CN204727802U - Prepare the system of polymethoxy dimethyl ether - Google Patents
Prepare the system of polymethoxy dimethyl ether Download PDFInfo
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- CN204727802U CN204727802U CN201420701828.5U CN201420701828U CN204727802U CN 204727802 U CN204727802 U CN 204727802U CN 201420701828 U CN201420701828 U CN 201420701828U CN 204727802 U CN204727802 U CN 204727802U
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- dimethyl ether
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- polymethoxy dimethyl
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Abstract
The utility model relates to a kind of system preparing polymethoxy dimethyl ether.This system comprises multi-stage reacting kettle and shell and tube cross-flow filtration device.Described multi-stage reacting kettle can receive reaction raw materials and solid catalyst to prepare polymethoxy dimethyl ether.Described shell and tube cross-flow filtration device is arranged at the downstream of the reactor that arbitrary level is closed on and receives from the mixed slurry of this reactor, isolates at least part of described solid catalyst to carry out filtration treatment to described mixed slurry.
Description
Technical field
The utility model relates to one and prepares polymethoxy dimethyl ether (Polyoxymethylene dimethyl-ethers, be called for short DMMn, n=3 ~ 8) system, particularly relate to a kind of system preparing polymethoxy dimethyl ether with catalyst separation device.
Background technology
The lower molecular weight acetals polymkeric substance that polymethoxy dimethyl ether is a class take Methylal(dimethoxymethane) as parent, sub-methoxyl group is main chain, its general formula is expressed as: CH
3o (CH
2o)
ncH
3.DMMn is the blend component of the clean diesel of generally acknowledging in the world, its cetane value up to 76, oxygen level 47% ~ 50%, without sulphur, without aromatic hydrocarbons, in diesel oil, concoct 10% ~ 20%, significantly can reduce cold filter point of diesel oil, and can significantly reduce the pollutant emissions such as tail gas solid particulate matter, NOx and CO.Physical property and the diesel oil of DMMn are close, and being blended in diesel oil to use does not need to transform vehicle motor and oil supply system.
The synthesis material of DMMn mainly comprises two portions, and a part is to provide the compound of paraformaldehyde, comprises formaldehyde solution, trioxymethylene, paraformaldehyde etc.; Another part provides end-caps, comprises methyl alcohol, dme, methylal etc.Preparation DMMn concrete technology research in, the raw material of employing and the kind of catalyzer all incomplete same, can be divided into by catalyst type difference: liquid acid catalysis method, solid acid catalysis method, ionic liquid-catalyzed method and metal oxide oxidation catalyst method etc.
In synthesis technique, normal employing liquid mineral acid is catalyzer in early days, and the United States Patent (USP) (patent No. is US2,449,469) as Dupont company uses the catalysis methanol such as sulfuric acid or hydrochloric acid, formaldehyde or paraformaldehyde synthesis DMMn.In recent years, be in the news with the multiple synthetic method that BASF and BP company is representative, as U.S. Patent Application Publication US2007/0260094A1 and Chinese patent CN101048357A all discloses the method for synthesis DMMn, it adopts an acidic catalyst (such as, mineral acid, sulfonic acid, heteropolyacid, acidic ion exchange resin, molecular sieve, silico-aluminate, silicon-dioxide, aluminum oxide, titanium dioxide and zirconium dioxide) to carry out catalysis methylal and trioxymethylene reaction obtains DMMn.In addition, Chinese patent CN102775284A discloses a kind of method using acid Pd/carbon catalyst to synthesize DMMn, and product main ingredient is DMM1-6; Chinese patent CN102320941A also discloses a kind of method using solid superacid as catalyst methyl alcohol and formaldehyde synthesis DMMn, substitutes trioxymethylene with formaldehyde.But use mineral acid or liquid acid to catalyze and synthesize DMMn in the synthetic method of above-mentioned DMMn, there is equipment corrosion and separation difficulty problem in it, thus adds follow-up intractability and cost, is unfavorable for using widely.
More existing during attempt, it uses solid acid to alleviate the problem of equipment corrosion as catalyzer, but it exists the problems such as the selectivity of target product DMMn is lower, in order to improve catalyst activity, usually solid catalyst is made ultrafine particle.But when reclaiming solid catalyst, adopt common settling process can cause with the superfine catalyst particle in separating reaction still the problem that settling time loss loss that is long, catalyzer is large, the separation and recovery of giving catalyzer are brought certain difficulty.
So need to provide a kind of system preparing polymethoxy dimethyl ether newly, it can while effectively preparing polymethoxy dimethyl ether, and the effective solid catalyst of energy, is convenient to reuse solid catalyst, saves cost.
Utility model content
The utility model embodiment provides a kind of system preparing polymethoxy dimethyl ether.This system comprises multi-stage reacting kettle and shell and tube cross-flow filtration device.Described multi-stage reacting kettle can receive reaction raw materials and solid catalyst to prepare polymethoxy dimethyl ether.Described shell and tube cross-flow filtration device is arranged at the downstream of the reactor that arbitrary level is closed on and receives from the mixed slurry of this reactor, isolates at least part of described solid catalyst to carry out filtration treatment to described mixed slurry.
The utility model another embodiment provides for a kind of system preparing polymethoxy dimethyl ether.This system comprises multi-stage reacting kettle, shell and tube cross-flow filtration device and spiral liquid separation device.Described multi-stage reacting kettle can receive reaction raw materials and solid catalyst to prepare polymethoxy dimethyl ether.Described shell and tube cross-flow filtration device is arranged at the downstream of last step reactor and receives from the mixed slurry of this reactor, isolates at least part of described solid catalyst to carry out filtration treatment to described mixed slurry.Described spiral liquid separation device is arranged between described shell and tube cross-flow filtration device and described last step reactor, in order to carry out rotary filter press to the mixed slurry from this reactor; Wherein, described shell and tube cross-flow filtration device can receive the part mixed slurry that is separated from this spiral liquid separation device to isolate solid catalyst wherein.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the utility model prepares a system embodiment of polymethoxy dimethyl ether; And
Fig. 2 is the schematic diagram that the utility model prepares another embodiment of the system of polymethoxy dimethyl ether.
Embodiment
Below will describe the specific embodiment of the present invention, and it is pointed out that in the specific descriptions process of these embodiments, in order to carry out brief and concise description, this specification sheets can not all do detailed description to all features of the embodiment of reality.Should be understandable that; in the actual implementation process of any one embodiment; as in the process of any one engineering project or design item; in order to realize the objectives of developer; in order to meet that system is correlated with or that business is relevant restriction; usually can make various concrete decision-making, and this also can change to another kind of embodiment from a kind of embodiment.In addition, it will also be appreciated that, although effort done in this performance history may be complicated and tediously long, but for those of ordinary skill in the art relevant to content disclosed by the invention, some designs that the basis of the technology contents of disclosure exposure is carried out, manufacture or production etc. changes just conventional technique means, not should be understood to content of the present disclosure insufficient.
Unless otherwise defined, the technical term used in claims and specification sheets or scientific terminology should be in the technical field of the invention the ordinary meaning that the personage with general technical ability understands." first ", " second " that use in patent application specification of the present invention and claims and similar word do not represent any order, quantity or importance, and are only used to distinguish different integral parts.The similar word such as " one " or " one " does not represent quantity limitation, but represents to there is at least one." comprise " or the similar word such as " comprising " mean to appear at " comprising " or " comprising " before element or object contain the element or object and equivalent element thereof that appear at " comprising " or " comprising " presented hereinafter, do not get rid of other elements or object." connection " or " being connected " etc. similar word be not defined in physics or the connection of machinery, be also not limited to direct or indirectly connect.
Fig. 1 is the schematic diagram that the utility model prepares system 10 1 embodiments of polymethoxy dimethyl ether.It should be noted that embodiment of the present utility model is only schematic, it is not construed as limiting the preparation system of reality.In some instances, system 10 also can comprise other any suitable devices jointly complete polymethoxy dimethyl ether preparation and be separated in native system 10 use solid catalyst.
As shown in Figure 1, system 10 includes reactor 11, first row tubular cross flow filtration unit 12, secondary series tubular cross flow filtration unit 13 and product storing device 14.In the present embodiment, system 10 includes the first step and is arranged in series and the reactor 11 of fluid communication to the 8th grade, and partial reaction still 11 is provided with catalyst inlet and feed(raw material)inlet.In non-restrictive example, system 10 also can be provided with 3 to 8 multi-stage reacting kettles 11 to prepare polymethoxy dimethyl ether.The polymethoxy dimethyl ether prepared through multi-stage reacting kettle 11 is finally stored in product storing device 14.In embodiment of the present utility model, when arranging 8 reactors 11, first and the 4th reactor 11 are provided with catalyst inlet and feed(raw material)inlet for adding live catalyst and reaction raw materials.
In the embodiment shown in fig. 1, first row tubular cross flow filtration unit 12 to be arranged between third stage reactor 11 and fourth stage reactor 11 and with the two fluid communication.The reacted mixed slurry that this first row tubular cross flow filtration unit 12 can receive from third stage reactor 11 carries out separating and filtering, and described mixed slurry comprises the complete raw material of reaction product, unreacted and solid catalyst.Pulpous state fluid 15 after separation enters in next stage (fourth stage) reactor 11 and further reacts, the solid catalyst simultaneously separated and complete the returning to flow in first step reactor 11 containing pulpous state reactant 16 circulations of solid sub-material and realize recycling of unreacted.
Similar, secondary series tubular cross flow filtration unit 13 to be arranged between the 8th order reaction still 11 and product storing device 14 and with the two fluid communication.The reacted mixed slurry (mark) that this secondary series tubular cross flow filtration unit 13 can receive from the 8th order reaction still 11 carries out separating and filtering.The polymethoxy dimethyl ether 17 of the preparation after separation enters in product storing device 14, the solid catalyst simultaneously separated and complete the returning to flow in first step reactor 11 containing pulpous state reactant 18 circulations of solid sub-material and realize recycling of unreacted.
Spent catalyst 19 after reaction inactivation also can directly be discharged into system outside without recycling.In addition, the carrying out adding live catalyst to promote reaction can be supplemented as required in reaction process.In this example, in first and fourth stage reactor 11 supplement add live catalyst.
As mentioned above, the utility model example is only schematic.In some instances, system 10 can arrange at least one shell and tube cross-flow filtration device, and the downstream that shell and tube cross-flow filtration device can be arranged at arbitrary order reaction still 11 is used for carrying out filtering separation to the mixed slurry from this order reaction still 11.Solid catalyst after separation can be returned at least one reactor of corresponding shell and tube cross-flow filtration device upstream and recycle.
In non-restrictive example, shell and tube cross-flow filter is made up of porous filter core material, and this porous filter core material adopts porous ceramics, sintering metal, porous sintered plastics, metallic fiber sintered felt or multilayer metal sintering net.In some instances, the pore diameter range of porous filter core material is 1 ~ 300 μm, and its aperture can regulate its size according to the order difference of shell and tube cross-flow filter position, the aperture with the order porous filter core material of strainer from leading portion to latter end can by diminishing gradually greatly.
Like this, in the process preparing polymethoxy dimethyl ether (DMMn), the position at shell and tube cross-flow filter place in reactive system optionally can be regulated according to the kind of reaction raw materials and varying in size of catalyzer ultrafine particle also to regulate the pore size of porous filter core material neatly, thus reach effectively the control polymerization degree of polyreaction and the requirement of DMMn quality product.
Fig. 2 is the schematic diagram that the utility model prepares another embodiment of system 10 of polymethoxy dimethyl ether.As shown in Figure 2, system 10 includes reactor 20, spiral liquid separation device 21, shell and tube cross-flow filtration device 22 and slurry tank 23.In the present embodiment, system 10 includes the first step to level V series-parallel connection setting and the reactor 20 of fluid communication, each reactor 20 is provided with catalyst inlet and facilitates reaction to generate polymethoxy dimethyl ether in order to injecting catalyst.In non-restrictive example, system 10 also can be provided with 3 reactors 20 communicated to 8 multiple stage fluids.The reactor 20 of intermediate stage receives the mixed slurry of upper level reactor, and the slurry transferring generated is carried out further reacting preparing polymethoxy dimethyl ether to next stage reactor.The preparation of polymethoxy dimethyl ether is finally completed through multi-stage reacting kettle 20.
In the reaction, reaction raw materials 24 enters in first step reactor 20 and reacts, and reacted mixed slurry flows into section by section in next stage reactor 20 and continues reaction.First the reacted mixed slurry 25 flowed out from last step (being level V in this example) reactor 20 carries out solid-liquid separation by spiral liquid separation device 21, take liquid as the top inflow shell and tube cross-flow filtration device 22 of mixed slurry 26 from spiral liquid separation device 21 of principal constituent, and be the bottom inflow slurry tank 23 of mixed slurry 27 from spiral liquid separation device 21 of principal constituent with solid catalyst.
Be that the mixed slurry 26 of principal constituent carries out further solid-liquid separation by shell and tube cross-flow filtration device 21 with liquid, product filtrate 28 flows into product stock tank (not shown), the solid catalyst after filtering and the fluid 29 that formed containing the complete particulate reaction raw materials of a small amount of unreacted then capable of circulation return to flow in last step (level V) reactor 20 realize recycling.In non-restrictive example, fluid 29 also can return in preposition arbitrary order reaction still 20 and realize recycling.
Be that mixed slurry 27 further sedimentation in slurry tank 23 of principal constituent is flowed out from its underpart with solid catalyst, after filtering separation by follow-up filtering unit 30, the solid catalyst of separation and enter to return preposition at least one after blend tank 32 mixes with live catalyst and fresh reactant raw material reactor 20 is interior containing the particulate reaction raw materials 31 that a small amount of unreacted is complete and realize recycling.The reacted mixing liquid 33 being entrained with a small amount of solid catalyst flowed out from slurry tank 23 top flow into shell and tube cross-flow filter again and carries out further solid-liquid separation.
Embodiment shown in this example is only schematic.In other examples, also any first order reaction still downstream can be provided with shell and tube cross-flow filtration device 22 and filtering separation is carried out to the slurry (or fluid) from this reactor.In non-restrictive example, also may correspond to each shell and tube cross-flow filtration device and be provided with spiral liquid separation device at its upstream, thus shell and tube cross-flow filtration device can carry out further filtering separation to the fluid from spiral liquid separation device.
In the utility model example, the continuous on-line filtration unit that system 10 uses spiral liquid separation device 21 to combine with shell and tube cross-flow filtration device 22 carrys out filtering catalyst.Similar to the shell and tube cross-flow filtration device used in Fig. 1, shell and tube cross-flow filtration device 22 is made up of porous filter core material, and described porous filter core material adopts porous ceramics, sintering metal, porous sintered plastics, metallic fiber sintered felt or multilayer metal sintering net.
In some instances, the pore diameter range of the porous filter core material of shell and tube cross-flow filtration device 22 is 1 ~ 300 μm, and its aperture can regulate its size according to the order difference of shell and tube cross-flow filter position, the aperture with the order porous filter core material of strainer from leading portion to latter end can by diminishing gradually greatly.
Like this, the continuous on-line filtration unit that the rotary filter press that this example provides combines with cross-flow filtration, in the process preparing polymethoxy dimethyl ether (DMMn), the sharp separation effect of spiral liquid separation device and the accurate separating effect of shell and tube cross-flow filtration device are combined effectively, play distinctive stalling characteristic each other to greatest extent, thus improve the production efficiency preparing polymethoxy dimethyl ether.
What the utility model provided the catalyzer continuous filtration unit prepared in polymethoxy dimethyl ether process can reclaim ultrafine solids catalyzer effectively, reduces the loss of catalyzer in sepn process, reduces the loss of catalyzer, improves the service efficiency of catalyzer.In addition, the catalyzer continuous filtration unit that the utility model provides optionally can change the operating parameters of filtering system according to the difference of reaction conditions, to meet the needs of variant production quality.Annexation between the filtration unit that the utility model provides and reactor is simple, is easy to dismounting, conveniently cleans and changes.
The utility model compared with prior art can realize continuous prodution object in the reactor of plural serial stage arranging cross-current type on-line filtration system, enhances productivity.Catalyst separating is fast, efficiency is high, reduces the loss loss of catalyzer in separation engineering, reduces production cost.
Be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.A series of detailed description listed is above only illustrating for possible embodiments of the present invention; they are also not used to limit the scope of the invention, all do not depart from the skill of the present invention Equivalent embodiments done of spirit or change all should be included within protection scope of the present invention.
Claims (10)
1. prepare a system for polymethoxy dimethyl ether, comprising:
Multi-stage reacting kettle, it can receive reaction raw materials and solid catalyst to prepare polymethoxy dimethyl ether; And
Shell and tube cross-flow filtration device, its downstream being arranged at the reactor that arbitrary level is closed on also receives the mixed slurry from this reactor, isolates at least part of described solid catalyst to carry out filtration treatment to described mixed slurry.
2. the system preparing polymethoxy dimethyl ether according to claim 1, is characterized in that, described shell and tube cross-flow filtration device can carry isolated solid catalyst described in it in preposition at least one reactor of this shell and tube cross-flow filtration device.
3. the system preparing polymethoxy dimethyl ether according to claim 1, is characterized in that, described multi-stage reacting kettle is arranged in series, and it includes 3 to 8 reactors be arranged in series.
4. the system preparing polymethoxy dimethyl ether according to claim 1, it is characterized in that, this system is provided with spiral liquid separation device further, it is arranged between the preposition reactor that described shell and tube cross-flow filtration device and this shell and tube cross-flow filtration device close on, in order to carry out rotary filter press to the mixed slurry from this reactor; Described shell and tube cross-flow filtration device can receive the part mixed slurry that is separated from this spiral liquid separation device to isolate solid catalyst wherein.
5. the system preparing polymethoxy dimethyl ether according to claim 4, is characterized in that, described shell and tube cross-flow filtration device is arranged at the downstream of last step reactor, and described multi-stage reacting kettle is series-parallel reaction still.
6. the system preparing polymethoxy dimethyl ether according to claim 4, is characterized in that, described shell and tube cross-flow filtration device carries its isolated solid catalyst in described last step reactor.
7. the system preparing polymethoxy dimethyl ether according to claim 4, it is characterized in that, this system is provided with slurry tank further, and is arranged at the downstream of described spiral liquid separation device, is used for carrying out settlement treatment to the mixed slurry from described spiral liquid separation device.
8. the system preparing polymethoxy dimethyl ether according to claim 7, is characterized in that, the liquid that described slurry tank can carry its top to flow out processes in described shell and tube cross-flow filtration device.
9. the system preparing polymethoxy dimethyl ether according to claim 7, it is characterized in that, this system is provided with blend tank further, and it can receive the solid catalyst in the fluid flowed out from described slurry tank bottom, and the mixed slurry after conveying allotment is in preposition every first order reaction still.
10. prepare a system for polymethoxy dimethyl ether, comprising:
Multi-stage reacting kettle, it can receive reaction raw materials and solid catalyst to prepare polymethoxy dimethyl ether;
Shell and tube cross-flow filtration device, its downstream being arranged at last step reactor also receives the mixed slurry from this reactor, isolates at least part of described solid catalyst to carry out filtration treatment to described mixed slurry; And
Spiral liquid separation device, it is arranged between described shell and tube cross-flow filtration device and described last step reactor, in order to carry out rotary filter press to the mixed slurry from this reactor; Wherein, described shell and tube cross-flow filtration device can receive the part mixed slurry that is separated from this spiral liquid separation device to isolate solid catalyst wherein.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420701828.5U CN204727802U (en) | 2014-11-20 | 2014-11-20 | Prepare the system of polymethoxy dimethyl ether |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420701828.5U CN204727802U (en) | 2014-11-20 | 2014-11-20 | Prepare the system of polymethoxy dimethyl ether |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926627A (en) * | 2014-12-26 | 2015-09-23 | 北京东方红升新能源应用技术研究院有限公司 | Continuous reaction device for synthetizing polymethoxy dimethyl ether |
| CN106278836A (en) * | 2016-08-16 | 2017-01-04 | 鄂尔多斯市易臻石化科技有限公司 | Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether |
| CN107138101A (en) * | 2017-06-27 | 2017-09-08 | 查都（上海）科技有限公司 | A kind of system of acetylene and formaldehyde deep reaction |
-
2014
- 2014-11-20 CN CN201420701828.5U patent/CN204727802U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926627A (en) * | 2014-12-26 | 2015-09-23 | 北京东方红升新能源应用技术研究院有限公司 | Continuous reaction device for synthetizing polymethoxy dimethyl ether |
| CN106278836A (en) * | 2016-08-16 | 2017-01-04 | 鄂尔多斯市易臻石化科技有限公司 | Intermediate concentration formaldehyde and the apparatus and method of methylal synthesis polymethoxy dimethyl ether |
| CN107138101A (en) * | 2017-06-27 | 2017-09-08 | 查都（上海）科技有限公司 | A kind of system of acetylene and formaldehyde deep reaction |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151028 Termination date: 20191120 |