CN109761771A - The method of polymerizable raw material is reduced in a kind of preparation of polymethoxy dimethyl ether - Google Patents
The method of polymerizable raw material is reduced in a kind of preparation of polymethoxy dimethyl ether Download PDFInfo
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- CN109761771A CN109761771A CN201910070662.9A CN201910070662A CN109761771A CN 109761771 A CN109761771 A CN 109761771A CN 201910070662 A CN201910070662 A CN 201910070662A CN 109761771 A CN109761771 A CN 109761771A
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Abstract
The invention discloses the methods that polymerizable raw material is reduced in a kind of preparation of polymethoxy dimethyl ether: by the byproduct PODE from product separator2Concentration formaldehyde tank is fully incorporated to mix with the highly concentrated formaldehyde solution in tank；It is mixed with PODE2Formalin be directly entered PODE synthesis reactor from concentration formaldehyde tank extraction and reacted；Reaction product after reaction enters product separator and is isolated to byproduct PODE2.The present invention passes through to PODE2It recycles, improves the product distribution in reactor, improve the selectivity of target product, reduce the crystalline deposit that oxymethylene polymerization is formed under low temperature, guarantee the normal operation of production.
Description
Technical field
The invention belongs to chemical production technology fields, for the production of polymethoxy dimethyl ether, specifically, being related to one kind
The method of polymerizable raw material is reduced in polymethoxy dimethyl ether preparation.
Background technique
Polymethoxy dimethyl ether (abbreviation PODE), molecular formula: CH3O (CH2O)nCH3 (n >=1), different polymerization degree ns
PODE, with PODEnIt indicates.Wherein PODE3-8Oxygen mass fraction (42%~51%) with higher and Cetane number (60 with
On), it is a kind of high cleaning Cetane number diesel oil blending component, physical property is close with diesel oil, is added in diesel oil and serves as fuel not
It will affect the combustibility of diesel oil and the discharge of COx and NOx can be reduced, 20% PODE is added in diesel oil3-8, particulate emission
Highest, which can reduce by 80%~90%, NOx, can reduce by 50%, be novel environment friendly diesel oil addO-on therapy generally acknowledged at present.
The research and development technique for the polymethoxy dimethyl ether reported at present mostly uses metaformaldehyde or paraformaldehyde is raw material,
CN104591984 propose prepare polymethoxy dimethyl ether as raw material so that formaldehyde is concentrated method, this method with concentration for 80% with
On formaldehyde concentrated liquid be raw material, react to obtain polymethoxy dimethyl ether with methanol or dimethoxym ethane.The method is solved with three
Polyformaldehyde or paraformaldehyde are the problems such as production capacity existing for the technique of raw material is limited, yield is lower, reaction measuring difficulties.This is always flowed
Journey includes methanol formaldehyde plant, dimethoxym ethane device, formaldehyde enrichment facility and polymethoxy dimethyl ether device.
But wherein spontaneous polymerization easily occurs for formalin, i.e., when low temperature is long placed in, easily occurs muddy, bottom inside solution
Generate paraformaldehyde white depositions.And concentration of formaldehyde is higher, is more easy to happen polycondensation reaction, generates the very big indissoluble of the degree of polymerization
Chain paraformaldehyde.The storage temperature of control basin is generallyd use in actual production at present, basin installs blender, avoids cold table
Face, the methods such as addition formol polymerization retarder prevent formaldehyde autohemagglutination.
To be concentrated in the device that formalin produces polymethoxy dimethyl ether as raw material, cannot additionally be inhibited by adding
The method of agent prevents formaldehyde autohemagglutination.When the heat tracing of formaldehyde basin and conveyance conduit breaks down, concentration formalin can pole
Crystalline deposit is easily formed, the normal operation of production is influenced.
Summary of the invention
In order to solve the technical issues of formaldehyde autohemagglutination of the existing technology is also easy to produce precipitating, it is poly- that the present invention provides one kind
Methoxyl group dimethyl ether is for the middle method for reducing polymerizable raw material.
The method that polymerizable raw material is reduced in polymethoxy dimethyl ether preparation provided by the invention mainly includes the following steps:
1) by the byproduct PODE from product separator2It is fully incorporated concentration formaldehyde tank and the high-concentration formaldehyde in tank is molten
Liquid mixing；
2) it is mixed with byproduct PODE2Formalin from concentration formaldehyde tank extraction be directly entered PODE synthesis reactor into
Row reaction；
3) reaction product after reacting enters product separator and is isolated to byproduct PODE2。
It is of course also possible to by the byproduct PODE from product separator2It is divided into two parts, a part introduces concentration formaldehyde
Tank, another part introduce concentration formaldehyde tank extraction pipeline in from be concentrated formaldehyde tank extract mix after be directly entered
PODE synthesis reactor is reacted.
The byproduct PODE for introducing concentration formaldehyde tank2Introduce be concentrated formaldehyde tank before be divided into two strands, one directly into
Enter and formaldehyde tank is concentrated, into dense after being mixed in the feeding line of another burst of introducing concentration formaldehyde tank with highly concentrated formaldehyde solution in pipe
Formal tank.
The byproduct PODE2Temperature when introducing concentration formaldehyde tank is 70~130 DEG C, and in device arrangement, formaldehyde is dense
Contracting tank arranges that the pipeline containing formaldehyde is short as far as possible close to polymethoxy dimethyl ether synthesis reactor, polymethoxy dimethyl ether synthesis
Raw material surge tank is no longer separately provided in reactor.
Method of the present invention is suitable for all techniques for preparing polymethoxy dimethyl ether as raw material so that formaldehyde is concentrated.
Method of the invention has the advantages that compared with prior art
1)PODE2It recycles, improves the product distribution in reactor, improve the selectivity of target product.
2)PODE2It can play the role of formol polymerization retarder and diluent, when event occurs for the heat tracing of Formaldehyde Tank and pipeline
When barrier, it is possible to reduce the crystalline deposit that oxymethylene polymerization is formed under low temperature guarantees the normal operation of production.
3) close to arrangement, polymethoxy dimethyl ether device is no longer independent for formaldehyde enrichment facility and polymethoxy dimethyl ether device
Raw material surge tank and reaction feed pump are set, not only reduce the equipment investment of device, and reduce in conventional design Central Plains
The setting of material surge tank and reaction feed pump enables the risk for leading to the problem of precipitating containing formaldehyde pipeline increase.
Detailed description of the invention
Fig. 1 is whole byproduct PODE2It is introduced directly into the process flow diagram of concentration formaldehyde tank；
Fig. 2 is whole byproduct PODE2It is divided to two strands of process flow diagrams for introducing concentration formaldehyde tank；
Fig. 3 is part byproduct PODE2Introduce the process flow diagram of concentration formaldehyde tank.
In figure: formaldehyde tank, 2- force (forcing) pump, 3-PODE synthesis reactor, 4- product separator, 5- byproduct is concentrated in 1-
PODE2, 6- highly concentrated formaldehyde solution.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing, but does not limit the scope of the invention.As shown in Figure 1, coming
From the byproduct PODE of product separator25 are all introduced directly into concentration formaldehyde tank 1 mixes with the highly concentrated formaldehyde solution in tank,
It is mixed with PODE2Formalin from concentration formaldehyde tank 1 extract out it is pressurized pump 2 pressurization after be directly entered PODE synthesis reactor 3
It is reacted, the reaction product after reaction enters product separator 4 and is isolated to byproduct PODE2 5。
As shown in Fig. 2, introducing the byproduct PODE of concentration formaldehyde tank 125 are divided into two strands before introducing concentration formaldehyde tank 1,
One is directly entered concentration formaldehyde tank 1, and the feeding line of another burst of introducing concentration formaldehyde tank 1 is interior and manages interior highly concentrated formaldehyde solution
Enter concentration formaldehyde tank 1 after 6 mixing.
As shown in figure 3, the byproduct PODE from product separator2It is divided into two parts, a part introduces concentration formaldehyde tank
1, another part introduce in the extraction pipeline of concentration formaldehyde tank 1 with from the extract that formaldehyde tank 1 is concentrated mix after into PODE
Synthesis reactor 3.
Polymethoxy dimethyl ether device is raw as raw material using 80% or more highly concentrated formaldehyde solution and methanol and/or dimethoxym ethane
Produce PODE3-8, device byproduct PODE2It recycles.The PODE recycled2, it is sent into the high-concentration formaldehyde of formaldehyde enrichment facility
Pipeline or concentration formaldehyde tank, PODE2Into formaldehyde enrichment facility temperature be 70~130 DEG C, mixed material through pump boosting after send to
PODE synthesis reactor in polymethoxy dimethyl ether device.Formaldehyde enrichment facility and polymethoxy dimethyl ether device close on cloth
It sets, shortens the duct length of the material containing formaldehyde between concentration formaldehyde tank and PODE synthesis reactor as far as possible.
Claims (5)
1. reducing the method for polymerizable raw material in a kind of polymethoxy dimethyl ether preparation, it is characterised in that mainly include the following steps:
1) by the byproduct PODE from product separator2The highly concentrated formaldehyde solution being fully incorporated in concentration formaldehyde tank and tank is mixed
It closes；
2) it is mixed with byproduct PODE2Formalin from concentration formaldehyde tank extraction be directly entered PODE synthesis reactor carry out it is anti-
It answers；
3) reaction product after reacting enters product separator and is isolated to byproduct PODE2。
2. reducing the method for polymerizable raw material in a kind of polymethoxy dimethyl ether preparation, it is characterised in that mainly include the following steps:
1) by the byproduct PODE from product separator2It is divided into two parts, a part introduces concentration formaldehyde tank, and another part draws
Enter to be concentrated in the extraction pipeline of formaldehyde tank with from the extract that formaldehyde tank is concentrated mix after be directly entered PODE synthesis reactor
It is reacted；
2) reaction product after reacting enters product separator and is isolated to byproduct PODE2。
3. method according to claim 1 or 2, it is characterised in that: the byproduct PODE for introducing concentration formaldehyde tank2?
It is divided into two strands before introducing concentration formaldehyde tank, one is directly entered concentration formaldehyde tank, and another strand introduces the feed pipe that formaldehyde tank is concentrated
Enter concentration formaldehyde tank after mixing in line with highly concentrated formaldehyde solution in pipe.
4. method according to claim 1 or 2, it is characterised in that: the byproduct PODE2It introduces when formaldehyde tank is concentrated
Temperature is 70~130 DEG C.
5. according to the method described in claim 3, it is characterized by: the byproduct PODE2Introduce temperature when concentration formaldehyde tank
It is 70~130 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910070662.9A CN109761771A (en) | 2019-01-25 | 2019-01-25 | The method of polymerizable raw material is reduced in a kind of preparation of polymethoxy dimethyl ether |
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| CN201910070662.9A CN109761771A (en) | 2019-01-25 | 2019-01-25 | The method of polymerizable raw material is reduced in a kind of preparation of polymethoxy dimethyl ether |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513141A (en) * | 2013-09-29 | 2015-04-15 | 苏州奥索特新材料有限公司 | Reaction system and method for preparing polyoxymethylene dimethyl ether |
| CN104591984A (en) * | 2014-12-12 | 2015-05-06 | 北京东方红升新能源应用技术研究院有限公司 | Method for preparing polymethoxy dimethyl ether from concentrated formaldehyde serving as raw material |
| CN106397143A (en) * | 2016-10-08 | 2017-02-15 | 江苏凯茂石化科技有限公司 | Process device and method for producing polyoxymethylene dimethyl ethers matched with formaldehyde by iron-molybdenum process |
| CN107286004A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工股份有限公司 | The refined method of polyoxymethylene dimethyl ether |
| CN107652169A (en) * | 2017-11-08 | 2018-02-02 | 江苏道尔顿石化科技有限公司 | A kind of preparation technology of polymethoxy dimethyl ether production formaldehyde alcoholic solution |
| CN107739301A (en) * | 2017-11-08 | 2018-02-27 | 江苏道尔顿石化科技有限公司 | A kind of polymethoxy dimethyl ether synthesis system and technique |
-
2019
- 2019-01-25 CN CN201910070662.9A patent/CN109761771A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513141A (en) * | 2013-09-29 | 2015-04-15 | 苏州奥索特新材料有限公司 | Reaction system and method for preparing polyoxymethylene dimethyl ether |
| CN104591984A (en) * | 2014-12-12 | 2015-05-06 | 北京东方红升新能源应用技术研究院有限公司 | Method for preparing polymethoxy dimethyl ether from concentrated formaldehyde serving as raw material |
| CN107286004A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工股份有限公司 | The refined method of polyoxymethylene dimethyl ether |
| CN106397143A (en) * | 2016-10-08 | 2017-02-15 | 江苏凯茂石化科技有限公司 | Process device and method for producing polyoxymethylene dimethyl ethers matched with formaldehyde by iron-molybdenum process |
| CN107652169A (en) * | 2017-11-08 | 2018-02-02 | 江苏道尔顿石化科技有限公司 | A kind of preparation technology of polymethoxy dimethyl ether production formaldehyde alcoholic solution |
| CN107739301A (en) * | 2017-11-08 | 2018-02-27 | 江苏道尔顿石化科技有限公司 | A kind of polymethoxy dimethyl ether synthesis system and technique |
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Application publication date: 20190517 |