CN105693479A - Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas - Google Patents
Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas Download PDFInfo
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- CN105693479A CN105693479A CN201610147992.XA CN201610147992A CN105693479A CN 105693479 A CN105693479 A CN 105693479A CN 201610147992 A CN201610147992 A CN 201610147992A CN 105693479 A CN105693479 A CN 105693479A
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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
Abstract
The invention discloses a process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas. The raw materials for synthesizing polyoxymethylene dimethyl ethers are the formaldehyde gas and a methylal solution. The process device comprises a fluidized bed reactor, an extracting recovering unit and a refining unit which are connected in sequence, the fluidized bed reactor comprises at least two reaction zones from bottom to top, each reaction zone is filled with a catalyst, the bottom of each reaction zone is provided with a gas distributor which is directly led to the reaction zone, each reaction zone is provided with a downcomer which is communicated with the adjacent reaction zones, and a screen mesh is arranged at the top end of each downcomer; the bottom of the fluidized bed reactor is provided with a formaldehyde gas inlet, and the top of the fluidized bed reactor is provided with a methylal solution inlet. By means of the process device special for preparing polyoxymethylene dimethyl ethers through the formaldehyde gas, the cost is reduced, the synthesizing conversion rate is increased, the yield is low, the good heat-removing effect is achieved, the reaction can be efficiently promoted, and controllability of the conversion degree is achieved.
Description
Technical field
The invention belongs to chemical production technology and equipment technical field, relate generally to special gas formaldehyde and prepare the process unit of polymethoxy dimethyl ether。
Background technology
The feature of China's energy resource structure is: rich coal, gas oil-poor, few, economic maintaining sustained and rapid growth is increasing to energy demand, the contradiction of society, expanding economy and oil supply。Since 2009, crude oil in China external dependence degree exceedes warning line (50%) in continuous 6 years, has a strong impact on the energy strategy safety of China。From China's energy strategy safety, in conjunction with China's primary energy structure feature, Development of Coal base liquid fuel synthetic technology has strategic significance undoubtedly。It addition, China's methanol production capacity is seriously superfluous, exploitation Downstream Products of Methanol, extension Chemical Industry chain, all there is realistic meaning。
Along with science and technology and economic progress, incity, city automobile quantity showed increased, and one of motor vehicle exhaust emission thing major reason becoming city haze。Compared to gasoline, diesel oil has higher boiling point, and H/C mass ratio is low, and therefore in diesel combustion process, the waste gas CO of discharge, oxynitride, particulate matter etc. are more, and the damage ratio gasoline caused is more serious。Therefore, improving diesel combustion efficiency, reduce disposal of pollutants, improving urban air-quality is important at present environmental protection task。
Polymethoxy dimethyl ether is a kind of universally acknowledged cleaning diesel oil component, its Cetane number >=70, not sulfur-bearing, aromatic-free。Add in diesel oil in 5%-20% ratio, it is possible to increase diesel cetane-number, promote burning, it will be apparent that reduce the discharge of the harmful gass such as PM2.5, PM10, NOx, CO in vehicle exhaust。Due to the excellent properties of polymethoxy dimethyl ether, its synthesis technique has become the heat subject of research both at home and abroad。
At present, polymethoxy dimethyl ether is react under the catalytic action of acidic catalyst with one or more in methanol or dimethoxym ethane and formalin/metaformaldehyde/paraformaldehyde to generate mostly。And this reaction is exothermic reaction, temperature height causes and reacts reverse carrying out, it is therefore desirable to withdraw heat。Regardless of whether be paraformaldehyde or all first metaformaldehyde needs heating to parse monomer formaldehyde could to participate in reaction, therefore system reaction temperature is significantly high, it is typically in more than 110 DEG C, and the mode of pressurization must be adopted to prevent the relatively low dimethoxym ethane of boiling point and methanol gasifying, therefore cause that energy consumption is high, equipment requirements is high。Additionally, under hot environment so, monomer formaldehyde has significantly high activity, it is easy to occur dismutation reaction to produce substantial amounts of formic acid, if do not separated by formic acid in system, formic acid can be cumulative and the molecular balance of polymethoxy dimethyl ether is brought significant negative impact, the yield causing reaction reduces, and therefore can only adopt in absorption or alkali and acid stripping method separating formic, cause complex process, and target product yield is low, synthesis cost is high。The selectivity of product DMMn3-8 and the amount of catalyst have close relationship, common fixing bed cannot realize adjusting the product degree of polymerization, thus result in n value too small or excessive, affect product quality。It has been experienced that be best suitable for doing the product that the degree of polymerization is DMMn3-5 of diesel fuel additives。
Summary of the invention
Goal of the invention: for above-mentioned Problems existing and defect, the invention provides a kind of gas formaldehyde and prepare the special process device of polymethoxy dimethyl ether, solve problem low with the cost height, Synthesis conversion and the yield that bring in paraformaldehyde/trimerization production process at present, and the present invention has and well moves thermal effect, being efficiently promoting reaction to carry out, transforming degree achieves controllability。
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of gas formaldehyde prepares the special process device of polymethoxy dimethyl ether, the raw material of described synthesis polymethoxy dimethyl ether is formaldehyde gas and dimethoxym ethane solution, described special process device includes the fluidized-bed reactor being sequentially connected with, extract and recovery unit and refined unit, described fluidized-bed reactor includes at least two-layer conversion zone from bottom to up, every layer of conversion zone is filled with catalyst, and the bottom of every layer of conversion zone all offers gas distributor directly and conversion zone UNICOM of lower floor, every layer of conversion zone is additionally provided with downspout by adjacent conversion zone UNICOM simultaneously, the top of described downspout is additionally provided with silk screen；The bottom of described fluidized-bed reactor is provided with formaldehyde gas entrance, and the top of fluidized-bed reactor arranges dimethoxym ethane solution inlet。
As preferably, described every layer of conversion zone is equipped with Catalyst packing mouth and catalyst discharge port。
As preferably, every layer of conversion zone of described fluidized-bed reactor is additionally provided with filling silk screen module, and described filling silk screen module is cage structure silk screen and is located at above gas distributor。
As preferably, described filling silk screen module is made up of many rustless steel steel wires, and described rustless steel steel wire is Torsion coil steel wire。Torsion coil steel wire in silk screen module of filling in the present invention constitutes the cage structure of multilamellar, make reaction raw materials can obtain maximized contact (especially multiple structure and Torsion coil structure steel wire in the module, accelerate the mixing contact of reaction raw materials, and can quickly remove reaction heat), and make reaction raw materials and catalyst substantially be solidificated in conversion zone reaction, reduce catalyst and pile up at downspout top silk screen with liquid stream。
As preferably, the bottom of described fluidized-bed reactor is provided with reactant liquor discharging opening, and this reactant liquor discharging opening arranges silk screen。
As preferably, described extractant recovery unit includes the lightness-removing column, extraction tower and the extractant recovery tower that are sequentially connected with, and the import of described lightness-removing column is connected with the reactant liquor discharging opening of fluidized-bed reactor, and the top of lightness-removing column is provided with condensation reflux unit。
As preferably, described extraction tower is packed tower or plate column, and the tower top of extraction tower is provided with reactant liquor charging aperture, is provided with extractant feed mouth at the bottom of tower, and reactant liquor and extractant are counter current contacting。
As preferably, described extractant recovery tower is packed tower or plate column, and tower top is connected to condenser and return tank and forms circulation with extractant recovery tower。
As preferably, described fluidized-bed reactor is provided with 4～6 layers of conversion zone。
Beneficial effect: compared with prior art, the invention have the advantages that and solve problem low with the cost height, Synthesis conversion and the yield that bring in paraformaldehyde/trimerization production process at present, and the present invention has and well moves thermal effect, being efficiently promoting reaction to carry out, transforming degree achieves controllability。In the present invention, it is higher that dimethoxym ethane solution fills the dimethoxym ethane concentration in silk screen module when entering into the superiors' conversion zone, with the participation extent of polymerization that can effectively reduce dimethoxym ethane when the bubbling of reactive multilayer section formaldehyde gas contacts, thus controlling the degree of polymerization of upper strata conversion zone, and then the DMMn product degree of polymerization after by reactive multilayer is made to reach expection。
The reaction of the fluidized-bed reactor in the present invention has more better heat transfer property than fixed bed reactors, whether radially still axial temperature Temperature Distribution is all visibly homogeneous, strenuous exercise due to bed, eliminate the laminar boundary layer near heat-transfer area so that it moves the thermal efficiency far above other types reactors such as fixing bed and blank pipes。
Accompanying drawing explanation
Fig. 1 is the structural representation of special process device of the present invention。
Wherein, fluidized-bed reactor 1, lightness-removing column 2, extraction tower 3, extractant recovery tower 4, DMM2 product tower 5, DMM3 ~ 5 product tower 6。
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, it is further elucidated with the present invention, it should be understood that these embodiments are merely to illustrate the present invention rather than restriction the scope of the present invention, after having read the present invention, the amendment of the various equivalent form of values of the present invention is all fallen within the application claims limited range by those skilled in the art。
In the present invention, the preparation referenced patents 104710292A full content of gas formaldehyde, repeats no more in present patent application。
As it is shown in figure 1, polymethoxy dimethyl ether of the present invention synthesis and separating-purifying device, including filling out fluidized-bed reactor, lightness-removing column, extraction tower, extractant recovery tower, DMM2 product tower, DMM3 ~ 5 product tower。Wherein:
Described fluidized-bed reactor includes at least two-layer conversion zone from top to bottom, it is preferred to 4 ~ 6 layers。The lower entrances of every layer of conversion zone arranges gas distributor, makes gas be uniformly distributed entrance bed。Downcomer inlet arranges silk screen, it is prevented that catalyst granules flows to next conversion zone with liquid。Every section of reactor is both needed to arrange catalyst charge mouth and catalyst discharge port。Described fluidized-bed reactor raw material adopts liquid dimethoxym ethane and gas formaldehyde。Liquid dimethoxym ethane is added by fluidized-bed reactor the first conversion zone top, sequentially passes through downspout and arrives last conversion zone。Gas formaldehyde is increased cooling tube by arranging the hot facility of shifting in described fluidized-bed reactor conversion zone as adopted, but this is not necessarily, it is preferable that be not provided with moving hot facility。Described fluidized-bed reactor leaves reactant liquor discharging opening in next section of bottom, and discharging opening arranges silk screen, it is prevented that discharging is catalyst loss。
The fluidized-bed reactor of the present invention includes at least two-layer conversion zone from bottom to up, every layer of conversion zone is filled with catalyst, and the bottom of every layer of conversion zone all offers gas distributor directly and conversion zone UNICOM of lower floor, every layer of conversion zone is additionally provided with downspout by adjacent conversion zone UNICOM simultaneously, and the top of described downspout is additionally provided with silk screen；The bottom of described fluidized-bed reactor is provided with formaldehyde gas entrance, and the top of fluidized-bed reactor arranges dimethoxym ethane solution inlet。Every layer of conversion zone of described fluidized-bed reactor is additionally provided with filling silk screen module, and described filling silk screen module is cage structure silk screen and is located at above gas distributor。Described filling silk screen module is made up of many rustless steel steel wires, and described rustless steel steel wire is Torsion coil steel wire。Torsion coil steel wire in silk screen module of filling in the present invention constitutes the cage structure of multilamellar, make reaction raw materials can obtain maximized contact (especially multiple structure and Torsion coil structure steel wire in the module, accelerate the mixing contact of reaction raw materials, and can quickly remove reaction heat), and make reaction raw materials and catalyst substantially be solidificated in conversion zone reaction, reduce catalyst and pile up at downspout top silk screen with liquid stream。
Described lightness-removing column charging aperture connects reactant liquor discharging opening bottom fluidized-bed reactor, and reactant liquor removes dimethoxym ethane in lightness-removing column。This tower top atmospheric operation, tower top arranges condenser and return tank, and reflux ratio preferably 1 ~ 2. tower top obtains pure component dimethoxym ethane。Tower reactor obtains the reactant liquor without dimethoxym ethane。Described lightness-removing column is atmospheric distillation tower, adopts filler or plate column。Reactant liquor enters lightness-removing column and first separates dimethoxym ethane, obtains being practically free of the reactant liquor of dimethoxym ethane from tower reactor。The outlet of still liquid connects extraction tower import, extraction tower tower reactor feeding extraction agent so that produce noted phase separation phenomena in extraction tower, and by controlling boundary height extraction levels liquid, lower floor obtains formalin, and upper strata obtains the product solution containing extractant。Supernatant liquid enters extractant recovery tower, reclaims extractant。Certainly, according to the difference adopting extractant boiling point, the position of extractant recovery tower can relative changes, for the extractant that boiling point is higher, it is possible to reclaim extractant after product separating。As preferably, extractant recovery tower is as the 3rd knockout tower。The extractant that recovered overhead obtains can recycle, the product for DMM2 ~ 8 that tower reactor arrives。
Described extraction tower adopts filler or plank frame, preferred filler, reactant liquor is added by extraction tower top, extractant has extraction tower bottom to add, reactant liquor and extractant counter current contacting, and the Organic substance based on DMMn in reactant liquor is dissolved in extractant, water and formaldehyde in reactant liquor cannot be dissolved in extractant, owing to there is obvious density contrast between them, therefore in tower, produce noted phase separation phenomena, by boundary Altitude control extraction upper liquid and subnatant。The still liquid removing formalin mainly contains DMM2 ~ 8 component and extractant component。
Described extractant recovery tower charging connects extraction tower upper liquid charging。It should be noted that the separation order that extractant reclaims not is fixing, it is relevant with the extractant kind adopted, and can be reclaimed by extractant for high boiling extractant after being placed on product tower。Preferred extractant recovery tower is after extraction tower。Extractant recovery tower adopts filler or plate column, atmospheric operation, and tower top adopts condenser and return tank, it is preferable that reflux ratio 1 ~ 4. overhead extraction extractant material, still liquid obtains product material DMM2 ~ 8。
According to described, still liquid product sends into DMM2 product。This tower employing filler or plate column, atmospheric operation, tower top adopts condenser and return tank, by controlling reflux ratio 0.5 ~ 2, the DMM2 product that extraction conforms to quality requirements。It is again exquisite that product for not meeting prescription will be fed into this tower charging, it is also possible to increases reflux ratio and improves product quality。
According to described, DMM2 product tower bottoms is DMM3 ~ 8 product。This still liquid sends into DMM3 ~ 5 product tower。This tower adopts filler or plate column, decompression operation, it is preferable that operation pressure 2 ~ 20kPa(absolute pressure), tower top adopts condenser and return tank, it is preferable that reflux ratio is that 0.5 ~ 2. tower top obtains DMM3 ~ 5 product。It should be noted that overhead product is not necessarily, different regions can control the product that extraction quality is different, such as in the area that south winter temperature is higher, the lowest temperature also condensation point far above DMM6, it is possible to suitably extraction part DMM6, better blended diesel component。For northern area, then on the contrary, it is necessary to control in product containing as far as possible few DMM6, it is to avoid wherein contain high condensation point blend component。
Claims (9)
1. a gas formaldehyde prepares the special process device of polymethoxy dimethyl ether, it is characterized in that: the raw material of described synthesis polymethoxy dimethyl ether is formaldehyde gas and dimethoxym ethane solution, described special process device includes the fluidized-bed reactor being sequentially connected with, extract and recovery unit and refined unit, described fluidized-bed reactor includes at least two-layer conversion zone from bottom to up, every layer of conversion zone is filled with catalyst, and the bottom of every layer of conversion zone all offers gas distributor directly and conversion zone UNICOM of lower floor, every layer of conversion zone is additionally provided with downspout by adjacent conversion zone UNICOM simultaneously, the top of described downspout is additionally provided with silk screen；The bottom of described fluidized-bed reactor is provided with formaldehyde gas entrance, and the top of fluidized-bed reactor arranges dimethoxym ethane solution inlet。
2. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 1, it is characterised in that: described every layer of conversion zone is equipped with Catalyst packing mouth and catalyst discharge port。
3. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 1, it is characterized in that: every layer of conversion zone of described fluidized-bed reactor is additionally provided with filling silk screen module, and described filling silk screen module is cage structure silk screen and is located at above gas distributor。
4. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 3, it is characterised in that: described filling silk screen module is made up of many rustless steel steel wires, and described rustless steel steel wire is Torsion coil steel wire。
5. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 1, it is characterised in that: the bottom of described fluidized-bed reactor is provided with reactant liquor discharging opening, and this reactant liquor discharging opening arranges silk screen。
6. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 1, it is characterized in that: described extractant recovery unit includes the lightness-removing column, extraction tower and the extractant recovery tower that are sequentially connected with, the import of described lightness-removing column is connected with the reactant liquor discharging opening of fluidized-bed reactor, and the top of lightness-removing column is provided with condensation reflux unit。
7. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 4, it is characterized in that: described extraction tower is packed tower or plate column, the tower top of extraction tower is provided with reactant liquor charging aperture, is provided with extractant feed mouth at the bottom of tower, and reactant liquor and extractant are counter current contacting。
8. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 4, it is characterised in that: described extractant recovery tower is packed tower or plate column, and tower top is connected to condenser and return tank and forms circulation with extractant recovery tower。
9. gas formaldehyde prepares the special process device of polymethoxy dimethyl ether according to claim 1, it is characterised in that: described fluidized-bed reactor is provided with 4～6 layers of conversion zone。
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| CN201610147992.XA CN105693479A (en) | 2016-03-15 | 2016-03-15 | Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas |
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| CN201610147992.XA CN105693479A (en) | 2016-03-15 | 2016-03-15 | Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106146266A (en) * | 2016-07-05 | 2016-11-23 | 江苏凯茂石化科技有限公司 | A kind of concentrated formaldehyde prepares process and the device of polymethoxy dimethyl ether |
| CN107556171A (en) * | 2017-06-27 | 2018-01-09 | 河南中鸿集团煤化有限公司 | A kind of polymethoxy dimethyl ether process units |
| CN107793300A (en) * | 2017-11-08 | 2018-03-13 | 江苏道尔顿石化科技有限公司 | A kind of reaction solution separating technology of polymethoxy dimethyl ether |
| CN108929305A (en) * | 2017-05-25 | 2018-12-04 | 邢台旭阳科技有限公司 | Gaseous formaldehyde mixture is directly used in the method and purposes of synthesizing formaldehyde downstream product |
| CN109096064A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The refining methd of polyoxymethylene dimethyl ethers |
| CN109096065A (en) * | 2017-06-21 | 2018-12-28 | 中国石油化工股份有限公司 | The method of purification of polyoxymethylene dimethyl ethers |
| CN109180440A (en) * | 2018-11-08 | 2019-01-11 | 凯瑞环保科技股份有限公司 | Extract catalytic tower |
| CN109232202A (en) * | 2018-11-08 | 2019-01-18 | 凯瑞环保科技股份有限公司 | A kind of one-step synthesis method DMM3-8Device and method |
| CN109745925A (en) * | 2019-02-26 | 2019-05-14 | 国家能源投资集团有限责任公司 | The loading method of n-butene direct hydration reactor |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107793300A (en) * | 2017-11-08 | 2018-03-13 | 江苏道尔顿石化科技有限公司 | A kind of reaction solution separating technology of polymethoxy dimethyl ether |
| CN109180440A (en) * | 2018-11-08 | 2019-01-11 | 凯瑞环保科技股份有限公司 | Extract catalytic tower |
| CN109232202A (en) * | 2018-11-08 | 2019-01-18 | 凯瑞环保科技股份有限公司 | A kind of one-step synthesis method DMM3-8Device and method |
| CN109232202B (en) * | 2018-11-08 | 2024-02-06 | 凯瑞环保科技股份有限公司 | One-step method for synthesizing DMM 3-8 Apparatus and method of (2) |
| CN109180440B (en) * | 2018-11-08 | 2024-03-19 | 凯瑞环保科技股份有限公司 | Extraction catalytic reaction tower |
| CN109745925A (en) * | 2019-02-26 | 2019-05-14 | 国家能源投资集团有限责任公司 | The loading method of n-butene direct hydration reactor |
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