CN105572167B - A kind of method for rapidly testing of wood plastic composite antioxygenic property - Google Patents
A kind of method for rapidly testing of wood plastic composite antioxygenic property Download PDFInfo
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- CN105572167B CN105572167B CN201610014673.1A CN201610014673A CN105572167B CN 105572167 B CN105572167 B CN 105572167B CN 201610014673 A CN201610014673 A CN 201610014673A CN 105572167 B CN105572167 B CN 105572167B
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- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
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Abstract
The present invention discloses a kind of method for rapidly testing of wood plastic composite antioxygenic property, the uniform wood plastic composite raw material of mixing is ground into powdered sample, during room temperature, the opening aluminium crucible for filling certain mass powdered sample and reference aluminium crucible are placed on the sample support of differential scanning calorimeter, after being passed through 5 10min of nitrogen of certain flow, experimental test temperature is warming up to certain rate, then 5 15min of constant temperature.Then, gas is switched to rapidly the oxygen of same traffic, continues constant temperature, until showing termination test when oxidation heat liberation reaches maximum on the heating curve of record.By analyzing heating curve, the oxidation induction time of wood plastic composite raw material is determined；And then derive the oxidation induction time of wood-plastic products；So as to quickly measure the antioxygenic property of wood-plastic products.It is an advantage of the invention that test process is simple, required sample mass is few, and accuracy, the repeatability and reproducibility of testing result are good and applied widely.
Description
Technical field
The present invention relates to a kind of method for rapidly testing of wood plastic composite antioxygenic property, belong to field of compound material,
Fall within Forestry Engineering field.
Background technology
Wood plastic composite（wood-plastic composites, WPC）It is using plant fiber and plastics to be main former
Material, and appropriate additive is added in, the Novel environment-friendlymaterial material being prepared with extrusion, molding or injection moulding has a vast market
Prospect and development potentiality.However the effect of WPC light, heat and oxygen etc. in storage, processing and routine use, heat easily occurs
Oxidation, aging, the color of material change, and influence product appearance, and the physical mechanical property of material can decline, and influence
The application field of material, the service life for shortening material.Therefore, in WPC product developments and performance test, material is correctly evaluated
Thermal stability and antioxygenic property be of great significance.The test of antioxygenic property can be WPC composition of raw materials and production work
The theoretical guidance with data of the definite offer of skill, and also there is reference significance for the prediction of WPC service lifes.
Currently, WPC gets growing concern for and approves in world wide, and yield and usage amount are all quick year by year
Increase；But China has a long way to go to the research and development and popularization and application of WPC with foreign countries, and wood-plastic products quality is irregular
Uneven, the speed of research is unable to catch up with the speed of application, also lacks the standard of system, only there are three relevant criterions so far：Country's mark
Quasi- GB/T 24508-2009 Wood-plastic floors, standard GB/T/T 24137-2009 wood-plastic decorative boards, forestry industry standard LY/T
1613-2004 squeezes wood-plastic composite panel.At present, the domestic industry that there is no wood plastic composite antioxygenic property test method
Standard and national standard, relative, the only code test of polyolefin plastics oxidation induction time and oxidation induction temperature
Method, such as standard GB/T/T 19466.6-2009 differential scanning calorimetries（DSC）6th part：Oxidation induction time（Isothermal
OIT）And oxidation induction temperature（Dynamic OIT）Measure, American Society Testing and Materials's ASTM D3895-07 differential scanning amounts
Standard test method of the hot method to the oxidation induction time of polyolefin, International Organization for standardization ISO 11357-6:2008 plastics are poor
Show scanning calorimetry（DSC）6th part：Oxidation induction time（Isothermal OIT）And oxidation induction temperature（Dynamic OIT）Measure.
But these standards are only applicable to polyolefin plastics, also fail to provide antioxygenic property of the unified method by plastic raw materials
It is inferred to the antioxygenic property of plastic product.
The content of the invention
There is heated oxygen effect for above-mentioned wood plastic composite and thermal-oxidative ageing easily occurs, and at present there is no wood plastics composites
The deficiencies of test method of material against oxidative performance, the object of the present invention is to provide a kind of wood plastic composite antioxygenic properties
Method for rapidly testing.
The present invention adopts the following technical scheme that implementation：A kind of wood plastic composite antioxygenic property of the present invention
Method for rapidly testing, it is characterized in that, carry out as follows：It will be crushed after uniform wood plastic composite raw material mixing will be blended
Into powdered sample, during room temperature, the opening aluminium crucible for filling certain mass powdered sample and reference aluminium crucible are positioned over differential
On the sample support for scanning calorimeter, after being passed through the nitrogen 5-10 min of certain flow, experiment is warming up to certain rate
Test temperature, then constant temperature 5-15 min；Gas is then switched to rapidly the oxygen of same traffic by gas converter, after
Continuous constant temperature, until the energy of record --- termination test when oxidation heat liberation reaches maximum is shown on the heating curve of time relationship；
Experiment finishes, and gas is switched to nitrogen and is cooled to room temperature instrument；By analyzing heating curve, wood plastic composite original is determined
The oxidation induction time of material；When deriving that the oxidation of wood-plastic products induces by the oxidation induction time of wood plastic composite raw material
Between；According to the length of wood-plastic products oxidation induction time, the antioxygenic property of wood-plastic products is measured.
The wood plastic composite, by quality proportioning：30 ~ 80 parts of plastic substrate, 10 ~ 50 parts of plant fiber, processing helps
Made of 1 ~ 20 part of agent, plastic substrate therein is polyethylene（PE）, polypropylene（PP）, polyvinyl chloride（PVC）Resin granular material or
One kind in powder, enhancing phase plant fiber therein is wood powder, bamboo powder, powdered rice hulls, Wheat Straw powder, one kind in bagasse or
The two or more mixtures formed with arbitrary proportion, and moisture content is 1% ~ 3%, average grain diameter is the mesh of 40 mesh ~ 200；It is therein to add
Work auxiliary agent for lubricant, coupling agent, interfacial compatibilizer, antioxidant, foaming agent, pigment, filler, one kind in impact modifier or
The two or more mixtures formed with arbitrary proportion.
The wood plastic composite raw material sample is to be ground into powdered sample of the grain size less than 1 mm by plastic crusher,
The quality of the wood plastic composite raw material powder sample of measurement is 8 mg-15 mg.
The nitrogen and oxygen is analysis level, and wherein up to more than 99.99%, the purity of oxygen reaches the purity of nitrogen
More than 99.5%；The flow of nitrogen and oxygen is 40-80 ml/min.
The experimental test temperature is 180 DEG C -200 DEG C；The heating rate is 10 DEG C/min-30 DEG C/min.
The oxidation induction time to start to be passed through oxygen as time zero, using when m- heat flow rate as X-Y axis draw
Heating curve for baseline, tangent line when which can reach maximum with oxidation heat liberation at the greatest gradient of exotherm intersects,
The intersection point corresponding time is oxidation induction time；Each sample retest 3 times, and using average value as last test
As a result.
According to a large number of experiments and theoretical proof, wood plastic composite raw material passes through extrusion molding either injection moulding or pressure sintering
It is prepared into during wood-plastic products, the antioxygenic property of wood-plastic products can decline;Wherein, the wood-plastic products that prepared by extrusion molding,
Its oxidation induction time is only the 20%-25% with the wood plastic composite raw material oxidation induction time of formula；Prepared by injection moulding
Wood-plastic products, oxidation induction time are only the 20%-30% with the wood plastic composite raw material oxidation induction time of formula；Hot pressing
Wood-plastic products prepared by method, oxidation induction time are only the 15%- with the wood plastic composite raw material oxidation induction time of formula
20%;Accordingly, it is capable to the oxidation induction time of wood-plastic products, wood moulding are derived by the oxidation induction time of wood plastic composite raw material
The oxidation induction time of product is longer, illustrates that its antioxygenic property is stronger.
The oxidation induction time and experimental test temperature, heating rate, sample mass, nitrogen and oxygen flow these
Test condition is related；When describing the oxidation induction time of wood-plastic products, the knot tested under which kind of test condition need to be particularly pointed out
Fruit when comparing the oxidation induction time of wood-plastic products, need to also be tested under same test condition.
The heating rate is the integral multiple of 10 DEG C/min.
The features and advantages of the invention are：Test method is simple, and the testing time is shorter, and it is few to test required sample mass,
Testing result accuracy, repeatability and reproducibility are good, and applied widely, suitable for testing extruded method, injection moulding, molding
Unexpanded, foaming polyethylene (PE) base, polypropylene prepared by method（PP）Base and polyvinyl chloride (PVC) base wood-plastic composite material.
Meanwhile only powdered wood plastic composite raw material need to be prepared as test sample, reduce and prepare wood plastic composite raw material
Into the complicated processes of wood-plastic products, test process is simple and quick.
Specific embodiment
The present invention is clear from reference to embodiment, the wood plastic composite, and composition of raw materials is as follows：Poly- third
63.3 parts of alkene, 30 parts of wood powder, 3 parts of antioxidant, interfacial compatibilizer maleic anhydride inoculated polypropylene（MAPP）2.7 parts, lubricant
1 part of stearic acid.（Described part refers to parts by weight）.
The polypropylene be weight average molecular weight Mw be 100000 ~ 500000, crystallinity for 30% ~ 80%, melt index (MI) be
The profax resin granular material of 0.5-20 g/10min；Wood powder is purchased from jewel bamboo powder Co., Ltd of Zhejiang Linan City, grain size 60-
120 mesh；Lubricant stearic acid is commercially available；Antioxidant is 1010/ phosphite antioxidant 168 of hindered phenol anti-oxidants
With mass ratio 1:The compound of 1 mixing, purchased from Ciba of Switzerland；MAPP is purchased from Nanjing De Ba Chemical Co., Ltd.s, grafting rate
For 1.09%.
The wood plastic composite raw material powder preparation method of sample is as follows：Wood powder is placed in 105 DEG C of baking oven
When drying 10 is small.By above-described formula, 40 DEG C of whens, put polypropylene, lubricant, antioxidant, interfacial compatibilizer, wood powder
Enter in high-speed mixer, after stirring is warming up to 110 DEG C, 10 min of incorporation time cools down discharging, premix is made, then will be pre-
Batch mixing is uniformly mixed through mixer is prepared into mixing material, and mixing temperature is 180 DEG C, 40 r/min of rotating speed, 15 min of mixing time；
Mixing material is finally ground into powdered sample of the grain size less than 1mm through plastic crusher.
The oxidation induction time test of wood plastic composite raw material is as follows：During room temperature, opening for 10 mg powdered samples will be filled
Mouth aluminium crucible and reference aluminium crucible are placed on the sample support of differential scanning calorimeter, and it is 50 ml/min's to be passed through flow
After nitrogen 5min, 200 DEG C are warming up to the heating rate of 20 DEG C/min, then constant temperature 5min.Then, it is fast by gas converter
Gas is switched to the oxygen that flow is 50 ml/min by speed, continues constant temperature, until the energy of record --- and the heat of time relationship is bent
Termination test when oxidation heat liberation reaches maximum is shown on line.Experiment finishes, and gas is switched to nitrogen and is cooled to instrument
Room temperature.Each sample retest 3 times, and using average value as last test result.
Three examples of implementation are respectively adopted extrusion molding, injection moulding and die pressing and prepare wood plastic composite below, and respectively
Molding wood-plastic products are ground into test powders of the grain size less than 1 mm through pulverizer, using wood plastics composite as described above
The test method of material feedstock oxidation induction time, the oxidation induction time of wood-plastic products, thus compares wood moulding after test shaping
The oxidation induction time of composite material raw material and wood-plastic products.
Embodiment one
Wood moulding particle after crushing through double screw extruder is melted, is blended, is squeezed out, cooling and shaping, shaping wood moulding
Composite board.Extruder barrel heat one section to five sections of temperature be respectively 186 DEG C, 180 DEG C, 175 DEG C, 172 DEG C,
170 DEG C, merging core temperature is 165 DEG C, and die heating temperature is 180 DEG C, 175 DEG C of mold temperature.By the WPC of extrusion molding
Product is ground into test powders of the grain size less than 1 mm through plastic crusher.
Embodiment two
By the wood moulding particle after crushing through injection molding machine injection molding, 185 DEG C of nozzle temperature, one section of 185 DEG C of temperature of injection, note
Penetrate two sections of 175 DEG C of temperature, one section of pressure 6MPa of injection, two sections of pressure 4.5MPa, dwell pressure 6.5MPa, 2.5s when injection is total,
Dwell time 10s.The WPC products of injection molding are ground into test powders of the grain size less than 1 mm through plastic crusher.
Embodiment three
Wood moulding uniform particle after crushing is spread in mold, moves into compact hot press, hot pressing temperature is 180 DEG C, in advance
Heat is fully melted to particulate material, and hot pressing 10min is then turned off hot press heating power supply, and natural cooling 15min then opens water
Cooling system is cooled to 60 DEG C, takes out sample, and test powders of the grain size less than 1 mm are ground into through plastic crusher.
Polypropylene base wood molding product in embodiment 1, example 2 and example 3, oxidation induction time are respectively 8.1 min, and 7.7
Min and 4.6 min, and the oxidation induction time of the polypropylene base wood-plastic composite material raw material is 28.2 min.
In conclusion the test method of the present invention can be used for testing the oxidation induction time of wood plastic composite, and can
The oxidation induction time of wood-plastic products, the oxidation of wood-plastic products are derived with the oxidation induction time by wood plastic composite raw material
Induction time is longer, and antioxygenic property is stronger.Wherein, the wood-plastic products that prepared by extrusion molding, oxidation induction time are same match somebody with somebody
The 20%-25% of the wood plastic composite raw material oxidation induction time of side；Wood-plastic products prepared by injection moulding, oxidation induction time
For the 20%-30% of the wood plastic composite raw material oxidation induction time of same formula；Wood-plastic products prepared by pressure sintering, oxidation lure
It is the 15%-20% with the wood plastic composite raw material oxidation induction time of formula to lead the time.
Claims (4)
1. a kind of method for rapidly testing of wood plastic composite antioxygenic property, it is characterized in that, it carries out as follows：It will blending
It is ground into powdered sample after uniform wood plastic composite raw material mixing, during room temperature, opening for certain mass powdered sample will be filled
Mouth aluminium crucible and reference aluminium crucible are positioned on the sample support of differential scanning calorimeter, are passed through the nitrogen 5- of certain flow
After 10 min, experimental test temperature is warming up to certain rate, then constant temperature 5-15 min；Then it is fast by gas converter
Gas is switched to the oxygen of same traffic by speed, continues constant temperature, until the energy of record --- it is shown on the heating curve of time relationship
Show termination test when oxidation heat liberation reaches maximum；Experiment finishes, and gas is switched to nitrogen and is cooled to room temperature instrument；It is logical
Analysis heating curve is crossed, determines the oxidation induction time of wood plastic composite raw material；It is induced by the oxidation of wood plastic composite raw material
Time derives the oxidation induction time of wood-plastic products；According to the length of wood-plastic products oxidation induction time, wood-plastic products are measured
Antioxygenic property；
The wood plastic composite, by quality proportioning：30 ~ 80 parts of plastic substrate, 10 ~ 50 parts of plant fiber, processing aid 1 ~
Made of 20 parts, plastic substrate therein is polyethylene（PE）, polypropylene（PP）, polyvinyl chloride（PVC）Resin granular material or powder
In one kind, enhancing phase plant fiber therein is wood powder, one or both of bamboo powder, powdered rice hulls, Wheat Straw powder, bagasse
The mixture formed above with arbitrary proportion, and moisture content is 1% ~ 3%, average grain diameter is the mesh of 40 mesh ~ 200；Processing therein helps
Agent is one or both of lubricant, coupling agent, interfacial compatibilizer, antioxidant, foaming agent, pigment, filler, impact modifier
The mixture formed above with arbitrary proportion；
The nitrogen and oxygen is analysis level, the wherein purity of nitrogen up to more than 99.99%, the purity of oxygen up to 99.5% with
On；The flow of nitrogen and oxygen is 40-80 ml/min；
The experimental test temperature is 180 DEG C -200 DEG C；The heating rate is 10 DEG C/min-30 DEG C/min, and is 10
DEG C/integral multiple of min.
2. a kind of method for rapidly testing of wood plastic composite antioxygenic property according to claim 1, it is characterised in that:
The wood plastic composite raw material sample is to be ground into powdered sample of the grain size less than 1 mm by plastic crusher, is measured
Wood plastic composite raw material powder sample quality be 8 mg-15 mg.
3. a kind of method for rapidly testing of wood plastic composite antioxygenic property according to claim 1 or 2, feature exist
In:
The oxidation induction time to start to be passed through oxygen as time zero, using when the heat drawn as X-Y axis of m- heat flow rate
Curve is baseline, and tangent line when which can reach maximum with oxidation heat liberation at the greatest gradient of exotherm intersects, the friendship
The point corresponding time is oxidation induction time；The oxidation induction time and experimental test temperature, heating rate, sample matter
Amount, these test conditions of nitrogen and oxygen flow are related；Which kind of when describing the oxidation induction time of wood moulding, need to particularly point out in survey
It is being tested under the conditions of examination as a result, when comparing the oxidation induction time of wood moulding, need to also be tested under same test condition, Mei Geshi
Sample retest 3 times, and using average value as last test result.
4. a kind of method for rapidly testing of wood plastic composite antioxygenic property according to claim 1 or 2, feature exist
In:
According to a large number of experiments and theoretical proof, either prepared by injection moulding or pressure sintering by extrusion molding for wood plastic composite raw material
Into during wood-plastic products, the antioxygenic property of wood-plastic products can decline；Wherein, the wood-plastic products that prepared by extrusion molding, oxygen
It is only the 20%-25% with the wood plastic composite raw material oxidation induction time of formula to change induction time；Wood moulding prepared by injection moulding
Product, oxidation induction time are only the 20%-30% with the wood plastic composite raw material oxidation induction time of formula；Hot pressing legal system
Standby wood-plastic products, oxidation induction time are only the 15%-20% with the wood plastic composite raw material oxidation induction time of formula；
Accordingly, it is capable to the oxidation induction time of wood-plastic products, wood-plastic products are derived by the oxidation induction time of wood plastic composite raw material
Oxidation induction time it is longer, illustrate that its antioxygenic property is stronger.
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