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Patent 2111921 Summary

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(12) Patent Application: (11) CA 2111921
(54) English Title: FORMULATED COMPOSITION OF PULP DIGESTING ASSISTANT AGENT
(54) French Title: FORMULATION D'ACCELERATEUR DE DIGESTION DE PATE
Status: Deemed Abandoned and Beyond the Period of Reinstatement - Pending Response to Notice of Disregarded Communication
Bibliographic Data
(51) International Patent Classification (IPC):
  • D21C 03/00 (2006.01)
  • D21H 17/06 (2006.01)
(72) Inventors :
  • KUMAGAI, KENJI (Japan)
  • KURATA, NAOJI (Japan)
  • SHOJI, SCIJI (Japan)
  • BABA, RYUJI (Japan)
  • SUGITA, YOSHIO (Japan)
(73) Owners :
  • NIPPON SHOKUBAI CO., LTD.
  • NIHON JORYU KOGYO CO., LTD.
(71) Applicants :
  • NIPPON SHOKUBAI CO., LTD. (Japan)
  • NIHON JORYU KOGYO CO., LTD. (Japan)
(74) Agent: BORDEN LADNER GERVAIS LLP
(74) Associate agent:
(45) Issued:
(22) Filed Date: 1993-12-20
(41) Open to Public Inspection: 1994-06-22
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
4-340704 (Japan) 1992-12-21

Abstracts

English Abstract


ABSTRACT OF THE DISCLOSURE
A formulated pulp digesting assistant agent is
provided which allows particulate anthraquinone to be easily
dispersed and dissolved in the pulp digesting liquid and
precludes the harm otherwise done to the environmental
hygiene by the powder as when it is drifted in a wind. This
composition is obtained by mixing a particulate
anthraquinone having an average particle diameter of not
more than 10 µm and a maximum particle diameter of not more
than 30 µm, 0.1 to 2% by weight, based on the amount of the
particulate anthraquinone, of a nonionic surfactant mixture
comprising an alkylene oxide adduct of a secondary alcohol,
having an HLB value in the range of 12 to 16 and carbon
numbers from 10 to 16 and an alkylene oxide adduct of an
alkyl phenol having HLB value in the range of 12 to 16 and
an alkyl group having carbon numbers from 6 to 12 at a
weight ratio in the range of 5 : 1 to 1 : 5, and 5 to 30% by
weight based on the amount of the formulated pulp digesting
assistant agent of water and/or an alcohol having a
molecular weight of not more than 200.


Claims

Note: Claims are shown in the official language in which they were submitted.


THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A formulated pulp digesting assistant agent
which comprises a particulate anthraquinone of an average
particle diameter of not more than 10 µm and a maximum
particle diameter of not more than 30 µm, 0.1 to 2% by
weight, based on the amount of said particulate
anthraquinone, of a nonionic surfactant mixture comprising a
first nonionic surfactant of an HLB value of 12 to 16 formed
of a secondary alcohol having carbon numbers from 10 to 16
possessing an alkylene oxide adduct having 7 to 20 mols of
ethylene oxide added thereto and a second nonionic
surfactant of an HLB value of 12 to 16 formed of an alkyl
phenol having the alkyl group carbon numbers from 6 to 12
possessing an alkylene oxide adduct having 8 to 15 mols of
ethylene oxide added thereto, the weight ratio of said first
to said second nonionic surfactant being in the range of 5 :
1 to 1 : 5 and the total amount of said first and second
nonionic surfactants being in the range of 0.1 to 2% by
weight based on the amount of said particulate
anthraquinone, and 5 to 30% by weight, based on 100% by
weight of said formulated pulp digesting assistant agent, of
water and/or an alcohol of a molecular weight of not more
than 200.
2. An agent according to claim 1, wherein the
average HLB value of said mixture of first and second
nonionic surfactants is in the range of 13 to 15.
3. An agent according to claim 1, wherein the total
content of said water and/or alcohol having a molecular
weight of not more than 200 is in the range of 10 to 20% by
weight, based on 100% by weight of said formulated pulp
digesting assistant agent.
4. An agent according to claim 1, wherein the
number of mols of ethylene oxide added in said first
nonionic surfactant is in the range of 9 to 15 and the
number of mols of ethylene oxide added in said second
nonionic surfactant is in the range of 10 to 14.
-18-

5. An agent according to claim l, wherein the
weight ratio of said first nonionic surfactant to said
second nonionic surfactant is in the range of 3 : 1 to 1 :
3.
6. An agent according to claim 1, wherein the total
amount of said first and second nonionic surfactants to be
used is in the range of 0.2 to 1% by weight, based on the
amount of said particulate anthraquinone.
7. An agent according to claim 1, wherein said
alcohol is an alcohol having a molecular weight of not more
than 120.
8. An agent according to claim 1, wherein the
content of said water and/or alcohol is in the range of 10
to 20% by weight based on the amount of said formulated pulp
digesting assistant agent.
9. An agent according to claim 1, wherein the
average particle diameter of said particular anthraquinone
is not more than 10 µm and the maximum particle diameter
thereof is not more than 30 µm.
-19-

Description

Note: Descriptions are shown in the official language in which they were submitted.


FORMULATED COMPOSITION OF :
PULP DIGESTING ASSISTANT AGENT
BACKGROUND OF THE INVENTION
Field of the Invention:
This invention relates to a formulated composition
of a powdery pulp digesting assistant agent. More
particularly, it relates to a powdery readily dispersible
formulated composition of pulp digesting assistant agent
which comprises anthraquinone in a particulate form, two
10 kinds of speoific nonionic surfactants, water, and/or an
alcohol having a molecular weight of not more than 200 and
manifests a high digesting power.
Description of the Prior Art:
In recent years, it has been found that when
15 anthraquinones heretofore used prevalently in dyes and
pigments are used as a pulp digesting assistant agent or a
redox catalyst, they contribute in a great measure to ~;-
increase the speed of digestion, lower the temperature of
digestion and consequently save steam, economize chemical
20 agents to be used, shorten the time of digestion and
consequently improve the rate of operation, exalt the
quality of pulp, and increase the yield of pulp. As a
result, the anthraquinones have been finding growing utility
in the pulp digesting assistant agent.
The anthraquinones, however, are not soluble in -~
water. When powdery anthraquinone is added in its
unformulated form to a pulp digesting liquid, therefore, the
greater part of the powder floats on the surface of the
digesting liquid and a considerably long time is required
30 for the powder to be thoroughly dispersed and dissolved in
the digesting liquid. As a result, the powdery
anthraquinone is at a disadvantage in failing to manifest
amply the catalytic effect thereof because it is not fully
dispersed or dissolved in the pulp digesting liquid within -
~5 the ordinary digesting time.
As means to overcome the disadvantage, a method of
-1-
v- , ,, ' ~ ,,,' : ~ .

using tetrahydroanthraquinone of a reduced form as diluted
~ in an aqueous alkali solution has been available. This
j method indeed is fine in respect that
tetrahydroanthraquinone is quickly dispersed and dissolved
in the pulp digesting liquid. It is at a disadvantage,
however, in requiring the entire aqueous alkali solution of
tetrahydroanthraquinone to be covered with nitrogen gas
while in transit and in use. Because, this solution is
oxidized on exposure to the air, and entails separation of
10 crystals of anthraquinone. And the cost of transportation
is expensive, because this solution is in a dilute form.
As another means to overcome the problem, a method
which allows effective use of particulate anthraquinone in
the pulp digesting liquid by having a surfactant,
15 particularly an anionic surfactant, deposited on the
anthraquinone particles thereby facilitating the dispersion
and dissolution of the particulate anthraquinone in the pulp
digesting liquid is disclosed (JP-A-54-100,332). The method
which involves deposition of an anionic surfactant among
20 other surfactants, however, has the disadvantage that since
this deposition gives rise to a composition having the
particulate anthraquinone kneaded in a pasty form with a
~olution of the ionic surfactant, this composition not only
entails a high cost of transportation but also requires
25 consumption of the ionic surfactant in a large amount as
compared with the particulate anthraquinone. In the
detailed description of the invention which relates to the
method under discussion, a mention is made to the effect
that nonionic surfactants among other surfactants are not
30 fit for dispersion of particulate anthraquinone. From this
statement, it is inferred that even if an anionic surfactant
is managed to be uniformly mixed at its initial
concentration of 100% with particulate anthraquinone, the
resultant mixture placed in the pulp digesting liquid
35 induces the "phenomenon of gelation" which ought to be
justly called a peculiar disposition owned by the nonionic
~.',,,`"'.-', .'`,,,',,':'i".'

surfactant and, instead of fulfilling the function of a
surfactant, rather covers the surface of anthraquinone
particles with a jellylike coat and further obstructs
dispersion and dissolution of anthraquinone in the pulp
digesting liquid and, as a result, fails to produce any
appreciable effect in the pulp digestion.
Canadian Patent No. 1,140,706 also discloses a
method which similarly resorts to use of a surfactant. Even
when an anionic surfactant is used as taught in the detailed
10 description of the invention relating to this method, this
invention can be hardly called satisfactory because it still
entails the problem of unduly heavy consumption of the
anionic surfactant. Again in the case of this invention,
the working examples cited in the specification invariably
15 represent cases of using an anionic surfactant. No mention
is made anywhere of a nonionic surfactant regarding the
structure, composition, or mode of use. The nonionic -~
surfactants which have many problems yet to be solved as to
method of use and selection of species are not easily taken
~0 up as subjects of study. In the existing state of affairs,
no method has yet been found for effective use of a nonionic
surfactant as a digesting assistant agent.
No actual case of using a nonionic surfactant for
the purpose under discussion has been reported to date. No
25 report has yet been published in literature as to the
effectiveness of a nonionic surfactant in promoting
dispersion and dissolution of anthraquinone in the pulp
digesting liquid. Thi~ fact may well be regarded as
reflecting the fact that this effectiveness of a nonionic
30 surfactant has not been uncovered to date.
I An object of this invention, therefore, is to
provide a formulated pulp digesting assietant agent which
allows anthraquinone used in a powdery form to be easily
dispersed and dissolved in the pulp digesting liquid,
35 enables the anthraquinone to manifest thoroughly the effect
thereof as a redox catalyst and, at the same time, precludes

the harms which would be possibly done to the environmental
hygiene by particulate anthraquinone when this powder is
drifted in course of handling.
SUMMARY OF THE INVENTION
We have made a diligent study on formulated pulp
digesting assistant agent with a view to accomplishing the
object described above and consequently found that a
formulated pulp digesting assistant agent which is perfectly
free from the problsm mentioned above is obtained by
10 depositing on the surface of anthraquinone particles what is
obtained by adding water and/or a low molecular water-
soluble alcohol to a mixture of two kinds of specific
nonionic surfactants. This invention has been perfected on
the basis of this knowledge.
1~ The objects of this invention are accomplished by
(1) a formulated pulp digesting assistant agent which
comprises a particulate anthraquinone of an average particle
diameter of not more than 10 ~m and a maximum particle
diameter of not more than 30 ~m, 0.1 to 2% by weight, based
20 on the amount of the particulate anthraquinone, of a
nonionic surfactant mixture comprising a first nonionic
surfactant of an HLB value of 12 to 16 formed of a secondary
alcohol having carbon numbers from 10 to 16 possessing an
alkylene oxide adduct of 7 to 20 moles of ethylene oxide
25 added thereto and a second nonionic surfactant of an HLB
value of 12 to 16 formed of an alkyl phenol having the alkyl
group carbon number from 6 to 12 possessing an alkylene
oxide adduct having 8 to 15 moles of ethylene oxide added
thereto, the weight ratio of the first to the second
30 nonionic surfactant being in the range of 5 : 1 to 1 : 5 and
the total amount of the first and second nonionic
surfactants being in the range of 0.1 to 2% by weight based
on the amount of the particulate anthraquinone, and 5 to 30
by weight, based on 100% by weight of the formulated pulp
35 digesting assistant agent, of water and/or an alcohol of
molecular weight of not more than 200.
:: .
-4-

The objects of this invention are further
accomplished by (2) a formulated pulp digesting assistant
agent set forth in (1) above, wherein the mixture of the
first and second nonionic surfactants has an average HLB
6 value in the range of 13 to 15.
The objects of this invention are also accomplished
by (3) a formulated pulp digesting assistant agent set forth
in (1) above, wherein the total content of water and/or an
alcohol of a molecular weight of not more than 200 is in the
10 range of 10 to 20% by weight based on 100% by weight of the
formulated pulp digesting assistant agent.
EXPLANATION OF THE PREFERRED ENBODIMENT
Now, this invention will be described in detail
below.
The particulate anthraquinone to be used in this
invention has an average particle diameter of not more than
10 ~m, preferably not more than 7 ~m, and normally not less
than 5~m. Generally, it has a maximum particle diameter of
not more than 30 ~m, preferably not more than 20 ~m, and
20 normally not less than 18~m. If the average particle
diameter exceeds 10 ~m, the undesirability arises that the
particulate anthraquinone is not sufficiently dispersed or
dissolved in the pulp digesting liquid within the ordinary
span of digesting time because the speed of dispersion and
25 dissolution in the pulp digesting liquid is low and
consequently the time for the dispersion and dissolution is
proportionately large. If the maximum particle diameter
exceeds 20 ~m, the disadvantage ensues that the speed of
dispersion and dissolution is similarly low.
The first nonionic surfactant which is one of the
two components of the mixture of two specific nonionic
surfactants to be used in this invention is a nonionic
surfactant of an HLB (hydrophile-lipophile balance) value in
the range of 12 to 16, preferably 13 to 1~ formed of a
36 secondary alcohol having carbon numbers from 10 to 16,
preferably 12 to 14, possessing an alkylene oxide adduct of
.x.
. ~ , "
: . . . . : .: ~ : , ~ ;; . , . -: ~ : : . ... ; ; .

7 to 20, preferably 9 to 15 mols of ethylene oxide added
thereto.
The second nonionic surfactant which is the other
component is a nonionic surfactant of an HLB value in the
range of 12 to 16, preferably 13 to 15, formed of an
alkylphenol having the alkyl group carbon numbers from 6 to
12, preferably 8 to 9 possessing an alkylene oxide adduct
having 8 to 16, preferably 10 to 14, mols of ethylene oxide
added thereto.
The weight ratio of the first to the second nonionic
surfactant to be used in this invention is such that the
weight ratio of the secondary alcohol possessing the
aforementioned alkylene oxide adduct (first nonionic
surfactant) to the alkyl phenol possessing the
15 aforementioned alkylene oxide adduct (second nonionic -
surfactant) is in the range of 5 : 1 to 1 : 5, preferably 3
: 1 to 1 : 3. If the weight ratio of the first to the
second nonionic surfactant deviates from the range specified
above, then the facilitation of dispersion and dissolution
20 of the particulate anthraquinone in the pulp digesting
liquid is attained only with difficulty. This difficulty is -
justified in the light of the fact that while a secondary
alcohol possessing an alkylene oxide adduct generally i5 a
surfactant widely known as excelling in permeating power and
25 thus is counted among the surfactants that exhibit the best ~
wetting power to hydrophobic fibers, this secondary alcohol ~-
when used alone requires a long time in causing particulate
anthraquinone to be dispersed and dissolved in the pulp
digesting liquid. The facilitation of the dispersion and
30 dissolution of the particulate anthraquinone in the pulp
digesting liquid is never attained unless the first and
second nonionic surfactants are simultaneously used as~
combined at a weight ratio in the range specified above.
The total amount of the mixture of nonionic
35 surfactants is generally in the range of 0.1 to 2% by
weight, preferably 0.2 to 1% by weight, based on the amount
' ' ~ ' '~' ' ' , . .' ' ' , ': ' ` .,' . .'; i ' '` . ' ' ` : : " , ` ' ` ' " .'. ' ,

of the particu]ate anthraquinone. If the total amount is
less than 0.1% by weight based on the amount of the
particulate anthraquinone, the mixture of nonionic
surfactants fails to cover completely the surface of
anthraquinone particles and the powder of anthraquinone
added to the pulp digesting liquid cannot be thoroughly ~-
dispersed or dissolved in the liquid because part of the
powder floats on the surface of the liquid.
The average HLB of the mixture of the two specific
10 anionic surfactants is in the range of 12 to 16, preferably
13 to 15. The outstanding digesting effect obtained by this
invention is never manifested unless this HLB falls in the
range specified above in exactly the same manner as the
weight ratio of the nonionic surfactants mentioned above.
1~The alcohol to be used in this invention has no
particular restriction except for the requirement that the
molecular weight thereof is generally not more than 200,
preferably not more than 120. As typical examples of the
alcohol which answers this description, lower monohydric
20 alcohols such as methanol, ethanol, propanol, and
isopropanol and dihydric alcohols such as ethylene glycol,
diethylene glycol, triethylene glycol, tetraethylene glycol,
propylene glycol, dipropylene glycol, 1,3-butylene glycol,
neopentyl glycol, and trihydric alcohols such as glycerol,
25 and etc. may be cited.
The total content of water and/or an alcohol of a
molecular weight of not more than 200 to be used in the
formulated pulp digesting assistant agent of this invention
is generally in the range of 5 to 30% by weight, preferably
30 10 to 20% by weight, based on 100% by weight of the agent.
If this content is less than 5% by weight, based on 100~ by
weight of the formulated pulp digesting assistant agent, the
amount of water and/or the alcohol of a molecular weight of
not more than 200 is unduly small relative to the amount of
35 the mixture of specific nonionic surfactants and
consequently this mixture yields to the phenomenon of

gelation and, as a result, the disadvantage arises that the
nonionic surfactants are deposited in the state obstructed
from producing the inherent functions thereof on the
anthraquinone particles and, when the pulp digesting
S assistant agent contacts the pulp digesting liquid, the
surfactants fail to manifest their functions of facilitating
dispersion and dissolution of anthraquinone in the pulp ~ -
digesting liquid. If the content mentioned above exceeds
30% by weight based on 100% by weight of the formulated pulp
10 digesting assistant agent, the excess of the total amount of
water andtor the alcohol of a molecular weight of not less
than 200 prevents the nonionic surfactants from being
deposited on the anthraquinone particles and consequently
separates itself from the anthraquinone particles and
15 renders insufficient the thoroughness of dispersion and
dissolution of the particulate anthraquinone in the pulp
digesting liquid.
The formulated pulp digesting assistant agent o~
this invention is preferable to be homogeneously blended by
20 the use of a suitable mixing device or stirring device
before it is placed and used in the pulp digesting liquid. ;
The pulp digesting liquid into which the pulp
digesting assistant agent of this invention is thrown does
not need to be particularly limited but may be any of the
25 digesting liquids in popular use. The composition may be
added to an alkaline digesting liquid for the Kraft process
or an acidic digesting liquid for the sulfurous acid
process.
When the formulated pulp digesting assistant agent
30 is used as a dispersion in water1 viscosity of the ~
dispersion may be controlled by adding a thickener, if - `
necessary. As the typical thickener, there are
carboxymethyl cellulose, starch, sodium polyarginate, sodium
polyacrylate, (anhydrous) sodium methasilicate, xanthan gum, ~ -
quar gum, carageenan and the like.
Now, this invention will be described more

specifically b~low with reference to working examples.
Naturally, this invention is not limited to these working
examples.
Example 1
In a rotary autoclave having an inner volume of 5
liters, 600 g of absolutely dry broadleaf tree chips, 0.3 g
of a formulated pulp digesting assistant agent, and sodium
hydroxide and sodium sulfide added thereto in such
respective amounts as to account for an active alkali
10 content of 16% by weight (as reduced to Na20), a sulfidity
of 25% by weight, and a liquid ratio of 3.6 liters/kg were
together heated to 166C over a period of about 70 minutes
and digested at 166C for 40 minutes.
The pulp consequently obtained was disintegrated and
15 then tested for kappa number and pulp yield. The results
are shown in Table 1. Table 1 shows that the pulp had a
kappa number of 16 and a pulp yie~d of 52.0% by weight.
The formulated pulp digesting assistant agent used
in this example was obtained by mixing 80 parts by weight of
20 particulate anthraquinone having an average particle
diameter of 5 ~m and a maximum particle diameter of 18 ~m, a
mixture comprising a first nonionic surfactant of an HLB
value of 14.5 formed of a linear alkyl secondary alcohol
having carbon numbers from 12 to 14 possessing an alkylene
25 oxide adduct of 12 mols of ethylene oxide added thereto
(product of Nippon Shokubai Co., Ltd.; hereinafter referred
to as "Softanol-120") and a second nonionic surfactant of an
HLB value of 13.3 formed of an alkyl phenol having the alkyl
group carbon numbers from 9 possessing an alkylene oxide
30 adduct of 10 mols of ethylene oxide added thereto (product
of Sanyo Chemical Industries Co., Ltd.; hereinafter referred
to as "Nonipol-100") at a weight ratio of 1 : 1, the total
amount of the mixture of nonionic surfactants being 0.4% by
weight based on the amount of the particulate anthraquinone,
3~ and 20% by weight, based on 100% by weight of the formulated
pulp digesting agent composition, of water.
~"' '.'. ' ~'., . . . ` ... ..

Control 1
The procedure of Example 1 was repeated, except that
the addition of the two specific nonionic surfactants was
omitted. The pulp consequently obtained was tested for
kappa number and pulp yield. The results are shown in Table
4. Table 4 shows that this pulp had a kappa number of 16
and a pulp yield of 50.8~ by weight.
In this experiment, the digestion was carried out at
166C for 52 minutes. In due consideration of the general
10 practice of comparing pulp yields on a common kappa number,
the time of digestion in this case had to be adjusted to the
value indicated above so as to equalize the kappa number,
though approximately, with that of Example 1.
By the same token, in Examples 2 to 22 and Controls
15 2 to 9, the times of digestion at 166C were adjusted
substantially to equalize the respective kappa numbers and
the pulp yields found on these equalized kappa numbers were
used for the purpose of comparison.
Examples 2 to 5
The procedure of Example 1 was repeated, except that
the weight ratio of the two specific nonionic surfactants
was varied as shown in Table 1~ The pulps consequently
produced were tested for kappa number and pulp yield. The
results were as shown in Table 1.
-10-

Table 1 -
. .
Example
1 Z 3 ~ _
Softanol-120 0.16 0.256 0.192 0.128 0.064
tparts by weight)
Nonipol-100 0.16 0.064 0.128 0.192 0.256
(parts by weight)
Total amount used 0.32 0.32 0.32 0.32 0.32
(parts by weight)
Kappa number 16 16 16 16 16
1 Pulp yield 52.0 51.7 52.0 52.0 51.8
(% by weight) I _
Controls 2 and 3
The procedure of Example 1 was repeated, except that
the weight ratio of the two specific nonionic surfactants
20 was varied as shown in Table 2. The pulps consequently
produced were tested for kappa number and pulp yield. The
results were as shown in Table 2.
Table 2
26 Control 2 Control 3
_
Softanol~-120 0.32 0
(parts by weight)
..
Nonipol-100 0 0.32
(parts by weight)
Total amount used 0.32 0.32
(parts by weight)
_
Kappa number 16 16
Pulp yield 51.0 51.2
( % by weight)

Examples 6 to 9
The procedure of Example 1 was repeated, except that
the total amount the two specific nonionic surfactants was
varied as shown in Table 3. The pulps consequently produced
5 were tested for pulp yield. The results were as shown in
Table 3.
In these experiments, the weight ratio of the two
specific nonionic surfactants was invariably fixed at 1
Table 3
: '
Example
6 _ _
Total amount used 0. o8 o . 4 o . 8 1 . 6 - ~ -
15 ( parts by weight)
Kappa number 16 16 16 16 : :
Pulp yield 51.7 52.0 51.9 51.7 I
(% by weight)
Note) The weight ratio of Softanol-120 to Nonipol-
100 was invariably fixed at 1 : 1. -
~ ~. ,' -
Controls 4 and 5
The procedure of Example 1 was repeated, except that
25 the total amount of the two specific nonionic surfactants to
be used was varied as indicated in Table 4. The pulps
consequently produced were tested for pulp yield. The
results of test were as shown in Table 4.
Again in this case, the weight ratio of the two
30 specific nonionic surfactants was invariably fixed at 1 : 1.
.
' '~'
-12-
, ~''

Table 4
. _
Control 3 Control 4 Control 5
_ _
Total amount used O O . 04 3 . 2
(parts by weight) _
Kappa number 16 16 16
Pulp yield 50.8 51.4 51. 4
(% by weight) _
Note) The weight ratio of Softanol-120 to
Nonipol-10Q to be used was invariably fixed at 1 :
1.
Example 10
The procedure of Example 1 was repeated, except that
15 a particulate anthraquinone having an average particle
diameter of 3 ~m and a maximum particle diameter of 18 ~m
was used instead. The pulp consequently produced was found
to have a kappa number of 16 and a pulp yield of 52.2~ by
weight.
The determination of the particle diameter was
carried out by the use of a supercentrifugal automatic
particle size testing device, CAPA-700 (produced by Horiba
Seisakusho K.K.).
Control 6
2~ The procedure of Example 1 was repeated, except that
a particulate anthraquinone having an average particle
diameter of 30 ~m and a maximum particle diameter of 60 ~m
was used instead. The pulp consequently produced was found
to have a kappa number of 16 and a pulp yield of 50.7% by
30 weight.
Examples 11 to 15
The procedure of Example 1 was repeated, except that
the amount of water added based on 80 parts by weight of
anthraquinone was varied as indicated in Table 5. The pulps
3~ consequently produced were tested for pulp yield. The
results were as shown in Table 5.
-13-
~. ,~;~ ~,; . : ; - . , . . :,
~ - .. ..... ~ -~ . . .
i~

Table 5
_
Example
:
11 12 13 14 15
Total amount used 5 9 14 27 34
(parts by weight)
Kappa number 16 16 16 16 16
: . ':
Pulp yield 51.6 51.9 52.0 51.9 51.7
10 (% by weight)
' . -
Controls 7 to 9
The procedure of Example 1 was repeated, except thatthe amount of water added based on 80 parts by weight of
15 anthraquinone was varied as indicated in Table 6. The pulps
consequently produced were tested for pulp yield. The ~-
results were a~ indicated in Table 6.
Table 6
_ Control 7 IControl 8 IControl 9
_
Total amount used 0 2 43
(parts by weight) ~ -
. ...
Kappa number 16 16 16
Pulp yield (% by 50.8 51.3 51.4
weight)
, . .
Example 16
The procedure of Example 1 was repeated, except that
30 an aqueous solution containing 50% by weight of ethylene
glycol was used in the place of water. The pulp
consequently produced was disintegrated and then tested for
kappa number and pulp yield. It was found to have a kappa
number of 16 and a pulp yield of 52.0~ by weight.
3s Example 17
The procedure of Example 1 was repeated, except that
-14-

an aqueous solution containing 40% by weight of diethylene
glycol was used in the place of water. The pulp
consequently produced was disintegrated and then tested for
kappa number and pulp yield. It was found to have a kappa
number of 16 and a pulp yield of 52.0~ by weight.
Examples 18 to 20
The procedure of Example 1 was repeated, except that
nonionic sur~actants having ethylene oxide addition mol
numbers indicated in Table 7 were used in the place of
10 Softanol-120 as the first nonionic surfactant. The pulps
consequently produced showed pulp yields as indicated in
Table 7.
Table 7
Example 18 _ _
Ethylene oxide 7 15 20
addition mol number
Kappa number 16 16 1 16
Pulp yield 51.8 52.0 51.8
(% by weight) _
Example 21 and 22
The procedure of Example 1 was repeated, except that
nonionic surfactants having ethylene oxide addition mol
25 numbers indicated in Table 8 were used in the place of
Nonipol-100 as the second nonionic surfactant. The pulps
consequently produced showed pulp yields indicated in T`ble
8. Table 8
30 Example 21 Example 22
_
Ethylene oxide 8 14
addition mol number
.
Kappa number 16 16
35 Pulp yield 51.8 51.9
(% by weight)
......... .

The for~ulated pulp digesting assistant agent
obtained in accordance with this invention can be used as an
amply effective digestion assistant not only in the
digestion by the kraft method, sulfurous acid method, and
soda method but also in the digestion by the semi chemical
method. They bring about decisively fine digesting effects
as compared with a digesting assistant formed solely of
anthraquinone. They produce a better digesting effect
reduced to available anthraquinone content as compared with
10 an aqueous alkali solution of tetrahydroanthraquinone which
is held to constitute an ideal form of use.
Further, in the formulated pulp digesting assistant
agent of this invention, since two specific nonionic -~
surfactants are jointly used for the purpose of precluding
15 the possible occurrence of the "phenomenon of gelation" of a
nonionic surfactant and, at the same time, these surfactants
are incorporated in the composition in combination with a
suitable amount of water and/or an alcohol having a
molecular weight of not more than 200, these nonionic
20 surfactants are deposited in the state retaining their
inherent functions intact on the anthraquinone particles.
When this agent is exposed to the pulp digesting liquid,
therefore, the combined function of the surfactants is
manifested at once in facilitating the dispersion and
25 dissolution of anthraquinone in the pulp digesting liquid.
Thus, the agents thoroughly manifest their effect as a redox
catalyst for anthraquinone. --
In the production of the formulated pulp digesting
assistant agent, the conventional method which uses a
30 particulate anthraquinone having an average particle
diameter in the neighborhood of 10 ~m is hardly practicable
because the powder which is drifted about the site of-
handling in a wind of such a low speed of about 2 m/sec.
poses a problem of environmental hygiene. In the formulated
35 pulp digesting assistant agent of this invention, the
combined addition of the nonionic surfactants and water ~ -~
-16-

and/or an alcohol having a molecular weight of not more than
200 imparts a wet state to the agent and perfectly prevents
the particulate anthraquinone from being drifted about in
the form of dust.
Further, the formulated pulp digesting assistant
agent of this invention can manifest an outstanding
digesting effect even when trees and plants as well as
conifers and broadleaf trees are used as pulpwood or chips.
This invention, therefore, is expected to lend itself
10 immensely to protection of environmental resources on a
commercial scale and contribute extensively to the progress
and prosperity of mankind.

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Administrative Status

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Event History

Description Date
Inactive: IPC from MCD 2006-03-11
Time Limit for Reversal Expired 1998-12-21
Application Not Reinstated by Deadline 1998-12-21
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 1997-12-22
Application Published (Open to Public Inspection) 1994-06-22

Abandonment History

Abandonment Date Reason Reinstatement Date
1997-12-22
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
NIPPON SHOKUBAI CO., LTD.
NIHON JORYU KOGYO CO., LTD.
Past Owners on Record
KENJI KUMAGAI
NAOJI KURATA
RYUJI BABA
SCIJI SHOJI
YOSHIO SUGITA
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Claims 1994-06-21 2 101
Abstract 1994-06-21 1 39
Drawings 1994-06-21 1 9
Descriptions 1994-06-21 17 936
Courtesy - Abandonment Letter (Maintenance Fee) 1998-02-01 1 187
Fees 1996-10-29 1 56
Fees 1995-11-26 1 50
Prosecution correspondence 1993-12-21 1 28