CN201292330Y - Integrated transesterification synthesis polycarbonate reactor - Google Patents
Integrated transesterification synthesis polycarbonate reactor Download PDFInfo
- Publication number
- CN201292330Y CN201292330Y CNU2008201241081U CN200820124108U CN201292330Y CN 201292330 Y CN201292330 Y CN 201292330Y CN U2008201241081 U CNU2008201241081 U CN U2008201241081U CN 200820124108 U CN200820124108 U CN 200820124108U CN 201292330 Y CN201292330 Y CN 201292330Y
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- Prior art keywords
- polymerization kettle
- welded
- phenol
- shell
- receiver
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 33
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 33
- 238000005809 transesterification reaction Methods 0.000 title claims abstract 3
- 230000015572 biosynthetic process Effects 0.000 title description 19
- 238000003786 synthesis reaction Methods 0.000 title description 19
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 34
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000009530 blood pressure measurement Methods 0.000 claims 1
- 238000005485 electric heating Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- ROORDVPLFPIABK-UHFFFAOYSA-N diphenyl carbonate Chemical compound C=1C=CC=CC=1OC(=O)OC1=CC=CC=C1 ROORDVPLFPIABK-UHFFFAOYSA-N 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- MNAHQWDCXOHBHK-UHFFFAOYSA-N 1-phenylpropane-1,1-diol Chemical compound CCC(O)(O)C1=CC=CC=C1 MNAHQWDCXOHBHK-UHFFFAOYSA-N 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- HKEUSHDVFNSFLJ-UHFFFAOYSA-N C(C=1C(C(=O)OC2=CC=CC=C2)=CC=CC1)(=O)OC1=CC=CC=C1.[C] Chemical compound C(C=1C(C(=O)OC2=CC=CC=C2)=CC=CC1)(=O)OC1=CC=CC=C1.[C] HKEUSHDVFNSFLJ-UHFFFAOYSA-N 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- 238000012696 Interfacial polycondensation Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229920000402 bisphenol A polycarbonate polymer Polymers 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Images
Classifications
-
- 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
- Y02P20/10—Process efficiency
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- Polyesters Or Polycarbonates (AREA)
Abstract
本实用新型涉及一种一体式酯交换法合成聚碳酸酯反应器；苯酚接收器连接在聚合釜外壳上；聚合釜外壳连接在聚合釜底座上；冷却水出口焊在苯酚接收器边缘位置，冷却水入口焊在聚合釜外壳的上部；苯酚接收器热电偶套管焊在与苯酚接收器上靠近中心线的位置上；真空泵抽气孔焊在聚合釜底座上；压力检测系统焊在聚合釜外壳上部；控温系统焊在聚合釜底座上；聚合釜外壳热电偶套管焊在聚合釜外壳上部；聚合釜热电偶套管焊在苯酚接收器上，聚合釜位于聚合釜外壳中聚合釜底座上，是由表面光滑的镍材构成的底部为半圆形的筒式结构，内设搅拌器；此设备实现了一个设备具有三个温度能够独立控制的反应区；结构简单，操作方便，造价低，不存在“三废”问题。
The utility model relates to an integrated polycarbonate reactor synthesized by transesterification; the phenol receiver is connected to the shell of the polymerization kettle; the shell of the polymerization kettle is connected to the base of the polymerization kettle; The water inlet is welded on the upper part of the polymerization kettle shell; the phenol receiver thermocouple sleeve is welded on the position close to the centerline of the phenol receiver; the vacuum pump exhaust hole is welded on the polymerization kettle base; the pressure detection system is welded on the upper part of the polymerization kettle shell The temperature control system is welded on the base of the polymerization kettle; the thermocouple casing of the polymerization kettle shell is welded on the upper part of the polymerization kettle casing; the thermocouple casing of the polymerization kettle is welded on the phenol receiver, and the polymerization kettle is located on the polymerization kettle base in the polymerization kettle shell It is a cylindrical structure with a semicircular bottom made of smooth nickel material, with a stirrer inside; this equipment realizes that one equipment has three reaction zones whose temperature can be independently controlled; the structure is simple, the operation is convenient, and the cost is low. There is no "three wastes" problem.
Description
Technical field
The utility model relates to a kind of integral type ester-interchange method melt phase polycondensation polycarbonate synthesis reactor.
Background technology
Bisphenol A polycarbonate is since polycarbonate in 1958 is commercially produced exploitation, it is obtaining huge development aspect kind and the purposes, as a kind of important thermoplastic engineering plastic, it has characteristics such as the good shock-resistance and the transparency, fields such as automobile making, health care, food, optical material and protective material have been entered, at present, polycarbonate just promptly expands to high-technology fields such as Aeronautics and Astronautics, military affairs.
At present, interfacial polycondensation phosgenation and ester-interchange method polycarbonate synthesis have been realized industrialization, and wherein phosgenation not only uses the phosgene of severe toxicity, also uses methylene dichloride, causes more serious pollution to environment; Simultaneously the technology of this synthetic method is very complicated, and has that plant investment is big, floor space wide and the high shortcoming of maintenance of the equipment expense.Compare with phosgenation, ester-interchange method polycarbonate synthesis technology is more succinct, avoid using phosgene and methylene dichloride, substantially there are not " three wastes ", be " cleaning procedure " and " green chemical industry ", but polymerization stage is to be finished by a plurality of conversion units, has problems such as power consumption is excessive and artificial.
US6204352B1 has announced a kind of equipment of polycarbonate synthesis.It is raw material with dihydroxyphenyl propane and carbonic ether that this patent provides a kind of, by the device of melt polymerization process polycarbonate synthesis.Polycarbonate of this device preparation has characteristics such as good color stability, foreign matter content are few.
CN2487736Y has announced that a kind of horizontal single-drum of producing polycarbonate stirs degassing reactor.This reactor rotates and stirs fully, has the good degassing, is specially adapted to need in time remove the reaction process that produces light-component gas greatly again as this class material viscosity of polycarbonate.
CN1304458C has announced a kind of method of polycarbonate and device of preparation polycarbonate of preparing.This device comprises the prepolymerization reactor with entrance and exit, post-polymerization device with entrance and exit, the mixing tank that communicates with prepolymerization reactor outlet and post-polymerization device inlet fluid, with the charging opening that end-capping reagent is joined in the mixing tank, wherein mixing tank is more than or equal to the 760mmHg lower seal.
At present, the equipment of phosgenation and melt-polycondensation polycarbonate synthesis is a lot, but complex structure is made up of a plurality of reaction members, complex operation, and investment is big, is unfavorable for polycarbonate study on the synthesis and amplification.
The utility model content
The purpose of this utility model provides a kind of integral type ester-interchange method polycarbonate synthesis reactor, polycarbonate is organically combined in same equipment synthetic the separation with phenol, the polymeric kettle part can form the high-temperature zone of temperature about 300 ℃, and polymeric kettle shell and phenol collector partly form 20～40 ℃ cold zone, this device has equipment and process simplification, floor space is little, and energy consumption is little, the advantage of reduced investment.
Integral type ester-interchange method polycarbonate synthesis reactor described in the utility model is made up of agitator, phenol receptor, condensation-water drain, polymeric kettle thermocouple sheath, phenol receptor thermocouple sheath, pressure-measuring system, polymeric kettle shell thermocouple sheath, polymeric kettle, polymeric kettle shell, temperature controlling system, nitrogen inlet, vacuum pump aspirating hole and polymeric kettle base.The phenol receptor is connected polymeric kettle shell upper end by flange and union lever; Polymeric kettle shell bottom is connected on the polymeric kettle base by flange; Condensation-water drain is welded in the top of phenol receptor marginal position and polymeric kettle shell; Phenol receptor thermocouple sheath be welded in the phenol receptor near on the position of medullary ray; The vacuum pump aspirating hole is welded on the polymeric kettle base; Pressure detecting system is welded in the polymeric kettle shell upper, is made of accurate vacuum meter and Mcleod vacuum gauge; Temperature controlling system is welded on the polymeric kettle base, adopts electrically heated and temperature programming; Polymeric kettle shell thermocouple sheath is welded in the polymeric kettle shell upper; The polymeric kettle thermocouple sheath is welded on the phenol receptor, polymeric kettle is arranged on the polymeric kettle shell polymeric kettle base, be to be semicircular core structure by the bottom that ganoid nickel material constitutes, in establish agitator, alr mode is the whipped form that frame, anchor formula or screw are fit to medium-high viscosity.
In the polycarbonate building-up process, reaction raw materials (diphenyl carbonate and dihydroxyphenyl propane) and catalyzer place polymeric kettle, heat to polymeric kettle by temperature controlling system, cause the temperature of polymeric kettle to raise.Because the vacuum of polymeric kettle shell and system, and around reactor, be provided with the multi-layer heat preserving layer, so the temperature in the polymeric kettle can make raw material reaction, and carry out to the positive reaction direction.Carrying out along with reaction, reaction system can constantly have phenol production, the vacuum of system reduces the boiling point of phenol greatly, like this phenol condensation of gas of Shang Shenging, be collected in the phenol collector, in whole polymerization process, keep the vacuum tightness of system with vacuum pump, the good airproof performance of this integral type polymerizer, vacuum can reach below the 5Pa, and lower vacuum tightness helps deviating from of phenol and excess carbon diphenyl phthalate in the high viscosity polycarbonate product.
Utilize the utility model, at first raw material (diphenyl carbonate and dihydroxyphenyl propane) and catalyzer are joined in the polymeric kettle, under slowly stirring, slowly be warming up to 120～140 ℃, adopt oilless vacuum pump to keep the vacuum tightness of system, vacuum tightness 0.09Mpa, insulation 20min; Temperature in the kettle is 140～180 ℃, during vacuum tightness 0.05～0.08MPa, and insulation 2h, the phenol that this moment, reaction system can be relatively large, phenol steam comes out from reaction system, condensation on the phenol collector, collect, keep the vacuum of reactive system, the molecular weight of polycarbonate is progressively increased; Temperature in the kettle is 200～280 ℃, and during vacuum tightness 0.01～0.0004MPa, reaction 5h evaporates phenol and small amount of carbon diphenyl phthalate in the high viscosity polycarbonate.
Reaction finishes, residual impurity in the polycarbonate product (phenol and diphenyl carbonate) content is below 0.05%wt (weight content), and in the polycarbonate synthesis process, do not introduce other media, the phenol that reclaims can be used as the raw material of diphenyl carbonate synthesis, not only greatly reduced production cost, and can guarantee that the product polycarbon resin is not subjected to external influence, thereby improve the degree of cleaning and the optical property of product.
The design possesses following characteristics:
1, in this integral reactor, can produce three humidity provinces, i.e. reaction zone, condensing zone and heat preservation zone.Wherein the temperature of reaction zone can reach more than 300 ℃, and the reaction of diphenyl carbonate and dihydroxyphenyl propane polycarbonate synthesis under the effect of catalyzer is exactly to take place in this zone; The temperature of condensing zone is between 20～40 ℃, and this condensable phenol gas that comes out from reactor in zone and excessive diphenyl carbonate are convenient to collect; The temperature of heat preservation zone with the well heater acting in conjunction, is kept the temperature in the polymeric kettle between room temperature～200 ℃.Realized polycarbonate is combined in the conversion unit synthetic the separation with phenol; Realized that a conversion unit has three humidity provinces, and the temperature of three humidity provinces can realize independent control.
2, compare with existing polycarbonate synthesis device, this device structure is simple, and requirement on machining accuracy is not high, and cost is low, does not have " three wastes " problem substantially.
3, easy to operate, each synthetic finishing, as long as open the phenol receptor successively, collect phenol, as the raw material of diphenyl carbonate synthesis, then the reaction product in the polymeric kettle is taken out, with methyl chloride cleaning reaction device, because the ratio between polymeric kettle shell and the polymeric kettle is suitable, these operations all are easy to carry out; If begin new test, can reaction raw materials be joined in the polymeric kettle by opposite order erecting equipment, phenol receptor and polymeric kettle shell are connected by flange, pressure testing successively, open water of condensation, stir, vacuumize, polycondensation is carried out in heating, finishes up to reaction.
Description of drawings
Fig. 1 integral type ester-interchange method polycarbonate synthesis structure of reactor synoptic diagram.
Wherein: 1, agitator 2, phenol receptor 3, water of condensation go out 4, polymeric kettle thermocouple sheath 5, phenol receptor thermocouple sheath 6, water of condensation go out 7, pressure-measuring system 8, polymeric kettle shell thermocouple sheath 9, polymeric kettle 10, polymeric kettle shell 11, temperature controlling system 12, nitrogen inlet 13, vacuum pump aspirating hole 14, polymeric kettle base
Embodiment
Below in conjunction with accompanying drawing integral type ester-interchange method polycarbonate synthesis structure of reactor described in the utility model is described in further detail.
Integral type ester-interchange method polycarbonate synthesis reactor described in the utility model is made up of agitator 1, phenol receptor 2, condensation- water drain 3,6, polymeric kettle thermocouple sheath 4, phenol receptor thermocouple sheath 5, pressure-measuring system 7, polymeric kettle shell thermocouple sheath 8, polymeric kettle 9, polymeric kettle shell 10, temperature controlling system 11, nitrogen inlet 12, vacuum pump aspirating hole 13 and polymeric kettle base 14.Phenol receptor 2 is connected polymeric kettle shell 10 upper ends by flange and union lever; Polymeric kettle shell 10 bottoms are connected on the polymeric kettle base 14 by flange; Condensation-water drain 6 is welded in phenol receptor 2 marginal positions, and condensation-water drain 3 is welded in the top of polymeric kettle shell 10; Phenol receptor thermocouple sheath 5 be welded in phenol receptor 2 near on the position of medullary ray; Vacuum pump aspirating hole 13 is welded on the polymeric kettle base 14; Pressure detecting system 7 is welded in polymeric kettle shell 10 tops, is made of accurate vacuum meter and Mcleod vacuum gauge; Temperature controlling system 11 is welded on the polymeric kettle base 14, adopts electrically heated and temperature programming; Polymeric kettle shell thermocouple sheath 8 is welded in polymeric kettle shell 10 tops; Polymeric kettle thermocouple sheath 4 is welded on the phenol receptor 2, polymeric kettle 9 is arranged on the polymeric kettle shell 10 polymeric kettle bases 14, be to be semicircular core structure by the bottom that ganoid nickel material constitutes, in establish agitator 1, alr mode is the whipped form that frame, anchor formula or screw are fit to medium-high viscosity.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008201241081U CN201292330Y (en) | 2008-11-24 | 2008-11-24 | Integrated transesterification synthesis polycarbonate reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2008201241081U CN201292330Y (en) | 2008-11-24 | 2008-11-24 | Integrated transesterification synthesis polycarbonate reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201292330Y true CN201292330Y (en) | 2009-08-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNU2008201241081U Expired - Lifetime CN201292330Y (en) | 2008-11-24 | 2008-11-24 | Integrated transesterification synthesis polycarbonate reactor |
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| Country | Link |
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| CN (1) | CN201292330Y (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702500A (en) * | 2012-06-18 | 2012-10-03 | 陕西延长石油（集团）有限责任公司 | Preparation method of aromatic polycarbonate |
| CN102812069A (en) * | 2010-03-24 | 2012-12-05 | 沙伯基础创新塑料知识产权有限公司 | Method of making polycarbonate |
| CN109880074A (en) * | 2019-02-25 | 2019-06-14 | 台州市欧威家具有限公司 | The preparation method of polycarbonate |
| CN111821928A (en) * | 2020-08-11 | 2020-10-27 | 扬州普立特科技发展有限公司 | A device suitable for synthesizing polycarbonate by melt transesterification |
-
2008
- 2008-11-24 CN CNU2008201241081U patent/CN201292330Y/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102812069A (en) * | 2010-03-24 | 2012-12-05 | 沙伯基础创新塑料知识产权有限公司 | Method of making polycarbonate |
| CN102812069B (en) * | 2010-03-24 | 2014-06-11 | 沙伯基础创新塑料知识产权有限公司 | Method of making polycarbonate |
| CN102702500A (en) * | 2012-06-18 | 2012-10-03 | 陕西延长石油（集团）有限责任公司 | Preparation method of aromatic polycarbonate |
| CN109880074A (en) * | 2019-02-25 | 2019-06-14 | 台州市欧威家具有限公司 | The preparation method of polycarbonate |
| CN109880074B (en) * | 2019-02-25 | 2020-08-11 | 浙江欧威家具股份有限公司 | Process for the preparation of polycarbonates |
| CN111821928A (en) * | 2020-08-11 | 2020-10-27 | 扬州普立特科技发展有限公司 | A device suitable for synthesizing polycarbonate by melt transesterification |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20090819 |