CN105622916A - Industrial production method for polycarbonate - Google Patents
Industrial production method for polycarbonate Download PDFInfo
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- CN105622916A CN105622916A CN201610155890.2A CN201610155890A CN105622916A CN 105622916 A CN105622916 A CN 105622916A CN 201610155890 A CN201610155890 A CN 201610155890A CN 105622916 A CN105622916 A CN 105622916A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/30—General preparatory processes using carbonates
- C08G64/307—General preparatory processes using carbonates and phenols
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Abstract
The invention relates to the field of chemical engineering, in particular to an industrial production method for polycarbonate, and provides a production process for continuously producing polycarbonate with diphenyl carbonate and bisphenol A as raw materials and a control method. The industrial production method for polycarbonate includes the steps of a material mixing stage, a reaction rectification stage, a transesterification stage, a condensation polymerization reaction stage and a final polymerization reaction stage. Continuous industrial production is achieved through control over the pressure and temperature.
Description
Technical field
The present invention relates to chemical field, refer more particularly to a kind of polycarbonate industrial process, taking diphenyl carbonate and dihydroxyphenyl propane as the production technique of raw material continuous production of polycarbonate and control method.
Background technology
It is the high molecular polymer containing carbonic acid ester group in molecular chain that polycarbonate (is called for short PC), according to the structure of ester group
The broad varietys such as aliphatics, aromatic series, aliphatic-aromatic can be divided into. Wherein owing to aliphatics and aliphatic-aromatic gather
The mechanical property of carbonic ether is lower, thus limits its application in engineering plastics. Only there is aromatic copolycarbonate at present
Obtain suitability for industrialized production. Due to the singularity on polycarbonate structure, now become in five large-engineering plastics rate of growth
Fast general engineering plastic.
The large-scale production technology of current polycarbonate (PC) mainly interface polycondensation and melt transesterification process. Interface polycondensation is taking phosgene and bisphenol A disodium salt as raw material, and reaction conditions is gentle, and equipment requirements is low, but needs the loaded down with trivial details postprocessing working procedures such as washing, desalination, desolventizing, uses a large amount of organic solvent, serious three wastes in process; Melt transesterification process technical process is simple, only just can obtain polycarbonate by direct reaction by raw material of dihydroxyphenyl propane and diphenyl carbonate, and not use the methylene chloride of toxicity, avoid the harm to environment. Although this method requires strictly in material purity, production unit, Technology etc., but along with the progress of chemical industry equipment, control instruments technology, it has been trend of the times that melt transesterification process replaces interface polycondensation.
The present invention provides a kind of polycarbonate industrial process, taking diphenyl carbonate and dihydroxyphenyl propane as the production technique of raw materials melt continuous production of polycarbonate by transesterification method and control method.
Summary of the invention
It is desirable to provide a kind of polycarbonate industrial process, taking diphenyl carbonate and dihydroxyphenyl propane as the production technique of raw materials melt continuous production of polycarbonate by transesterification method and tool body controlling means.
The present invention is realized by following technical scheme:
A kind of polycarbonate industrial process, comprises the steps:
A, diphenyl carbonate and dihydroxyphenyl propane are with the ratio of mol ratio 1:1.05 ~ 1:1.1, enter charging surge tank, it is delivered to the circulation of batch mixing preheater by batch mixing recycle pump to heat and mix, in charging surge tank, temperature controls at 170 DEG C ~ 180 DEG C, Liquid level is the 65% ~ 75% of liquidometer, open batch mixing fresh feed pump, by mass transport in charging surge tank to entry mixers; The phenol solution of catalyzer and the mass ratio of mixture are the ratio of 1:4.7 ~ 1:4.8, enter entry mixers respectively, after mixing, material enters reactive distillation system after being heated by feed preheater, and feed preheater outlet mixture temperature controls at 190 DEG C ~ 195 DEG C;
B, reactive distillation system pressure control-79 ~-82KPa, bottom temperature 195 ~ 200 DEG C, tower top temperature 110 DEG C ~ 120 DEG C, reflux ratio 2:1 ~ 1:1, the phenol that tower top obtains contains a small amount of diphenyl carbonate mass transport and processes to lighting end recovery system; Tower reactor Liquid level is the 70% ~ 75% of liquidometer, and the material part through preliminary transesterification reaction is delivered to reactive distillation system reboiler heat exchange by tower reactor recycle pump, and returns tower reactor; Another part kettle material is delivered to transesterification reaction system by reactive distillation system discharging pump and continues transesterification reaction;
C, transesterification reaction system pressure control-85 ~-90KPa, temperature 205 ~ 210 DEG C, open when liquid level is more than 20% and stir, and ensure that normal running liquid level is at the 60% ~ 65% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system from reactive system top, opens transesterification reaction system discharging pump to prepolymerization reaction system feeding;
-97KPa when the initial-94KPa of d, prepolymerization reaction system pressure progressively drops to normal running, temperature 230 ~ 235 DEG C, open when liquid level is more than 15% and stir, and ensure that normal running liquid level is at the 60% ~ 65% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system from reactive system top, opens prepolymerization reaction system discharging pump to horizontal stirring reaction system feeding;
Initial-the 97KPa of e, horizontal stirring reaction system pressure progressively drops to normal running-99KPa, temperature 270 ~ 275 DEG C, open when liquid level is more than 15% and stir, stirring velocity 2r/min also progressively increases to values for normal operation 4r/min, ensure that normal running liquid level is at the 75% ~ 80% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system from reactive system top, opens horizontal stirring reaction system discharging pump to poly-reactive system charging eventually;
F, the eventually initial-99.5KPa of poly-reacting system pressure progressively drop to normal running-99.8KPa, temperature 285 ~ 290 DEG C, open when liquid level is more than 15% and stir, stirring velocity 1r/min also progressively increases to values for normal operation 2r/min, ensure that normal running liquid level is at the 75% ~ 80% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system from reactive system top, opens poly-reactive system discharging pump eventually and polycarbonate is delivered to granulating system.
In the industrial process of above-mentioned a kind of polycarbonate, in step a, diphenyl carbonate and dihydroxyphenyl propane mixture are from entering charging surge tank to reaching Liquid level value liquidometer 65% ~ 75%, and required time is 2h ~ 2.5h.
In the industrial process of above-mentioned a kind of polycarbonate, in step b, mixture enters reactive distillation system and reaches the 70% ~ 75% of controlling valu liquidometer to reactive distillation system tower reactor liquid level, and required time is 3h.
In the industrial process of above-mentioned a kind of polycarbonate, in step b, in reactive distillation system kettle material, phenol mass content is 8% ~ 10%.
In the industrial process of above-mentioned a kind of polycarbonate, in step c, material enters transesterification reaction system and reaches the 60% ~ 65% of values for normal operation liquidometer to transesterification reaction system liquid level, and required time is 3h.
In the industrial process of above-mentioned a kind of polycarbonate, in steps d ,-97KPa when the initial-94KPa of prepolymerization reaction system pressure progressively drops to normal running, its method reduces pressure 1KPa until reaching values for normal operation in every 20 minutes.
In the industrial process of above-mentioned a kind of polycarbonate, in steps d, material enters prepolymerization reaction system and reaches the 60% ~ 65% of values for normal operation liquidometer to prepolymerization reaction system liquid level, and required time is 1.5h.
In the industrial process of above-mentioned a kind of polycarbonate, in step e ,-99KPa when the initial-97KPa of horizontal stirring reaction system pressure progressively drops to normal running, its method reduces pressure 0.5KPa until reaching values for normal operation in every 15 minutes.
In the industrial process of above-mentioned a kind of polycarbonate, in step e, horizontal stirring reaction system stirring velocity 2r/min also progressively increases to values for normal operation 4r/min, and its method increases 0.5r/min until reaching values for normal operation in every 15 minutes.
In the industrial process of above-mentioned a kind of polycarbonate, in step e, material enters horizontal stirring reaction system to horizontal stirring reaction system liquid level and reaches values for normal operation liquidometer 75% ~ 80%, and required time is 2.5h.
In the industrial process of above-mentioned a kind of polycarbonate, in step f ,-99.8KPa when the initial-99.5KPa of poly-reacting system pressure progressively drops to normal running eventually, its method reduces pressure 0.05KPa until reaching values for normal operation in every 15 minutes.
In the industrial process of above-mentioned a kind of polycarbonate, in step f, gathering reactive system stirring velocity 1r/min eventually and progressively increase to values for normal operation 2r/min, its method increases 0.25r/min until reaching values for normal operation in every 15 minutes.
In the industrial process of above-mentioned a kind of polycarbonate, in step f, material enters poly-reactive system eventually and reaches values for normal operation liquidometer 75% ~ 80% to poly-reactive system liquid level eventually, and required time is 3.5h.
The useful effect of the present invention is being: the industrial process providing a kind of polycarbonate; Provide ripe production technique and concrete processing parameter and control method; Using reactive distillation system to carry out the first step reaction of transesterify, the proposition being more conducive to melt transesterification process by-product phenol is produced; Polycarbonate production popularization easier.
Accompanying drawing explanation
Fig. 1 is the schema of a kind of polycarbonate industrial process.
Nomenclature:
F1--diphenyl carbonate charging
F2--dihydroxyphenyl propane charging
F3--catalyst phenol solution feed
V1--charging surge tank
E1--batch mixing preheater
M1--entry mixers
E2--feed preheater
T1--reactive distillation system
P1--batch mixing recycle pump
P2--batch mixing fresh feed pump
P3--tower reactor recycle pump
E3--reactive distillation system reboiler
P4--reactive distillation system discharging pump
R1--transesterification reaction system
P5--transesterification reaction system discharging pump
R2--prepolymerization reaction system
P6--prepolymerization reaction system discharging pump
The horizontal stirring reaction system of R3--
The horizontal stirring reaction system discharging pump of P7--
R4--is poly-reactive system eventually
P8--is poly-reactive system discharging pump eventually
T2--lighting end recovery system
Z--granulating system.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, so that the technician of this area more understands
The present invention, but therefore do not limit the present invention.
With 50,000 tons/year of polycarbonate production techniques, the present invention is further described:
Before charging, all device nitrogen is replaced, and uses nitrogen protecting system.
(1) the mixing of materials stage
A, to charging surge tank transporting molten dihydroxyphenyl propane, flow set is that 5611kg/h runs automatically; Setting diphenyl carbonate and dihydroxyphenyl propane raw materials components mole ratio 1:1.08, melting diphenyl carbonate charging amount is with dihydroxyphenyl propane feed variation; After charging surge tank has liquid level, open batch mixing recycle pump, mixing of materials evenly and is delivered to batch mixing preheater, material is heated up, and control mixture temperature at 170 DEG C ~ 180 DEG C, the volume of charging surge tank must ensure that material has the residence time of 2.5 hours when reaching control liquid level, to mix;
B, when charging surge tank liquid level reaches operation value bottom limit level meter 65%, open batch mixing fresh feed pump, and slowly adjust feed rate to 10487kg/h, batch mixing charging amount and charging surge tank level set are interlocked, by adjustment batch mixing charging amount to ensure charging surge tank level stability simultaneously;
C, batch mixing mix in entry mixers with catalyst phenol solution feed, and setting catalyst charge amount and batch mixing charging amount mass ratio are 1:4.8, and catalyst charge amount adjusts automatically with batch mixing charging amount; Batch mixing containing catalyzer enters feed preheater and carries out heat exchange, and controls temperature out and reach 190 DEG C, and after heat exchange, batch mixing enters reactive distillation system.
(2) reactive distillation and the transesterification reaction stage
A, reactive distillation system pressure control-79 ~-82KPa, bottom temperature 195 ~ 200 DEG C, tower top temperature 110 DEG C ~ 120 DEG C, reflux ratio 2:1 ~ 1:1; Select the mode of reactive distillation, be more conducive to the separation of by-product phenol, transesterification reaction can be carried out faster; Reactive distillation system tower reactor has enough volumes, ensures batch mixing in residence time of tower reactor at more than 3h, so that material can fully react; The temperature of control tower reactor is to ensure to have a certain amount of phenol after the reaction in material; Tower top light constituent is delivered to the process of light constituent recovery system;
B, transesterification reaction system pressure control-85 ~-90KPa, temperature 205 ~ 210 DEG C, when liquid level there be not stirring arm more than 20%, opens and stirs; And ensure that normal running liquid level is at the 60% ~ 65% of liquidometer, to guarantee that residence time of material is at more than 3h, material has the enough reaction times; In system, light constituent is delivered to the process of light constituent recovery system from top.
(3) the prepolymerization reaction stage
Pressure-94KPa when a, prepolymerization reaction system initial charge, temperature 230 ~ 235 DEG C, opens when liquid level is more than 15% and stirs, and within every 20 minutes simultaneously, reducing pressure 1KPa until reaching-97KPa, continuing to be fed to normal running liquid level at the 60% ~ 65% of liquidometer; Prepolymerization reaction system has enough volumes, ensures that the residence time of batch mixing in system is at more than 1.5h, so that material can fully react; In system, light constituent is delivered to the process of light constituent recovery system from top;
Pressure-97KPa when b, horizontal stirring reaction system initial charge, temperature 270 ~ 275 DEG C, opens when liquid level is more than 15% and stirs, and within every 15 minutes simultaneously, reducing pressure 0.5KPa until reaching-99KPa, continuing to be fed to normal running liquid level at the 75% ~ 80% of liquidometer; Horizontal stirring reaction system has enough volumes, ensures that the residence time of batch mixing in system is at more than 2.5h, so that material can fully react; In system, light constituent is delivered to the process of light constituent recovery system from top.
(4) step of reaction is gathered eventually
Pressure-99.5KPa during poly-reactive system initial charge eventually, temperature 285 ~ 290 DEG C, opens when liquid level is more than 15% and stirs, and within every 15 minutes simultaneously, reducing pressure 0.05KPa until reaching-99.8KPa, continuing to be fed to normal running liquid level at the 75% ~ 80% of liquidometer; Horizontal stirring reaction system has enough volumes, ensures that the residence time of batch mixing in system is at more than 3.5h, so that material can fully react; In system, light constituent is delivered to the process of light constituent recovery system from top;
Poly-reacting rear material is delivered to granulating system granulation and forms product eventually.
The light constituent composition that every one-phase produces is different, and reactive distillation system light constituent carries separately light constituent recovery system to process; Transesterify system and precondensation system light constituent merge conveying light constituent recovery system process; Horizontal stirring reaction system and eventually poly-reactive system light constituent merging are delivered to the process of light constituent recovery system.
Claims (7)
1. a polycarbonate industrial process, it is characterised in that: taking diphenyl carbonate and dihydroxyphenyl propane as raw material production polycarbonate, comprise the following steps:
A, diphenyl carbonate and dihydroxyphenyl propane are with the ratio of mol ratio 1.:1.05 ~ 1:1.1, enter charging surge tank (V1), it is delivered to batch mixing preheater (E1) circulation by batch mixing recycle pump (P1) to heat and mix, charging surge tank (V1) interior temperature controls at 170 DEG C ~ 180 DEG C, Liquid level is the 65% ~ 75% of liquidometer, and feed time is controlled to 2h ~ 2.5h; Open batch mixing fresh feed pump (P2), by charging surge tank (V1) interior mass transport to entry mixers (M1); The phenol solution of catalyzer and the mass ratio of mixture are the ratio of 1:4.7 ~ 1:4.8, enter entry mixers (M1) respectively, after mixing, material enters reactive distillation system (T1) after being heated by feed preheater (E2), and feed preheater (E2) exports mixture temperature and controls at 190 DEG C ~ 195 DEG C; Mixture enters reactive distillation system (T1) and reaches the 70% ~ 75% of controlling valu liquidometer to reactive distillation system (T1) tower reactor liquid level, and required time is 3h;
B, reactive distillation system (T1) pressure-controlling-79 ~-82KPa, bottom temperature 195 ~ 200 DEG C, tower top temperature 110 DEG C ~ 120 DEG C, reflux ratio 2:1 ~ 1:1, the phenol that tower top obtains contains a small amount of diphenyl carbonate mass transport and processes to lighting end recovery system (T2); Tower reactor Liquid level is the 70% ~ 75% of liquidometer, and the material part through preliminary transesterification reaction is delivered to reactive distillation system reboiler (E3) heat exchange by tower reactor recycle pump (P3), and returns tower reactor; Another part kettle material is delivered to transesterification reaction system (R1) by reactive distillation system discharging pump (P4) and continues transesterification reaction; Material enters transesterification reaction system (R1) and reaches the 60% ~ 65% of values for normal operation liquidometer to transesterification reaction system (R1) liquid level, and required time is 3h;
C, transesterification reaction system (R1) pressure-controlling-85 ~-90KPa, temperature 205 ~ 210 DEG C, open when liquid level is more than 20% and stir, and ensure that normal running liquid level is at the 60% ~ 65% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system (T2) from reactive system top, opens transesterification reaction system discharging pump (P5) to prepolymerization reaction system (R2) charging; Material enters prepolymerization reaction system (R2) and reaches the 60% ~ 65% of values for normal operation liquidometer to prepolymerization reaction system (R2) liquid level, and required time is 1.5h;
-97KPa when the initial-94KPa of d, prepolymerization reaction system (R2) pressure progressively drops to normal running, temperature 230 ~ 235 DEG C, open when liquid level is more than 15% and stir, and ensure that normal running liquid level is at the 60% ~ 65% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system (T2) from reactive system top, opens prepolymerization reaction system discharging pump (P6) to the charging of horizontal stirring reaction system (R3); Material enters horizontal stirring reaction system (R3) to horizontal stirring reaction system (R3) liquid level and reaches values for normal operation liquidometer 75% ~ 80%, and required time is 2.5h;
Initial-the 97KPa of e, horizontal stirring reaction system (R3) pressure progressively drops to normal running-99KPa, temperature 270 ~ 275 DEG C, open when liquid level is more than 15% and stir, stirring velocity 2r/min also progressively increases to values for normal operation 4r/min, ensure that normal running liquid level is at the 75% ~ 80% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system (T2) from reactive system top, opens horizontal stirring reaction system discharging pump (P6) to poly-reactive system (R4) charging eventually; Material enters poly-reactive system (R4) eventually and reaches values for normal operation liquidometer 75% ~ 80% to poly-reactive system (R4) liquid level eventually, and required time is 3.5h;
F, the eventually initial-99.5KPa of poly-reactive system (R4) pressure progressively drop to normal running-99.8KPa, temperature 285 ~ 290 DEG C, open when liquid level is more than 15% and stir, stirring velocity 1r/min also progressively increases to values for normal operation 2r/min, ensure that normal running liquid level is at the 75% ~ 80% of liquidometer, a small amount of light constituent is delivered to lighting end recovery system (T2) from reactive system top, opens poly-reactive system discharging pump (P8) eventually and polycarbonate is delivered to granulating system (Z).
2., by method described in claim 1, it is characterized in that: in claim 1 step b, in reactive distillation system (T1) kettle material, phenol mass content is 8% ~ 10%.
3. by method described in claim 1, it is characterized in that: in claim 1 steps d ,-97KPa when the initial-94KPa of prepolymerization reaction system (R2) pressure progressively drops to normal running, its method reduces pressure 1KPa until reaching values for normal operation in every 20 minutes.
4. by method described in claim 1, it is characterized in that: in claim 1 step e,-99KPa when the initial-97KPa of horizontal stirring reaction system (R3) pressure progressively drops to normal running, its method reduces pressure 0.5KPa until reaching values for normal operation in every 15 minutes.
5. by method described in claim 1, it is characterized in that: in claim 1 step e, horizontal stirring reaction system (R3) stirring velocity 2r/min also progressively increases to values for normal operation 4r/min, and its method increases 0.5r/min until reaching values for normal operation in every 15 minutes.
6. by method described in claim 1, it is characterized in that: in claim 1 step f,-99.8KPa when the initial-99.5KPa of poly-reactive system (R4) pressure progressively drops to normal running eventually, its method reduces pressure 0.05KPa until reaching values for normal operation in every 15 minutes.
7. by method described in claim 1, it is characterized in that: in claim 1 step f, gather reactive system (R4) stirring velocity 1r/min eventually and progressively increase to values for normal operation 2r/min, its method increases 0.25r/min until reaching values for normal operation in every 15 minutes.
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| CN108789913A (en) * | 2018-06-20 | 2018-11-13 | 北京濮源新材料技术研究院(普通合伙) | Raw material blending device and hybrid technique for continuous production makrolon |
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