Paper and paperboard are the essential requirements of

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1 RESEARCH ARTICLE 42 Pine Needle - An Evaluation of Pulp and Paper Making Potential Priti S.Lal, 1 Arvind Sharma 2 and Vimlesh Bist 3 1 scientist Central Pulp & Paper Research Institute, Saharanpur 2 scientist Central Pulp & Paper Research Institute, Saharanpur 3 Scientist and Head of PCPB,Div. of Central Pulp & Paper Research Institute (Received March 27, 2013; Accepted April 27, 2013) Abstract In the present studies Pine needles are evaluated for pulp and paper making properties. Different studies reported different composition of Pine needles. The pine needles collected from hilly zones of India has, 43 lignin, 52 holocellulose and 5.8 extractives content. In order to understand the paper making potential, study on pulping, bleaching and paper making properties of pine needle has been carried out. Kraft cooking of pine needle using 24 active alkali resulted into unbleached pulp of kappa number 28 and unbleached pulp yield of 24. Due to high lignin content the unbleached pulp kappa number is also high. Pulp after DEpD bleaching could be bleached to 75 ISO. Fiber morphological properties of pine needle fiber were also carried out. Index Terms Pine needles, Chemical composition, Kraft pulping, Chlorine bleaching, Papermaking I. INTRODUCTION Paper and paperboard are the essential requirements of human life. The demand of Paper and paperboard is increasing constantly. The current global demand is 402 million tons per annum produced by 7745 mills producing 192 million tones of pulp. The paper demand has doubled in 20 years from million tones in 1990 to 402 million tons in 2011.the forecast for paper production by 2021 is projected at 521 million tons per annum.[1-2]. The fast growing demand has drawn utmost attention for utilization of forest wastes, agricultural residues/wastes,and non-wood fibrous materials for the production of pulp, which will help in reducing the environmental pollution. Pine needles, Pine Needles, are the adult leaves, which are green bundled in clusters (fascicles) of 1 6, commonly 2 5, needles together. Pine needles have many uses, whether they are cut from the tree, freshly fallen, or dried. Pine needles are commonly used in gardening and landscaping, can be made into decorative yet practical crafts, and even have nutritional value when ingested. Pine needles are composition has cellulose (>50) and lignin as main component. Because of * Corresponding author E- mail: cppri.pcpb@gmail.com the composition of pine needle its utilization for paper making is another area which can be explored for value added utilization of pine needle. leaves of pine, is a very new raw material and very few studies are available in literature to evaluate the paper making potential of pine needle. There is variation in composition of pine needle based on the geographical location. As reported by Ray et al [3] composition reported for pine needle is 68.5 hollocellulose, 4.56 extractives and 31.0 lignin, while in studies carried out by Jan Asadullah [4] Pine needles (pine leaves) were analyzed for their chemical constituents, and the dimensions of the extracted fibers were determined to assess their utilization for pulp making according to their studies Cellulose content of pine needles (41) was comparable to softwood (42), whereas the lignin content (35.1) was high as compared to both softwood (28) and hardwood (20). Ash content of pine needles (3.2) was less than wheat straw (4-9) and comparable to bagasse (1.5-5 ). The average length of the pine needle fibre (13mm) was greater than fibres of sugarcane (1.7 mm), wheat straw (1.4 mm) and esparto (1.2mm), but less than cotton (30 mm). The average diameter of pine needle fibre (32 ìm) was greater than all the common fibres used for papermaking.the composition of pine needle as per study carried out by Ghosh and Ghosh [5] has reported hollocellulose, 3.24 extractives and lignin. In the present study a complete paper making evaluation of pine needles obtained from pines of Indian hills is described. It includes proximate chemical analysis, pulping, bleaching and evaluation of physical strength properties II. MATERIALS AND METHODS Collection and Preparation of raw material 20 kg of pine needle sample was collected from Uttarakhand hill region of India. Sample was received in the form of long fibrous mass. It was chopped manually in order to get uniform representative sample. The material was kept in polythene bags to attain a uniform moisture level. Proximate chemical analysis of pine needles Complete proximate analysis of pine needles and eucalyptus for various parameters viz. ash content, cold, hot and N/10 NaOH

2 43 solubility, klason lignin, Acid insoluble lignin, and holocellulose content were determined by standard procedure cited Table 1. Table 1 Standards of Proximate chemical analysis S.No. Method 1. Ash APPITA P3M Lignin TAPPI-T Holocellulose Wise et al Paper Trade J 122 No (1946) 4. Alpha cellulose TAPPI203OS74 5. Pentosan UV Method 6. Hot water solubility APPITA P4M Cold water solubility TAPPI 207om NaOH solubility TAPPI 212om-98 PULPING OF PINE NEEDLES Cooking chemical optimization Pulping experiments were performed in a series digester consisting of six bombs each of 2.5 liter capacity, rotating in an electrically heated polyethylene glycol bath. At the end of the cooking time, the bombs were removed and quenched in the water tank to depressurize the bombs and the cooked mass from each bomb was taken for washing. Washing was carried out with hot water till the cooked mass was free from spent liquor. After thorough washing, the unscreened pulp yield was determined and the pulp was screened in laboratory Serla screen by using mesh of 0.20 mm. slot width. Kappa number of the screened pulp was determined as per the TAPPI standard procedure T-236-OS-76. The constant cooking conditions are given below: Constant Cooking Conditions Raw material in each bomb : 200g Sulphidity : 20 Bath ratio : 1:5 Cooking temp. o C : 168 o C Cooking time, min. : 120 min Determination of pulp kappa number, brightness and viscosity Pulp was analyzed for yield, kappa number (Tappi T:236 OM 99), brightness (ISO 2470) and intrinsic viscosity (Scan C15:62) Conditions for different stages of Bleaching Process Consistency ( ) Reaction time (min ) Reaction temp ( C ) Chlorine Dioxide-1stage Alkali extraction-ep stage Chlorine Dioxide-D2stage ph maintained Evaluation of Physical Strength Properties Unbleached & bleached pulp samples were evaluated for using the following standard methods (Table 3) Table 3 Evaluation of Physical Strength Properties S.No. Method 1. Freeness ISO DP Basis Weight ISO Thickness ISO R Bulk ISO534:1988(E) 5. Tensile Index ISO Tear Index ISO Bursting Index ISO Folding ISO DIS Opacity ISO 2471 FIBER CHARACTERISTICS OF PULP Fibre length and diameter of bleached pulp were characterized (Table 4) DEpD bleaching of pulp Bleaching optimization of unbleached grade pulp following sequence DEpD was carried out. DEpD bleaching sequence is now a days common environment friendly bleaching process for production of bleached pulp. Following conditions were maintained during the bleaching of unbleached pulp Table 2. Table 2

3 44 TABLE 4 S.No. Method 1. Fiber Length IS Fiber Diameter III. RESULTS AND DISCUSSION Proximate Chemical Analysis (chemical composition) of Pine Needles Results of proximate chemical analysis and its comparison with Eucalyptus [6] were depicted in Table 5. Table 5 Proximate chemical analysis for Pine needles and eucalyptus Pine needle Eucalyptus Ash Cold water solubility Hot water solubility N/10 alkali solubility Alcohol benzene solubility Lignin content Holocellulose Alpha cellulose Beta cellulose Gama cellulose The results of proximate analysis were compared with eucalyptus, conventionally used raw material in Indian Paper industry. The pine needle contains high lignin and lower holocellulose content. The alcohol benzene solubility in raw material indicates the higher extractives than eucalyptus. The ash content is also high i.e.4.45, which indicates high silica and inorganic in pine needle. Kraft Cooking Chemical Optimization The details of cooking chemical optimizations were depicted in Table 6.

4 45 Table 6 Kraft cooking chemical optimization Process Conditions/ Test Results Unit Cook 1 Cook 2 Cook 3 Cook 4* Active alkali Na 2 O Cooking Temp. o C Sulphidity Heating Time (min) Cooking Time (min.) Bath ratio 1:5 1:5 1:5 1:5 Unscreened Yield Rejects Kappa Number Different dosages of active alkali were taken to optimize the kappa number for bleachable grade of pulp. Kraft cooking with dosages 18, 20, 22 and 24 as Na2O were applied inorder to get desired kappa number i.e as per the trend of unbleached pulp production in Indian paper industry. Results depicted in Table-2 clearly indicate cooking chemical demand for pine needle is high due to high lignin content. Unscreened pulp yield is also low due to lower holocellulose content. By using 24 cooking chemical unbleached pulp of kappa number 28 is obtained while yield was only 21.0 which is very low. Large scale cooking of raw material with 24 cooking chemical was carried out. The unbleached pulp kappa number 28 was obtained was further taken for bleaching experiments. Results of Bleaching Experiment The results of bleaching optimization of unbleached pulp of kappa number 28 were depicted in Table 7. Dose applied for large scale bleaching for strength properties evaluationthe unbleached pulp of 28 kappa number was subjected to bleaching, by DEpD sequence. It was observed that initial brightness (15.6) is very poor, which has resulted into final low brightness i.e. 75 (ISO) FIBER CHARACTERISTICS OF PULP Results of Fibre Characteristics were depicted in Table 8. The average fiber length of pine needle sample is 0.70 mm and eucalyptus is 0.81mm (6). As such there is no remarkable difference was observed in fiber length of both the raw materials. The average fiber width of pine needle sample is µm and eucalyptus is µm.

5 46 Table 7 Bleaching of Pine Needles pulp A. Results Unbleached pulp Kappa number 28 Intrinsic Viscosity (cm3/g 817 Unbleached pulp brightness, ISO 15.6 Bleaching Sequence Applied DEpD CHLORINE DIOXIDE STAGE ( D 1 ) DIOXIDE ADDED, AS AVL. CHLORINE, 9 PH 2.4 EXTRACTION STAGE (EP) NAOH ADDED, 3.0 HYDROGEN PEROXIDE ADDED, 0.5 PH 11 DEP KAPPA NUMBER 4.3 DEP STAGE VISCOSITY.CM3/G 811 DEP BRIGHTNESS 65.8 DIOXIDE STAGE ( D 2 ) DIOXIDE ADDED, 1 2 DIOXIDE CONSUMED, BRIGHTNESS, ISO BLEACHED YIELD, - 95 VISCOSITY.CM3/G FIBER CHARACTERISTICS OF PULP Results of Fibre Characteristics were depicted in Table 8. Table 8 Fibre Characteristics of Pine needles and Eucalyptus fibre length Unit Pine needle Eucalyptus mm fibre Width µm The average fiber length of pine needle sample is 0.70 mm and eucalyptus is 0.81mm (6). As such there is no remarkable difference was observed in fiber length of both the raw materials. The average fiber width of pine needle sample is µm and eucalyptus is µm. Bauer Mc Nett. Fiber Classification of Pine Needle Pulp The results of Bauer Mc Nett fiber classification of unbleached and bleached pulp were given in Table 9.

6 47 Sl Table 9 Bauer Mc Nett. Fiber Classification of Pine Needle Pulp unbleached pulp bleached pulp A. Fiber fraction The total useful fiber content (+50 and +100 fraction) of pine needle pulp are substantial, though the long fiber content (+30) are very low. The trend is almost similar to that of hardwoods. The fines are high (-200) and decreased marginally after bleaching. Physical Strength Properties of both Unbleached and Bleached Pulp The results of physical strength properties were depicted in Table 10 below. PFI (rev) Table 10 Physical Strength Properties of both Unbleached and Bleached Pulp Freeness ml,csf Apparent Density g/ cm3 Burst Index KPam 2 /g Tensile Index Nm/g Fold Kohler Molin(log) Porosity Bendtsen (ml/min.) Opacity () Unbleached pulp nil Bleached pulp nil The result of pulp strength before and after bleaching indicates that pine needle pulp has substantial good strength for production of good quality paper. The burst index and tensile index of pulp is good enough compared to other cellulosic raw material. [2] RISI, Forecast, 2010, August 2010, Annual Review, RISI, IV. CONCLUSIONS USA. Pine needles has more than 50 holocellulose, and hence can [3] A Ray, A. and Das, M, 2010, Eco friendly utilization of be used for production of pulp and paper. Though it contains hazardous pine needle waste for the production of paper, higher lignin which results into high bleach chemical demand. Conference Proceedings of American Institute of Chemical Instead of bleached variety it can be utilized for production of Engineers, AIChE, USA. semi bleached grade pulp, unbleached kraft paper, filler or [4] Asadullah, Jan 2006, Investing of pine needles for paper/board. pulp/paper industry, Pak J.of Sci. Ind. Res., 49(6): [5] Ghosh& Ghosh, (2011),Utilization of pine needles as bed REFERENCES material in solid state fermentation for production of lactic acid [1] Kulkarni, H.D. 2013,Pulp and paper industry raw material by lactobacillus strain, Bio Resources, 6(2): scenario- ITC plantation a case study, IPPTA J., 25(1 ): [6] CPPRI Report on CESS sponsored project on Preparation of Monograph of different fibrous raw material used by Indian Paper Industry, 2005