CN102407090B - Device and method for lowering influences of sublimates on reaction - Google Patents
Device and method for lowering influences of sublimates on reaction Download PDFInfo
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- CN102407090B CN102407090B CN201110318150.3A CN201110318150A CN102407090B CN 102407090 B CN102407090 B CN 102407090B CN 201110318150 A CN201110318150 A CN 201110318150A CN 102407090 B CN102407090 B CN 102407090B
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Abstract
The invention discloses a device and method for lowering influences of sublimates on a reaction, and the reaction device is characterized in that a reactor is connected with a heat exchanger, a refrigerant and a heating medium are connected with the heat exchanger through a refrigerant-heating medium conveyor pipeline, and the refrigerant and the heating medium are controlled to circulate in the heat exchanger by a control switch. The preparation method comprises the following steps of: introducing the refrigerant in the heat exchanger before material sublimation temperature is reached, and introducing the heat medium in the heat exchanger to enable the sublimates in the heat exchanger to be refluxed in the reactor after the sublimation temperature is reached for a while. The device and method for lowering influences of sublimates on a reaction have the advantages that: the problem that sublimates and oligomers can block the pipe opening of a condenser can be effectively solved, the accuracy in formula design can be improved, the cleaning frequency of the reactor condenser can be reduced, and the smooth operation of preparation each time can be ensured.
Description
Technical field
The present invention relates to a kind of device of easy sublimate on reaction impact that reduce, the present invention also provides a kind of method of easy sublimate on reaction impact that reduce.
Background technology
Polymerisation is the basic chemical method of the multiple organic synthesis material of preparation, and its reaction unit is generally made up of reactor, material steam pipe, condenser, feed back pipe and cooling water system.Because polymerisation mostly is exothermic reaction, in polymerization process, in the time having easy distillation material in the raw material adding, along with reaction temperature exceedes the sublimation temperature of this material, it can produce distillation phenomenon.General sublimate can be sublimated in the condenser of reactor, light affect the accuracy of reaction ratio, heavy as in LCP production process, the oligomer being distilled out of in sublimate and course of reaction can condense in the condenser mouth of pipe, cause the low molecule of generation to discharge, the product degree of polymerization is very low.
Summary of the invention
The invention provides a kind of apparatus and method of easy sublimate on reaction impact that reduce.
In order to reach above object, the present invention has adopted following technical scheme, described reaction unit is that a reactor connects heat exchanger, refrigerant is connected with heat exchanger by cold and hot matchmaker's feed-line with heating agent, and its cold and hot matchmaker circulation in heat exchanger of suspension control switch control.
In addition, described gauge tap is timing change-over switch, and connects refrigerant and heating agent, and cold and hot matchmaker's switching is by the control of timing change-over switch, and timing can be according to the sublimation condition adjustment of different material; Described heat exchanger is one-level, secondary or multi-stage heat-exchanger.
Its preparation process comprises: in the time that heat exchanger is one-level heat exchanger, heat exchanger is reaching before the sublimation temperature of raw material logical refrigerant, reach after sublimation temperature certain hour, heat exchanger is switched to logical heating agent sublimate, oligomer in heat exchanger are back in reactor.
In the time that heat exchanger is two-stage heat exchanger, I and II heat exchanger, reaching logical refrigerant before the sublimation temperature of raw material, reaches after sublimation temperature certain hour, and one-level heat exchanger leads to heating agent, and two-stage heat exchanger leads to refrigerant; After gathering certain sublimate in heat exchanger, switch to the logical refrigerant of one-level heat exchanger, the logical heating agent of two-stage heat exchanger makes the sublimate in two-stage heat exchanger be back to one-level heat exchanger; After two-stage heat exchanger refluxes, one-level heat exchanger being adjusted into logical heating agent state is back in reactor the sublimate in one-level heat exchanger.
Cold and hot matchmaker's temperature range between-40 ℃～400 ℃, preferably 0 ℃～330 ℃.
Above reactor, connect two-stage heat exchanger, cold and hot matchmaker is switched in heat exchanger timing, easy sublimate and oligomer are refluxed back in reactor, can switch the heating agent of heat exchanger and make it to be back to reactor according to the working condition in reactor like this, thereby prevent that sublimate is collected in heat exchanger.This reaction unit is timing change-over switch and cold and hot matchmaker's feed-line also, and timing change-over switch connects cold and hot matchmaker, cold and hot matchmaker's switching is by the control of timing change-over switch, timing capable of regulating, its cold and hot matchmaker's temperature between-40 ℃～400 ℃, preferably 0 ℃～330 ℃, like this, thereby the external condition that can adjust according to the cold and hot medium in the response situation adjustment heat exchanger in reactor whole reaction system, comprises reaction temperature, concentration of component.
The apparatus and method of the easy sublimate of reduction of the present invention on reaction impact, its advantage is: the problem that can effectively solve sublimate thing and the oligomer obstruction condenser mouth of pipe, improve the accuracy of formula Design, reduce the clearing times of reactor condenser, guaranteed carrying out smoothly of each preparation; Above reactor, connect two-stage heat exchanger, heat exchanger shell side timing for cutting changes cold and hot matchmaker, and easy sublimate and oligomer are refluxed back in reactor, has reduced the easily impact of sublimate on reaction formula in raw material.
Accompanying drawing explanation
Fig. 1 is the structural representation of reaction unit.
The specific embodiment
Below by the specific embodiment, the present invention is described, but is not limited to this.
The device of the easy sublimate of described reduction on reaction impact, comprises that a reactor 1 connects heat exchanger 2, refrigerant 4 and heating agent 5 and is connected with heat exchanger 2 by cold and hot matchmaker's feed-line 6, and suspension control switch 3 is controlled its cold and hot matchmaker circulation in heat exchanger 2; Described gauge tap 3 is timing change-over switch, and connects refrigerant 4 and heating agent 5, and cold and hot matchmaker's switching is controlled by timing change-over switch 3, and timing can be according to the sublimation condition adjustment of different material; Described heat exchanger 2 also can be secondary or multi-stage heat-exchanger.
Embodiment 1:
In 20L reactor, add the raw material of the generation liquid crystal that 6kg contains terephthalic acid (TPA), temperature reaction, the logical refrigerant of I and II heat exchanger in temperature-rise period, when temperature reaches 300 ℃ of logical heating agents of one-level heat exchanger after 10 minutes, two-stage heat exchanger leads to refrigerant; After 10 minutes, switch to the logical refrigerant of one-level heat exchanger, two-stage heat exchanger leads to heating agent; After the cold and hot matchmaker's exchange of two-stage heat exchanger in 10 minutes.32 ℃ of refrigerant temperatures during this time, 300 ℃ of heat medium temperatures, are warming up to 350 ℃ of reactions discharging in 1 hour, take condenser system apart, find that condenser tube side is substantially without buildup, continuous polymerization 3 times, condenser tube side is substantially without buildup.
Comparative example 1:
In 20L reactor, add the raw material of the generation liquid crystal that 6kg contains terephthalic acid (TPA), temperature reaction, the logical cooling water of condenser shell side in temperature-rise period, is warming up to 350 ℃ of reactions discharging in 1 hour.Take condenser system apart, find that condenser tube side buildup is a lot, caliber diminishes.Continuous polymerization 3 times, condenser tube side stops up.
Can find by embodiment and comparative example, adopt and reduce easy sublimate to reacting in the reactor after the device affecting, reactant and the product gathered greatly reduce, can find out the condenser system of nursing one's health through cold and hot matchmaker, the shortcoming that the line clogging that the reactant of can fully avoiding easily distilling brings or reactant composition concentration reduce, and make course of reaction more balanced.
Claims (4)
1.
oneplant and reduce the method for easy sublimate on reaction impact, its operating procedure comprises: a. heat exchanger is two-stage heat exchanger, I and II heat exchanger (2) is reaching before the sublimation temperature of raw material logical refrigerant (4), reach after sublimation temperature certain hour, one-level heat exchanger leads to heating agent (5), and two-stage heat exchanger leads to refrigerant (4); B. after gathering certain sublimate in two-stage heat exchanger (2), switch to the logical refrigerant (4) of one-level heat exchanger, the logical heating agent (5) of two-stage heat exchanger makes the sublimate in two-stage heat exchanger be back to one-level heat exchanger; C. after two-stage heat exchanger backflow, one-level heat exchanger being adjusted into logical heating agent state is back in reactor the sublimate in one-level heat exchanger.
2. a kind of method of easy sublimate on reaction impact that reduce according to claim 1, is characterized in that: cold and hot matchmaker's temperature range is between-40 ℃～400 ℃.
3. a kind of method of easy sublimate on reaction impact that reduce according to claim 1 is characterized in that: in step c, two-stage heat exchanger is adjusted to logical refrigerant state simultaneously.
4. a kind of method of easy sublimate on reaction impact that reduce according to claim 2, is characterized in that: cold and hot matchmaker's temperature range is 0 ℃～330 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110318150.3A CN102407090B (en) | 2011-10-19 | 2011-10-19 | Device and method for lowering influences of sublimates on reaction |
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| CN201110318150.3A CN102407090B (en) | 2011-10-19 | 2011-10-19 | Device and method for lowering influences of sublimates on reaction |
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| CN102407090A CN102407090A (en) | 2012-04-11 |
| CN102407090B true CN102407090B (en) | 2014-05-14 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4391617A (en) * | 1978-09-15 | 1983-07-05 | Way Peter F | Process for the recovery of vaporized sublimates from gas streams |
| US4406118A (en) * | 1972-05-12 | 1983-09-27 | Funk Harald F | System for treating and recovering energy from exhaust gases |
| US4435580A (en) * | 1982-05-03 | 1984-03-06 | The Badger Company, Inc. | Process for the production of phthalic anhydride |
| CN1046096C (en) * | 1993-11-30 | 1999-11-03 | 康姆普莱默私人公司 | A process for removing elemental sulfur from a gas stream |
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2011
- 2011-10-19 CN CN201110318150.3A patent/CN102407090B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4406118A (en) * | 1972-05-12 | 1983-09-27 | Funk Harald F | System for treating and recovering energy from exhaust gases |
| US4391617A (en) * | 1978-09-15 | 1983-07-05 | Way Peter F | Process for the recovery of vaporized sublimates from gas streams |
| US4435580A (en) * | 1982-05-03 | 1984-03-06 | The Badger Company, Inc. | Process for the production of phthalic anhydride |
| CN1046096C (en) * | 1993-11-30 | 1999-11-03 | 康姆普莱默私人公司 | A process for removing elemental sulfur from a gas stream |
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| CN102407090A (en) | 2012-04-11 |
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