, there appeared to be no trend within thelimit of the experiments.

Comparison of Sodium Sulfite Pulps with Calcium Acid

Sulfite and Sulfate Pulps from Black Spruce

Conventional calcium-base sulfite and sulfate pulps were made from the sameshipment of black spruce as was used for the alkaline sodium sulfite experi-ments described above. Yield, brightness, chemical composition, and strengthdata for the three kinds of pulps may be found in table 3. Data are given 'intable 3 for two sodium sulfite pulps to enable comparison with the sulfite andsulfate pulps at the' same permanganate number. The chief points of interestabout the sodium sulfite pulps are their brightness, nearly that of sulfitepulp; their strength, equal to or greater than that of the sulfate pulp; andtheir relatively low yield. The yield of sodium sulfite pulp was approximately15 percent lower than that of the 'sulfite or sulfate pulps, a serious drawbackin these days of wood shortages and high wood costs. The amount of chemicalon a sodium oxide base used in producing the sodium sulfite pulp was 25 percentmore than that used for the sulfate_pulp. Further, the . use of a cooking liquorwith a high concentration of sodium sulfite (and a resulting large excess ofchemical over that required for pulping) in order to accelerate the pulping toa rate permitting relatively short pulping times, could possibly result in twoto three times as much chemical on a soda base going to the recovery system insodium sulfite pulping as in sulfate pulping, if some scheme of reuse of thespent sodium sulfite liquor were not employed. Finally, the sodium sulfitedigestions, although made at the elevated temperature of 180° C., requiredsomewhat longer digestion times than the acid sulfite digestions and greatlylonger times than the sulfate digestions.

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Page 8: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

Comparison of Softwood, Aspen, and Black Maple

Sodium Sulfite Pulps

Three varieties of spruce, balsam fir, and two northern hardwoods were pulpedunder similar conditions with sodium sulfite buffered with sodium sulfide.The digestion results and pulp data may be found in table 4. The white (Piceaglauca) and Engelmann (Picea Engelmannii) spruce and balsam fir (Abies balsamea)appeared to give somewhat higher yields of pulp than the black spruce, but thestrengths of all the pulps were in the same range as those of the black sprucepulp, The Engelmann spruce pulp was possibly higher in tearing strength thanthe others. The quaking aspen (Populus tremuloides) was pulped somewhat moreeasily than the black spruce, as was shown by the slightly shorter cooking time,lower permanganate number, and lower concentration of sodium sulfite used inthe pulping liquor, although the chemical consumption was approximately thesame for the two woods. The black maple (Ater nigrum) was pulped more diffi-cultly than the aspen, although the differences may have been largely due tothe relatively low concentration of sodium sulfite in the cooking liquor.The high screenings value for the maple digestion, an indication of nonuniformpulping, may also have been a result of this low concentration. The yields ofthe hardwood pulps were substantially higher than that of the black sprucepulp. The yield of black maple pulp was exceptionally high, but the yield ofaspen pulp was lower than that usually obtained in acid sulfite and sulfatepulping to the same lignin content. The unbleached hardwood pulps showedbrightness values as high as or higher than might be expected from the corre-sponding unbleached sulfite pulps. The strengths of the hardwood sodium sul-fite pulps were greatly below those of the corresponding black spruce andother softwpod pulps. On the other hand, the strengths of the hardwoodsodium sulfite pulps after processing to 550-cubic-centimeter freeness(Schopper-Riegier) were practically the same as the strengths of spruceacid sulfite pulp (table 3). Unprocessed or slightly processed hardwoodpulps, however, were considerably weaker than spruce acid sulfite pulp atthe same high freeness value. The strengths of the hardwood sodium sulfitepulps check with those previously reported (6) for aspen and maple.

PULPING WITH SODIUM SULFITE BUFFERED UITH SODIUM BICARBONATE

Pulping with sodium sulfite buffered with sodium bicarbonate is generallycalled neutral sodium sulfite pulping. The cooking liquor at the start ofthe digestion has a pH value of 8.0 to 8.5. During the course of the diges-tion the pH value of the pulping liquor drops somewhat, so that the finalvalue is nearly neutral, 7.2 to 7.6. This type of pulping liquor is usedextensively in semichemical pulping.

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Page 9: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

Varying Yield in Pulping Jack Pine

In these experiments, jack pine slabs (Pinus banksiana) from wood cut in theregion north of Lake Superior were pulped with a sodium sulfite liquor bufferedwith sodium bicarbonate to produce pulp varying from 48.4 to 78.4 percent.The digestions were made of 5/8-inch chips in the same digester as describedpreviously. The pulping liquor was made from technical-grade sodium sulfiteand sodium bicarbonate. Pulping was done according to a two-stage process asfollows: The chips were steamed in the digester at atmospheric pressure for0.5 hour. The steamed chips were then impregnated for 1 hour at 120° C. withneutral sodium sulfite liquor. The excess liquor not absorbed by the chipswas then removed and fortified for a subsequent impregnation. The digestionwas then conducted with the chemicals left in the chips and digester. Thedigestion conditions may be found in table 5.

All of the partially or fully pulped chips were fiberized in a commercial-size disk fiberizer to a freeness value near 850 cubic centimeters (Schopper-Riegler). The pulps were then screened over a flat diaphragm screen with0.012-inch slots and lapped on a wet machine. The yields were determined byfiberizing an aliquot of the unfiberized material in a 5-pound beater anddetermining the loss of soluble matter on fiberizing. The pulps fiberizedin the Bauer mill were tested for strength and chemical composition accord-ing to standard methods. The results may be found in table 6.

Chemical Consumption and Pulping Time•

The total amount of chemical (sodium sulfite plus sodium bicarbonate) consumed in the pulping varied from 53.3 percent of wood weight for, the pulp oflowest-yield (48.4 percent) to 22.0 percent for the pulp of highest-yield(78.4 percent). The relatively high concentration of sodium sulfite in thespent liquor (table 5) indicated that the actual chemical requirements wereabout 10 percent less than found in these experiments. In comparison withsulfate pulping to the same lignin content, the neutral sodium sulfite pulping,as conducted in these experiments and as calculated on a sodium oxide base,consumed about 45 percent more chemical.

The time at the pulping temperature of 170° C. varied from 14 hours (convertedfrom 180° C.) for the lowest-yield pulp to 3.0 hours for the highest-yieldpulp. The variation appeared to be linear within this range.

Chemical Composition

The neutral sodium sulfite pulps were analyzed for lignin, holocellulose, andalpha cellulose. The chemical-composition data and the percentages of theseveral constituents removed during pulping (table 6) were plotted againstpulp yield, and the resulting curves may be found in figures 2 and 3. Inproceeding from the highest- to the lowest-yield pulps ) the lignin contentdecreased and the holocellulose and alpha cellulose contents increased in anearly linear direction (fig. 2). The percentage of each constituent removed

Report No. R1728 -8-

Page 10: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

during pulping increased with a decrease in yield (fig: 3). There was atendency for less alpha cellulose than hemicellulose to.be removed with de-creasing yield, as indicated by the ratios of alpha cellulose to holocellulosecontents from the data in table 6. There was also a tendency for relativelyless lignin than nonlignin (including holocellulose) to be removed, as indi-cated by the ratios of lignin removed to lower yield from the data in table 6.

Appreciable amounts of both holocellulose and alpha cellulose, in addition tothe considerable amount of lignin, were removed in pulping to the yield of77.4 percent, the highest yield for which data were available.

Pulp Strength

The strengths of test sheets from the various pulps processed to 800-cubic-centimeter and 550-cubiccentimeter freeness (Schopper-Riegler) according tothe standard beater test, were plotted against pulp yield. The resulting,curves may be found in figure 4. The pulps appeared to show maximum valuesin bursting, tearing, and tensile strengths at pulp yields of 55 to 60 per-cent. The decreases in these maximum-strength properties in increasing theyield to the highest value of 78.4 percent, were of the rather moderate orderof 25 to 30 percent. The folding endurance, on the other hand, ; was highestin the lowest-yield pulp and was about three times as high as in the highest-yield pulp.

The fact that the jack pine neutral sodium sulfite pulps made in yields of 75to 80 percent were quite strong, is interesting because of the indicated possi-bility of producing high-yield pulps for use in paper and board products re-quiring relatively higher-strength pulps. Experiments at the Forest ProductsLaboratory have indicated that jack pine sulfate pulps produced in yields near75 percent, on the other hand, may be only one-third or less as strong aspulp produced in 50-percent yield, except in tearing strength, for whichproperty the loss in strength is relatively small.

Comparison of Jack Pine Neutral Sulfite and Sulfate Pulps

A high-yield sulfate pulp was made from the same kind of jack pine chips aswere used in the neutral sodium sulfite pulping experiments previously des-cribed. The yield of sulfate pulp was 56,5 percent, or in the range of yieldsin which the neutral sodium sulfite pulps showed maximum values in most oftheir strength properties. The strength properties of the sulfate pulp andof a neutral sodium sulfite pulp at the same yield are given in table 6. Thedata for the neutral sodium sulfite pulp were interpolated from the relation-ships between yield and chemical composition in figures 2 and 3 and strength

properties in figure 4. The high-yield sulfate and neutral sodium sulfitepulps are indicated in table 6 as not differing appreciably in bursting, tear-ing, and tensile strengths. The sulfate pulp, however, had nearly twice thefolding endurance of the neutral sulfite pulp. The folding-endurance data maybe considered to show that the sulfate pulp is a softer and more resilientpulp than the more brittle neutral sodium sulfite pulp. Although the strengthvalues, except for folding endurance, are approximately at the maximum that

Report No. 81728 -9-

Page 11: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

. can be expected from the neutral sodium sulfite pulp under the pulping condi-tions employed, it is likely that the strength properties of the sulfate pulpwould be increased to a certain extent by pulping to a somewhat lower yield.

LITERATURE CITED

1. Aronovsky,,S. I., and Gortner, R. A. Ind. Eng. Chem. 25, No. 11: 1260-1265 (Nov. 1933).

2. Bradley, Linn, and McKeefe, E. R. Paper Trade Jour. 88, No. 8: 131-133(Feb. 21, 1929).

3. Bray, M. W., and Eastwood, P. R. Paper Trade Jour. 90, No. 25: 57-60(June 19, 1930).

4. Bray, M. Vv., and Eastwood, P. R. Paper Trade Jour. 93, No. 17: 38-42(Oct. 22, 1931).

5. Chidester, G. H., and Billington, P.S. Paper Trade Jour. 104, No. 6: 39-42(Feb. 11, 1937).

6. Chidester, G. H., and McGovern, J. N. Paper Trade Jour, 108, No. 6: 31-32(Feb. 9, 1939).

7. Clark, J. D. Paper Trade Jour. ' 83, No. 22: 43-45 (Nov. 25, 1926).8. Cross, C. F. British Patent 4984 (1880).9. Cross, C. F., and Bevan, E. J. Forestry Exhibition Re ports, Edinburgh (1886)

No.20(in CrossecBevans,Cellulose,Longmans,Greene&Co.,Ne w York, p.209) (1903).10. Cross and Bevan (Cross, C. F., Bevan, E. J., and Beadle, C.), Cellulose,

Longmans, Greene & Co., New York, p. 98, 210 (1903).11. Drewsen, P. Paper Trade Jour. 83, No. 24: 41-42 (Dec. 8, 1926).12. Haffner, L. C„ and Kobe, K. A., Paper Trade Jour. 111, No. 9: 93-98 (Aug.

29, 1940).13. Hausen, J. Paper Trade Jour. 84; No. 9: 51-60 (Mar. 3, 1927).14. Kobe, K. A., and Hanson, John M. Paper Trade Jour. 117, No. 2: 25-26

(July 8, 1943).15. Murdock, H. R. Paper Trade Jour. 124, No. 4: 51-52 (Jan. 23, 1947).16. Rawling, F. G., and Staidl, J. A. Paper Trade Jour. 81, No. 8: 49-51

(Aug. 20, 1925).17. Rue, J. D. Paper Trade Jour. 81, No. 16: 54-56 (Oct. 15, 1925).18. Schellhorn, F. S. Paper Trade Jour. 119, No. 23: 39-46*(Dece 7, 1944).19. Sutermeister, Edwin. Chemistry of Pulp and Paper Making, 3rd edition,

New York, Wiley (1941).20. Wells, B. D. Paper Trade Jour. 119, No. 21: 107-108 (Nov. 23, 1944).

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Page 13: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

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Page 14: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

Table 3.--Comparison of calcium acid sulfite, sodium sulfite, and sulfate pulpsfrom black spruce

: Acid : Sodium,: Sodium : Sul-,Type of pulp •sulfitel:sulfiteS:sulfite2: fate

: •. .

Total yield percent: 50.2 : 42.5 : 43.2 • 49.8

Screenings percent: .5 : .9 : 3.2 .2. :

Permanganate number 15.0 : 16.5 : 22.8 : 22.0

60 : 54Color percent blue on Ives photometer: : 52 31

Chemical composition: :.•. : .

Lignin. percent: 1.1 : 1.6 : , 3.8 : 4.2

Cross and Bevan cellulose percent: 93.1 : 93.6 : 91.4 : 93.5Alpha cellulose .percent: 76.6 : 78.3 : 75.8 • 75.9Total pentosans percent: 6.0 : 9.5 : 9.7 : 9.8

Solubility in 1 percent: :

caustic soda percent: 8.7 : 4.3 • 3.8

Pulp strength -- 25x40-500 ream:

Bursting strength at 800 cc. 5 • : : :

pts. per lb. per ream: 1.10 : 1.86 : 1.78 : 1.59•

Bursting strength at 550 cc. • : : :

pts. per lb. per ream: 1.22 : 1.97 : 1.92 : 1.75

Tearing strength at 800 cc. • : •. :

gm. per lb. per ream: 1.22 : 1.93 : 1.62 : 1.78

Tearing strength at 550 cc. • : : :

gm. per lb. per ream: .86 : . 1.48 : 1.18 : 1.36

Tensile strength at 800 cc. •• •

lb. per sq. in.: 8,800 : 9,500 : 8,800 : 9,350•

Tensile strength at 550 cc lb. per sq. in.: 11,300 : 12,200 : 12,650 : 12,650

at 800 cc. double folds: 450 : 1,200 : 1,045 : 1,300

Folding endurance at' 50 cc. .double folds: 775 : 1,300 : 1,200 : 1,300

Folding endurance

1Digestions 5005, 5006.

?Digestions 5028, 5030, 504 1 5037, 5038,5039, 5042, 5043, 5044, 5045.

Report No. 81728

)3 Digestions 5029, 5031.

IlDi gestions 2607, 2614, 2646.5Schopper-Riegler freeness.6Schopper instrument used.

Page 15: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

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Page 16: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

Table 5.--Experimental conditions and yields for neutral sodium sulfitedigestions of jack pine

Diges-: Impregnation conditions) : Cooking conditions : Total : Yield

tion : : :digestion: of

number: Liquor -

. Chemicals :Time at : Pres- : Spent : time : pulp

: concentration : absorbed : 170° C.: sureg: liquor:

: .4. :-. : : : : . :

:Sodium :Sodium :Sodium :Sodium : : :Sodium :

:sulfite:bicar- isulfite:bicar- : : :sulfite:

bonate: : bonate:

:Gm. per:Gm. per:Gm. per:Gm. per: Hours :Lb. per:Gm. per: Hours :Percent

liter : liter : liter : liter : : sq.in.: liter : :--___ ,

5244 : 148.5 : 30.8: 43.3 : 10.0. 47.0 : 148 : 24.2 : 10.0 : 48.4: . : • •. : . •

5241 : 141.3 : 34.4 : 35.5 : 8.4 : 10.2 : 120 : 24.0 : 13.2 : 62.1

5245 : 121.1 : 30.9 : 27.3 : 8.4 : 6.0 : 121 : 26.8 : 9.2 : 69.6

5242 : 100.0. 25.0. 19.9 : 5.6 : 3.0 : 123 : 25.7 : 6.2 : 77.4

5258-59: 89.3 : 22.7 : 16.9 : 5.0 : 3.5 : 128 : 13.8 : 6.7 : 78.0

-Impregnation at 120° C. for 1 hour for all digestions.

4ressure not relieved.

3.180 C.

a

Report No. 81728

Page 17: SOME EXPERIMENTS IN SODIUM SULFITE !PULPING

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