Gondorukem Processing To Be Sizing Agent For Additive Substance In PapermakingMAHAMMAD KHADAFI, IKE ROSTIKA, TAUFAN HIDAYATCENTER FOR PULP AND PAPERMINISTRY OF INDUSTRY

OUTLINE

1 IntroductionMaterials and Method Result and DissucssionConclusion

234

Introduction

• Gondorukem (Resina Colophium) is solid form of resin that obtain from pine tree (Pinus Merkusii) and produced by steam distillation process of fresh liquid resin.

Gondorukem

Volatile Compound

Pinus MerkusiiBy Product

Pine Resin (Oleoresin)

Steam distillationExtraction

(Rezzi et al., 2005)

IntroductionSizing Papermaking

• Sizing in papermaking is a process to inhibit the aqueous liquid penetration in paper by modified the hydrophilic fiber surface structure to hydrophobic layer. Either in the body of sheet of paper (internal sizing) or through the surface of sheet (surface sizing).

Forming

(Gess, 1996) ; ( Hubbe, 2007)

IntroductionRosin as Sizing Agent

Pimarane Type

Abitane Type

• Chemical composition of gondorukem is 90% - 95% diterpenic monocarboxylic acid compound that has ampliphilic molecules reactive group. The component of rosin chemical compound divided into pimarane and abitane type

(Soltes and Zinkel, 1989)

IntroductionRosin as Sizing Agent

• Rosin can be applied as paper sizing agent in the acidic condition (pH < 7). Because of that rosin has several weaknesses such as : effluent is polutant, corrosive in paper machine and paper strength (physical properties) losses and also yellowing.• Reinforce rosin (rosin fortified) is the result of rosin modification by chemical reaction

of abietic acid with maleic or fumaric anhydride with temperature over 100oC to obtain the structure with higher hydrophilicity characters.

H+

Over 100oC

Rosin Fortified (MPA)(Kirk and Othmer,

1972)

Materials and MethodMaterials

Equipment that used are:a) Soxhlet apparatusb) Agitator c) Water bathd) Physical properties

testere) Extraction flaskf) Cobb 60 testerg) Heating mantle

Materials that used are:a) Gondorukemb) Alumc) Ethanold) NaOHe) Sulphuric acidf) Maleat anhydrideg) Gliserineh) Commercial rosin

emulsioni) PAC

Materials and MethodPhysical and chemical properties testing

• Based on direct observationColour• Based on SNI 08-7070-2005Water Content• Based on SNI 7636 : 2011Softening Point• Based on RSNI3 7676 : 2010Acid number• Based on TAPPI T628 cm - 01Saponification

number• Solubility on toluena with

comparison 1:1Solubility

• Based on SNI 7636 : 2011Dirt content

Materials and MethodPreparation of Rosin Emulsion

Solid gondorumkem• Crushed

Gondorukem powder• Doing acid and saponification number tester

Result from calculation• Count ratio of NaOH needs

The needs of NaOH obtained• Saponification reaction with alcohol medium T = 90oC

Saponification rosin• Added maleic anhydride T = 180oC

Reinforce rosin• Solubility test

Rosin emulsion

Result and DiscussionPhysical and Chemical properties of Gondorukem

TestingGondorukem Spesificati

on (SNI 7636 : 2011)Grade X Grade WW

Colour*(Gardner standard)

Yellow (6) Yellow - Brown (7) 6 – 7

Softening point 88oC 90oC ≥ 78oCSaponification

number 199,74 195,84 170 - 220

Dirt content 0,07% 0,04% ≤ 0,05%Solubility in

Toluen Soluble Soluble Soluble

Acid number 179,92 176,58 160 - 190Water Content 2,30% 1,82% -

• Both of gondorukem meet the standard spesification based on SNI 7636:2011, but gondorukem for grade WW is more favourable to be rosin sizing agent than grade X due to lower impurity content; lower acid number (free carboxylic group) and also higher softneing point.

Result and DiscussionChromatograms of fatty acid component analysis (GC-MS method)

Gondorukem grade X

Gondorukem grade WW

Result and DiscussionFatty Acid Composition of Gondorukem (GC-MS method)

Fatty acid composition

Gondorukem

Grade WW Grade XSaturated fatty acid 43,20% 45,68%

Butyrate (C-4) 0% 23,10%

Caproate (C-6) 11,40% 7,42%

Undecanoic (C-11) 5,56% 4,58%

Capric (C-10) 6,14% 5,89%

Palmitoleic (C-18) 20,10% 5,56%

Unsaturated fatty acid 56,80% 54,32%

• Analysis of fatty acid composition can be obtain that grade WW has more unsaturated fatty acid composition than grade X. And also there’s small number of short chain saturated fatty acid, it means that grade X is easy oxidized by free air condition.

Result and DiscussionProcess of making rosin emulsion

NaOH PelletsEthanol +

Alcoholic NaOH

Solution

Condition T 150oC, 180 rpm, 1

hour

+

Maleic anhydride0%, 3%, 5% & 8%

Gondorukem Powder

Result and DiscussionApplication on Papermaking

1 2 3 40

20

40

60

80

100

120

Rosin standardRosin MA 0% Rosin MA 3% Rosin MA 5% Rosin MA 8%

Number of Sample

Cob

b fa

ctor

(g/m

2)

• The result of Cobb test factor can be conclude that Rosin emulsion with 3% of MA treatment has similarity water penetration factor with rosin standard.

Graph for handsheet water penetration testing (Cobb test)

Result and DiscussionApplication on Papermaking

Rosin standard

Rosin MA 0%

Rosin MA 3%

Rosin MA 5%

Rosin MA 8%

010203040506070

61.8754.28

63.08

48.16 51.66

Tearing Index

Tear

Inde

ks (

Nm

/g)

Rosin standard

Rosin MA 0%

Rosin MA 3%

Rosin MA 5%

Rosin MA 8%

020406080

100120

8059.8

95.972.1 66.5

Grammage with size 200cm2

Gsm

Tot

al

Rosin standard

Rosin MA 0%

Rosin MA 3%

Rosin MA 5%

Rosin MA 8%

00.5

11.5

22.5

32.47 2.56 2.66

2.22.5

Tensile Index

Perc

enta

ge (

%)

Rosin standard

Rosin MA 0%

Rosin MA 3%

Rosin MA 5%

Rosin MA 8%

01234567 6.62

5.936.59

4.55.53

Tensile Energy Adsorpsion

TEA

(K

gfm

/m2)

Conclusion Gondorukem grade WW meets the spesification standard based on SNI

7636 : 2011 for making rosin emulsion than gondorukem grade X

By adding 3% maleic anhydride, rosin emulsion can be obtained in optimum condition with average Cobb Testing Factor 25,34 lower than rosin emulsion standard 27,64.

The physical properties of handsheet with 3% MA rosin emulsion is higher for testing parameter such as tearing index, grammage, TEA and tensile index than 0%, 5% and 8% MA treatment.