UTILIZATION OF WHITE-POCKET DOUGLAS-FIR:
PULPING AND CHEMICAL CONVERSION
November 1953
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Nee Mil
APR 201954
UNITED STATES WEPARTMENT OF AGRICULTURE
LLFOREST SERVICE
L)/FOREST PRODUCTS LABORATOR Y
Madison 5, Wisconsin
In Cooperation with the University of Wisconsin
UTILIZATION OF WHITE-POCKET DOUGLAS-FIRS
PULPING AND CHEMICAL CONVERSION
By
J. S. MARTIN, Chemical Engineer
R. M. KINGSBURY, Chemist
J. N. McGOVERN, Chemical Engineer
and
R. A. LLOYD, Chemical Engineer
Forest Products Laboratory? . Forest Service
U. S. Department of Agriculture
Summary
White-pocket Douglas-fir was tested for its suitability for the production
of kraft, semichemical, and rayon grades of pulp and for the production of
wood sugar. The experiments showed that a considerable amount of white
pocket can be present without loss in the yield of kraft pulp and without
a great loss in the strength of the pulp. Strength losses can be minimized
by mixing the white-pocket Douglas-fir with the sound wood of normally
associated softwood species.
White pocket showed no effect on the yield of semichemical pulps made under
the mildest conditions and produced in the highest yields, but when stronger
conditions were used to give lower yields, the wood with white pocket gave
less pulp than did the sound wood.
Corrugating and liner boards of satisfactory quality were made from both
the neutral sulfite and the sulfate types of semichemical pulp, but the
latter proved to be more economical from the standpoint of chemical requirements. Douglas-fir in the intermediate stage of white pocket was made into
textile grade rayon pulp by the prehydrolysis-sulfate process.
No significant difference was noticed between the behavior of Douglas-fir
with or without white pocket in the production of wood sugar, except that
some modification of procedure would be indicated if advanced white pocket
were present in large amounts. The yield of sugar from the white-pocket
material was comparable to that from the normal wood.
Maintained at Madison, Wis., in cooperation with the University of
Wisconsin.
Rept, No. 1961
Agriculture-Madison
Introduction
In the Douglas-fir region of the Northwest, a large amount of material is
left on the ground after logging. These defective logs, broken chunks, and
unmerchantable tops are left in the woods because there is no market at
present for this type of wood. Much of the defective material is caused by
an organism, Fomes pini, that attacks the heartwood of Douglas-fir and leaves
it in a pitted or white-pocket condition from which it derives its common
name of "white pocket."
Losses from Fomes pini in old-growth vary by stands and range from less than
5 percent to more than 60 percent of the gross volume in board feet. The
higher losses are found in'the Douglas-fir stands in the southern half of
Oregon and northwestern California. 2– Profitable utilization of these waste
materials is necessary to attain maximum returns from extensive forest stands
of this type.
The Forest Products Laboratory has conducted experiments to test the
possibility of usin g white-pocket wood for lumber, veneer, pulp, and for
other mechanical uses. This report summarizes experiments to determine
the suitability of white-pocket old-growth Douglas-fir for the production
of kraft, semichemical, and rayon grades of pulp, and for conversion into
wood,: sugar by hydrolysis.
Production of Paper-Grade Sulfate Pulp
'95
.4 44
Comparison of Sound and Decayed Woods
A description of the six samples of Douglas-fir used in the sulfate pulping
tests for the production of strong (kraft) paper-grade pulp is given in
table 1. They consisted of sound material from whole logs, sound material
adjfgent to white-pocket material, and white-pocket material in various
stages of development ranging from an incipient stage to an , extremely advanced stage.
The-density values are important factors in determining the yield of pulp
obtainable from a unit volume of wood and the weight of chips that can be
charged to a digester. The density values'of the samples containing the
incipient,firm, and advanced stages were similar to those of the sound wood
(lot 1). Chemical analysis indicated that the sound wood surrounding whitepocket areas (lot 1A) and the woods containing incipient, firm, and advanced
white pocket all had essentially the same chemical composition, but they all
had definitely lower holoceilulose and pentosan content and a little lower
alpha-cellulose content than did the sound wood of lot 1. Judged by the
chemical composition and the density values of these samples, the extent
4ftce, J. S., and Wagg, J. W. Conk Rot of Old-Growth Douglas-fir in
Western Oregon. Oregon Forest Products Laboratory Bull. 4, June 1953.
Rept. No. 1961
-2-
of the deterioration was less than that indicated by their visual appearance
and, fortunately, less than that required to interfere with normal reactions
with sulfate cooking liquors.
The sample with extreme white pocket (lot 5) was honeycombed and contained
a fairly uniform distribution of the white pocket, Its low density of 14.7
pounds per cubic foot was about one-half that of the other samples tested.
Chemical analysis showed it to have a higher alkali solubility and lower
alpha cellulose and lignin content than did the sound wood. In general, the
chemical analysis indicated that the organism destroyed all constituents with
about equal intensity.
Sulfate Pulping for Paper-Grade Pulp
The pulping conditions were established by a series of experiments on the
sound material from lot 1. The optimum conditions arrived at were:
Chemicals charged per 100 pounds of moisture-free wood:
20.0 pounds
Sodium hydroxide and sodium sulfide 15,6 pounds
Calculated as sodium oxide 39.1 grams
Initial chemical concentration per liter
30.0
percent
Sulfidity (based on active alkali)... 4.0
Liquor-wood ratio 170°
C.
Maximum temperature 1.5
hours
From room temperature to maximum temperature
1.5 hours
At maximum temperature ... Under these conditions, the amount of chemical consumed for all samples was
about 85 percent of the total charged. The amounts charged and consumed are
comparable with general mill practice for the production of kraft pulp.
The results of pulping the white-pocket fir indicated that all lots were as
satisfactorily reduced as the sound wood of lot 1. Except for the wood
with extreme white pocket (lot 5),the yields of screened pulp (including the
sound wood samples) were within a narrow range of 43.5 to 45.1 percent and
not in order with the observed degree of White pocket.
The yield of screened pulp from the wood with extreme white pocket was 41.8
percent on a weight basis, which was only a little lower than that from the
sound wood. Because of the low density of this sample, however, the yield
was 50 percent less than that from the sound wood on a volume basis. This
type of material would be difficult to handle in a mill wood room because of
its friability.
The moisture content of the freshly chipped wood ready for pulping was much
lower for the several lots of wood containing white pocket (22-23 percent)
than for the two lots of sound material (33-38 percent). Presuming that
this is a natural situation, and since dry chips pack more loosely than moist
chips, it appears that the only Changes necessary for satisfactory pulping
of the white-pocket material would be in the adjustment of the chemical
Rept. No. 1961
-3-
charge to compensate for the lower weight of wood substance in the digester..
This adjustment is necessary so as not to overcook the white-pocket material
to the detriment of pulp yield and quality.
The pulps from the white-pocket samples appeared to bleach easier than those
from the sound woods.
The results indicate that the following strength properties might be
expected in kraft pulps made from the various materials:
(a) Pulp made from sound old-growth Douglas-fir wood
slightly lower in bursting strength and significantly
strength than southern pine sulfate pul p and probably
be used for purposes now served by southern pine pulp
bursting strength or a fine-fibered pulp are needed.
will probably be
higher in tearing
could be expected to
except where maximum
(b) The pulp obtained from sound -flood surrounding white-pocket areas has
about the same bursting strength as that from wood containing incipient
white pocket, Its tearing strength is about equal to that normally expected
from sound Douglas-fir.
(c)
Sulfate pulps made from Douglas-fir
be lower in bursting strength than pulps
to the observed amount of white pocket.
made from wood containing advanced white
percent of that of southern pine pulp,
wood containing white-pocket will
made from sound wood in proportion
The bursting strength of the pulp'
pocket would probably be about 75
(d) The tearing strength of the pulps from the white-pocket woods (except
for lot 5) may be higher than that of pulp from the sound Douglas-fir, while
the tearing strength of lot 5 may be a little lower than that of southern
pine kraft.
Values for the relative bursting and tearing strength of the various Douglasfir sulfate pulps and southern pine kraft are given in table 2.
It is evident that a considerable amount of white pocket can be present in
Douglas-fir without loss in yield of pulp and without a great loss in
strength. The lowered strength can be compensated for by mixing pulp from
the white-pocket material with pulp from sound wood from other softwoods
normally associated with Douglas-fir, For example, the following mixture,
which simulates that naturally occurring in some stands, was found to give
a yield of about 46 percent of screened pulp and to have good bursting
strength and tearing strength (see table 2):
Douglas-fir from lots 1 and IA Douglas-fir . from lot 2 Douglas-fir from lots 3 and 4 Mountain hemlock, noble fir and
lodgepole pine Rept. No. 1961 -4-
By weight
25 percent of each
10 percent
5 percent of each
10 percent of each
Production of Semichemical Pulps
and Liner and Corrugating Boards
Semichemical pulps made by partial chemical pulping followed by mechanical
fiberizing are produced commercially in yields of 65 to 80 percent in contrast
with the range of 45 to 50 percent for chemical pulps. The purpose of this
process is to utilize wood as efficiently as possible and to take advantage
of certain properties inherent in this type of pulp. Semichemical pulps are
now made mostly from hardwoods for use in container board, particularly corrugating medium, and, after bleaching, in fine papers. There is a small amount
of softwood semichemical pulp made, and experimental investigations have
shown promising indications that the use of softwoods for this purpose can
be expanded. The semichemical process, therefore, was applied to the
Douglas-fir of lots 1, 3, and 4, respectively (see table 1). Both the
neutral sulfite and sulfate semichemical processes were used, and selected
pulps were made into standard-weight corrugating and liner boards, which
are the components of the widely used corrugated fiberboard.
Neutral Sulfite Semichemical Pulps and Boards
Douglas-fir was readily pulped with sodium sulfite solution buffered with
sodium bicarbonate as the pulping reagent. Pulps were made in yields of 53
to 77 percent. The amount of sodium sulfite, based on the wood, varied from
about 28 to 17 percent,and the time at the cooking temperature of 175° C.
varied from about 7 hours to 1 hour, respectively, for this yield range. The
amount of sodium bicarbonate used to maintain a slightly alkaline condition
was about 5 percent of the wood. The pulps made under the mildest conditions
and produced in the highest yields showed no effect of white pocket on yield,
but with stronger conditions used to give lower yields the wood with white
pocket gave about 5 percent less pulp than did the sound wood. The pulping
of Douglas-fir with the neutral sulfite reagent required large amounts of
cooking chemical and fiberizing energy. For example, 1 ton of pulp (air-dry
basis) made in a yield of 76 percent had a chemical requirement of 460 pounds
of sodium carbonate and 105 pounds of sulfur and an energy requirement of
about 40 horsepower-days per ton of air-dry pulp. (This is in contrast with
average requirements of about 250 pounds of soda ash, 60 pounds of sulfur,
and 15 horsepower-days per ton of hardwood semichemical pulp.) The chemical
requirements increased and the energy requirement decreased with decrease in
yield. It would probably be uneconomical to make pulp in yields below 70
percent, if the chemicals were not recovered.
Pulp strength -was not affected by white pocket regardless of yield; in fact,
the pulps from the white-pocket materials actually were stronger in these
few experiments than those from the sound wood, although this would not be
expected in the average from a large number of tests or in mill production.
The pulps made in yields near 75 percent had bursting- and tearing-strength
values about one-half those of the kraft pulps from the sound Douglas-fir.
These pulps were also much lower in folding endurance. Pulp strength
increased with decrease in yield to the extent that pulps made in yields
Rept. No. 1961
-5-
of 53 to 57 percent had about Eto percent of the strength of the kraft pulp
from sound wood as shown in table 2.
Corrugating boards were made from pulps produced in yields near 75 percent
from the wood of lots 1 and 3. These boards were equal in properties,: such
as bursting, tearing, and folding strength, to the strongest commercial
corrugating boards, but were somewhat lower in stiffness as measured by flatcrush resistance after corrugating. (The latter is probably the most
important criterion of the quality of corrugating board,) As far as the
usual strength properties are concerned, Douglas-fir neutral sulfite pulps
could be made in yields as high as 80 percent, but they apparently would
need to be blended' with other pulps that would impart stiffness to the
corrugating board,' or a stiffening agent would need'to be added.
Liner boards were made from all of the semichemical pulps from the sound
woods and from those containing white pocket.. Although the boards from the
lot 3 wood were somewhat lower in strength than the others, it was not believed that the condition of the'wood had 'a serious effect on the quality
of the liner boards within the range of conditions studied. The boards from
the pulps made in yields near 75 percent approached the bursting-strength
requirement for a test liner, which is a minimum of 100 pounds per square
inch, Mullen. They had a high resistance to tearing, but were somewhat low
in folding endurance, a possible indication of substandard bending properties.
The boards made from the lower yield pulps generally' met the test liner
specification for bursting strength and showed promise for use for this
purpose. The -highest yield pulps would probably have considerable use in
boards that do not require the highest strength properties, and if blended
with strong kraft pulps from Douglas-fir or other softwoods, they might be
used in the stronger boards.
Sulfate Semi-chemical Pulps and
Boards
Douglas-fir was also readily made into semichemical pulps in yields Hof 55 to
75 percent using a sulfate pulping liquor. This range of yields was obtained
by reducing the total chemical used from 15 to 8.75 percent, and the cooking
time at 170° C. from 1-.5 to 0 hour in comparison with 20 percent chemical and
1.5 hours-at 170° C. for the_ kraft pulps. Thus, the sulfate semichemical
pulps, in contrast with the neutral sulfite type, had low, economical chemical requirements. At the highest yields, the presence of white pocket had no
effect on pulp yield, but at the lowest yields about 5 percent less pulp was
obtained under the same pulping conditions from the wood with advanced white
pocket than from the sound wood. The pulps made in the lowest yields from
the wood with advanced white pocket were also weaker in bursting strength by
25 percent than the corresponding pulp from the sound wood. Pulp strength
decreased in proceeding from the kraft pulp through to the pulps made in the
highest yield of 75 percent. At this high yield, the pulps had roughly 60
percent of the bursting and tearing strength of the kraft pulps and only about
10 p ercent of the folding endurance. (See table 2 for relative strength of
the kraft pulp.)
Rept. No. 1961
-6-
Corrugating boards were made from selected pulps covering the range of
yield and wood conditions. The boards made from the highest yield pulps,
although unaffected by the white pocket, tended to be low in strength, except in tearing resistance and in crush resistance of the corrugated board.
The results of these few tests were not promising for the commercial use
of high percentages of the highest yield sulfate semichemical pulps in
corrugating board. The corrugating boards made from the lower yield sulfate
semichemical pulps had good strength properties except for stiffness, which
was lower than desirable in comparison with the highest quality commercial
corrugating board. As with the neutral sulfite boards, some means of
stiffening would appear to be needed before these boards could compete
with boards made from conventional pulps.
The liner boards made from the strongest sulfate pulps, that is those made
in the high yield of 55 percent, had bursting-strength values of 75 and 90
pounds per square inch in boards made from wood with advanced white pocket
and from sound woods, respectively. Other strength properties were also
lower in boards made from wood containing white pocket. None met the bursting strength requirement of 100 pounds per square inch for test liner board
even though made in the relatively heavy weight of 47 pounds per 1,000
square feet, but they would be acceptable in other strength properties.
The liner boards made from pulps in the intermediate yield class of 63
percent were even lower in bursting strength. These pulps probably would
have limited possibilities if used independently of other stronger pulps.
The lower-yield sulfate semichemical pulps would be expected to be useful
in container liner boards not having the highest strength requirements and
they undoubtedly could be blended with strong kraft pulps for producing
higher quality container boards and other board products, as mentioned for
the neutral sulfite counterparts. Depending on quality requirements,
probably up to 50 percent of the wood with advanced white pocket could be
used in many high quality board products.
Production of Rayon-Grade Pulp
Wood Used
White-pocket Douglas-fir was tested as a source for viscose rayon pulp.
The wood had an intermediate stage of white pocket, as described by lot 3
in table 1.
In chemical composition, the wood was lower in alpha cellulose, the desirable
component for rayon-grade pulp, than sound Douglas-fir. It compared favorably to southern pine, which is used in the commercial production of this
kind of pulp. A notable characteristic of white-pocket Douglas-fir is the
low content of pentosan, an unwanted material in rayon-grade pulp. In the
sample of wood used in this work, the pentosan content was somewhat less
than half the amount found in southern pine. Test values for the wood are
given in table 3.
Rept. No. 1961
-7-
Pulping and Purification Treatments
Two purified pulps were prepared from the white-pocket Douglas-fir wood using
different pulping and purification treatments that were thought might produce
different physical characteristics in the cellulose as well as differences in
its chemical nature.
The wood Was.pulped by the prehydrolysis-sulfate process in which the chips
are cooked first with water or steam and then pulped by the usual sulfate
process. 34 the prehydrolysis step, acidic conditions are developed that
remove some of. the unwanted hemidellaese (including some of the pentosans)
and apparently renders most of the remaining portion susceptible to removal
in the sulfate pulping stage. Sulfate pulping without prehydrolysis does
not remove much of the pentosans, and it does not consistently produce
pulps that are satisfactorily reaCtive'(thetiS, will form easily filtrable
viscose solutions)' in the conversion to viscose rayon,
By using different amounts of chemical in the pulping stage, two unbleached
pulps were obtained that differed appreciably in disperse viscosity but were
nearly alike in other characteristics as shown in table 3. The first of these,
digestion 4038, was purified by sequential treatments with chlorine, sodium
hypochlorite, and sodium hydroxide solutions. Conditions in these treatments
were selected so that the disperse viscosity was reduced from 17.2 centipoises to the desired low level of 6 n 4 centipoises. More than 90 percent
of the decrease was achieved in the first two stages so as to permit removal
of undesired degradated products by the alkaline-extraction treatment.
The second unbleached pulp, digestion 4042, Was purified by sequential treatments with chlorine, sodium hydroxide solution, and sodium hypochlorite ,. These
treatments decreased the disperse viscosity from 10.1'centipoises to about 'the
same level as that of the first pulp, and again the conditions were such that
no measurable decrease in viscosity occurred after the alkaline-extraction
treatment.
Evaluation of
the Purified PulEs
A comparison of the composition of the 2 experimental pulps and 2 commercial
viscose pulps of tire-cord grade is given in table 3. As shown by these
data, the Douglas-fir pulps were equal in composition and in some respects
superior to domestic commercial viscose pulps used in tire-cord manufacture.
Viscose rayon yarns and tire cords were made from the experimental pulps in
an industrial laboratory.
The better tire cord, from the standpoint of
fatigue resistance, was obtained from the pulp (digestion 4038) in which the
viscosity was lowered more during its purification than the other. This
difference in fatigue resistance is evidence of differences in the physical
characteristics of the cellulose obtained by the two methods of preparation.
The fatigue resistance was about 20 percent below the resistance of tire-cord
rayon now made from commercial prehydrolysis-sulfate pulp.
However, the rayon yarns made from both pulps were adequate in strength for
textile grade. On the basis of chemical composition, they appeared to be
suitable for the explosives grade of cellulose nitrate.
Rept. No. 1961
-8-
Wood Sugar from White-Pocket Douglas-Fir
Studies on the chemical conversion of white-pocket Douglas-fir were
limited to the evaluation of its sugar-producing properties. To determine the potential sugar content of the material, a quantitative
saccharifiaation procedure was used, and the yield of sugar was determined by standard analytical methods. The fermentability of the sugars
produced was also determined. The potential sugar values were determined
for Douglas-fir containing no white pocket, light white pocket, and extensive white pocket (similar to that of lot 5). The data based on bark-free
wood are listed in table 4. Even though nearly half of the wood substance
has been destroyed in material containing extensive white pocket, the
potential sugar content based on the dry weight has not been seriously
changed. The total reducing sugar value has been affected somewhat more
than the fermentable sugar value, indicating a preferential removal of the
more easily hydrolyzable hemicellulose.
No significant difference was noticed between the behavior of Douglas-fir
with or without white pocket in the wood-hydrolysis pilot plant. If the
extensive white pocket material had been segregated and hydrolyzed separately,
however, it would be expected that this material would have behaved more
like sawdust than chips, and lower packing pressures would have had to be
used during loading to prevent overdensification of the bed. On passing
through the hog, the extensive white-pocket material broke up considerably
more than did the sound Douglas-fir. It was found that over 70 percent of
hogged light white-pocket Doug las-fir went through a 1/4-inch mesh, while
only 30 percent of sound material that had been similarly hogged went through
the 1/4-inch mesh screen.
In all of the hydrolysis runs on white-pocket Douglas-fir, the material used
represented a cross section of the white-pocket material received at this
Laboratory. Because of its similarity to Douglas-fir without white pocket,
Douglas-fir with white pocket was used as charge stock for much of our wood
hydrolysis development work on this species.- An operating procedure that
resulted from this research was used on 11 consecutive white-pocket hydrolysis
runs. The average yield for these runs was 39 percent, and the average sugar
concentration of the composite hydrolyzates was 5.4 percent. These figures
are comparable to the values that can be obtained by the same procedure
from Douglas-fir of low bark content. To obtain these yields the charge was
first steamed to 293° F., and dilute sulfuric acid at 293° F. was added at
such a rate as to give a water-to-wood ratio of 2.0 at the end of 30 minutes.
The water temperature was then raised to 343° F., and the water-to-wood
ratio was increased to 2.5 in 15 minutes. At this ratio, the charge was
substantially covered with a 0.7 percent sulfuric acid solution. Sugar
solution was then started off at such a rate as to maintain a high liquor
level in the vessel, and 0.6 percent acid liquor was pumped in at 10 percent
of the weight of dry charge per minute. The temperature was increased at a
constant rate to 365° F. in 15 minutes. These operating conditions consume
a quantity of acid equal to 6 percent of the charge and require a total pumping time of less than 2-1/2 hours to produce the sugar yield of 39 percent
and the concentration of 5.4 percent.
Rept. No. 1961
-9-
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Table 2.--Comparison of , strength of the experimental sulfate pulps
,with commercial southern pine sulfate pulps
Kind of sulfate pulp
: Bursting : Tearing
: strength : strength
.
;
: Percent : Percent
100
:
100
Sound wood from lot 1 95
:
120
Wood surrounding white pocket areas, lot lA 85
:
165
Stained mood with incipient white pocket, lot 2:
85
:
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80
:
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75
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Southern pine Douglas-fir:
Wood with firm or intermediate white pocket,
lot
3
Wood with advanced white pocket, lot 4 Wood
with extremely advanced white pocket,
lot 5 Mixture of species Rept. No. 1961
75
90
105
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wood
Potentiall
: Potential!,
: reducing : fermentable
sugar
sugar
:
Percent : Percent
58
Normal 67
White pocket, light 6657
White pocket, extensive..:
/Based on ovondry method.
Rept. No. 1961
62
56