CN104016838A - Multi-reaction system for continuously preparing polyethylene methoxyethoxy dimethyl ether by adopting ionic liquid catalyst - Google Patents
Multi-reaction system for continuously preparing polyethylene methoxyethoxy dimethyl ether by adopting ionic liquid catalyst Download PDFInfo
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- CN104016838A CN104016838A CN201410204856.0A CN201410204856A CN104016838A CN 104016838 A CN104016838 A CN 104016838A CN 201410204856 A CN201410204856 A CN 201410204856A CN 104016838 A CN104016838 A CN 104016838A
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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
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Abstract
The invention discloses a multi-reaction system for continuously preparing polyethylene methoxyethoxy dimethyl ether by adopting an ionic liquid catalyst. The multi-reaction system mainly comprises two zones, namely a reaction zone and a separation zone. The multi-reaction system comprises the following processes: firstly, carrying out acetalation reaction on methylal, methanol and concentrated formaldehyde to generate polyethylene methoxyethoxy dimethyl ether under the action of an ionic liquid catalyst, and then entering the separation zone to rectify to obtain the product. The methylal, methanol and concentrated formaldehyde solution are taken as initial reaction materials, and the polyethylene methoxyethoxy dimethyl ether is prepared by adopting continuous acetalation reaction. Compared with other industrial devices, the multi-reaction system is simple in flow, low in energy consumption, simple in separation of a catalyst, high in separation efficiency, and high in product purity, and the modes such as extractive distillation and the like are adopted.
Description
Technical field
The present invention relates to a kind ofly take ionic liquid as catalyzer the method for methylal, methyl alcohol and the synthetic polymethoxy dimethyl ether of concentrated formaldehyde reaction.
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 to take the lower molecular weight acetal polymer that methoxyl group is 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.
Polymethoxy dimethyl ether (DMM
n) to adopt methyl alcohol, formaldehyde, concentrated formaldehyde, paraformaldehyde or ethylene glycol acetal be raw material in getting up early, 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, and methylal and trioxymethylene (or paraformaldehyde) are raw material, reacts 8 ~ 12h at 100 ℃, obtains DMM
3-8content 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 at the N of 1.0MPa
2under carry out, shortened the reaction times widely, DMM
3-8productive 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 component DMM of oil dope
3-8the not high defect of selectivity.BP company (US 6160174, US 62655284) is studied heterogeneous catalyst, and take methyl alcohol, formaldehyde, dme and methylal is raw material, wherein DMM
3-8content only have 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 method and many reactive systems that adopts ionic-liquid catalyst continuous production polymethoxy dimethyl ether.
A method that adopts ionic-liquid catalyst continuous production polymethoxy dimethyl ether, step is as follows:
A, acetalation
Take ionic liquid as catalyzer, using methylal and concentrated formaldehyde as reactant, at reactor, carry out continuous acetalation, ionic-liquid catalyst accounts for 0.1 ~ 10wt% of reaction raw materials, the mol ratio of concentrated formaldehyde and methylal is 1.0 ~ 3.0, and reaction product is mainly the DMM1-6 that reaction generates;
Or take ionic liquid as catalyzer, using methyl alcohol and concentrated formaldehyde as reactant, at reactor, carry out continuous acetalation, 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, through the first light constituent recovery tower C1, be separated into the first light constituent and reaction mixture, the first light constituent condensing reflux continues reaction to reactor R1, and reaction 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 controlled by 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 multi-reaction kettle system for ionic-liquid catalyst continuous production polymethoxy dimethyl ether, comprise raw material premixing tank V1, raw material premixing tank V2, reactor R1, reactor R2, 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, raw material premixing tank V2 is connected with the opening for feed of reactor R2, the discharge port of reactor R2 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; Described reactor R2 is stirred autoclave, is further provided with reaction temperature control unit E3.
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 a plurality of tank reactors, 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, why adopt two polymerization reaction kettles, be for more effective and reasonable recycling rare formaldehyde solution of producing in device, wherein, technique prepared by methyl alcohol, methylal and concentrated formaldehyde all belongs to maturation process, with respect to take the technique that trioxymethylene is raw material, its flow process has been simplified greatly, and energy consumption also reduces greatly.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention, only draws main equipment, and the equipment such as other instrument, pump, valve, tundish omit.
Embodiment
Content of the present invention further illustrates flow process by means of accompanying drawing:
As shown in Figure 1,
1) methyl alcohol and concentrated formaldehyde are controlled through Flow-rate adjustment, enter into continuously in certain proportion raw material premixing tank V1; Methylal and concentrated formaldehyde are controlled through Flow-rate adjustment, enter into continuously in certain proportion raw material premixing tank V2.After the first light constituent, the second light constituent, the 3rd light constituent and the part recycling catalyst etc. that the circulation of rear system comes measure by under meter, after raw material premixing tank V1 mixes, be sent in reactor R1 together with raw material; Part recycling catalyst enters into raw material premixing tank V2, after mixing, sends into reactor R2 with raw material; In two reactors, with nitrogen, be forced into reaction pressure, by external circulation heater E1, E2, be heated to temperature of reaction respectively, there is acetalation in reaction raw materials, the reaction product that reactor flows out continuously mainly contains the DMM that reaction generates under the effect of ionic-liquid catalyst
1-6, water, catalyzer and unreacted formaldehyde, methyl alcohol.
The mol ratio of concentrated formaldehyde or paraformaldehyde and methyl alcohol is 1.0 ~ 3.0,1 ~ 10wt% that the consumption of ionic-liquid catalyst is total reactant, and temperature of reaction is 110 ℃ ~ 130 ℃, and reaction pressure is 1.0MPaG ~ 3.0 MPaG, and reaction time is 40 ~ 120min.
2) reaction solution flows out from reactor R1 and R2, enters into anti-the first light constituent recovery tower C1; Wherein, the part light constituent in reaction solution, is mainly formaldehyde, methyl alcohol, water and DMM
1deng, 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 anti-the first light constituent recovery tower tower is 40 ~ 60 ℃, and working pressure is-0.01 ~ 0.1MPaG, adopts packing tower, and packed height is 10 ~ 20 meters.
3), from the reaction mixture of coming at the bottom of C1 tower and the extraction agent of coming from extraction agent storage tank, respectively from extraction tower C2 two endfeeds, after extraction tower extraction, the water in reaction solution, goes out to the second light constituent recovery tower C3 from tower bottom flow; Product component in reaction solution, along with extraction agent flows out from tower top, enters into soda-wash tower C4;
The service temperature of extraction tower C2 is 30 ~ 60 ℃, and working pressure is 0 ~ 0.1MPaG, adopts packing tower, and packed height is 20 ~ 35 meters.
4) the second light constituent recovery tower is mainly by component recovery tower C3, the useful component in water to be steamed from water, is back to respectively raw material premixing tank V1 and V2;
5) extraction tower tower top out extraction phase enter into the soda-wash tower C4 corrosivess such as alkali cleaning, the formic acid in neutralized product that circulate, prevent the corrosion of equipment and the decomposition of product;
The service temperature of soda-wash tower is 50 ~ 100 ℃, and working pressure is 0 ~ 0.1MPaG, adopts packing tower, and packed height is 10 ~ 20 meters.
6) reaction solution after soda-wash tower alkali cleaning, enters into the 3rd light constituent recovery tower C5; Light constituent in reaction solution is as DMM
1from overhead extraction, be back to raw material premixing tank V1; At the bottom of tower, component enters into extraction agent recovery tower C6 and carries out the recovery of extraction agent;
The service temperature of the 3rd light constituent recovery tower is 40 ~ 60 ℃, 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 C6 is that extraction agent is separated with reaction solution, and extraction agent, from overhead extraction, is back to extraction tower C2 and reuses, and at the bottom of tower, component enters into the 4th light constituent recovery tower C7 and carries out component recovery;
The service temperature of extraction agent recovery tower is 60 ~ 100 ℃, and working pressure is 0 ~ 0.1MPaG, adopts tray column, and number of theoretical plate is 10 ~ 30.
8) effect of the 4th light constituent recovery tower C7 is mainly by the DMM in reaction solution
2deng material and product separation, DMM
2from overhead extraction, be back to raw material premixing tank V1; Product, from extraction at the bottom of tower, after overcooling, is sent to products pot and stores;
The service temperature of the 4th light constituent recovery tower is 80 ~ 150 ℃, 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 ℃;
Reaction pressure: 2.0 MPaG;
Concentrated formaldehyde and methanol feeding ratio: 2.5:1;
Concentrated formaldehyde and methylal charge ratio: 2.5:1;
Catalyst levels: 5%;
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 ℃;
Reaction pressure: 3.0 MPaG;
Concentrated formaldehyde and methanol feeding ratio: 3:1;
Concentrated formaldehyde and methylal charge 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 ℃;
Reaction pressure: 1.0 MPaG;
Concentrated formaldehyde and methanol feeding ratio: 1:1;
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
Take ionic liquid as catalyzer, using methylal and concentrated formaldehyde as reactant, at reactor, carry out continuous acetalation, ionic-liquid catalyst accounts for 0.1 ~ 10wt% of reaction raw materials, the mol ratio of concentrated formaldehyde and methylal is 1.0 ~ 3.0, and reaction product is mainly the DMM1-6 that reaction generates;
Or take ionic liquid as catalyzer, using methyl alcohol and concentrated formaldehyde as reactant, at reactor, carry out continuous acetalation, 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, through the first light constituent recovery tower C1, be separated into the first light constituent and reaction mixture, the first light constituent condensing reflux continues reaction to reactor R1, and reaction 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 R1 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 materials such as 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 controlled by 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. a multi-reaction kettle system that adopts ionic-liquid catalyst continuous production polymethoxy dimethyl ether, it is characterized in that, it comprises raw material premixing tank V1, raw material premixing tank V2, reactor R1, reactor R2, 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, raw material premixing tank V2 is connected with the opening for feed of reactor R2, the discharge port of reactor R2 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 E3.
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; Described reactor R2 is stirred autoclave, is further provided with reaction temperature control unit E2.
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 (2)
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| CN106800500A (en) * | 2017-01-17 | 2017-06-06 | 凯瑞环保科技股份有限公司 | A kind of process for preparing polymethoxy dimethyl ether |
| CN109761766A (en) * | 2019-01-31 | 2019-05-17 | 天津大学 | A kind of separating technology of the polymethoxy dimethyl ether system containing formaldehyde |
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Application publication date: 20140903 |