CN215049780U

CN215049780U - Dual-purpose device for disproportionation and rectification

Info

Publication number: CN215049780U
Application number: CN202121286764.3U
Authority: CN
Inventors: 陈坤; 魏天荣; 於国伟; 孙苏红; 薛耘芸
Original assignee: Hubei Sanning Carbon Phosphorus Based New Material Industry Technology Research Institute Co ltd; Hubei Sanning Chemical Co Ltd
Current assignee: Hubei Sanning Carbon Phosphorus Based New Material Industry Technology Research Institute Co ltd; Hubei Sanning Chemical Co Ltd
Priority date: 2021-06-09
Filing date: 2021-06-09
Publication date: 2021-12-07
Anticipated expiration: 2031-06-09

Abstract

The utility model discloses a dual-purpose device for disproportionation and rectification, which comprises a reaction kettle, wherein the reaction kettle is a methyl phenyl carbonate disproportionation reactor, a material outlet at the top of the reaction kettle is connected with a feed inlet of a rectifying tower, the rectifying tower is also provided with a material inlet, the top of the rectifying tower is connected with a condenser through a pipeline, the condenser is connected with a separator through a pipeline, the separator is provided with two outlets, one outlet is connected with the rectifying tower through a pipeline, and the other outlet is connected with a first step reactor for ester exchange through a pipeline; the utility model discloses before not only reducing the disproportionation reaction, cauldron liquid preliminary treatment process reduces the input of equipment, and the required heat make full use of the disproportionated required heat of methyl phenyl carbonate of the required heat of cauldron liquid rectification has improved the utilization ratio of heat energy moreover, has reduced manufacturing cost.

Description

Dual-purpose device for disproportionation and rectification

Technical Field

The utility model relates to the field of chemical industry, specifically indicate a dual-purpose device of disproportionation and rectification.

Background

Diphenyl carbonate is an organic carbonate with wide application, can be used for synthesizing a plurality of organic intermediates, polycarbonate, plasticizer and solvent, and has wide application in the fields of electronics, electrics, glazing, sheets, automobile industry and the like; in addition, DPC is also used for synthesis of chemical products such as polyarylate, p-hydroxybenzoic acid polyester, monoisocyanate, and the like, and also as a plasticizer for polyamide and polyester, and has a wide range of applications in the fields of agricultural chemicals, medicines, and the like.

Due to environmental protection problems, the technical route of synthesizing diphenyl carbonate by ester exchange of dimethyl carbonate and phenol is the first choice. In order to improve the reaction conversion rate and the product yield, a proper method is adopted to break the chemical equilibrium limit, and Kim Won Bae proposes a process route for synthesizing diphenyl carbonate by a two-step method, namely, when the ester exchange reaction is carried out to a certain extent, the intermediate methyl phenyl carbonate is separated out to carry out disproportionation reaction independently, and similar process technologies are available in the patents US 5344954 and US 5426207.

However, the methyl phenyl carbonate rich in methyl is separated to carry out disproportionation reaction independently, and phenol and a small amount of dimethyl carbonate in the ester exchange kettle liquid need to be distilled under reduced pressure, so that not only is the process complicated, but also the production cost is increased.

Therefore, it is necessary to design a dual-purpose device for disproportionation and rectification to solve the above problems.

Disclosure of Invention

An object of the utility model is to overcome the aforesaid not enough, a dual-purpose device of disproportionation and rectification is provided, through the design that increases a plate rectifying column at disproportionation reation kettle, ester exchange cauldron liquid is gone into at rectifying column middle part pump, midbody methyl phenyl carbonate reacts in column plate and reactor and generates diphenyl carbonate, the required temperature of disproportionation provides the heat for the rectification of cauldron liquid, lead to reactor and rectifying column bottom enrichment methyl phenyl carbonate, the phenol of top enrichment and disproportionation product-dimethyl carbonate behind the condenser, collect in the separator, separate. Thus, the utilization rate of heat is improved, the cost is reduced, and the working procedure of separating phenol in advance is also reduced.

The utility model discloses a solve above-mentioned technical problem, the technical scheme who adopts is: the utility model provides a dual-purpose device of disproportionation and rectification, includes reation kettle, reation kettle is methyl phenyl carbonate disproportionation reactor, and reation kettle top material export links to each other with the rectifying column feed inlet, still is equipped with the material import on the rectifying column, and the rectifying column tower top links to each other with the condenser through the pipeline, the condenser passes through the pipeline and is connected with the separator, and the separator has two exports, and one of them export is passed through the pipeline and is connected with the rectifying column, and another export passes through the first step reactor of pipe connection ester exchange.

Preferably, a heating jacket is arranged outside the reaction kettle.

Preferably, a coaxial rotating and stirring mechanism is arranged in the reaction kettle, and a stirring paddle of the coaxial rotating and stirring mechanism is in a slant paddle type, an anchor type or a frame type.

Preferably, the rectifying column is a plate column, and the number of plates is 5 to 20.

Preferably, the condensing medium adopted by the condenser is circulating water with the temperature of 80-100 ℃.

Preferably, the condenser structure is in the form of a shell-and-tube condenser or a double-tube condenser.

Preferably, heat-preservation heating jackets are arranged on pipelines connected with the rectifying tower and the condenser, the condenser and the separator, and the separator and the rectifying tower.

The utility model has the advantages that:

1. before disproportionation reaction, a kettle liquid pretreatment procedure is reduced, and equipment investment is reduced;

2. the heat required by the rectification of the kettle liquid fully utilizes the heat required by the disproportionation of the methyl phenyl carbonate, thereby improving the utilization rate of heat energy and reducing the production cost;

3. chemical reaction occurs on each tower plate in the reaction section, and the total conversion rate of raw materials can be improved by increasing the total reaction volume;

4. low production cost and easy popularization and use.

Drawings

FIG. 1 is a schematic diagram of a dual-purpose apparatus for disproportionation and rectification;

in the figure, a reaction kettle 1, a rectifying tower 2, a condenser 3 and a separator 4.

Detailed Description

The invention is described in further detail below with reference to the figures and the embodiments.

As shown in figure 1, the dual-purpose device for disproportionation and rectification comprises a reaction kettle 1, wherein the reaction kettle 1 is a methyl phenyl carbonate disproportionation reactor, a material outlet at the top of the reaction kettle 1 is connected with a feed inlet of a rectification tower 2, the rectification tower 2 is also provided with a material inlet, and the material temperature is 100-160 ℃. 2 tops of towers of rectifying column are connected with condenser 3 through the pipeline, condenser 3 is connected with separator 4 through the pipeline, and separator 4 has two exports, and one of them export is connected with rectifying column 2 through the pipeline, and another export is through the first step reactor of pipe connection ester exchange. Part of the material flows back to the rectifying tower 2 through the separator 4, and part of the material is recycled to the first step reactor of the ester exchange.

In this embodiment, the reaction kettle 1 is a methyl phenyl carbonate disproportionation reactor, the kettle body is made of hastelloy or stainless steel or zirconium, nickel-based alloy or other composite materials, and the lining is made of polytetrafluoroethylene or enamel or PP.

Preferably, the reaction kettle 1 is externally provided with a heating jacket. The arrangement improves the heat preservation effect of the reaction kettle 1, and the external heating temperature of the reaction kettle 1 can reach 300 ℃ at most.

Preferably, a coaxial rotating and stirring mechanism is arranged in the reaction kettle 1, and a stirring paddle of the coaxial rotating and stirring mechanism is in a form of an oblique paddle type, an anchor type or a frame type.

Preferably, the rectification column 2 is a tray column having a tray number of 5 to 20.

Preferably, the condensing medium adopted by the condenser 3 is circulating water with the temperature of 80-100 ℃.

Preferably, the condenser 3 is in the form of a shell-and-tube condenser or a double-tube condenser, wherein the tubes are stainless steel, brass or pure copper.

Preferably, heat-preservation heating jackets are arranged on pipelines connected with the rectifying tower 2 and the condenser 3, the condenser 3 and the separator 4, and the separator 4 and the rectifying tower 2. The arrangement improves the heat preservation effect of the device, improves the utilization rate of heat energy and reduces the production cost.

The working principle of the embodiment is as follows: in this example, the main components of the bottoms obtained in the first step of transesterification of dimethyl carbonate and phenol were phenol, methyl phenyl carbonic acid, and small amounts of diphenyl carbonate and dimethyl carbonate. After preheating, the mixture is pumped to a feed inlet of a rectifying tower of the device, and the temperature of the materials in the reactor is set to be 100-230 ℃. The boiling point of the fraction at the top of the tower is controlled by controlling the feeding amount and the reflux amount of the separator, and the fraction is collected at the top of the tower. Part of the material collected by the separator is used as reaction raw material and is pumped into the first step of the ester exchange reactor through a pipeline.

The utility model discloses an increase the design of a board-like rectifying column at disproportionation reation kettle, ester exchange cauldron liquid is gone into at rectifying column middle part pump, and midbody methyl phenyl carbonate reacts in column plate and reactor and generates diphenyl carbonate, and the required temperature of disproportionation provides the heat for the rectification of cauldron liquid, leads to reactor and rectifying column bottom enrichment methyl phenyl carbonate, and the phenol of top enrichment and disproportionation product-dimethyl carbonate are behind the condenser, collect, separate in the separator. Thus, the utilization rate of heat is improved, the cost is reduced, and the working procedure of separating phenol in advance is also reduced.

The above embodiments are merely preferred technical solutions of the present invention, and should not be considered as limitations of the present invention, and the features in the embodiments and the examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention shall be defined by the claims and the technical solutions described in the claims, including the technical features of the equivalent alternatives as the protection scope. Namely, equivalent alterations and modifications within the scope of the invention are also within the scope of the invention.

Claims

1. The utility model provides a dual-purpose device of disproportionation and rectification, includes reation kettle (1), its characterized in that: reation kettle (1) is methyl phenyl carbonate disproportionation reactor, and reation kettle (1) top material export links to each other with rectifying column (2) feed inlet, still is equipped with the material import on rectifying column (2), and rectifying column (2) top of the tower passes through the pipeline and links to each other with condenser (3), condenser (3) are connected with separator (4) through the pipeline, and separator (4) have two exports, and one of them export is passed through the pipeline and is connected with rectifying column (2), and another export passes through the first step reactor of pipe connection ester exchange.

2. The dual-purpose device for disproportionation and rectification according to claim 1, wherein: and a heating jacket is arranged outside the reaction kettle (1).

3. The dual-purpose device for disproportionation and rectification according to claim 1, wherein: the reaction kettle (1) is internally provided with a coaxial rotating and stirring mechanism, and a stirring paddle of the coaxial rotating and stirring mechanism is in a slant paddle type, an anchor type or a frame type.

4. The dual-purpose device for disproportionation and rectification according to claim 1, wherein: the rectifying tower (2) is a plate tower, and the number of the plate is 5-20.

5. The dual-purpose device for disproportionation and rectification according to claim 1, wherein: the condensing medium adopted by the condenser (3) is circulating water with the temperature of 80-100 ℃.

6. The dual-purpose device for disproportionation and rectification according to claim 1, wherein: the condenser (3) is in a structural form of a shell-and-tube condenser or a double-tube condenser.

7. The dual-purpose device for disproportionation and rectification according to claim 1, wherein: the pipelines connected with the rectifying tower (2) and the condenser (3), the condenser (3) and the separator (4), and the separator (4) and the rectifying tower (2) are all provided with heat-preservation heating jackets.