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USO05l41598A

UllltEd States Patent [19]

[11] Patent Number:

Richman et a].

[45]

Date of Patent:

5,141,598
Aug. 25, 1992

[54] PROCESS AND COMPOSITION FOR

DEINKING DRY TONER ELECTROSTATIC

FOREIGN PATENT DOCUMENTS.

PRINTED WASTEPAPER

727506

[75] Inventors: Sandra K. Richman, Jacksonville

Bea h; Mary Beth Letscher,

Darhngton, W. B., A New Process for Demlung Elec

_

[73] Assignee:

OTHER PUBLICATIONS
.

J a Cl;0mm 8 both of Fla

2/ 1966 Canada .................................. .. 162/5

Betz PaperChem, 11112., Jacksonville,

trostatic-Printed Secondary Fiber", TAPP] Proceedings,

1938 pulping confercnce, pp, 95-100,

Fla.

Primary Examiner--Peter Chin

[2]] Appl' No: 691210

[22] Filed:

Apr. 25, 1991

A. PaiROfT

[51] git. Clci5 ............................................. nigggCl

iii} F5111.;8x11"Ii:3:..............::::::::::::: .......... 3162/5

_

[56]

Attorney, Agent, or FirmAlexander D. Ricci; Richard

References cued
U.S. PATENT DOCUMENTS

[57]

ABSTRACT

Acomposmonandmemodfordmkmgdryeke
trostatic printed wastepaper is disclosed. The composi

tion comprises a combination of: (1) aliphatic petroleum

distillates, (2) an alkylphenoxypoly-(ethyleneoxy) etha

3.635,789 1/1972 Green .................................... .. 162/5

4.162.186 7/1979 Wood et a1.
162/7

m1 and (3) 3 cthmylmd polycxypmpylcne glyml'

The method comprises administering a sufficient

4.276.118

amgunt of this combination to a sample of electrostatic

6/198] Quick ................................ ._ 162/5

4.518459 5/1985
4.561.933 12/1985

Freis et a1. ........................ .. 162/5

Wood 6181. .......................... .. 162/5

4.666.558
4.820.379 4/1989
5/1987 Wood
Darlington
8161. ............................ .. 162/5

timed was: a e, f r wh h mam] '

p P
0
1
en 5 dewed

8 Claims, N0 Drawings

5,141,598

glomeration at an ambient pH, alleviating the need for

PROCESS AND COMPOSITION FOR DEINKING
DRY TONER ELECTROSTATIC PRINTED
WASTEPAPER

caustic or acid tanks in the mill environment.

SUMMARY OF THE INVENTION

The components of the present invention comprise

BACKGROUND OF THE INVENTION

(l) aliphatic petroleum distillates (solvent), (2) an alkyl

phenoxypoly(ethyleneoxy) ethanol (surfactant) and (3)
an ethoxylated polyoxypropylene glycol (surfactant).

Dry toner electrostatic printing inks, including laser

and xerographic inks, are important and growing con~

All components are commercially available.
taminants in the area of wastepaper recycling. Tradi~
tionally, paper has been printed with water or oil-based 10
DETAILED DESCRIPTION OF THE
inks which were adequately removed by conventional
INVENTION

deinking procedures. In these methods, secondary ?ber

The present inventors have discovered that the addi

is mechanically pulped and contacted with an aqueous
tion of a speci?c solvent/surfactant blend to the pulper
medium containing a surfactant. Ink is separated from
signi?cantly enhances the agglomeration of electro
pulp ?bers as a result of mechanical pulping and the
static toner particles, allowing for their separation from
action of the surfactant. The dispersed ink is separated
?ber through centrifugal cleaning and/or screening.
from pulp ?bers by such means as washing or ?otation.
This agglomeration is anticipated to be seen at pH levels
Conventional deinking processes have shown mini
ranging from 5.0 to 11.0, with no signi?cant deposition
mal success in dealing with dry toner electrostatic print
ing inks, with the necessary chemical and mechanical 20 of ink expected to be present on pulping equipment. (A
pI-l higher than 11.0 or lower than 5.0 is also believed to
treatments of the furnish proving to be time consuming
and often rendering a furnish which is unacceptable for
be effective). The formulation allows for agglomeration
many applications. The development of a deinking pro
at an ambient pH, alleviating the need for caustic or
gram for office waste contaminated with electrostatic
acid tanks in the mill environment.
printed copy will make this furnish more amenable to 25
The aliphatic petroleum distillates (A) are saturated
the recycling process.
hydrocarbons having carbon numbers in the range of
The ability to recycle office waste will prove com
C9-Cl2. The chemical structures of the remaining raw
mercially advantageous and will have a signi?cant im
materials are as follows:
pact on the conservation of virgin ?ber resources. Al
though electrostatic printed waste has not reached the

Alkylphenoxypoly-(ethyleneoxy) ethanol

volume of impact printed waste commonly seen in the

industry, indications are such that usage of electrostatic

CXHZX+ 1"C6H4O-(CH2CH2O),,l-l

print is increasing steadily and that waste copies avail

n = l-6

able to the recycling industry will also increase.

x = 8-12

The present invention enhances the agglomeration

and subsequent removal of electrostatic toner particles

Ethoxylated Polyoxypropylene Glycol

through centrifugal cleaners by using speci?c combina~

tions of commercially available raw materials (solvents
and surfactants). It is believed that this can be accom

plished at a wide range of pH levels (5.0 to 11.0) and

will render a furnish that is virtually free of electrostatic
printing ink after subsequent mechanical treatment. The

invention allows for the separation of ink particles and

associated binder from pulp ?bers, and causes the parti

For the application of electrostatic toner particle

cles to agglomerate to a critical range of size and den 45 agglomeration, the effective hydrophile-lipophile bal
ance of the tested surfactants is less than or equal to 10.
sity, which affords their most efficient removal from the

It is believed that the effective temperature range for

the agglomeration of electrostatic toner particles is
from ll0-l90 F.

pulp slurry by centrifugal cleaners.

The present invention demonstrates that a combina
tion of solvents and surfactants with low HLBs enhance

the agglomeration of electrostatic toner particles, al

lowing removal through centrifugal cleaning and/or

50

A beaker test method was utilized to determine the

impact of various raw materials on toner agglomeration

without the presence of ?ber. This method allowed for
the visual evaluation of toner con?guration after treat

screening. HLB is an abbreviation for hydrophile-lipo

phile balance as related to the oil and water solubility of
ment and permitted the particles to be sized using the
a material. A high HLB indicates that the hydrophilic
portion of the molecule is dominant, while a low HLB 55 Brinkmann Particle Size Analyzer. When raw materials

indicates that the hydrophobic portion of the molecule

is dominant. The water solubility of materials increases

were screened using this method, those demonstrating

signi?cant particle agglomeration were advanced to the

Deinking/Repulping Apparatus (the pulper) for an

with increasing HLB. Traditional deinking processes
evaluation of performance in the presence of ?ber.
utilize a wide variety of high HLB (generally greater
than 10) nonionic and/or anionic surfactants or disper 60 The experimental procedure was as follows: Approx
sants to wet and disperse ink particles to a range of size

imately 0.01 grams of toner was added to a beaker con

(about 0.5 to 15 microns) which allows for their most

taining 100 milliliters of deionized water. Each solution

efficient subsequent removal by washing and/or froth

of toner and water was mixed on a magnetic stirrer at a

pH of 7.0, a temperature of 150 F. and a contact time of

?otation processes.
Agglomeration is anticipated to be seen at pH levels 65 60 minutes. About 5l4 parts of raw material or experi
ranging from 5.0 to 11.0, with no signi?cant deposition
mental product per million parts of solution was added
of ink expected to be present on pulping equipment. The
to the beaker. Upon completion of contact time, particle
advantage of this formulation is that it allows for ag
con?gurations were noted, and solution were ?ltered

5,141,598

and held for size evaluation using the Brinkmann Parti

appended claims and this invention generally should be

cle Size Analyzer.

construed to cover all such obvious forms and modi?ca

tions which are within the true spirit and scope of the

The pulper was then used to evaluate selected raw

materials. This apparatus consists of a Waring blender

present invention.

jar with the blades reversed to provide a mixing action

of the ?bers. The stirring of the blender is controlled by

We claim:

1. In the deinking of electrostatic printed wastepaper,

a process for enhancing the agglomeration of electro
static toner particles, said process comprising adding to
an aqueous slurry of the electrostatic printed wastepa

a motor connected to a Servodyne controller. Tempera

ture of the pulp in the blender is provided by a heating

mat attached to a temperature controller. The typical

furnish consistency in the laboratory pulper is 5%, and

per an amount, sufficient for deinking of a combination

a stirring speed of 750 rpm is used to simulate the me

chanical action of a hydropulper.
Electrostatic printed wood-free ?ber was used as the

of (a) aliphatic petroleum distillates, (b) an alkylphenox

ypoly-(ethyleneoxy) ethanol and (c) an ethoxylated

polyoxypropylene glycol, the hydrophile/lipophile

furnish. Twenty pounds of raw material or experimental

balance of both (b) and (c) being less than or equal to 10,

product per ton of ?ber were added to the pulper, at a

and the weight ratio of (a):(b):(c) being about 6:1:3.

temperature of 150' F., a pH of 7.0, and a pulping time

of 60 minutes.

2. The process as recited in claim 1 wherein the ali

phatic petroleum distillates are saturated hydrocarbons

having carbon numbers in the range of C9-C12.

DESCRIPTION OF THE PREFERRED

EMBODIMENT
3. The process as recited in claim 1 wherein the alkyl
20
phenoxypoly-(ethyleneoxy) ethanol is a compound of
The laboratory results found in Table 1 demonstrate
the formula
the effectiveness of the present invention. A nonyl
phenoxypoly(ethyleneoxy) ethanol with a molecular
weight of 286 and an ethoxylated polyoxypropylene
glycol with a molecular weight of 3800 are preferred 25
with n from 1 to 5.

components.

4. The process as recited in claim 1 wherein the eth

TABLE 1

oxylated polyoxypropylene glycol is a compound of the

Pulper Results at 150 F.. pH 7.0. 60 Minute Pulping Time

HLB
Minimum Particle
Condition
of Material
Size (Microns)
Untreated Control
20 lbs/ton Nonylphenoxypoly~

0
14.2

l-2
4.5

8.8

l0.0

4.6

15.0

1.0

18.0

'

40.0

formula

(ethyleneoxy) ethanol
(Mol. Wt. 748, n = 12)

20 lbs/ton Nonylphenoxypoly-

(ethyleneoxy) ethanol

35 with n from about 1 to 45 and m from about 14-77.

5. The process as recited in claim 1 wherein agglom

eration of electrostatic toner particles occurs at a'pH of

(Mol. Wtv 396. n = 4)

20 lbs/ton Nonylphenoxypoly-

about 5.0 to 12.0

6. The process as recited in claim 1 wherein agglom
eration of electrostatic toner particles occurs at a tem
perature of about 110 to 190 F.
7. The process as recited in claim 1 wherein the alkyl

(ethyleneoxy) ethanol
(B. MOI. Wt. = 286, n = L5)

20 lbs/ton Ethoxylated

Polyoxypropylene Glycol
(C, Mol. Wt. = 3800)
20 lbs/ton Formulation

(60% A: l0% B: 30% C)

phenoxypoly-(ethyleneoxy) ethanol is a compound of

the formula

An HLB cannot be accurately calculated for a blended formulation.

45

Note the effectiveness of each material (e. g., B and C) in

increasing laser ink particle size, as compared to the
untreated control. However, the experimental formula
tion in its preferred ratios (60% A/ 10% B/30% C)

with n from 1 to 5, and the ethoxylated polyoxypropyl

ene glycol is a compound of the formula

showed a signi?cant increase in particle size as com 50

pared to individual components.

CH3

The effective ratio range of each of the raw materials

in the formulation is believed to be:

'

HOCHICHZCHICH2O)R(CHZCHO)M(CHZC20),[CH2CH2OH

10-60% Aliphatic Petroleum Distillates

10-89% Alkylphenoxypoly-(ethyleneoxy) ethanol

with n from about 1 to 45 and m from about 14 to 77.

l80% Ethoxylated Polyoxypropylene Glycol

8. The process as recited in claim 1 wherein agglom

eration of electrostatic toner particle's occurs at a pH of
While this invention has been described with respect
to particular embodiments thereof, it is apparent that
about 5.0 to 12.0 and a temperature of about 110 to 190'
F.
numerous other forms and modi?cations of this inven
O
Q
t
C
l
tion will be obvious to those skilled in the art. The 60

65