Title of Invention

A METHOD OF REDUCING THE RESIN CONTENT OF CHEMICAL PUMPS

Abstract The invention relates to a method of reducing the resin content of chemical pulps comprising heating wood chips to an aqueous alkaline medium in the presence of an effective deresinating amount of an alkyl alcohol alkoxylate of formula RO[ (CH2 CHCH3 O)x (CH2 CH2 O)y] M wherein R is C8 - C22 alkyl; x is 1- 20, y is 20-80 and M is H or an alkali metal.
Full Text

TECHNICAL FIELD
This invention relates to the chemical processing of wood pulps to reduce resin
content. More particularly, this invention is the use of alkyl alcohol alkoxylate
surfactants in kraft and sulfite cooking processes.
BACKGROUND OF THE INVENTION
In the pulping process, delignification is the primary reaction that allows wood
fibers to be separated from one another. Various mechanical and chemical methods are
used to effect this separation, but the most widely used technique is known as kraft or
sulfite process, since it produces pulp which gives high strength and good aging
properties to paper products.
In the kraft process, a cooking liquor (white liquor) of sodium hydroxide and
sodium sulfite is used to extract the lignin from wood. The process of extraction or
delignification is carried out in digesters, either batch or continuous. The pH in the
digester is generally between about 11 and about 14.
The liquor temperature is maintained between about 150 to about 175 ° C. A
period of from about 2 to about 3 hours is usually required for complete digestion. The
pulp is then washed before being further treatment such as bleaching prior to
manufacture of paper products.
Cooking liquor penetration of wood chips is vital to the success of the pulping
process. Pulp uniformity correlates directly with the ease of paper manufacturing
operations and quality of end products. Adequate movement of cooking liquor into the
wood is an essential first step in the pulping process. Removal of sufficient lignin for
fiber liberation requires the penetration and diffusion of pulping liquor into the chip and
then uniform distribution throughout the wood.

The two mechanisms that transport cooking chemicals into wood are
penetration and diffusion. Penetration is the flow of cooking liquor into wood pores,
while diffusion is the transport of dissolved chemicals as a result of a concentration
gradient.
In kraft digesters, nonuniformity results from different wood species, chip size,
chip age, errors in determining chip moisture content and pulping conditions. If the
chips are too thick, a less homogenous pulp is produced because the alkali in the chip is
consumed faster than it can be replaced by diffusion. Thus, the outer fibers are
extensively delignified before the inner core has had an opportunity to react. The
thickness of chips is always variable on a commercial scale. Deficient penetration
during cooking results in higher screen rejects and shives in the final pulp, a high lignin
content at a given yield, and inferior bleachability and end-use properties.
Nonuniform pulping can also occur in chips due to the interference of resin
content. The resin in wood is primarily located in the parenchyma cells and lumen.
The intact cell walls effectively protect the resin from contact with cooking chemicals.
Digestion and deresination can be considered to occur in the following manner:
1) Wetting of wood chips and resin by an aqueous alkaline fluid;
2) Penetration of the wood chips by this fluid;
3) Break-up resin and fatty acid aggregates and defibering of the wood chips
promoted by invasion of aqueous alkaline fluid into the chip flow channels; and
4) Stabilizing dispersed resin particles thus reducing their redeposition onto
cellulose fibers.
Surfactants can aid the above steps of the process through different mechanisms
such as wetting, emulsifying, and dispersing these resinous materials into and out of
wood structure. This results in a lower pulp resin content after cooking and washing
stages. For dissolving grade pulps, it is necessary to reduce the pulp resin content to
very low levels to prevent adverse effects of resin on acetate and viscose properties. In
papermaking pulps, these extractives, when liberated during the processing of the wood

chips to pulp and paper products, can cause troublesome pitch deposits on mill
equipment, press picking and off quality production. Hence, effective pulp deresination
aids can be useful in the manufacture of paper pulps as well as dissolving pulps.

U.S. Patent No. 5,728,265 discloses the use of alkoxylated branched and
unbranched aliphatic alcohols having 3 to 22 carbon atoms as chip penetrants.
SUMMARY OF THE INVENTION
This invention is a method of reducing the resin content of chemical pulps
comprising heating wood chips in an aqueous alkaline medium in the presence of an
effective deresinating amount of an alkyl alcohol alkoxylate of formula
RO[(CH2CHCH3O)x(CH2CH2O)y]M wherein R is C4 to C40 alkyl; x is 1-50; y is 0-100
and M is H or an alkali metal.
In another aspect, this invention is a cooking liquor comprising sodium
hydroxide and sodium sulfite and an alkyl alcohol alkoxylate of formula
RO[(CH2CHCH3O)x(CH2CH2O)y]M wherein R is C4 to C40 alkyl; x is 1-50; y is 0-100
and M is H or an alkali metal.
In another aspect, this invention is a deresinated pulp prepared by heating wood
chips in an aqueous alkaline medium in the presence of an effective deresinating
amount of an alkyl alcohol alkoxylate of formula RO[(CH2CHCH3O)x(CH2CH2O)y]M
wherein R is C4 to C40 alkyl; x is 1-50; y is 0-100 and M is H or an alkali metal.
DETAILED DESCRIPTION OF THE INVENTION
"Alkyl alcohol" means compound or mixture of compounds of formula ROH
where R is a straight or branched C4-C40 alkyl group.
"Hydroxide base" means the hydroxide (OH) salts of alkali metals such as
sodium, potassium, calcium, magnesium lithium, and the like.
"White liquor" means an aqueous mixture of alkali metal hydroxide and a
sulfite with or without further additives and in concentrations well known in the art.
The Kappa number, which is directly proportional to the amount of lignin remaining in

the pulp, is the volume (in milliliters) of 0.1 N potassium permanganate solution
consumed by one gram of moisture-free pulp under the conditions specified in TAPPI
method T 236 cm-85.
The alkyl alcohol alkoxylates of this invention have formula
RO[(CH2CHCH3O)x(CH2CH2O)y]M wherein R is C4 to C40 alkyl; x is 1-50; y is 0-50
and M is H or an alkali metal.
The alkyl alcohol alkoxylates are prepared by heating a C4-C40 alkyl alcohol, or
mixture of C4-C40 alkyl alcohols, both designated herein as ROH, with propylene oxide,
and optionally ethylene oxide in the presence of a hydroxide base. Preferably the
reaction is conducted at a temperature of about 150 °C in a pressure vessel at a pressure
of about 50 to about 75 psi. The resulting alkoxylate may be either left in salt form or
neutralized with acid.
The ethylene oxide and propylene oxide may be added in random or block
fashion. "Block polymer" means the polymer resulting from block addition of the
propylene oxide and ethylene oxide. "Hetero polymer" means the polymer resulting
from random addition of the propylene oxide and ethylene oxide.
Random addition of ethylene oxide and propylene oxide involves both
components being added to the alcohol simultaneously, such that the rate of addition to
the alcohol is controlled by their relative amounts and reaction rates. Thus, in the case
of random addition, it is understood the above formula is not a structural formula but
rather is representative only of the molar amounts, x and y, of ethylene oxide and
propylene oxide that are added to the alcohol ROH.
In the case of block addition, either the ethylene oxide or propylene oxide is
added first to the alcohol and allowed to react. The other component is then added and
allowed to react. In the case of block addition, the above formula is representative of
the structure of the alkoxylated alcohol, except that the (C2H4O)X and (C3H6O)y groups
may be reversed depending on whether the propylene oxide or ethylene oxide is added
first. The resulting polymer is a highly water soluble solid.
In a preferred aspect of this invention, M is H.

In another preferred aspect, M is K.
In another preferred aspect, R is C8-C22 alkyl.
In another preferred aspect, R is C16 alkyl.
In another preferred aspect, x is 1-20.
In another preferred aspect y is 20-80.
In another preferred aspect, x is 1-20, y is 20-80 and X is H.
In another preferred aspect, the alkyl alcohol alkoxylate is a block polymer.
In another preferred aspect, the alkyl alcohol alkoxylate is a hetero polymer.
The method of this invention comprises contacting wood chips and the like with
a digester aid which is a liquid mixture comprised of white liquor containing at least
one alkyl alcohol alkoxylate surfactant as described herein to obtain pulp for producing
paper. The surfactant concentration in the white liquor and the contact time with the
pulp chips are each adjusted such that resinous components are extracted from the pulp
without substantial degradation of cellulose. After contacting at least a portion of the
wood chips with the digester aid, the combination is heated to a digestion temperature
typically above about 150 °C. The heating is also referred to as cooking.
The alkyl alcohol alkoxylate surfactant is preferably diluted with water and
added as an aqueous solution to the white liquor after the liquor is diluted to a strength
appropriate for the Kraft cook. The aqueous alkyl alcohol surfactant composition can
also be added to a mixture of white and black liquor or black liquor only, or it can be
used in treating the wood chips prior to adding the wood chips to the cooking liquor.
After the wood has been digested to form a pulp slurry according to the present
invention, and washed to remove the inorganics and dissolved organics, the pulp slurry
is then provided to a papermaking machine. Paper may then be produced from the pulp
slurry according to known procedures of papermaking. Although the specific
percentages and process parameters described herein are preferred, other percentages
and parameters may be utilized.

In a preferred aspect, the cooking is done at a temperature of about 150 °C to
about 175 °C.
In another preferred aspect, the cooking is done in the presence of about 0.5 to
about 2 pounds per ton of alkyl alcohol alkoxylate on an oven dried chip basis.
The foregoing may be better understood by reference to the following examples,
which are presented for purposes of illustration and are not intended to limit the scope
of this invention.
Example 1
Pulping Studies
Pulping studies are carried out in a Lorentzen & Wettre autoclave digester
consisting of eight autoclaves (0.5 liter each) rotating in a heated glycol bath. In these
experiments, a known amount of kraft cooking liquor (sodium hydroxide and sodium
sulfite) is added into the wood chips to achieve the desired degree of pulp
delignification. A 5% stock solution of each alkyl alcohol alkoxylate surfactant is
prepared in a 100 ml volumetric flask. The surfactant charge is tested at a constant
charge of 0.05% (o.d. chips). The surfactant solution is added to the kraft cooking
liquor and thoroughly mixed before transferring into the autoclaves. A control
experiment is also run simultaneously in each set.
Each of the autoclaves is charged with the wood chips and liquor, sealed and
placed in the oil bath. The initial temperature of the oil bath is 50 °C. The temperature
is then ramped up and held at 170 °C for 1-3 hours to obtain the desired level of
delignification. During the cook, the autoclaves rotate end-over-end to facilitate
mixing and uniform heat transfer.
At the conclusion of the cook, the autoclaves are removed from the oil bath and
the reaction is quenched by cooling the autoclaves to 40 °C for 10 minutes. The
contents of the autoclaves are then disintegrated in a Waring blender for 2 minutes.
The resulting pulp is extensively washed over a cheese cloth in a Buchner funnel and
screened on a Voith flat screen with 0.20 mm slots. After screening, the rejects (un

cooked material), kappa number (amount of residual lignin in the pulp), deresination
(residual extractives in the pulp) and black liquor residual active alkali are determined.
The resin content of the chemical pulp is significantly reduced (65-70%
deresination) when cooked in the presence of the alkyl alcohol alkoxylate surfactant of
this invention. Furthermore, compared with other chemistries used commercially for
deresination, the alkyl alcohol alkoxylate surfactant provides up to three fold higher
deresination efficiency, resulting in improved deresination at substantially lower
additive levels (0.5-1 lb/ton of pulp) compared to the currently used conventional
chemistries (2-3 lb/ton of pulp).
Although this invention has been described in detail for the purpose of
illustration, it is to be understood that such detail is solely for that purpose and that
numerous modifications, alterations and changes can be made therein by those skilled
in the art without departing from the spirit and scope of the invention except as it may
be limited by the claims. All changes which come within the meaning and range of
equivalency of the claims are to be embraced within their scope.

WE CLAIM
1. A method of reducing the resin content of chemical pulps comprising
heating wood chips to an aqueous alkaline medium in the presence of an
effective deresinating amount of an alkyl alcohol alkoxylate of formula RO[
(CH2 CHCH3 O)x (CH2 CH2 O)y] M wherein R is C8 - C22 alkyl; x is 1-20, y is
20-80 and M is H or an alkali metal.
2. The method as claimed in claim 1 wherein M is H.
3. The method as claimed in claim 1 wherein M is K.
4. The method as claimed in claim 1 wherein R is O16 alkyl.
5. The method as claimed in claim 1 wherein the alkyl alcohol alkoxylate is a
block polymer.
6. The method as claimed in claim 1 wherein the alkyl alcohol alkoxylate is a
hetero polymer.
7. The method as claimed in claim 1 wherein the heating is done at a
temperature of 150°C to 175°C.
8. The method as clamed in claim 1 wherein heating is done in the presence
of 0.5 to 2 pounds per ton of alkyl alcohol alkoxylate on an oven dried
chip basis.

9. A cooking liquor comprising sodium hydroxide and sodium sulfite and the
alkyl alcohol alkoxylate as claimed in claim 1.



ABSTRACT

TITLE "A METHOD OF REDUCING THE RESIN CONTENT OF CHEMICAL PULPS"
The invention relates to a method of reducing the resin content of chemical
pulps comprising heating wood chips to an aqueous alkaline medium in the
presence of an effective deresinating amount of an alkyl alcohol alkoxylate of
formula RO[ (CH2 CHCH3 O)x (CH2 CH2 O)y] M wherein R is C8 - C22 alkyl; x is 1-
20, y is 20-80 and M is H or an alkali metal.

Documents:

250-KOLNP-2005-(12-08-2013)-CORRESPONDENCE.pdf

250-KOLNP-2005-ABSTRACT.pdf

250-KOLNP-2005-CLAIMS.pdf

250-KOLNP-2005-CORRESPONDENCE.pdf

250-KOLNP-2005-DESCRIPTION (COMPLETE).pdf

250-KOLNP-2005-EXAMINATION REPORT.pdf

250-KOLNP-2005-FORM 1.pdf

250-KOLNP-2005-FORM 18.pdf

250-KOLNP-2005-FORM 2.pdf

250-KOLNP-2005-FORM 26.pdf

250-KOLNP-2005-FORM 3.pdf

250-KOLNP-2005-OTHERS.pdf

250-KOLNP-2005-REPLY TO EXAMINATION REPORT.pdf

250-KOLNP-2005-SPECIFICATION.pdf


Patent Number 261094
Indian Patent Application Number 250/KOLNP/2005
PG Journal Number 23/2014
Publication Date 06-Jun-2014
Grant Date 03-Jun-2014
Date of Filing 23-Feb-2005
Name of Patentee NALCO COMPANY
Applicant Address 1601 DIEHL ROAD, NAPERVILLE, ILLINOIS 60563-1198, UNITED STATES OF AMERICA
Inventors:
# Inventor's Name Inventor's Address
1 DUGGIRALA, PRASAD, Y 2403 SISTERS COURT, NAPERVILLE, IL 60564, USA
2 SVARZ, JAMES J. 1119 WICKHAM COURT, NAPERVILLE, IL 60564, USA
PCT International Classification Number D21C 3/02
PCT International Application Number PCT/US2003/011065
PCT International Filing date 2003-04-10
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 10/201,332 2002-07-23 U.S.A.