CN103214638A - Preparation method of branching unit-containing polyether-ether-ketone terpolymer - Google Patents
Preparation method of branching unit-containing polyether-ether-ketone terpolymer Download PDFInfo
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- CN103214638A CN103214638A CN2013101530640A CN201310153064A CN103214638A CN 103214638 A CN103214638 A CN 103214638A CN 2013101530640 A CN2013101530640 A CN 2013101530640A CN 201310153064 A CN201310153064 A CN 201310153064A CN 103214638 A CN103214638 A CN 103214638A
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Abstract
The invention discloses a preparation method of branching unit-containing polyether-ether-ketone terpolymer and belongs to the field of high polymer materials. The preparation method of the branching unit-containing polyether-ether-ketone terpolymer is characterized in that the molar ratio of 4,4'-difluoro diphenyl ketone to hydroquinone to 1,3,5-tri(4-fluorobenzenzoyl) benzene is (15-21):(15-21):1; catalyst is Na2CO3 and K2CO3; the molar ratio of the Na2CO3 to the K2CO3 to the hydroquinone is 0.9:0.1:(1.02-1.05); diphenyl sulfone is used as the solvent; the catalyst is added under the temperature of 140 DEG C to 160 DEG C; the heat is preserved for 2 hours under 200 DEG C to 220 DEG C, the heat is preserved for 1 hour under 250 DEG C to 280 DEG C, and the heat is preserved for 2-5 hours under 300 DEG C to 320 DEG C; the solvent and the catalyst are poured to acetone for sedimentation, refluxed for three times by acetone, refluxed once by alcohol, boiled for three times each being 30 minutes, and preserved for 3-4 hours in a vacuum oven of 120 DEG C. The preparation method of the branching unit-containing polyether-ether-ketone terpolymer has the effect and beneficial effects that the branching unit-containing polyether-ether-ketone resin can be used for improving the glass-transition temperature, improving the using temperature range and prolonging the using time under the high-temperature environment.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of preparation method who contains the branching unit polyetheretherketoneterpolymer terpolymer.
Background technology
Along with society constantly develops, people constantly increase the demand of high temperature material, accelerated high temperature resistant novel material research step, and the polyether-ether-ketone of having outstanding performance in the high temperature material shows one's promises, and is widely applied in the every field because of it has good temperature resistance, high strength, high-modulus or the like excellent comprehensive performance.But the general processing temperature height of polyether-ether-ketone resin, can only be dissolved in the vitriol oil etc., its application is brought certain limitation, and the performance of single polyether-ether-ketone resin be difficult to satisfy its service requirements in all multiple-projects field.
Though polyether-ether-ketone has excellent comprehensive performances, but in order further to improve the performance of polyether-ether-ketone, reduce the polyether-ether-ketone processing temperature, improve its use temperature and to the polyether-ether-ketone functionalization, enlarge the polyaryletherketone range of application, the scientific worker has done a large amount of modification work both at home and abroad in recent years.Second-order transition temperature (the T of pure polyether-ether-ketone resin
g) 143
oC, fusing point (T
m) 343
oC.The present invention is with 4; 4 '-difluoro benzophenone, Resorcinol, 1; 3; 5-three (4-fluorobenzene acyl group) benzene is raw material; prepare and contain branching unit structural polyether ether ketone terpolymer, improved second-order transition temperature, improve its use temperature scope; and prolong its duration of service in the high temperature field, the meaning of practical application is arranged in actual production.
Summary of the invention
The objective of the invention is to contain the branching unit polyetheretherketoneterpolymer terpolymer and produce the second-order transition temperature that branching unit improves polyether-ether-ketone, improve its use temperature scope, and prolong its duration of service in the high temperature field by preparation.
The solution of the present invention is:
The present invention adopts with 1,3,5-three (4-fluorobenzene acyl group) benzene, Resorcinol, 4, and 4 '-difluoro benzophenone is a raw material, 4,4 '-difluoro benzophenone, Resorcinol, 1,3,5-three (4-fluorobenzene acyl group) benzene mole ratio is 15 ~ 21:15 ~ 21:1; Catalyzer is Na
2CO
3And K
2CO
3, Na
2CO
3,K
2CO
3,The Resorcinol mol ratio is 0.9:0.1:1.02 ~ 1.05; With the sulfobenzide is solvent, 140
oC ~ 160
oAdd above-mentioned catalyzer under the C temperature, start to stir and continue to heat up, 200 ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300 ~ 320
oKeep 2 ~ 5h under the temperature of C, pour sedimentation in the acetone into, and reflux three times with acetone, alcohol reflux once, poach three times, each 30min is 120
oKeep 3 ~ 4h in the C vacuum drying oven, obtain the grey powder, prepare a kind of branching unit polyetheretherketoneterpolymer terpolymer that contains.
Effect of the present invention and benefit are that the polyether-ether-ketone resin that contains the branching unit structure has improved second-order transition temperature, have promoted the use temperature scope and have prolonged its duration of service under hot environment.
Description of drawings
Fig. 1 contains branching unit polyetheretherketoneterpolymer terpolymer DSC spectrogram.
Fig. 2 contains branching unit polyetheretherketoneterpolymer terpolymer TGA spectrogram.
Embodiment
Be described in detail the specific embodiment of the present invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1:
In the 100ml there-necked flask, add 4.579g 4,4 '-difluoro benzophenone, 2.311g Resorcinol, 0.444g 1,3,5-three (4-fluorobenzene acyl group) benzene and 27g sulfobenzide are 140
oC-160
oAdd catalyzer under the C temperature, Na
2CO
32.059g and K
2CO
30.296g, start stirring, continue to heat up, 200
oC ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300
oC ~ 320
oKeep 2h under the C temperature, sedimentation in acetone refluxes 3 times through acetone, alcohol reflux once, poach 3 times, each 30min.120
oC vacuum drying oven 4h obtains subject polymer.
Embodiment 2:
In the 100ml there-necked flask, add 3.273g 4,4 '-difluoro benzophenone, 1.652g Resorcinol, 0.444g 1,3,5-three (4-fluorobenzene acyl group) benzene and 27g sulfobenzide are 140
oC-160
oAdd catalyzer under the C temperature, Na
2CO
31.471g and K
2CO
30.211g, start stirring, continue to heat up, 200
oC ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300
oC ~ 320
oKeep 2h under the C temperature, sedimentation in acetone refluxes 3 times through acetone, alcohol reflux once, poach 3 times, each 30min.120
oC vacuum drying oven 4h obtains subject polymer.
Embodiment 3:
In the 100ml there-necked flask, add 4.579g 4,4 '-difluoro benzophenone, 2.311g Resorcinol, 0.444g 1,3,5-three (4-fluorobenzene acyl group) benzene adds the 27g sulfobenzide, at last 140
oC-160
oAdd catalyzer under the temperature of C, Na
2CO
32.185g and K
2CO
30.243g, start stirring, continue to heat up, 200
oC ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300
oC ~ 320
oKeep 2h under the C temperature, sedimentation in acetone refluxes 3 times through acetone, alcohol reflux once, poach 3 times, each 30min.120
oC vacuum drying oven 4h obtains subject polymer.
Embodiment 4:
In the 100ml there-necked flask, add 4.579g 4,4 '-difluoro benzophenone, 2.311g Resorcinol, 0.444g 1,3,5-three (4-fluorobenzene acyl group) benzene and 27g sulfobenzide are 140
oC-160
oAdd catalyzer under the temperature of C, Na
2CO
32.059g and K
2CO
30.296g, start stirring, continue to heat up, 200
oC ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300
oC ~ 320
oKeep 3h under the C temperature, sedimentation in acetone refluxes 3 times through acetone, alcohol reflux once, poach 3 times, each 30min.120
oC vacuum drying oven 3h obtains subject polymer.
Embodiment 5:
In the 100ml there-necked flask, add 4.579g 4,4 '-difluoro benzophenone, 2.311g Resorcinol, 0.444g 1,3,5-three (4-fluorobenzene acyl group) benzene and 27g sulfobenzide are 140
oC-160
oAdd catalyzer under the temperature of C, Na
2CO
32.059g and K
2CO
30.296g, start stirring, continue to heat up, 200
oC ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300
oC ~ 320
oKeep 5h under the C temperature, sedimentation in acetone refluxes 3 times through acetone, alcohol reflux once, poach 3 times, each 30min.120
oC vacuum drying oven 3h obtains subject polymer.
Claims (1)
1. the preparation method who contains the branching unit polyetheretherketoneterpolymer terpolymer is characterized in that 4,4 '-difluoro benzophenone, Resorcinol, 1,3, and the mol ratio of 5-three (4-fluorobenzene acyl group) benzene is 15 ~ 21:15 ~ 21:1; Catalyzer is Na
2CO
3And K
2CO
3, Na
2CO
3,K
2CO
3,The mol ratio of Resorcinol is 0.9:0.1:1.02 ~ 1.05; With the sulfobenzide is solvent, 140
oC ~ 160
oAdd above-mentioned catalyzer under the C temperature, 200 ~ 220
oKeep 2h under the C temperature, 250
oC ~ 280
oKeep 1h under the C temperature, 300 ~ 320
oKeep 2 ~ 5h under the temperature of C, pour sedimentation in the acetone into, and reflux three times with acetone, alcohol reflux once, poach three times, each 30min is 120
oKeep 3 ~ 4h in the C vacuum drying oven, obtain the grey powder, prepare a kind of branching unit polyetheretherketoneterpolymer terpolymer that contains.
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| CN2013101530640A CN103214638A (en) | 2013-04-27 | 2013-04-27 | Preparation method of branching unit-containing polyether-ether-ketone terpolymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101530640A CN103214638A (en) | 2013-04-27 | 2013-04-27 | Preparation method of branching unit-containing polyether-ether-ketone terpolymer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103214638A true CN103214638A (en) | 2013-07-24 |
Family
ID=48812835
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788632A (en) * | 2015-04-27 | 2015-07-22 | 吉林省中研高性能工程塑料股份有限公司 | Preparation method of high-purity polyether-ether-ketone |
| CN110483763A (en) * | 2019-08-22 | 2019-11-22 | 大连理工大学 | One kind branching type o-phthalonitrile resin of based structures containing benzoyl and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660755A (en) * | 2004-12-10 | 2005-08-31 | 吉林大学 | 1,3,5 three[4-(4-fluorobenzene acyl) phenoxy] benzene monomer and synthesizing method |
| CN101215404A (en) * | 2008-01-04 | 2008-07-09 | 吉林大学 | Special-purpose material for spinning-stage polyetheretherketone resin and preparation method thereof |
-
2013
- 2013-04-27 CN CN2013101530640A patent/CN103214638A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660755A (en) * | 2004-12-10 | 2005-08-31 | 吉林大学 | 1,3,5 three[4-(4-fluorobenzene acyl) phenoxy] benzene monomer and synthesizing method |
| CN101215404A (en) * | 2008-01-04 | 2008-07-09 | 吉林大学 | Special-purpose material for spinning-stage polyetheretherketone resin and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| SEUNG-YEOP KWAK ET AL: "Processability of Hyperbranched Poly(ether ketone)s with Different Degrees of Branching from Viewpoints of Molecular Mobility and Comparison with Their Linear Analogue", 《MACROMOLECULES》, vol. 33, 13 September 2000 (2000-09-13), pages 7557 - 7563, XP002565806, DOI: doi:10.1021/ma991569r * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788632A (en) * | 2015-04-27 | 2015-07-22 | 吉林省中研高性能工程塑料股份有限公司 | Preparation method of high-purity polyether-ether-ketone |
| CN104788632B (en) * | 2015-04-27 | 2017-07-21 | 吉林省中研高性能工程塑料股份有限公司 | A kind of preparation method of high-purity polyether-ether-ketone |
| CN110483763A (en) * | 2019-08-22 | 2019-11-22 | 大连理工大学 | One kind branching type o-phthalonitrile resin of based structures containing benzoyl and preparation method thereof |
| CN110483763B (en) * | 2019-08-22 | 2022-03-29 | 大连理工大学 | Branched phthalonitrile resin containing benzoyl structure and preparation method thereof |
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Application publication date: 20130724 |