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Analysis of pulp components in Analysis of pulp components in a DIP - - PowerPoint PPT Presentation

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Analysis of pulp components in Analysis of pulp components in a DIP process with tube flow a DIP process with tube flow fractionation fractionation Ossi Laitinen Laitinen Ossi Fibre and Particle Fibre and Particle Engineering Laboratory

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8th Research Forum on Recycling 26.09.2007

Analysis of pulp components in Analysis of pulp components in a DIP process with tube flow a DIP process with tube flow fractionation fractionation

Ossi Ossi Laitinen Laitinen Fibre and Particle Fibre and Particle Engineering Laboratory Engineering Laboratory

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8th Research Forum on Recycling 26.09.2007

Outline Outline

  • Introduction

Introduction

  • Materials & Methods

Materials & Methods

  • Results

Results

  • Pulp component analysis

Pulp component analysis

  • Residual ink and brightness

Residual ink and brightness

  • Microscope analysis

Microscope analysis

  • Conclusions

Conclusions

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8th Research Forum on Recycling 26.09.2007

Aim of study Aim of study

  • In this study fresh and aged raw material were

In this study fresh and aged raw material were compared in similar process conditions compared in similar process conditions

  • How aging affects to raw material, especially

How aging affects to raw material, especially behaviour of ink? behaviour of ink?

  • Fractional approach give answer to:

Fractional approach give answer to:

  • Detachment of ink in different fibre length class

Detachment of ink in different fibre length class

  • How much ink exits in each fibre length class?

How much ink exits in each fibre length class?

  • What is attached ink size distribution?

What is attached ink size distribution?

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8th Research Forum on Recycling 26.09.2007

Introduction Introduction

  • Different environments to study aging and

Different environments to study aging and thermal aging: thermal aging:

  • Laboratory scale

Laboratory scale

  • Lack of actual process conditions

Lack of actual process conditions

  • Mill scale

Mill scale

  • Raw material changes

Raw material changes

  • Pilot scale

Pilot scale

  • Accurate raw material control

Accurate raw material control

  • Process conditions near industrial conditions

Process conditions near industrial conditions

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8th Research Forum on Recycling 26.09.2007

Materials & Methods Materials & Methods

  • Pulps

Pulps

  • 1

1-

  • loop continuous deinking pilot plant

loop continuous deinking pilot plant

  • Raw material ONP

Raw material ONP-

  • OMG (50%

OMG (50%-

  • 50%)

50%)

  • Alkaline soap chemistry

Alkaline soap chemistry

  • Two separate trials in similar conditions:

Two separate trials in similar conditions:

  • Fresh material: 10 weeks old

Fresh material: 10 weeks old

  • Aged material: 30 weeks old

Aged material: 30 weeks old

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Continuous deinking pilot plant Continuous deinking pilot plant

sampling

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Sampling points Sampling points

Sampling point Description of the test point Drum pulper Samples from batch drum pulping Pulper accept tank (PAC) Pulping samples after dilution Flotation feed (FFE) Flotation cell feed samples Flotation accept (FAC) Flotation cell accept samples Flotation reject (FRE) Flotation cell reject samples Wire press outlet (WPO) (final pulp) Pilot process product

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8th Research Forum on Recycling 26.09.2007

Pulping performances Pulping performances

Pulping performances Raw material 50% ONP & 50% OMG (central European) Pulping consistency 16% Pulping temperature 50°C Pulping batch 35 kg (air dry) NaOH 10 [kg/t] Waterglass 9.3 [kg/t] Commercial fatty acid soap 6 [kg/t] H2O2 10 [kg/t] Hardness [°dH]

  • adj. CaCl2

20 [°dH]

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8th Research Forum on Recycling 26.09.2007

Analysis Analysis

  • Tube flow fractionation

Tube flow fractionation

  • Dry content and ash content

Dry content and ash content

  • Brightness and residual ink

Brightness and residual ink

  • Microscope and image analysis

Microscope and image analysis

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8th Research Forum on Recycling 26.09.2007

Tube flow fractionation Tube flow fractionation

  • Sample is separated

Sample is separated into 4 fractions with into 4 fractions with continuous water flow continuous water flow

  • FR1: flakes (> 4mm)

FR1: flakes (> 4mm)

  • FR2: long fibres (1.85mm)

FR2: long fibres (1.85mm)

  • FR3: short fibres (0.6mm)

FR3: short fibres (0.6mm)

  • FR4: fines (< 0.2mm)

FR4: fines (< 0.2mm)

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8th Research Forum on Recycling 26.09.2007

Laboratory measurements Laboratory measurements

  • Pulp dry content (ISO 638)

Pulp dry content (ISO 638)

  • Ash content of pulp (ISO 1762)

Ash content of pulp (ISO 1762)

  • Brightness of pulp (L&W

Brightness of pulp (L&W Elrepho Elrepho spectrophotometer) spectrophotometer)

  • Residual ink of pulp (L&W

Residual ink of pulp (L&W Elrepho Elrepho spectrophotometer) spectrophotometer)

  • Hyperwashing

Hyperwashing (150 mesh wire screen) (150 mesh wire screen)

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8th Research Forum on Recycling 26.09.2007

Microscope and image analysis Microscope and image analysis

  • Each fraction was filtered out onto

Each fraction was filtered out onto membrane filter foils in order to investigate membrane filter foils in order to investigate the samples with a microscope ( the samples with a microscope (Leica Leica DCF320) DCF320)

  • Sample images were analysed with image

Sample images were analysed with image analysis software ( analysis software (Matrox Matrox Inspector) Inspector) that that calculated the number, length, width and calculated the number, length, width and area of dark particles (i.e. ink particles) area of dark particles (i.e. ink particles)

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Results Results

  • Pulp component analysis

Pulp component analysis

  • Slushing rate, mass proportions of fractions

Slushing rate, mass proportions of fractions

  • Residual ink and brightness

Residual ink and brightness

  • Ink fragmentation, ink reduction, brightness

Ink fragmentation, ink reduction, brightness development development

  • Microscope analysis

Microscope analysis

  • Attached and free ink in different fractions

Attached and free ink in different fractions

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Slushing rate in pulping Slushing rate in pulping

  • Aged material

Aged material slushed slushed poorer during drum poorer during drum pulping pulping

Drum pulping

1 2 3 4 5 6 7 8 9 10 FR1 mass percentages [%] Fresh 4.8 3.7 2.9 Aged 8.5 8.1 5.9 10 min 20 min 30 min

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Mass proportions of fractions Mass proportions of fractions

  • No considerable differences in mass proportions during

No considerable differences in mass proportions during process due to pumping and screening process due to pumping and screening

Fresh pulp Proportion of flakes [%] Proportion of long fibres [%] Proportion of short fibres [%] Proportion of fines [%]

Pulper (20min) 3.7 37.6 23.2 35.4 PAC 1.0 35.3 22.6 41.0 FFE 0.3 34.1 22.3 43.2 FAC 1.7 35.9 23.0 39.4 FRE 0.3 8.7 14.2 76.7 WPO 2.6 43.7 26.4 27.3

Aged pulp Proportion of flakes [%] Proportion of long fibres [%] Proportion of short fibres [%] Proportion of fines [%]

Pulper (20min) 8.1 37.4 22.6 31.9 PAC 1.9 39.8 23.7 34.6 FFE 1.4 33.4 23.9 41.3 FAC 1.8 35.1 24.7 38.4 FRE 0.4 12.6 12.8 74.2 WPO 3.0 44.9 27.9 24.2

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Residual ink Residual ink

  • Residual ink values were much higher in case of

Residual ink values were much higher in case of aged raw material aged raw material

500 1000 1500 2000

Residual ink [ppm]

Fresh 1291 1082 182 210 Aged 1825 1611 460 474 PAC FFE FAC WPO 100 200 300 400 500

Residual ink [ppm]

Fresh 182 132 Aged 460 298 FAC FAC HW

HW = hyperwashing

flotation accept & hyperwashing

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Brightness Brightness

  • Brightness was 5

Brightness was 5-

  • 8 point higher along the pilot

8 point higher along the pilot process line process line

30 35 40 45 50 55 60 65 70 Brightness [% ISO] Fresh 45.5 48.4 64.7 61.7 Aged 40.3 43.0 56.7 55.5 PAC FFE FAC WPO

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Microscopy analysis Microscopy analysis

  • FR2 & FR3 : Attached ink particles

FR2 & FR3 : Attached ink particles

  • FR4: Floatable free ink

FR4: Floatable free ink

flotation feed flotation accept

1000 10000 100000 1000000 Total area of ink particles [pixels] Fresh 9722 18448 193099 Aged 12466 47827 131676 FR2 FR3 FR4 1000 10000 100000 1000000 Total area of ink particles [pixels] Fresh 10530 16381 7955 Aged 13566 34673 10114 FR2 FR3 FR4

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Ink reduction in flotation Ink reduction in flotation

  • Free ink in FR4: Good removing during

Free ink in FR4: Good removing during flotation flotation

  • Attached in FR2 & FR3: Poor ink

Attached in FR2 & FR3: Poor ink reduction values reduction values

%, 100 ⋅ − =

F A F C

C C C E

Ink reduction [%] FR2 FR3 FR4 Total Fresh material ≈ 0 11 96 83 Aged material ≈ 0 28 92 71

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Size distribution of ink particles in Size distribution of ink particles in Fraction 2 (Flotation accept) Fraction 2 (Flotation accept)

50 100 150 200 250 3-7 μm 7-10 μm 10-15 μm 15-20 μm 20-25 μm 25-30 μm 30-35 μm 35-45 μm 45-55 μm 55-70 μm

  • ver

70 μm Particle size categories [μm] Numbers of ink particles in different size categories FR2 aged FR2 fresh

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8th Research Forum on Recycling 26.09.2007

Size distribution of ink particles in Size distribution of ink particles in Fraction 3 (Flotation accept) Fraction 3 (Flotation accept)

100 200 300 400 500 600 700 800 900 1000 3-7 μm 7-10 μm 10-15 μm 15-20 μm 20-25 μm 25-30 μm 30-35 μm 35-45 μm 45-55 μm 55-70 μm

  • ver

70 μm Particle size categories [μm] Numbers of ink particles in different size categories FR3 aged FR3 fresh

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Size distribution of ink particles in Size distribution of ink particles in Fraction 4 (Flotation accept) Fraction 4 (Flotation accept)

100 200 300 400 500 600 700 800 900 1000 3-7 μm 7-10 μm 10-15 μm 15-20 μm 20-25 μm 25-30 μm 30-35 μm 35-45 μm 45-55 μm 55-70 μm

  • ver

70 μm Particle size categories [μm] Numbers of ink particles in different size categories FR4 aged FR4 fresh

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Conclusions Conclusions

  • Fractional approach give detailed information:

Fractional approach give detailed information:

  • Slushing rate: How raw material is

Slushing rate: How raw material is slushed slushed during during pulping pulping

  • Ink detachment: Amount of attached/detached ink

Ink detachment: Amount of attached/detached ink in different size categories in different size categories

  • Floatability or

Floatability or washability washability of ink in pulp

  • f ink in pulp
  • Tool for quality control

Tool for quality control

  • Testing of chemicals

Testing of chemicals