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Amazon Papyrus Chemicals (Thailand) Co. Ltd 12 t h Floor, Boonmitrr Building 138 Silom Road,

Amazon Papyrus Chemicals (Thailand) Co. Ltd 12 th Floor, Boonmitrr Building 138 Silom Road, Thailand Tel: (66 02) 634 3495-8 Fax: (66 02) 634 3499

Activated Filler - Increasing Filler Levels

Presented at Asian Paper 2012, Bangkok

Peter de Clerck Business Development Manager, Amazon-Papyrus Chemicals

Abstract:

The communications paper sector is under increasing price pressure, white paper producers are looking to cheaper furnishes and higher filler contents. Increased filler addition leads to reduced retention and weaker paper. The Activated Filler concept reduces these negative effects by directly treating the filler to a) reduce interference with fibre-to-fibre bonding b) make micro-agglomerated filler itself a bonding centre As a result the filler retention is improved and white water becomes cleaner. The principles behind these improvements and the effects on strength and optical properties are presented and explained. The differing roles of GCC and PCC in such systems are examined.

Introduction

Mineral pigments are used to improve functional paper properties such as appearance, sheet formation, smoothness, dimensional stability, brightness, opacity and printability. Pigments are also added as fillers or adulterants to reduce the furnish costs by replacing more expensive fibre components.

Increasing filler content affects several areas of paper production, including runability, energy demand, retention, formation, sheet strength, caliper, porosity, optical properties and so forth. Papermakers seeks to obtain the benefits of increased filler content while minimising any negative impact.

AREA OF CONCERN

EFFECT OF INCREASING FILLER CONTENT

Wet end

Wet web strength reduced

Retention

FPR reduced

Drainage

Increased drainage rate

Formation

Can be beneficial or detrimental

Chemical demand

May increase due to larger surface area

Clothing

Dramatically increased wire abrasion, felt filling.

Dry end surface strength

Increased dusting and fluffing due to the reduction in surface pick strength

PAPER PROPERTIES

Strength

Tensile and burst reduced

Bulk

Decreased

Stiffness

Decreased

Two sidedness

Increased difference

Table 1 Some problems associated with increased filler contents.

It is necessary to understand why increasing the filler loading affects these parameters.

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Effects of Filler

Increased Surface Area

Effects of Filler Increased Surface Area Filler has a much higher specific surface area than fibre,

Filler has a much higher specific surface area than fibre, so adding filler increases the specific surface area of the furnish. This increased surface area reduces the efficiency of adsorbed wet end chemicals e.g. sizing chemicals and strength agents. The greater the surface area increase, the greater the impact. This may be seen for example in sizing demand.

the impact. This may be seen for example in sizing demand. Fig. 1 – The effect
the impact. This may be seen for example in sizing demand. Fig. 1 – The effect
the impact. This may be seen for example in sizing demand. Fig. 1 – The effect

Fig. 1 – The effect of increased surface area on size efficiency (1)

Bonding Disruption

The most obvious effect of adding filler is the reduction in sheet strength.

Effect of Filler on Burst Strength

100% Dispersed Clay 90% 80% 70% 60% 50% 40% 30% 20% 10% 0% 0% 5%
100%
Dispersed Clay
90%
80%
70%
60%
50%
40%
30%
20%
10%
0%
0%
5%
10%
15%
20%
25%
30%
35%
% of Original Burst

Clay loading

Fig. 2 – The effect of increased filler loading on burst strength (2)

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The strength loss is particularly notable as there is both a decrease in the number

The strength loss is particularly notable as there is both a decrease in the number of fibres in the sheet and a reduction of fibre-fibre contact area.

Beazley, Dennison and Taylor (1979) (3) demonstrated a linear inverse relationship between tensile strength and filler specific surface area.

Papermakers have long added starch and gums to increase paper strength, notably to compensate for the loss of

bonding when adding filler. An early Chinese formula for paper requires three materials – fibre, kaolin and starch. Strength agents were normally added to the thick stock and there adsorbed to the surfaces of the furnish components. Selective treatment of furnish components has been proposed e.g. US patent 2,140,394 was issued

to Ruff in 1938 for cooking starch together with filler to improve paper strength

(4)

.

Starch-Filler Composites

Starch was found to be highly effective in filler modification. It can be anchored on the filler surfaces or used to encapsulate the filler particles to enhance fibre-filler bonding. Some patents call for filler to be mixed with starch before cooking, the starch then being partially cooked. This procedure produces a sticky starch-pigment aggregate and will generate “fish-eyes” if not well dispersed. Other patents call for the partially cooked starch-pigment gel to be dried and then ground before being re-introduced to the furnish. Yet other patents call for the insolubilisation of the starch in situ by adding cross-linking agents or stearates. (5 - 9) .

cross-linking agents or stearates. ( 5 - 9 ) . Fig. 3 – Coatd filler (

Fig. 3 – Coatd filler (10)

Optical properties such as opacity and brightness decrease when large amounts of starch are incorporated into the sheet.

Filler modification using the starch-gel coating method can improve fibre-filler bonding but does not produce robust filler flocs. When cationic starch is used in this process the generated composites will be of similar cationic charge and so repel each other. Retention to the anionic fibre surfaces is favoured. When non-ionic starch is used to treat fillers, retention is dominated by filtration mechanisms only.

Paper Strength

Paper strength is largely determined by the number, strength and distribution of bonds between the sheet components. The most important of these is the contribution from inter-fibre bonding and the bonding distribution network (i.e. formation).

Hydrogen bonds predominate in paper, forming and strengthening during sheet consolidation, dewatering and drying. Fibre surfaces must come into close proximity for hydrogen bonds to form, filler particles may easily disrupt fibre-fibre bond formation. Interference may come from both fibre separation (large particles may increase fibre separation distances) and surface coverage (coverage of fibre surfaces occludes bonding sites).

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How the filler is located within the paper is important. Eklund at al. (1991) (

How the filler is located within the paper is important. Eklund at al. (1991) (11) stated that fillers can be incorporated in a fibre structure in three different ways, each having a different impact on the paper properties.

each having a different impact on the paper properties. Fig. 4 – Fillers Incorporated in a

Fig. 4 – Fillers Incorporated in a Fibre Structure

1. Expansion: Filler expands the fibre network and thus lowers its density. The expansion of the fibre network improves the light scattering properties of the paper. The filler particles interfere with the fibre-fibre interactions and mechanical properties are lowered as a consequence.

2. Void Filling: Filler locates in the voids between the fibres It does not interfere with fibre-fibre interactions. Mechanical properties are unaffected but the light scattering will increase. There is no volume expansion of the fibre network and the density of the paper is increased.

3. Insertion: Filler inserts between the fibres but does not result in full fibre separation The insertion of filler does not affect the overall light scattering if there are no additional voids formed. Fibre-fibre contact area is reduced, lowering the mechanical properties.

Hence the pore volume relative to unfilled papers may be higher (expansion), lower (void filling) or similar (insertion).

Particle Size

Particle size has a significant effect. For pigment particles greater than 5µm the impact is dominated by particle shape and number as large particles disrupt points of interfibre bonding (expansion). For particles less than 2µm the surface coverage effects becomes more important as fibrils and fibres become coated, preventing fibril collapse and consolidation on drying (insertion).

Papermakers are now using GCC having 60-70% particles less than 2 micron (70%<2 µm) in pursuit of enhanced optical properties of paper. Previously GCC of around 20%<2 µm was normal. Furnish specific surface areas are increased accordingly.

The selection of filler type is also important. PCC and calcined clay are aggregated fillers that have large internal void volumes. By contrast, clay and GCC are dense fillers with a high packing density, resulting in decreased bulk.

Filler Incorporation:

Great ingenuity has been applied to increasing filler levels in paper. Various methods of incorporating filler in the

, fines-filler composites (16) , filler

sheet have been explored, including lumen loading

modification (17,18) , and fiber engineering (19,20) . The reader is referred to the literature for further details on these.

(12,13)

, cell wall loading

(14,15)

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Pre-flocculation – Concept

Pre-flocculation – Concept One approach to reduce the negative effects of increased filler content is to

One approach to reduce the negative effects of increased filler content is to preflocculate the filler prior to addition to the paper stock (21-25) . The interference with fibre-to-fibre bonding is reduced, the filler aggregates are more easily retained in the web, drainage may be enhanced and less retention chemicals are needed.

may be enhanced and less retention chemicals are needed. Fig. 5 – Reduced interference from pre-flocculated

Fig. 5 – Reduced interference from pre-flocculated fillers

Mabee (26) reported that filler preflocculation could provide an approximate 26% increase in first pass ash retention and 13% increase in the tensile strength when using the same amount of filler.

The reduced surface area of the furnish and improved filler retention result in lower chemical additive requirements.

retention result in lower chemical additive requirements. Fig. 6 – The effect of pre-flocculate filler loading

Fig. 6 – The effect of pre-flocculate filler loading on burst strength (2)

Optical Properties

Light scattering is due to the reflection and refraction of light at air/cellulose, air/filler and cellulose/filler interfaces. With less coverage of the fibre surface and less air-filler interfaces, preflocculation will reduce the scattering efficiency of the pigment.

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The opacifying effects of fillers such as PCC, calcined clay and TiO 2 are greatly

The opacifying effects of fillers such as PCC, calcined clay and TiO 2 are greatly reduced by preflocculation.

clay and TiO 2 are greatly reduced by preflocculation. Fig. 7 – The effect of pigment

Fig. 7 – The effect of pigment on opacity (27)

As may be seen, both bonding and opacity are dependent on fibre-fibre bonding. There is an inverse relationship between tensile strength and opacity.

inverse relationship between tensile strength and opacity. Fig. 8 – relationship between tensile and opacity The

Fig. 8 – relationship between tensile and opacity

The strength/opacity relationship is maintained for both un-flocculated and pre-flocculated filler, confirming that the prime effect of filler preflocculation is in maintaining fibre-fibre bonding.

Hence with pre-flocculated filler we may attain similar tensile strength and light scattering at higher filler levels.

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Preflocculating Filler:

Preflocculating Filler: The flocculation treatment and shear forces encountered determine the size distribution and

The flocculation treatment and shear forces encountered determine the size distribution and stability of the flocs. Generating filler flocs of a stable size under paper machine conditions is a significant challenge. A combination of high shear stability and narrow floc size distribution is required for the success of filler preflocculation technology.

The size of the filler flocs have been shown to be very important for the tensile strength of the paper. Larger flocs promote a higher tensile strength (z-direction strength has been shown to be much less affected).

A porous floc structure will enhance optical and printing properties.

Flocculation Mechanisms:

The correct type of flocculation is important. There are four recognised types of polymer-induced flocculation; macromolecule bridging, charge neutralization, patch flocculation and network flocculation.

Coagulation Coagulation or charge neutralization occurs when the repulsive forces separating particles are overcome by poly- electrolyte addition, allowing particles to come together under the influence of the weak van der Walls forces.

Bridging flocculation The polymer has to reach across the electrical double layer of two similarly-charged particles. A polymer with high molecular weight and low charge density is preferred.

Patch flocculation Patches of the charged particle surfaces are covered by material with an opposite charge. These patches may attract oppositely charged surfaces on other similarly partially-covered particles. Generally a compound with moderate charge density and relatively low molecular weight is used.

Network flocculation Network flocculation can be induced by electrostatic interaction or by hydrogen bonding between two interacting components.

In filler pre-flocculation systems the flocculation mechanism will be either coagulation or patching. These flocs may

be disrupted by shear and subsequently reform when the shear is reduced.

Single-Polymer Flocculation (28)

Patching and charge neutralisation are the dominant floc types produced by low molecular weight polymers. Such flocs tend to have a relatively small particle size and break down under the high shear forces of a modern paper machine.

Bridging predominates in flocs formed by a high molecular weight flocculent. The flocs tend to have a broad floc size distribution that is difficult to control due to poor mixing of viscous flocculent with the pigment slurry - becoming worse at higher filler solids levels. High shear rates are needed to generate a regular floc-size distribution.

When adding a single ionic agent the charge balance of the treated system is determined by the added charge. Overall charge balance will limit the optimum treatment. This is a major concern in single-polymer systems.

Cationic Starch (24,37)

Mention should be made of cationic starch treatment. Starch may be fully or partially dispersed (depending on the starch type and cooking process) and so produces both bridging and charge neutralisation. Sheared flocs readily reform and are more stable than those formed with C-PAM.

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Dual Polymer Flocculation (29-35)

Dual Polymer Flocculation ( 2 9 - 3 5 ) Dual polymer systems comprises the addition

Dual polymer systems comprises the addition of a flocculating agent to a filler dispersion, shearing of the dispersion, addition of a second flocculating agent and then further shearing of the resultant flocs to the desired particle size. Many sources propose a weak initial flocculation followed by a robust second flocculation, the resulting slurry then being sheared to produce the desired floc size.

Dual polymer systems produce flocs with better shear stability and a narrower particle size distribution than flocs from single polymer systems.

MicroPolymers (36)

Microparticles and micropolymers may also be used alone or with other polymers to produce flocculated pigment slurries. Flocs formed by micro-particle bridging may have the same large, open structure as those formed by bridging polymers but with the added advantage of floc reformation after shearing.

Reported Benefits of Preflocculation:

A

series of benefits are reported for preflocculated filler, including

o

internal bonding is maintained / enhanced

o

equivalent strength and opacity achieved at higher filler contents

o

filler retention, formation and drainage are improved

o

energy savings in refining due to higher strength / less fibre

o

better press dewatering

o

energy savings in drying

o

improved wet web strength

Encapsulated Filler

Paper Strength

In papermaking practice, dry strength aids have long been used to compensate for the loss of paper strength due

to filler loading. Preflocculated filler alone allows for just a few percentage points increase in filler loading.

Filled paper is a composite material. Bonds between all furnish components play a contribution. Thus far we have focused on fibre-fibre bonds. Fibre-filler bonds and filler-filler bonds also contribute to paper strength. Of these bonds, filler-filler bonds will be the weakest.

fibre-filler bonding fibre-fibre bonding filler-filler bonding
fibre-filler
bonding
fibre-fibre
bonding
filler-filler
bonding

Fig. 9 – Bonding Issues

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In a highly oriented paper the mode of failure in MD tensile is mainly the

In a highly oriented paper the mode of failure in MD tensile is mainly the shearing of inter-fibre bonds. As bonding increases fibre failure will eventually predominate. For Z-direction tensile the mode of failure is adhesive failure (between two elements) or cohesive failure (within an element, layer or film). CD tensile is a combination of these two failure modes.

Fibre-fibre bonds may be increased in a number of ways and are not reviewed here. Fibre-filler bonds may be improved by starch and other dry strength additives previously adsorbed on the filler or fibre surface.

Filler-filler bonding is an obvious area of weakness. Improvement here is a more difficult task. Polymers used to preflocculate fillers are often present in too low a concentration to generate significant inter-particle bonding.

Activated Filler

Activated Filler takes the prefloc process to the next level. AmiForm™ is a branched, amphoteric micropolymer. Reaction with filler is by patching and particle bridging. When mixed with filler it partakes in particulate bridging, generating robust, open flocs that will reform after shearing. The micro-polymer also acts as a binder in the dried mineral floc. Being amphoteric there is no net contribution to the wet end charge balance and so addition rates may be adjusted over a significant range. The amphoteric charge gives little interference with optical brighteners added to the stock.

Untreated 2 kg/t AmiForm
Untreated
2 kg/t AmiForm
3 kg/t AmiForm 5 kg/t AmiForm
3 kg/t AmiForm
5 kg/t AmiForm

Fig. 10 – Activated Filler. Addition rates are per tonne of filler.

The pre-flocculated filler results in easier wire and press section dewatering, together with improved wet web strength. The optimum average particle size appears to be about 40 to 75 µm.

Conclusions:

Filler pre-treatment is receiving much renewed interest

Encapsulation and pre-flocculation are receiving most attention

Floc size and floc tenacity are important for pre-flocculated fillers

Poor filler-to-filler bonding is a potential weak point with pre-flocculated fillers

AmiForm ™ Activated Filler addresses the issues of floc size, floc tenacity and filler-filler bonding

Further Developments:

Encapsulated Prefloc

- but that is a topic for a future presentation.

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Case Study #1

Description

- Asia, 900 t/d.

- Gapformer

- Plain Paper Copier, 80 gsm

Results

- Reduced white water turbidity

- Sheet ash rises from 22.7% to 23.8%

- Filler addition reduced by 2%

- Steady improvement in formation index

WhitewaterTurbidity

2800 2700 2600 2500 2400 2300 2200 2100 2000 8:00 10:00 12:00 14:00 16:00 18:00
2800
2700
2600
2500
2400
2300
2200
2100
2000
8:00
10:00 12:00 14:00 16:00 18:00 20:00 22:00
0:00
2:00
4:00
6:00
8:00
10:00 12:00
Turbidity (NTU)

Time

Case Study #2

Description

- Asia, 900 t/d.

- Gapformer

- Plain Paper Copier, 70 gsm

Results

- Reduced white water turbidity

- FPR increased 2%

- Filler addition reduced by 4%

- Filler content increased

- Drainage improved

White Water Turbidity

4500 4300 4100 3900 3700 3500 3300 3100 2900 AmiForm Trial 2700 2500 2:00 4:00
4500
4300
4100
3900
3700
3500
3300
3100
2900
AmiForm Trial
2700
2500
2:00
4:00
6:00
8:00
10:00
12:00
14:00
16:00
18:00
20:00
22:00
0:00
Turbidity (NTU)

Time

16:00 18:00 20:00 22:00 0:00 Turbidity (NTU) Time F ormation Index F ormation 68 67 66

F ormation Index

F ormation

68 67 66 65 64 63 62 61 06:00 12:00 18:00 00:00 06:00 12:00 18:00
68
67
66
65
64
63
62
61
06:00
12:00
18:00
00:00
06:00
12:00
18:00

Time

Remark

Before Trial

During Trial

Time

06:00 - 09.00

09:00 - 12.00

Dosage AmiForm 528 (kg/t CaCO3)

0

5

Particle Size (µm)

2.54

4.17

W/W Turbidity (NTU)

4190

3750

Machine Speed (m/min)

1281

1270

Drainage Time (sec/500 ml)

31

29

FPR (%)

74

76

FPAR (%)

44

47

Filler Addition (l/min)

75

72

Filler Content (%)

21.8

22.4

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References:

References: 1 Applications of Wet-End Paper Chemistry Au and Thorn (Eds.). Blackie Academic, Glasgow, 1995 2

1 Applications of Wet-End Paper Chemistry Au and Thorn (Eds.). Blackie Academic, Glasgow, 1995

2 The Hylode System For Fibre Replacement R.D. Mather PIRA Papermakers Conference, 1982

3 Influence of Mineral Fillers on Paper Strength: Its Mechanism and Practical Means of Modification Beazley, K.M., Dennison, S. R., and Talyor, J. H 11th ESPRA European Meeting, 1979

4 Method of Preparing a Starch Enveloped Material H.T. Ruff US Patent 2,140,394 Dec 13, 1938

5 Agglomerated Fillers Used in Paper R.R. Davidson US Patent 4,115,187 Sep 19, 1978

6 Preflocculated Filler Compositions for Use in the Manufacture of Paper L.E. Shiel US Patent 4,174,998 Nov 20, 1979

7 Compositions for Use With Papermaking Fillers Brooks et al. US Patent 4,272,297 Jun 9, 1981

8 Paper Making Process Utilizing Fillers with Hardened Envelopes of Cationic Starch Suden et al. US Patent 4,710,270 Dec 1, 1987

9 Improvement of paper properties using starch-modified precipitated calcium carbonate filler Yulin Zhao, ZeShan Hu, Art Ragauskas & Yulin Deng February 2005 Vol 4, No 2, Tappi Journal

10 The effect of pre-flocculation of fillers on paper strength Marcus Petersson Dissertation, Chalmers University of Technology Goteborg, Sweden 2011

11 Paper Chemistry - An Introduction Eklund et al DT Paper Science Publications, 1991

12 Lumen-loaded paper pulp Green, H. V., Fox, T. J., and Scallan, A. M. Pulp & Paper-Canada 83(7), 39-43, 1982

13 Filler loading in the lumen or/and cell wall of fibers - A literature review Kumar, P., Negi, Y. S., and Singh, S. P. BioResources 6(3), 3526-3546, 2011

14 In-Situ Cellulose Fibres Loading With Calcium Carbonate Precipitated By Different Methods Ciobanu et al Cellulose Chem. Technol., 44 (9), 379-387, 2010

15 The microporosity of pulp - The precipitation of inorganic fillers within the micropores of the cell-wall. Allan et al Tappi Journal 75(1), 175-178, 1992

16 Improving the combinations of critical properties and process parameters of printing and writing papers and paperboards by new paper-filling methods Silenius, P. Dissertation/Thesis, Helsinki University of Technology, Helsinki, Finland, 2002

17 Clay-starch composites and their application in papermaking Yoon, S. Y., and Deng, Y. L. J. Appl. Polym. Sci. 100(2), 1032-1038, 2006

18 The microporosity of pulp - The properties of paper made from pulp fibers internally filled with

calcium-carbonate. Allan, G. G., Negri, A. R., and Ritzenthaler, P. Tappi Journal 75(3), 239-244,

1992

19 Graft polymerization of vinyl acetate onto silica Nguyen, V., Yoshida, W., and Cohen, Y. J. Appl. Polym. Sci. 87(2), 300-310, 2003

20 Preparation and application of cationic cellulose fibers modified by in-situ grafting of cationic PVA. Sang, Y., and Xiao, H. Colloids and Surfaces - Aphysicochemical and Engineering Aspects 335(1-3), 121-127, 2009

21 Producing Dispersions of Preflocculated Fillers for Use in Papermaking D.E. Smith US Patent 4,295,933 Oct 20, 1981

22 Preparation of Filler Compositions for Paper Harvey, R.D. and Klem, R.E. US Patent 4,799,964 Jan 24, 1989

23 Method for Manufacturing Filler-containing Paper G. Gavelin US Patent 4,889,594 Dec 26, 1989

24 Modification of Fillers to Allow Higher Retained Ash Contents M.G. Riddell Paper, Jan 5, 1976

25 40% filler loaded paper… dream or reality?

Mrs A.J. Hayes Paper Technology & Industry, Apr/May 1985

26 Controlled Filler Preflocculation: Improved Formation, Strength and Machine Performance Mabee, S.W. TAPPI Papermakers Conference (2001)

27 Optimization of Pigment Performance in Paper B.Alince Fundamentals of Papermaking, Trans. 9th Fund. Res. Symp., Cambridge, 1989

28 Cationic Polymer-modified Filler Material

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R.A. Gill US Patent 5,147,507 Sep 15, 1992

R.A. Gill US Patent 5,147,507 Sep 15, 1992 29 Pre-flocculation of GCC with cationic PAM and

29 Pre-flocculation of GCC with cationic PAM and cationic Starch and the Influence of their dosage and shear rate on prefloc size. Kyong Ho Lee and Hak Lae Lee Korea TAPPI Vol.38.No.4, 2006

30 Papermaking Using Cationic Starch and Carboxymethyl Cellulose or Its Additionally Substituted Derivatives. Taggart et al. US Patent 5,061,346 Oct 29, 1991

31 Controllable Filler Preflocculation Using Dual a Polymer System Cheng, W. and Gray, R.T. US Patent 8,088,213 B2 Jan 3, 2012

32 Pre-flocculation of fillers - Evaluation of different flocculation conditions Sara Wiik, Thesis, Lulea University of Technology

33 Increasing Filler Content in Paper Anuchate Saenkhot Paperex 2011

34 New Technology for Increased Filler Use and Fiber Savings in Graphics Grades Cheng et al. TAPPI PaperCon 2011

35 Increasing ash without compromise - A comprehensive approach Menard et al TAPPI PaperCon 2011

36 Paper Products Comprising Filler Materials Preflocculated Using Starch Granules and/or Polymerized Mineral Networks. Palmer et al. US Patent 6,494,991 B1 Dec 17, 2002

37 Pre-flocculation of precipitated calcium carbonate filler by cationic starch for highly filled mechanical grade paper. Yizhou Sang, Michael McQuaid and Peter Englezos BioResources 7(1), 354-373, 2012

The reader’s attention is also drawn to the following two additional works.

1 Bonding Material Coated Clay for Improving Paper Properties Se-Young Yoon Dissertation, Georgia Institute of Technology May 2007

2 On the nature of joint strength in paper - a review of dry and wet strength resins used in paper manufacturing Tom Lindstrom, Lars Wagberg and Tomas Larsson 13th Fundamental Research Symposium, Cambridge, Sept

2005

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