CN204569779U - A kind of process unit for polymethoxy dimethyl ether raw material production - Google Patents

A kind of process unit for polymethoxy dimethyl ether raw material production Download PDF

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Publication number
CN204569779U
CN204569779U CN201520165378.7U CN201520165378U CN204569779U CN 204569779 U CN204569779 U CN 204569779U CN 201520165378 U CN201520165378 U CN 201520165378U CN 204569779 U CN204569779 U CN 204569779U
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China
Prior art keywords
raw material
reaction
tower
dimethyl ether
polymethoxy dimethyl
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Expired - Fee Related
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CN201520165378.7U
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Chinese (zh)
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叶子茂
向家勇
张鸿伟
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JIANGSU KAIMAO CHEMICAL TECHNOLOGY Co Ltd
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JIANGSU KAIMAO CHEMICAL TECHNOLOGY Co Ltd
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Abstract

The utility model discloses a kind of process unit for polymethoxy dimethyl ether raw material production, this device comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, and the bottom of described raw material tower is connected with reaction decker by pipeline.The utility model with formaldehyde solution with low cost for basic raw material, prepare the raw material that polymethoxy dimethyl ether is produced, and by fixed-bed reactor after mixing with methylal according to the raw material that this technique obtains, transformation efficiency is high, and high for the selectivity of DMM3 ~ 8 product.

Description

A kind of process unit for polymethoxy dimethyl ether raw material production
Technical field
The utility model belongs to chemical production technology and equipment technical field, relates generally to producing and manufacturing technique and the device of polymethoxy dimethyl ether.
Background technology
(Chinese also can be polyoxymethylene dimethyl ether to polymethoxy dimethyl ether, polyoxymethylene dimethyl ethers, polymethoxy methylal, polyoxymethylene dimethyl ethers etc.), i.e. polyoxymethylene dimethyl ethers (PODE), it is the common name of a class material, and its molecular structural formula is CH 3o (CH 2o) nCH 3, there is higher cetane value (cetane number, CN.When n=3 ~ 8, CN>76) and oxygen level (42 ~ 49%).When the value of n is 3 ~ 8, its physical and chemical performance, combustionproperty and diesel oil closely, can be used as diesel-dope, and the addition in diesel oil can reach 30% (v/v), keeps higher cetane value and combustionproperty simultaneously.The oilness of diesel oil can be improved, reduce combustion fumes and generate, diesel oil combustion position within the engine can be improved, improve thermo-efficiency, the particulate matter in reduction combustion tail gas and the discharge of NOx.Also possibility diesel oil substitute, directly as diesel-fuel.
The raw material that current polymethoxy dimethyl ether mainly adopts is paraformaldehyde, concentrated formaldehyde solution or trioxymethylene and methylal.Because paraformaldehyde and trioxymethylene are solid formaldehyde, reaction conditions is harsher, the relatively high general control of reaction pressure is at 1 ~ 2.5MPa, thus cause equipment cost high, and the reaction of solid formaldehyde and methylal generally adopts suspension bed and fluidized-bed reactor, catalyzer life cycle is short, the large and trioxymethylene of loss and paraformaldehyde raw materials cost high; Concentrated formaldehyde solution is raw material, cause being that the transformation efficiency of raw material reaction polymethoxy dimethyl ether is relatively low with concentrated formaldehyde due to the existence of water in reaction process, more difficult and product separation energy consumption is also higher to product separation, and above-mentioned reaction is not high for the selectivity of DMM3 ~ 8 product.
Summary of the invention
Goal of the invention: for above-mentioned Problems existing and defect, the utility model provides a kind of process unit for polymethoxy dimethyl ether raw material production, with 37 ~ 50% more cheap formaldehyde solutions for basic raw material, prepare the raw material that polymethoxy dimethyl ether is produced.And by fixed-bed reactor after mixing with methylal according to the raw material that this technique obtains, transformation efficiency is high, and high for the selectivity of DMM3 ~ 8 product.
Technical scheme: for achieving the above object, the utility model is by the following technical solutions: a kind of process unit for polymethoxy dimethyl ether raw material production, comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, wherein: be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, described in carry the bottom of heating up in a steamer reaction decomposes section and be connected with reaction decker by pipeline.
As preferably, described deacidifying device is ion exchange tower.
As preferably, the exchang medium of filling in described deacidifying device is silica gel or weak base anion-exchange resin.
Beneficial effect: compared with prior art, the utility model directly uses the formaldehyde of 37 ~ 50% common concentration to be preparation of raw material, utilizes the feature of auxiliary and formaldehyde reaction, the raw material of configuration polymethoxy dimethyl ether.Because raw material is the most general formaldehyde solution in market, simple and easy to get, with low cost.The program carried out depickling process before reacting, and reduced acidity to auxiliary consumption in the reaction.And the program strictly controls the temperature in raw material tower, and adopt the raw material tower of this invention, considerably increase the reversed reaction time of subsystem and formaldehyde solution, thus again reduce the consumption of auxiliary.This raw material device not adopts the mode of conventional liquid of top of the tower backflow, but adopts the DMM2 in a large amount of DMM or polymethoxy dimethyl ether reaction product or reaction solution to reflux, and greatly increases the processing safety of this device.And the water of batching of the present utility model directly only containing formaldehyde and DMM or DMM2, PPM level content, this raw material prepare polymethoxy dimethyl ether reaction conversion ratio and selectivity high.
Accompanying drawing explanation
Fig. 1 is the schema of polymethoxy dimethyl ether technique for producing raw material method described in the utility model.
Wherein, deacidifying device 1, preheater 2, reaction decker 3, dehydration tower 4, vacuum extractor 5, raw material tower 6, liquid pump 7.
Embodiment
Below in conjunction with the drawings and specific embodiments, illustrate the utility model further, these embodiments should be understood and be only not used in restriction scope of the present utility model for illustration of the utility model, after having read the utility model, the amendment of those skilled in the art to the various equivalent form of value of the present utility model has all fallen within the application's claims limited range.
As shown in Figure 1, process unit for polymethoxy dimethyl ether raw material production of the present utility model, comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, wherein: be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, described in carry the bottom of heating up in a steamer reaction decomposes section and be connected with reaction decker by pipeline.Major processes is as follows:
37 ~ 50% formaldehyde solutions market bought or produces, carry out depickling process through silica gel or macropore weak basic anion exchange resin, after depickling process, solution acid content is (1 ~ 10ppm).Formaldehyde solution after depickling process is by after being preheating to 60 ~ 100 DEG C, abundant hybrid reaction is carried out with auxiliary in reaction decker (adopting in tower or basin), reacted component due to density ratio water little, through leave standstill after, supernatant liquid through pump delivery to dehydration tower.Wherein said auxiliary is unitary saturated alcohol or binary saturated alcohol and ether material, one in preferred isopropylcarbinol, 4-methyl-2-amylalcohol or hexalin, in fact the unitary saturated alcohol equal prodigiosin of carbonatoms between 3 ~ 9 and formaldehyde form reaction product that is water-fast but easily thermolysis, but there are differences in concrete heat decomposition temperature and transformation efficiency.
The reaction product obtained in reaction decker has thermolysis effect, and dehydration tower controls at vacuum operating, and moisture is deviate from by the tower top that dewaters, and by being pumped into raw material tower bottom dehydration tower, the working pressure in dehydration tower is 20 ~ 100KPa.In raw material tower, lower end is mainly stripping section and reactant decomposition section, control this section of temperature 120 ~ 160 DEG C, upper end is by supplementing the DMM2 component backflow in methylal or polymethoxy dimethyl ether product, obtain methylal and formaldehyde (or mix products of DMM2 and formaldehyde) at raw material tower top, direct gas phase is as the reaction raw materials of polymethoxy dimethyl ether.Be auxiliary bottom raw material tower, by being pumped into reaction unit recycle.
Above production method mainly includes deacidifying device, mixed reactor, dewatering unit, raw material preparation facilities.Major control index, in charging formaldehyde, acid content can not more than 1000ppm; Hybrid reaction controls temperature of reaction 80 ~ 100 DEG C, reaction time 1 ~ 5h; Dehydration tower red-tape operati pressure 20 ~ 100KPa (A), service temperature controls 60 ~ 100 DEG C; Raw material tower controls pressure-fired, and tower top service temperature controls 90 ~ 120 DEG C, and tower reactor section temperature is 160 ~ 220 DEG C.Wherein raw material tower is rectifying tower, the region residence time long Reaction Separation being beneficial to formaldehyde and auxiliary system of major control tower reactor section 140 ~ 200 DEG C, thus formaldehyde can depart from by reaction system, and the transformation efficiency that formaldehyde departs from is high, because the formaldehyde gas detached 100 ~ 120 DEG C time is easily polymerized in tower, therefore adopt the material of boiling point in this region to carry out the concentration refluxing to dilute formaldehyde, prevent polymerization.This backflow adopts the DMM2 in a large amount of DMM or polymethoxy dimethyl ether reaction product or reaction solution to reflux, and adopts this system to reflux the DMM2 selectivity that can also effectively improve in reaction system.

Claims (3)

1. the process unit for polymethoxy dimethyl ether raw material production, it is characterized in that: comprise connect successively deacidifying device, reaction decker, dehydration tower and raw material tower, wherein: be provided with preheater between described deacidifying device and reaction decker, the top of described dehydration tower is provided with vaccum-pumping equipment; Reaction decomposes section is heated up in a steamer for carrying in the bottom of described raw material tower, and top is feed back mixing section and is provided with polymethoxy dimethyl ether reaction raw materials reflux inlet, described in carry the bottom of heating up in a steamer reaction decomposes section and be connected with reaction decker by pipeline.
2. process unit according to claim 1, is characterized in that: described deacidifying device is ion exchange tower.
3. process unit according to claim 2, is characterized in that: the exchang medium of filling in described deacidifying device is silica gel or weak base anion-exchange resin.
CN201520165378.7U 2015-03-24 2015-03-24 A kind of process unit for polymethoxy dimethyl ether raw material production Expired - Fee Related CN204569779U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104725202A (en) * 2015-03-24 2015-06-24 江苏凯茂石化科技有限公司 Process device and method for production of poly methoxy dimethyl ether raw material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104725202A (en) * 2015-03-24 2015-06-24 江苏凯茂石化科技有限公司 Process device and method for production of poly methoxy dimethyl ether raw material

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