CN105524266A - Preparation method for polycarbonate - Google Patents
Preparation method for polycarbonate Download PDFInfo
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- CN105524266A CN105524266A CN201510759145.4A CN201510759145A CN105524266A CN 105524266 A CN105524266 A CN 105524266A CN 201510759145 A CN201510759145 A CN 201510759145A CN 105524266 A CN105524266 A CN 105524266A
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- preparation
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- polycarbonate
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- prepolymer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides a preparation method for polycarbonate, which belongs to the field of material preparation. The preparation method is characterized by comprising the following steps: adding weighed BPA, DPC and a catalyst into a reaction vessel; replacing air in the reaction vessel with N2, adjusting the temperature of the reaction vessel to 165 DEG C and carrying out a reaction for 30 min, then adjusting the temperature of the reaction vessel to 180 DEG C and carrying out a reaction for 1 h, adjusting the temperature to 195 DEG C and carrying out a reaction for 1 h, vacuumizing the reaction vessel, closing all the valves and power supply, eluting out the catalyst with a solvent after a melt is cooled in the reaction vessel, and then carrying out drying so as to obtain a prepolymer; and placing the prepolymer in a reactor, replacing air with CO2, subjecting the reactor to cooling and pressure release, collecting a product and drying the product to a constant weight so as to obtain PC. On the basis of the characteristics of impinging stream reinforced material transfer and dissolving of a reaction by-product, i.e., micromolecular phenol, with SC-CO2, solid polymerization of PC is realized in the supercritical impinging stream reactor, so the performance of prepared carbonic ester is effectively improved; and the preparation method is simple and is easy to promote and apply.
Description
Technical field
The invention belongs to field of material preparation, particularly relate to a kind of preparation method of polycarbonate.
Background technology
Along with the fast development of science and technology, all there is larger change according to the demand of self in the starting material of every profession and trade.Chain carbonic ester containing flexibility in bisphenol A polycarbonate (PC) structure and the phenyl ring of rigidity, make it have the property that other engineering plastics many do not possess, be widely used in the fields such as electronic apparatus, building, automobile making, aerospace, optics.PC industrialized production method mainly contains phosgenation and melt transesterification process.Phosgenation adopts poisonous phosgene, and produces a large amount of organic pollutants, waste water and solid waste; Melt transesterification process adopts high temperature, and side reaction is increased, and the color and luster of product is poor.
Summary of the invention
The present invention is intended to solve the problem, and provides a kind of preparation method of polycarbonate.
A preparation method for polycarbonate, is characterized in that comprising the steps:
(1) first accurately take 11.03gBPA, 10.56gDPC and 0.0079g catalyzer, add in the stainless steel cauldron with whipping appts, cover tightly sealed reactor;
(2) N is used
2air in replacement reaction kettle, regulates temperature of reaction kettle to 165 DEG C, after reaction 30min, regulate temperature of reaction kettle to 180 DEG C, after question response 1h, then rise to 195 DEG C, reaction 1h, being evacuated to vacuum tightness is close all valves and power supply after 0.03MPa, 5min, at room temperature, after melt cools in a kettle., collect low molecular weight prepolymer solid, wash out catalyzer with solvent, grind and sieve out particle after dry and make prepolymer;
(3) prepolymer is placed in reactor, uses CO
2displaced air, the CO imported and exported by balanced reaction device
2flow keeps reacting kettle inner pressure constant, carries out cooling pressure release process to reactor, collects product, is dried to constant weight, obtains PC.
The preparation method of a kind of polycarbonate of the present invention, is characterized in that the time of displaced air described in step (2) is 0.5h.
The preparation method of a kind of polycarbonate of the present invention, is characterized in that the mixing speed of reactor described in step (2) is 800r/rain.
The preparation method of a kind of polycarbonate of the present invention, is characterized in that described in step (2), vacuum pump is circulating water type vacuum pump.
The preparation method of a kind of polycarbonate of the present invention, is characterized in that described in step (3), the displaced air time is 30min.
The preparation method of a kind of polycarbonate of the present invention, is transmitted and SC-CO by percussion flow fortification substance
2the feature of solubilizing reaction small molecular by product phenol, in overcritical impact flow reactor, achieves the solid state polymerization of PC, and the performance of prepared carbonic ether is effectively improved, and this preparation method preparation technology is simple, is easy to promote the use of.
Embodiment
A preparation method for polycarbonate, is characterized in that comprising the steps:
(1) first accurately take 11.03gBPA, 10.56gDPC and 0.0079g catalyzer, add in the stainless steel cauldron with whipping appts, cover tightly sealed reactor;
(2) N is used
2air in replacement reaction kettle, regulates temperature of reaction kettle to 165 DEG C, after reaction 30min, regulate temperature of reaction kettle to 180 DEG C, after question response 1h, then rise to 195 DEG C, reaction 1h, being evacuated to vacuum tightness is close all valves and power supply after 0.03MPa, 5min, at room temperature, after melt cools in a kettle., collect low molecular weight prepolymer solid, wash out catalyzer with solvent, grind and sieve out particle after dry and make prepolymer;
(3) prepolymer is placed in reactor, uses CO
2displaced air, the CO imported and exported by balanced reaction device
2flow keeps reacting kettle inner pressure constant, carries out cooling pressure release process to reactor, collects product, is dried to constant weight, obtains PC.
The preparation method of a kind of polycarbonate of the present invention, the time of displaced air described in step (2) is 0.5h.Described in step (2), the mixing speed of reactor is 800r/rain.Described in step (2), vacuum pump is circulating water type vacuum pump.The displaced air time described in step (3) is 30min.First polycondensation by-product phenol by the internal surface of solid pre-polymer particles, must diffuse to outside surface.Intraparticle diffusivity increases with the reduction of prepolyer granule particle diameter, and after particle diameter is less than certain value, internal diffusion speed is unaffected, and inside diffusional resistance is negligible.After prepolyer granule particle diameter is less than 0.143mm, the number-average molecular weight increase in time of PC is no longer subject to the impact of prepolyer granule size, reduces the molecular weight that particle diameter can not increase PC further, can think that the inside diffusional resistance of phenol is got rid of.Phenol needs to pass through SC-CO from solid prepolymer outside surface
2the detention layer that fluid is formed at particle exterior surface, diffuses to bodies of fluid, and the external diffusion resistance of generation reduces with the increase of rate of flow of fluid: flow velocity increases. and detention layer is thinning, and resistance reduces, and spread coefficient increases, and rate of diffusion improves.Be the prepolymer of 0.078 ~ 0.098mm to particle diameter, at CO
2flow is respectively 10, and 15,20 and 30mL/min, temperature is 1100C, and pressure is under 10MPa condition, and carry out polycondensation further within the identical polycondensation time, the number-average molecular weight of PC is minimum when C02 flow is 10mL/min, works as CO
2after flow is greater than 15mL/min, the number-average molecular weight of the PC of identical polycondensation time is of slight difference, the number-average molecular weight of PC increases with the increase of temperature, but polycondensation reaction time is in 0 ~ 6h, molecular weight under differing temps is almost linear increase, and the polycondensation time, the speed that number-average molecular weight increases slowed down more than after 6h, temperature is higher, slows down more obvious.This may be higher due to temperature, and speed of reaction is faster, and the reaction times is longer in addition, and make the number-average molecular weight of PC larger, the viscosity of reaction system increases thereupon.When the polycondensation time more than 6h after, in system, the resistance of polycondensation by-product phenol diffusion can not be got rid of, removing in time of phenol is obstructed, whole polymerization process is caused not only to control by Kinetic, also by the control of phenol diffusion, slow down so the number-average molecular weight of PC is advanced the speed, temperature is higher, slows down more obvious.
Claims (5)
1. a preparation method for polycarbonate, is characterized in that comprising the steps:
(1) first accurately take 11.03gBPA, 10.56gDPC and 0.0079g catalyzer, add in the stainless steel cauldron with whipping appts, cover tightly sealed reactor;
(2) N is used
2air in replacement reaction kettle, regulates temperature of reaction kettle to 165 DEG C, after reaction 30min, regulate temperature of reaction kettle to 180 DEG C, after question response 1h, then rise to 195 DEG C, reaction 1h, being evacuated to vacuum tightness is close all valves and power supply after 0.03MPa, 5min, at room temperature, after melt cools in a kettle., collect low molecular weight prepolymer solid, wash out catalyzer with solvent, grind and sieve out particle after dry and make prepolymer;
(3) prepolymer is placed in reactor, uses CO
2displaced air, the CO imported and exported by balanced reaction device
2flow keeps reacting kettle inner pressure constant, carries out cooling pressure release process to reactor, collects product, is dried to constant weight, obtains PC.
2. the preparation method of a kind of polycarbonate as claimed in claim 1, is characterized in that the time of displaced air described in step (2) is 0.5h.
3. the preparation method of a kind of polycarbonate as claimed in claim 1, is characterized in that the mixing speed of reactor described in step (2) is 800r/rain.
4. the preparation method of a kind of polycarbonate as claimed in claim 1, is characterized in that described in step (2), vacuum pump is circulating water type vacuum pump.
5. the preparation method of a kind of polycarbonate as claimed in claim 1, is characterized in that described in step (3), the displaced air time is 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510759145.4A CN105524266A (en) | 2015-11-10 | 2015-11-10 | Preparation method for polycarbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510759145.4A CN105524266A (en) | 2015-11-10 | 2015-11-10 | Preparation method for polycarbonate |
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| Publication Number | Publication Date |
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| CN105524266A true CN105524266A (en) | 2016-04-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510759145.4A Pending CN105524266A (en) | 2015-11-10 | 2015-11-10 | Preparation method for polycarbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114437333A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | Preparation method of bio-based polycarbonate |
-
2015
- 2015-11-10 CN CN201510759145.4A patent/CN105524266A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114437333A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | Preparation method of bio-based polycarbonate |
| CN114437333B (en) * | 2020-10-31 | 2024-03-08 | 中国石油化工股份有限公司 | Preparation method of bio-based polycarbonate |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160427 |
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| WD01 | Invention patent application deemed withdrawn after publication |