CN106631722A - DMMn synthesis device and synthesis method adopting DMMn synthesis device - Google Patents
DMMn synthesis device and synthesis method adopting DMMn synthesis device Download PDFInfo
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- CN106631722A CN106631722A CN201611007531.9A CN201611007531A CN106631722A CN 106631722 A CN106631722 A CN 106631722A CN 201611007531 A CN201611007531 A CN 201611007531A CN 106631722 A CN106631722 A CN 106631722A
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- China
- Prior art keywords
- dissolving tank
- polymer reactor
- polyformaldehyde
- dimethyl ether
- polymerization
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
Abstract
The invention discloses a DMMn synthesis device and a synthesis method adopting the DMMn synthesis device. The DMMn synthesis device comprises a dissolving tank A and a dissolving tank B, wherein a methylal feed port and an alpha-polyformaldehyde feed port I are formed in the upper end of the dissolving tank A; a first polymerization reactor and a second polymerization reactor which are communicated at the top are arranged on one side of the dissolving tank A, the bottom of the first polymerization reactor is communicated with the bottom of the dissolving tank A through a communicating pipe I, and a first high-pressure pump is mounted at the bottom of the communicating pipe I; the dissolving tank B is arranged on one side of the second polymerization reactor, the bottom of the second polymerization reactor is communicated with the top of the dissolving tank B, and an alpha-polyformaldehyde feed port II is formed in the top of the dissolving tank B; a third polymerization reactor and a fourth polymerization reactor which are communicated at the top are arranged on one side of the dissolving tank B, the bottom of the third polymerization reactor is communicated with the bottom of the dissolving tank B through a communicating pipe II, and a second high-pressure pump is mounted on the communicating pipe II; a DMMn discharge pipeline is arranged at the bottom of the fourth polymerization reactor. The raw materials are added reasonably, and a technology of first decomposition and later polymerization is adopted, so that the technical problem of DMMn synthesis with alpha-polyformaldehyde is solved.
Description
Technical field
The present invention relates to chemical industry synthesis field, more particularly to a kind of polymethoxy dimethyl ether synthesizer and its synthesis side
Method.
Background technology
Polymethoxy dimethyl ether, also known as polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ethers, polymethoxy methylal, are one
The common name of class material, its skeleton symbol can be expressed as：CH3O(CH2O)nCH3(wherein, n >=1, general value is less than 10, with DMMn
Represent).
Two kinds of routes of existing synthesis technique in the world, a kind of metaformaldehyde route, a kind of formaldehyde route, metaformaldehyde route
Process is simple, raw material metaformaldehyde high cost, the bad acceptance in market after industrialization, formaldehyde route process route is long, once
Rate is low to separate difficulty, has a large amount of hemiacetals to generate in building-up process, is close to finished product boiling point, it is difficult to which separation is clear from finished product, plus
Big separation costs, affect product quality.
Countries in the world and studies in China department, more using the route of metaformaldehyde, but due to metaformaldehyde it is expensive, institute
With the polymethoxy dimethyl ether high cost produced with the method.In preparation method by methyl alcohol and formaldehyde, water is used as anti-
Product is answered, polymethoxy dimethyl ether can be hydrolyzed in the presence of acidic, form unstable hemiacetal.And in final products
Containing hemiacetal, the flash-point of diesel fuel mixtures will be to a certain extent reduced, and then damage the quality of the mixture, meanwhile, bavin
The flash-point of oil mixture is too low to be caused no longer meet the specification requirement that related DIN standards specify.And hemiacetal and poly- methoxy
Base dimethyl ether has close boiling point, and hemiacetal is once generated, it will be difficult to separated from product.Formed as primary product
Dimer equally there is low boiling, so similarly reduce flash-point, so unsuitable for as diesel fuel additives.Trimerization first
Aldehyde route, formalin route is required for more than 60% content of formaldehyde, and existing formaldehyde production technology concentrate is big to 60% needs one
Expense.Paraformaldehyde route, due to polymerization when initiator presence shade to the later stage polymerization, with reference to the presence water content of water
It is unable to reach less than 1%.The achievement of many research departments, because Cost Problems cannot be introduced into industrialized production.
Additionally, α-polyoxymethylene weight is big, course of dissolution viscosity is excessive, make general stirring do cannot normal work, polymerization
Product it is abnormal, viscosity is big when in the world existing synthesizer can not meet α-polyformaldehyde synthesis polymethoxy dimethyl ether, makes
Product slates are unreasonable, the bad control of N values.
The content of the invention
It is an object of the invention to provide a kind of polymethoxy dimethyl ether synthesizer and its synthetic method, solve trimerization first
Aldehyde route raw material high cost, formaldehyde route complex process separates expensive, final products high cost, and α-polyformaldehyde synthesizes poly- methoxy
Viscosity is big during base dimethyl ether, makes product slates unreasonable, the preparation side of the polymethoxy dimethyl ether of the problem of the bad control of N values
Method.
Above-mentioned purpose is realized by below scheme：
A kind of polymethoxy dimethyl ether synthesizer, including dissolving tank A, dissolving tank B, dissolving tank A upper ends are provided with dimethoxym ethane charging
Mouth, α-polyformaldehyde charging aperture one, bottom is provided with outlet；
Dissolving tank A sides are provided with the first polymer reactor, second polymer reactor of top mutually UNICOM, the first polymer reactor
Bottom inlet, by being connected communicating pipe one, is provided with the first high-pressure pump with dissolving tank A outlet at bottoms on communicating pipe one；
Second polymer reactor side is provided with dissolving tank B, the second polymer reactor bottom and dissolving tank B tops reactant liquor import phase
Connection, dissolving tank B tops are additionally provided with α-polyformaldehyde charging aperture two；
Dissolving tank B sides are provided with third polymerization reactor, the 4th polymer reactor that top is connected, third polymerization reactor bottom
Portion, by being connected communicating pipe two, is provided with the second high-pressure pump with dissolving tank B bottoms on communicating pipe two；
4th polymer reactor bottom is provided with polymethoxy dimethyl ether discharge pipe.
Described polymethoxy dimethyl ether synthesizer, it is characterised in that described the first polymer reactor, the second polymerization
Catalyst is filled with reactor, third polymerization reactor, the 4th polymer reactor, catalyst adopts resin cation.
Described polymethoxy dimethyl ether synthesizer, it is characterised in that the second described polymer reactor bottom with it is molten
The first safety valve is respectively equipped with the top of solution tank B on the connecting pipe of reactant liquor import, the 4th polymer reactor bottom discharge pipeline
Door, the second safety valve.
The method that a kind of synthesizer described in utilization claim 1 prepares polymethoxy dimethyl ether, it is characterised in that：Bag
Include following steps：
1）, prepare raw material：According to weight portion 2:1 ratio prepares dimethoxym ethane, α-polyformaldehyde；
2）, for the first time add α-polyformaldehyde depolymerization：Ready dimethoxym ethane is added in dissolving tank A, α-poly- first is then passed through again
Aldehyde charging aperture one adds α-polyformaldehyde, and at 80 ~ 180 DEG C, time control makes dimethoxym ethane and α-polyformaldehyde to temperature control in 2 ~ 12h
Fully it is dissolved into mixed liquor one；
3）, first set reaction：After the completion of dissolving, mixed liquor is sent to the first polymer reactor and second by the first high pressure pump work
Reacted in polymer reactor, 50 ~ 150 DEG C of temperature, 1 ~ 3MPA of pressure, time control obtains low polymerization degree and gather in 20 ~ 30h
Methoxyl group dimethyl ether solution, between degree of polymerization N1 ~ 3；
4）, the first high pressure pump work, the second high-pressure pump and dissolving tank B do not work, by low polymerization degree polymethoxy dimethyl ether solution
It is sent to dissolving tank B；
5）, again add α-polyformaldehyde depolymerization：Dissolving tank B works, and secondary addition α-polyformaldehyde, addition is identical with first time,
, at 80 ~ 180 DEG C, time control is in 2 ~ 12h for dissolving tank B temperature controls so that low polymerization degree polymethoxy dimethyl ether solution and two
Secondary addition α-polyformaldehyde is fully dissolved into mixed liquor two；
6）, secondary response again：First high-pressure pump and dissolving tank A do not work, the second high pressure pump work, and mixed liquor two is sent to into the 3rd
Reacted in polymer reactor and the 4th polymer reactor, 50 ~ 150 DEG C of temperature, 1 ~ 3MPA of pressure, time control 20 ~
30h, obtains higher degrees of polymerization polymethoxy dimethyl ether solution, i.e. polymethoxy dimethyl ether finished product, between degree of polymerization N2 ~ 5.
Beneficial effects of the present invention are：
1st, α-polyformaldehyde of the present invention and methylal synthesis polymethoxy dimethyl ether, the product synthesized with metaformaldehyde is identical
100% is dissolved in diesel oil, and long-time is not stratified to dissolve each other completely；
2nd, the polymethoxy dimethyl ether of other formaldehyde products productions, is not strictly disjointed only 30% or so and is dissolved in diesel oil, completely
Metaformaldehyde is instead of, whole process is simple processing charges low cost is made；
3rd, present configuration is novel in design, can by α-polyformaldehyde synthesis polymethoxy dimethyl ether when, dimethoxym ethane and α-polyformaldehyde
Mixing depolymerization is carried out through dissolving tank A, then coordinates the first polymer reactor, the second polymer reactor primary first-order equation, dissolving tank B holds
Secondary to add secondary α-polyformaldehyde, Jing third polymerization reactors, the 4th polymer reactor secondary response again efficiently solves α-poly- first
Aldehyde add fashionable viscosity it is big distribution it is undesirable, the finished product N values of product are controllable, the good product quality of polymerization；
4th, present invention employs and first decompose the technique being polymerized again, the technology for solving α-polyformaldehyde synthesis polymethoxy dimethyl ether is difficult
Topic.
Description of the drawings
Fig. 1 is the structural representation of the present invention.
Specific embodiment
Polymethoxy dimethyl ether synthesizer, including dissolving tank A, dissolving tank B, dissolving tank A upper ends are provided with dimethoxym ethane charging
Mouth 1, α-polyformaldehyde charging aperture 1, bottom is provided with outlet；
Dissolving tank A sides are provided with the first polymer reactor 3, second polymer reactor 4 of top mutually UNICOM, the first polymerisation
The bottom inlet of device 3, by being connected communicating pipe 1, is provided with the first high-pressure pump 6 with dissolving tank A outlet at bottoms on communicating pipe 1；
The side of second polymer reactor 4 is provided with dissolving tank B, the bottom of the second polymer reactor 4 and dissolving tank B top reactant liquor imports
It is connected, dissolving tank B tops are additionally provided with α-polyformaldehyde charging aperture 27；
Dissolving tank B sides are provided with third polymerization reactor 8, the 4th polymer reactor 9 that top is connected, third polymerization reactor
8 bottoms, by being connected communicating pipe 2 10, are provided with the second high-pressure pump 11 with dissolving tank B bottoms on communicating pipe 2 10；
The bottom of 4th polymer reactor 9 is provided with polymethoxy dimethyl ether discharge pipe 12.
Filling in first polymer reactor 3, the second polymer reactor 4, third polymerization reactor 8, the 4th polymer reactor 9
There is catalyst 13, catalyst adopts resin cation.
The bottom of second polymer reactor 4 and connecting pipe, the 4th polymer reactor bottom of dissolving tank B top reactant liquor imports
The first safety-valve 14, the second safety valve 15 are respectively equipped with portion's discharge pipe.
A kind of method that utilization synthesizer prepares polymethoxy dimethyl ether, it is characterised in that：Comprise the following steps：
1）, prepare raw material：According to weight portion 2:1 ratio prepares dimethoxym ethane, α-polyformaldehyde；
2）, for the first time add α-polyformaldehyde depolymerization：Ready dimethoxym ethane is added in dissolving tank A, α-poly- first is then passed through again
Aldehyde charging aperture one adds α-polyformaldehyde, and at 80 ~ 180 DEG C, time control makes dimethoxym ethane and α-polyformaldehyde to temperature control in 2 ~ 12h
Fully it is dissolved into mixed liquor one；
3）, first set reaction：After the completion of dissolving, mixed liquor is sent to the first polymer reactor and second by the first high pressure pump work
Reacted in polymer reactor, 50 ~ 150 DEG C of temperature, 1 ~ 3MPA of pressure, time control obtains low polymerization degree and gather in 20 ~ 30h
Methoxyl group dimethyl ether solution, between degree of polymerization N1 ~ 3；
4）, the first high pressure pump work, the second high-pressure pump and dissolving tank B do not work, by low polymerization degree polymethoxy dimethyl ether solution
It is sent to dissolving tank B；
5）, again add α-polyformaldehyde depolymerization：Dissolving tank B works, and secondary addition α-polyformaldehyde, addition is identical with first time,
, at 80 ~ 180 DEG C, time control is in 2 ~ 12h for dissolving tank B temperature controls so that low polymerization degree polymethoxy dimethyl ether solution and two
Secondary addition α-polyformaldehyde is fully dissolved into mixed liquor two；
6）, secondary response again：First high-pressure pump and dissolving tank A do not work, the second high pressure pump work, and mixed liquor two is sent to into the 3rd
Reacted in polymer reactor and the 4th polymer reactor, 50 ~ 150 DEG C of temperature, 1 ~ 3MPA of pressure, time control 20 ~
30h, obtains higher degrees of polymerization polymethoxy dimethyl ether solution, i.e. polymethoxy dimethyl ether finished product, between degree of polymerization N2 ~ 5.
Claims (4)
1. a kind of polymethoxy dimethyl ether synthesizer, including dissolving tank A, dissolving tank B, dissolving tank A upper ends are provided with dimethoxym ethane and enter
Material mouth, α-polyformaldehyde charging aperture one, bottom is provided with outlet；
Dissolving tank A sides are provided with the first polymer reactor, second polymer reactor of top mutually UNICOM, the first polymer reactor
Bottom inlet, by being connected communicating pipe one, is provided with the first high-pressure pump with dissolving tank A outlet at bottoms on communicating pipe one；
Second polymer reactor side is provided with dissolving tank B, the second polymer reactor bottom and dissolving tank B tops reactant liquor import phase
Connection, dissolving tank B tops are additionally provided with α-polyformaldehyde charging aperture two；
Dissolving tank B sides are provided with third polymerization reactor, the 4th polymer reactor that top is connected, third polymerization reactor bottom
Portion, by being connected communicating pipe two, is provided with the second high-pressure pump with dissolving tank B bottoms on communicating pipe two；
4th polymer reactor bottom is provided with polymethoxy dimethyl ether discharge pipe.
2. polymethoxy dimethyl ether synthesizer according to claim 1, it is characterised in that the first described polymerisation
Be filled with catalyst in device, the second polymer reactor, third polymerization reactor, the 4th polymer reactor, catalyst using sun from
Subtree fat.
3. polymethoxy dimethyl ether synthesizer according to claim 1, it is characterised in that the second described polymerisation
It is respectively equipped with the connecting pipe of device bottom and dissolving tank B top reactant liquor import, the 4th polymer reactor bottom discharge pipeline
First safety-valve, the second safety valve.
4. the method that the synthesizer described in a kind of utilization claim 1 synthesizes polymethoxy dimethyl ether, it is characterised in that：Including
Following steps：
1）, prepare raw material：According to weight portion 2:1 ratio prepares dimethoxym ethane, α-polyformaldehyde；
2）, for the first time add α-polyformaldehyde depolymerization：Ready dimethoxym ethane is added in dissolving tank A, α-poly- first is then passed through again
Aldehyde charging aperture one adds α-polyformaldehyde, and at 80 ~ 180 DEG C, time control makes dimethoxym ethane and α-polyformaldehyde to temperature control in 2 ~ 12h
Fully it is dissolved into mixed liquor one；
3）, first set reaction：After the completion of dissolving, mixed liquor is sent to the first polymer reactor and second by the first high pressure pump work
Reacted in polymer reactor, 50 ~ 150 DEG C of temperature, 1 ~ 3MPA of pressure, time control obtains low polymerization degree and gather in 20 ~ 30h
Methoxyl group dimethyl ether solution, between degree of polymerization N1 ~ 3；
4）, the first high pressure pump work, the second high-pressure pump and dissolving tank B do not work, by low polymerization degree polymethoxy dimethyl ether solution
It is sent to dissolving tank B；
5）, again add α-polyformaldehyde depolymerization：Dissolving tank B works, and secondary addition α-polyformaldehyde, addition is identical with first time,
, at 80 ~ 180 DEG C, time control is in 2 ~ 12h for dissolving tank B temperature controls so that low polymerization degree polymethoxy dimethyl ether solution and two
Secondary addition α-polyformaldehyde is fully dissolved into mixed liquor two；
6）, secondary response again：First high-pressure pump and dissolving tank A do not work, the second high pressure pump work, and mixed liquor two is sent to into the 3rd
Reacted in polymer reactor and the 4th polymer reactor, 50 ~ 150 DEG C of temperature, 1 ~ 3MPA of pressure, time control 20 ~
30h, obtains higher degrees of polymerization polymethoxy dimethyl ether solution, i.e. polymethoxy dimethyl ether finished product, between degree of polymerization N2 ~ 5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611007531.9A CN106631722A (en) | 2016-11-16 | 2016-11-16 | DMMn synthesis device and synthesis method adopting DMMn synthesis device |
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|---|---|---|---|
| CN201611007531.9A CN106631722A (en) | 2016-11-16 | 2016-11-16 | DMMn synthesis device and synthesis method adopting DMMn synthesis device |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926627A (en) * | 2014-12-26 | 2015-09-23 | 北京东方红升新能源应用技术研究院有限公司 | Continuous reaction device for synthetizing polymethoxy dimethyl ether |
| CN104974025A (en) * | 2014-04-11 | 2015-10-14 | 清华大学 | Polymethoxyl dimethyl ether production method |
-
2016
- 2016-11-16 CN CN201611007531.9A patent/CN106631722A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974025A (en) * | 2014-04-11 | 2015-10-14 | 清华大学 | Polymethoxyl dimethyl ether production method |
| CN104926627A (en) * | 2014-12-26 | 2015-09-23 | 北京东方红升新能源应用技术研究院有限公司 | Continuous reaction device for synthetizing polymethoxy dimethyl ether |
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