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The bases of special methods of biomass processing into prospective materials. Tutorial

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Procedure.
1. Make specimens of plastics from cellulose containing wood
particles of different fractions in laboratory.
The sequence of a specimen making process:
select portions of hardwood and softwood aggregate to make a
specimen with fractional size 0.5 mm;
moisten the portion of the aggregate up to 20 % humidity;
fill the aggregate in the mold, mold by cold perform method at a
pressure of 1 MPa to make a transportable briquette;
produce hot pressing of the briquette at a working pressure of 5 MPa; press plates temperature 180 0C with continuous cooling to 18– 25 0C, while maintaining the working pressure;
normalize the quality of the resulting specimens under normal
conditions for 1 day;
cut out boards for specimens.
2. Test physical and mechanical properties of the resulting plastics in accordance with standard methods for wood boards: strength is tested in accordance with GOST 10635-88 «Particle boards. Methods for determining ultimate strength and modulus of elasticity in bending», physical properties are tested in accordance with GOST 10634-88 «Wood particle boards. Methods of determination of physical properties».
2.1. Determination of strength and modulus of elasticity in bending.
Preparing specimens for testing
The specimens should be in the form of rectangular parallelepiped with thickness equal to the board thickness. It should be 50 mm wide, its length should be 10–15-fold of thickness plus 50 mm. One half of the specimens are cut off along the testing board, the other half is cut off across the board. The thickness of the specimen is measured at the center of the transverse.
The length of the specimen is measured by its longitudinal axis, the width is measured by its transverse axis.
Testing
The distance between the centers of support is 10–15-fold of the specimen thickness. The specimen is put on the supports of the testing machine marks so that the longitudinal axis of the specimen is perpendicular to the axes of the supports, and the transverse axis is at the same vertical plane with the vertical axis of the knife blade.
51
In the experiment one half of the specimens with the same orientation
2
23bhH
Fl
=
( )
( )
12
3
12
3
4 SSbh
FFl
E
=
are put face up and the other half is put face down on the test device supports.
To determine the flexural strength the specimen is loaded at a constant speed up to destruction and the maximum load is recorded with an accuracy1 %. Time from start of loading to failure of the specimen should be 60 ± 20 s.
To determine the flexural modulus the specimen is loaded at a knife moving speed 12 mm/min up to 1/3 of the breaking load. At least eight readings of the specimen deflection are taken at regular intervals of load increment.
The deflection is measured in the plane of loading up to 0.01 mm. The measuring device sensor should not be affected by local crushing of the specimen.
The results of load increment and deflection are plotted in a straight­line graph, making average value spread from the linear law.
Processing results
The flexural strength of the specimen σ (MPa) is calculated using the formula below:
, (3)
where F – loading force acting on the specimen at the moment of destruction, Н;
l – the supports span of the testing machine, mm; b – the width of the specimen, mm; h – the thickness of the specimen, mm.
The result is rounded up to the first decimal place.
The flexural modulus of the specimen Е (MPa) is calculated using the formula below:
, (4)
where l – the supports span of the testing machine, mm;
b – the width of the specimen, mm; h – the thickness of the specimen,
mm;
F2-F1 – the fixed (2-3 intervals) load increment, Н;
S2-S1 – the deflection increment corresponding to the fixed load increment determined according to the graph up to 0.1 mm.
52
The result is rounded up to a whole number.
w
%100
1
12
=
m
mm
w
The result of testing a board is the arithmetic mean from the test results of all specimens taken from this same board. These values are expressed accurate to one decimal place and to a whole number respectively.
2.2. Determination of physical properties: water absorption and
thickness swelling.
The specimens are weighed with an error not exceeding 0.1 % maximum in half an hour after conditioning. The thickness of the specimen depending on its size is measured:
(25х25) mm – at one point in the center of the face;
(100х100) mm – at four points.
The specimens are placed into a can with water at a temperature of 20 ± 1 0С. They should not be in contact with each other and with the bottom and side walls of the can. The specimens should be kept at (20 ± 2) mm below the water surface. The specimens with (100х100) mm size are placed in an upright position. The exposure time of the specimens in water should be:
– h±5 min for the specimens with (25х25) mm size;
h±15 min for the specimens with (100х100) mm size.
The sequential test is allowed for 2 and 24 h, but the second time the specimens immerse into water no later than in 10 min. After exposure the specimens are taken from water.
To determine the thickness swelling the surface of the specimens is dried of water drops with filter paper.
To determine the water absorption the specimens with (100х100) mm size each are placed individually in a horizontal position between two sheets of filter paper and piled. The specimens with (25х25) mm size are laid in rows between sheets of filter paper. The load is put on the specimens for 30 s. Then the load and filter paper are removed. The specimens are weighed for the second time. The thickness is measured no later than 10 min after taking the specimens from water.
The water absorption of the specimen
expressed in % is
calculated using the formula below:
53
, (5)
where m1 – the mass of the specimen before immersion into water, g;
w
t
%100
1
12
=
t
tt
t
w
№ of the speci­men
The aggregate
Frac­tion, mm
Stren gth, MPa
Thick­ness swell­ling, %
Volu­me swell­ling, %
Water absorp­tion, %
The mass loss during combus­tion, %
1
Birch
2
Pine
3
Annual
m2 – the mass of the specimen after immersion into water, g. The result is rounded up to the first decimal place.
The thickness swelling of the specimen
expressed in % is
calculated using the formula below:
, (6)
where t1 – the thickness of the specimen before water immersion, mm; t2 – the thickness of the specimen after it has been taken off the water, mm.
The result is rounded up to the first decimal place.
The result of testing a board is the arithmetic mean from the test results of all specimens taken from this same board. These values are expressed accurate to one decimal place.
The results of the research are presented in the form of the table.
2.5.4. Technology for producing the wood-polymer composite (WPCs)
by extrusion
Objectives: to conduct experimental study on the preparation and determination WPCs physical and mechanical properties by extrusion
Materials and reagents: wood sawdust, wood flour, thermoplastics, antioxidant.
54
Equipment:
testing sieve;
laboratory oven;
scales with an accuracy of 0.1;
calendering machine;
extruder;
liquid thermostat with an accuracy of temperature control ± 1.0
0
С; desiccator; cans from glass or enameled steel; ruler; distilled water.
Procedure.
Make specimens of WPCs in laboratory. The sequence of the specimen making process:
1) Preparation of the components: dry wood particles to moisture content of less than 1 % and fractionate by size. Part of the aggregate is milled to the size of wood flour.
2) Dosing. The following ratio between wood flour and thermoplastics is used: 80/20, 70/30, 60/40.
Fig. 2.5. Schematic diagram of the rolling machine:
1 – wood particles, 2 – polypropylene, 3 –rolls
3) Mixing of the components takes place in the rolling machine. The result is semi-finished WPCs suitable for loading into the extruder.
4) Extrusion. The resulting semi-finished WPCs are sent into a single-screw extruder. First, the cylinder is heated to the specified temperature then the screw is started. Each polymer has its own temperature in accordance with reference data. The temperature for each polymer is
55
selected in accordance with reference data. The melting temperature of polypropylene is known to be about 175 0С.
The single-screw extruder is used to produce WPCs (fig. 2.6). The components of WPCs are poured into the hopper. Loading of inter turn space under the hopper bin takes place in the screw length segment that equals to (1–1.5) D. The beads are forced forward due to the difference of friction force of the polymer on the inner surface of the cylinder and the surface of the screw. The polymer adjacent to the surface of the cylinder begins to melt. Since the depth of screw cut decreases as the material flows, the resulting pressure makes the cork be tightly pressed to the hot cylinder wall where the polymer melts.
Fig. 2.6. Scheme of horizontal single-screw extruder:1 – drive motor;
2 – extruder head; 3– heater barrel; 4 – barrel ; 5 – screw; 6 – hopper;
7 – axiallager; 8 – extruder gear ; 9 – tachometer; 10 – voltage regulator;
11 – multimeter for measuring temperature; 12 – die; 13 – ammeter;
14 – voltmeter
2. Test physical and mechanical properties of the resulting plastics in accordance with standard methods: density is tested in accordance with GOST 15139-69 «Plastics. Methods for the determination of density (mass density)», strength is tested in accordance with GOST 25.602-80 «Design calculation and strength tests. Methods of mechanical testing of polymeric
56
composite materials. Test for compression properties at normal, elevated and low temperatures», GOST 25.601-80 «Design calculation and strength tests. Methods of mechanical testing of polymeric composite materials. Test for tensile properties on plane specimens at normal, elevated and low temperatures», GOST 25.604-82 «Design calculation and strength tests. Methods of mechanical testing of polymeric composite materials. Test for bending properties at normal, elevated and low temperatures», GOST 4650­80 «Plastics. Methods for the determination of water absorption».
2.1. Determination of compressive strength. Similarly to the procedure described in the laboratory work № 6.
2.2. Determination of water absorption.
Similarly to the procedure described in the laboratory work № 7.
2.3. Determination of WPCs bending properties.
Preparing the specimens for testing.
To determine the maximum bending stress, the modulus of elasticity and the dependence of the deflection on load when loading a specimen up to destruction the specimen in the form of a strip of rectangular cross section is used. The specimens are cut or shaped of the panels in the direction of the principal axes of the material orthotropy. In accordance with GOST 2789-73 the specimens should have a smooth flat surface no rougher than Rа = 20 uM without blistering, chipping, cracks, delamination and other defects visible to the naked eye. The specimens are conditioned before the test in accordance with GOST 12423-66, if special conditioning is not listed in the normative and technical documentation for composite materials. The process from the end of preparation of molded specimens or composite material that they are cut from to their testing including time for conditioning should take not less than 16 hours. Numbering the specimens is carried out with paint with a soft pencil before the test. The thickness of the specimen is measured with accuracy up to 0.05 mm. The width is measured in three places of its test portion with accuracy up to 0.10 mm. The arithmetic mean values of thickness and width of the specimen are determined. The results are recorded in the test report.
Testing
The test at normal temperature is carried out in a room or enclosed space at temperature and relative air humidity specified in technical documentation for the testing material. If there are no specifications, the test is carried out at one of the standard atmospheres in accordance with GOST 12423-66.
57
The test at elevated and low temperature is carried out in specially
и
n
F
wbhFl
=
3
3
и
п
4
F
provided heat chambers and cryochambers. The test temperature and its permissible variations are determined in accordance with specifications or standards for the material. Otherwise they are determined in accordance with GOST 14359-69.
Testing at elevated and low temperature the time required for a complete heating or cooling of the specimen before the test should be specified in the regulatory and technical documentation on the test material. If there are no specifications, the specimen is exposed at the given temperature at least for 20 min for 1 mm of its thickness.
The specimen is set with its wide side on the supports of the testing machine. The upper surface of the specimen comes in contact with the heated loading tip. The fit of the specimen to the supports of the tip surface is determined. The rate of loading tip displacement is determined according to the specifications of the material. If there are no specifications the rate equals 5–20 mm/min. While determining the modulus of elasticity the specimen is loaded with a given constant speed. Deflection values and corresponding load are recorded. If the diagram deviates from the linear one the test is stopped. The specimen is unloaded. While determining the dependence of the deflection on load the specimen is loaded with a given constant speed. The deflection and the load are continuously recorded up to destruction of the specimen. While determining the tensile strength the maximum load that precedes the destruction of the specimen is recorded.
While determining the modulus of elasticity the specimen can be loaded stepwise or continuously up to the load that does not exceed 50 % of destructive one. Under continuous loading deflection and load are recorded automatically. In the case of a step loading deflection measurements are performed at each load value. The number of steps should be at least four. The recommended value is 5–10% of the maximum load before to the destruction of the specimen.
Processing results
The modulus of elasticity in transverse bending
expressed in
MPa is calculated using the formula below:
, (7)
58
where
F
w
F
wbh
Fcl
=
3
2
и
4
3
F
2
max
F5,1
bh
l
=
№ of the specimen
The aggre­gate
Fraction, mm
Density, kg/m
3
Compres­sive strength, MPa
Flexu­ral strength, MPa
Water absorp­tion, mg
– increment of load, МН;
l –support span, mm;
b, h – width and height of the specimen, mm;
– increment of deflection in the middle of the specimen
corresponding to load change of
, mm.
The modulus of elasticity in pure bending Еи expressed in MPa is calculated using the formula below:
. (8)
Tensile strength in transverse bending  expressed in MPa is calculated using the formula below:
, (9)
where F
– maximum load when at the moment of the specimen
max
destruction, МН.
2. Present the results of the research in the form of the table:
2.5.5. Technology for producing the wood-polymer composite by casting process
Objectives: to conduct experimental studies on the preparation and
determination WPCs physical and mechanical properties by casting method.
Materials and reagents:
wood sawdust; wood meal of various grades and species; thermoplastics; antioxidant.
59
Equipment:
Thermoplastics, %
Wood sawdust, %
40
60
30
70
20
80
Thermoplastics, %
Wood meal, %
40
60
30
70
20
80
testing sieve; laboratory oven; scales with an accuracy of 0.1; rolling machine; casting machine; liquid thermostat with an accuracy of temperature control ± 1.0 desiccators;
– сans from glass and enameled steel; – ruler; – distilled water; – phosphorus pentoxide or other dryers.
Procedure.
Prepare specimens of WPCs in laboratory. The sequence of the specimen preparation process:
1) Preparation of the components: drying of wood meal and sawdust
to a moisture content of less than 1 %.
2) Weighing components. The components ratio is presented in Table
2.4 and 2.5.
0
C;
Table2.4
Table2.5
3) Calendering. The ingredients are put into the machine one by one: polyethylene, then wood meal with additives. The mixing process takes about 10 min. The result is a tape, semi-finished WPCs.
60