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Патент USA US3069317

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United rates Patent
“Fine
1
2
In general, the deinking agent employed contains an
3,069,307
aqueous alkali solution which may in addition contain
OXYALKYLATED PHENOL PROCESS
William M. Boaz, Kirkwood, and Kenneth J. Lissant, St.
one or more of the following: a detergent, for example
sodium soaps of fatty acids or abietic acid, sulfonated oil,
etc.; a dispersing agent to prevent agglomeration of the
pigment after release and to emulsify any unsaponi?able
Louis, Mo., assignors to Petroiite Corporation, Wilming
ton, Del., a corporation of Delaware
No Drawing. Filed Apr. 20, 1960, Ser. No. 23,389
g 4 Claims.
3,059,307
Patented Dec. 18, 1962
material; a softening agent such as kerosene or mineral‘
oil, etc. to soften the vehicle of the inks; an agent such
(Cl. 162—5).
This invention relates to a process of deinking paper
characterized by treating imprinted paper products with
an aqueous solution containing a minor amount of an
as clay, a silicate, etc., for selective adsorption after 're-»
10 lease from the ?ber to prevent redeposition on the ?ber;
oxyalkylated aromatic phenol compound
a basic exchange chemical to prevent formation of calci-t
um soaps, etc.
Since paper manufacture does not damage or alter the
The cooked and de?bered pulp is then diluted to less Y
character of the essential ?ber from which the paper is
than 1% concentration and rii?ed and screened to re
originally made, such ?ber may be recovered from used 15 move oversized objects and unde?bered pieces of paper.
paper and reused, time after time, in the manufacture of
This material is then washed with voluminous amounts of
fresh paper stock. The limitations in respect to the prac
water, an average of 20,000 gallons of water per ton of
tical recovery of ?ber from used paper are to be found in
pulp, to separate the ?ber from other substances by wash-t
the dif?culty and expense of thoroughly deinking printed
ing or screening or by a ?otation process. The disposal‘
paper stock to upgrade it to the color and quality of the 20 of large amounts of water used in the process poses a,
original paper stock. Therefore, cost is essential in de
stream pollution problem which must be remedied in most-1
inking and a process which cannot deink economically has
areas of the country.
'1
no commercial value;
The problem of deinking has been further complicated
Many processes have been used for deinking paper so
by certain recent changes in the paper industry which have
as to make the ?bers thereof reuseable. These processes, 25 increased the dii?culty of deinking, among which changes.
however, are generally expensive, laborius, time-consum
are the following:
ing, and/or complicated. Most of these processes are
(1) The increased use of groundwood containing small
commercially unsatisfactory because: (1) they are too
slivers of wood rubbed from pulp wood present jagged
costly; (2) they produce a pulp which is not of a suf?cient
sawtooth endswhich afford excellent crevices .for trapping.
brightness and cleanliness, or (3) they require unusual
and expensive equipment for their practice. ‘Many proc
esses are costly because of the type and large quantities
of chemicals needed. They often fail ,to initially free
enough ink so as to result in imparting irreversible colora—
tion to the ?bers, leave carbon agglomerates therein, or
darken the paper because of the heat and/or chemical
employed, all or each of which reduces the brightness of
the recovered pulp.
In general, in preparing used paper for deinking and
recovery of ?ber, the stock to be salvaged is ?rst thor 40
oughly cleansed of super?cial dirt and macerated by
means of any suitable system or apparatus.
Then the
maceratum is boiled, subjected to the cooking and de
the carbon particles of the printer’s ink, thus making it,
increasingly difficult to produce a ‘reuseable pulp 'of' high
quality of whiteness. In addition groundwo‘od tends. to"
’ darken with the application of heat and/orbase.
(2) Many of the improved new. inks currently ‘in. use:
are non-saponi?able with caustic, and generally require.
more drastic cooking conditions during deinking, thus‘
tending to further degrade the cellulosic ?ber.
(3) Certain paper coatings such as casein and soy~i
bean proteins hardened with formaldehyde require for 1
their removal higher temperatures which also degrade the
(4) The increased ?ller content of paper, now lap-V.v
proaching an average of 25%, results in increased shrink-‘1
?bering in a suitable aqueous alkali to soften the paper
age during deinking which increases the cost of deinked
?bers, loosen and disintegrate at least part of the ink and
stock.
45
other matter adhering to’the ?bers, and thoroughly agi
Among ‘the disadvantages of vprior processes are the
tated, either while in the alkaline solution or subsequently,
following:
'
'
1
to disintegrate and de?ber the stock as thoroughly as pos
sible.
Thereafter, the pulp is rif?ed and screened and
subsequently dewatered, preferably through suitable rolls,
(1) Long cooking periods at elevated vtemperatures re
quire large expenditures of energy with increased expense.
(2) High temperatures and strong chemicals employed
?lter, or the like, to remove a considerable portion of the 50 in these processes tend to deleteriously affect the ?bers so
loosened ink. It is then washed and dewate-red for re
that they are not always of the same quality as those from
moval of additional quantities of the loosened ink as many
fresh paper pulp.
times as may be practical and expedient.
‘
(3) The use of large amounts of caustic-containing:
Thus, all commercially successful processes for deinking 55 water poses a stream pollution problem which requires
waste paper involve the following steps:
expensive pollution control systems.
(1) Dusting and maceration.
A statement of the deinking problems and proposed’
(2) Alkali cooking and de?bering.
solutions thereof can be found, for example, in the fol
(3) Ri?'ling and screening.
(4) Washing.
In general, the sorted, dusted and macerated paper is 60
cooked with an aqueous deinking agent at a temperature
of from 140° F. to its boiling point for 25-48 hours at
concentrations of 4—25% by weight of paper in the alkali
solution. Heat consumption will vary inversely with the
concentration and viscosity of the stock. De?bering is
generally accomplished during the cooking operation.
lowing patents: 2,673,798, 2,607,678, 2,580,161, 2,219,-.
781, 2,112,562, 2,077,059, 2,005,742, 1,993,362, etc.
The desideratum of a deinking process is to be able (1‘) v
to pulp imprinted paper in the presence of an aqueous
solution containing a minor amount of an inexpensive de
inking agent at about room temperature so as to free the'
ink therefrom, (2) to remove the ink-containing solu
tion from the pulp by a simple expedient, and (3) to re
cover a pulp which is commercially acceptable, prefer
8,069,807
3
ably,havingfsubstantially the same properties and bright
example 40-98%, and preferably 50-98,‘ with an opti
ness of the original paper. All of these should be per
formed in simple equipment and at low cost. It is also
desirable to be able to employ a deinking solution that
mum of 70-90% of the alkylene oxide.
In certain cases, it is advantageous to react the phenol
with alkylene oxides in a random fashion so as to form
can be repeatedly recycled after being freed of carbon
particles derived from the ink.
a random copolymer on the oxyalkylene chain, i.e. the
(OR),,OH chain could be AABAABBABABBBA. In
addition, the alkylene oxidescan be reacted in an alter
nate fashion to form block copolymers on the chain, for
We have now discovered a process of deinking paper
products which ful?lls; allof these requirements charac
terizedby treating imprintedv paper products'with a de:
example
inking solution containing'a minor amount of an oxy 10
BBBBAAAABBBBAAAA
alkylated; aromatic phenol compound, for example an
oxyalkylated phenol.’ The processis carried out at about,
O1‘
rgomternperature and in, the absence of strong chemi
calsrsuch ascausticand the like, so that no degradation
or, darkening of- the paper occurs. The cost of the oxy
15
alkylated phenol is extremely low, since it is itself inex
pensive and__is_ employed in very low volume concentra
tions, for exampleless than about 2%, such as 1%, for
example .001 to 1%, but preferably 0.33 to 0.033%.
BBBBAAACCCAAAABBBB
where A is vthe unit derived from one alkylene oxide, for
example ethylene oxide, andB is_ the unitderived from;
a second alkylene oxide,vfor example propylenezoxida,
and C is the unit derived from ,athird alkylene oxide, for
Higher, percentagescan beemployed such- as 3—5% or 20
example, butyleneoxide, etc. Thuskthese compounds
morebut without economic advantage. In, fact, the eco
include bis- and ter-polymers, or higher copolymers. pow
nomics of any deinking process is so important that the
lymerized randomly or in a blockwisefashion or inmanyv
deinking; agentrmustbe very powerful one which is ef-,
variations of sequential additions.
fective at‘ extremely low- concentrations'in. the system.
Thus, -—(OR),,-- in the, above-formula:canlbegwritten.
Our deinkingt agentgis, so- effective that in screening spe
—-A,,BbCc—- or any variation thereof, ,wherein a,,bl;and.-c:
ci?c members of-the classwe select those that are effec
arezero or atnumberk provided at least one oftthemds,
tiveideinkers. at concentrations of.0.033 to 0.33%. In
greater than zero. ,
addition,_uponlremoval of the ink.- from the pulp-freed
Thus, phenol itself, can, be-_>oxyalkylated,,as well-aswa:
solution, one should be able to recycle this solution in the
process,~ for example 5 to 10m 20 or more times, or 30 hydrocarbon substituted such as an alkylated ‘phenol cone-v
taining 1-5 ring-attached alkyl, groups-such.v as methyl,
substantially inde?nitely, with additional “make-up” solu
tion ,addedlto replace operational ‘losses.
ethyl, propyl, butyl, pentyl, hexyl,'_heptyl,, octyl,_nonyl~,r
decyl, dodecyl, tridecyl, tetradecyl, pentadecyl,_hexadecy__l,-,
In general, the process is carried out by pulping im
printed paperwithan aqueous solution containing minor
heptadecyl, octadecyl, _ etcr, _ including. unsaturated. ana-~
papertas well as the. solvent so that the solvent can be
noliccompounds having condensed; ring st-ructures,gsuch.
asnaphthyl radicals, i.e.v
amounts of an oxyalkylated phenol, andthen removing 35 logues, thereof such aspentadecenyl, ,etc., as wellias;cycl0:~
aliphatic groups such as cyclohexyl,andarornaticzgroups.
the carbon particles from the paper pulp by any satisfac
such as phenyl, etc.,_ In additiornwthe,alkyhgrougcan;
torysmeans, for example, those means well known tov the
contain other elements besides-carbonand.hydrogen, for,
deinking art, such as by ?ltration, centrifugation, ?ota
example, oxygen such as in an alkoxygroup, etc, The.
tion, etc. Flotation isaa very usefulexpedient since it
simultaneously. removes the carbon particles from the 4.0 term, “aromatic phenolicucompound? also;,includes;,phe-,.~.
recycled without further treatment.- Where» ?ltration is
employed, the solvent'which contains carbon particles
from the printing ink-is ?rst ?ltered'from the paper pulp
by-employing a. coarse ?lter and then ?ltered from the
solventlbylemploying a ?ne‘ ?lter-before recycling.
The deinking. agents employed in this invention arev
oxyalkylated aromatic phenolic compounds such as oxy
alkylated‘ phenols, for.v example those represented by- the
formula ,®.—(-OA),,OH, but. preferably -
50
R»,
as well as those derivedhfr'om biséphenol-‘A;
(O A) nOH
Ralf
where @ is an aromatic radical, where R is a hydrocar
bon grouphaving for example. 1-30 or more carbon atoms
such as 4 to 20 carbon atoms, but preferably 6 to 14
carbon atoms; A is the radical derived from the alkylene
oxide,’for example, ethylene oxide, propylene oxide, butyl
ene oxide, etc.; m=O-5, for example l-3, but preferably
1-2, and n is the number of moles of alkylene oxide
added such as l-200 or more, for example 4 to 150, but
60
where R is H or alkyl,I etc. Other oxyalkylate'di aromatic
phenolic compounds can also be employed.‘
In general, the process of ‘this vinvention is' carried out
by treating imprinted paper, which has-preferably been
sorted, dusted and macerated, with ‘an aqueous solution
containing a minor amount'of an- oxyalkylated phenol.
In practice, the waste paper to be treated‘is-preferably
subdivided in relatively small pieces as‘by passing'the
preferably l5-to 90. The optimum number of moles-of
waste paper through a conventional‘ shreddingmachine:
alkylene oxide addedwill depend on the particular phenol 70 The exact size of ‘the-piecesis not material, it being'adé
employed‘as the- starting material, the type or types of
visable merely to so subdivide the’ wastepaper-asto"
alkyleneoxides added, the order of addition of the alkyl
avoid the presence of a‘ thick bulky-mass‘which' might
ene oxides, etc, However, we have found that to achieve
damage ' the ~ beater a in which the “wastev paper‘ is Subse-‘
thee-brightness ‘desired in the deinked paper the oxyalkyl
ated phenol should contain at least 40% by weight, for
contact with the aqueous solution.
quently trcated'and-to' exposeethe-inked- paper ~to intimate"
5
3,069,307
6
After the paper has been shredded, it is introduced into
the aqueous solution in an operating beating engine in
suf?cient quantity to provide a suspension which the
beater can satisfactorily handle. In practice, we employ
solutions of the deinking compound to be tested in con
centrations of 1.7, 0.33, and 0.033% by volume. To 300
a suspension of approximately from about one to ten
chopped newsprint.
The deinking agents are evaluated by preparing aqueous
ml. of each of these solutions is added 10 grams of dry,
percent by weight, or higher, solid content, but prefer
Pulping is effected in a Waring
Blender. The pulp formed is then ?ltered through a
ably about two to ?ve percent, with an optimum of about
screen. This sheet thus formed is then repulped in about
2.5 to 4 percent.
300 ml. water and ?ltered through a Buchner funnel
The mass in the beater is circulated around the beater
where it is drained by suction. This sheet is then tested
and subjected to the action of the beater wheel until 10 for GE. brightness. The GE. brightness of pulped paper
“shiners” have practically disappeared from the mass.
without deinking agent is about 38.5 and its pulped edges
The time required for this operation will vary with the
about 53.5. The results are presented in the following
particular apparatus employed. Further beating pro
table:
motes an excess of ?ne ?bers which may not be desirable
in preparing paper. Beating time varies with the par
ticular system and apparatus employed, but ordinarily
in the laboratory the beating of the mass is continued
TABLE I
from about one-half to three minutes, or longer, for ex
ample about one to two minutes with an optimum of
CYCLOHEXYL PHENOL
about one to one and one-half minutes, or until the ?ber 20
is completely freed of ink and other extraneous material
present. However, these times will vary in the plant,
depending on the effectiveness of the apparatus employed.
After completion of the beating action the mass is
Withdrawn from the beater and the excess liquid is sep~
arated from the ?ber content which is then Washed, if
desired. The separation and working of the ?bers may,
Ex.
f
Moles
EtO
Percent
per mol.
EtO
phenol
7. 2
7. 6
8. 0
8. 4
8. 8
G.E. brightness readings at
1.7%
0.333%
64. 3
65.6
66.6
67. 7
68.8
0.033%
43. 2
43. 4
44. 4
45. 6
43.02
for example, be advantageously accomplished by passing
the mass from the beater directly to a continuous ?lter of
the Oliver type. In this type of ?lter a perforated drum
rotates in a tank containing the suspension and by the
action of reduced pressure or suction the liquid is drawn
through the perforations leaving a mat of ?ber on the
OOTYL PHENOL
5.15
5. 28
5. 63
6.04
9. 37
9. 5
12. 5
16. 0
20. 0
30
surface of the drum, through which subsequent ?ltering
takes place.
During the rotation of the drum the mat
of ?ber on the surface thereof can be subjected to sprays
of water or the aqueous solution of the deinking com
pound. Heat as well as reduced pressure can also be
used to remove water. Other types of apparatus can
52. 5
53. O
54. 6
56. 3
66. 7
67.0
72. 8
77. 4
81. 0
86. 5
41. 6
42. 3
42. 8
41. 1
46.1
46. 3
45.6
46.0
46. 2
44. 4
also be employed.
After separation and washing, the ?ber is conveyed to
a storage chest for use in the manufacture of paper or
it is suspended in water and passed over a drum or screen
DIOO'I‘YL PHENOL
to form laps or sheets of pulp. While the foregoing
process results in the production of white pulp, if desired
in some instances one may subject the recovered ?ber
to a bleaching operation in which case it is advantageous
to pass the ?ber from the continuous ?lter to a chest
Where the ?ber is subjected to the action of a bleaching
agent, for example 1% chlorine bleach, after which the
bleached ?ber is thoroughly washed with water. This
washing may also be advantageously conducted by the
deink additional paper.
In other words, the aqueous
of ink or other undesirable matter, and reused to treat
additional waste paper. The reuse of the deinking
medium can be carried out batchwise or continuously.
For economical reasons, We prefer to carry out the
process can be carried out at temperatures lower or higher
than room temperature such as from 0°—50° C. or higher,
if desired, for reasons of economics and color, we prefer '
to carry out the process at around room temperature
and with temperature preferably ranging no higher than
around 50° C.
37. 3
38. 5
39. 7
5. 06
41. 2
40. 1 .
5. 78
6. 4
7. 23
8. 46
44. 5
47.0
50. 0
54.0
42. 7
44. 3
43. 6
45.4
NONYL PHENOL
deinking medium is separated from the paper pulp, freed
process at about room temperature. In addition, by
maintaining the temperature close to room temperature
better color is obtained in the product. Although the
28.6
33. 4
37. 5
ii
use of a continuous ?lter of the Oliver type although
other conventional means may be employed.
The process can also be carried out continuously such
as by removing the ink from the aqueous medium, by
any suitable means, for example, by ?ltration, settling
and decantation, ?otation, etc., and combinations thereof
and thereupon reusing the aqueous deinking medium to
2. 89
3. 62
4. 34
1.3
20 6
2. 0
3.0
28. 6
37. 5
41. 6
38.6
3. 77
43.0
________ .
4.0
5.0
45.1
50 0
5,64
53. 0
6. 0
54. 5
7.0 _
58. 3
8. 52
63. 0
42. 05
40. 6
43. 0
40. 9
________ __
49. 2
48. 3
10.0
66.6
__________________ __
11.0
68.8
__________________ __
12. 2
13. 5
23. 3
71.0
73. 0
85. 0
30.0
v
________ _
35. 0
.
8
40. 6
49. 0
49. 5
47.4
46. 4
48. 3
47.4
42. 2
45.07
47. 7
48. 2
46. 9
45.4
48. 3
36. 6
40.0
45.0
50.0
55. 2
60.0
65. 0
70.0
75. 0
161. 5
48.7
46. 9
46. 02
46. 6
46. 6
46. 9
46. 8
46. 8
45.6
47.2
450. 0
________ -..
3,069,307
S
?
brightness of the treated paper deinked with the respective
compounds is shown in the following table:
TABLE I—Continued
DINONYL PHENOL
Moles
EtO
TABLE II
GE. brightness readings atPercent
.
.
.
.
OXYALKYLATED NONYL PHENOL
5
.
EtO
per mol.
phenol
‘ 0.333%
A
0.033%
5oeqo
Ex
EtO
moles
10
N
en1
B
Percent Bright- Ex.
EtO
ness
Moles PrO
added after
oxyethylation
Percent
EtO
Per
cent Bright
PrO
ness
o
1....
11.0
68.8
45.07
141...
0
2.-.3.-..
4....
30.0
30.0
30.0
85. 6
85. 6
85.6
45.4
45.4
45. 4
27...
37...
4a...
3.0
6.0
9.0
77.0
70.0
64.0
10.1
18. 3
25.3
47.0
48. 0
45.8
5. ...
30. 0
85. 6
45.4
5a.. .
12.0
59. 1
31. 2
46.5
6....
7...8....
9....
35.0
35.0
35.0
35.0
87. 5
87.5
87. 5
87. 5
48.3
48.3
48.3
48. 3
62...
70...
81.-90...
3.0
6.0
9. 0
12.0
79. 6
73.0
67.4
62. 7
9.0
16.4
22. 8
28. 4
45.4
45.9
45.2
47. 1
10.. .
11..-
40.0
40. 0
40.0
40.0
89.0
89. 0
89. 0
89.0 t
46. 9
46. 9
46. 9
46. 9
102..
1111..
1211..
131..
3.0
6. 0
9. 0
12.0
81. 7
75. 5
70. 3
65.9
8.0
14. 9
20.8
26.0
46.4
47. 9
48. 0
46.4
47.7
20 12.-.
13...
14. ..
N) Dr
30
35
DODECYL PHENOL
1. 0
2. 0
15. 7
30. 0
35. 0
40. 7
45. 0
50. 0
55. 0
60. 0
65. 0
70. 0
38. 6
38. 4
48. 3
49. 3
49. 0
48. l
48. 9
47. 4
48. 4
48. 1
48. 1
47. 8
_____________ -.
45. 0
90.0
46.02
14” ..
3.0
83.4
7. 3
15...
45.0
90.0
46. 02
157..
6.0
77.6
13. 6
16.--
45. 0
90. 0 . 45. 02
16a._
9. 0
72. 6
19. 1
17. ..
45.0
18-.. ' 56.0
90.0
91. 0
45.02
46.6
17s..
182..
12.0
3. 0
68. 5 _ 24.0
85.0
6. 7 -
46.8
46. '1
1'1...
20-..
50. 0
50.0
91.0
91.0 .
46; 6
46.6
19a._
201..
6.0
13. 0
79. 5
69. 3
12. 5 .
23.8
46.9
46.0
21. __
50.0 ‘
91.0
46.6
210 .-
20. 0
61. 4
32. 4
45. 0
22. ._
5s. 2
91. 7
23...
55. 2
24...
55. 2
25. .. ' 55. 2
91. 7
91. 7
92. 7
26...
-
47.4
45. 7
46.6
221..
10.0
75. 1
17. 9
45. s
4s. 6
46. 6
46.6
231..
411..
_ 250..
26. o
30.0
40.0
63. 7
55. 3
48. 9
3o. 5
30. 7 ‘
46. 7
45.8
4s. 2
45. h
60.0
92. 3
46. 9
I 262..
10.0
76. 6
27. ..
60.0
92. 3
46.9
27a..
20.0
65.6 ' 28. 8
47. 2
28...
29.-.
60.0
60. 0
92. 3
92. 3
46. 9
46. 9
231..
29m.
30. 0
40. 0'
57. 4
51. 0
37. 8
44. 3
44. 2
45.5
30. . .
65.0
92. 9 i 46. 8
307._
10.0
78. 1
15. 8
46.8
31-..
32.-33-.-
65.0
65.0
65.0
92. 9
92.9
92. 9
3111..
31"..
331__
20.0
30.0
40. 0
67. 4
59. 4
52. 9
27. 4
36.1
43.0
46. 1
46.7
46.6
34. __
70.0
93. 4
46. 8
46.8
46.8
16. 8
46. 2
46.8
3 i7 ..
15.0
74. 0
20.8
46.2
35. ..
70.0
93. 4
46.8
352..
25.0
64. 9
30. 5
45.0
36...
70.0
93. 4
46. 8
362..
35. O
57. 8
38. 2
44. 8
37. ._
70.0 -
93. 4
46.8
37L.
50.0
49. 7
46.8
43.8
38..39.-.
40-..
4] ...
75.0 ' 93. 7
75.0
93. 7
75.0
98. 7
75.0
93. 7
45.6
45. 6
45.6
45.6
3%..
3112-.
40a..
4111..
10.0
80. 5
20. 0
70. 5
30. 0 . 62. 7
40.0
56. 5
14.1
24. 8
33. 1
39. 8
46.0
45.0
46.0
47.0
In the above Tables I and II, it is to be noted that ?ltra
tion was employed. Where ?otation is employed in place
of ?ltration employing the same compound, an increased
brightness of 4-7 points is obtained over the ?ltra
tion process. In addition, less deinking agent is as effec
tive, or more effective, in a ?otation process as compared
to the ?ltration process.
Thus, in the preferred embodiment the ink is removed
from the system by means of ?otation. Ink particles in
this system are susceptible of froth ?otation in a conven
DIDODECYL PHENOL
6. 0‘
-
12. 0
14. 0
16. 0
-
tional apparatus, the speci?c technique to be employed
38. 0
38. 5
55. 3
59. 0
43. 0
43. 8
62. 1
-
45. 0
18.10
64. 7
45. 9
20. 0
67. 2
43. 3
22. 9 25. 0» 30. 1
'
70. 0
71. 4
76. 9
47; 3
44. 8
46. 3
35.0 -
78.1
45.8
40. 1
44. 9
50. 0
55. 1
60. 3
65. 1
>70. 0‘
80. 5
82. 0
83. 6
85. 2
86. 1
87. 1
87. 6
44. 4'
43. 2
45. 0
43. 6
43. 7
44. 4
45. 9
with a given pulp for maximum separation of the ink
particles varying somewhat with the nature of the pulp.
With certain pulps, it is possible to ?oat the ink away
55 from the ?ber without the addition of ?otation agents.
To some extent it is desirable to use a frothing agent.
With other pulps it may be desirable to use a ?otation
agent. After the ink particles have been ?oated away
in the froth from the ?otation cell, the cleaned pulp is
60 removed, dewatered and washed and used in the manner
described above.
.
7
Examples of suitable ?otation apparatus which can be
employed in )deinking can be found in US. Patent
2,005,742.
In the following examples’ nonyl phenol was ?rst re
acted with ethylene oxide to yield a product containing
the number of moles shown in the table.
Part of. this product was removed from the reaction
mixture and the remainder was then reacted with propyl 70
ene oxide to the extent shown in the table.
Both the
The following examples illustrate the use of the ?ota
tion in conjunction with this process.
The following examples were carried out by pulping 20
grams of cut newsprint in 600 ml. of aqueous deinking
agent by means of a Waring Blendor.
As a ?oatation
aid, the following agents were added to the pulp: 0.1
gram sodium sul?de as a 1% solution, two drops of pine
oxyethylated nonyl phenol (A) and the oxyethylated,
oil and four drops of turpentine. The pulped product
oxypropyla'ted nonyl phenol‘ (B) were then tested for their
was then placed in a ?otation cell in which air was bub
bled from an inlet in the bottom. After a ?otation time
deinking, properties according to the above process em
ploying ?ltration in a-concentration of 0.033%. The 75 of about five minutes, the surface froth was skimmed o?
3,069,307
and the pulp then ?ltered through a Buchner funnel to
form a sheet. Where recycling of solvent was employed,
a “make up” of about 15% aqueous deinking agent of
the same concentration Iwas employed (i.e. 90 ml. addi
tional). The results are present in the 'following table:
TABLE III
oxyalkylated phenols which can be employed to yield a
clean pulp.
Deinked paper is a very important source of raw ma
terial for the manufacture of book and magazine papers,
5 labels, coated papers, etc. Waste ledger papers, bonds,
etc., can be deinked making possible the reduction in the
amount of virgin pulp required in such grades as patent
coated boards, Bristols, envelope papers, etc., as well as
in book, magazine, and cover papers. Deinked ground
Flotation Deinking
Deinking agent
GE
Ex.
Method employed
Name
Concentration
10 wood papers can be used advantageously as subliners in
bright
patent~coated, multicylinder boards and as a substantial
ness
portion of the liner furnish in manila-lined boards. They
are also being used in considerable quantity for the man
1"... None ______________________ __ Newsprint pulped
in
38. 4 15
ufacture of hangings, newsprint, poster paper, mimeo
graph paper, catalog papers, tissues, and similar papers
53. 5
deinked paper are well known to the art.
water without chemi
cal aid or ?otation.
in which groundwood is ordinarily used. Other uses of
Filtration employed.
2 ________ _.do___
,
White edges of neWs-
print pulped in water
without chemical aid
or ?otation:
Having thus described our invention what we claim as
new and desire to obtain by Letters Patent is:
Filtra
tion employed.
3_.___ Dinonyl phenol
plus 40 moles
0.1
20
Flotation ______________ -_
51.9
___-_do ................. ..
50. 7
E20.
0.01
0.001
do .-_
0.06
_____do__ _
47.3
49.8
0.06
Recycle 1st _.
49. 8 25
0. 06
Recycle 2nd___
51. 4
0.06
Recycle 3rd. __
50. 1
0.06
0. 06
0.06
0.06
0.06
Recycle 4th____
Recycle 5th_
Recycle 6th.
Recycle 7th.
Recycle 8th-..
40. 8
49. 8
49. 8
49. 8
49.8 30
NoTE.—-Exan1ples 3 through 14 above relate to newsprint.
Although newsprint has been used to illustrate our
process, any imprinted cellulosic material can be salvaged
for reuse by the process of the present invention, for ex- 35
ample various kinds of imprinted paper, such as imprinted
newsprint, rotogravure newsprint, bookstock, magazine
stock, ledger stock, cardboard, etc. The term, “paper
l. A process of deinking paper products characterized
by pulping imprinted paper with a caustic-free aqueous
solution consisting essentially of a minor amount of an
oxyalkylated phenolic compound in water, removing the
ink particles from the aqueous solution, and thereupon
separating the paper pulp from the aqueous solution.
2. The process of claim 1 wherein the oxyalkylated
phenol contains at least 40% alkylene oxide.
3. The process of claim 2 wherein the oxyalkylated
phenol contains at least 50% alkylene oxide.
4. The process of claim 3 wherein the oxyalkylated
phenol contains at least 70% alkylene oxide.
References (Jited in the ?le of this patent
UNITED STATES PATENTS
1,925,372
1,988,363
Darling ______________ .... Sept. 5, 1933
Snyder ______________ .._ Jan. 15, 1935
2,005,742
Hines _______________ __ June 25, 1935
2,753,309
Figdor _______________ __ July 3, 1956
products” as employed in the speci?cation and claims, in
cludes all of such products.
OTHER REFERENCES
40
In addition, it should be realized that the above deink
Ellis:
Printing
Inks, pub. by Reinhold Pub., 1940, pp.
ing agents are merely exemplary of a wide variety of
480—483.
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