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Patent 2287602 Summary

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(12) Patent: (11) CA 2287602
(54) English Title: BIOLOGICAL METHOD OF DEINKING PRINTED WASTEPAPER
(54) French Title: PROCEDE BIOLOGIQUE DE DESENCRAGE
Status: Expired and beyond the Period of Reversal
Bibliographic Data
(51) International Patent Classification (IPC):
  • D21C 5/02 (2006.01)
  • C12N 9/24 (2006.01)
  • C12N 9/42 (2006.01)
(72) Inventors :
  • EOM, TAE JIN (Republic of Korea)
  • OW, STEVEN SAY-KYOUN (Republic of Korea)
(73) Owners :
  • KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY
  • KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY
(71) Applicants :
  • KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY (Republic of Korea)
  • KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY (Republic of Korea)
(74) Agent: DOUGLAS B. THOMPSONTHOMPSON, DOUGLAS B.
(74) Associate agent:
(45) Issued: 2007-07-03
(22) Filed Date: 1990-12-14
(41) Open to Public Inspection: 1992-06-15
Examination requested: 1999-12-10
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: None

Abstracts

English Abstract


ABSTRACT OF THE DISCLOSURE
A biological method of deinking printed
wastepaper consisting of the steps of disintegrating of
printed wastepaper in hot water containing cellulase or
pectase and removing ink particles from fibers by froth
flotation or washing.


Claims

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


11
We claim:
1. A method of de-inking waste printed paper, comprising
a) pulping waste printed paper with an enzyme capable of dislodging ink
particles from
the waste printed paper in an aqueous medium at a pH between about 3 to less
than 8, with alkali
added only in an amount sufficient to effect a pH adjustment and not in an
amount effective to
enhance de-inking efficiency, the ink being dislodged from the waste printed
paper by action of
the enzyme; and
b) removing the dislodged ink particles from the resulting pulp containing
medium.
2. A method of recycling waste printed paper, comprising:
a) pulping waste printed paper;
b) contacting waste printed paper with an enzyme capable of dislodging ink
particles from the waste printed paper in an aqueous medium at a pH between
about 3 to less
than 8, with alkali added only in an amount sufficient to effect a pH
adjustment and not in an
amount effective to enhance de-inking efficiency, the ink being dislodged from
the waste printed
paper by action of the enzyme; and
c) removing dislodged ink particles from the resulting pulp containing medium.
3. The method of Claim 1 or 2 wherein dislodged ink particles are removed by
flotation.
4. The method of Claim 1 or 2 wherein dislodged ink particles are removed by
washing.
5. The method of Claim 1 or 2 wherein the amount of enzyme used is in the
range of about
0.005 to about 5 percent-by-weight based on the dry weight of the wastepaper.
6. The method of Claim 1 or 2, wherein the enzyme is selected from the class
consisting of
cellulases, pectiuases, and mixtures thereof.
7. The method of Claim 1 or 2 wherein the pulping occurs at a consistency of
pulp of
between about 4% to 7%.

12
8. The method of Claim 1 or 2 wherein the pulping occurs at a consistency of
pulp of
between about 12% to 15%.
9. The method of Claim 1 or 2 wherein the temperature of the pulping is in a
range of from
about 20°C up to about 60°C.
10. The method of Claim 1 or 2, wherein the enzyme is a cellulose used in an
amount
between about 0.005 and about 5.0 percent-by-weight based on the dry weight of
the waste
printed paper, the contacting being carried out at a temperature between about
20°C and about
60°C.
11. The method of claim 1 or 2 wherein the enzyme enhances removal of
materials selected
from the group consisting of heavily coated inks, highly polymerized inks, non-
impact inks, and
cured polymer resins.
12. The method of claim 1 or 2 wherein the enzyme is effective to enhance
removal of cured
polymer resins.
13. The method of claim 1 or 2 wherein the enzyme is effective to debond fiber
bonding
14. The method of claim 1 or 2 wherein the enzyme degrades by enzymatic
hydrolysis.
15. The method of Claim 10, wherein the pulping occurs at a consistency of 12-
15% of pulp.

Description

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


CA 02287602 2006-02-10
1
TITLE OF THE INVENTION
BIOLOGICAL METHOD OF DEINKING PRINTED WASTEPAPER
NAMES OF INVENTORS
TAE JIN EOM
STEVEN SAY-KYOUN OW
FIELD OF THE INVENTION
The present invention relates to a method of deinking
printed wastepaper.
CROSS-REFERENCE TO OTHER APPLICATIONS
This application is a Divisional Patent Application
of Canadian Patent Application Serial No. 2,032,256, filed
December 14, 1990.
BACKGROUND OF THE INVENTION
Deinking of pulp fibre is essentially a laundering or
cleaning process in which ink is considered to be the dirt.
Chemicals along with heat and mechanical energy, are
used to dislodge the ink particles from fibers and to disperse
them in the aqueous medium. The ink particulars are then
separated from the pulp fibers, either by washing or flotation
or by using a modern hybrid process that combines the two
elements.
The chemicals used for the conventional deinking
process are surfactants which function as detergents to remove
ink from fiber, keep the ink particles dispersed to prevent
redisposition on the fibers, and provide a foaming action for
the froth flotation of ink particles.
A typical surfactant is a long chain molecule with a
hydrophobic part to the one end and a hydrophillic part to the
other end. The hydrophobic part may consist of fatty acid,
fatty alcohol, alkylphenols or other oil soluble surfactants.

CA 02287602 2006-02-10
2
The hydrophillic part of the deinking surfactant
usually consists of anion molecules such as carboxyl acid salts
or sulfonic acid salts and nonionic molecules such as
polyoxyethylenated chains.
The typical surfactants commonly used in the washing
and froth flotation deinking process are: sodium and potassium
salts of strait chain fatty acid (soap), linear
alkylbenzenesulfontate (LAS), olefine sulfonate, long chain
fatty alcohol, polyoxyethylenenated alkylphenols,
alkylphenolethoxylates, and polyoxyethylenated strait chain
alcohols.
The major disadvantage of using these surfactants in
the deinking process is excess foaming in the subsequent pulp
stock flow and paper making process lines. In addition, some of
the above surfactants are resistant to biodegradation in the
effluent treatment stages causing a serious environmental
problem.
In the froth flotation deinking process, a collector
is added to agglomerate ink into large particles and attach them
to the air bubbles. Collectors are required for effective
flotation and are usually anionic long-chain fatty acid soap.
Fatty acid collectors are precipitated with calcium ions to form
larger, insoluble ink particles and collector particles. With
injection of air in the flotation cells, the agglomerated ink
particles adhere to the bubbles, rise to the surface and are
skimmed off from the system.
Major disadvantages of the flotation method using the
fatty acid collector is a pitch deposition and calcium scaling
problems in the subsequent stock lines and paper making
equipment. Besides the surfactants, other chemicals are caustic
soda, sodium silicate, metal ion chelating agents and hydrogen
peroxide.

CA 02287602 2006-02-10
3
The hydrogen peroxide bleaching agent has to be added
in order to prevent a pulp colour yellowing caused by the
additions of caustic soda and to improve brightness of pulp
fibers.
With the advance in the modern printing and
photocopying technology, conventional deinking with the aid of
surfactants encounters serious problems with the wastepaper
printed with the use of heavily coated, highly polymerized, or
nonimpact inks, such as ultraviolet, heatset, Xerox, laser and
ink jet. These inks usually contain cured polymer resins which
bind ink particles so strongly on the fiber surface that it is
impossible to dislodge the ink completely during the wastepaper
defiberizing (pulping) stage with the conventional deinking
chemicals. Excess heat and mechanical energy are also required
along with the ineffective conventional chemicals.
In the conventional flotation deinking process for
newsprint wastepaper a major technical problem is experienced
with fine ink particles embedded in the fibre bundles and
between fibrils which are almost impossible to remove from the
fibers by a washing and/or flotation process.
SIJNlN.fARY OF THE INVENTION
This invention provides a new and much improved
method of deinking printed wastepaper. This method is effective
in newsprint deinking, as well as the deinking of wood free
printed wastepaper such as whiteledger, laser printed,
xerographic copypaper and computer printout wastepaper.
This invented deinking method is to remove ink
particles with the use of biological activity of enzyme on the
cellulose fiber surface and a dispersing function of enzyme
protein on ink particles.
In contrast to the conventional method no alkali and
deinking surfactants are required although some surfactants can

CA 02287602 2006-02-10
4
be used along with the enzyme to enhance the deinking
efficiency. In the froth flotation process the fatty acid
collectors are not required. Since caustic soda is not used in
the newsprint deinking, hydrogen peroxide bleaching agent is not
also required for yellowing prevention.
The elimination of the fatty acid collector in this
biological deinking process will solve the persistent pitch and
scale deposition problem associated with the conventional
flotation process using the fatty acid type soap and calcium
salts and silicates.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
This method will now be described.
Printed Wastepaper, such as old newsprint or printed
wood free wastepaper, is disintegrated in a conventional pulper
(consistency 4-7%) or in a high consistency pulper, 12-15%, at
the water temperature ranging from room temperature up to 60 C.
The addition level of enzyme is 0.005% to 5.0% based on dry
weight of wastepaper, pH of the stock slurry is adjusted in the
range of 3.0 to 8Ø As compared to the conventional pulping
process using caustic and surfactants in pulping, the process
using enzymes can be completed in a relatively short period and
ink particles are completely separated from the fiber surface
and dispersed well. The dispersed inks are removed out of pulp
fibers by conventional washing process equipment such as a
vibration screen and a drum washer without the aid of detergent
surfactants. The ink particles dispersed with the action of
enzyme protein can be also selectively removed out of the
diluted pulp slurry with conventional flotation equipments in
which air is injected into the pulp to provide bubbles to pick
up the particles. No fatty acid collector is required in the
case of waste newsprint. A small amount of fatty acid collector

CA 02287602 2006-02-10
may be added to enhance the ink removal efficiency in the case
of laser-printed wastepaper.
This biological deinking process is to lower pulping
energy to a large extent since the addition of enzyme results in
5 a reduction in pulping time, as compared to the pulping in the
absence enzyme, of almost 50% reduction. The observed faster
and easier pulping in the presence of enzyme may be attributed
to an unique biological activity of enzyme which is effective to
debond the fiber bonding and dislodge the inks bonded on the
fiber surface as well as within the fibrils. A partial
enzymatic hydrolysis of cellulose within micro structure of
fiber surface may occur during the pulping stage. This
biological activity of enzyme takes out fine ink particles
embedded within fiber bundles, fibrils and fines which have been
impossible to be taken out by conventional deinking chemicals.
According to this biological deinking method of old
newsprint the addition of hydrogen peroxide to prevent the fiber
yellowing is not required, which will result in a substantial
reduction of deinking chemical cost as compared to the
conventional deinking process using caustic soda, hydrogen
peroxide, chelating agent and sodium silicates.
It should be pointed out that the physical strength
properties of the resulting pulp fiber prepared by this invented
method are found to be higher than those of the corresponding
pulp prepared by the conventional method, in addition to the
much higher resulting pulp brightness. The enzyme addition does
not appear to degrade the fiber strength, instead improving the
fiber strength for reasons that are as yet unknown.
Example 1.
Deinking of old newsprint with a cellulolytic enzyme.
A sample of old newsprint wastepaper was added to a
pulper which was filled with 40 C water at the consistency of 4%
and a cellulase was dissolved at the dosage level of 0.1% based

CA 02287602 2006-02-10
6
on oven dry weight of wastepaper. The wastepaper was soaked for
minutes and then disintegrated for 5 minutes. After a
complete disintegration of wastepaper, one half of the pulp
slurry was diluted to a 1% consistency.
5 The diluted pulp slurry was moved to an air flotation
cell and then the dispersed ink particles were removed out of
the pulp slurry by skimming off a froth containing ink particles
out of the cell while injecting air through a porous plate. The
flotation time for the complete removal of the ink froth was one
10 minute.
The other half of the pulp slurry was washed on a
laboratory vibration screen to remove the dispersed ink
particles.
The resulting recycled pulp fibers obtained by the
flotation and the washing step were evaluated for pulp
brightness and mechanical strength properties. To compare this
enzyme treated deinking pulp to the conventional deinking pulp,
the same sample of wastepaper was treated in the pulper with the
addition of 1.0% NaOH, 0.3% HO, 3% sodium silicate solution
(water glass), 0.8% of SERFAX MT-90 (Trademark) (fatty acid
soap) and 0.2% IGEPAL 660 (Trademark) based on oven dry weight
of wastepaper. The pulping time was 10 minutes for a complete
disintegration. After diluting to 1% consistency, the dispersed
ink particles were removed by the flotation method with the
laboratory flotation cell as described above.
As shown in Table 1, the brightness of the pulp
deinked with enzyme was much higher than that of the pulp
deinked with the conventional chemicals and the mechanical
strength of the enzyme-deinked pulp was also superior to that
pulp deinked with the fatty acid collector and the dispersant
(IGEPAL 660 TM). The microscopic observation revealed that the
pulp prepared by the present invention contained more long fiber

CA 02287602 2006-02-10
7
fractions and has smoother fiber surface and looked less
mechanically damaged.
Table 1.Comparison of properties of recycled pulp by method of
present invention and the conventional method.
brightness tensile index tear index
($) (N.m/g) (mN.m/g)
KONP AONP KONP AONP KONP AONP
flotation 47.1 45.2 28.9 32.4 11.7 13.6
present
method
washing 50.3 48.6 29.3 32.9 11.8 14.1
SERFAX MT-90TM 45.1 38.4 30.1 32.8 10.8 13.1
KONP: Korean old newspaper
AONP: American old newspaper
The enzyme treated pulp gave cleaner and brighter pulp
with the washing as compared to the flotation ink removal.
The enzyme addition appeared to accelerate the wastepaper
disintegration to a large extent. When the old newspaper was
disintegrated in the conventional pulper at the 4% consistency,
the addition of 0.5% enzyme reduced the pulping time from 5
minutes (no enzyme addition) to 30 seconds for a complete
disintegration as shown in Table 2.
Table 2.Relation between enzyme addition and disintegration
time.
Enzyme (%) 0.5 0.1 0

CA 02287602 2006-02-10
8
disintegration 30> 60-120 300<
time (sec)
Example 2.
Deinking of laser CPO (computer printout) with
cellulolytic enzyme.
It is almost impossible to achieve a complete removal
of laser beam cured ink particles from laser CPO wastepaper with
the conventional deinking chemicals, because the ink particles
are so strongly adhered to the fiber surface that alkali and
general deinking surfactants in the conventional deinking
chemicals are not able to dislodge and disperse in the pulp
water slurry.
A sample of laser CPO wastepaper was added to water
in a laboratory high consistency pulper at the consistency of
12.5% and a cellulase was added to the water at the dosage level
of 0.2% based on the dry weight of paper. At stock water
temperature of 20-35 C, the pulping was carried out for 20
minutes. The completely disintegrated pulp slurry was diluted to
0.5% and then dispersed ink particles were removed out of the
pulp slurry using the laboratory flotation cell as explained in
Example 1. In this case, to increase the ink removal efficiency
and selectivity a small amount of the conventional fatty acid
collector, SERFAX MT-90 (trademark), of 0.3% based on dry weight
of wastepaper was added prior to the air flotation and the
flotation time was 3 minutes. To compare to enzyme deinked
pulp, the conventional deinked pulp was prepared by the same way
but the different chemical conditions as follows:
1% NaOH on dry weight of wastepaper
0.1% IGEPAL 660 Tm dispersant
0.8% SERFAX MT-90 '
pulping temperature : 50 C
pulping time : 30 minutes
calcium salt addition to the flotation cell: 200 ppm
flotation time : 3 minutes

CA 02287602 2006-02-10
9
The brightness and the strength properties of the
resulting pulp samples were compared in Table 3.
As shown in the table, the image analysis of the
paper samples indicates that the number of the residual ink
particles was much less, about 10 times, for the pulp deinked
with the enzyme and the tensile strength was also higher as
compared to the pulp prepared with the conventional chemicals.
A recycled chemical pulp of high quality in terms of
dirt count and fiber strength properties can be obtained with
the use of enzyme in a combination of a small amount of fatty
acid collector by the flotation method.

CA 02287602 2006-02-10
Table 3.Comparison of pulp properties recycled by the method of
present invention and conventional method.
5
brightness dirt amount tensile index
(o) (count/area) (N.m/g)
10 enzyme: MT-90-
(0.3%) 79.0 450 34.3
MT-90 (90%) 80.6 4,330 26.3
Example 3.
Deinking of waste newsprint by pectinolytic enzyme.
As the same method to example 1, the waste newsprint
containing 0.1% of pectase was soaked for 10 minutes at 40C and
disintegrated for 5 minutes. Diluting the disintegrated pulp to
1%, the ink particles are removed by flotation for 1 minute.
As shown in Table 4, the brightness and tensile
strength of paper sheet prepared by the method of the present
invention are improved.
Table 4.Comparison of the method of using pectinolytic enzyme
with conventional method.
brightness tensile index
M (N.m/g)
present method 44.2% 33.3%
MT-90 (0.8%) 38.4% 32.8%

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Administrative Status

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Event History

Description Date
Inactive: IPC removed 2021-10-27
Inactive: IPC assigned 2021-10-27
Inactive: IPC assigned 2021-10-27
Inactive: IPC expired 2013-01-01
Inactive: IPC removed 2012-12-31
Inactive: Reversal of expired status 2012-12-02
Time Limit for Reversal Expired 2010-12-14
Letter Sent 2009-12-14
Inactive: Late MF processed 2008-12-22
Letter Sent 2008-12-15
Letter Sent 2008-02-18
Inactive: Office letter 2008-01-24
Grant by Issuance 2007-07-03
Inactive: Cover page published 2007-07-02
Pre-grant 2007-04-16
Inactive: Final fee received 2007-04-16
Inactive: Office letter 2007-02-21
Inactive: Corrective payment - s.78.6 Act 2007-01-19
Notice of Allowance is Issued 2006-10-19
Letter Sent 2006-10-19
4 2006-10-19
Notice of Allowance is Issued 2006-10-19
Inactive: Approved for allowance (AFA) 2006-10-06
Amendment Received - Voluntary Amendment 2006-09-15
Inactive: S.30(2) Rules - Examiner requisition 2006-03-17
Inactive: S.29 Rules - Examiner requisition 2006-03-17
Inactive: IPC from MCD 2006-03-12
Amendment Received - Voluntary Amendment 2006-02-10
Inactive: Correction to amendment 2005-12-14
Amendment Received - Voluntary Amendment 2005-12-07
Inactive: S.30(2) Rules - Examiner requisition 2005-06-07
Inactive: S.29 Rules - Examiner requisition 2005-06-07
Amendment Received - Voluntary Amendment 2005-05-16
Inactive: S.30(2) Rules - Examiner requisition 2004-11-17
Inactive: S.29 Rules - Examiner requisition 2004-11-17
Amendment Received - Voluntary Amendment 2004-09-20
Inactive: S.30(2) Rules - Examiner requisition 2004-03-24
Amendment Received - Voluntary Amendment 2004-02-09
Inactive: S.30(2) Rules - Examiner requisition 2003-08-07
Letter sent 2003-07-08
Advanced Examination Determined Compliant - paragraph 84(1)(a) of the Patent Rules 2003-07-08
Inactive: Advanced examination (SO) 2003-06-11
Inactive: Advanced examination (SO) fee processed 2003-06-11
Amendment Received - Voluntary Amendment 2003-05-08
Inactive: S.30(2) Rules - Examiner requisition 2002-11-12
Inactive: Entity size changed 2002-01-11
Letter Sent 2000-01-24
Inactive: Entity size changed 2000-01-24
Inactive: Office letter 2000-01-14
Inactive: Cover page published 1999-12-22
All Requirements for Examination Determined Compliant 1999-12-10
Request for Examination Requirements Determined Compliant 1999-12-10
Request for Examination Received 1999-12-10
Inactive: IPC assigned 1999-12-08
Inactive: CPC assigned 1999-12-08
Inactive: First IPC assigned 1999-12-08
Divisional Requirements Determined Compliant 1999-11-23
Letter sent 1999-11-23
Application Received - Regular National 1999-11-23
Application Received - Divisional 1999-10-19
Application Published (Open to Public Inspection) 1992-06-15

Abandonment History

There is no abandonment history.

Maintenance Fee

The last payment was received on 2006-11-06

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Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY
KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY
Past Owners on Record
STEVEN SAY-KYOUN OW
TAE JIN EOM
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 2003-05-07 3 99
Claims 1999-10-18 4 110
Description 1999-10-18 10 407
Abstract 1999-10-18 1 9
Cover Page 1999-12-21 1 20
Claims 2004-09-19 3 80
Claims 2005-05-15 3 62
Claims 2005-12-06 2 61
Description 2006-02-09 10 383
Claims 2006-09-14 2 73
Cover Page 2007-06-13 1 24
Reminder - Request for Examination 1999-12-20 1 119
Acknowledgement of Request for Examination 2000-01-23 1 180
Commissioner's Notice - Application Found Allowable 2006-10-18 1 161
Maintenance Fee Notice 2009-01-21 1 171
Late Payment Acknowledgement 2009-01-21 1 164
Late Payment Acknowledgement 2009-01-21 1 164
Maintenance Fee Notice 2010-01-24 1 170
Correspondence 2000-01-13 1 9
Correspondence 2002-01-10 1 44
Fees 2002-12-08 1 30
Fees 2003-11-27 1 27
Fees 2004-12-08 1 31
Fees 2005-12-08 1 27
Fees 2006-11-05 1 27
Correspondence 2007-02-20 1 15
Correspondence 2007-04-15 1 27
Correspondence 2008-01-23 1 17
Fees 2007-12-12 1 27
Correspondence 2008-02-17 1 14
Correspondence 2008-02-10 2 48