CN209193846U - A kind of production technology device of novel DMMn - Google Patents

A kind of production technology device of novel DMMn Download PDF

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Publication number
CN209193846U
CN209193846U CN201821558202.8U CN201821558202U CN209193846U CN 209193846 U CN209193846 U CN 209193846U CN 201821558202 U CN201821558202 U CN 201821558202U CN 209193846 U CN209193846 U CN 209193846U
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tower body
dmmn
tower
partition
filler
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CN201821558202.8U
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向家勇
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Qingdao Zhuohui Chuang Neng New Energy Technology Co., Ltd
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Three Li Hubei Sweetgum Science And Technology 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
    • Y02P20/10Process efficiency

Abstract

The utility model discloses the production technology devices of novel DMMn a kind of, device includes reactive distillation column, the tower body of the reactive distillation column is equipped with material inlet, partition is equipped in tower body, the partition catalytic filler that is equipped with interior with respect to the tower of the side of material inlet is as catalytic reaction zone, filler is equipped in the tower of the other side of the partition as water district, the water district is equipped with intake, is respectively equipped with filler above and below the partition;The top of tower body is equipped with light fraction outlet, and the light fraction outlet connects external hanging type reactor by pipeline, catalytic filler is filled in the external hanging type reactor, and its outlet and the material inlet of tower body are connected by circulation;The bottom of the tower body is exported by pipeline equipped with crude product.The utility model reduces the positive progress that water content in reaction system is conducive to balanced reaction, improves the reaction efficiency and yield of DMMn, reduces the subsequent process for refining process of DMMn crude product, reduce production cost.

Description

A kind of production technology device of novel DMMn
Technical field
The utility model belongs to chemical production technical field more particularly to polymethoxy dimethyl ether (DMMn, n=3~8) Preparation process and device.
Background technique
China's derv fuel quality relatively Europe and north America region for be it is relatively low, be mainly manifested in sulfur content, ten In six alkane values and the content of aromatic hydrocarbons.45 or so, part light diesel fuel is only capable of reaching 40 China's derv fuel Cetane number average value, Therefore it is difficult to improve the performance of diesel engine.Although China has put into effect new derv fuel standard (GB19147-2009) for 2010, But existing oil refining process is difficult to produce satisfactory derv fuel.Arene content is high, and Cetane number is caused to decline, and fires It burns not exclusively, automobile exhaust pollution is than more serious.
Since diesel combustion pollutant emission is excessive, nearly 2 years statistical data are indicated, the nitrogen oxidation of China Diesel vehicle discharge For object close to the 70% of vehicle mass exhaust total quantity, particulate matter is more than 90%.Automotive emission have become air pollution it is important because Element, and haze weather frequently occurs, and how effectively to administer PM2.5, tail gas pollution of motor-driven vehicle, becomes the hot spot of social concerns. Start with from the oil product in source, could really solve the problems, such as diesel vehicle " black smoke from exhaust ", increases diesel oil oxygen-containing component by expert It is considered diesel oil cleaning developing direction.The presence of oxygen atom allows fuel to be produced from burning for oxygen effect, and oxidizing fire is more Completely;And not sulfur-bearing in fuel, it can significantly reduce the discharge amount of soot, particle and carbon monoxide, pollution be effectively reduced, improve The thermal efficiency of engine, energy conservation, good economy performance, and can be reconciled with terminal.
Polymethoxy dimethyl ether (DMM3~8) it is the novel environment-friendly for reducing oil consumption and reducing flue gas emission generally acknowledged in the world Fuel oil blend component has Cetane number high (80~100), and low temperature flow is good, can improve the combustibility of diesel oil, reduces The discharge of vehicle exhaust.Its physical property is close with diesel oil, be blended into diesel oil be used without to vehicle motor oil supply system into Row transformation.External major company carries out R and D to the production technology in succession, is shown by test and application study: addition 20% this oxycompound, smoke intensity highest, which can reduce by 80%~90%, NOx, can reduce by 50%, while the thermal efficiency is also than existing It is being applied alone diesel oil to want high.But the technology of this kind of compound of synthesis has not been achievable industrialization in the world at present, this is because DMM3~8Synthesis process complexity, severe reaction conditions, equipment seriously corroded, the reasons such as product yield is low and seriously affect The development of its technology.
Polymethoxy dimethyl ether (DMM3-8) also known as polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ethers, the contracting of polymethoxy first Aldehyde, is the common name of a substance, and skeleton symbol can indicate are as follows: CH3O (CH2O) nCH3 (wherein, n >=1, general value less than 10, It is indicated with DMMn).
The country mostly uses metaformaldehyde, paraformaldehyde etc. and methanol for raw material at present, complex technical process, and feed product disappears Consumption and energy consumption are higher, and exist in polycondensation reaction control severe reaction conditions, process is complicated, product yield is undesirable, A series of problems, such as equipment seriously corroded, catalyst is at high cost.
A kind of patent of method that polymethoxy dimethyl ether is prepared by methanol and formaldehyde of Publication No. CN104341279A The technology with methanol and formalin directly as raw material production DMMn is disclosed, but formalin is brought into and is in the technology Water content in system is excessively high, reduces reaction yield and efficiency, and the subsequent purification of also not subsequent DMMn product brings process cumbersome, To improve production cost.
Summary of the invention
Goal of the invention: being directed to above-mentioned existing problem and shortage, and the purpose of the utility model is to provide a kind of novel The production technology device of DMMn reduces the positive progress that water content in reaction system is conducive to balanced reaction, improves DMMn Reaction efficiency and yield, the subsequent process for refining process of DMMn crude product is reduced, to reduce production cost.
Technical solution: in order to solve the above-mentioned technical problem, the utility model uses a kind of following technical scheme: novel DMMn Production technology device, including reactive distillation column, the tower body of the reactive distillation column is equipped with material inlet, be equipped in tower body every Plate, the partition with respect to being equipped with catalytic filler in the tower of the side of material inlet as catalytic reaction zone, the partition it is another Filler is equipped in the tower of side as water district, the water district is equipped with intake, is respectively equipped with above and below the partition Filler;The top of the tower body is equipped with light fraction outlet, and the light fraction outlet connects external hanging type reactor by pipeline, described Catalytic filler is filled in external hanging type reactor, and its outlet and the material inlet of tower body are connected by circulation;The bottom of the tower body It is exported by pipeline equipped with crude product.
Preferably, being connected with condenser on the pipeline of the light fraction outlet at the top of the tower body, and pipeline is equipped with branch Pipe is connect with tower body.
Preferably, the bottom of the tower body is additionally provided with reboiler, and it is connect with tower body bottom cycle.
The utility model additionally provides the manufacturing technique method of DMMn based on above-mentioned apparatus a kind of, comprising the following steps:
(1) smart from reaction after mixing using formaldehyde that pure methanol and mass concentration are 37~65% concentration as reaction raw materials The reaction zone in the material inlet feeding tower of tower is evaporated, for control reaction zone temperature at 80~150 DEG C, reactive distillation tower pressure interior force is 1 Two steps occur under the action of catalytic filler and react to obtain dimethoxym ethane and DMMn for~5KG, material;
(2) reaction obtain comprising dimethoxym ethane, formaldehyde, first alcohol and water light component in reactive distillation column rectifying flow up And it exports and flows out from tower top light component;Reaction obtains the heavy constituent comprising water, formaldehyde and DMMn and flows downward, by filling out for lower section Material carries out rectification process, further steams light component;
(3) light component flowed out from tower top is sent into the catalysis of external hanging type reactor further progress after condenser condenses Reaction, and send the thing liquid after reaction back to reactive distillation column;
(4) reactive distillation tower bottom control temperature 180~220 DEG C by the component comprising water in heavy constituent steam from every The intake of the water district of plate produces, and balanced reaction forward direction is pushed to carry out;From the thick production of the bottom of reactive distillation column extraction DMMn Product.
Preferably, the temperature of the intake is 120~160 DEG C.
Preferably, the DMMn crude product part of the reactive distillation column tower bottom extraction is recycled by reboiler and is sent into reaction Rectifier bottoms.
Preferably, the external hanging type reactor has multiple reactors to connect or/and compose in parallel.
The utility model has the advantages that compared with prior art, the utility model has the advantage that (1) effectively shortens process flow, Reduce appliance arrangement, reduces operation difficulty and equipment funds investment;(2) balanced reaction is promoted by system online acquisition water Forward direction carries out, and improves reaction efficiency and target product yield.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the production technology device of methoxyl group dimethyl ether DMMn described in the utility model.
Wherein, tower body 1, partition 2, material inlet 3, catalytic filler 4, filler 5, condenser 6, external hanging type reactor 7, water intaking Area 8, reboiler 9.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the utility model is furtherd elucidate, it should be understood that these embodiments are only used for Illustrate the utility model rather than limitation the scope of the utility model, after having read the utility model, art technology Personnel fall within the application range as defined in the appended claims to the modification of the various equivalent forms of the utility model.
The production technology principle of the utility model polymethoxy dimethyl ether DMMn is: being urged first by methanol and formaldehyde Change reaction on filler and obtain dimethoxym ethane, then synthesizes to obtain polymethoxy diformazan with formalin to produce obtained dimethoxym ethane Ether, chemical reaction process are as follows:
As shown in Figure 1, the production process of the utility model DMMn is specific as follows:
(1) smart from reaction after mixing using formaldehyde that pure methanol and mass concentration are 37~65% concentration as reaction raw materials The reaction zone in the material inlet feeding tower of tower is evaporated, controls reaction zone temperature at 80~120 DEG C, tower pressure interior force is in 1~5KG, object The reaction of two steps occurs under the action of catalytic filler for material, and catalysis oxidation obtains dimethoxym ethane first, and dimethoxym ethane is that formaldehyde reacts To DMMn, polymerization reaction can be continued to participate in for the low polymerization degree of n=1 or 2;The formalin of higher concentration is former as reaction Expect it is also possible, only when concentration of formaldehyde is higher, when water content is lower, the utility model efficiency of producing drinking water relative reduction, save The ratio relative drop of cost, therefore for the formaldehyde of 37~65% concentration, effect is best.
(2) it mainly includes dimethoxym ethane, formaldehyde, first alcohol and water that reaction, which obtains light component, and rectifying is upward in reactive distillation column It flows and is exported from tower top light component and flowed out;Reaction obtains the heavy constituent comprising water, formaldehyde and DMMn (n > 2) and flows downward, and passes through The filler for crossing lower section carries out rectification process, further steams light component to realize rectification process;
(3) contain the complete dimethoxym ethane of unreacted, formaldehyde and methanol from the light component that tower top flows out, condensed by condenser Afterwards, it is sent into further progress catalysis reaction in external hanging type reactor, improves reaction yield, and send the product after reaction back to reaction Rectifying column carries out circular response;
(4) at the same time, reactive distillation tower bottom control temperature is at 200 DEG C or so by the component comprising water in heavy constituent It steams and is produced from the intake of the water district of partition, intake temperature is controlled at 150~160 DEG C, and the water content of recovered water is reachable 99% (and a small amount of formaldehyde etc.), so as to push balanced reaction forward direction to carry out, recovered water is as technique water circulation use. From the crude product of the bottom of reactive distillation column extraction DMMn, mainly including DMMn, Yi Jishui, dimethoxym ethane etc., and it is sent to subsequent fine Process processed further refines purification.

Claims (3)

1. a kind of production technology device of novel DMMn, it is characterised in that: including reactive distillation column, the tower of the reactive distillation column Body is equipped with material inlet, and partition is equipped in tower body, and the partition is interior with respect to the tower of the side of material inlet to be equipped with catalytic filler Filler is equipped with as catalytic reaction zone, in the tower of the other side of the partition as water district, the water district is equipped with intake, Filler is respectively equipped with above and below the partition;The top of the tower body is equipped with light fraction outlet, the light fraction outlet External hanging type reactor is connected by pipeline, catalytic filler, and the object of its outlet and tower body are filled in the external hanging type reactor Material entrance is connected by circulation;The bottom of the tower body is exported by pipeline equipped with crude product.
2. the production technology device of novel DMMn according to claim 1, it is characterised in that: the light component at the top of the tower body Condenser is connected on the pipeline of outlet, and pipeline is equipped with branch pipe and connect with tower body.
3. the production technology device of novel DMMn according to claim 1, it is characterised in that: the bottom of the tower body is additionally provided with Reboiler, and connect with tower body bottom cycle.
CN201821558202.8U 2018-09-21 2018-09-21 A kind of production technology device of novel DMMn Active CN209193846U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110559678A (en) * 2019-10-21 2019-12-13 无锡赫利邦化工科技有限公司 rectifying tower for synthesizing and separating polymethoxy dimethyl ether and use method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110559678A (en) * 2019-10-21 2019-12-13 无锡赫利邦化工科技有限公司 rectifying tower for synthesizing and separating polymethoxy dimethyl ether and use method thereof
CN110559678B (en) * 2019-10-21 2024-02-27 无锡赫利邦化工科技有限公司 Rectifying tower for synthesizing and separating polymethoxy dimethyl ether and application method thereof

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Effective date of registration: 20200708

Address after: No.117, YINGSHANHONG Road, gugugukou, Huangdao District, Qingdao City, Shandong Province

Patentee after: Qingdao Zhuohui Chuang Neng New Energy Technology Co., Ltd

Address before: 430070 Hubei city of Wuhan province East Lake New Technology Development Zone, Luoyu Road shops along the Street No. 490-518 Optics Valley world city B block 1 Building 2 unit 8 room 20

Patentee before: HUBEI SANLIFENGXIANG TECHNOLOGY Co.,Ltd.