CN206214896U - Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis - Google Patents

Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis Download PDF

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Publication number
CN206214896U
CN206214896U CN201621105296.4U CN201621105296U CN206214896U CN 206214896 U CN206214896 U CN 206214896U CN 201621105296 U CN201621105296 U CN 201621105296U CN 206214896 U CN206214896 U CN 206214896U
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China
Prior art keywords
cylinder
extractant
filter cartridge
rotating filter
dimethyl ether
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Expired - Fee Related
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CN201621105296.4U
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Chinese (zh)
Inventor
叶子茂
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JIANGSU KAIMAO CHEMICAL TECHNOLOGY Co Ltd
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JIANGSU KAIMAO CHEMICAL TECHNOLOGY Co Ltd
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Priority to CN201621105296.4U priority Critical patent/CN206214896U/en
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Abstract

The utility model discloses extractant recycle device in a kind of synthesis of polymethoxy dimethyl ether, the device includes recycling cylinder (1), is respectively provided at the inlet (4) and reaction solution liquid outlet (5) that recycle cylinder (1) bottom and top, the extractant liquid outlet (3) for being located at recycling cylinder (1) side wall, and the filter assemblies (2) in recycling cylinder (1) are located at, wherein:Refined filtration cylinder (22) and rotating filter cartridge (21) that the filter assemblies (2) are made including inorganic ceramic, the rotating filter cartridge (21) is concentric to be located in refined filtration cylinder (22), the inwall of the rotating filter cartridge (21) is provided with screw thread, and the bottom and top of the rotating filter cartridge (21) connect with the inlet (4) and reaction solution liquid outlet (5) of recycling cylinder (1) respectively.The utility model can effectively reclaim extractant, make extractant recycle, and significantly reduce production cost, economic well-being of workers and staff be improved, while energy-conserving and environment-protective.

Description

Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis
Technical field
The utility model is related to chemical production technology and equipment technical field, and in particular to a kind of polymethoxy dimethyl ether is closed Into middle extractant recycle device and method.
Background technology
In the production process of polymethoxy dimethyl ether, extraction is essential link, it is therefore desirable to used substantial amounts of Extractant.Extractant is to recycle in whole reaction, but produces polymethoxy dimethyl ether with current process A small amount of extractant can be contained in produced waste water, this has resulted in the waste of extractant.It is estimated to draw, often produce 1 Ton polymethoxy dimethyl ether, waste water will outward arrange 11KG extractants, the market price of extractant about in 10 yuan/kg, thus quite 110 yuan are increased in the cost for producing polymethoxy dimethyl ether per ton, if coming by annual 100000 tons of polymethoxy dimethyl ethers of production Calculate, then annual about to lose 11,000,000 yuan, so serious reduces production profit.
Extractant can also be polluted to environment, and it can exist for a long time in nature, and water resource is caused directly Infringement.Although the extraction agent content not being recovered is very low, it is discharged by waste water, is constantly produced in the environment, migrates, is turned Change and degrade, and human body (such as respiratory tract, skin, alimentary canal) is entered with number of ways, be enriched with human body, greatly threaten The health of the mankind.
For with prior art, problems still cannot be well solved.
In summary, the extractant in waste water how is efficiently reclaimed, production cost is saved, environmental pollution is reduced, at present It is still a problem.
The content of the invention
Goal of the invention:The utility model is wasted for extractant, and production cost is improved, and the problems such as cause environmental pollution, is carried Extractant recycle device and method in having supplied a kind of polymethoxy dimethyl ether to synthesize.
Technical scheme:In order to solve the above technical problems, the utility model proposes in a kind of synthesis of polymethoxy dimethyl ether Extractant recycle device, including recycle cylinder, be respectively provided at inlet and the reaction on recycling cylinder bottom and top Liquid liquid outlet, the extractant liquid outlet of recycling cylinder side wall is located at, and is located at the filter assemblies in recycling cylinder, its In:
Refined filtration cylinder and rotating filter cartridge that the filter assemblies are made including inorganic ceramic, the rotating filter cartridge is concentric to be set In refined filtration cylinder, the inwall of the rotating filter cartridge is provided with screw thread, the bottom and top of the rotating filter cartridge respectively with recycling The inlet of cylinder is connected with reaction solution liquid outlet, and the inlet is additionally provided with force (forcing) pump, and the outer wall of the refined filtration cylinder is additionally provided with and adds Hot adjoining pipe, the space between the refined filtration cylinder and recycling cylinder is also associated with vaccum-pumping equipment.
Preferably, the material of the refined filtration cylinder is aluminum oxide, silica, titanium oxide or zirconium oxide;The rotating filter cartridge Material be aluminum oxide or silica.
Preferably, the aperture of the rotating filter cartridge is 0.45~0.55 μm, porosity is 40~60%, the refined filtration cylinder Aperture be 0.22~0.25 μm, porosity be 20~50%.
Preferably, the screw thread of the rotating filter cartridge inwall is 55 ° of screw threads, pitch is 30~50mm.
Preferably, the filter assemblies internal pressure is 3~5MPa, temperature is 90~95 DEG C
Preferably, being provided with filter screen at described extractant liquid outlet, inlet and reaction solution liquid outlet.
The utility model additionally provides extractant in a kind of synthesizing for polymethoxy dimethyl ether based on said apparatus Recovery method, comprises the following steps:
First, mixed liquor is sent into rotating filter cartridge in the presence of force (forcing) pump through inlet pressurization, and at 90~95 DEG C Under conditions of vacuumizing, make mixed liquor along rotating filter cartridge inwall to exosmosis;
In process of osmosis, the formaldehyde autopolymer in the mixed liquor is adsorbed by rotating filter cartridge first, and extractant is through rotation Filter cylinder enters into buffering transition in refined filtration cylinder, then goes the removal of impurity through refined filtration cylinder adsorption filtration again, enters into recycling cylinder It is interior, and discharged by extractant liquid outlet;
Preferably, the vacuum environment negative pressure between the refined filtration cylinder and recycling cylinder is -0.1MPa.
Adsorbing separation goes out extractant and the mixed liquor of formaldehyde autopolymer is discharged by reaction solution liquid outlet.
Beneficial effect:The utility model can effectively reclaim the extractant in waste water, largely avoid extraction The waste of agent, reduces production cost, so as to improve production interests;Meanwhile, the rate of recovery of extractant is improved, reduce extraction in waste water The content of agent is taken, pollution is reduced.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model;
Fig. 2 is filter assemblies structural representation of the present utility model.
Wherein, recycling cylinder 1, filter assemblies 2, rotating filter cartridge 21, refined filtration cylinder 22, extractant liquid outlet 3, inlet 4 With reaction solution liquid outlet 5.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the utility model is further elucidated.
Extractant reclaims profit during a kind of polymethoxy dimethyl ether synthesis is proposed according to above-mentioned technical proposal, in the present embodiment With device, including recycling cylinder 1, be respectively provided at the recycling bottom of cylinder 1 and top inlet 4 and reaction solution liquid outlet 5, The extractant liquid outlet 3 of the recycling side wall of cylinder 1 is located at, and is located at the filter assemblies 2 in recycling cylinder 1, wherein:
Refined filtration cylinder 22 and rotating filter cartridge 21 that the filter assemblies 2 are made including inorganic ceramic, the rotating filter cartridge 21 are same Axle center be located at refined filtration cylinder 22 in, the inwall of the rotating filter cartridge 21 is provided with screw thread, the bottom and top of the rotating filter cartridge 21 Connected with the inlet 4 and reaction solution liquid outlet 5 of recycling cylinder 1 respectively, the inlet 4 is additionally provided with force (forcing) pump, the essence The outer wall of filter cylinder 22 is additionally provided with heating adjoining pipe, and the space between the refined filtration cylinder 22 and recycling cylinder 1 is also associated with vacuumizing Equipment.
The utility model additionally provides extractant in a kind of synthesizing for polymethoxy dimethyl ether based on said apparatus Recovery method, comprises the following steps:
First, mixed liquor is pressurizeed in feeding rotating filter cartridge 21 in the presence of force (forcing) pump through inlet 4, and 90~95 DEG C and under conditions of vacuumizing, make mixed liquor along the inwall of rotating filter cartridge 21 to exosmosis;
In process of osmosis, the formaldehyde autopolymer in the mixed liquor is adsorbed by rotating filter cartridge 21 first, and extractant is through rotation Turn filter cylinder 21 and enter into buffering transition in refined filtration cylinder 22, then go the removal of impurity through refined filtration 22 adsorption filtrations of cylinder again, enter into back Receive in process cartridge 1, and discharged by extractant liquid outlet 3;
Adsorbing separation goes out extractant and the mixed liquor of formaldehyde autopolymer is discharged by reaction solution liquid outlet 5.
Because waste water mixed liquor is Chemical Manufacture gained waste water, wherein the particle for not readily dissolving may be contained, so in extraction Filter screen is provided with agent liquid outlet 3, inlet 4 and reaction solution liquid outlet 5.Filter screen can effectively stop the particle in waste water, some things The particle of matter may have corrosivity, and being filtered off can also protect process units, and the service life of extension fixture reduces dimension Difficulty is repaiied, it is cost-effective.
The filter assemblies 2 used in the present embodiment are inoranic membrane, when the rotating filter cartridge 21 works, for a long time by inside Mixed liquor impacts, therefore mechanical strength to rotating filter cartridge 21 has higher requirements, and its material is mainly aluminum oxide and silica.And The major function of refined filtration cylinder 22 is that coarse filtration liquid is purified, therefore refined filtration cylinder uses various material, such as aluminum oxide, silica, Titanium oxide and zirconium oxide, more effectively isolate extractant, while increasing the contact area of refined filtration cylinder and coarse filtration liquid, support strength It is significantly less than rotating filter cartridge 21.
In the present embodiment, the aperture of the rotating filter cartridge 21 is 0.45 μm, and porosity is 50%, the aperture of the refined filtration cylinder It it is 0.22 μm, porosity is 30%.Rotating filter cartridge 21 is that mixed liquor is pre-processed, and the requirement to aperture is low, and refined filtration cylinder 22 aperture is smaller, more targeted screening extractant, and the porosity of refined filtration cylinder 22 is also significantly lower than rotating filter cartridge 21, because In actual production, process relaxes when coarse filtration liquid flows to refined filtration cylinder 22, if the porosity of refined filtration cylinder is high, can become filter effect Difference.
Because that containing organic solutions such as polymethoxy dimethyl ether and extractants, can cause to damage in mixed liquor to organic film, Organic film need to just be changed using after a period of time, and service life is significantly shorter than inorganic ceramic, for economics, inorganic Ceramics are a kind of more excellent selections.Each item data of the filter assemblies 2 selected in the present embodiment compared with the conventional film such as institute of table 1 Show, the product yield of inorganic ceramic gained aborning is substantially better than organic film, and the filter assemblies of the present embodiment are compared to normal The inorganic ceramic product yield seen is higher, up to more than 90%.Although organic film cost is relatively low, its mechanical strength is poor, Organic film film layer is relatively thin, can not operationally apply high pressure, and inorganic ceramic can then work under high pressure, and institute is used in the present embodiment Filter component 2 works under 3~5MPa pressure, and to the spatial decimation vacuum between refined filtration cylinder 22 and recycling cylinder 1.Because changing Work production work amount is big, and will necessarily calculate the cost of production problem, and the service life of film is more long more can be cost-effective, inorganic ceramic with Filter assemblies 2 in the present embodiment are ceramic materials, can enter horizontal high voltage backwash, and power of regeneration is strong, can Reusability, and have The cleaning regenerative process of machine film is complex, and maintenance cost is higher, it is impossible to use for a long time.It is to use in view of the utility model Extractant in polymethoxy dimethyl ether is reclaimed, therefore operating temperature of the present utility model is unsuitable too high, when temperature is too high Useless accessory substance can be produced, polymethoxy dimethyl ether purity is reduced, also difficulty is brought to reclaim extractant.
Table 1
Data in consolidated statement 1, the pressure that the present embodiment applies to filter assemblies 2 is 3MPa, and temperature is 95 DEG C, refined filtration cylinder The negative pressure in the space between 22 and recycling cylinder 1 is -0.1MPa, now to the yield of extractant about 92%.
Because extractant is inconsistent with the molecular size of other materials in organic phase logistics, the analysis of the selectivity of filter assemblies 2 Go out extractant.In actual production, the annular space between filter assemblies 2 and recycling cylinder 1 is extracted using vavuum pump true It is empty.In the present embodiment, filter assemblies 2 include the rotating filter cartridge 21 in refined filtration cylinder 22 and refined filtration cylinder 22, and the rotating filter cartridge 21 is first Solution is tentatively filtered, the inwall of rotating filter cartridge 21 is provided with screw thread, and mixed liquor can be in the presence of force (forcing) pump, along rotation The spiral inner wall of filter cylinder 21 is delivered up, the contact area of increase and the inwall of rotating filter cartridge 21, while also ensure that filter assemblies Make full use of, improve filter efficiency, while rotation also makes whole process more steady.The angle of thread described in the present embodiment is 55 °, pitch is 30mm, compared with conventional tubular filter, newly-increased screw thread can make mixed liquor can fully with rotating filter cartridge 21 Barrel contacted, and increase the contact area of mixed liquor and barrel, take full advantage of the space of rotating filter cartridge 21 so that Improve separative efficiency.
The utility model is used in particular for the recovery operation of extractant when polymethoxy dimethyl ether synthesizes, it is worth noting that, The filter assemblies 2 use membrane technology.Membrane technology is separated as new isolation of purified and the technology of concentration with tradition Operation compares, low to the requirement of the condition of working environment, especially low to temperature requirement, additionally, membrane technology also have energy consumption it is low, The features such as efficiency high, process is simple, small investment.The a large amount of waste water of output during polymethoxy dimethyl ether is synthesized, it is therein Extraction agent content is low, it is desirable to which the extractant workload reclaimed in waste water is big, and not only efficiency is low to reclaim extractant using conventional method Under, and complex process, energy consumption is excessive, and is extremely difficult to ideal effect.By contrast, will easily be permitted with film process Many, the effect for reclaiming extractant is preferable, it is often more important that, the process is simple in removal process, without complicated operation, subtracts significantly Light workload.Reclaim extractant and not only saved production cost, it is often more important that mitigate harm of the waste water to environment, extraction The organic efficiency of agent is higher, and the content in waste water is lower, and the pollution to environment is also just smaller.
It should be understood that these embodiments are merely to illustrate the utility model rather than limit scope of the present utility model, readding Read after the utility model, modification of the those skilled in the art to the various equivalent form of values of the present utility model falls within the application Appended claims limited range.

Claims (6)

1. extractant recycle device during a kind of polymethoxy dimethyl ether synthesizes, it is characterised in that:Including recycling cylinder (1), it is respectively provided at and recycles the inlet (4) and reaction solution liquid outlet (5) of cylinder (1) bottom and top, is located at recycling The extractant liquid outlet (3) of cylinder (1) side wall, and the filter assemblies (2) in recycling cylinder (1) are located at, wherein:
Refined filtration cylinder (22) and rotating filter cartridge (21) that the filter assemblies (2) are made including inorganic ceramic, the rotating filter cartridge (21) concentric to be located in refined filtration cylinder (22), the inwall of the rotating filter cartridge (21) is provided with screw thread, the rotating filter cartridge (21) Bottom and top respectively with recycling cylinder (1) inlet (4) and reaction solution liquid outlet (5) connect, the inlet (4) Force (forcing) pump is additionally provided with, the outer wall of refined filtration cylinder (22) is additionally provided with heating adjoining pipe, refined filtration cylinder (22) and recycling cylinder (1) Between space be also associated with vaccum-pumping equipment.
2. extractant recycle device during polymethoxy dimethyl ether according to claim 1 synthesizes, it is characterised in that:Institute The material for stating refined filtration cylinder (22) is aluminum oxide, silica, titanium oxide or zirconium oxide;The material of the rotating filter cartridge (21) is oxidation Aluminium or silica.
3. extractant recycle device during a kind of polymethoxy dimethyl ether according to claim 1 synthesizes, its feature exists In:The aperture of the rotating filter cartridge (21) is 0.45~0.55 μm, and porosity is 40~60%, the aperture of refined filtration cylinder (22) It it is 0.22~0.25 μm, porosity is 20~50%.
4. extractant recycle device during polymethoxy dimethyl ether synthesizes according to claim 1, it is characterised in that:It is described The screw thread of rotating filter cartridge (21) inwall is 55 ° of screw threads, and pitch is 30~50mm.
5. extractant recycle device during a kind of polymethoxy dimethyl ether according to claim 1 synthesizes, its feature exists In:Filter assemblies (2) internal pressure is 3~5MPa, and temperature is 90~95 DEG C.
6. extractant recycle device during a kind of polymethoxy dimethyl ether according to claim 1 synthesizes, its feature exists In:Described extractant liquid outlet (3), inlet (4) and reaction solution liquid outlet (5) place are provided with filter screen.
CN201621105296.4U 2016-10-08 2016-10-08 Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis Expired - Fee Related CN206214896U (en)

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Application Number Priority Date Filing Date Title
CN201621105296.4U CN206214896U (en) 2016-10-08 2016-10-08 Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis

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Application Number Priority Date Filing Date Title
CN201621105296.4U CN206214896U (en) 2016-10-08 2016-10-08 Extractant recycle device in a kind of polymethoxy dimethyl ether synthesis

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106422501A (en) * 2016-10-08 2017-02-22 江苏凯茂石化科技有限公司 Device and method for recycling extraction agent in polyoxymethylene dimethyl ether synthesis

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106422501A (en) * 2016-10-08 2017-02-22 江苏凯茂石化科技有限公司 Device and method for recycling extraction agent in polyoxymethylene dimethyl ether synthesis

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Granted publication date: 20170606

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