CN109725020A - A kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound - Google Patents
A kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound Download PDFInfo
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- CN109725020A CN109725020A CN201811389205.8A CN201811389205A CN109725020A CN 109725020 A CN109725020 A CN 109725020A CN 201811389205 A CN201811389205 A CN 201811389205A CN 109725020 A CN109725020 A CN 109725020A
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Abstract
The invention belongs to polypropylene thermal analysis fields, and in particular to a kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound.Including polyolefin resin to be placed in the crucible of differential scanning calorimeter, under the protection of nitrogen, it is warming up to 200 DEG C and stops 5 minutes; to eliminate remaining thermal history; then 40 DEG C are down to the rate of temperature fall of 10 DEG C/min, then are heated up eight times with the heating rate of 10 DEG C/min, 4 DEG C of each lapse of temperature；Rise to 167-139 DEG C of stop 15min；40 DEG C all are down to the rate of temperature fall of 10 DEG C/min after heating every time, and stops 2min；Finally 200 DEG C are warming up to 10 DEG C/min；Changes of heat flux is recorded, heat classification melting curve is obtained.This method is not necessarily to a large amount of solvents, at low cost and do not pollute the environment, can preferable analyzing influence lithium battery diaphragm PP Pipe Compound peak melting, greatly improve the accuracy to raw material selection, and simple to operate.
Description
Technical field
The invention belongs to polypropylene thermal analysis fields, and in particular to a kind of electric to polypropylene lithium using differential calorimetric scan instrument
The heat analysis method of the fractional crystallization of pond diaphragm PP Pipe Compound.
Background technique
Main lithium battery diaphragm PP Pipe Compound is polyolefin in the market, based on polypropylene and polyethylene.Wherein, polypropylene
As semi-crystalline polymer, there is excellent mechanical property and chemical-resistance, become the head for preparing lithium battery PP Pipe Compound
Material selection.And acrylic resin film forming stability includes molecular weight and its distribution and its crystallization and orientation, these are all by shadow
The performances such as pore-forming and the rebound degree for the microporous barrier prepared are rung, therefore can polypropylene have sternly as lithium battery diaphragm PP Pipe Compound
The requirement of lattice, it is particularly significant to the stability of acrylic resin.
To the analysis method of the film forming stability of acrylic resin, there are mainly three types of methods at present, first is that xylene soluble part
Test, the method is toxic and is unable to the stability of accurate evaluation polypropylene film forming；Second is that stepwise isothermal crystallization method (SIC), this side
Method takes a long time, and is unable to whether accurate evaluation resin material can be used for the production of lithium battery diaphragm；Third is that being carried out with pilot-plant
Test, simulation production line carries out membrane test, then carries out analysis test to film forming, usually requires repeatedly to test, and waste is a large amount of
Man power and material.
Summary of the invention
Present invention aim to address a kind of heat analysis method of the fractional crystallization of acrylic resin, this method has operation
Simply, quickly, can quickly evaluate the film forming stability of acrylic resin.
Technical scheme is as follows:
A kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound, comprising the following steps:
(1) polyolefin resin is placed in the crucible of differential scanning calorimeter, under the protection of nitrogen, is warming up to 200 DEG C
It stops 5 minutes, to eliminate remaining thermal history, is then down to 40 DEG C with the rate of temperature fall of 10 DEG C/min, stops 2min；
(2) it is heated up eight times with the heating rate of 10 DEG C/min again, 4 DEG C of each lapse of temperature；Rise to 167-139 DEG C of stop
15min；
(3) 40 DEG C all are down to the rate of temperature fall of 10 DEG C/min after heating every time, and stop 2min；
(4) 200 DEG C finally are warming up to 10 DEG C/min；
(5) changes of heat flux is recorded, heat classification melting curve is obtained.
Further, the temperature range of eight heatings is 167-139 DEG C.
Further, it is warming up to after target temperature every time and is all cooled to 40 DEG C.
Beneficial effects of the present invention
The present invention is not necessarily to a large amount of solvents, at low cost and do not pollute the environment, can preferable analyzing influence lithium battery diaphragm
The peak melting of PP Pipe Compound greatly improves the accuracy to raw material selection, and simple to operate.
Detailed description of the invention
Fig. 1 is the melting curve of the hot fractional crystallization of two kinds of polypropylene specimens.
In figure, PP1- import polypropylene lithium battery diaphragm PP Pipe Compound,
The country PP2- polypropylene lithium battery diaphragm PP Pipe Compound PP2,
PP3- polypropylene lithium battery diaphragm PP Pipe Compound.
Specific embodiment
The present invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1
The present embodiment uses a kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound, and it is poly- for import to test raw material
Propylene lithium battery diaphragm PP Pipe Compound PP1,
1. weighing polypropylene 5mg, it is placed in the crucible of differential scanning calorimeter, under the protection of nitrogen, at 200 DEG C of temperature
Then lower stop 5min is down to 40 DEG C to eliminate remaining thermal history with the rate of temperature fall of 10 DEG C/min, stop 2min；
2. rising to 167 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
3. rising to 163 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
4. rising to 159 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
5. rising to 155 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
6. rising to 151 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
7. rising to 147 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
8. rising to 143 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
9. rising to 139 DEG C with the heating rate of 10 DEG C/min, 15min is stopped, then be down to the rate of temperature fall of 10 DEG C/min
40 DEG C, stop 2min；
10. finally rising to 200 DEG C with the heating rate of 10 DEG C/min.
Embodiment 2
The present embodiment uses a kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound, step and 1 phase of embodiment
Together, test raw material is domestic polypropylene lithium battery diaphragm PP Pipe Compound PP2.
Embodiment 3
The present embodiment uses a kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound, step and 1 phase of embodiment
Together, test raw material is general polypropylene lithium battery diaphragm PP Pipe Compound PP3.
The fractional crystallization test result of two kinds of polypropylene lithium battery diaphragm PP Pipe Compounds in table 1
| Test raw material | Peak temperature | Swarming number | Wafer thickness breadth coefficient |
| PP1 | 174.64,180.93 | 2 | 1.199 |
| PP2 | 174.25,180.49 | 2 | 1.198 |
| PP3 | 173.22,179.74 | 2 | 1.184 |
Seen from table 1, two kinds of acrylic resins are on heat classification melting curve, due to the raising of isotacticity constituent content,
Wafer thickness improves, and is less susceptible to stretching film forming, stability decline in process, it is easier to be film breakage, this result and drawing
The test result of film machine is consistent.
Claims (3)
1. a kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound, which comprises the following steps:
(1) polyolefin resin is placed in the crucible of differential scanning calorimeter, under the protection of nitrogen, is warming up to 200 DEG C and stops 5
Minute, 40 DEG C then are down to the rate of temperature fall of 10 DEG C/min, stops 2min；
(2) it is heated up eight times with the heating rate of 10 DEG C/min again, 4 DEG C of each lapse of temperature；Rise to 167-139 DEG C of stop 15min；
(3) 40 DEG C all are down to the rate of temperature fall of 10 DEG C/min after heating every time, and stop 2min；
(4) 200 DEG C finally are warming up to 10 DEG C/min.
2. the fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound according to claim 1, which is characterized in that described
Eight times heating temperature ranges be 167-139 DEG C.
3. the fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound according to claim 1, which is characterized in that described
Be warming up to after target temperature every time and be all cooled to 40 DEG C.
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| CN201811389205.8A CN109725020A (en) | 2018-11-21 | 2018-11-21 | A kind of fractional crystallization method of polypropylene lithium battery diaphragm PP Pipe Compound |
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Citations (6)
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| JPH05322811A (en) * | 1992-05-19 | 1993-12-07 | Shimadzu Corp | Method for sorting remolding of crystalline thermoplastic |
| KR20010084132A (en) * | 2000-02-24 | 2001-09-06 | 유현식 | Method for measuring tactic unit distribution in homo polypropylene using thermal fractionated crystallization and differential scanning calorimetry analysis |
| CN102156147A (en) * | 2011-03-07 | 2011-08-17 | 四川大学 | Method for detecting film forming stability of polypropylene in bidirectional stretching by using thermal analysis method |
| CN102183539A (en) * | 2011-03-07 | 2011-09-14 | 四川大学 | Method for quickly detecting crosslinked polyethylene cable insulating material structure |
| CN105479781A (en) * | 2015-12-14 | 2016-04-13 | 成都慧成科技有限责任公司 | Method for increasing content of beta crystals of polypropylene through thermal treatment |
| CN106596624A (en) * | 2016-12-21 | 2017-04-26 | 深圳市星源材质科技股份有限公司 | Fractional crystallization analysis method of polyolefin resin |
-
2018
- 2018-11-21 CN CN201811389205.8A patent/CN109725020A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05322811A (en) * | 1992-05-19 | 1993-12-07 | Shimadzu Corp | Method for sorting remolding of crystalline thermoplastic |
| KR20010084132A (en) * | 2000-02-24 | 2001-09-06 | 유현식 | Method for measuring tactic unit distribution in homo polypropylene using thermal fractionated crystallization and differential scanning calorimetry analysis |
| CN102156147A (en) * | 2011-03-07 | 2011-08-17 | 四川大学 | Method for detecting film forming stability of polypropylene in bidirectional stretching by using thermal analysis method |
| CN102183539A (en) * | 2011-03-07 | 2011-09-14 | 四川大学 | Method for quickly detecting crosslinked polyethylene cable insulating material structure |
| CN105479781A (en) * | 2015-12-14 | 2016-04-13 | 成都慧成科技有限责任公司 | Method for increasing content of beta crystals of polypropylene through thermal treatment |
| CN106596624A (en) * | 2016-12-21 | 2017-04-26 | 深圳市星源材质科技股份有限公司 | Fractional crystallization analysis method of polyolefin resin |
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