The concentrating and separating device of a kind of dimethyl carbonate and methyl alcohol
Technical field
The utility model relates to the separation technology field of dimethyl carbonate (DMC) and methyl alcohol (MEOH) azeotropic mixture, specifically is the device of a kind of concentrating and separating dimethyl carbonate and methyl alcohol.
Background technology
Dimethyl carbonate (DMC) be the recently new pollution that emerges less, broad-spectrum basic chemical industry raw material.Owing to contain methoxyl group, carbonyl and carbonyl methyl in its molecule, have good reactivity, therefore can be used as carbonylation, carbonyl methoxylation and methylating reagent, in order to replace phosgene, methylchloroformate, DMS and the methyl chloride that tradition is used.DMC has good solubility property in addition, and not only the intermiscibility with other solvent is good, also has characteristics such as higher evaporating temperature and evaporation rate be fast, can be used as low poison solvent and is used for coating and pharmaceuticals industry, also can be used as the electrode solution composition of anhydrous lithium battery.Oxygen content height in the DMC molecule can improve octane number, increases the gasoline oxygen content, improves efficiency of combustion, reduces tail gas pollution.Therefore it has special meaning as green intermediate to environmental protection, is described as the new foundation stone in the organic synthesis.
The process of industry Synthesis of dimethyl carbonate mainly contains alcoholysis of urea, methanol carbonyl oxidizing process and ester-interchange method, no matter adopt which kind of method, methyl alcohol all can not transform fully when DMC was synthesized in industry, what obtain at first all can only be low concentration DMC and methanol mixture, but under atmospheric pressure, become more readily available the binary azeotrope that methyl alcohol and DMC form, its quality group becomes: methyl alcohol 70%, DMC30% adopts common rectifier unit to want further to separate purification DMC and is difficult to accomplish.
Existing DMC and methyl alcohol separator have the low temperature crystallization device, extracting rectifying device, sequence of constant boiling and rectification device, compression rectification device etc.The low temperature crystallization plant energy consumption is bigger, operating difficulties; Compression rectification appliance arrangement apparatus cost height, complicated operation, steam consumption quantity height; The extracting rectifying device is introduced extractant the 3rd component, and the extractant consumption is big, reclaims the energy consumption height of extractant, and the rate of recovery of DMC is low; Azeotropic distillation device loss nonvariant boiling reagent, the quality of product DMC are difficult to guarantee that operating process is long that control module is many.Thereby seek a kind of more simple, convenient and effective separator, be necessary.
Summary of the invention
At above shortcomings in the prior art, the utility model provides a kind of novel dimethyl carbonate and methyl alcohol concentrating and separating device, and it is simple and reasonable for structure, and energy consumption is low, can effectively separate the separative efficiency height with the methyl alcohol azeotrope to dimethyl carbonate.
The utility model is achieved by the following technical solution: the concentrating and separating device of a kind of dimethyl carbonate and methyl alcohol, it comprises dimethyl carbonate pre-concentration tower apparatus, have charging aperture, hold back material outlet, the infiltration evaporation film condensing device of infiltration material outlet, dimethyl carbonate treating column device, the material outlet at dimethyl carbonate pre-concentration tower apparatus top is communicated with by the charging aperture of pipeline with the infiltration evaporation film condensing device; The infiltration material outlet of infiltration evaporation film condensing device is communicated with through the charging aperture of condenser with dimethyl carbonate treating column device by pipeline, and it is held back material and discharges from holding back material outlet.
The course of work of the present utility model is: dimethyl carbonate and methanol mixture material are introduced into dimethyl carbonate pre-concentration tower apparatus and carry out pre-concentration, the methyl alcohol that obtains through pre-concentration is discharged from the bottom of dimethyl carbonate pre-concentration tower apparatus, then enters the infiltration evaporation film condensing device by the material outlet at its top through the dimethyl carbonate of pre-concentration and carbinol mixture material and further concentrates.Infiltrating and vaporizing membrane in the infiltration evaporation film condensing device in the utility model has the selection trafficability characteristic, process comprising selective absorption, infiltration and vaporization, dimethyl carbonate preferentially enters the film side by infiltrating and vaporizing membrane, and methyl alcohol then is trapped within an other side of infiltrating and vaporizing membrane.The dimethyl carbonate that sees through infiltrating and vaporizing membrane enters the further prepared calcium carbonate dimethyl ester of dimethyl carbonate treating column device finished product after condenser condenses, the finished product after making with extra care is discharged from the bottom of dimethyl carbonate treating column device.Infiltrating and vaporizing membrane is held back concentrated methyl alcohol and is discharged from the material outlet of holding back of infiltration evaporation film condensing device.Wherein, the material that enters the infiltration evaporation film condensing device by dimethyl carbonate pre-concentration tower apparatus can adopt vapour phase charging or liquid phase feeding.
Still contain a spot of not saturating film material owing to hold back material, in order to make the further concentrating and separating of material, the material outlet of holding back of infiltration evaporation film condensing device is communicated with by the charging aperture of pipeline with dimethyl carbonate pre-concentration tower apparatus, and making infiltrating and vaporizing membrane hold back concentrated methyl alcohol, to be back to use dimethyl carbonate pre-concentration tower apparatus recycling.
In order to make full use of material, the residue outlet of dimethyl carbonate treating column device is communicated with by the charging aperture of pipeline with the infiltration evaporation film condensing device, and the residual material after refining passes back into the infiltration evaporation film condensing device, and is recycling.
For the ease of saturating film material by infiltrating and vaporizing membrane and be convenient to the film material and enter dimethyl carbonate treating column device and make with extra care, the utility model is provided with the vacuum extraction device on the infiltration material outlet of infiltration evaporation film condensing device and the pipeline between the dimethyl carbonate treating column device, utilize pumped vacuum systems to provide power for the infiltration evaporation film condensing device.
The utility model is simple in structure, it adopts infiltrating and vaporizing membrane concentrating and separating technology, can not be subjected to the influence of dimethyl carbonate and methanol azeotropic point, the azeotropic mixture of dimethyl carbonate and methyl alcohol is effectively separated, separate back dimethyl carbonate mass concentration through infiltrating and vaporizing membrane and can reach 30%-99%, production technology is simple, the efficient height, and operating cost is low.
Description of drawings
Fig. 1 is the structural representation of the utility model embodiment 1;
Among the figure, 1, dimethyl carbonate pre-concentration tower apparatus, 2, the infiltration evaporation film condensing device, 3, dimethyl carbonate treating column device, 4, the charging aperture of dimethyl carbonate pre-concentration tower apparatus, 5, the material outlet of dimethyl carbonate pre-concentration tower apparatus, 6, the methyl alcohol outlet, 7, the charging aperture of infiltration evaporation film condensing device, 8, the infiltration material outlet of infiltration evaporation film condensing device, 9, the infiltration evaporation film condensing device hold back material outlet, 10, the charging aperture of dimethyl carbonate treating column device, 11, the residue outlet of dimethyl carbonate treating column device, 12, the dimethyl carbonate product outlet of dimethyl carbonate treating column device, 13, condenser, 14, vavuum pump, 15, cooling liquid outlet, 16, the cooling fluid inlet, 17, infiltrating and vaporizing membrane.
The specific embodiment
Below in conjunction with accompanying drawing and non-limiting embodiment the utility model is further described:
Embodiment 1
As shown in drawings, the concentrating and separating device of dimethyl carbonate shown in the present embodiment and methyl alcohol, comprise dimethyl carbonate pre-concentration tower apparatus 1, infiltration evaporation film condensing device 2, condenser 13, dimethyl carbonate treating column device 3, wherein, methyl alcohol outlet 6 is arranged at dimethyl carbonate pre-concentration tower apparatus 1 bottom, its top has material outlet 5 to be communicated with the charging aperture 7 of infiltration evaporation film condensing device 2 by pipeline, the material outlet 9 of holding back of infiltration evaporation film condensing device 2 is communicated with by the charging aperture 4 of pipeline with dimethyl carbonate pre-concentration tower apparatus 1, its infiltration material outlet 8 is communicated with condenser 13 by pipeline, the infiltration material outlet of condenser 13 is communicated with by the charging aperture 10 of pipeline with dimethyl carbonate treating column device 1, is provided with vavuum pump 14 and is communicated with condenser 13.The residue of dimethyl carbonate treating column device 3 outlet 11 is communicated with the charging aperture 7 of infiltration evaporation film condensing device 2 by pipeline, and dimethyl carbonate product outlet 12 is arranged at the bottom of dimethyl carbonate treating column device 3.Dimethyl carbonate pre-concentration tower apparatus in the present embodiment and dimethyl carbonate treating column device can adopt the destilling tower and the rectifying column of prior art respectively.
Other parts of present embodiment adopt prior art, do not repeat them here.
The course of work of the present utility model is: material to be separated is introduced into dimethyl carbonate pre-concentration tower apparatus 1 and carries out pre-concentration, discharge from the methyl alcohol outlet 6 of dimethyl carbonate pre-concentration tower apparatus 1 bottom through the methyl alcohol that pre-concentration obtains, the dimethyl carbonate of process pre-concentration and the material outlet 5 of carbinol mixture material from dimethyl carbonate pre-concentration tower apparatus 1 top enter infiltration evaporation film condensing device 2 and further concentrate.Dimethyl carbonate preferentially enters the film side by infiltrating and vaporizing membrane 17, and methyl alcohol then is trapped within an other side of infiltrating and vaporizing membrane 17.After entering condenser 13 condensations, the dimethyl carbonate that sees through infiltrating and vaporizing membrane 17 enters dimethyl carbonate treating column device 3 further prepared calcium carbonate dimethyl ester finished products.Finished product after refining is discharged from the dimethyl carbonate product outlet 12 of dimethyl carbonate treating column device 3 bottoms, and its residual material passes back into infiltration evaporation film condensing device 2 further concentrating and separating from the residue outlet 11 of top of tower.Infiltrating and vaporizing membrane 17 is held back concentrated methyl alcohol, and to be back to dimethyl carbonate pre-concentration tower apparatus 1 charging aperture from material outlet 9 recycling.
In the present embodiment, hold back concentrated methyl alcohol by infiltration evaporation film condensing device 2 and also can directly not be back to dimethyl carbonate pre-concentration tower apparatus 1, be back to dimethyl carbonate pre-concentration tower apparatus 1 again, carry out recycling and can be drained into surge tank earlier.
In the present embodiment, make with extra care, also can before the charging aperture of dimethyl carbonate treating column device, add booster pump for condensed dimethyl carbonate being sent into smoothly dimethyl carbonate treating column device.
The foregoing description only is used for explanation of the present utility model, is not to its restriction, and those skilled in the art also can make a change on this basis.