CN106146310A - A kind of device producing dimethyl carbonate and technique - Google Patents
A kind of device producing dimethyl carbonate and technique Download PDFInfo
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- CN106146310A CN106146310A CN201610743871.1A CN201610743871A CN106146310A CN 106146310 A CN106146310 A CN 106146310A CN 201610743871 A CN201610743871 A CN 201610743871A CN 106146310 A CN106146310 A CN 106146310A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a kind of device producing dimethyl carbonate and technique, wherein device includes reactive distillation column and extractive distillation column;Described reactive distillation column sidepiece is provided with reactive distillation column methanol charging aperture and reactive distillation column Allyl carbonate charging aperture, and tower top is provided with reactive distillation column overhead discharging opening, is provided with discharging opening at the bottom of reactive distillation column tower at the bottom of tower;Described extractive distillation column sidepiece is provided with extractive distillation column material inlet and extractant feed mouth, and tower top is provided with extracting rectifying column overhead discharging opening, is provided with discharging opening at the bottom of extractive distillation column tower at the bottom of tower;The reactive distillation column overhead discharging opening of described reactive distillation column is connected with the extractive distillation column material inlet of extractive distillation column;The extracting rectifying column overhead discharging opening of described extractive distillation column is connected with the reactive distillation column methanol charging aperture of reactive distillation column.The inventive method is simple, effective, workable, it is easy to amplify industrialized production, wide market.
Description
Technical field
The present invention relates to a kind of device utilizing Novel standardized packing to produce dimethyl carbonate and technique, belong to Chemical Engineering Technology
Field.
Background technology
Dimethyl carbonate is nontoxic, environmental protection, can be used for making Merlon, polyurethane, the raw materials for production of medicine, and alternative has
The dimethyl sulfate of poison, methyl chloride, phosgene etc. methylate and carbonylation agent, also act as gasoline additive, are also simultaneously
A kind of cleaning, the green solvent of safety, thus it has again " the new foundation stone of 21 century organic synthesis " and the title of " green chemical products ".
In recent years, along with Merlon production capacity is increased sharply, market is the most urgent to the demand of oxide spinel dimethyl ester.
The method of preparation dimethyl carbonate mainly has: phosgenation, oxidative carbonylation of methanol method, ester-interchange method, urea alcoholysis
Method.Wherein, carbonic acid third (second) alkene ester and methanol ester exchange the ester exchange of dimethyl carbonate coproduction third (second) glycol simultaneously is produced
Method becomes current most common production technology because its environmental protection has substituted phosgenation.
The reaction equation of this technology is as follows:
This operation condition is gentle, be not related to poisonous or severe corrosive solvent, it is easy to accomplish industrialization.But this reaction is subject to
Balance limits, and Allyl carbonate conversion per pass is low.It is circulated reaction by separation Allyl carbonate in product and can improve raw material
Conversion ratio, but operation is complicated, energy consumption is high.The mode of current industrial widely used reactive distillation, by constantly removing product, makes
This reaction tends to complete.
Additionally, due to product dimethyl carbonate and methanol azeotropic, deposit difficulty in separation.How to obtain highly purified carbon
Dimethyl phthalate, and reclaim methanol to greatest extent, it is another major issue of this technology.
Patent CN 201310692281.7 proposes and carries out homogeneous reaction rectification with Feldalat NM for catalyst, and by adding
Pressure distillation separation C dimethyl phthalate and the technique of methanol.
Patent 03150229.6 proposes and carries out homogeneous reaction rectification with carbinol base metallic catalyst, and by pressurizeing, subtracting
Press two tower distillation separation C dimethyl phthalate and the techniques of methanol.
Patent CN 200810016481.X separates based on carbinol base metallic catalyst homogeneous reaction rectification compression rectification
Dimethyl carbonate and the technique of methanol, it is proposed that solve carbinol base metallic catalyst and separate the new technology of difficulty with propylene glycol.
Above-mentioned patent all uses homogeneous catalyst, there is the problem that catalyst separates.It addition, because of dimethyl carbonate and methanol
Azeotropic, need to use pressurization-depressurization two tower rectification to separate, high to equipment requirements, and energy consumption is big.
Patent CN201410300187.7 proposes a kind of by alkali metal compound and/or alkaline earth metal compound and phosphatization
Compound and the composite catalyst of molecular sieve composition, can be used for being catalyzed cyclic carbonate and dimethyl carbonate be synthesized with methanol
Technique.
Patent CN201410498142.5 proposes one and is combined hydroxy imidazole resin for catalyst carbon with strong base
Vinyl acetate and the method for methanol-fueled CLC dimethyl carbonate.
Above-mentioned patent proposes the synthesis carrying out dimethyl carbonate with heterogeneous catalysis replacement homogeneous catalyst, solves
The difficult problem that catalyst separates, but do not provide the technical scheme that can be used for industrialized production.
Summary of the invention
Goal of the invention: the technical problem to be solved is for the deficiencies in the prior art, and provides a kind of technique to want
Seek the device producing dimethyl carbonate low, that dimethyl carbonate production efficiency high and the energy consumption of reactive distillation product later separation is low
And technique.
Technical scheme: for solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of device producing dimethyl carbonate, it is characterised in that: include reactive distillation column and extractive distillation column;
Described reactive distillation column sidepiece is provided with reactive distillation column methanol charging aperture and the charging of reactive distillation column Allyl carbonate
Mouthful, tower top is provided with reactive distillation column overhead discharging opening, is provided with discharging opening at the bottom of reactive distillation column tower at the bottom of tower;
Described extractive distillation column sidepiece is provided with extractive distillation column material inlet and extractant feed mouth, and tower top is provided with extraction
Rectifying tower top discharging opening, is provided with discharging opening at the bottom of extractive distillation column tower at the bottom of tower;
The reactive distillation column overhead discharging opening of described reactive distillation column and the extractive distillation column feedstock of extractive distillation column
Mouth is connected;
The extracting rectifying column overhead discharging opening of described extractive distillation column feeds with the reactive distillation column methanol of reactive distillation column
Mouthful it is connected, the extractant recovery tower charging aperture phase of discharging opening at the bottom of the extractive distillation column tower of extractive distillation column and extractant recovery tower
Even.
Also include that an extractant recovery tower, described extractant recovery tower sidepiece are provided with extractant recovery tower charging aperture, tower top
It is provided with extractant recovery tower tower top discharging opening, at the bottom of tower, is provided with discharging opening at the bottom of extractant recovery tower tower;Described extractant recovery tower
Discharging opening at the bottom of extractant recovery tower tower is connected with the extractive distillation column extractant feed mouth of extractive distillation column.
Rectifying section and conversion zone at described reactive distillation column are provided with window diversion type filler, this window diversion type filler
Packing sheet be corrugated filler tablet, at corrugated filler tablet crest with trough, offer the diversion window connected corrugated filler tablet both sides
Mouthful.
Described window diversion type filler is made up of assembly A and the assembly B being alternately arranged in described reactive distillation tower section,
Catalyst granules is filled out in assembly A or assembly B.
Described assembly A and assembly B becomes spiral line type superposition or slabbing superposition.
The arbitrary described carbonate device of producing of preceding claim is used to carry out the technique of dimethyl carbonate production,
It is characterized in that, comprise the steps:
Step one, Allyl carbonate is joined in reactive distillation column by reactive distillation column Allyl carbonate charging aperture, will
Methanol after fresh methanol and separation and recovery is joined in reactive distillation column by reactive distillation column methanol charging aperture, Allyl carbonate
Under catalyst action, generation dimethyl carbonate and propylene glycol is reacted, from light group of reactive distillation column overhead discharging opening extraction with methanol
Point, from discharging opening extraction heavy constituent at the bottom of reactive distillation column tower;
The light component of step 2, step one extraction is entered extractive distillation column by extractive distillation column material inlet, and by extracting
Take rectifying column extractant feed mouth add extractant, after extracting rectifying, light component by extracting rectifying column overhead discharging opening extraction,
Heavy constituent is by discharging opening extraction at the bottom of extractive distillation column tower, and the light component of extraction is to reclaim the methanol obtained, by reactive distillation column first
Alcohol charging aperture enters reactive distillation column and continues to participate in reactive distillation.
Also include: step 3, the heavy constituent of step 2 extraction are entered extractant recovery tower by extractant recovery tower charging aperture,
After rectification, light component is target product dimethyl carbonate, and by extractant recovery tower tower top discharging opening extraction, heavy constituent is by extractant
Discharging opening extraction at the bottom of recovery tower;
Step 4, the restructuring of step 3 extraction are divided into the extractant that recovery obtains, by extractive distillation column extractant feed mouth
Enter extractive distillation column and continue to participate in extracting rectifying.
Described extractant is phenol, ethylene glycol, water, furfural or aniline.
The number of plates of described reactive distillation column is 30-50 block, and operation pressure is 0.01-0.5MPa;Described extractant reclaims
The number of plates of tower is 20-40 block, and operation pressure is 0.01-0.5MPa.
The theoretical cam curve of described extractive distillation column is 40-60 block, and operation pressure is 0.01-0.5MPa.
Beneficial effect:
(1) use extracting rectifying to realize dimethyl carbonate to separate with methanol, can operate at ambient pressure, reduce technique and want
Asking, relatively pressurization-depressurization rectification process significantly reduces equipment investment and energy consumption;Extractant of the present invention can use phenol, its
There is preferable effect of extracting.Additionally, when downstream process for by dimethyl carbonate and phenol reactant prepare diphenyl carbonate and then
When producing polycarbonate products, phenol is utilized to carry out extracting and can avoid bringing new material in reaction system into, and product carbonic acid
Dimethyl ester nor affects on its production participating in downstream diphenyl carbonate containing a small amount of phenol.It is raw material when using ethylene carbonate
When producing dimethyl carbonate, because by-product is ethylene glycol, the most now utilize ethylene glycol as extractant, the economy of technique can be improved
Property.
(2) reactive distillation column uses window diversion type structured packing, increases gas liquid interfacial area, improves filling surface
Liquid film renewal rate, thus improve gas-liquid mass transfer efficiency;Use window diversion type structured packing, facilitate views with solid catalysis
Agent carries out heterogeneous catalytic reaction, solves the separation problem of catalyst and product.
(3) filler uses the form that assembly A and assembly B is alternately arranged, catalyst filling in assembly A, and wraps up with silk screen
Fixing, this form is conducive to controlling Catalyst packing total amount and the distribution situation in reaction tower thereof.
Accompanying drawing explanation
Fig. 1 is a kind of schematic diagram utilizing Novel standardized packing to produce carbonate device described in embodiment 1;
Fig. 2 is the top view that reactive distillation column packing layer assembly A and assembly B stacked and crimped placement;
Fig. 3 is reactive distillation column packing layer assembly A and the alternately arranged top view being disposed vertically of assembly B;
Fig. 4 is the centre section schematic diagram of Fig. 3;
Fig. 5 is the structural representation of corrugated filler tablet.
In figure: 1-reactive distillation column, 2-extractive distillation column, 3-extractant recovery tower, 4-assembly A, 5-assembly B, 6-crest,
7-trough, 8-water conservancy diversion window, a-Allyl carbonate, b-methanol, c-extractant, d-dimethyl carbonate, e-propylene glycol crude product.
Detailed description of the invention
Below by embodiment, technical solution of the present invention is described in detail, but protection scope of the present invention is not limited to
In described embodiment.
Embodiment 1:
A kind of device utilizing Novel standardized packing to produce dimethyl carbonate, including reactive distillation column 1, extractive distillation column 2
With extractant recovery tower 3.
Reactive distillation column sidepiece is provided with reactive distillation column methanol charging aperture and reactive distillation column Allyl carbonate charging aperture, tower
Top is provided with reactive distillation column overhead discharging opening, is provided with discharging opening at the bottom of reactive distillation column tower at the bottom of tower.
The rectifying section of reactive distillation column and conversion zone use window diversion type structured packing, window diversion type structured packing
Packing sheet is corrugated filler tablet, as shown in Figure 5, including crest 6, trough 7 and is positioned at crest and trough by what otch was formed
On water conservancy diversion window 8.Comprising the assembly A and assembly B of two kinds of different structures in every layer of packing layer, assembly A is that window diversion is filled out
Tablet, outer wrapping silk screen, in fill out catalyst granules, assembly B is structured packing sheet, and assembly A stacks with assembly B and crimps, then
Fix with banding sheet, form catalytic rectification packing, as shown in Figure 2.Assembly A and assembly B can also be that lamellar is sequentially overlapped formation
Catalytic rectification packing, shown in Fig. 3.
Extractive distillation column sidepiece is provided with extractive distillation column material inlet and extractant feed mouth, and tower top is provided with extracting rectifying
Column overhead discharging opening, is provided with discharging opening at the bottom of extractive distillation column tower at the bottom of tower.
Extractant recovery tower sidepiece is provided with extractant recovery tower charging aperture, and tower top is provided with extractant recovery tower tower top discharging
Mouthful, it is provided with discharging opening at the bottom of extractant recovery tower tower at the bottom of tower.
The reactive distillation column overhead discharging opening of reactive distillation column and the extractive distillation column material inlet phase of extractive distillation column
Even;
The reactive distillation column methanol charging aperture phase of the extracting rectifying column overhead discharging opening of extractive distillation column and reactive distillation column
Even, discharging opening at the bottom of the extractive distillation column tower of extractive distillation column is connected with the extractant recovery tower charging aperture of extractant recovery tower;
At the bottom of the extractant recovery tower tower of extractant recovery tower, discharging opening enters with the extractive distillation column extractant of extractive distillation column
Material mouth is connected.
In the present embodiment, the processing step using said apparatus to carry out dimethyl carbonate production is:
1.1, Allyl carbonate is joined in reactive distillation column by reactive distillation column Allyl carbonate charging aperture, by fresh
Methanol after methanol and separation and recovery is joined in reactive distillation column by reactive distillation column methanol charging aperture, Allyl carbonate and first
Alcohol reacts generation dimethyl carbonate and propylene glycol under catalyst action.Through rectifying action, containing methanol and dimethyl carbonate azeotropic
The light component of thing is by reactive distillation column overhead discharging opening extraction, and the heavy constituent containing propylene glycol and a small amount of impurity is by reactive distillation column tower
End discharging opening extraction.
(2-7 block is rectifying section to reactive distillation column totally 28 blocks of column plates, and 8-22 block is catalyst reaction section, and 23-27 block is
Stripping section).Wherein, methanol is added by the 22nd block of plate, and feed flow rates is 18240kg/h, and Allyl carbonate is added by the 8th block of plate,
Feed flow rates is 7140kg/h.Use nitrogen-containing basic resin catalyst, reaction temperature 60-65 DEG C, operate pressure 0.1MPa, carbonic acid
Propylene conversion ratio 99.9%.
1.2, the methanol of step 1.1 extraction and the azeotropic mixture of dimethyl carbonate, partial reflux to reactive distillation column, its remaining part
Divide and entered extractive distillation column by reactive distillation column material inlet, and added extractant by extractive distillation column extractant feed mouth,
After extracting rectifying, light component methanol is by extracting rectifying column overhead discharging opening extraction, containing extractant and the restructuring of dimethyl carbonate
Divide by discharging opening extraction at the bottom of extractive distillation column tower.
(2-5 block plate is exhausting section to extractive distillation column totally 46 blocks of column plates, and 6-39 block plate is rectifying section, 40-45 block plate
For stripping section).With phenol as extractant, the 6th block of plate adding, flow rate is 15040kg/h, containing being total to of methanol and dimethyl carbonate
Boiling thing is added by the 39th block of plate, operates pressure 0.13MPa.
1.3, the phenol of step 1.2 extraction and the mixture of dimethyl carbonate are entered extraction by extractant recovery tower charging aperture
Agent recovery tower, after rectification, dimethyl carbonate is by extractant recovery tower tower top discharging opening extraction, and phenol is at the bottom of by extractant recovery tower tower
Discharging opening extraction.
Extractant recovery tower totally 30 blocks of column plates, the heavy constituent of extractive distillation column is added by the 7th block of plate, operates pressure
0.1MPa。
1.4, the light component of step 1.3 extraction is target product dimethyl carbonate, purity 99.99%.
1.5, the light component of step 1.2 extraction is to reclaim the methanol obtained, containing a small amount of dimethyl carbonate, by reactive distillation column
Methanol charging aperture enters reactive distillation column and continues to participate in reactive distillation.
1.6, the restructuring of step 1.3 extraction is divided into the phenol that recovery obtains, containing a small amount of dimethyl carbonate, by extractive distillation column
Extractant feed mouth enters extractive distillation column and continues to participate in extracting rectifying.
1.7, the heavy constituent of step 1.1 extraction is mainly composed of by-product propylene glycol, send follow-up workshop section to continue rectification and separates.
Table 1: reactive distillation column, extractive distillation column and the charging of extractant recovery tower, discharging flow rate and composition in embodiment 1
Embodiment 2:
The Novel standardized packing that utilizes used in the present embodiment produces the device of dimethyl carbonate, with the phase in embodiment 1
With.
In the present embodiment, use said apparatus carry out reactive distillation and produce the processing step of dimethyl carbonate be:
1.1, Allyl carbonate is joined in reactive distillation column by reactive distillation column Allyl carbonate charging aperture, by fresh
Methanol after methanol and separation and recovery is joined in reactive distillation column by reactive distillation column methanol charging aperture, Allyl carbonate and first
Alcohol reacts generation dimethyl carbonate and propylene glycol under catalyst action.Through rectifying action, containing methanol and dimethyl carbonate azeotropic
The light component of thing is by reactive distillation column overhead discharging opening extraction, and the heavy constituent containing propylene glycol and part methanol is by reactive distillation column tower
End discharging opening extraction.
(2-9 block is rectifying section to reactive distillation column totally 32 blocks of column plates, and 10-25 block is catalyst reaction section, 26-31 block
For stripping section).Wherein, methanol is added by the 25th block of plate, and feed flow rates is 10240kg/h, and Allyl carbonate is added by the 10th block of plate
Entering, feed flow rates is 4080kg/h.Use phenolic resin load C aO catalyst, reaction temperature 60-65 DEG C, operate pressure
0.1MPa, propylene carbonate ester conversion rate 99.9%.
1.2, the methanol of step 1.1 extraction and the azeotropic mixture of dimethyl carbonate, partial reflux to reactive distillation column, its remaining part
Divide and entered extractive distillation column by reactive distillation column material inlet, and added extractant by extractive distillation column extractant feed mouth,
After extracting rectifying, light component methanol is by extracting rectifying column overhead discharging opening extraction, containing extractant and the restructuring of dimethyl carbonate
Divide by discharging opening extraction at the bottom of extractive distillation column tower.
(2-4 block plate is exhausting section to extractive distillation column totally 48 blocks of column plates, and 5-40 block plate is rectifying section, 41-47 block plate
For stripping section).With ethylene glycol as extractant, the 5th block of plate adding, flow rate is 1860kg/h, containing methanol and dimethyl carbonate
Azeotropic mixture is added by the 40th block of plate, operates pressure 0.1MPa.
1.3, the ethylene glycol of step 1.2 extraction and the mixture of dimethyl carbonate are entered extraction by extractant recovery tower charging aperture
Taking agent recovery tower, after rectification, dimethyl carbonate is by extractant recovery tower tower top discharging opening extraction, and ethylene glycol is by extractant recovery tower
Discharging opening extraction at the bottom of tower.
Extractant recovery tower totally 15 blocks of column plates, the heavy constituent of extractive distillation column is added by the 5th block of plate, operates pressure
0.1MPa。
1.4, the light component of step 1.3 extraction is target product dimethyl carbonate, purity 99.99%.
1.5, the light component of step 1.2 extraction is to reclaim the methanol obtained, containing a small amount of dimethyl carbonate, by reactive distillation column
Methanol charging aperture enters reactive distillation column and continues to participate in reactive distillation.
1.6, the restructuring of step 1.3 extraction is divided into the ethylene glycol that recovery obtains, containing a small amount of dimethyl carbonate, by extracting rectifying
Tower extractant feed mouth enters extractive distillation column and continues to participate in extracting rectifying.
1.7, the heavy constituent of step 1.1 extraction is mainly composed of by-product propylene glycol, send follow-up workshop section to continue rectification and separates.
Table 2: reactive distillation column, extractive distillation column, extractant recovery tower and the charging of methanol distillation column in embodiment 2, go out
Stream rate and composition
Although as it has been described above, represented and described the present invention with reference to specific preferred embodiment, but it must not be explained
For the restriction to the present invention self.Under the spirit and scope of the present invention premise defined without departing from claims, can be right
Various changes can be made in the form and details for it.
Claims (10)
1. the device producing dimethyl carbonate, it is characterised in that: include reactive distillation column and extractive distillation column;
Described reactive distillation column sidepiece is provided with reactive distillation column methanol charging aperture and reactive distillation column Allyl carbonate charging aperture, tower
Top is provided with reactive distillation column overhead discharging opening, is provided with discharging opening at the bottom of reactive distillation column tower at the bottom of tower;
Described extractive distillation column sidepiece is provided with extractive distillation column material inlet and extractant feed mouth, and tower top is provided with extracting rectifying
Column overhead discharging opening, is provided with discharging opening at the bottom of extractive distillation column tower at the bottom of tower;
The reactive distillation column overhead discharging opening of described reactive distillation column and the extractive distillation column material inlet phase of extractive distillation column
Even;
The reactive distillation column methanol charging aperture phase of the extracting rectifying column overhead discharging opening of described extractive distillation column and reactive distillation column
Even.
The device producing dimethyl carbonate the most according to claim 1, it is characterised in that also include that an extractant reclaims
Tower, described extractant recovery tower sidepiece is provided with extractant recovery tower charging aperture, and tower top is provided with extractant recovery tower tower top discharging opening,
Discharging opening at the bottom of extractant recovery tower tower it is provided with at the bottom of tower;Discharging opening and extraction at the bottom of the extractant recovery tower tower of described extractant recovery tower
The extractive distillation column extractant feed mouth of rectifying column is connected.
The device producing dimethyl carbonate the most according to claim 1 and 2, it is characterised in that at described reactive distillation column
Rectifying section and conversion zone be provided with window diversion type filler, the packing sheet of this window diversion type filler is corrugated filler tablet,
Corrugated filler tablet crest with offer the water conservancy diversion window connected corrugated filler tablet both sides at trough.
The device producing dimethyl carbonate the most according to claim 3, it is characterised in that described window diversion type filler by
The assembly A being alternately arranged in described reactive distillation tower section and assembly B is constituted, and fills out catalyst particles in assembly A or assembly B
Grain.
The device producing dimethyl carbonate the most according to claim 4, it is characterised in that described assembly A becomes spiral shell with assembly B
Rotation linear superposition or slabbing superposition.
6. use the arbitrary described carbonate device of producing of claim 1-5 to carry out the technique of dimethyl carbonate production, its
It is characterised by, comprises the steps:
Step one, Allyl carbonate is joined in reactive distillation column by reactive distillation column Allyl carbonate charging aperture, by fresh
Methanol after methanol and separation and recovery is joined in reactive distillation column by reactive distillation column methanol charging aperture, Allyl carbonate and first
Alcohol reacts generation dimethyl carbonate and propylene glycol under catalyst action, from the reactive distillation column overhead light component of discharging opening extraction,
From discharging opening extraction heavy constituent at the bottom of reactive distillation column tower;
The light component of step 2, step one extraction is entered extractive distillation column by extractive distillation column material inlet, and by extraction essence
Evaporating tower extractant feed mouth and add extractant, after extracting rectifying, light component is by extracting rectifying column overhead discharging opening extraction, restructuring
Dividing by discharging opening extraction at the bottom of extractive distillation column tower, the light component of extraction is to reclaim the methanol obtained, reactive distillation column methanol enter
Material mouth enters reactive distillation column and continues to participate in reactive distillation.
Technique the most according to claim 6, it is characterised in that also include:
Step 3, the heavy constituent of step 2 extraction are entered extractant recovery tower, after rectification, light group by extractant recovery tower charging aperture
Being divided into target product dimethyl carbonate, by extractant recovery tower tower top discharging opening extraction, heavy constituent is gone out by the bottom of extractant recovery tower
Material mouth extraction;
Step 4, the restructuring of step 3 extraction are divided into the extractant that recovery obtains, extractive distillation column extractant feed mouth enter
Extractive distillation column continues to participate in extracting rectifying.
Technique the most according to claim 7, it is characterised in that described extractant be phenol, ethylene glycol, water, furfural or
Aniline.
Technique the most according to claim 8, it is characterised in that described extractant is phenol.
Technique the most according to claim 7, it is characterised in that the number of plates of described reactive distillation column is 30-50 block, behaviour
It is 0.01-0.5MPa as pressure;The number of plates of described extractant recovery tower is 20-40 block, and operation pressure is 0.01-0.5MPa;
The theoretical cam curve of described extractive distillation column is 40-60 block, and operation pressure is 0.01-0.5MPa.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106588655A (en) * | 2016-12-30 | 2017-04-26 | 开封中科新材料有限公司 | Device and production technology for synthesizing dimethyl carbonate through reaction between urea and methyl alcohol |
CN107739311A (en) * | 2017-11-28 | 2018-02-27 | 屈强好 | The method that azeotropic mixture is handled in dimethyl carbonate technique and diphenyl carbonate technique |
CN109280043A (en) * | 2017-07-19 | 2019-01-29 | 王圣洁 | Method and device for manufacturing propylene carbonate and dimethyl carbonate |
CN111004151A (en) * | 2018-10-08 | 2020-04-14 | 王圣洁 | Device and method for producing hexamethylene-1, 6-dicarbamate |
CN111848400A (en) * | 2020-08-26 | 2020-10-30 | 中建安装集团有限公司 | Device and process for preparing dimethyl carbonate by reactive distillation coupled extraction distillation |
CN114163330A (en) * | 2021-12-16 | 2022-03-11 | 邢台市茂新化工产品有限公司 | Refining method of dimethyl carbonate crude product |
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CN106588655B (en) * | 2016-12-30 | 2023-08-08 | 开封中科新材料有限公司 | Device and production process for synthesizing dimethyl carbonate by using reaction of urea and methanol |
CN109280043A (en) * | 2017-07-19 | 2019-01-29 | 王圣洁 | Method and device for manufacturing propylene carbonate and dimethyl carbonate |
CN107739311A (en) * | 2017-11-28 | 2018-02-27 | 屈强好 | The method that azeotropic mixture is handled in dimethyl carbonate technique and diphenyl carbonate technique |
CN111004151A (en) * | 2018-10-08 | 2020-04-14 | 王圣洁 | Device and method for producing hexamethylene-1, 6-dicarbamate |
CN111004151B (en) * | 2018-10-08 | 2022-04-19 | 王圣洁 | Device and method for producing hexamethylene-1, 6-dicarbamate |
CN111848400A (en) * | 2020-08-26 | 2020-10-30 | 中建安装集团有限公司 | Device and process for preparing dimethyl carbonate by reactive distillation coupled extraction distillation |
CN114163330A (en) * | 2021-12-16 | 2022-03-11 | 邢台市茂新化工产品有限公司 | Refining method of dimethyl carbonate crude product |
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