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WO2013034811A1 - Procédé de fabrication d'un composant de matériau, composant de matériau et son utilisation et produit de papier - Google Patents

Procédé de fabrication d'un composant de matériau, composant de matériau et son utilisation et produit de papier Download PDF

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Publication number
WO2013034811A1
WO2013034811A1 PCT/FI2012/050870 FI2012050870W WO2013034811A1 WO 2013034811 A1 WO2013034811 A1 WO 2013034811A1 FI 2012050870 W FI2012050870 W FI 2012050870W WO 2013034811 A1 WO2013034811 A1 WO 2013034811A1
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WO
WIPO (PCT)
Prior art keywords
starting material
grinding
moisture content
wood
freezing
Prior art date
Application number
PCT/FI2012/050870
Other languages
English (en)
Inventor
Nina PYKÄLÄINEN
Tarja Sinkko
Lauri Talikka
Pasi Karinkanta
Mirja Illikainen
Jouko NIINIMÄKI
Original Assignee
Upm-Kymmene Corporation
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from FI20115879A external-priority patent/FI20115879L/fi
Application filed by Upm-Kymmene Corporation filed Critical Upm-Kymmene Corporation
Publication of WO2013034811A1 publication Critical patent/WO2013034811A1/fr

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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12—Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse

Definitions

  • the invention relates to a method for manu ⁇ facturing a material component. Further, the invention relates to a material component and a use of the mate ⁇ rial component. Further, the invention relates to a paper product.
  • WO 2009/080894 is a method for making organic pigment wherein the pigment is formed from a starting material of plant origin.
  • the starting material is pulverized to a suitable par ⁇ ticle size by mechanical grinding in at least two grinding steps to form the organic pigment.
  • Known from publication WO 2010/146244 is a paper product and its manufacturing method wherein the paper product is formed from fiber-based pulp to which a material com ⁇ ponent of plant origin is added.
  • the material compo ⁇ nent of plant origin is a material which is formed from small particles and which is formed from a source material of plant origin selected at least mainly from the group of bark free wood, stem parts of plants and their combinations.
  • the objective of the invention is to disclose a new and cost-effective and energy-effective method for manufacturing a material component.
  • Another objec ⁇ tive of the invention is to produce a new material component and a final product.
  • SUMMARY OF THE INVENTION The method for manufacturing a material component from a starting material of plant origin so that the material component is formed by grinding from the starting material according to the present inven- tion is characterized by what is presented in claim 1.
  • the material component according to the pre ⁇ sent invention is characterized by what is presented in claim 21.
  • the paper product according to the present invention is characterized by what is presented in claim 23.
  • Fig 1 is a flow chart illustration of a meth- od according to one embodiment of the present inven ⁇ tion
  • FIG. 2 is a flow chart illustration of a method according to another embodiment of the present in ⁇ vention
  • Fig 3 is a flow chart illustration of a method according to another embodiment of the present in ⁇ vention.
  • Figs 4 to 11 show results from the tests.
  • DETAILED DESCRIPTION OF THE INVENTION a ma ⁇ terial component is manufactured from a starting mate ⁇ rial of plant origin (1,12) so that the material com ⁇ ponent (7) is formed by grinding (4) from the starting material (1,12) .
  • the starting material (1,12) is pre-treated (2,5,6) in order to improve the degradation of the starting material, i.e. the degradation of the material of plant origin, during the grinding (4) of the starting materi- al.
  • FIG. 1 One embodiment of the method of the present in ⁇ vention is shown in figure 1. Another embodiment of the method of the present invention is shown in figure 2. Another embodiment of the method of the present inven- tion is shown in figure 3.
  • the invention is specially based on improving properties of the material component.
  • the starting material is pre-treated before and/or during the grind ⁇ ing, then the degradation of the starting material can be improved during the grinding. Then it is provided the material component with improved properties, such as the lower median particle size, aspect ratio with narrower particle size, aspect ratio distributions.
  • a starting material of plant origin refers any material or composition containing plant parts, plant fibers, wood, wood fibers and such plant origin components.
  • the starting material may contain one or more plant origin components.
  • suitable and desired additives can be added into the starting material.
  • the starting material includes material which is se ⁇ lected from a group consisting of wood-based material, fiber-based material and their combinations.
  • the wood-based material is selected from the group consisting of wood bits, dust, sawdust, chips, damp wood, bark free wood, waste wood, fiber pulp, wood pulp, cellulose, mechanical pulp, wood fibers, recycled fibers, derivates thereof and their combinations.
  • the starting material of plant origin is a wood-based material.
  • the fiber-based material is formed from material selected from the group consist ⁇ ing of graminaceous plants, grasses, herbaceous plants, cereals, straw, plant bits, stem parts of plants, culm parts of plants, aqueous or sewage sludg ⁇ es, sludge pulps, fiber-based industrial waste flows, algae, derivates thereof and their combinations.
  • the starting material of plant origin is a fiber-based material.
  • the grinding refers to any reduction of the starting material, e.g. by mechanically.
  • the grinding may be selected from the group of pulverization, grinding, crushing, cutting, chopping, breaking up of a material, e.g. by braying or rubbing, to a desired particle size or other suitable grinding method or their combinations.
  • the expression grinding should be understood as any method suitable to be used in the present invention including also its modifications.
  • the grinding is mechanical pulverization.
  • the degradation refers to any degradation, disintegration, degrading, micronisa- tion or other suitable degradation method or their combinations.
  • the wood-based starting ma ⁇ terial (1,12) is pre-treated (2,5,6) to improve the degradation of the wood during the grinding (4) .
  • the starting material is pre-treated by the pre-treatment method selected from the group consisting of increasing dry matter content (5), torrefaction (2), freezing (6), chemical pre- treatment and their combinations.
  • the starting materi ⁇ al can be pre-treated by one or more pre-treatment method.
  • the starting material can be pre-treated in one or more steps.
  • the start ⁇ ing material is pre-treated so that moisture content of the starting material is controlled. In one embodi ⁇ ment the moisture content of the starting material is decreased. In one embodiment the moisture content of the starting material is increased.
  • the mois ⁇ ture content of the starting material is controlled to between 0.1 - 70 %, in one embodiment between 1 - 70 %. In one embodiment the moisture content of the starting material is controlled to between 0.1 - 50 %, in one embodiment between 1 - 50 %.
  • the start ⁇ ing material is pre-treated so that the dry matter con- tent of the starting material is increased (5) .
  • the dry matter content of the feed is increased (5) before the grinding (4) .
  • the starting material is dried before the grinding.
  • the dry matter content of the starting material is arranged to between 50 - 100 %, in one embodiment between 70 - 100 o
  • dry matter content affects the properties of the starting material during the grinding.
  • the crystallinity of the ground wood powder is closely related to the dry matter content of the feed.
  • the start ⁇ ing material is treated under the cryogenic conditions in the grinding.
  • the median values of the particle sizes is decreased by decreasing the moisture content of the starting material and/or using the cryogenic processing conditions.
  • the relative degree of crystallinity of the cellulose is influenced by the moisture content of the starting material, the cryogenic processing conditions and the processing time.
  • the start ⁇ ing material is pre-treated by a torrefaction (2) .
  • the starting mate ⁇ rial is dried quickly.
  • the torrefac ⁇ tion (2) is made before the grinding (4) .
  • the torrefaction affects the prop ⁇ erties of the material component.
  • the torre- faction it may be decreased median particle size.
  • Fur ⁇ ther, in a preferred embodiment distributions of aspect ratio and median particle size are narrower.
  • the torrefaction (2) is carried out at temperatures between 160 - 240 ° C. In one embodiment the torrefaction (2) is carried out at temperatures between 190 - 240 ° C, in one embodiment between 200 - 230 ° C, and in one embodiment about 220 ° C; then physical properties of the starting material, preferably wood, can be changed.
  • the starting material is heat-treated at temperatures over 150 ° C; then thermal degradation of the starting material, e.g. degradation of hemicellulose and cellulose of the starting materi ⁇ al, is preferably starting.
  • the torrefaction (2) is carried out during below 30 min. In one embodiment the torrefaction (2) is carried during below 20 min, in one embodiment during below 10 min, preferably between 1 - 5 min.
  • the start ⁇ ing material is pre-treated by a freezing (6) .
  • the freezing (6) is carried out with liquid nitrogen.
  • the freezing (6) is carried out with carbon dioxide.
  • the freezing (6) is made by heat transfer, preferably by means of a transmitter agent or a metal surface.
  • dry matter content of the starting ma ⁇ terial is between 70 - 100 %, in one embodiment be ⁇ tween 80 - 100 % and in one embodiment 85 - 95 % be ⁇ fore the freezing (6) .
  • the freezing affects the proper ⁇ ties, such as small median particle size and aspect ra ⁇ tio with narrower distributions, of the material compo ⁇ nent.
  • the crystal- Unity index of the starting material can be dropped by means of the freezing.
  • the freezing (6) is made by Cryo-method .
  • the freezing (6) is made before the grinding (4) .
  • the freezing (6) is made in connection of the grinding (4) . In one embodiment the freezing (6) is made during the grinding (4) .
  • the freezing is used as an additional step in the manufacturing the material com- ponent .
  • the starting material is pre-treated by one pre-treatment method. In one embod ⁇ iment the starting material is pre-treated by more than one pre-treatment method.
  • the starting material is pre-treated by the torrefaction (2) and by the freez ⁇ ing (6) .
  • the torrefaction (2) is made before grinding (4) and the freezing (6) is made during grinding (4) .
  • the torrefac- tion (2) and the freezing (6) is made before grinding (4) .
  • the operation of grinding devices e.g. mills, is typically based on focusing pressure, cut ⁇ ting, abrasion, compaction and/or on an effect of a collision provided by blast or on an equivalent oper- ating principle.
  • the operation of grinding devices can be based also on cutting by acoustic wave or reduction of particle size by blasting. Most of the grinding de ⁇ vices operate as a combination of many operating principles .
  • the starting material is ground by a grinding method selected from the group consisting of crushing-based grinding, attrition-based grinding, abrasion-based grinding, cutting-based grinding, blasting-based grinding, explosion-based grinding, wet grinding, dry grinding, grinding under pressure, other suitable grinding method and their combinations.
  • the grinding device used for grinding the starting material is selected from the group consisting of impact mill, air jet mill, sand mill, bead mill, pearl mill, ball mill, vibration mill, screw mill, extrusion device, other suitable device and their combinations.
  • the grinding can be made in one or more grinding steps by one or more grinding methods.
  • the material component is formed by grinding a starting material in one or more steps.
  • the material component (7) of the present in ⁇ vention can be used in manufacturing (8) a final product (9) selected from a group consisting of paper product, composite product and their combinations. In one embodiment the material component of the present in ⁇ vention is used as a final product.
  • the final product (9) can be a paper product formed from paper which contains the material compo- nent of the present invention.
  • a pa ⁇ per refers to any fiber-based paper and card board and the equivalent.
  • the paper may be formed from any fi ⁇ ber-based pulp (10), such as chemical pulp, mechanical pulp, chemimechanical pulp, recycled pulp, fiber pulp and/or their mixtures or the equivalent.
  • the paper product may contain suitable fillers, additives, pigments and different surface treatment and coating agents.
  • the paper product may be in the form of a web or a sheet or in other form suitable for the purpose of use.
  • the paper product may be selected from the group of SC papers, newsprints, WFU, coated papers, such as LWC and WFC, and soft tissues.
  • the material component of the pre ⁇ sent invention may be used as a filler, pigment, addi ⁇ tive or such in the paper product.
  • the method according to the present invention provides the material component with good quality. When improving the degradation of the starting material so then it may be provided better properties of the material component and the final product.
  • the method of the present invention offers a possibility to prepare the material component from plant-based starting material cost-effectively and en ⁇ ergy-effectively .
  • the present invention provides an industrial- ly applicable, simple and affordable way of making the material component from the starting material of plant origin.
  • the method according to the present invention is easy and simple to realize as a production process.
  • the method according to the present invention is suitable for use in the manufacture of the differ ⁇ ent material components from different starting mate ⁇ rials of plant origin.
  • the material component (7) is manufactured by grinding (4) from a wood-based starting material (1) which is spruce sawdust.
  • the starting material (1) is pre-treated in two steps in order to improve the degra ⁇ dation of wood during the grinding (4) .
  • the starting material (1) is pre-treated by a torrefaction (2) before the grinding.
  • the torrefaction is made at temperature about 220 ° C during 5 min.
  • the pre-treated material (3) is fed into the grinding (4) .
  • the grinding is made by a vibrating ball mill on a laboratory scale.
  • the starting material is pre-treated by a freezing (6) during the grinding (4) .
  • the freezing (6) is made by Cryo-method with liquid nitrogen (-196 ° C). Residual grinding material (11) is removed from the grinding stage (4) .
  • the material component with small median particle size and aspect ratio with narrower distribu ⁇ tions While comparing a normal grinding to the grind ⁇ ing with the effect of the nitrogen freezing it was possible to produce smaller median particle size and aspect ratio with narrower distributions when dry mat- ter content of the starting material was preferably below 80 - 85 %.
  • the starting material had dry matter content between 50 - 92 % the crystallinity in ⁇ dex of wood dropped from 40 % to 20 - 30 % when grind ⁇ ing with the nitrogen freezing.
  • the starting ma- terial had dry matter content about 99 % the crystal- Unity index of wood dropped below 10 % in the cryo ⁇ genic milling.
  • the formed material component (7) was tested in paper application.
  • the material component (7) is added into the paper pulp (10) in the manufacturing (8) of the paper product (9) . It was discovered that the material component acts very good as an additive in the paper product.
  • a material component (7) is formed.
  • the material component (7) is manufactured by grinding (4) from a fiber-based starting material (12) which is plant-based material.
  • the starting material (12) is pre-treated in one step in order to improve the degradation of hemicellulose and cellulose during the grinding (4) .
  • the starting material (12) is pre-treated by increasing (5) the dry matter content of the starting material (12) before the grinding (4) .
  • the pre-treated material (3) is fed into the grinding (4). Residual grinding material (11) is removed from the grinding stage (4) .
  • the formed material component (7) is used in paper application.
  • the material component (7) is added into the paper pulp (10) in the manufacturing (8) of the paper product (9) .
  • Example 3 In this example and in figure 3, a material component (7) is formed.
  • the material component (7) is manufactured by grinding (4) from a wood-based starting material (1) which is wood powder.
  • the starting material (1) is pre- treated in one step in order to improve the degradation of wood during the grinding (4) .
  • the starting material (1) is pre-treated by increasing (5) the dry matter con ⁇ tent of the starting material (1) before the grinding (4) .
  • the pre-treated material (3) is fed into the grinding (4) to form the material component (7) .
  • a vibrating ball mill is used in the grinding.
  • Residual grinding material (11) is removed from the grinding stage (4) .
  • the crystallinity of the ground wood powder is closely related to the dry matter content of the feed. It is possible to achieve almost totally amorphous, such as wood without crystal ⁇ line cellulose, wood powder when grinding screened saw ⁇ dust with 99 % dry matter content. In this study the en- ergy consumption was lower when dry matter content was higher .
  • the formed material component (7) is used in paper application.
  • the material component (7) is added into the paper pulp (10) in the manufacturing (8) of the paper product (9) .
  • the cryogenic processing conditions it was possible to produce pow ⁇ ders with smaller median sizes and narrower size distributions than with the ambient processing condi- tions.
  • the relative degree of crystallinity of the cellulose was influenced by the moisture content of the feed, the processing time and the cryogenic pro ⁇ cessing conditions.
  • Pulverised wood can be utilised in various industrial areas, for example, as reinforcement and filler material for composites or as a raw material source for various degradable chemicals.
  • the small size of the wood particles grants a large specific surface area, which is essential in applications in which the surface activeness is important.
  • the high aspect ratio of the wood particles is important in composite applications, and the relative amount of crystalline cellulose affects the reaction kinetics of cellulose based materials.
  • the median size, specific surface area and crystallinity of the cellulose of the produced wood powders were found to decrease as a function of pulverisation time. It was also found out that the shapes of the particles became more homogeneous and roundish when a longer pulverisation time was used.
  • the processing feeds had a moisture content of 11%
  • the crystallinity of the cellulose was found to decrease less than with the feeds containing lower moisture content processed un- der similar conditions.
  • the studies related to the processing of the wood powder with the vibration mill are limited to conditions in which the moisture con ⁇ tent of the feeds is less than 11%, and there is no available information about the effect of cryogenic conditions on the pulverisation of wood. Therefore, more information about the effect of the moisture con ⁇ tent of the feed and the cryogenic conditions on the pulverisation of wood with a vibration mill is needed to gain a better understanding of the size reduction process.
  • the raw material used in this study was Nor ⁇ way spruce (Picea abies) sawdust from a Finnish sawmill.
  • the sawdust contained a moisture content of 50% and was screened with a vibrating screen using a 4 mm sieve.
  • the underflow was divided into several iden ⁇ tical feed samples.
  • the feed samples were dried in an oven at a temperature of 80°C for various drying times to obtain feeds with different moisture contents.
  • the feed containing the highest moisture content (50 ⁇ 6 ) was not dried at all.
  • the grinding experiments were conducted with the oscillatory ball mill, CryoMill (Retsch) , in which one 25 mm steel ball was used as a grinding medium.
  • the feeds were placed in a 50 ml grinding jar, and in each experiment, 2.0 g (total weight) of the feed was ground for various grinding times with a vibration frequency of 25 Hz at room temperature (ambient or normal conditions) .
  • Replicates were performed from the grinding experiments where the feeds having moisture content of 50% and grinding time over 6 minutes was used. Replicates were performed also from the grinding experiments involving grinding time of 10 minutes. In addition to grinding at room temperature, cryogenic grinding experiments were carried out.
  • the feed inside the grinding jar was exposed to the freezing effect by cooling the outer wall of the jar with nitrogen liquid before grinding (pre- freezing stage) and during grinding.
  • pre- freezing stage the mill was operated slowly at a vi ⁇ bration frequency of 5 Hz while the jar was exposed to the liquid nitrogen for seven minutes.
  • the grinding was carried out as de ⁇ scribed for the ambient conditions.
  • the processing under ambient conditions is shortened as X AC and under cry ⁇ ogenic conditions as x CryoC .
  • the moisture content of the feed is expressed as a number after the shortened form of processing conditions, for example X AC50', which indicates that the feed with the moisture con ⁇ tent of 50% was ground under ambient conditions.
  • the dry matter content of the feeding samples was measured with an MA100 moisture analyser (Sartori- us Mechatronics ) .
  • the moisture content was calculated by extracting the measured dry matter content from 100%.
  • the moisture content of the feeding samples was found to vary by up to 2 percentage points compared with what it was be- fore the experiments.
  • the produced wood powders were split into two portions. The first portion was mixed with water at a 0.2% by weight consistency. Before dilution, the wood powder was dispersed with Sokalan CP 5 dispersant by adding 1 ml of dispersant per 100 mg of wood (dry mass) . The diluted samples were stirred for 30 minutes with a magnetic stirrer and kept 6 minutes in an ul ⁇ trasonic bath to ensure comprehensive dispersion. Af ⁇ ter the dispersion stage, the particle size and aspect ratio distributions were measured from the diluted samples .
  • the volumetric particle size distributions of the ground products were measured using the laser dif ⁇ fraction method (Beckmann Coulter LS 13320) .
  • the maxi- mum size that can be measured with this technique is 2 mm, so if there are any particles that are larger than 2 mm (according to method) , the particle size distri ⁇ bution is not complete. In these cases, the calculated median size would be smaller than it would be if the whole distribution is measured.
  • the dimensionless val ⁇ ue ⁇ * which represents the width of the particle size distributions, was calculated as ( 1 )
  • d 90 and d 10 are the particle sizes corresponding to the 90% and 10% values in the volumetric cumulative size distribution, respectively.
  • This value takes into account particles that make up 80% of the whole volume and therefore describes the width of the volume-based particle size distribution.
  • the cumulative projected area -based aspect ratio distribution of the powders was calculated from optical images acquired with a CCD camera from a tube flow of the diluted powder samples. The flow was introduced into a cuvette with a rectan ⁇ gular shaped cross section during imaging. The aspect ratio distribution was used to calculate the median aspect ratio and the width of the aspect ratio distri ⁇ bution, the latter being defined as the difference be- tween the aspect ratios corresponding to the 90% and 10% values in the distribution.
  • At least 120,000 par ⁇ ticles from each ground product were analysed to cal ⁇ culate the aspect ratio distribution.
  • images were taken from selected samples with a field emission scanning elec ⁇ tron microscope (FESEM, Zeiss Ultra Plus) .
  • the second portion of the selected pulverised powders was dewatered by pressure and compressed into tablets.
  • the relative degree of the crystallinity in terms of the crystal- Unity index (Crl) was calculated from the measured XRD-profiles according to the method developed by Segal et al .
  • Fig. 4 shows the median size and width of the particle size distribution of the wood powders pro ⁇ quizzed under non-cryogenic conditions using feeds of three different moisture contents (1%, 27%, 50 % ) cL S cL function of grinding time.
  • the confidence level in Fig. 4 is estimated only for the experiments with rep ⁇ licates.
  • Fig. 4a shows that the lower moisture content of the feed resulted in a smaller achievable median size in the non-cryogenic grinding.
  • the processing of the feeds with moisture contents of 1%, 27% and 50% resulted in minimum median sizes of approximately 16 ym, 27 ym and 39 ym, respectively.
  • the median size under one hundred micrometres was ob ⁇ tained after 2 minutes of grinding in the case of ACl and AC27 and after 10 minutes in the case of AC50.
  • the width of the particle size distribution follows a sim- ilar trend as that of the median particle size as a function of grinding time (Fig. 4b) .
  • Fig. 4 shows particle size distribution prop ⁇ erties such as (a) median size and (b) the width of the particle size distribution as a function of grind- ing time processed under ambient conditions.
  • the data points with an empty space indicate that there are particles larger than 2 mm, and the whole distribution was not measured. Therefore, these points present val ⁇ ues of median size and ⁇ * that are too small.
  • the er- ror bars shown in the figure represent the confidence interval according to the normal distribution with the 95% confidence level.
  • Fig. 5 shows the median size and width of the size distribution for wood powders processed under cryogenic conditions.
  • Fig. 5 shows particle size distribution prop ⁇ erties such as (a) median size and (b) the width of the particle size distribution as a function of grind ⁇ ing time processed under cryogenic conditions.
  • the da- ta points with an empty space indicate that there are particles larger than 2 mm, and therefore the entire distribution was not measured. Therefore, these points present median size and ⁇ * values that are too small.
  • the error bars shown in the figure for the experiments ground for 10 minutes represent the confidence inter- val according to the normal distribution with the 95% confidence level.
  • Fig. 6 shows the particle size distribution properties of the pul- verised wood powders as a function of moisture content when a grinding time of ten minutes was used.
  • the low ⁇ er the moisture content the smaller the median size and width of the particle size distribution in the case of the powders pulverised under non-cryogenic conditions.
  • Cryogenic grinding decreased the median size and the width of the particle size distribution compared with the powders that were produced without cryogenic conditions.
  • the higher moisture content of the feed resulted in a greater difference in the medi- an size and width of the particle size distribution between the powders produced under cryogenic and ambi ⁇ ent conditions.
  • Fig. 6 shows particle size distribution prop ⁇ erties such as (a) the median size and (b) the width of the size distribution of the pulverised wood as a function of the moisture content of the feed.
  • the er ⁇ ror bars represent the confidence interval according to the normal distribution at the 95% confidence lev ⁇ el.
  • the confidence intervals for the size properties are estimated for every black-coloured data point shown in the figure, whereas the blue data points rep- resent a single experiment. Data points with an empty space indicate that the particle size distribution did not include the larger particles (2 mm) and therefore these points represent values of median size and ⁇ * that are too small.
  • Fig. 7 shows the median aspect ratio and the width of the aspect ratio distribution of the pulverised wood as a function of the moisture content of the feed for grinding times of 10 and 30 minutes.
  • the largest median aspect ratio and the widest aspect ratio distribution was gained with the non-cryogenic grinding from the feed containing the highest moisture content.
  • the median aspect ratio and the width of the as- pect ratio distribution of the powders increased when the moisture content of the feed increased.
  • the cryogenic grinding there were only small differences between the aspect ratio properties of the powders produced from feeds with different moisture contents.
  • the median aspect ratio was 1.5-1.8, while in the case of powders produced in non-cryogenic con ⁇ ditions, it was 1.5-3.1.
  • the median aspect ratio and the width of the aspect ratio of the product was the same or even higher in the case of cryogenic grinding.
  • the width of the aspect ratio distribution follows a simi ⁇ lar trend as the median aspect ratio when considering the non-cryogenic and cryogenic processes separately.
  • Fig. 7 shows projected area -based aspect ra ⁇ tio distribution properties: (a-b) the median aspect ratio and (c-d) the width of the aspect ratio distri ⁇ bution of the pulverised wood as a function of the moisture content of the feed.
  • the error bars represent the confidence interval according to the normal dis ⁇ tribution at the 95% confidence level.
  • the confidence intervals for the median aspect ratio and the width of the aspect ratio distribution are estimated for every black-coloured data point shown in the figure, whereas the blue, red and purple data points represent single experiments .
  • Fig. 8 photos from three different wood powder samples are presented in Fig. 8.
  • category S presents the smallest particles
  • cat- egory M the medium sized particles
  • category L the largest particles found in the photos of the samples.
  • the median aspect ratio is 3.0 and the width of the particle size distribution is 6.6 (produced with the setup AC50)
  • numerous elongated particles in the size categories M and L are observed.
  • the median aspect ratio is 2.1 and the width of the aspect ratio distribution is 2.5 (produced with the setup AC27), some elongated particles can be found alongside non- elongated particles from categories M and L.
  • FIGS. 9a-b show the elongated shape of the particles containing the high median as- pect ratio and the broad aspect ratio distribution.
  • Figs. 9c-d show the roundish shape of the particles with the low median aspect ratio and narrow aspect ra ⁇ tio distribution.
  • Fig. 8 shows charged coupled device camera photos from three wood powder samples containing dif ⁇ ferent aspect ratio (AR) distribution properties. For each sample, three different photos, which are divided into three categories according to size, are shown. Category L stands for the photos in which some of the largest particles within the sample are shown, S stands for the photos in which some of the smallest observable particles within the sample are shown and M stands for the photos in which some of the particles falling between categories L and S are shown.
  • Category L stands for the photos in which some of the largest particles within the sample are shown
  • S stands for the photos in which some of the smallest observable particles within the sample are shown
  • M stands for the photos in which some of the particles falling between categories L and S are shown.
  • Fig. 9 shows FESEM images of particles taken from two wood powder samples containing different as ⁇ pect ratio (AR) distribution properties: (a-b) show particles from powder containing a median aspect ratio of 3.0 and an aspect ratio distribution width of 6.6 and (c-d) show particles from powder containing a me ⁇ dian aspect ratio of 1.5 and an aspect ratio distribu ⁇ tion width of 1.1.
  • AR ⁇ pect ratio
  • Fig. 10 shows the XRD-profiles and crystal ⁇ linity indexes (Crl) of the fresh and oven dried feed material.
  • the amorphous background is different for wood than cellulose due to components such as lignin and hemicelluloses , but it is important that the re ⁇ sults in this study are comparable to each other.
  • Fig. 10 shows the XRD-profiles and crystal- Unity indexes (Crl) of the fresh and oven dried feed.
  • the coloured dashed lines represent the diffraction angles used to determine the relative degree of crys ⁇ tallinity (Crl) in the method developed by Segal et al .
  • the red dashed line represents the diffraction an- gle, the intensity of which contributes strongly to the crystalline region, and the blue dashed line rep ⁇ resents the diffraction angle, the intensity of which contributes strongly to the amorphous region.
  • Fig. 10 shows the XRD profiles and the crys- tallinity indexes of the wood powders produced under cryogenic and non-cryogenic conditions using the two different grinding times and the feeds containing sev ⁇ eral different moisture contents.
  • the changes in the crystallinity of the cellulose can be observed from the XRD-profiles , in which the two-peaked profile of the feed (see Fig. 10) is transformed into a one- peaked profile of the pulverised wood when the mois ⁇ ture content of the feed decreases (see Fig. 11) .
  • Ac ⁇ cording to Figs. 10 and 11 the Crl of the wood de ⁇ creased by at least 5%-units after pulverisation.
  • the lower the moisture content of the feed the lower the value of Crl, which can drop to as low as -21%.
  • Crl remains generally unaffected by the longer grinding time when the moisture content of the feed is higher than 27%.
  • the Crl values of the pulverised powders varied between 20% and 30%, with no distinct correlation to the moisture content of the feed when the grinding was done under cryogenic condi ⁇ tions for ten minutes and with feeds containing mois- ture content greater than 8%.
  • the value of Crl decreased to 10% over ten minutes of pulverisation.
  • the Crl decreased from 10% to -9%, while the moisture content of the feed decreased from 50% to 1%.
  • the crystallinity index appears to be a good parameter for detecting differences in the relative crystallinity of cellulose in wood, although negative values can also be obtained.
  • a strong de ⁇ crease in the crystallinity of the cellulose has been reported, although the specific surface area and thus the particle size remained almost constant.
  • non-cryogenic milling with the oscillatory ball mill a similar effect was found when the mois- ture content of the feed was very low but not with the high moisture contents.
  • the particle size did not completely even out at a certain level as a function of grinding time.
  • cryogenic grinding the relative degree of crystallinity of the powders produced decreased sub ⁇ stantially between grinding times of ten and thirty minutes, although the changes in the particle size were rather small.
  • Fig. 11 shows the XRD-profiles and crystal ⁇ linity indexes (Crl) of the wood powders produced from the feeds containing different moisture contents.
  • Norway spruce sawdust and the properties of the pow ⁇ ders obtained are strongly influenced by the moisture content of the feed.
  • the lower moisture content of the feed results in a smaller me ⁇ dian size and narrower size distribution, whereas the particles shape become rounder.
  • the relative degree of crystallinity of the cellulose in the wood decreases as a function of decreasing moisture content and is affected by the processing time when the moisture con ⁇ tent of the feed is low.
  • the size and shape properties are almost independent of the moisture content of the feed. With the cryogenic grinding it is possible to produce wood powders containing smaller median size and narrower size distribution compared with the non- cryogenic grinding.
  • the rela ⁇ tive degree of crystallinity is influenced by the moisture content of the feed and, especially, by the processing time.
  • the effects of moisture content and processing time on the relative degree of crystallini- ty differ between ambient and cryogenic processing conditions .
  • the method according to the present invention is suitable in different embodiments to be used for making the most different kinds of material compo ⁇ nents.
  • the material component according to the present invention is suitable in different embodiments to be used in different final products, e.g. paper products and composite products.

Landscapes

  • Debarking, Splitting, And Disintegration Of Timber (AREA)

Abstract

L'invention se rapporte à un procédé de fabrication d'un composant de matériau à partir d'un matériau de départ d'origine végétale de sorte que le composant de matériau soit formé par broyage à partir du matériau de départ. Selon l'invention, le matériau de départ est prétraité afin d'améliorer la dégradation du matériau de départ pendant le broyage du matériau de départ. En outre, l'invention se rapporte à un composant de matériau, à une utilisation du composant de matériau et à un produit de papier.
PCT/FI2012/050870 2011-09-07 2012-09-07 Procédé de fabrication d'un composant de matériau, composant de matériau et son utilisation et produit de papier WO2013034811A1 (fr)

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FI20115879A FI20115879L (fi) 2011-09-07 2011-09-07 Menetelmä materiaalikomponentin valmistamiseksi, materiaalikomponentti ja sen käyttö sekä paperituote
FI20115879 2011-09-07
FI20116283 2011-12-19
FI20116283 2011-12-19

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015052380A1 (fr) 2013-10-11 2015-04-16 Upm-Kymmene Corporation Procédé de fabrication d'un papier, papier et son utilisation, composition de fabrication et composition à base de bois

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2310459A1 (de) * 1973-03-02 1974-09-12 Fritz Dr Opderbeck Verfahren zum erzeugen von faserstoff aus pflanzlichem material
WO1990005208A1 (fr) * 1988-11-10 1990-05-17 Sven Ljungbo Procede permettant de reduire la consommation d'energie lors de la production mecanique de pate a papier
US20080022595A1 (en) * 2006-07-31 2008-01-31 Eric Lemaire Process for preparing a feed containing biomass intended for subsequent gasification
US20080053631A1 (en) * 2004-04-28 2008-03-06 Eberhard Perplies Method and Device for Grinding Cellulose
WO2009036480A1 (fr) * 2007-09-21 2009-03-26 Lenzing Ag Poudre de cellulose et son procédé de préparation
WO2009080894A1 (fr) * 2007-12-21 2009-07-02 Upm-Kymmene Oyj Procédé de fabrication d'un pigment organique
EP2172590A1 (fr) * 2008-09-29 2010-04-07 Messer Austria GmbH Procédé et dispositif de préparation de matières brutes lors de la fabrication de papier, de carton ou de plaques de fibres
WO2010063029A1 (fr) * 2008-11-28 2010-06-03 Kior Inc. Comminution et densification de particules de biomasse
WO2010068773A1 (fr) * 2008-12-10 2010-06-17 Kior Inc. Procédé de préparation d'un matériau composite biomasse-catalyseur pouvant être fluidisé
JP2011127256A (ja) * 2009-12-18 2011-06-30 Daio Paper Corp 再生粒子の製造方法及び再生粒子

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2310459A1 (de) * 1973-03-02 1974-09-12 Fritz Dr Opderbeck Verfahren zum erzeugen von faserstoff aus pflanzlichem material
WO1990005208A1 (fr) * 1988-11-10 1990-05-17 Sven Ljungbo Procede permettant de reduire la consommation d'energie lors de la production mecanique de pate a papier
US20080053631A1 (en) * 2004-04-28 2008-03-06 Eberhard Perplies Method and Device for Grinding Cellulose
US20080022595A1 (en) * 2006-07-31 2008-01-31 Eric Lemaire Process for preparing a feed containing biomass intended for subsequent gasification
WO2009036480A1 (fr) * 2007-09-21 2009-03-26 Lenzing Ag Poudre de cellulose et son procédé de préparation
WO2009080894A1 (fr) * 2007-12-21 2009-07-02 Upm-Kymmene Oyj Procédé de fabrication d'un pigment organique
EP2172590A1 (fr) * 2008-09-29 2010-04-07 Messer Austria GmbH Procédé et dispositif de préparation de matières brutes lors de la fabrication de papier, de carton ou de plaques de fibres
WO2010063029A1 (fr) * 2008-11-28 2010-06-03 Kior Inc. Comminution et densification de particules de biomasse
WO2010068773A1 (fr) * 2008-12-10 2010-06-17 Kior Inc. Procédé de préparation d'un matériau composite biomasse-catalyseur pouvant être fluidisé
JP2011127256A (ja) * 2009-12-18 2011-06-30 Daio Paper Corp 再生粒子の製造方法及び再生粒子

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015052380A1 (fr) 2013-10-11 2015-04-16 Upm-Kymmene Corporation Procédé de fabrication d'un papier, papier et son utilisation, composition de fabrication et composition à base de bois

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