CN104003855B - Methyl alcohol is the system of initial reaction raw material continuous production polymethoxy dimethyl ether - Google Patents
Methyl alcohol is the system of initial reaction raw material continuous production polymethoxy dimethyl ether Download PDFInfo
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- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
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Abstract
The invention discloses the system that a kind of methyl alcohol is initial reaction raw material continuous production polymethoxy dimethyl ether, mainly comprise that formaldehyde prepares unit, methylal prepares unit and polymethoxy dimethyl ether prepares unit: the Main Function that formaldehyde prepares unit is under the effect of catalyzer, and material benzenemethanol is oxidized to formaldehyde solution; The effect that methylal prepares unit is under the effect of solid acidic resin catalyst, part formaldehyde solution and methyl alcohol is reacted, is prepared into methylal; The effect that polymethoxy dimethyl ether prepares unit is under the effect of ionic-liquid catalyst, methyl alcohol, methylal respectively with the condensation reaction of formaldehyde solution, prepare polymethoxy dimethyl ether, reaction product, after separating-purifying, obtains polymethoxy dimethyl ether product.The present invention is compared to trioxymethylene or paraformaldehyde route, and its flow process is simple, and energy consumption is low, simple to operate, in the implementation while product recycling, also achieves the recycling of sewage, is very applicable to large-scale industrial production.
Description
Technical field
The invention discloses a kind of using methyl alcohol as initial reaction raw material, the process unit system of continuous production polymethoxy dimethyl ether.
Background technology
Along with the minimizing day by day of petroleum resources, and the demand of countries in the world to fuel oil is growing, and the research and development of various countries to novel energy all increase dynamics.
Along with the continuous lifting of rapid development of economy and living standards of the people, China constantly increases petroleum demand, and due to scarcity of resources, China became net importer from 1993 from net exporter, and external dependence degree improves year by year, and 2012 years more than 55%.Petroleum resources have become one of the most responsive, weakest link affecting economical operation.In recent years along with the quick growth of vehicle guaranteeding organic quantity, the consumption of oil product sharply increases, and the pollution that fuel oil causes is also day by day serious.The current carbon monoxide in big city more than 80%, the oxynitride of more than 40%, from automotive emission.
In the face of the contradiction of resource, environment and economic development, national conditions in conjunction with China are exploited natural resources the coal-based chemical industry product innovation of relative abundance, under the prerequisite of efficiency utilization methyl alcohol, the blend component of clean diesel is produced with Non oil-based route technological development, supplement the deficiency of China's clean diesel, be very important.
China is coal production state maximum in the world, and 75% of current China coal mining amount uses as fuel poor benefit, and synthetic gas and methyl alcohol become the main outlet of Coal Chemical Industry.The nineties in last century, due to oil crisis, coal liquifaction and methanol-to-olefins technology obtain exploitation, but because raw material availability is less than 45%, energy expenditure is high, and at substantial water resources, its technical development and industrial application are very limited.
Coal-based methanol is China's development Chemical Industry the most rapidly, and be the product of the first link in Chemical Industry chain, its downstream may extend to other Chemicals multiple.According to the latest data display that Chinese nitrogen fertilizer industry association issues, by the end of the year 2012, China's methyl alcohol aggregated capacity will reach 5149.1 ten thousand tons, account for 50% of global aggregated capacity.The whole industry methanol device duty ratio that goes into operation improves 4.3 percentage points last year, but still only has 60.8%, and output is 3,129 ten thousand tons, Apparent con-sumption 3,622 ten thousand tons, and production capacity surplus situation is serious, and existing consumer field cannot digest the production capacity increased fast.
The production of the output of methyl alcohol and consumption and derived product and utilisation technology are developed closely related, there is technology barrier at present in the exploitation of this type of products production technology.Develop these domestic markets in short supply, particularly can the Downstream Products of Methanol production technology of petroleum replacing Chemicals, be not only methyl alcohol problem of excess production capacity to find a way out, and be the important technology route producing clean fuel oil from coal, be conducive to making up China's oil problem in short supply, promote that China's methanol industry develops well.
Polymethoxy dimethyl ether take methoxyl group as the lower molecular weight acetal polymer of main chain, and general formula is CH
3(OCH
2)
noCH
3, be high boiling point colourless liquid, can be used as the properties-correcting agent of resol, solvent, softening agent and releasing agent etc.The compound of n=3 ~ 6 is diesel oil oxygenation agents of a kind of excellent property, its physical property is close with diesel oil, not only have very high cetane value, its oxygen level is also very high, when adding 15% in diesel oil, do not need to transform vehicle motor oil supply system, obviously can improve the combustioncharacteristics of diesel oil, improve diesel quality, increase oxygen level more than 7%, reduce discharging the tail gas pollution of more than 50%, significantly reduce the discharge of oxynitrides and carbon monoxide.
Polymethoxy dimethyl ether (DMMn) getting up early adopts methyl alcohol, formaldehyde, concentrated formaldehyde, paraformaldehyde or ethylene glycol acetal to be raw material, with sulfuric acid or hydrochloric acid catalysis synthesis.In recent years, BASF AG (WO 2006/045506 A1, CA 2581502) uses the protonic acid such as sulfuric acid, trifluoromethanesulfonic acid to be catalyzer, methyl alcohol and trioxymethylene (or paraformaldehyde) are raw material, react 8 ~ 12h, obtain the content of DMM3-8 lower than 26% at 100 DEG C.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 react and carry out under the N2 of 1.0MPa, shorten the reaction times widely, 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 with methyl alcohol, formaldehyde, dme and methyl alcohol for raw material, wherein the content of DMM3-8 only has 11.6%.The method catalyst activity is low, complex process, is difficult to realize industrialization.
Summary of the invention
In order to overcome the deficiencies in the prior art, main purpose of the present invention is to provide the system that methyl alcohol is initial reaction raw material continuous production polymethoxy dimethyl ether.
Methyl alcohol is a system for initial reaction raw material continuous production polymethoxy dimethyl ether, and it comprises, and formaldehyde prepares unit, methylal prepares unit and polymethoxy dimethyl ether prepares unit,
A, formaldehyde prepare unit
Using methyl alcohol, air and water vapour as reactant, after evaporation gasification, enter the reaction carrying out continuous print producing formaldehyde by methanol oxidation in reactor, reaction product is after absorption tower absorbs, obtain two bursts of formaldehyde solutions as intermediate product, wherein one is supplied to polymethoxy dimethyl ether as raw material and prepares unit, and one formaldehyde solution is supplied to methylal as raw material and prepares unit in addition;
B, methylal prepare unit
Prepare unit and polymethoxy dimethyl ether from formaldehyde respectively to prepare unit and to come the solution of two strands of by-products containing formaldehyde, with methanol solution after proportioning, enter reactive distillation column reaction and prepare methylal solution, reaction product, after rectification and purification, obtains highly purified methylal solution; After water reactive distillation process in formaldehyde solution, reach effluent-disposal standard and be directly sent to sewage treatment unit;
C, polymethoxy dimethyl ether prepare unit
The formaldehyde solution that unit comes is prepared from formaldehyde, the methylal solution that unit comes is prepared with methyl alcohol and from methylal, under the effect of ionic-liquid catalyst, polymethoxy dimethyl ether is generated through acetalation, reaction product is after rectification process, obtain polymethoxy dimethyl ether product and one contains the solution of formaldehyde, then should return methylal and prepare unit and carry out formaldehyde and recycle process by the solution containing formaldehyde.
Described formaldehyde prepares unit, and it comprises methanol evaporator E101, formaldehyde reaction device R101, the first absorption tower C110, second absorption tower C120; Methanol evaporator E101 is connected with the opening for feed of formaldehyde reaction device R101, the discharge port of formaldehyde reaction device R101 is connected with the opening for feed of the first absorption tower C110, first absorption tower C110 tower top is connected with the opening for feed of second absorption tower C120, the tower top of second absorption tower C120 is connected with the opening for feed of methanol evaporator E101, and the tower reactor of second absorption tower C120 is connected with the tower top feeding line of the first absorption tower C110.
Described methylal prepares unit, and it comprises methylal pre-reactor R201, reactive distillation column C210, methylal rectifying tower C220, component recovery tower C230; Methylal pre-reactor R201 is connected with the opening for feed of reactive distillation column C210, the tower top of reactive distillation column C210 is connected with the opening for feed of methylal rectifying tower C220, methylal rectifying tower C220 tower top is connected with the opening for feed of component recovery tower C230, the tower top of component recovery tower C230 is connected with the refluxing opening of reactive distillation column C210, and the tower reactor of component recovery tower C230 is connected with methylal pre-reactor R201 feeding line.
Described polymethoxy dimethyl ether prepares unit, and it comprises reactor R301, the first light constituent recovery tower C310, extraction tower C320, soda-wash tower C330, the second light constituent recovery tower C340, extraction agent recovery tower C350, the 3rd light constituent recovery tower C360, vaporizer E301, the discharge port of reactor R301 is connected with the opening for feed of the first light constituent recovery tower C310, first light constituent recovery tower C310 tower reactor is connected with the opening for feed of extraction tower C320, the tower top of extraction tower C320 is connected with the opening for feed of soda-wash tower C330, the tower top of soda-wash tower C330 is connected with the opening for feed of the second light constituent recovery tower C340, second light constituent recovery tower C340 tower reactor is connected with the opening for feed of extraction agent recovery tower C350, the tower reactor of extraction agent recovery tower C350 is connected with the opening for feed of the 3rd light constituent recovery tower C360, the tower top of the 3rd light constituent recovery tower C360 is connected with the feed-pipe of reactor R301, the tower top of extraction agent recovery tower C350 is connected with the feed-pipe of extraction tower C320, the tower top of the second light constituent recovery tower C340 is connected with the feed-pipe of reactor R301, the tower reactor of extraction tower C320 is connected with the feed-pipe of reactor R301 by vaporizer E301.
Described formaldehyde prepares the second absorption tower C120 tower reactor of unit, is that the opening for feed of the methylal pre-reactor R201 preparing unit with methylal is connected.
Described formaldehyde prepares the first absorption tower C110 tower reactor of unit, is that the opening for feed of the reactor R301 preparing unit with polymethoxy dimethyl ether is connected.
Described methylal prepares the methylal rectifying tower C220 tower reactor of unit, is that the opening for feed of the reactor R301 preparing unit with polymethoxy dimethyl ether is connected.
Described polymethoxy dimethyl ether prepares the another one outlet of the vaporizer E301 of unit, is that the opening for feed of the reactor R201 preparing unit with methylal is connected.
The polymethoxy dimethyl ether ionic-liquid catalyst prepared described in unit is acidic ionic liquid catalysts, cationic moiety be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one or more in pyridylium and heterocyclic onium cations, 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.
Beneficial effect of the present invention: prepare polymethoxy dimethyl ether for the route of formaldehyde and methylal intermediates by Methanol, it is a brand-new preparation system, compared with preparing polymethoxy dimethyl ether with trioxymethylene, paraformaldehyde, paraformaldehyde route, its flow process simplifies greatly, facility investment, simple to operate, all large reduction of energy consumption, be very applicable to large-scale industrial production.
Linking between unit is very smooth, compared with reclaiming the formaldehyde solution of by-product with the high-pressure rectification of other devices, this device can well be recycled formaldehyde and prepare the formaldehyde solution that unit and polymethoxy dimethyl ether prepare unit by-product, make it turn waste into wealth, make it become polymethoxy dimethyl ether prepare the reaction raw materials of unit and reuse, high-pressure rectification reclaims formaldehyde, can not energy consumption large, in High Temperature High Pressure situation, formaldehyde is strong to equipment corrosion, equipment material requires high, by route of the present invention, then greatly reduces investment and the energy consumption of equipment.
The formaldehyde-containing wastewater produced in native system, unified recovery enters methylal and prepares unit and recycle, its treating processes is simple, and energy consumption is low, can reach the emission standard of sewage work after process, the useful component in efficient recovery formaldehyde waste water.
Accompanying drawing explanation
Fig. 1 is the structural representation of present system, only draws main equipment, and other the equipment such as instrument, pump, valve, tundish omits.
Embodiment
As shown in Figure 1,
A, formaldehyde prepare unit
Formaldehyde prepares unit, and it comprises methanol evaporator E101, formaldehyde reaction device R101, the first absorption tower C110, second absorption tower C120.Methyl alcohol, air and water vapour, in certain proportion, enter into vaporizer E101, after evaporator E101 evaporation gasification, enter in formaldehyde reaction device R101, under the effect of silver catalyst, carry out the reaction that continuous print methanol oxidation generates formaldehyde, reaction product is after the first absorption tower C110 and second absorption tower C120 absorbs, obtain two bursts of formaldehyde solutions as intermediate product, wherein, the formaldehyde solution that first absorption tower C110 tower reactor is produced, the reactor R301 of polymethoxy dimethyl ether for unit is supplied to as raw material, the formaldehyde solution of second absorption tower C120 tower reactor institute by-product, the methylal pre-reactor R201 that methylal prepares unit is supplied to as raw material.
Wherein, the mol ratio of air and methyl alcohol is 1.5 ~ 1.7, and the mol ratio of water vapour and methyl alcohol is the concentration of formaldehyde that the 0.1 ~ 0.5, first absorption tower C110 tower reactor is produced is 60% ~ 80%, and the formaldehyde solution concentration of second absorption tower C120 tower reactor institute by-product is 15% ~ 25%.
B, methylal prepare unit
Methylal prepares unit, and it comprises methylal pre-reactor R201, reactive distillation column C210, methylal rectifying tower C220, component recovery tower C230;
Prepare the second absorption tower C120 tower reactor of unit and polymethoxy dimethyl ether from formaldehyde respectively to prepare unit vaporizer E301 and to come two bursts of formaldehyde solutions, with methanol solution after proportioning, enter methylal pre-reactor R201 and carry out pre-reaction, reaction product enters reactive distillation column C210 continuation reaction again and prepares methylal, reaction product is after methylal rectifying tower C220 rectification and purification, obtain highly purified methylal solution, be sent to as raw material the reactor R301 that polymethoxy dimethyl ether prepares unit; The water of reactive distillation column C210 tower reactor, can reach effluent-disposal standard and directly be sent to sewage treatment unit.
Wherein, it is 15% ~ 25% that formaldehyde prepares the formaldehyde solution concentration that unit comes, it is 13% ~ 23% that polymethoxy dimethyl ether prepares the formaldehyde solution concentration that unit comes, and the mass ratio of methyl alcohol and formaldehyde solution is 0.3 ~ 0.5, and the concentration of the methylal solution obtained is 90% ~ 99%.
C, polymethoxy dimethyl ether prepare unit
Polymethoxy dimethyl ether prepares unit, and it comprises reactor R301, the first light constituent recovery tower C310, extraction tower C320, soda-wash tower C330, the second light constituent recovery tower C340, extraction agent recovery tower C350, the 3rd light constituent recovery tower C360, vaporizer E301.The formaldehyde solution that unit comes is prepared from formaldehyde, and prepare from methylal the methylal solution that unit comes, also has methanol solution, send into reactor R301 together, under the effect of ionic-liquid catalyst, generate polymethoxy dimethyl ether through acetalation, reaction product enters into the first light constituent recovery tower C310, the first light constituent then Returning reactor R301 continuation participation reaction of the first light constituent recovery tower C310 recovered overhead, the product mixture at the bottom of tower then sends into extraction tower C320; Product mixture is after extraction tower C320 extracts, tower top extraction phase enters into soda-wash tower C330 and carries out alkali cleaning neutralizing treatment, the catalyzer of tower reactor is then sent into vaporizer E301 mutually and is evaporated, one after evaporator evaporation is containing formaldehyde solution, be sent to as raw material the methylal pre-reactor R201 that methylal prepares unit to carry out repeating to recycle, remaining catalyzer phase in vaporizer, then Returning reactor R301 continues to participate in reaction; Through in soda-wash tower C330 alkali cleaning and after extraction phase, then enter into the second light constituent recovery tower C340 and carry out the second light constituent recovery, the second light constituent then Returning reactor continuation participation reaction of recovered overhead, the extraction phase of tower reactor, then send into the recovery that extraction agent recovery tower C350 carries out extraction agent, after extraction agent recovery tower C350 tower top steams, be back to extraction tower C320 and continue to participate in extraction; Tower reactor component then continues to be fed into the recovery that the 3rd light constituent recovery tower C360 carries out the 3rd light constituent, and the 3rd light constituent, after overhead extraction, is back to reactor R301 and continues to participate in reaction, the tower reactor polymethoxy dimethyl ether product that then output purity is very high.
Wherein, preparing from formaldehyde the formaldehyde solution concentration that unit comes is 60% ~ 80%, the concentration preparing the methylal solution that unit is come from methylal is 90% ~ 99%, going to from vaporizer E301 the concentration that methylal prepares the formaldehyde solution of unit methylal pre-reactor R201 is 13% ~ 23%, and the mol ratio of methyl alcohol, methylal and formaldehyde solution is 2:1:1 ~ 5.
Claims (6)
1. methyl alcohol is a system for initial reaction raw material continuous production polymethoxy dimethyl ether, it is characterized in that, it comprises, and formaldehyde prepares unit, methylal prepares unit and polymethoxy dimethyl ether prepares unit,
A, formaldehyde prepare unit
Using methyl alcohol, air and water vapour as reactant, after evaporation gasification, enter the reaction carrying out continuous print producing formaldehyde by methanol oxidation in reactor, reaction product is after absorption tower absorbs, obtain two bursts of formaldehyde solutions as intermediate product, wherein one is supplied to polymethoxy dimethyl ether as raw material and prepares unit, and one formaldehyde solution is supplied to methylal as raw material and prepares unit in addition; Described formaldehyde prepares unit, and it comprises methanol evaporator E101, formaldehyde reaction device R101, the first absorption tower C110, second absorption tower C120; Methanol evaporator E101 is connected with the opening for feed of formaldehyde reaction device R101, the discharge port of formaldehyde reaction device R101 is connected with the opening for feed of the first absorption tower C110, first absorption tower C110 tower top is connected with the opening for feed of second absorption tower C120, the tower top of second absorption tower C120 is connected with the opening for feed of methanol evaporator E101, and the tower reactor of second absorption tower C120 is connected with the tower top feeding line of the first absorption tower C110;
B, methylal prepare unit
Prepare unit and polymethoxy dimethyl ether from formaldehyde respectively to prepare unit and to come the solution of two strands of by-products containing formaldehyde, with methanol solution after proportioning, enter reactive distillation column reaction and prepare methylal solution, reaction product, after rectification and purification, obtains highly purified methylal solution; After water reactive distillation process in formaldehyde solution, reach effluent-disposal standard and be directly sent to sewage treatment unit; Described methylal prepares unit, and it comprises methylal pre-reactor R201, reactive distillation column C210, methylal rectifying tower C220, component recovery tower C230; Methylal pre-reactor R201 is connected with the opening for feed of reactive distillation column C210, the tower top of reactive distillation column C210 is connected with the opening for feed of methylal rectifying tower C220, methylal rectifying tower C220 tower top is connected with the opening for feed of component recovery tower C230, the tower top of component recovery tower C230 is connected with the refluxing opening of reactive distillation column C210, and the tower reactor of component recovery tower C230 is connected with methylal pre-reactor R201 feeding line;
C, polymethoxy dimethyl ether prepare unit
The formaldehyde solution that unit comes is prepared from formaldehyde, the methylal solution that unit comes is prepared with methyl alcohol and from methylal, under the effect of ionic-liquid catalyst, polymethoxy dimethyl ether is generated through acetalation, reaction product is after rectification process, obtain polymethoxy dimethyl ether product and one contains the solution of formaldehyde, then should return methylal and prepare unit and carry out formaldehyde and recycle process by the solution containing formaldehyde, described polymethoxy dimethyl ether prepares unit, and it comprises reactor R301, the first light constituent recovery tower C310, extraction tower C320, soda-wash tower C330, the second light constituent recovery tower C340, extraction agent recovery tower C350, the 3rd light constituent recovery tower C360, vaporizer E301, the discharge port of reactor R301 is connected with the opening for feed of the first light constituent recovery tower C310, first light constituent recovery tower C310 tower reactor is connected with the opening for feed of extraction tower C320, the tower top of extraction tower C320 is connected with the opening for feed of soda-wash tower C330, the tower top of soda-wash tower C330 is connected with the opening for feed of the second light constituent recovery tower C340, second light constituent recovery tower C340 tower reactor is connected with the opening for feed of extraction agent recovery tower C350, the tower reactor of extraction agent recovery tower C350 is connected with the opening for feed of the 3rd light constituent recovery tower C360, the tower top of the 3rd light constituent recovery tower C360 is connected with the feed-pipe of reactor R301, the tower top of extraction agent recovery tower C350 is connected with the feed-pipe of extraction tower C320, the tower top of the second light constituent recovery tower C340 is connected with the feed-pipe of reactor R301, the tower reactor of extraction tower C320 is connected with the feed-pipe of reactor R301 by vaporizer E301.
2. system according to claim 1, is characterized in that, described formaldehyde prepares the second absorption tower C120 tower reactor of unit, is that the opening for feed of the methylal pre-reactor R201 preparing unit with methylal is connected.
3. system according to claim 1, is characterized in that, described formaldehyde prepares the first absorption tower C110 tower reactor of unit, is that the opening for feed of the reactor R301 preparing unit with polymethoxy dimethyl ether is connected.
4. system according to claim 1, is characterized in that, described methylal prepares the methylal rectifying tower C220 tower reactor of unit, is that the opening for feed of the reactor R301 preparing unit with polymethoxy dimethyl ether is connected.
5. system according to claim 1, is characterized in that, described polymethoxy dimethyl ether prepares the another one outlet of the vaporizer E301 of unit, is that the opening for feed of the reactor R201 preparing unit with methylal is connected.
6. system according to claim 1, it is characterized in that, the polymethoxy dimethyl ether ionic-liquid catalyst prepared described in unit is acidic ionic liquid catalysts, cationic moiety be selected from quaternary ammonium cation, season phosphine positively charged ion, glyoxaline cation, one or more in pyridylium and heterocyclic onium cations, 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.
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| CN104628539B (en) * | 2015-02-04 | 2018-02-13 | 中国科学院兰州化学物理研究所苏州研究院 | The separation method and system of polymethoxy dimethyl ether |
| CN104817440B (en) * | 2015-05-14 | 2016-07-13 | 江苏凯茂石化科技有限公司 | Formaldehyde absorption process unit and method in a kind of polymethoxy dimethyl ether synthesis |
| 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 |
| CN109384652A (en) * | 2017-08-07 | 2019-02-26 | 中国石化扬子石油化工有限公司 | The synthetic method and application of polyethoxy dimethyl ether |
| US10322397B2 (en) * | 2017-09-01 | 2019-06-18 | Gas Technologies Llc | Upgrading of a raw blend into a diesel fuel substitute: poly(dimethoxymethane) |
| CN107721831B (en) * | 2017-11-08 | 2023-05-16 | 无锡赫利邦化工科技有限公司 | Bubbling externally hung reaction system for synthesizing polymethoxy dimethyl ether and synthesis method |
| CN110156575B (en) * | 2019-04-17 | 2023-06-06 | 天津大学 | Reactive distillation-vapor permeation coupling process for polymethoxy dimethyl ether synthesis |
| CN110078600B (en) * | 2019-04-17 | 2023-06-20 | 天津大学 | Reactive distillation process device and method for synthesizing polymethoxy dimethyl ether |
| CN111574340B (en) * | 2020-04-27 | 2023-05-02 | 陈华 | System and method for synthesizing polymethoxy dimethyl ether from methanol |
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