CN204644228U - A kind of dewatering process device for the synthesis of polymethoxy dimethyl ether - Google Patents

A kind of dewatering process device for the synthesis of polymethoxy dimethyl ether Download PDF

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Publication number
CN204644228U
CN204644228U CN201520313067.0U CN201520313067U CN204644228U CN 204644228 U CN204644228 U CN 204644228U CN 201520313067 U CN201520313067 U CN 201520313067U CN 204644228 U CN204644228 U CN 204644228U
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Prior art keywords
tower
outlet
reaction solution
surge tank
reaction
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Expired - Fee Related
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CN201520313067.0U
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Chinese (zh)
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叶子茂
向家勇
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JIANGSU KAIMAO CHEMICAL TECHNOLOGY Co Ltd
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JIANGSU KAIMAO CHEMICAL TECHNOLOGY Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/582Recycling of unreacted starting or intermediate materials

Abstract

The utility model discloses a kind of dewatering process device for the synthesis of polymethoxy dimethyl ether, comprise raw material surge tank, multi-stage type reactor, reaction solution surge tank and lightness-removing column, the outlet of described raw material surge tank is connected with multi-stage type reactor inlet, the tower top of described multi-stage type reactor is provided with gaseous phase outlet, is provided with reaction solution outlet at the bottom of tower; Described reaction solution outlet and reaction solution surge tank are communicated with and are connected with lightness-removing column afterwards; The tower top of described lightness-removing column is provided with methylal outlet, is provided with at the bottom of DMM2 outlet, tower and is provided with products export in tower.It is anhydrous state that the utility model can control reaction system, thus improves the yield of polymethoxy dimethyl ether, also reduces the reaction conditions of reaction system simultaneously, reduces energy consumption of reaction.

Description

A kind of dewatering process device for the synthesis of polymethoxy dimethyl ether
Technical field
The utility model belongs to chemical production technology and equipment technical field, relates generally to polymethoxy dimethyl ether producing and manufacturing technique.
Background technology
The feature of China's energy structure is: rich coal, oil-poor, weak breath, and 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 barrier 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.In addition, China's methyl alcohol production capacity is seriously superfluous, exploitation Downstream Products of Methanol, extends Chemical Industry chain, all has realistic meaning.
Polymethoxy dimethyl ether is a kind of universally acknowledged clean diesel component, its cetane value >=70, not sulfur-bearing, aromatic free.Add in diesel oil in 5%-20% ratio, can diesel cetane-number be improved, promote burning, reduce the discharge of the obnoxious flavoures such as PM2.5, PM10, NOx, CO in vehicle exhaust significantly.
Due to the excellent properties of polymethoxy dimethyl ether, its synthesis technique has become the heat subject of research both at home and abroad.Polymethoxy dimethyl ether reacts under the katalysis of an acidic catalyst with one or more in methyl alcohol or methylal and formalin/trioxymethylene/paraformaldehyde to generate.And can decompose under the acidic conditions that exists at water of this reaction product.Dehydration becomes and improves the key of Synthesis conversion, and the boiling point of water is close with reaction intermediate component dmm2, again because of water and the azeotropic of formaldehyde, causes the common rectifying tower of use to be difficult to realize good dehydrating effect.At present mainly with molecular sieve adsorption, film dewaters or adds other component reaction or sponge moisture.Complex process and a large amount of waste can be caused, or bring impurity into and enter reaction system.
Summary of the invention
Goal of the invention: for above-mentioned Problems existing and defect, the utility model provides a kind of for the synthesis of polymethoxy dimethyl ether dewatering process device, and the effective elimination moisture of reactant while avoiding the bringing into of moisture, it does not introduce foreign matter.
Technical scheme: for achieving the above object, the utility model is by the following technical solutions: a kind of above-mentioned dewatering process device for the synthesis of polymethoxy dimethyl ether, comprise raw material surge tank, multi-stage type reactor, reaction solution surge tank and lightness-removing column, the outlet of described raw material surge tank is connected with multi-stage type reactor inlet, the tower top of described multi-stage type reactor is provided with gaseous phase outlet, is provided with reaction solution outlet at the bottom of tower; Described reaction solution outlet and reaction solution surge tank are communicated with and are connected with lightness-removing column afterwards; The tower top of described lightness-removing column is provided with methylal outlet, is provided with at the bottom of DMM2 outlet, tower and is provided with products export in tower.
As preferably, at the bottom of described tower, be also connected with rectification cell.
As preferably, described reaction tower tower body comprises at least two-layer conversion zone from top to bottom, and every layer of conversion zone is provided with column plate and forms bending runner, is filled with catalyzer between column plate, also be provided with vapor riser between the conversion zone of adjacent two layers, reaction tower tower top is also provided with gaseous phase outlet; Every layer of conversion zone is equipped with import and the outlet of band valve.
Beneficial effect: compared with prior art, formaldehyde gas within the utility model selection water content 0.1% and the methylal of high density are as reaction solution, first reduce bringing into of moisture from raw material business, utilize the hydrolysis reaction of methylal to remove residual water-content further simultaneously; Accomplish the recycling of reactant in whole technological process, adopt the methylal of formaldehyde as reaction solution simultaneously, relative to solid formaldehyde donor, the pressure and temperature of reaction system reduces further, thus reduces energy consumption.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Wherein, raw material surge tank 1, multi-stage type reactor 2, reaction solution surge tank 3, lightness-removing column 4.
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.
The dewatering process for the synthesis of polymethoxy dimethyl ether that the utility model provides, first bringing into of moisture is reduced from raw material, select the formaldehyde gas within water content 0.1% and the methylal (99%-99.5%) being dissolved in high density forms the methylal solution of formaldehyde, thus make reactant be react in the liquid phase, relative to paraformaldehyde and trioxymethylene, reaction conditions is reduced, then greatly reduce the water-content in reaction system relative to formaldehyde solution, avoid the existence of water to reduce the yield of polymethoxy dimethyl ether.The methylal of high density is containing a small amount of methyl alcohol, and decrease the amount of moisture that methyl alcohol participates in discharging when reaction generates methylal or dme, high-concentration methylal contacts with water and decomposition reaction can occur under acidic catalysis conditions simultaneously, and the hydrolysis reaction of methylal is as follows:
Contriver finds through lot of experiments: the intermediate component dimer DMM2 in polymethoxy dimethyl ether building-up process, certain azeotropy is had with glassware for drinking water, therefore reaction solution is again in lightness-removing column, controlling to suitable pressure and temperature makes water and DMM2 form azeotrope, thus depart from the middle part of lightness-removing column, realize dehydration object.The building-up process of polymethoxy dimethyl ether is as follows:
Below illustrate processing method step: as shown in Figure 1, the methylal solution of formaldehyde extracts (formaldehyde content is about 10-35%) out from reaction solution surge tank, and send into multi-stage type reactor, in multi-stage type reactor, formaldehyde and methylal polymerization reaction take place in liquid-phase system produces DMM2 ~ 8; Meanwhile, also there is side reaction: 1mol methylal reacts with 1mol water and generates the formaldehyde of 2mol methyl alcohol and 1mol under acidic catalysis conditions, thus can remove further containing a small amount of moisture in system, thus improve product yield.Generate a small amount of methyl alcohol and methylal is vaporized to tower top with the form of azeotrope under reacting liberated heat effect, overhead condenser is by its condensation, and partial reflux, material consists of the azeotropic of the methyl alcohol of 95-97 methylal and 3-5%.Variable-pressure rectification device of refining 99-99.5% methylal is delivered in part extraction.This process relies on methylal decomposition and consumption moisture, and utilizes methylal and methanol azeotropic to depart from methyl alcohol to achieve the interior object of dewatering of device.
Reaction solution pumps in reaction solution surge tank, enters in lightness-removing column.Methylals a large amount of in removed overhead reaction solution, 6. water-free reaction solution at the bottom of tower is delivered to next unit by logistics and is carried out rectifying, and the azeotropic of tower mid-way recovered water and intermediate component dmm2 forms, and azeotropic temperature is about 60-80 DEG C.Deliver to methylal synthesis unit.Thus realize second step dehydration.

Claims (3)

1. the dewatering process device for the synthesis of polymethoxy dimethyl ether, it is characterized in that: comprise raw material surge tank, multi-stage type reactor, reaction solution surge tank and lightness-removing column, the outlet of described raw material surge tank is connected with multi-stage type reactor inlet, the tower top of described multi-stage type reactor is provided with gaseous phase outlet, is provided with reaction solution outlet at the bottom of tower; Described reaction solution outlet and reaction solution surge tank are communicated with and are connected with lightness-removing column afterwards; The tower top of described lightness-removing column is provided with methylal outlet, is provided with at the bottom of DMM2 outlet, tower and is provided with products export in tower.
2. process unit according to claim 1, is characterized in that: be also connected with rectification cell at the bottom of described tower.
3. process unit according to claim 1, it is characterized in that: described reaction tower tower body comprises at least two-layer conversion zone from top to bottom, and every layer of conversion zone is provided with column plate and forms bending runner, catalyzer is filled with between column plate, also be provided with vapor riser between the conversion zone of adjacent two layers, reaction tower tower top is also provided with gaseous phase outlet; Every layer of conversion zone is equipped with import and the outlet of band valve.
CN201520313067.0U 2015-05-14 2015-05-14 A kind of dewatering process device for the synthesis of polymethoxy dimethyl ether Expired - Fee Related CN204644228U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105693479A (en) * 2016-03-15 2016-06-22 江苏凯茂石化科技有限公司 Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas
CN110508018A (en) * 2019-09-03 2019-11-29 中国石油大学(华东) Produce the device and method of polymethoxy dimethyl ether

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105693479A (en) * 2016-03-15 2016-06-22 江苏凯茂石化科技有限公司 Process device special for preparing polyoxymethylene dimethyl ethers through formaldehyde gas
CN110508018A (en) * 2019-09-03 2019-11-29 中国石油大学(华东) Produce the device and method of polymethoxy dimethyl ether
CN110508018B (en) * 2019-09-03 2022-02-25 中国石油大学(华东) Device and method for producing polymethoxy dimethyl ether

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Granted publication date: 20150916

Termination date: 20180514