CN104016839A - Method and system for continuously preparing polyoxymethylene dimethyl ether by utilizing ionic liquid catalyst - Google Patents
Method and system for continuously preparing polyoxymethylene dimethyl ether by utilizing ionic liquid catalyst Download PDFInfo
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- CN104016839A CN104016839A CN201410204957.8A CN201410204957A CN104016839A CN 104016839 A CN104016839 A CN 104016839A CN 201410204957 A CN201410204957 A CN 201410204957A CN 104016839 A CN104016839 A CN 104016839A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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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
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Abstract
The invention discloses a method and a system for continuously preparing polyoxymethylene dimethyl ether by utilizing an ionic liquid catalyst. The system mainly comprises two areas, i.e., a reaction area and a refining area. The method comprises the following steps: firstly, carrying out an acetalation reaction on methyl alcohol and concentrated formaldehyde in the presence of the ionic liquid catalyst so as to generate the polyoxymethylene dimethyl ether; and then, rectifying the polyoxymethylene dimethyl ether in the refining area. According to the method and the system which are disclosed by the invention, an aqueous solution of the polyoxymethylene dimethyl ether is taken as an initial reaction raw material on which the continuous acetalation reaction is carried out so as to prepare the polyoxymethylene dimethyl ether, so that compared with other industrial devices, the system and the method are simple in process, low in energy consumption, simple in catalyst separation due to the adoption of an extractive distillation mode and the like, high in separation efficiency and high in polyoxymethylene dimethyl ether purity. A novel tank reactor is adopted, so that the method and the system which are disclosed by the invention are suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of method and system that adopt ionic-liquid catalyst continuous production polymethoxy dimethyl ether.
Background technology
Along with the minimizing day by day of petroleum resources, and countries in the world are growing to the demand of fuel oil, and various countries have all strengthened dynamics to the research and development of novel energy.
Polymethoxy dimethyl ether is the lower molecular weight acetal polymer taking methoxyl group as main chain, and general formula is CH
3(OCH
2)
noCH
3, be high boiling point colourless liquid, can be used as properties-correcting agent, solvent, softening agent and the releasing agent etc. of resol.The compound of n=3～6 is diesel oil oxygenation agents of a kind of excellent property, its physical property and diesel oil are close, not only have very high cetane value, its oxygen level is also very high, the in the situation that of adding 15% in diesel oil, do not need vehicle motor oil supply system to transform, can obviously improve the combustioncharacteristics of diesel oil, improve diesel quality, increase oxygen level more than 7%, reduce discharging more than 50% tail gas pollution, significantly reduce the discharge of oxynitrides and carbon monoxide.
It is raw material that polymethoxy dimethyl ether (DMMn) getting up early adopts methyl alcohol, formaldehyde, concentrated formaldehyde, paraformaldehyde or ethylene glycol acetal, synthetic with sulfuric acid or hydrochloric acid catalysis.In recent years, it is catalyzer that BASF AG (WO 2006/045506 A1, CA 2581502) is used the protonic acids such as sulfuric acid, trifluoromethanesulfonic acid, methyl alcohol and trioxymethylene (or paraformaldehyde) are raw material, react 8 ~ 12h at 100 DEG C, obtain the content of DMM3-8 lower than 26%.The method severe reaction conditions, transformation efficiency is low with the component concentration that can be used as oil dope.2005, the people (EP 1505049 AI) such as De Gregori adopted bronsted acid catalyst, and reaction is carried out under the N2 of 1.0MPa, has shortened widely the reaction times, and DMM3-8 productive rate can reach 51.2%.There is seriously corroded, separation difficulty in above-mentioned catalyzer, can not recycle, to process energy consumption large, and products distribution is unreasonable, trioxymethylene transformation efficiency and can be used for the not high defect of component DMM3-8 selectivity of oil dope.BP company (US 6160174, US 62655284) is studied heterogeneous catalyst, and taking methyl alcohol, formaldehyde, dme and methyl alcohol as raw material, wherein the content of DMM3-8 only has 11.6%.The method catalyst activity is low, and complex process is difficult to realize industrialization.
Summary of the invention
Main purpose of the present invention is to provide a kind of taking methyl alcohol and concentrated formaldehyde as raw material, and taking ionic liquid as catalyzer, the method and system of the synthetic polymethoxy dimethyl ether of successive reaction, mainly comprise two regions: reaction zone and refining district.
A method that adopts ionic-liquid catalyst continuous production polymethoxy dimethyl ether, step is as follows:
A, acetalation
Taking ionic liquid as catalyzer, using methyl alcohol and concentrated formaldehyde as reactant, carry out continuous acetalation at reactor, temperature of reaction is 105 DEG C ~ 130 DEG C, reaction pressure is 1.0MPaG ~ 3.0MPaG, reaction time is 40 ~ 120min, and ionic-liquid catalyst accounts for 0.1 ~ 10wt% of reaction raw materials, and the mol ratio of concentrated formaldehyde and methyl alcohol is 1.0 ~ 3.0; Reaction product is mainly DMM1-6, the water that reaction generates;
B, refining
The reactant that reaction product, catalyzer and unreacted are complete, be separated into the first light constituent and product mixture through the first light constituent recovery tower C1, the first light constituent condensing reflux continues reaction to reactor, and product mixture enters extraction tower C2 and carries out separation and recovery of catalyst; Catalyzer goes out from extraction tower C2 underflow, after falling liquid film film-type evaporator E2 transpiring moisture, catalyzer phase Returning reactor continues to participate in reaction, extraction phase is through soda-wash tower C3 alkali cleaning, after Multistage rectifying tower rectifying, obtain in order respectively the second light constituent, extraction agent, the 3rd light constituent, DMM3-6, light constituent 2, extraction agent, the restructuring material that grades, the second light constituent, the 3rd light constituent Returning reactor R1 continue reaction, and extraction agent returns to extraction tower C2 and continues extraction.
Described acetalation is carried out under the state of continuous feeding and discharging, and the mean residence time of reactant is by the control of reactant liquid level.
Described ionic liquid is acidic ionic liquid catalysts, cationic moiety is selected from one or more in quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, pyridylium and heterocycle positively charged ion, and anionicsite is selected from p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid with one or more in, bisulfate ion and trifluoroacetic acid root.
Described cationic moiety is selected from glyoxaline cation, and anionicsite is selected from methylsulphonic acid root or bisulfate ion.
The material of described reactor is 316L stainless steel.
The mass ratio of described extraction agent and raw material charging is 0.1 ~ 3.
Adopt a system for ionic-liquid catalyst continuous production polymethoxy dimethyl ether, it comprises raw material premixing tank V1, reactor R1, the first light constituent recovery tower C1, extraction tower C2, soda-wash tower C3, the second light constituent recovery tower C4, extraction agent recovery tower C5, the 3rd light constituent recovery tower C6, falling liquid film film-type evaporator E2, raw material premixing tank V1 is connected with the opening for feed of reactor R1, the discharge port of reactor R1 is connected with the opening for feed of the first light constituent recovery tower C1, the first light constituent recovery tower C1 tower reactor is connected with the opening for feed of extraction tower C2, the tower top of extraction tower C2 is connected with the opening for feed of soda-wash tower C3, the tower top of soda-wash tower C3 is connected with the opening for feed of the second light constituent recovery tower C4, the second light constituent recovery tower C4 tower reactor is connected with the opening for feed of extraction agent recovery tower C5, the tower reactor of extraction agent recovery tower C5 is connected with the opening for feed of the 3rd light constituent recovery tower C6, the tower top of the 3rd light constituent recovery tower C6 is connected with the feed-pipe of raw material premixing tank V1, the tower top of extraction agent recovery tower C5 is connected with the feed-pipe of extraction tower C2, the tower top of the second light constituent recovery tower C4 is connected with the feed-pipe of raw material premixing tank V1, the tower reactor of extraction tower C2 is connected with the feed-pipe of raw material premixing tank V1 by falling liquid film film-type evaporator E2.
Described reactor R1 is stirred autoclave, is further provided with reaction temperature control unit E1.
The material of described reactor is 316L stainless steel.
Described extraction tower C2 adopts structured packing, packed height is 10 ~ 40 meters, inner-tower filling material or the column plate of the second light constituent recovery tower C4, extraction agent recovery tower C5, the 3rd light constituent recovery tower C6 all adopt stainless steel, and packed height is 10 ~ 40 meters, and theoretical plate number is 10 ~ 50.
Beneficial effect of the present invention: what reaction zone adopted is tank reactor, built-in stirring system, external pump circulation and heat-exchange system, improved the deficiency that unit scale is little, floor space is large of annular reactor existence used in the past, can realize the large-scale industrial production of product.
The present invention adopts ionic-liquid catalyst, and the selectivity that the transformation efficiency of reaction can reach 90%, DMM3-6 can reach 45%.Side reaction is few, and transformation efficiency is high.
Refining district comprises reaction solution Distallation systm, extracting system, the catalyzer concentrated recycle system, caustic washing system and rectifying separation system etc., makes product obtain effective separation, has reached product standard.
It is initial reaction raw material that the present invention adopts methyl alcohol and concentrated formaldehyde solution, adopt successive polymerization, acetalation to prepare polymethoxy dimethyl ether, wherein, technique prepared by methyl alcohol and concentrated formaldehyde can adopt maturation process, with respect to the technique taking trioxymethylene as raw material, its flow process has been simplified greatly, and energy consumption also reduces greatly.
The present invention adopts extraction fractional distillation, can solve easily catalyzer phase and the difficult problem of product separation in reaction product; Catalyzer by falling film evaporator transpiring moisture, can solve the Recycling of catalyzer, and effectively control the loss of catalyzer mutually.
Brief description of the drawings
Fig. 1 is the structural representation of system of the present invention, only draws main equipment, and the equipment such as other instrument, pump, valve, tundish omits.
Embodiment
As shown in Figure 1,
1) methyl alcohol, concentrated formaldehyde, recovery light constituent, circulation ionic-liquid catalyst, as reactant, enter into raw material premixing tank V1 and carry out proportioning mixing, then carry out continuous acetalation by sending into tank reactor R1; Tank reactor R1 carries out under the state of continuous feeding and discharging, reactor R1 provides strong turbulence by agitator and the recycle system, reactant is fully mixed with catalyzer, the mean residence time of reactant is by the control of reactant liquid level, temperature of reaction is controlled by external heat exchanger E1, reaction will lean on the seperating range control valve regulation nitrogen pressure of reactor head to provide reaction required pressure, the reaction product that tank reactor R1 flows out continuously, mainly contain DMM1-6, water that reaction generates, also have complete formaldehyde, methyl alcohol and the catalyzer of unreacted.
The mol ratio of concentrated formaldehyde and methyl alcohol is 1.0 ~ 3.0,0.1 ~ 10wt% that the consumption of ionic-liquid catalyst is total reactant, and temperature of reaction is 105 DEG C ~ 130 DEG C, and reaction pressure is 1.0MPaG ~ 3.0MPaG, and reaction time is 30 ~ 120min.
2) reaction solution, from reactor R1 flows out, enters into the first light constituent recovery tower C1; Wherein, the part light constituent in reaction solution, is mainly formaldehyde, methyl alcohol, water and DMM1 etc., and after overhead condensation is cooling, extraction is back to raw material and premixed device V1; At the bottom of tower, component is sent to extraction tower C2 and extracts;
The service temperature of the first light constituent recovery tower tower is 40 ~ 150 DEG C, and working pressure is-0.01 ~ 0.1MPaG, adopts packing tower, and packed height is 10 ~ 20 meters.
3) extraction agent of coming from the reaction solution of coming at the bottom of C1 tower and extraction agent storage tank, respectively from extraction tower C2 two endfeeds, after extraction tower extraction, catalyzer phase and water in reaction solution, go out to the concentrated recycle system of catalyzer from tower bottom flow; Product component in reaction solution, is following extraction agent and is flowing out from tower top, enters into caustic washing system;
The service temperature of extraction tower is 50 ~ 100 DEG C, and working pressure is 0 ~ 0.1MPaG, adopts packing tower, and packed height is 20 ~ 35 meters.
4) the concentrated recycle system of catalyzer is mainly by falling film type evaporation E2, the moisture in catalyzer to be steamed, and reaches after the effect of concentrate, then is back to raw material premixing tank V1;
5) extraction tower C2 tower top out extraction phase enter into the soda-wash tower C3 corrosivess such as alkali cleaning, the formic acid in neutralized product that circulate, improve its pH value, prevent the corrosion of equipment and the decomposition of product;
The service temperature of soda-wash tower C3 is 50 ~ 100 DEG C, and working pressure is 0 ~ 0.1MPaG, adopts packing tower, and packed height is 10 ~ 20 meters.
6) reaction solution after soda-wash tower C3 alkali cleaning, enters into the second light constituent recovery tower C4; The second light constituent in reaction solution, if DMM1 is from overhead extraction, is back to raw material premixing tank V1; At the bottom of tower, component enters into extraction agent recovery tower C5 and carries out the recovery of extraction agent;
The service temperature of the second light constituent recovery tower is 50 ~ 100 DEG C, and working pressure is 0 ~ 0.3MPaG, adopts tray column, and number of theoretical plate is 10 ~ 20.
7) Main Function of extraction agent recovery tower C5 is that extraction agent is separated with reaction solution, and extraction agent is from overhead extraction, and the extraction tower C2 being back to above carries out recirculation utilization, and at the bottom of tower, component enters into the 3rd light constituent recovery tower C6 and carries out heavy constituent recovery;
The service temperature of the 3rd light constituent recovery tower is 50 ~ 100 DEG C, and working pressure is 0 ~ 0.1MPa, adopts tray column, and number of theoretical plate is 10 ~ 30.
8) effect of the 3rd light constituent recovery tower is mainly that DMM2, from overhead extraction, is back to raw material premixing tank V1 by material and product separation such as the DMM2 in reaction solution; Product, from extraction at the bottom of tower, after overcooling, is sent to products pot and stores;
The service temperature of the 3rd light constituent recovery tower is 50 ~ 150 DEG C, and working pressure is-0.01 ~ 0.1MPaG, adopts tray column, and number of theoretical plate is 10 ~ 40.
embodiment mono-
After product and each component reaction reach balance, sample, by gas chromatograph quantitative analysis, its result is as shown in table 1 below:
Temperature of reaction: 120 DEG C;
Reaction pressure: 2.0 MPaG;
Concentrated formaldehyde and methanol feeding ratio: 2.5:1;
Catalyst levels: 4%;
embodiment bis-
After product and each component reaction reach balance, sample, by gas chromatograph quantitative analysis, its result is as shown in table 2 below:
Temperature of reaction: 130 DEG C;
Reaction pressure: 3.0 MPaG;
Concentrated formaldehyde and methanol feeding ratio: 3:1;
Catalyst levels: 10%;
embodiment tri-
After product and each component reaction reach balance, sample, by gas chromatograph quantitative analysis, its result is as shown in table 3 below:
Temperature of reaction: 110 DEG C;
Reaction pressure: 1.0 MPaG;
Concentrated formaldehyde and methanol feeding ratio: 1:1;
Catalyst levels: 1%;
Claims (10)
1. a method that adopts ionic-liquid catalyst continuous production polymethoxy dimethyl ether, is characterized in that, step is as follows:
A, acetalation
Taking ionic liquid as catalyzer, using methyl alcohol and concentrated formaldehyde as reactant, carry out continuous acetalation at reactor, temperature of reaction is 105 DEG C ~ 130 DEG C, reaction pressure is 1.0MPaG ~ 3.0 MPaG, reaction time is 40 ~ 120min, and ionic-liquid catalyst accounts for 0.1 ~ 10wt% of reaction raw materials, and the mol ratio of concentrated formaldehyde and methyl alcohol is 1.0 ~ 3.0; Reaction product is mainly DMM1-6, the water that reaction generates;
B, refining
The reactant that reaction product, catalyzer and unreacted are complete, be separated into the first light constituent and product mixture through the first light constituent recovery tower C1, the first light constituent condensing reflux continues reaction to reactor, and product mixture enters extraction tower C2 and carries out separation and recovery of catalyst; Catalyzer goes out from extraction tower C2 underflow, after falling liquid film film-type evaporator E2 transpiring moisture, catalyzer phase Returning reactor continues to participate in reaction, extraction phase is through soda-wash tower C3 alkali cleaning, after Multistage rectifying tower rectifying, obtain in order respectively the second light constituent, extraction agent, the 3rd light constituent, DMM3-6, the second light constituent, the 3rd light constituent Returning reactor R1 continue reaction, and extraction agent returns to extraction tower C2 and continues extraction.
2. method according to claim 1, is characterized in that, described acetalation is carried out under the state of continuous feeding and discharging, and the mean residence time of reactant is by the control of reactant liquid level.
3. method according to claim 1, it is characterized in that, described ionic liquid is acidic ionic liquid catalysts, cationic moiety is selected from one or more in quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, pyridylium and heterocycle positively charged ion, and anionicsite is selected from p-methyl benzenesulfonic acid root, trifluoromethane sulfonic acid root, methylsulphonic acid with one or more in, bisulfate ion and trifluoroacetic acid root.
4. method according to claim 3, is characterized in that, described cationic moiety is selected from glyoxaline cation, and anionicsite is selected from methylsulphonic acid root or bisulfate ion.
5. method according to claim 1, is characterized in that, the material of described reactor is 316L stainless steel.
6. method according to claim 1, is characterized in that, the mass ratio of described extraction agent and raw material charging is 0.1 ~ 3.
7. one kind adopts the system of ionic-liquid catalyst continuous production polymethoxy dimethyl ether, it is characterized in that, it comprises raw material premixing tank V1, reactor R1, the first light constituent recovery tower C1, extraction tower C2, soda-wash tower C3, the second light constituent recovery tower C4, extraction agent recovery tower C5, the 3rd light constituent recovery tower C6, falling liquid film film-type evaporator E2, raw material premixing tank V1 is connected with the opening for feed of reactor R1, the discharge port of reactor R1 is connected with the opening for feed of the first light constituent recovery tower C1, the first light constituent recovery tower C1 tower reactor is connected with the opening for feed of extraction tower C2, the tower top of extraction tower C2 is connected with the opening for feed of soda-wash tower C3, the tower top of soda-wash tower C3 is connected with the opening for feed of the second light constituent recovery tower C4, the second light constituent recovery tower C4 tower reactor is connected with the opening for feed of extraction agent recovery tower C5, the tower reactor of extraction agent recovery tower C5 is connected with the opening for feed of the 3rd light constituent recovery tower C6, the tower top of the 3rd light constituent recovery tower C6 is connected with the feed-pipe of raw material premixing tank V1, the tower top of extraction agent recovery tower C5 is connected with the feed-pipe of extraction tower C2, the tower top of the second light constituent recovery tower C4 is connected with the feed-pipe of raw material premixing tank V1, the tower reactor of extraction tower C2 is connected with the feed-pipe of raw material premixing tank V1 by falling liquid film film-type evaporator E2.
8. system according to claim 7, is characterized in that, described reactor R1 is stirred autoclave, is further provided with reaction temperature control unit E1.
9. system according to claim 7, is characterized in that, the material of described reactor is 316L stainless steel.
10. system according to claim 7, it is characterized in that, described extraction tower C2 adopts structured packing, packed height is 10 ~ 40 meters, inner-tower filling material or the column plate of the second light constituent recovery tower C4, extraction agent recovery tower C5, the 3rd light constituent recovery tower C6 all adopt stainless steel, packed height is 10 ~ 40 meters, and theoretical plate number is 10 ~ 50.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935825A (en) * | 2017-12-28 | 2018-04-20 | 四川鑫达新能源科技有限公司 | Polymethoxy dimethyl ether refining spearation system and the method that polymethoxy dimethyl ether is prepared using the system |
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| CN102249869A (en) * | 2010-05-18 | 2011-11-23 | 中国科学院兰州化学物理研究所 | Technical process for catalytically synthesizing polymethoxy dimethyl ether by ionic liquid |
| CN102701923A (en) * | 2012-06-11 | 2012-10-03 | 北京科尔帝美工程技术有限公司 | System device and process for preparing polymethoxy dimethyl ether |
| CN103772163A (en) * | 2012-10-18 | 2014-05-07 | 中国科学院兰州化学物理研究所 | Reaction system and process for continuously preparing polyoxymethylene dimethyl ether |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102249869A (en) * | 2010-05-18 | 2011-11-23 | 中国科学院兰州化学物理研究所 | Technical process for catalytically synthesizing polymethoxy dimethyl ether by ionic liquid |
| CN102701923A (en) * | 2012-06-11 | 2012-10-03 | 北京科尔帝美工程技术有限公司 | System device and process for preparing polymethoxy dimethyl ether |
| CN103772163A (en) * | 2012-10-18 | 2014-05-07 | 中国科学院兰州化学物理研究所 | Reaction system and process for continuously preparing polyoxymethylene dimethyl ether |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107935825A (en) * | 2017-12-28 | 2018-04-20 | 四川鑫达新能源科技有限公司 | Polymethoxy dimethyl ether refining spearation system and the method that polymethoxy dimethyl ether is prepared using the system |
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Application publication date: 20140903 |