CN107748175A - A kind of device and method for determining mesophase pitch softening point - Google Patents
A kind of device and method for determining mesophase pitch softening point Download PDFInfo
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- CN107748175A CN107748175A CN201710880822.7A CN201710880822A CN107748175A CN 107748175 A CN107748175 A CN 107748175A CN 201710880822 A CN201710880822 A CN 201710880822A CN 107748175 A CN107748175 A CN 107748175A
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- 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
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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Abstract
The invention discloses a kind of device and method for determining mesophase pitch softening point, described device by salt bath container, heating mantle, temperature sensor, pressure-strain piece, sample cup for liquid, connect sample cup, shot, inert gas shielding pipe, console etc. and form.Salt bath container outer wall wraps up for heating mantle, salt bath container content has fused salt, open an aperture in sample cup for liquid bottom, sample cup for liquid and connect sample cup and be connected through a screw thread, immerse in salt bath container, sample cup for liquid places mesophase pitch sample, and it is passed through inert gas, prevent mesophase pitch to be oxidized, connect placement force foil gauge in sample cup, caused strain signal is transferred signals in external control stand by pressure-strain transmission line.The present invention has the advantages that simple in construction, easy to operate, test result is accurate, manual operation error is small.
Description
Technical field
The invention belongs to softening point test device and method and technology field, and in particular to one kind measure mesophase pitch softening
The device and method of point.
Background technology
Mesophase pitch has the characteristic of liquid crystal, and in heat, light, electrically and magnetically etc. each side has the thing of special similar crystal
Attribute is managed, and is still in fluid characteristics in mobility, viscosity and deformation etc., is the high-quality presoma for producing carbon product,
Obtained preferably preparing MCMB, high-performance pitch Carbon fibe, Mesophase Pitch-Derived Carbon Foam, nuclear graphite etc.
Ground application.
Softening point is one of important indicator for evaluating mesophase pitch performance, at present generally using ring and ball method measure softening
Point, national standard《GB/T4507-2014 asphalt softening point determination methods（Ring and ball method）》In due to water-bath, the limitation of oil bath, softening point is surveyed
Scope is tried at 30-157 DEG C.And the softening point of mesophase pitch is higher, generally greater than 200 DEG C, mesophase pitch is determined at present
Softening point uses needling method, and detection means includes heating furnace, sample cell（With air guide side pipe）, instrument board, molten salt bath.Sample cell
Be made up of glass, after salt bath heating fusing, sample cell be put into salt bath, progressively heated, at the same watch in pipe sample it is heated after
Dynamically.Nitrogen is passed through sample cell by air guide side pipe, avoids bitumen blowing, and takes away a small amount of decomposition gas.By fine steel needle, insert
Enter sample cell, piece is melt into when feel pitch is micro-, when being integrated with soft feel, as softening point.Needling method, which surveys softening point, needs people
To judge, lack the judge index of quantization, operating error is big, the series of samples being more or less the same particularly with softening point, it is difficult to have
Effect measurement.
The content of the invention
Present invention aim to address the problem of existing detection device result is inaccurate, human error is big, there is provided Yi Zhongjie
Structure is simple, can accurately measure the device and method of mesophase pitch softening point.
The technical solution adopted by the present invention is：
A kind of device for determining mesophase pitch softening point, it includes salt bath container 1, heating mantle 2, fused salt 4, sample cup for liquid 5, inertia
Gas-shielded pipe 7, it is characterised in that the outer wall of salt bath container 1 is wrapped up by heating mantle 2, and salt bath container 1 is built with fused salt 4, sample cup for liquid 5
An aperture is opened in bottom, sample cup for liquid 5 and connects sample cup 6 and is connected through a screw thread, and immerses simultaneously in salt bath container 1, has in sample cup for liquid 5 lazy
Property gas-shielded pipe 7, connecing the bottom of sample cup 6 has pressure-strain piece 8, there is temperature sensor 3 among fused salt 4, and rack for test tube 9 fixes sample
Cup 5, shot 10 are placed on sample mesophase pitch upper surface, pressure-strain piece 8 and temperature sensor 3 respectively with console
11 connections.
The fused salt held in described salt bath container be natrium nitrosum, sodium nitrate and potassium nitrate mixture, natrium nitrosum
Mass fraction is 30-50%, and sodium nitrate mass fraction is 3-20%, and potassium nitrate mass fraction is 40-60%.
The diameter D1 of described sample cup for liquid is 10mm-30mm, and height H1 is 1-2 times of diameter D1, and bottom is provided with a diameter of
4-8mm aperture.
The described diameter D2 for connecing sample cup is 10mm-30mm, and height H2 is 23-28mm, and connecing the pressure placed in sample cup should
Become distance of the upper surface of piece away from sample cup for liquid medial small hole lower edge as 16-22mm, the upper surface of pressure-strain piece is away from sample cup for liquid
The preferred distance of medial small hole lower edge is 19mm.
The diameter D3 of described shot is 4mm-8mm.
A kind of method that mesophase pitch softening point is determined using said apparatus, is comprised the following steps：
(1) preparation of samples, mesophase pitch sample is dried and crushed, grind first one piece it is straight with sample cup for liquid small hole at bottom part
The big cylindrical sample such as footpath, remaining mesophase pitch after crushing then is sieved with 1mm sieve, take the lower interphase drip of sieve
It is blue or green；
(2) sample is loaded, and cylindrical sample is first blocked to the small hole at bottom part of sample cup for liquid, and the lower mesophase pitch of sieve is loaded into sample
Cup, and flat, height of specimen 5-50mm is shaken in jolt ramming, sieves lower mesophase pitch upper face center and places shot, will be tried by screw thread
Sample cup is connected with connecing sample cup；
(3) be put into fused salt in salt bath container, highly no more than salt bath container height 2/3, with 6-20 DEG C/min heating speed
Rate heating melts fused salt；
(4) treat that fused salt is just molten into liquid, nitrogen be passed through in inert gas shielding pipe, by sample cup for liquid with connect sample cup be collectively disposed at it is molten
In salt bath, sample cup for liquid is fixed with rack for test tube；
(5) continue to heat fused salt liquid according to 1-3 DEG C/min heating rate；
(6) gradually dropped in the presence of shot after cylindrical sample softening in sample cup for liquid, the pressure touched in sample cup should
When becoming piece, strain signal is transferred to console by pressure-strain piece, and console records the signal of temperature sensor simultaneously, now right
The temperature answered is the softening point of sample；
(7) twice, the difference of test result is not more than 1.5 DEG C to same sample parallel testing twice, takes its average value as softening point
Test result.
The invention has the advantages that：
1）Mesophase pitch softening point structure of the detecting device is simple and convenient to operate, homogeneous heating, high sensitivity.
2）Have the advantages that test speed is fast, result is accurate, manual operation error is small.
Brief description of the drawings
Fig. 1 is a kind of apparatus structure schematic diagram for determining mesophase pitch softening point.
Brief description of the drawings 1 is salt bath container, 2 be heating mantle, 3 be temperature sensor, 4 be fused salt, 5 be sample cup for liquid, 6 be to connect
Sample cup, 7 be inert gas shielding pipe, 8 be pressure-strain piece, 9 be rack for test tube, 10 be shot, 11 be console.
Embodiment
As shown in figure 1, a kind of device for determining mesophase pitch softening point, it includes salt bath container 1, heating mantle 2, fused salt
4th, sample cup for liquid 5, inert gas shielding pipe 7, it is characterised in that the outer wall of salt bath container 1 is wrapped up by heating mantle 2, and salt bath container 1 is built-in
There is a fused salt 4, an aperture is opened in the bottom of sample cup for liquid 5, sample cup for liquid 5 and connects sample cup 6 and is connected through a screw thread, and immerses salt bath container 1 simultaneously
It is interior, there is inert gas shielding pipe 7 in sample cup for liquid 5, connecing the bottom of sample cup 6 has pressure-strain piece 8, has temperature sensor among fused salt 4
3, rack for test tube 9 fixes sample cup for liquid 5, and shot 10 is placed on sample mesophase pitch upper surface, and pressure-strain piece 8 and temperature pass
Sensor 3 is connected with console 11 respectively.
The fused salt held in described salt bath container be natrium nitrosum, sodium nitrate and potassium nitrate mixture, natrium nitrosum
Mass fraction is 30-50%, and sodium nitrate mass fraction is 3-20%, and potassium nitrate mass fraction is 40-60%.
The diameter D1 of described sample cup for liquid is 10mm-30mm, and height H1 is 1-2 times of diameter D1, and bottom is provided with a diameter of
4-8mm aperture.
The described diameter D2 for connecing sample cup is 10mm-30mm, and height H2 is 23-28mm, and connecing the pressure placed in sample cup should
Become distance of the upper surface of piece away from sample cup for liquid medial small hole lower edge as 16-22mm, the upper surface of pressure-strain piece is away from sample cup for liquid
The preferred distance of medial small hole lower edge is 19mm.
The diameter D3 of described shot is 4mm-8mm.
A kind of method that mesophase pitch softening point is determined using said apparatus, is comprised the following steps：
(1) preparation of samples, mesophase pitch sample is dried and crushed, grind first one piece it is straight with sample cup for liquid small hole at bottom part
The big cylindrical sample such as footpath, remaining mesophase pitch after crushing then is sieved with 1mm sieve, take the lower interphase drip of sieve
It is blue or green；
(2) sample is loaded, and cylindrical sample is first blocked to the small hole at bottom part of sample cup for liquid, and the lower mesophase pitch of sieve is loaded into sample
Cup, and flat, height of specimen 5-50mm is shaken in jolt ramming, sieves lower mesophase pitch upper face center and places shot, will be tried by screw thread
Sample cup is connected with connecing sample cup；
(3) be put into fused salt in salt bath container, highly no more than salt bath container height 2/3, with 6-20 DEG C/min heating speed
Rate heating melts fused salt；
(4) treat that fused salt is just molten into liquid, nitrogen be passed through in inert gas shielding pipe, by sample cup for liquid with connect sample cup be collectively disposed at it is molten
In salt bath, sample cup for liquid is fixed with rack for test tube；
(5) continue to heat fused salt liquid according to 1-3 DEG C/min heating rate；
(6) gradually dropped in the presence of shot after cylindrical sample softening in sample cup for liquid, the pressure touched in sample cup should
When becoming piece, strain signal is transferred to console by pressure-strain piece, and console records the signal of temperature sensor simultaneously, now right
The temperature answered is the softening point of sample；
(7) twice, the difference of test result is not more than 1.5 DEG C to same sample parallel testing twice, takes its average value as softening point
Test result.
Embodiment 1
Mesophase pitch sample A is dried and crushed, grinds one piece of a diameter of 4mm cylindrical sample, with 1mm sieve
Remaining sample after crushing is sieved, takes the lower mesophase pitch of sieve.By cylindrical sample block diameter D1 be 10mm, height H1 be
The small hole at bottom part of a diameter of 4mm of 10mm, small hole at bottom part sample cup for liquid 5, the lower mesophase pitch of sieve is loaded into sample cup for liquid 5, and jolt ramming
Flat, height of specimen 8mm is shaken, lower mesophase pitch upper face center is sieved and places the shot 10 that diameter D3 is 4mm, by sample cup for liquid 5
Be 10mm with diameter D2, the sample cup 6 that connects that height H1 is 23mm be connected, connect the 6 inner placement of sample cup pressure-strain piece 8 upper surface away from
The distance of the medial small hole lower edge of sample cup for liquid 5 is 16mm.Be put into fused salt 4 in salt bath container 1, fused salt 4 by 50wt% natrium nitrosums,
10wt% sodium nitrate and 40wt% potassium nitrate composition, fused salt 4 is melted with 6 DEG C/min heating rate heating, treats that fused salt 4 just melts
For liquid, nitrogen is passed through in inert gas shielding pipe 7, by sample cup for liquid 5 and sample cup 6 is connect and is placed in molten salt bath, and consolidated with rack for test tube 9
Determine sample cup for liquid 5, progressively heated according to 1 DEG C/min heating rate, the pressure in sample cup 6 is touched after cylindrical sample softening
During foil gauge 8, strain signal is transferred to console 11 by pressure-strain piece 8, the temperature sensor 3 that now console 11 is shown
Temperature is 223.5 DEG C, does parallel testing according to above-mentioned steps, the temperature for the temperature sensor 3 that console 11 is shown is 224.1
DEG C, the difference of two times result is not more than 1.5 DEG C for 0.6 DEG C, and 223.8 DEG C of its average value is sample A softening point.
Embodiment 2
Mesophase pitch sample B is dried and crushed, grinds one piece of a diameter of 6mm cylindrical sample, with 1mm sieve
Remaining sample after crushing is sieved, takes the lower mesophase pitch of sieve.By cylindrical sample block diameter D1 be 20mm, height H1 be
The small hole at bottom part of a diameter of 6mm of 30mm, small hole at bottom part sample cup for liquid 5, the lower mesophase pitch of sieve is loaded into sample cup for liquid 5, and jolt ramming
Flat, height of specimen 15mm is shaken, lower mesophase pitch upper face center is sieved and places the shot 10 that diameter D3 is 6mm, by sample cup for liquid 5
Be 20mm with diameter D2, the sample cup 6 that connects that height H1 is 25mm be connected, connect the 6 inner placement of sample cup pressure-strain piece 8 upper surface away from
The distance of the medial small hole lower edge of sample cup for liquid 5 is 19mm.Fused salt 4 is put into salt bath container 1, fused salt 4 is by 45% natrium nitrosum, 15%
Sodium nitrate and 40% potassium nitrate composition, fused salt 4 is melted with 6 DEG C/min heating rate heating, treats that fused salt 4 is just molten into liquid,
Nitrogen is passed through in inert gas shielding pipe 7, sample cup for liquid 5 is placed in molten salt bath with connecing sample cup 6, and sample is fixed with rack for test tube 9
Cup 5, is progressively heated according to 2 DEG C/min heating rate, and the pressure-strain piece in sample cup 6 is touched after cylindrical sample softening
When 8, strain signal is transferred to console 11 by pressure-strain piece 8, and now the temperature for the temperature sensor 3 that console 11 is shown is
240.5 DEG C, parallel testing is done according to above-mentioned steps, the temperature for the temperature sensor 3 that console 11 is shown is 240.1 DEG C, twice
As a result difference is 0.4 DEG C and is not more than 1.5 DEG C, and 240.3 DEG C of its average value is sample B softening point.
Embodiment 3
Mesophase pitch sample C is dried and crushed, grinds one piece of a diameter of 8mm cylindrical sample, with 1mm sieve
Remaining sample after crushing is sieved, takes the lower mesophase pitch of sieve.By cylindrical sample block diameter D1 be 30mm, height H1 be
The small hole at bottom part of a diameter of 8mm of 60mm, small hole at bottom part sample cup for liquid 5, the lower mesophase pitch of sieve is loaded into sample cup for liquid 5, and jolt ramming
Flat, height of specimen 45mm is shaken, lower mesophase pitch upper face center is sieved and places the shot 10 that diameter D3 is 8mm, by sample cup for liquid 5
Be 30mm with diameter D2, the sample cup 6 that connects that height H1 is 28mm be connected, connect the 6 inner placement of sample cup pressure-strain piece 8 upper surface away from
The distance of the medial small hole lower edge of sample cup for liquid 5 is 22mm.Fused salt 4 is put into salt bath container 1, fused salt 4 is by 40% natrium nitrosum, 20%
Sodium nitrate and 40% potassium nitrate composition, fused salt 4 is melted with 20 DEG C/min heating rate heating, treats that fused salt 4 is just molten into liquid
Body, nitrogen is passed through in inert gas shielding pipe 7, by sample cup for liquid 5 and connect sample cup 6 and be placed in molten salt bath, and fix examination with rack for test tube 9
Sample cup 5, progressively heated according to 3 DEG C/min heating rate, the pressure-strain in sample cup 6 is touched after cylindrical sample softening
During piece 8, strain signal is transferred to console 11 by pressure-strain piece 8, now the temperature for the temperature sensor 3 that console 11 is shown
For 251.5 DEG C, parallel testing is done according to above-mentioned steps, the temperature of the temperature sensor 3 that console 11 is shown is 251.9 DEG C, two
The difference of secondary result is 0.4 DEG C and is not more than 1.5 DEG C, and 251.7 DEG C of its average value is sample C softening point.
Embodiment 4
Mesophase pitch sample D is dried and crushed, grinds one piece of a diameter of 6mm cylindrical sample, with 1mm sieve
Remaining sample after crushing is sieved, takes the lower mesophase pitch of sieve.By cylindrical sample block diameter D1 be 20mm, height H1 be
The small hole at bottom part of a diameter of 6mm of 30mm, small hole at bottom part sample cup for liquid 5, the lower mesophase pitch of sieve is loaded into sample cup for liquid 5, and jolt ramming
Flat, height of specimen 20mm is shaken, lower mesophase pitch upper face center is sieved and places the shot 10 that diameter D3 is 6mm, by sample cup for liquid 5
Be 20mm with diameter D2, the sample cup 6 that connects that height H1 is 25mm be connected, connect the 6 inner placement of sample cup pressure-strain piece 8 upper surface away from
The distance of the medial small hole lower edge of sample cup for liquid 5 is 19mm.Fused salt 4 is put into salt bath container 1, fused salt 4 is by 35% natrium nitrosum, 15%
Sodium nitrate and 50% potassium nitrate composition, fused salt 4 is melted with 10 DEG C/min heating rate heating, treats that fused salt 4 is just molten into liquid
Body, nitrogen is passed through in inert gas shielding pipe 7, by sample cup for liquid 5 and connect sample cup 6 and be placed in molten salt bath, and fix examination with rack for test tube 9
Sample cup 5, progressively heated according to 2 DEG C/min heating rate, the pressure-strain in sample cup 6 is touched after cylindrical sample softening
During piece 8, strain signal is transferred to console 11 by pressure-strain piece 8, now the temperature for the temperature sensor 3 that console 11 is shown
For 259.7 DEG C, parallel testing is done according to above-mentioned steps, the temperature of the temperature sensor 3 that console 11 is shown is 260.5 DEG C, two
The difference of secondary result is 0.8 DEG C and is not more than 1.5 DEG C, and 260.1 DEG C of its average value is sample D softening point.
Embodiment 5
Mesophase pitch sample E is dried and crushed, grinds one piece of a diameter of 6mm cylindrical sample, with 1mm sieve
Remaining sample after crushing is sieved, takes the lower mesophase pitch of sieve.By cylindrical sample block diameter D1 be 20mm, height H1 be
The small hole at bottom part of a diameter of 6mm of 30mm, small hole at bottom part sample cup for liquid 5, the lower mesophase pitch of sieve is loaded into sample cup for liquid 5, and jolt ramming
Flat, height of specimen 18mm is shaken, lower mesophase pitch upper face center is sieved and places the shot 10 that diameter D3 is 6mm, by sample cup for liquid 5
Be 20mm with diameter D2, the sample cup 6 that connects that height H1 is 25mm be connected, connect the 6 inner placement of sample cup pressure-strain piece 8 upper surface away from
The distance of the medial small hole lower edge of sample cup for liquid 5 is 19mm.Fused salt 4 is put into salt bath container 1, fused salt 4 is by 35% natrium nitrosum, 10%
Sodium nitrate and 55% potassium nitrate composition, fused salt 4 is melted with 10 DEG C/min heating rate heating, treats that fused salt 4 is just molten into liquid
Body, nitrogen is passed through in inert gas shielding pipe 7, by sample cup for liquid 5 and connect sample cup 6 and be placed in molten salt bath, and fix examination with rack for test tube 9
Sample cup 5, progressively heated according to 2 DEG C/min heating rate, the pressure-strain in sample cup 6 is touched after cylindrical sample softening
During piece 8, strain signal is transferred to console 11 by pressure-strain piece 8, now the temperature for the temperature sensor 3 that console 11 is shown
For 270.3 DEG C, parallel testing is done according to above-mentioned steps, the temperature of the temperature sensor 3 that console 11 is shown is 269.7 DEG C, two
The difference of secondary result is 0.6 DEG C and is not more than 1.5 DEG C, and 270.0 DEG C of its average value is sample E softening point.
Embodiment 6
Mesophase pitch sample F is dried and crushed, grinds one piece of a diameter of 6mm cylindrical sample, with 1mm sieve
Remaining sample after crushing is sieved, takes the lower mesophase pitch of sieve.By cylindrical sample block diameter D1 be 20mm, height H1 be
The small hole at bottom part of a diameter of 6mm of 30mm, small hole at bottom part sample cup for liquid 5, the lower mesophase pitch of sieve is loaded into sample cup for liquid 5, and jolt ramming
Flat, height of specimen 15mm is shaken, lower mesophase pitch upper face center is sieved and places the shot 10 that diameter D3 is 6mm, by sample cup for liquid 5
Be 20mm with diameter D2, the sample cup 6 that connects that height H1 is 25mm be connected, connect the 6 inner placement of sample cup pressure-strain piece 8 upper surface away from
The distance of the medial small hole lower edge of sample cup for liquid 5 is 19mm.Fused salt 4 is put into salt bath container 1, fused salt 4 is by 30% natrium nitrosum, 10%
Sodium nitrate and 60% potassium nitrate composition, fused salt 4 is melted with 10 DEG C/min heating rate heating, treats that fused salt 4 is just molten into liquid
Body, nitrogen is passed through in inert gas shielding pipe 7, by sample cup for liquid 5 and connect sample cup 6 and be placed in molten salt bath, and fix examination with rack for test tube 9
Sample cup 5, progressively heated according to 2 DEG C/min heating rate, the pressure-strain in sample cup 6 is touched after cylindrical sample softening
During piece 8, strain signal is transferred to console 11 by pressure-strain piece 8, now the temperature for the temperature sensor 3 that console 11 is shown
For 295.3 DEG C, parallel testing is done according to above-mentioned steps, the temperature of the temperature sensor 3 that console 11 is shown is 294.9 DEG C, two
The difference of secondary result is 0.4 DEG C and is not more than 1.5 DEG C, and 295.1 DEG C of its average value is the softening point of sample F.
Claims (8)
1. a kind of device for determining mesophase pitch softening point, it includes salt bath container (1), heating mantle (2), fused salt (4), sample
Cup (5), inert gas shielding pipe (7), it is characterised in that salt bath container (1) outer wall is wrapped up by heating mantle (2), salt bath container (1)
Built with fused salt (4), an aperture is opened in sample cup for liquid (5) bottom, sample cup for liquid (5) and connects sample cup (6) and is connected through a screw thread, and soaks simultaneously
Enter in salt bath container (1), have inert gas shielding pipe (7) in sample cup for liquid (5), connecing sample cup (6) bottom has pressure-strain piece (8),
There are temperature sensor (3), the fixed sample cup for liquid (5) of rack for test tube (9) among fused salt (4), shot (10) is placed among sample
Asphalt phase upper surface, pressure-strain piece (8) and temperature sensor (3) are connected with console (11) respectively.
A kind of 2. device for determining mesophase pitch softening point as claimed in claim 1, it is characterised in that described sample cup for liquid
(5) diameter D1 is 10mm-30mm, and height H1 is 1-2 times of diameter D1, and bottom is provided with a diameter of 4-8mm aperture.
3. a kind of device for determining mesophase pitch softening point as claimed in claim 1, it is characterised in that described connects sample cup
(6) diameter D2 is 10mm-30mm, and height H2 is 23-28mm.
4. a kind of device for determining mesophase pitch softening point as claimed in claim 1, it is characterised in that described connects sample cup
(6) inner distance of the upper surface for the pressure-strain piece (8) placed away from sample cup for liquid (5) medial small hole lower edge is 16-22mm.
A kind of 5. device for determining mesophase pitch softening point as claimed in claim 4, it is characterised in that pressure-strain piece (8)
Distance of the upper surface away from sample cup for liquid (5) medial small hole lower edge be 19mm.
6. a kind of device for determining mesophase pitch softening point as claimed in claim 1, it is characterised in that described shot
Diameter D3 is 4mm-8mm.
7. a kind of device for determining mesophase pitch softening point as claimed in claim 1, it is characterised in that described fused salt is
The mixture of natrium nitrosum, sodium nitrate and potassium nitrate, natrium nitrosum mass fraction are 30-50%, and sodium nitrate mass fraction is 3-
20%, potassium nitrate mass fraction is 40-60%.
8. a kind of application of the device of measure mesophase pitch softening point as described in claim any one of 1-7, its feature exist
In comprising the following steps：
(1) preparation of samples, mesophase pitch sample is dried and crushed, grind first one piece it is straight with sample cup for liquid small hole at bottom part
The big cylindrical sample such as footpath, remaining mesophase pitch after crushing then is sieved with 1mm sieve, take the lower interphase drip of sieve
It is blue or green；
(2) sample is loaded, and cylindrical sample is first blocked to the small hole at bottom part of sample cup for liquid, and the lower mesophase pitch of sieve is loaded into sample
Cup, and flat, height of specimen 5-50mm is shaken in jolt ramming, sieves lower mesophase pitch upper face center and places shot, will be tried by screw thread
Sample cup is connected with connecing sample cup；
(3) be put into fused salt in salt bath container, highly no more than salt bath container height 2/3, with 6-20 DEG C/min heating speed
Rate heating melts fused salt；
(4) treat that fused salt is just molten into liquid, nitrogen be passed through in inert gas shielding pipe, by sample cup for liquid with connect sample cup be collectively disposed at it is molten
In salt bath, sample cup for liquid is fixed with rack for test tube；
(5) continue to heat fused salt liquid according to 1-3 DEG C/min heating rate；
(6) gradually dropped in the presence of shot after cylindrical sample softening in sample cup for liquid, the pressure touched in sample cup should
When becoming piece, strain signal is transferred to console by pressure-strain piece, and console records the signal of temperature sensor simultaneously, now right
The temperature answered is the softening point of sample；
(7) twice, the difference of test result is not more than 1.5 DEG C to same sample parallel testing twice, takes its average value as softening point
Test result.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738477A (en) * | 2019-02-26 | 2019-05-10 | 王志明 | High softening-point analyzer mother liquor and preparation method and application method |
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Application publication date: 20180302 |