CN204958762U - Ionic liquid catalysis transesterification preparation diphenyl carbonate's device - Google Patents
Ionic liquid catalysis transesterification preparation diphenyl carbonate's device Download PDFInfo
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- CN204958762U CN204958762U CN201520753988.9U CN201520753988U CN204958762U CN 204958762 U CN204958762 U CN 204958762U CN 201520753988 U CN201520753988 U CN 201520753988U CN 204958762 U CN204958762 U CN 204958762U
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Abstract
This device discloses an ionic liquid catalysis transesterification preparation diphenyl carbonate's device, including reaction - rectifying column, first reboiler, first condenser, disproportionation ware, second condensing tower, distillation column, light component tower and product tower, export of reaction - rectifying column top of the tower and first condenser entry linkage, the export of first condenser divide into two branch roads, respectively with waste liquor recovery jar and reaction - rectifying column, export of reaction - rectification tata cauldron and disproportionation ware entry linkage, export of disproportionation ware top and second condenser entry linkage, the export of second condenser divide into two branch roads, be connected with waste liquor recovery jar and disproportionation ware respectively, export of disproportionation ware bottom and distillation column entry linkage, export of distillation column top and light component tower entry linkage, export and product tower entry linkage at the bottom of the light component tata. This device simple structure, easy operation, but serialization production can make result diphenyl carbonate's productivity >= 80%, purity >= 99.6%.
Description
Technical field
The utility model relates to a kind of organic synthesis plant, is specifically related to the device that a kind of ionic liquid-catalyzed transesterification reaction prepares diphenyl carbonate.
Background technology
The traditional method of current production polycarbonate is phosgenation, although this method technical maturity, good product quality, owing to employing the phosgene of severe toxicity, does not meet the inherent requirement of Green Chemistry, eliminated gradually.And be expected to progressively replace phosgenation with the novel process that diphenyl carbonate and dihydroxyphenyl propane are raw material production polycarbonate.Environment-friendly advantage that this technique is given prominence to because of it has competitive power in the production of polycarbonate.Developed country blocks very tight to the relevant advanced manufacturing technology of polycarbonate industrial chain and starting material." 15 " and the Eleventh Five-Year Plan period, based on the achievement in research of Mianyang, Sichuan morning twilight chemical research institute, domestic Duo Jia large and medium-sized enterprise is just at planning polycarbonate large production equipment, but enter the less of substantive construction period, trace it to its cause in market study process, find the domestic critical materials diphenyl carbonate lacking non-phosgene synthesis polycarbonate exactly, China there is no reliably, batch diphenyl carbonate product-feed source.China does not have diphenyl carbonate large-scale production technology that is ripe, that have independent intellectual property right; this objective reality constrains the development of China's polycarbonate industry, and this also makes the related process of Development and Production diphenyl carbonate become the focal issue of investigator's concern.
As the eco-friendly catalyzer of a class, acidic ion liquid not only have liquid acid good fluidity, acid site density is large and strength of acid is high and the advantage such as to be evenly distributed, also there is easily separated, the characteristic that can be recycled of solid acid, be successfully applied to some transesterification reaction.
Summary of the invention
Goal of the invention: the utility model object is for the deficiencies in the prior art, provides a kind of ionic liquid-catalyzed transesterification reaction to prepare the device of diphenyl carbonate.
Technical scheme: a kind of ionic liquid-catalyzed transesterification reaction prepares the device of diphenyl carbonate, comprises reaction rectification tower, reboiler, the first condenser, disproportionation reactor, the second condensing tower, distillation tower, lights column and product tower, the head tank of phenol and the head tank outlet of methylcarbonate are connected with described reaction rectification tower entrance, described reaction rectification column overhead outlet is connected with described first condenser inlet, described first condensator outlet is divided into two branch roads, article one, branch road is connected with devil liquor recovery tank entrance, partial reflux liquid is led back to reaction rectification tower by another branch road, described reaction rectification tower tower reactor outlet is connected with described disproportionation reactor entrance, described disproportionation reactor top exit and described second condenser inlet, described second condensator outlet is divided into two branch roads, article one, branch road is connected with devil liquor recovery tank entrance, another branch road is connected with described disproportionation reactor entrance, described disproportionation reactor outlet at bottom is connected with described distillation tower entrance, described distillation tower top exit is connected with described lights column entrance, described lights column tower bottom outlet is connected with described product tower entrance.
Preferably, for avoiding raw material to reduce reactive behavior because of cooling, the second reboiler between described disproportionation reactor with described distillation tower, is connected.
Preferably, for promoting the counter current contact of raw material, catalyzer, improve and reaction rectification tower described in transesterify efficiency arranges starting phenol and catalyst inlet and methylcarbonate material inlet, described starting phenol and catalyst inlet are arranged at the middle and upper part of described reaction rectification tower, and described methylcarbonate material inlet is arranged at the middle and lower part of described reaction rectification tower.
Preferably, for improving manipulation accuracy, simplify the operation flow process, and described reaction rectification tower, the first reboiler, the first condenser, disproportionation reactor, the second condensing tower, distillation tower, lights column are connected by DCS Controlling System with product tower.
Beneficial effect: (1) this device, by arranging pressurization transesterification reaction-rectifier unit and decompression disproportionation reaction-rectifier unit, can make productive rate >=80% of product diphenyl carbonate, purity >=99.6%; (2) this apparatus structure is simple, easy to operate, can be continuously produced, and improves productive rate.
Accompanying drawing explanation
Fig. 1 is the gas chromatogram of the first step transesterification reaction tower bottoms in embodiment 1;
Fig. 2 is the gas chromatogram after thick product diphenyl carbonate in embodiment 1 after disproportionation reaction is dissolved in methyl alcohol;
Fig. 3 is that in embodiment 1, sterling diphenyl carbonate is dissolved in the gas chromatogram after methyl alcohol;
Fig. 4 is diphenyl carbonate in embodiment 1
1hNMR spectrogram;
Fig. 5 is the utility model device schema;
Wherein, 1. reaction rectification tower, 2. reboiler, 3. the first condenser, 4. disproportionation reactor, 5. the second condensing tower, 6. distillation tower, 7. lights column, 8. product tower, 9. the second reboiler.
Embodiment
Below by accompanying drawing, technical solutions of the utility model are described in detail, but protection domain of the present utility model is not limited to described embodiment.
Embodiment 1: the device preparing diphenyl carbonate for ionic liquid-catalyzed transesterification reaction, comprises reaction rectification tower 1, reboiler 2, first condenser 3, disproportionation reactor 4, second condensing tower 5, distillation tower 6, lights column 7 and product tower 8, the head tank of phenol and the head tank outlet of methylcarbonate are connected with described reaction rectification tower 1 entrance, described reaction rectification tower 1 tower top outlet is connected with described first condenser 3 entrance, described first condenser 3 outlet is divided into two branch roads, article one, branch road is connected with devil liquor recovery tank entrance, partial reflux liquid is led back to reaction rectification tower 1 by another branch road, described reaction rectification tower 1 tower reactor outlet is connected with described disproportionation reactor 4 entrance, described disproportionation reactor 4 top exit and described second condenser 5 entrance, described second condenser 5 outlet is divided into two branch roads, article one, branch road is connected with devil liquor recovery tank entrance, another branch road is connected with described disproportionation reactor 4 entrance, described disproportionation reactor 4 outlet at bottom is connected with described second reboiler 9 entrance, described second reboiler 9 outlet is connected with described distillation tower 6 entrance, described distillation tower 6 top exit is connected with described lights column 7 entrance, described lights column 7 tower bottom outlet is connected with described product tower 8 entrance.
For promoting the counter current contact of raw material, catalyzer, improve on reaction rectification tower described in transesterify efficiency and starting phenol and catalyst inlet a and methylcarbonate material inlet b are set, described starting phenol and catalyst inlet are arranged at the middle and upper part of described reaction rectification tower, and described methylcarbonate material inlet is arranged at the middle and lower part of described reaction rectification tower; For improving manipulation accuracy, simplify the operation flow process, and described reaction rectification tower, the first reboiler, the first condenser, disproportionation reactor, the second condensing tower, distillation tower, lights column are connected by DCS Controlling System with product tower.
The method utilizing said apparatus to carry out ionic liquid-catalyzed transesterification reaction to prepare diphenyl carbonate, specifically comprises the steps:
(1) phenol and methylcarbonate are at [MimN (CH
2)
4sO
3h] [HSO
4] carry out compressive reaction-rectifying under ionic-liquid catalyst condition and grasped, methyl phenyl carbonate and methyl alcohol is obtained after transesterification reaction, the feed ratio of phenol and methylcarbonate is 4, catalyst loading is the 1wt% of phenol and methylcarbonate total amount, and in compressive reaction-rectifying, pressure is 1.5MPa, and the reaction times is 1.5h, described compressive reaction-rectifying is carried out in rectifying tower, rectifying bottom temperature is 220 DEG C, and tower top temperature is 163 DEG C, and reflux ratio is 10; Concrete reaction mechanism is as follows:
(2) methyl phenyl carbonate will prepared in step (1), in disproportionation reactor, Depressor response operation is carried out under the catalytic condition of ionic-liquid catalyst, final product diphenyl carbonate is obtained after disproportionation reaction, catalyst loading is the 1wt% dropping into methyl phenyl carbonate amount, vacuum tightness in Depressor response process is 0.065MPa, temperature of reaction is 190 DEG C, and the reaction times is 4h; Concrete reaction mechanism is as follows:
(3) the end reaction liquid that step (2) obtains is distilled under vacuum tightness 6mmHg condition, collect and obtain methyl phenyl carbonate product.
Fig. 1 is the gas chromatogram of the first step transesterification reaction tower bottoms, as can be seen from Figure, the first step transesterification reaction successfully synthesizes methyl phenyl carbonate, phenol conversion can reach 99.8%, methyl phenyl carbonate selectivity is 88.8%, the selectivity of this step diphenyl carbonate reaches 9.8%, and the selectivity of by product methyl-phenoxide is less than 1%.
Fig. 2 is that after disproportionation reaction, thick product diphenyl carbonate is dissolved in the gas chromatogram after methyl alcohol, and disproportionation reaction successfully synthesizes diphenyl carbonate as can be seen from Figure, and diphenyl carbonate productive rate can reach 82.8%.
Fig. 3 is the gas chromatogram after sterling diphenyl carbonate is dissolved in methyl alcohol, and diphenyl carbonate purity can reach 99.7%.
Fig. 4 is sterling diphenyl carbonate
1hNMR spectrogram, successfully synthesize diphenyl carbonate, and result is consistent with gas-chromatography test result by figure can find out.
Embodiment 2: the reaction unit in the present embodiment is in the same manner as in Example 1, specifically comprises the following steps:
(1) phenol and methylcarbonate are at [(C
2h
5)
3n (CH
2)
4sO
3h] [HSO
4] carry out compressive reaction-rectifying under ionic-liquid catalyst condition and grasped, methyl phenyl carbonate and methyl alcohol is obtained after transesterification reaction, the feed ratio of phenol and methylcarbonate is 1, catalyst loading is the 0.5wt% of phenol and methylcarbonate total amount, and in compressive reaction-rectifying, pressure is 0.5MPa, and the reaction times is 1h, described compressive reaction-rectifying is carried out in rectifying tower, rectifying bottom temperature is 200 DEG C, and tower top temperature is 160 DEG C, and reflux ratio is 8; Concrete reaction mechanism is as follows:
(2) methyl phenyl carbonate will prepared in step (1), in disproportionation reactor, Depressor response operation is carried out under the catalytic condition of ionic-liquid catalyst, final product diphenyl carbonate is obtained after disproportionation reaction, catalyst loading is the 0.5wt% dropping into methyl phenyl carbonate amount, vacuum tightness in Depressor response process is 0.05MPa, temperature of reaction is 160 DEG C, and the reaction times is 3h; Concrete reaction mechanism is as follows:
(3) the end reaction liquid that step (2) obtains is distilled under vacuum tightness 5mmHg condition, collect and obtain methyl phenyl carbonate product.
In the present embodiment the first step, phenol conversion can reach 99.7%, and the productive rate of product diphenyl carbonate is 81.9%, and final product diphenyl carbonate purity can reach 99.6%.
Embodiment 3: the reaction unit in the present embodiment is in the same manner as in Example 1, specifically comprises the following steps:
(1) phenol and methylcarbonate are at [(CH
3)
3n (CH
2)
4sO
3h] [HSO
4] carry out compressive reaction-rectifying under ionic-liquid catalyst condition and grasped, methyl phenyl carbonate and methyl alcohol is obtained after transesterification reaction, the feed ratio of phenol and methylcarbonate is 5, catalyst loading is the 2wt% of phenol and methylcarbonate total amount, and in compressive reaction-rectifying, pressure is 2.5MPa, and the reaction times is 3h, described compressive reaction-rectifying is carried out in rectifying tower, rectifying bottom temperature is 250 DEG C, and tower top temperature is 165 DEG C, and reflux ratio is 11; Concrete reaction mechanism is as follows:
(2) methyl phenyl carbonate will prepared in step (1), in disproportionation reactor, Depressor response operation is carried out under the catalytic condition of ionic-liquid catalyst, final product diphenyl carbonate is obtained after disproportionation reaction, catalyst loading is the 2wt% dropping into methyl phenyl carbonate amount, vacuum tightness in Depressor response process is 0.07MPa, temperature of reaction is 200 DEG C, and the reaction times is 6h; Concrete reaction mechanism is as follows:
(3) the end reaction liquid that step (2) obtains is distilled under vacuum tightness 7mmHg condition, collect and obtain methyl phenyl carbonate product.
In the present embodiment the first step, phenol conversion can reach 99.65%, and the productive rate of product diphenyl carbonate is 81.5%, and final product diphenyl carbonate purity can reach 99.63%.
Embodiment 4 is identical with reaction unit with the implementation method of embodiment 1, and its difference is that the present embodiment intermediate ion liquid catalyst is [MimN (CH
2)
4sO
3h] [TsO], in the present embodiment the first step, phenol conversion can reach 99.68%, and the productive rate of product diphenyl carbonate is 80.9%, and final product diphenyl carbonate purity can reach 99.62%.
Embodiment 5 is identical with reaction unit with the implementation method of embodiment 1, and its difference is that the present embodiment intermediate ion liquid catalyst is [PyN (CH
2)
4sO
3h] [HSO
4] phenol conversion can reach 99.67% in the present embodiment the first step, the productive rate of product diphenyl carbonate is 80.6%, and final product diphenyl carbonate purity can reach 99.65%.
Embodiment 6 is identical with reaction unit with the implementation method of embodiment 1, and its difference is that the present embodiment intermediate ion liquid catalyst is [PyN (CH
2)
4sO
3h] phenol conversion can reach 99.62% in [TsO] the present embodiment the first step, and the productive rate of product diphenyl carbonate is 81.1%, and final product diphenyl carbonate purity can reach 99.61%.
Embodiment 7 is identical with reaction unit with the implementation method of embodiment 1, and its difference is that the present embodiment intermediate ion liquid catalyst is [PyN (CH
2)
4sO
3h] phenol conversion can reach 99.63% in [MsO] the present embodiment the first step, and the productive rate of product diphenyl carbonate is 81.3%, and final product diphenyl carbonate purity can reach 99.61%.
Embodiment 8 is identical with reaction unit with the implementation method of embodiment 1, and its difference is that the present embodiment intermediate ion liquid catalyst is [PyN (CH
2)
4sO
3h] phenol conversion can reach 99.64% in [AcO] the present embodiment the first step, and the productive rate of product diphenyl carbonate is 81.0%, and final product diphenyl carbonate purity can reach 99.63%.
As mentioned above, although represented with reference to specific preferred embodiment and described the utility model, it shall not be construed as the restriction to the utility model self.Under the spirit and scope prerequisite of the present utility model not departing from claims definition, various change can be made in the form and details to it.
Claims (4)
1. ionic liquid-catalyzed transesterification reaction prepares a device for diphenyl carbonate, it is characterized in that comprising reaction rectification tower, the first reboiler, the first condenser, disproportionation reactor, the second condensing tower, distillation tower, lights column and product tower, the head tank of phenol and the head tank outlet of methylcarbonate are connected with described reaction rectification tower entrance, described reaction rectification column overhead outlet is connected with described first condenser inlet, described first condensator outlet is divided into two branch roads, article one, branch road is connected with devil liquor recovery tank entrance, partial reflux liquid is led back to reaction rectification tower by another branch road, described reaction rectification tower tower reactor outlet is connected with described disproportionation reactor entrance, described disproportionation reactor top exit and described second condenser inlet, described second condensator outlet is divided into two branch roads, article one, branch road is connected with devil liquor recovery tank entrance, another branch road is connected with described disproportionation reactor entrance, described disproportionation reactor outlet at bottom is connected with described distillation tower entrance, described distillation tower top exit is connected with described lights column entrance, described lights column tower bottom outlet is connected with described product tower entrance.
2. ionic liquid-catalyzed transesterification reaction prepares the device of diphenyl carbonate according to claim 1, it is characterized in that being connected the second reboiler between described disproportionation reactor with described distillation tower.
3. ionic liquid-catalyzed transesterification reaction prepares the device of diphenyl carbonate according to claim 1, it is characterized in that described reaction rectification tower is arranged starting phenol and catalyst inlet and methylcarbonate material inlet, described starting phenol and catalyst inlet are arranged at the middle and upper part of described reaction rectification tower, and described methylcarbonate material inlet is arranged at the middle and lower part of described reaction rectification tower.
4. ionic liquid-catalyzed transesterification reaction prepares the device of diphenyl carbonate according to claim 1, it is characterized in that described reaction rectification tower, the first reboiler, the first condenser, disproportionation reactor, the second condensing tower, distillation tower, lights column are connected by DCS Controlling System with product tower.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977401A (en) * | 2017-04-28 | 2017-07-25 | 濮阳市宏源石油化工有限公司 | Using ionic liquid as the method for accelerator diphenyl carbonate synthesis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977401A (en) * | 2017-04-28 | 2017-07-25 | 濮阳市宏源石油化工有限公司 | Using ionic liquid as the method for accelerator diphenyl carbonate synthesis |
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