CN110261435A - Method for measuring combustion heat value of thermosetting composite polystyrene board - Google Patents
Method for measuring combustion heat value of thermosetting composite polystyrene board Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 229920001187 thermosetting polymer Polymers 0.000 title claims abstract description 35
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 32
- 239000004793 Polystyrene Substances 0.000 title abstract description 10
- 229920002223 polystyrene Polymers 0.000 title abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 136
- 239000001301 oxygen Substances 0.000 claims abstract description 136
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 136
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 115
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000012360 testing method Methods 0.000 claims abstract description 42
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 25
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 25
- 239000012153 distilled water Substances 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 11
- 229920000265 Polyparaphenylene Polymers 0.000 claims description 32
- -1 polyphenylene Polymers 0.000 claims description 32
- 239000008188 pellet Substances 0.000 claims description 27
- 238000002360 preparation method Methods 0.000 claims description 11
- 230000001706 oxygenating effect Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 238000007707 calorimetry Methods 0.000 claims description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 229960004365 benzoic acid Drugs 0.000 description 25
- 238000005303 weighing Methods 0.000 description 8
- 238000005070 sampling Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000004035 construction material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004825 constant-volume calorimetry Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a method for measuring the combustion heat value of a thermosetting composite polystyrene board, which comprises the following steps: removing a part of 5-10 mm of the surface of the sample, and randomly intercepting at least 5 sample blocks from the middle of the sample as a test sample, wherein the minimum mass of the sample blocks is 50 g; taking 0.5g of sample small squares for each sample block by using a saw blade, grinding each sample block respectively, and collecting all ground powder and particles as five test samples for use; the test was carried out by the crucible method; 10mL of distilled water is not added into the oxygen bomb; the heat capacity E (MJ/K) of the calorimeter, the oxygen bomb and the accessories thereof is calibrated by measuring the total heat value of 5 groups of standard benzoic acid samples with the mass of 0.4 g-1.0 g; the heat value of the thermosetting composite polystyrene board is measured.
Description
Technical field
The invention belongs to environment-friendly insulating material development technical fields, specifically, being related to a kind of thermosetting composite polyphenylene plate combustion
Heat the measuring method of value.
Background technique
The combustion heat value of construction material is the important parameter for characterizing its potential fire risk, is to calculate its combustion heat release
Amount and the essential basic data of fire load.Combustion heat value is the natural quality of material, and the outer dimension of material and is made
It is unrelated with state etc., can be used for evaluating the potential fire load of construction material, be evaluate classification system for fire performance test method it
One.In industry and practical application, combustion heat value is determined generally by test, and the test method generallyd use at present is oxygen bomb
Calorimetry.
Method of oxygen steel bomb is measured using oxygen bomb calorimeter, and oxygen bomb calorimeter is for measuring solid, liquid fuel heat
The metrical instrument of value.Basic principle is: a certain amount of combustion heat standard substance benzoic acid burns in the oxygen bomb of calorimeter, releases
Heat make entire calorimetric system (including the water or other media, oxygen bomb, blender, thermometer etc. in inner cylinder, inner cylinder) by first
State temperature TAIt is raised to final states temperature TB, then by a certain amount of measured matter, condition same as described above carries out burning measurement again.Due to
The calorimeter used is identical, and calorimetric system temperature changes another cause, thus the calorific value of available measured matter.
Existing method is the distilled water that 10mL is poured into oxygen bomb, for the acidity generated during absorption test
Gas.But due to thermosetting composite polyphenylene plate granular polystyrene light weight and volume is big, fryer phenomenon occurs when burning in oxygen bomb,
It splashes inside distilled water, causes imperfect combustion.The sample preparation of original method sample is to take the representational sample of 50g, by sample by
Secondary grinding obtains powdered sample.There cannot be thermal decomposition when grinding again.Sample will using staggeredly grind by the way of into
Row grinding.If sample cannot be ground, other modes can be used by sample, little particle or sheet material is made.Because of thermosetting composite polyphenylene
Plate is combined by inorganic slurry and organic granular polystyrene, and inorganic slurry powder is separated with granular polystyrene when grinding,
When 0.5g sample is taken as test specimen, for the calorific value of the big survey of the accounting of inorganic slurry with regard to small, inorganic slurry accounting is small, measures
Calorific value it is just big, sampling do not have representativeness.
In short, the lesser modified polyphenyl plate of some density ratios, granular polystyrene, light material etc. are during the test often
There is " fryer " phenomenon, sample flashes in oxygen bomb, causes imperfect combustion, make test data parallel error, and it is very poor larger, it to weigh
The multiple requirement that repeatedly can just meet validity.The repeatability and reliability of data are poor.
Summary of the invention
In view of this, this method can the present invention provides a kind of measuring method of thermosetting composite polyphenylene plate combustion heat value
It allows thermosetting composite polyphenylene plate completely burned in oxygen bomb, and improves the repeatability and reliability of test result.
In order to solve the above-mentioned technical problem, the invention discloses a kind of measurement sides of thermosetting composite polyphenylene plate combustion heat value
Method, comprising the following steps:
Step 1, calorimeter, oxygen bomb and its attachment thermal capacity E (MJ/K) be 0.4g~1.0g by 5 groups of quality standard
Benzoic acid sample carries out gross calorific value measurement to be demarcated；
Step 2, sample preparation: removing the part 5~10mm of sample surfaces, from any interception at least five sample block conduct in sample centre
Sample, sample block minimum mass are 50g；The sample small cube for respectively taking 0.5g to each sample block with saw blade, then respectively to each sample
Block is ground, and all powder, particle after collecting grinding are used as five test specimens；
Step 3, calibration: it is tested with crucible method；
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate.
Optionally, the demarcating steps in step 1 are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put
Enter crucible；Ignition wire is connected to two electrodes；The ignition wire weighed is touched into small pellet.
Optionally, the crucible 20~30mm of height, diameter 25mm (full-size for having cut top) in step 3, bottom
It is smooth.
Optionally, the calorific value of thermosetting composite polyphenylene plate is measured including checking each instrument in step 4
And continuous mode.
Optionally, each instrument is checked specifically: check two electrodes and ignition wire, it is ensured that it contacts good；
Tighten oxygen bomb sealing cover, connect oxygen bomb and oxygen valve, carefully open oxygen cylinder, to oxygen bomb oxygenating to pressure reach 3.0MPa~
3.5MPa；Oxygen bomb is put into calorimeter inner cylinder；A certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen
Bullet weighs it, and institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g；It checks and ensures that oxygen bomb does not have
Leakage, without bubble, is put into outer cylinder for calorimeter inner cylinder；Temperature measuring apparatus, turn on agitator and timer are installed.
Optionally, continuous mode specifically: adjust inner cylinder water temperature, keep itself and outer cylinder water temperature essentially identical；Every one minute
Inner cylinder water temperature should be recorded, inner cylinder water temperature is adjusted, until the continuous-reading deviation in 10min is no more than ± 0.01k；By temperature at this time
Degree is used as initial temperature (Ti)；Turn-on current circuit, lights sample；For adiabatic calorimetry instrument: quickly being risen in calorimeter inner cylinder
The water temperature of thermophase, outer cylinder should be consistent as far as possible with inner cylinder water temperature；Its maximum temperature difference is no more than ± 0.04k；Every
An inner cylinder water temperature should be recorded within one minute, until the continuous-reading deviation in 10min is no more than ± 0.01k；By temperature at this time
As maximum temperature (Tm)；Oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Compared with prior art, the present invention can be obtained including following technical effect:
1) invention provides for the sampling modes of the sample, keep test specimen more representative, by the sample for intercepting 0.5g
Product small cube is ground again, and all samples after collecting grinding avoid test result deviation caused by sampling, guarantee test sample
It is representative, homogeneity.
2) sample of the present invention can completely burned, phenomenon of " complaining and quarrel loudly " will not occur.10mL distilled water, sheet are not added in oxygen bomb
Benzoic acid is placed on crucible bottom, and sample is placed on above benzoic acid, and ignition wire protrudes into bottom can contact benzoic acid as far as possible, tightens oxygen bomb
Sealing cover reaches 3.2MPa to oxygen bomb oxygenating to pressure.Authenticity, the accuracy of guarantee test result.
3) present invention can be used it is special increase crucible, convenient for the installation of test specimen, make test specimen burning more
Sufficiently.
Certainly, it implements any of the products of the present invention it is not absolutely required to while reaching all the above technical effect.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the schematic diagram that crucible method of the present invention is tested；
Fig. 2 is the comparison diagram of sample imperfect combustion and completely burned of the present invention.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with embodiment, whereby to the present invention how application technology hand
Section solves technical problem and reaches the realization process of technical effect to fully understand and implement.
The invention discloses a kind of measuring methods of thermosetting composite polyphenylene plate combustion heat value, comprising the following steps:
Step 1 carries out equipment Alignment: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment to automatic calorimeter first
Gross calorific value measurement can be carried out by the standard benzoic acid sample that 5 groups of quality are 0.4g~1.0g to be demarcated.Demarcating steps are such as
Under: the small pellet of benzoic acid is weighed, 0.1mg is accurate to；Small pellet is put into crucible；Ignition wire is connected to two electrodes；It will
The ignition wire of weighing touches small pellet；
It is tested according to following test procedure, water equivalent is the average value of 5 calibration results；Very poor the following table 1 of meeting
Regulation.
Table 1
| Thermal capacity | < 1500 | 9000~11000 | 14000~15000 |
| It is very poor | 9 | 40 | 60 |
Step 2, sample preparation: sample is representative, removes the part 5~10mm of sample surfaces, from any interception in sample centre
For at least five sample block as sample, sample block minimum mass is 50g；The sample small cube of 0.5g is respectively taken to each sample block with saw blade, so
Each sample block is ground respectively afterwards, all powder, particle after collecting grinding are used as five test specimens；
The sample of combustion heat value test wants representative and uniformity, is otherwise affected to test result, especially
It is bigger for some sample effects that cannot produce powder by grinding.This is mainly due to most of construction materials to produce
With it is relatively rough in manufacturing process, caused by product itself property is uneven.Especially when building material is by several compositions
When composition, phenomenon is especially prominent.
The present invention devises two kinds of sampling methods to verify influence of the preparation method to combustion heat value test result.To same
Factory formula, the sample of production technology are criticized, sampling mode is divided to two kinds, the first, surface (5~10) part mm is removed first, is appointed
Meaning at least five sample blocks of interception are 50g as sample, each sample block minimum mass, and sample is gradually ground and obtains powdered examination
Sample.Second, from any interception at least five sample block in sample centre as sample, sample block minimum mass is 50g；With saw blade to every
A sample block respectively takes the sample small cube of 0.5g, then grinds respectively to each sample block, collect grinding after all powder,
Grain is used as five test specimens.Measured result is as shown in table 2.
Influence of the sampling mode of 2 sample of table to sample A test result
The data of contrast table 2 it is found that sample preparation method to the calorimeter test of thermosetting composite polyphenylene plate the result is that there is shadow
Loud.Second of sampling mode keeps sample almost the same with raw material in composition, more representative and uniformity.
Step 3 is tested according to crucible method as defined in GB14402-2007 standard.By the sample weighed and sheet benzene
Formic acid is put into crucible, but sheet benzoic acid should be placed on crucible bottom, and sample is placed on above benzoic acid；The ignition wire that will have been weighed
It is connected on two electrodes；The position of ignition wire is adjusted, ignition wire protrudes into sample bottom, is allowed to as far as possible and the sheet benzene in crucible
The good contact of formic acid.Crucible height can be used it is special increase 20~30mm of crucible, diameter 25mm (has cut the maximum on top
Size), bottom is smooth；10mL distilled water (as shown in Figure 1) is not added in oxygen bomb.
Wherein, the crucible height in GB14402-2007 standard is 14mm~19mm, and diameter 25mm (has cut top most
Large scale), crucible space is smaller, when the small thermosetting composite polyphenylene plate of density takes the sample of 0.5g crucibles not under, and
And it is easy to happen " fryer " phenomenon, cause imperfect combustion；The present invention extends sample combustion by the height of increase crucible to reach
The time is burnt, fryer phenomenon is prevented, to reach completely burned.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, oxygen bomb sealing cover is tightened, oxygen bomb and oxygen valve is connected, carefully opens oxygen cylinder, gives oxygen bomb oxygenating
Reach 3.0MPa~3.5MPa to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble)
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
The calculating of thermosetting composite polyphenylene plate combustion heat value:
When calculating the gross calorific value of sample burning, it should carry out, be calculated by following equation, with MJ/ under conditions of constant volume
Kg is indicated.For auto testing instrument, the gross calorific value that burns can be directly obtained, and as test result.
In formula:
PCS --- gross calorific value, unit are mega joules per kilogram (MJ/kg)；
The water equivalent of water is filled in E --- calorimeter, oxygen bomb and its attachment and oxygen bomb, unit is megajoule every Kelvin
(MJ/K)；
Ti --- initial temperature, unit are Kelvin (K)；
Tm --- maximum temperature, unit are Kelvin (K)；
B --- the correction value of the combustion heat value of oxidizer used in test, unit is megajoule (MJ), such as ignition wire, benzene
Formic acid or other oxidizers；
C --- with the external temperature corrected value for carrying out heat exchange, unit is Kelvin (K).Repairing for Insulating sheath is used
Positive value is 0；
The quality of m --- sample, unit are kilogram (kg).
For thermosetting composite polyphenylene plate, whether completely burned is to influence heating-value determination precision and accuracy to sample
One key factor.Thermosetting composite polyphenylene plate lower for some density, granular polystyrene are more, it is difficult to grind into powder, matter
Amount is again relatively lighter.It being provided in national standard, combustion heat value test sample used is about 0.5g, when using crucible test method, crucible
It often can not load, need to be compacted.Because thermosetting composite polyphenylene plate is to be used with polystyrene foam particles or plate for heat preservation matrix
The compounded homogeneous plate-shaped products of inorganic agent take sample to put less and do not have representativeness, and the result measured is very poor big, is unsatisfactory for
The requirement of experimental result validity.According to the distilled water for putting 10mL in standard requirements oxygen bomb, the purpose is to during absorption test
The sour gas that sample combustion generates, prevents oxygen bomb to be corroded.But discovery sample has " fryer " phenomenon after testing, sample when burning
It is easy to splash, falls on oxygen bomb wall with bottom, cause imperfect combustion, test result numerical value is less than normal, even occurs negative value sometimes
(benzoic acid falls into imperfect combustion inside water cause) (as shown in Figure 2 a).The present invention devises two methods and carrys out judgement sample survey
The accuracy of test result.One is 10mL water is added in oxygen bomb, one is 10mL water is not added in oxygen bomb.First respectively to two methods
The calibrating of thermal capacity repeatability is carried out, material combustion then is carried out to two methods of appeal respectively with thermosetting composite polyphenylene plate sample
Calorific value detection.The calibrating of thermal capacity repeatability is shown in Table 3, and measurement result is shown in Table 4.
The calibrating of 3 thermal capacity repeatability of table
Add influence of the water to sample B test result in 4 oxygen bomb of table
By adding 10mL distilled water in oxygen bomb known to 4 data of table, oxygen bomb is opened after the test, oxygen bomb inner wall and bottom are also
There is unburned granular polystyrene, test result deviation is big, does not meet the requirement of result validity.10mL distilled water is not added in oxygen bomb,
Oxygen bomb is opened after the test, without unburned granular polystyrene, sample energy completely burned in oxygen bomb.
By the way that 10mL distillation water sample energy completely burned (as shown in Figure 2 b) is not added known to test in oxygen bomb.
Embodiment 1
Step 1, sample preparation: removing the part 5~10mm of sample surfaces, from any interception at least five sample block conduct in sample centre
Sample, sample block minimum mass are 50g；The sample small cube for respectively taking 0.5g to each sample block with saw blade, then respectively to each sample
Block is ground, and all powder, particle after collecting grinding are used as five test specimens；
Step 2 is tested (as shown in Figure 1) with crucible method；Crucible height 30mm, diameter 25mm (have cut top
Full-size), bottom is smooth.
Step 3, calibration: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment can by 5 groups of quality be 0.4g~
The standard benzoic acid sample of 1.0g carries out gross calorific value and measures to be demarcated；
Demarcating steps are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected
It is connected to two electrodes；The ignition wire weighed is touched into small pellet；10mL distilled water is not added in oxygen bomb.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, oxygen bomb sealing cover is tightened, oxygen bomb and oxygen valve is connected, carefully opens oxygen cylinder, gives oxygen bomb oxygenating
Reach 3.2MPa to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble).
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Embodiment 2
Step 1, sample preparation: removing the part 5~10mm of sample surfaces, from any interception at least five sample block conduct in sample centre
Sample, sample block minimum mass are 50g；The sample small cube for respectively taking 0.5g to each sample block with saw blade, then respectively to each sample
Block is ground, and all powder, particle after collecting grinding are used as five test specimens；
Step 2 is tested with crucible method；Crucible height 20mm, diameter 25mm (full-size for having cut top), bottom
Portion is smooth.
Step 3, calibration: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment can by 5 groups of quality be 0.4g~
The standard benzoic acid sample of 1.0g carries out gross calorific value and measures to be demarcated；
Demarcating steps are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected
It is connected to two electrodes；The ignition wire weighed is touched into small pellet；10mL distilled water is not added in oxygen bomb.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, oxygen bomb sealing cover is tightened, oxygen bomb and oxygen valve is connected, carefully opens oxygen cylinder, gives oxygen bomb oxygenating
Reach 3.0MPa to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble)
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Embodiment 3
Step 1, sample preparation: removing the part 5~10mm of sample surfaces, from any interception at least five sample block conduct in sample centre
Sample, sample block minimum mass are 50g；The sample small cube for respectively taking 0.5g to each sample block with saw blade, then respectively to each sample
Block is ground, and all powder, particle after collecting grinding are used as five test specimens；
Step 2 is tested with crucible method；Crucible height 25mm, diameter 25mm (full-size for having cut top), bottom
Portion is smooth.
Step 3, calibration: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment can by 5 groups of quality be 0.4g~
The standard benzoic acid sample of 1.0g carries out gross calorific value and measures to be demarcated；
Demarcating steps are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected
It is connected to two electrodes；The ignition wire weighed is touched into small pellet；10mL distilled water is not added in oxygen bomb.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, oxygen bomb sealing cover is tightened, oxygen bomb and oxygen valve is connected, carefully opens oxygen cylinder, gives oxygen bomb oxygenating
Reach 3.5MPa to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble)
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Comparative example 1
Step 1, sample preparation: removal surface (5~10) part mm, any at least five sample blocks that intercept are as sample, each sample
Block minimum mass is 50g, and sample is gradually ground and obtains powdered sample；
Step 2 is tested with crucible method；Crucible height 19mm, diameter 25mm, bottom are smooth.
Step 3, calibration: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment can by 5 groups of quality be 0.4g~
The standard benzoic acid sample of 1.0g carries out gross calorific value and measures to be demarcated；
Demarcating steps are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected
It is connected to two electrodes；The ignition wire weighed is touched into small pellet；10mL distilled water is not added in oxygen bomb.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, oxygen bomb sealing cover is tightened, oxygen bomb and oxygen valve is connected, carefully opens oxygen cylinder, gives oxygen bomb oxygenating
Reach 3.2MPa to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble)
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Comparative example 2
Step 1, sample preparation: removing the part 5~10mm of sample surfaces, from any interception at least five sample block conduct in sample centre
Sample, sample block minimum mass are 50g；The sample small cube for respectively taking 0.5g to each sample block with saw blade, then respectively to each sample
Block is ground, and all powder, particle after collecting grinding are used as five test specimens；
Step 2 is tested with crucible method；Crucible height 19mm, diameter 25mm, bottom are smooth.
Step 3, calibration: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment can by 5 groups of quality be 0.4g~
The standard benzoic acid sample of 1.0g carries out gross calorific value and measures to be demarcated；
Demarcating steps are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected
It is connected to two electrodes；The ignition wire weighed is touched into small pellet；Add 10mL distilled water in oxygen bomb.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, add 10mL water in oxygen bomb, tighten oxygen bomb sealing cover, connect oxygen bomb and oxygen valve, carefully open oxygen
Gas cylinder reaches 3.2MPa to oxygen bomb oxygenating to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble)
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Comparative example 3
Step 1, sample preparation: removing the part 5~10mm of sample surfaces, from any interception at least five sample block conduct in sample centre
Sample, sample block minimum mass are 50g；The sample small cube for respectively taking 0.5g to each sample block with saw blade, then respectively to each sample
Block is ground, and all powder, particle after collecting grinding are used as five test specimens；
Step 2 is tested with crucible method；Crucible height 19mm, diameter 25mm, bottom are smooth.
Step 3, calibration: the thermal capacity E (MJ/K) of calorimeter, oxygen bomb and its attachment can by 5 groups of quality be 0.4g~
The standard benzoic acid sample of 1.0g carries out gross calorific value and measures to be demarcated；
Demarcating steps are as follows: weighing the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected
It is connected to two electrodes；The ignition wire weighed is touched into small pellet；10mL distilled water is not added in oxygen bomb.
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate:
Step 4.1 checks each instrument:
Step 4.1.1, two electrodes and ignition wire are checked, it is ensured that it contacts good；
Step 4.1.2, add 10mL water in oxygen bomb, tighten oxygen bomb sealing cover, connect oxygen bomb and oxygen valve, carefully open oxygen
Gas cylinder reaches 3.2MPa to oxygen bomb oxygenating to pressure.
Step 4.1.3, oxygen bomb is put into calorimeter inner cylinder.
Step 4.1.4, a certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is carried out
It weighs, institute's water consumption should be identical with institute's water consumption in calibration process, is accurate to 1g.
Step 4.1.5, it checks and ensures that oxygen bomb does not leak (without bubble)
Step 4.1.6, calorimeter inner cylinder is put into outer cylinder.
Step 4.2, continuous mode:
Step 4.2.1, temperature measuring apparatus, turn on agitator and timer are installed.
Step 4.2.2, inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical.Inner cylinder water should be recorded every one minute
Temperature adjusts inner cylinder water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as starting temperature
Spend (Ti)；
Step 4.2.3, sample is lighted in turn-on current circuit.
Step 4.2.4, for adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k.An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k.Using temperature at this time as maximum temperature (Tm)；
Step 4.2.5, oxygen bomb is taken out from calorimeter, oxygen bomb is opened in slow pressure release.
Above description has shown and described several preferred embodiments of invention, but as previously described, it should be understood that invention is not
It is confined to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification
And environment, and can be carried out within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge
Change.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of invention, then it all should be in the appended power of invention
In the protection scope that benefit requires.
Claims (6)
1. a kind of measuring method of thermosetting composite polyphenylene plate combustion heat value, which comprises the following steps:
Step 1, calorimeter, oxygen bomb and its attachment thermal capacity E (MJ/K) be 0.4g~1.0g by 5 groups of quality standard benzene first
Sour sample carries out gross calorific value measurement to be demarcated；
Step 2, sample preparation: removing the part 5~10mm of sample surfaces, among the sample any interception at least five sample block as sample,
Sample block minimum mass is 50g；The sample small cube of 0.5g is respectively taken to each sample block with saw blade, then each sample block is carried out respectively
Grinding, all powder, particle after collecting grinding are used as five test specimens；
Step 3, calibration: it is tested with crucible method；
Step 4 is measured the calorific value of thermosetting composite polyphenylene plate.
2. the measuring method of thermosetting composite polyphenylene plate combustion heat value according to claim 1, which is characterized in that in step 1
Demarcating steps it is as follows: weigh the small pellet of benzoic acid, be accurate to 0.1mg；Small pellet is put into crucible；Ignition wire is connected to two
A electrode；The ignition wire weighed is touched into small pellet.
3. the measuring method of thermosetting composite polyphenylene plate combustion heat value according to claim 1, which is characterized in that in step 3
Crucible 20~30mm of height, diameter 25mm, cut the full-size on top, bottom is smooth.
4. the measuring method of thermosetting composite polyphenylene plate combustion heat value according to claim 1, which is characterized in that in step 4
To the calorific value of thermosetting composite polyphenylene plate be measured including to each instrument carry out check and continuous mode.
5. the measuring method of thermosetting composite polyphenylene plate combustion heat value according to claim 4, which is characterized in that each instrument
Device is checked specifically: checks two electrodes and ignition wire, it is ensured that it contacts good；Oxygen bomb sealing cover is tightened, oxygen bomb is connected
And oxygen valve, oxygen cylinder is carefully opened, reaches 3.0MPa~3.5MPa to oxygen bomb oxygenating to pressure；Oxygen bomb is put into calorimeter
Inner cylinder；A certain amount of distilled water is injected in calorimeter inner cylinder, can flood oxygen bomb, it is weighed, institute's water consumption
Should be identical with institute's water consumption in calibration process, it is accurate to 1g；It checks and ensures that oxygen bomb does not leak, it, will be in calorimeter without bubble
Cylinder is put into outer cylinder；Temperature measuring apparatus, turn on agitator and timer are installed.
6. the measuring method of thermosetting composite polyphenylene plate combustion heat value according to claim 4, which is characterized in that continuous mode
Specifically: inner cylinder water temperature is adjusted, keeps itself and outer cylinder water temperature essentially identical；Inner cylinder water temperature should be recorded every one minute, adjust inner cylinder
Water temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k；Using temperature at this time as initial temperature (Ti)；It connects
Current loop lights sample；For adiabatic calorimetry instrument: be rapidly heated the stage in calorimeter inner cylinder, the water temperature of outer cylinder should with it is interior
Cylinder water temperature is consistent as far as possible；Its maximum temperature difference is no more than ± 0.04k；An inner cylinder water should be recorded every one minute
Temperature, until the continuous-reading deviation in 10min is no more than ± 0.01k；Using temperature at this time as maximum temperature (Tm)；From calorimetric
Oxygen bomb is taken out in instrument, oxygen bomb is opened in slow pressure release.
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