Deinking Studies at TCIRD

PULPING AND BLEACHING DIVISION

 Optical Properties of pulp from different mills
Particulars B. UV B. with B. at F. % W. % L a b Dirt Ash
Excluded UV % 100% Count content
% UV %
Pulp from 76.63 80.61 88.99 12.35 106.38 91.49 1.84 -5.62 154 5.3
Emami
Pulp from 74.86 78.11 84.58 9.61 95.48 91.05 0.94 -3.60 164 9.3
Rama
(Surat)
Pulp from 84.38 89.34 100.25 15.80 120.61 94.91 2.13 -7.37 271 2.4
Century
Emami 80.33 85.34 95.88 15.55 -- -- -- -- 51 20.6
Paper

Physical Properties of pulp from different mills

Particulars GSM Bulk Tensile Tear Burst Porosity Smoothness Double
Index Index Index fold

Pulp from 73.75 1.69 15.17 6.2 1.1 3.11 418 5

Emami
Pulp from Rama 70.75 1.68 22.10 7.3 1.4 3.02 220 5
(Surat)
Pulp from 68.3 1.51 27.16 7.5 1.8 6.65 200 11
Century
Emami Paper 74.8 1.35 19.94 3.7 1.3 6.21 184 8
Suggestions during the last presentation
 Check (visually) the pulp for rejects after 5,10,15 min . of
pulping by passing through 22mesh under flow of water.
 Perform the complete deinking experiments for one sided
printed , 2 side printed SOP from the same stock and
compare it with the stock (SOP) obtained from the mill.
 Perform some dummy experiments to generate filtrates of
flotation 1& 2.Flitrates to be stored in cold room.
 Not to use filtrate of flotation 1 in flotation 2,instead use
flotation 2 filtrate in flotation 1.
 Filtrate of flotation 1 can be used in pulping and screening.
 Use fresh water in only bleaching stages
 Optimization of pulping time(for pulper
fabricated in TCIRD)

Particulars SET 1 SET 2 SET 3

Pulping Time, min. 5 10 15

Consistency, % 10 10 10
Sodium hydroxide, % 1.5 1.5 1.5

Sodium silicate, % 1.0 1.0 1.0

pH 10.5-11.2 10.5-11.2 10.5-11.2

Surfactant,% 0.04 0.04 0.04
Water used Flotation Flotation Flotation

Rejects/… gm O.D. 3.2/16.3 1.7/18.2 0.2/19.1

Rejects/330 gm O.D. 64.7 30.8 2.01

Rejects after 5,10,15 min . of pulping by passing through 22mesh under flow of water.
Pulping Course Flotation Fine P Bleaching
Screening 1 Screening

IF 1 OF 1
Dilution at 1% IF 2

Dilution at 1% (flotation2)
Flotation
2
Simulation of deinking loop at lab scale
OF 2

Reductive
bleaching

Raw Materials to be studied:

•Mixed Office Waste (received from Rama Newsprint, Surat)
•Coated Book Stock (received from Rama Newsprint, Surat)
To be used alone and in different combinations (mixed in different ratio)
 Consistency Water used(back Comments
% water)
Pulping 10 ~3 litres (Flotation 1)
Flotation 1 1.0 ~29 litres (Pulping 1 dummy experiment only to
+Flotation2) generate back water
Screening -- N.A.( 27 litres from
flotation 1)
P bleaching 15 Fresh One dummy( same conditions with
same back water) experiment to
generate 300 gm of pulp for
Flotation 2
Flotation2 1.0 ~29 litres (Fresh 1 dummy experiment only to
+Flotation2 in 50:50) generate back water

Red. 4.0 Fresh

Bleaching
In every stage it requires filtering ,wt, dryness for yield calculation.
To complete one experiment we have to perform 3 experiments
It takes 2.5 days to complete 1 experiment & 1.5 days for analysis
( Sheets, B, W, L, a ,b, Dirt, ash, strength, yield calculation).In total 9-10 days
for one simple experiment.
 Deinking Experiments
Particulars Pulping Flotation1 Screening P Flotation 2 Red.
Bleaching Bleaching

Consistency, % 10 1 -- 15 1 4
Sodium 1.5/1.0 -- -- 1 -- --
hydroxide, % /0.5
Sodium silicate, 1.0 -- -- 1.0 -- --
%
pH 9.4 -11.2 7.0 -- 10.5-11.2 7.0 4.0
Surfactant,% 0.04 0.04 -- -- 0.04 --
Hydrogen -- -- -- 1.5 -- --
Peroxide,%
Sodium -- -- -- -- -- 1.0
dithionite, %
Air flow , l/min. -- 12 -- -- 12 --

Water used Flotation Pulping1+ Flotation Fresh Flotation Fresh

1 flotation 2 1+ fresh 2+ fresh
 MOW 2 MOW 3 MOW 4 MOW 8 MOW 6
Particulars ( 1.5% ( 1.0% NaOH) ( 0.5% (Two sided (No
NaOH) no no sorting NaOH) no print) sorting)
sorting sorting

PULPING
Consistency, % 10 10 10 10 10

Sodium
1.5 1.0 0.5 1.5 1.5
hydroxide, %
Sodium silicate,
1.0 1.0 1.0 1.0 1.0
%
Surfactant,% 0.04 0.04 0.04 0.04 0.04

Hydrogen
-- -- -- -- --
Peroxide,%
Pulping time
15 15 15 15 15
,min.
Water used Fresh Fresh Fresh Flotation Flotation
 MOW 2 MOW 3 MOW 4 MOW 8 MOW 6
Particulars
( no sorting) ( no sorting) ( no sorting) (Two sided (No sorting)
print)

PULPING
Sodium
1.5 1.0 0.5 1.5 1.5
hydroxide, %
Brightness UV
73.87 73.0 72.72 66.55 72.88
Excluded %
Brightness with
76.91 76.5 75.99 70.88 75.96
UV %
Whiteness % 109.5 104.4 103.42 87.71 107.73
L 89.8 89.6 89.24 84.58 89.48

a 2.83 1.87 2.84 2.18 1.89

b -7.15 -5.6 -6.2 -4.62 -6.86

Dirt Count/No.
5648 5963 6166 11409 6209
Of specks
Ash content % 14.4 14.73 15.21 15.98 14.78
 MOW 2 MOW 3 MOW 4 MOW 8 MOW 6
Particulars
( 1.5% NaOH) ( 1.0% NaOH) ( 0.5% NaOH) (Two sided (No sorting)
no sorting no sorting no sorting print)

Flotation 1
In pulping
Sodium 1.5 1.0 0.5 1.5 1.5
hydroxide, %
Consistency,
1 1 1 1 1
%
Sodium -- -- -- --
--
hydroxide, %
Sodium -- -- -- -- --
silicate, %
Surfactant,% 0.04 0.04 0.04 0.04 0.04
Hydrogen
-- -- -- -- --
Peroxide,%
Pulping + Pulping + Pulping + Pulping + Pulping +
Water used
Fresh Fresh Fresh Flotation 2 Flotation 2
 MOW 2 MOW 3 MOW 4 MOW 8 MOW 6
Particulars
( 1.5% NaOH) no ( 1.0% NaOH) ( 0.5% NaOH) (Two sided (No sorting)
sorting no sorting no sorting print)

Flotation 1
In pulping
Sodium 1.5 1.0 0.5 1.5 1.5
hydroxide, %
Pulping + Fresh Pulping + Fresh Pulping + Pulping +
Water used Pulping + Fresh
Flotation 2 Flotation 2
Brightness UV
78.2 76.4 75.11 69.85 74.67
Excluded %
Brightness with
82.3 80.3 79.6 73.65 79.02
UV %
Whiteness % 103.5 108.27 107.9 103.16 106.14
L 92.4 91.31 90.56 88.32 91.40
a 1.7 2.81 3.54 2.55 2.97
b -4.7 -6.65 -6.49 -6.35 -5.81
Dirt Count/No.
974 1100 1132 2742 952
Of specks
Ash content % 7.8 8.69 9.22 9.78 8.47
 MOW 2 MOW 3 MOW 4 MOW 8 MOW 6
Particulars
( 1.5% ( 1.0% NaOH) ( 0.5% NaOH) (Two sided (No sorting)
NaOH) no no sorting no sorting print)
sorting

Peroxide Bleaching
Consistency, % 15 15 15 15 15
Sodium
1.0 1.0 1.0 1.0 1.0
hydroxide, %
Sodium silicate, 1.5 1.5 1.5 1.5 1.5
%
Surfactant,% -- -- -- -- --
Hydrogen
1.5 1.5 1.5 1.5 1.5
Peroxide,%
Water used Fresh Fresh Fresh Fresh Fresh
pH 10.7 10.5 10.5 10.7 10.7
 MOW 2 MOW 3 MOW 4 MOW 8 MOW 6
Particulars
( 1.5% ( 1.0% NaOH) no ( 0.5% NaOH) no (Two sided (No sorting)
NaOH) no sorting sorting print)
sorting

Peroxide Bleaching
Brightness UV
Excluded % 79.9 77.84 77.41 73.37 77.64

Brightness with UV
% 84.1 81.46 81.29 77.81 80.37

Whiteness % 104.8 104.4 100.64 103.25 98.64

L 93.1 92.3 92.51 89.32 91.3
a 1.6 2.5 2.39 1.86 2.47
b -4.7 -3.73 -4.07 -6.66 -5.64
Dirt Count/No. Of
specks 920 967 909 2503 1108

Specks area, mm2

m (filled)
/ 2 49.6 38.9 28.1 -- --

Specks area, mm2

m (Holey)
/ 2 49.62 38.7 28.1 -- --
 MOW 2 MOW 3 MOW 4 MOW 6 MOW 6
Particulars
( 1.5% NaOH) ( 1.0% ( 0.5% NaOH) (Two sided (No sorting)
no sorting NaOH) no no sorting print)
sorting

Flotation 2

Consistency, % 1 1 1 1 1

Sodium -- -- --
-- --
hydroxide, %
Sodium silicate, -- -- -- -- --

%
Surfactant,% 0.04 0.04 0.04 0.04 0.04

Flotation 1 + Flotation 1+ Flotation 1+ Flotation 2 + Flotation 2 +

Water used
Fresh Fresh Fresh Fresh Fresh
 MOW 2 MOW 3 MOW 4 MOW 6 MOW 6
Particulars
( 1.5% NaOH) ( 1.0% NaOH) ( 0.5% NaOH) (Two sided (No sorting)
no sorting no sorting no sorting print)

Flotation 2
81.1 78.7 77.98 75.37 78.64
Brightness UV
Excluded %
Brightness with 85.3 83.17 82.86 80.21 83.37
UV %
105.5 105.82 101.94 97.34 104.64
Whiteness %
93.8 93.02 92.71 89.32 92.9
L
1.58 3.03 3.3 1.86 3.4
a
-4.5 -5.8 -3.7 -6.66 -5.64
b
351 374 325 951 652
Dirt Count/No. Of
specks
15.34 16.36 9.88 -- --
Specks area,
mm2 /m2 (filled)
15.32 13.34 9.88 -- --
Specks area,
mm2 /m2 (Holey)
5.1 4.7 4.82 -- --
Ash content %
 MOW 2 MOW 3 MOW 4 MOW 6 MOW 6
Particulars
( 1.5% ( 1.0% ( 0.5% (Two sided (No
NaOH) no NaOH) no NaOH) no print) sorting)
sorting sorting sorting

Reductive Bleaching (Dithionite)

Consistency, % 4 4 4 4 4

Sodium -- -- -- --
--
hydroxide, %

Dithionite,% 1.0 1.0 1.0 1.0 1.0

Water used Fresh Fresh Fresh Fresh Fresh

 MOW 2 MOW 3 MOW 4 MOW 6 MOW 6
Particulars
( 1.5% NaOH) ( 1.0% NaOH) ( 0.5% NaOH) (Two sided (No sorting)
no sorting no sorting no sorting print)

Reductive Bleaching (Dithionite)

Brightness UV
85.3 83.5 81.955 79.12 82.98
Excluded %

Brightness with UV % 89.2 87.8 86.3 84.25 87.6

Whiteness % 108.8 106.5 107.6 102.57 107.1

L 95.6 94.4 94.6 91.34 94.1

a 1.4 1.66 1.76 1.86 2.1

b -4.4 -5.12 -4.63 -6.2 -5.27

Dirt Count/No. Of
241 150 153 478 341
specks
Specks area, mm2 /m2
10.5 7.602 7.4 -- --
(filled)
Specks area, mm2 /m2
10.4 7.604 7.43 -- --
(Holey)
Ash content % 4.9 3.5 4.9 -- --
Brightness % (UV Excluded) at different stages
Brightness % (UV Excluded) at different stages
Dirt/Speck count at different stages
Dirt/Speck count at different stages
 Salient Findings
 There was a difference of 3.86 points of brightness (79.12
to 82.98) in case of double side printed raw material as
compared to as such (having both single as well as double side printed SOP)
respectively with usage of back water.
 There was a difference of 3.35 points of brightness (81.95
to 85.3) as the dose of alkali was increased from 0.5 to
1.5%.
 Around 3 % loss of brightness was there when back water
was used in flotation processes.
 Dirt/Specks increased in case of deinking of two sided
printed material.
 Parameters targeted for specific raw Material
Targets Sorted office pack: Coated Book Stock
Brightness %
Target brightness at OF1 73-75% UV excluded 78% UV excluded
( Outlet of flotation 1)
Target brightness at outlet of P bleaching 76.78% UV excluded 81% UV excluded
Target brightness at OF2 77-79% UV excluded 83% UV excluded
( Outlet of flotation 2)
Target brightness 81-83% UV excluded No need for Dispersion 2
( Outlet of Dispersion 2)
No. of Specks (≥100µm)
No. of specks per m2 1100-3000 4000-7000
( Outlet of Flotation 1)
No. of specks per m2 600-700 Less than 200
( Outlet of Flotation 2)
Specks area (≥100µm)
Specks area (≥100µm)After flotation 1 400-600 200-400
Specks area,mm2/m2 (≥100µm)After flotation 2 ~100 ~100
Specks area,mm2/m2(≥100µm)After dispersion Less than 100 No Dispersion 2 stage
2
Yield%
Yield % (Pulping) Presently No fixed target Presently No fixed target
Yield % (Flotation 1) 90.0-92.0 82.0-84.0
Yield %( Flotation 2) 96.0-98.0 94.0-96.0
Total Yield % 65-68 68-72
 Raw Materials available
S.l.N Type of recovered paper Wt (Kg)
o.
1. Multi grade (Emami) 11.293
2. Coated Book stock ( Rama) 9.760
3. Sorted Office Pack ( Rama) 2.800
4. Old Record ( Rama) 7.817
5. Old Record ( Emami) 6.242
6. Magazine grade (Indigenous) 5.672
7. Old Newsprint (Indigenous) --

Separately and in combination of different ratios (Mill specific or

otherwise)
 Research areas
1. Optimization of process conditions (raw material ratio, pH, alkali
dose, air flow, flotation selectivity, bleaching ,dispersion) to
achieve final brightness to the maximum level without
compromising the pulp yield.
2. Enzymatic deinking of mixed office waste and newsprint (by
using commercial enzymatic products)

3 Part A: Identification ,characterization & measurement of stickies

(macro as well as micro) by using different methods.

3 Part B: Product Development for sticky control

4. Isolation ,biochemical characterization , purification of alkali

stable cellulases and formulations of enzymatic products for
deinking of recycled fibre.

5. Yield improvement in deinking of mixed office waste.

6. Waste water treatment through dissolved air flotation.

 Dissolved Air Flotation
•Physical process

•Separation of suspended solids and dispersed liquid from a

liquid by addition of saturated air-water mixture which
releases micro bubbles.

•Skimming operation removes the particles floated to the

surface.
Flow diagram
 33
Partners in
Industrial Progress
 Physical Properties at different
stages

Particulars GSM Bulk Tensile Tear Burst Porosity Smoothness Double

Index Index Index fold

Final pulp 73.9 1.64 26.07 7.7 1.7 3.24 347 9

(MOW 2)
Final pulp 74.5 1.60 25.47 7.5 1.8 3.47 371 17
(MOW 3)
Final pulp 71.8 1.63 23.57 7.4 1.6 4.12 304 11
(MOW 4)
 WORK SCHEDULE
S. No Activity Q1 Q2 Q3 Q4 Q5 Q6 Q7 Q8
i Procurement of enzymes, evaluation of __
enzyme/ enzyme components for deinking of
waste paper
ii Selection of best enzymes and optmzn. of _______
process conditions and determination of best
stage for enzyme addition
ii Selection of suitable dispersants & optmzn. ___________
of flotation conditions, bleaching conditions
and bleach dosings
iv Evaluation of deinking efficiency by redn. in
residual ink, chemicals & ash content, _______
brightness gain, and flotation efficiency;
study of drainage & strength properties of
deinked pulp
v Study on the effect of fibre furnish and fillers, _______
sizing agents, additives on the efficiency of
enzymes
vi Study of enzymatic deinking with different _______
types of waste paper
vii Analysis of data and report writing __
A variety of enzymes have been used for deinking, which includes: Cellulases,
Hemicellulases, Lipases, Esterases, Pectinases, Amylases & lignolytic
enzymes
Hemicellulases, cellulases & Lignolytic enzymes alter the fiber surface or
bond in the vicinity of ink particles, thereby freeing the ink for removal by
washing or flotation
Amylase enzyme influence the degradation of starch layer on the surface of
the paper. The toner particle adhering to the paper surface released by the
enzymatic treatment undergoes subsequent separation from the pulp
suspension via flotation
Amylase facilitates the removal of small ink particles
Amylase and cellulase also combine synergistically, increasing the effect of
each other
Enzymatic deinking formulation can replace all other
deinking agents traditionally used in the pulper and make
the deinking chemistry much simpler and easier to control
• Reduce dirt counts
• Improve pulp brightness and yield
• Cost Reduction
• Reduce or eliminate the use of defoamers
• Environmental friendly
 Objective
To develop enzymatic deinking as an alternative technology for up gradation of
different grades of waste papers especially difficult to deink papers like MOW,
SOW & Laser Waste.

1. Selection of appropriate enzymes/enzyme combinations for deinking

according to paper grade and print technology

2. Determination of optimum process conditions for enzymatic deinking

3. Evaluation of enzymatic deinking on paper production rate, paper

quality and effluent water quality
 Objective

• Optimization of raw material ratio

• Optimization of the pulping phase

• Improvement in flotation selectivity

• Bleaching optimization

• Dispersion optimization
Achieve final brightness to the maximum level depending on the
raw material without compromising the pulp yield
•Reduced chemical consumption

•Reduced cost

•Reduced pollution

• Increased pulp quality

 The recycling industry is in search of new technologies,
which can improve the quality, reduce the production cost
and can be accommodated easily in to the existing process
design. Recent research with enzymes showed that enzymatic
deinking may be an alternative solution.
 Enzymatic Deinking with cellulase, xylanase, amylase and
lipase enzyme separately and in combinations
 Synergistic application of different enzymes and compatible
surfactants
• Enzyme Dosing point
• Enzyme - Surfactant Synergy
• Enzyme dose/Enzyme combinations
• Enzyme Retention time
• Pulping/Slushing time
• Mixed Office waste (MOW)/Sorted Office Pack (SOP)

• Coated Book Stock (CBS)

• Old Newsprint (ONP)

• Old Magazine grade (OMG)

• Laser Waste (LW)

Separately and in combination of

different ratios (Mill specific or otherwise)

Consistency, %: 10 – 15

Soaking time, min.: 20 – 30

Slushing/ Pulping time, min.: 20 – 30

Temperature ,°C: Ambient – 70

Optimization of the pulping/flotation phase

Measurement of
• Optical Properties (Brightness, L*, a*, b* etc.)
• ERIC value
• Dirt/Speck Count
• Pulping Yield