CN110496576A - A kind of synthesis of polymethoxy dimethyl ether and separation system - Google Patents
A kind of synthesis of polymethoxy dimethyl ether and separation system Download PDFInfo
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- CN110496576A CN110496576A CN201910873341.2A CN201910873341A CN110496576A CN 110496576 A CN110496576 A CN 110496576A CN 201910873341 A CN201910873341 A CN 201910873341A CN 110496576 A CN110496576 A CN 110496576A
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- reactor
- pipe
- dimethoxym ethane
- dimethyl ether
- formaldehyde
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- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 23
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 23
- 238000000926 separation method Methods 0.000 title claims abstract description 19
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 125
- 238000006243 chemical reaction Methods 0.000 claims abstract description 75
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 claims abstract description 48
- 230000003197 catalytic effect Effects 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 28
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 19
- 150000001241 acetals Chemical class 0.000 claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 238000004821 distillation Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 6
- 238000000066 reactive distillation Methods 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 3
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 239000000047 product Substances 0.000 description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 10
- 239000003245 coal Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000002283 diesel fuel Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229930040373 Paraformaldehyde Natural products 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000003502 gasoline Substances 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920002866 paraformaldehyde Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical compound C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006280 diesel fuel additive Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/04—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
-
- 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
-
- 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
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses polymethoxy dimethyl ether synthesis to synthesize with a kind of polymethoxy dimethyl ether of separation technology field and separation system, including pre-reactor, the feed inlet of pre-reactor is connected separately with formaldehyde pipe and dimethoxym ethane pipe, the discharge port of pre-reactor is connected with crude reaction liquid pipe, one end of crude reaction liquid pipe is connected with catalytic rectifying tower, catalytic rectifying tower includes the conversion zone and stripping section of upper-lower section, the top material mouth of conversion zone is connected with unreacted dimethoxym ethane mother tube, the outer wall material mouth of conversion zone is connected with unreacting acetal mother tube, the outer wall of stripping section is provided with catalytic distillation tower reboiler by pipeline, the bottom end material mouth of stripping section is connected with production tube, finished product extraction pump is provided on the pipeline of production tube, intermediate reaction liquid extraction pump is provided on the pipeline of unreacting acetal mother tube, one end of unreacting acetal mother tube is connected with plug-in Reactor, the material mouth of plug-in reactor are connected with dimethoxym ethane proportion pipe.
Description
Technical field
The invention discloses a kind of synthesis of polymethoxy dimethyl ether and separation system, specially polymethoxy dimethyl ether is synthesized
With separation technology field.
Background technique
Global energy comes into the serious productive life.High-grade energy is fewer and fewer, and energy prices are growing.Special crude oil
After crisis, various countries have started the underproduction step by step and have improved crude oil price.The following oil price will gradually rise.And China's energy resource structure
Feature is: rich coal, oil-poor, few gas, economic maintaining sustained and rapid growth is increasing to energy demand, society, expanding economy with
The contradiction of oil supply becomes increasingly conspicuous.Development of coal, which is liquefied as oil tech, undoubtedly has strategic significance.In addition, China's methanol produces
Can be serious superfluous, exploitation Downstream Products of Methanol extends Chemical Industry chain, all has realistic meaning.Northwest producing coal industry is through state
The multiple industrial restructuring of family, after the original rough industrial chain of coal further upgrades.The further deep processing of coal be methanol and under
The tendency of trip has become the trend of the following emerging coal industry.
With the progress of social economy, automobile quantity be increased significantly, and motor vehicle exhaust emission object has become city haze
One of the major reasons.Compared to gasoline, diesel oil has higher boiling point, and H/C mass ratio is low, therefore discharges in diesel combustion process
Exhaust gas CO, oxynitrides, particulate matter etc. it is more, caused by damage ratio gasoline it is more serious.Therefore, diesel combustion effect is improved
Rate reduces disposal of pollutants, and improving urban air-quality is environmentally friendly task important at present.
Polymethoxy dimethyl ether is a kind of universally acknowledged cleaning diesel oil component, its Cetane number >=70, not sulfur-bearing, no
Containing aromatic hydrocarbons.It is added in diesel oil in 5%~20% ratio, can be improved diesel cetane-number, promote burning, it will be apparent that reduces vapour
The discharge of the pernicious gases such as PM2.5, PM10, NOx, CO in tail gas.Due to the excellent properties of polymethoxy dimethyl ether, synthesis
Technique has become the heat subject studied both at home and abroad.
Currently, polymethoxy dimethyl ether is that (formaldehyde may be from formalin/tri- with formaldehyde with dimethoxym ethane/methanol mostly
Polyformaldehyde/paraformaldehyde) generation is reacted under the catalytic action of acidic catalyst.And this reaction is exothermic reaction, temperature height is made
It is carried out at reaction is reverse, it is therefore desirable to withdraw heat.Regardless of being that paraformaldehyde or metaformaldehyde need heating to parse first
Monomer formaldehyde could participate in reacting out, therefore system reaction temperature is very high, generally at 110 DEG C or more, therefore lead to energy consumption height, set
It is standby to require height.In addition, monomer formaldehyde has very high activity under the conditions of pyroreaction, it is a large amount of to be easy to happen disproportionated reaction production
Formic acid, if formic acid in system not separated, formic acid can it is cumulative and to the reaction of polymethoxy dimethyl ether balance
Significant negative impact is brought, causes the yield of reaction to reduce, separation is difficult.Technique can only be de- using absorption or alkali neutralization at present
Sour method separating formic, causes complex process, and target product yield is low, and synthesis cost is high.The choosing of reaction product DMMn3~8
Selecting property and the amount of catalyst have close relationship, and common fixed bed cannot achieve the adjustment product degree of polymerization, therefore cause n value mistake
It is small or excessive, influence product quality.Test proves that the degree of polymerization for being most suitable for doing diesel fuel additives is the product of DMMn3~5.
Summary of the invention
The purpose of the present invention is to provide a kind of synthesis of polymethoxy dimethyl ether and separation systems, to solve above-mentioned background skill
The problem of investment of production proposed in art is at high cost, Synthesis conversion and yield are low etc..
To achieve the above object, the invention provides the following technical scheme: a kind of synthesis of polymethoxy dimethyl ether and segregative line
System, including pre-reactor, the feed inlet of the pre-reactor are connected separately with formaldehyde pipe and dimethoxym ethane pipe, the pre-reactor
Discharge port is connected with crude reaction liquid pipe, and one end of the crude reaction liquid pipe is connected with catalytic rectifying tower, the catalytic rectifying tower packet
The conversion zone and stripping section of upper-lower section are included, the top material mouth of the conversion zone is connected with unreacted dimethoxym ethane mother tube, described anti-
The outer wall material mouth of section is answered to be connected with unreacting acetal mother tube, the outer wall of the stripping section is provided with catalytic rectifying tower by pipeline
Reboiler, the bottom end material mouth of the stripping section are connected with production tube, and finished product extraction pump, institute are provided on the pipeline of the production tube
It states and is provided with intermediate reaction liquid extraction pump on the pipeline of unreacting acetal mother tube, one end of the unreacting acetal mother tube connects
It is connected to plug-in reactor, the material mouth of the plug-in reactor is connected with dimethoxym ethane proportion pipe, and the material mouth of the plug-in reactor is logical
The material mouth for crossing pipeline and conversion zone connects, and the material mouth of the plug-in reactor is connected with recycle feed pipe, the recycle feed pipe
One end and conversion zone material mouth connect.
Preferably, the pipeline height of the plug-in reactor and conversion zone is located at unreacted dimethoxym ethane mother tube and unreacted
Between formaldehyde raw material pipe.
Preferably, the outer wall of the unreacted dimethoxym ethane mother tube and unreacting acetal mother tube is enclosed with insulating layer.
Preferably, one end of the production tube is connected with the material mouth of rectification cell or storage element.
A kind of synthesis of polymethoxy dimethyl ether and separation method, the method steps are as follows:
Step 1: the dimethoxym ethane point for being 88~94% with mass concentration by the formalin that mass concentration is 55-85%
Not Tong Guo formaldehyde pipe and dimethoxym ethane tube pump to pre-reactor, reaction obtains crude reaction liquid；
Step 2: upper semisection is conversion zone in catalytic rectifying tower, and lower semisection is stripping section, and conversion zone is catalytic filler section,
Crude reaction liquid can be made the reaction was continued by including catalyst, and the light component raw material dimethoxym ethane for being pumped into catalytic rectifying tower is evaporated to tower top, be closed
At polymethoxy dimethyl ether product and reaction raw materials formaldehyde be heavy constituent, during the two drops down onto tower reactor, formaldehyde reaches critical
Temperature is vaporized again to tower interlude, and forming tower interlude is high-concentration formaldehyde region；
Step 3: unreacting acetal mother tube is pumped by the extraction of intermediate reaction liquid by content of formaldehyde high among catalytic rectifying tower
Material pumps out, and adds raw material by the dimethoxym ethane that unreacted dimethoxym ethane mother tube is drawn, pump after dimethoxym ethane allotment ratio to
Plug-in reactor further converts the formaldehyde for having neither part nor lot in reaction.
Preferably, the quantity of the plug-in reactor is provided with 1-5 group.
Preferably, the pre-reactor is fixed bed reactors, and reaction temperature is 50~150 DEG C, reaction pressure 0.1
~2.0Mpa.
Preferably, the plug-in reactor is fixed bed reactors, and reaction temperature is 50~150 DEG C, and reaction pressure is
0.1~2.0Mpa.
Preferably, reactive distillation section is that filler package catalyst mode is installed in the catalytic rectifying tower, and stripping section is
Bubble-cap type rectifying plate.
Compared with prior art, the beneficial effects of the present invention are: dmmn is synthesized exothermic reaction and dimethoxym ethane water by this system
Heat of desorption reaction bonded one, efficiently utilizes energy.Reaction temperature is low, effectively reduces formaldehyde high temperature and is easily disproportionated generation formic acid
Amount, reduce formic acid separating difficulty and equipment requirement.This system will separate and the combination of reactive distillation makes process succinctly tight
It gathers, investment is low, and energy consumption is reduced to the greatest extent.
Detailed description of the invention
Fig. 1 is structure of the invention block diagram.
In figure: 100 pre-reactors, 110 formaldehyde pipes, 120 dimethoxym ethane pipes, 130 crude reaction liquid pipes, 200 catalytic rectifying towers,
210 conversion zones, 211 unreacted dimethoxym ethane mother tubes, 212 unreacting acetal mother tubes, 220 stripping sections, 221 catalytic rectifying towers are again
Boil device, 222 production tubes, 230 finished products extraction pump, 300 intermediate reaction liquid extraction pump, 310 plug-in reactors, 320 dimethoxym ethanes proportion
Pipe, 330 recycle feed pipes.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, the present invention provides a kind of technical solution: a kind of synthesis of polymethoxy dimethyl ether and separation system, packet
Pre-reactor 100 is included, the feed inlet of pre-reactor 100 is connected separately with formaldehyde pipe 110 and dimethoxym ethane pipe 120, pre-reactor 100
Discharge port be connected with crude reaction liquid pipe 130, one end of crude reaction liquid pipe 130 is connected with catalytic rectifying tower 200, catalytic rectifying tower
200 include the conversion zone 210 and stripping section 220 of upper-lower section, and the top material mouth of conversion zone 210 is connected with unreacted dimethoxym ethane raw material
Pipe 211, the outer wall material mouth of conversion zone 210 are connected with unreacting acetal mother tube 212, and the outer wall of stripping section 220 is set by pipeline
It is equipped with catalytic distillation tower reboiler 221, the bottom end material mouth of stripping section 220 is connected with production tube 222, on the pipeline of production tube 222
It is provided with finished product extraction pump 230, intermediate reaction liquid extraction pump 300 is provided on the pipeline of unreacting acetal mother tube 212, not instead
One end of formaldehyde raw material pipe 212 is answered to be connected with plug-in reactor 310, the material mouth of plug-in reactor 310 is connected with dimethoxym ethane proportion
Pipe 320, the material mouth of plug-in reactor 310 are connected with recycle feed pipe 330, one end of the recycle feed pipe 330 and conversion zone
210 material mouth connection.
Step 1: the dimethoxym ethane point for being 88~94% with mass concentration by the formalin that mass concentration is 55-85%
Not Tong Guo formaldehyde pipe 110 and the pump of dimethoxym ethane pipe 120 to pre-reactor 100, reaction obtains crude reaction liquid；
Step 2: upper semisection is conversion zone 210 in catalytic rectifying tower 200, and lower semisection is stripping section 220, and conversion zone 210 is
Catalytic filler section, crude reaction liquid can be made the reaction was continued by including catalyst, be pumped into the light component raw material dimethoxym ethane of catalytic rectifying tower 200
It is evaporated to tower top, the polymethoxy dimethyl ether product and reaction raw materials formaldehyde of synthesis are heavy constituent, during the two drops down onto tower reactor,
Formaldehyde reaches critical-temperature and is vaporized again to tower interlude, and forming tower interlude is high-concentration formaldehyde region；
Step 3: unreacting acetal mother tube 212 pumps 300 for first high among catalytic rectifying tower by the extraction of intermediate reaction liquid
Aldehyde material pumps out, and adds raw material by the dimethoxym ethane that unreacted dimethoxym ethane mother tube 211 is drawn, and carries out dimethoxym ethane and deploys ratio
Pump further converts the formaldehyde for having neither part nor lot in reaction to plug-in reactor 310 after example.
Preferably, the quantity of the plug-in reactor 310 is provided with 1-5 group.
Preferably, the pre-reactor 100 is fixed bed reactors, and reaction temperature is 50~150 DEG C, and reaction pressure is
0.1~2.0Mpa.
Preferably, the plug-in reactor 310 is fixed bed reactors, and reaction temperature is 50~150 DEG C, reaction pressure
For 0.1~2.0Mpa.
Preferably, reactive distillation section is that filler package catalyst mode is installed in the catalytic rectifying tower 200, stripping section
For bubble-cap type rectifying plate.
Embodiment
The dimethoxym ethane logistics that the high-concentration formaldehyde that mass concentration is 81% is 92% with mass concentration is passed through into formaldehyde respectively
Pipe 110 and the pump of dimethoxym ethane pipe 120 are to pre-reactor 100, and reaction obtains crude reaction liquid in pre-reactor 100, and by thick anti-
It answers liquid pipe 130 to be discharged, be preheated to 80 DEG C of high-concentration formaldehyde and heat the dimethoxym ethane after pressurization, temperature 60 C, pressure 0.2Mpa,
The mass ratio of formaldehyde and dimethoxym ethane is 1:1 in reactant；
| Pipeline ingredient | Formaldehyde % | Water % | Methanol % | Dimethoxym ethane % | Dmm2-8% |
| Formaldehyde pipe | 81% | 18.0 | 1.0 | - | - |
| Dimethoxym ethane pipe | 92 | 0.5 | 7.5 | - | - |
| Crude reaction liquid pipe | 20.25 | 4.88 | 5.88 | 69.0 | - |
Material after the reaction of pre-reactor 100, it can be seen that water conversion ratio to 20% or so, dimethoxym ethane conversion ratio
30.7%, formaldehyde conversion 17.1%.Water is largely converted, and water content is further reduced in system, so that reaction is flat
Weighing apparatus obtains great promotion.
Crude reaction liquid pump contacts further anti-to the top of catalytic rectifying tower conversion zone 210 with the catalyst filling in tower
It answers.Its boiling point of the product of generation is relatively high, drops down onto tower reactor.Unreacted raw material dimethoxym ethane is from unreacted dimethoxym ethane mother tube
211 extraction are reused to refined unit；
The lower semisection of catalytic rectifying tower 200 is stripping section 220, and the disengagings such as impurity formaldehyde, water, methanol in product are clean
Afterwards.Tower reactor obtains the higher dmmn of purity (n=2-8) product.Dmmn product is sent by 230 extraction of finished product extraction pump by production tube
It is stored to tank field.Tower top temperature is 55 DEG C, and bottom temperature is 110 DEG C, pressure 0.1Mpa；
After tower top and tower reactor sampling analysis, after contrasting calculating with feed composition, obtaining the final conversion ratio of formaldehyde is
98.2%, it almost realizes and is totally converted.Methylal synthesis unit is entered by the formaldehyde that tower top overflows and further reacts generation first
Acetal is recycled；
200 upper semisection middle of catalytic rectifying tower is concentrated on by the unreacted formaldehyde that tower reactor is evaporated.By intermediate reaction liquid
300 extraction of extraction pump, and match in pipe 300 with dimethoxym ethane and give after dimethoxym ethane mixing match to plug-in reactor 310.Through secondary counter
The reaction liquid pipeline answered is sent catalytic rectifying tower 200 back to again and is separated；
Targetedly contrived experiment is carried out according to reaction equilibrium condition, keeps reaction ratio suitable, reaction temperature is optimal
Equilbrium position, reaction conversion ratio reach maximum, and reaction rate is most fast, obtain optimal intermediate extraction position.Ensure simultaneously highly concentrated
Spending formaldehyde, there is no polymerisms.
In pre-reactor 100, reaction temperature is higher, and higher temperature greatly accelerates the conversion rate of reaction.But for
Exothermic reaction, high temperature inhibit balance positive mobile.
Although hereinbefore having been made with reference to some embodiments, present invention is described, of the invention not departing from
In the case where range, various improvement can be carried out to it and can be with equivalent without replacement component therein.Especially, as long as not
There are structural conflict, the various features in presently disclosed each embodiment can be combined with each other by any way
It uses, the description for not carrying out exhaustion to the case where these combinations in the present specification is only to be in omit length and economize on resources
The considerations of.Therefore, the invention is not limited to specific embodiments disclosed herein, and including falling within the scope of the appended claims
All technical solutions.
Claims (9)
1. a kind of polymethoxy dimethyl ether synthesis and separation system, it is characterised in that: described pre- anti-including pre-reactor (100)
The feed inlet of device (100) is answered to be connected separately with formaldehyde pipe (110) and dimethoxym ethane pipe (120), the discharging of the pre-reactor (100)
Mouth is connected with crude reaction liquid pipe (130), and one end of the crude reaction liquid pipe (130) is connected with catalytic rectifying tower (200), described to urge
Change the conversion zone (210) and stripping section (220) that rectifying column (200) include upper-lower section, the top material mouth of the conversion zone (210) connects
It is connected to unreacted dimethoxym ethane mother tube (211), the outer wall material mouth of the conversion zone (210) is connected with unreacting acetal mother tube
(212), the outer wall of the stripping section (220) is provided with catalytic distillation tower reboiler (221), the stripping section by pipeline
(220) bottom end material mouth is connected with production tube (222), and finished product extraction pump is provided on the pipeline of the production tube (222)
(230), intermediate reaction liquid extraction pump (300), the unreacted are provided on the pipeline of the unreacting acetal mother tube (212)
One end of formaldehyde raw material pipe (212) is connected with plug-in reactor (310), and the material mouth of the plug-in reactor (310) is connected with first
Acetal proportion pipe (320), the material mouth of the plug-in reactor (310) are connected with recycle feed pipe (330), the recycle feed pipe
(330) one end is connect with the material mouth of conversion zone (210).
2. a kind of polymethoxy dimethyl ether synthesis according to claim 1 and separation system, it is characterised in that: described plug-in
The pipeline height of reactor (310) and conversion zone (210) is located at unreacted dimethoxym ethane mother tube (211) and unreacting acetal raw material
It manages between (212).
3. a kind of polymethoxy dimethyl ether synthesis according to claim 1 and separation system, it is characterised in that: described not anti-
Dimethoxym ethane mother tube (211) and the outer wall of unreacting acetal mother tube (212) is answered to be enclosed with insulating layer.
4. a kind of polymethoxy dimethyl ether synthesis according to claim 1 and separation system, it is characterised in that: the finished product
One end of pipe (222) is connected with the material mouth of rectification cell or storage element.
5. a kind of a kind of polymethoxy dimethyl ether synthesis such as of any of claims 1-4 and separation method, feature
Be: the method steps are as follows:
Step 1: the dimethoxym ethane that the formalin that mass concentration is 55-85% is 88~94% with mass concentration is led to respectively
Formaldehyde pipe (110) and dimethoxym ethane pipe (120) pump are crossed to pre-reactor (100), reaction obtains crude reaction liquid；
Step 2: catalytic rectifying tower (200) interior upper semisection is conversion zone (210), and lower semisection is stripping section (220), conversion zone
It (210) is catalytic filler section, crude reaction liquid can be made the reaction was continued by including catalyst, be pumped into the light component of catalytic rectifying tower (200)
Raw material dimethoxym ethane is evaporated to tower top, and the polymethoxy dimethyl ether product and reaction raw materials formaldehyde of synthesis are heavy constituent, and the two drops down onto
During tower reactor, formaldehyde reaches critical-temperature and is vaporized again to tower interlude, and forming tower interlude is high-concentration formaldehyde region；
Step 3: unreacting acetal mother tube (212) pumps (300) for first high among catalytic rectifying tower by the extraction of intermediate reaction liquid
Aldehyde material pumps out, and adds raw material by the dimethoxym ethane that unreacted dimethoxym ethane mother tube (211) is drawn, carries out dimethoxym ethane allotment
It pumps after ratio to plug-in reactor (310) and further converts the formaldehyde for having neither part nor lot in reaction.
6. a kind of polymethoxy dimethyl ether synthesis according to claim 5 and separation method, it is characterised in that: described plug-in
The quantity of reactor (310) is provided with 1-5 group.
7. a kind of polymethoxy dimethyl ether synthesis according to claim 5 and separation method, it is characterised in that: described is pre-
Reactor (100) is fixed bed reactors, and reaction temperature is 50~150 DEG C, and reaction pressure is 0.1~2.0Mpa.
8. a kind of polymethoxy dimethyl ether synthesis according to claim 5 and separation method, it is characterised in that: described is outer
Hanging reactor (310) is fixed bed reactors, and reaction temperature is 50~150 DEG C, and reaction pressure is 0.1~2.0Mpa.
9. a kind of polymethoxy dimethyl ether synthesis according to claim 5 and separation method, it is characterised in that: described urges
Changing reactive distillation section in rectifying column (200) is that filler package catalyst mode is installed, and stripping section is bubble-cap type rectifying plate.
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