CN107285999A - A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method - Google Patents
A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method Download PDFInfo
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- CN107285999A CN107285999A CN201710572049.8A CN201710572049A CN107285999A CN 107285999 A CN107285999 A CN 107285999A CN 201710572049 A CN201710572049 A CN 201710572049A CN 107285999 A CN107285999 A CN 107285999A
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- parsing
- hemiacetal
- dmmn
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 125000000217 alkyl group Chemical group 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 150000002373 hemiacetals Chemical class 0.000 claims abstract description 24
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000066 reactive distillation Methods 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 19
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000009835 boiling Methods 0.000 claims abstract description 7
- 238000007171 acid catalysis Methods 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 239000011973 solid acid Substances 0.000 claims abstract description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 82
- 238000006116 polymerization reaction Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 5
- 230000009286 beneficial effect Effects 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims description 3
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 238000013517 stratification Methods 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000126 substance Substances 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
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 210000003722 extracellular fluid Anatomy 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000000926 separation method Methods 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
Classifications
-
- 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
-
- 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
- B01J19/24—Stationary reactors without moving elements inside
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method, including tower body, include boiling section again successively from bottom to up in the tower body, parse section, reactive distillation section and tower top section, the tower body parsing section is provided with hemiacetal entrance, dimethoxym ethane entrance is provided with the top of the tower body, the reactive distillation section is provided with multistage rectification section and is mounted with solid acid catalysis resin, and the extraction mouths of DMM3 5 and DMM2 extraction mouths are sequentially provided with from bottom to up in reactive distillation section, the bottom of the parsing section is exported provided with isooctanol, reboiler is also associated with outside the tower for boiling section again of the tower body bottom, the bottom for boiling section again is provided with restructuring sub-export.Present invention reduces synthesis technique step, process energy consumption is reduced.
Description
Technical field
The invention belongs to the examination process and dress of field of energy and chemical technology, more particularly to alkyl polyoxyether PODEn
Put.
Background technology
The characteristics of China's energy resource structure is：Rich coal, oil-poor, few gas, economic maintaining sustained and rapid growth are more next to energy demand
It is bigger, the contradiction of society, expanding economy and oil supply.Since 2009, crude oil in China external dependence degree connects
Exceed warning line (50%) within continuous 6 years, have a strong impact on the energy strategy safety of China.From China's energy strategy safety, with reference to
China's primary energy structure feature, development Coal-based Liquid Fuel synthetic technology undoubtedly has strategic significance.In addition, China's methanol
Production capacity is seriously superfluous, exploitation Downstream Products of Methanol, extension Chemical Industry chain, all with realistic meaning.
Alkyl polyoxyether PODEn is that cleaning just has component, and Cetane number is more than 70, not sulfur-bearing, aromatic-free.By 5%-
20% ratio is added in diesel oil, it is possible to increase diesel cetane-number, promote burning, it will be apparent that reduction vehicle exhaust in PM2.5,
The discharge of the pernicious gases such as PM10, NOx, CO.Current alkyl polyoxyether PODEn production, is generally made using methanol or dimethoxym ethane
For end-capping reagent, polymerisation is obtained under catalyst action with formaldehyde/metaformaldehyde/paraformaldehyde, or directly uses end-capping reagent
Synthesize and obtain with formaldehyde gas.The reaction temperature of the synthesis technique is higher, generally reaches more than 110 DEG C, and must pass through pressurization
Mode prevents the dimethoxym ethane or methanol gasifying that boiling point is told somebody what one's real intentions are, and causes energy consumption to raise, and equipment requirement and input increase.Meanwhile, formaldehyde
The content of the invention
Goal of the invention：It is poly- it is an object of the invention to provide a kind of alkyl for above-mentioned existing problem and shortage
Oxygen ether DMMn reaction tower and manufacturing technique method, and synthesis technique step is shortened, reduce process energy consumption.
Technical scheme：In order to solve the above-mentioned technical problem, the present invention uses following technical scheme：A kind of alkyl polyoxyether
Include boiling section, parsing section, reactive distillation section and tower again successively from bottom to up in DMMn reaction tower, including tower body, the tower body
Section is pushed up, the tower body parsing section, which is provided with the top of hemiacetal entrance, the tower body, is provided with dimethoxym ethane entrance, and the reactive distillation section is set
There is multistage rectification section and be mounted with solid acid catalysis resin, and DMM3-5 extraction mouths are sequentially provided with from bottom to up in reactive distillation section
Mouth is produced with DMM2, the bottom of the parsing section exports provided with isooctanol, is also connected with outside the tower for boiling section again of the tower body bottom
There is reboiler, the bottom that section is boiled again is provided with restructuring sub-export.
Preferably, the parsing section is bubble cap plate section.So as to the first being beneficial to enough free air spaces after parsing
Aldehyde gas rapid increase avoids the auto polymerization of formaldehyde from blocking circulation path.
It is former using hemiacetal and dimethoxym ethane as reaction present invention also offers a kind of alkyl polyoxyether DMMn manufacturing technique methods
Material, by reaction tower parse section hemiacetal entrance by hemiacetal send into reaction tower and parsing section decompose obtain formaldehyde and
Temperature at the top and bottom of isooctanol, the parsing section is controlled in 150 ± 5 DEG C and 180 ± 5 DEG C respectively, parses obtained formaldehyde
Gas ramp up into reactive distillation section, parsing obtain isooctanol liquid decline and analytically tower bottom isooctanol outlet adopt
Go out；The dimethoxym ethane is sent into from tower top dimethoxym ethane entrance simultaneously, and the temperature of the top and bottom of control reactive distillation section is 80 ± 5
DEG C and 150 ± 5 DEG C, the dimethoxym ethane from upper spray it is lower with the formaldehyde gas that rises solid acid catalysis resin surface progress
Polymerisation obtains the alkyl polyoxyether DMMn of the alkyl polyoxyether DMMn products, at the same time different polymerization degree of different polymerization degree
Product carries out rectifying in reactive distillation section, and produces mouth and DMM2 extraction mouth extraction DMM3-5 products and DMM2 from DMM3-5 respectively
Product, the temperature range of DMM3-5 extraction mouths and DMM2 the extraction mouth is respectively 110~120 DEG C and 90~95 DEG C；It is incomplete
Again boil section of the material liquid comprising dimethoxym ethane and hemiacetal of reaction in tower body bottom enters upper strata by reboiler cycle gasification
Reactive distillation section continue polymerisation and rectifying, the heavy constituent of the degree of polymerization more than 5 is produced from the restructuring sub-export of bottom.
Further, the hemiacetal passes through reaction by formaldehyde raw material gas and isooctanol in 80~100 DEG C, and by quiet
Put the hemiacetal organic phase that layering extracting upper strata is obtained.
Further, the gas component that is additionally provided with of the tower top is exported, and sends reaction tower top back to by condensing reflux.
Beneficial effect：Compared with prior art, the present invention is directly gathered using hemiacetal and dimethoxym ethane in reaction tower
Rectification process is closed, formaldehyde concentration step is reduced and increases the water content reduced in reaction system so as to improve turning for formaldehyde
Rate and product yield.Simultaneously by one side polymerisation while progress rectifying separation, reduces the separating-purifying of subsequent product
Difficulty.
Brief description of the drawings
Fig. 1 is the structural representation of alkyl polyoxyether DMMn of the present invention reaction tower.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
The present invention rather than limitation the scope of the present invention, after the present invention has been read, those skilled in the art are each to the present invention's
The modification for planting the equivalent form of value falls within the application appended claims limited range.
As shown in figure 1, the present invention is using hemiacetal and dimethoxym ethane as reaction raw materials.First, methanol evaporator, blender are passed through
Four vigour obtained with filter obtain formaldehyde raw material gas in oxidator by catalysis oxidation, then enter formaldehyde raw material pneumatic transmission
Absorb synthesis tower bottom entrance, from tower top spray and under isooctanol inhaled in column plate section and packing section with formaldehyde raw material gas
Receive and react generation hemiacetal material, when formaldehyde raw material gas rises to the packing section of higher level, suction is made by multistage pump circulation outside tower
Receive after liquid circulation is uniformly distributed from the spray equipment circulated sprinkling above filler through distributor and repeatedly do not absorbed anti-with rising
The formaldehyde raw material gas contact absorbing reaction answered, improves formaldehyde raw material gas and is completely absorbed, and enter in 80~100 DEG C with isooctanol
The hemiacetal material that row absorbing reaction is obtained.Because hemiacetal is that oil phase is insoluble in water, and not absorbed formaldehyde and water completely
Dilute formalin is formed, both are absorbing the extracting section stratification of synthesis tower bottom, and phase interstitial fluid is controlled by liquid-level controller
Face within a certain height, and by extracting upper strata hemiacetal organic phase.Quick and easy it can be obtained by this method by first
Moisture removal in aldehyde base feed, eliminates formalin concentration step and greatly reduces process energy consumption.
The hemiacetal entrance that obtained hemiacetal parses section by reaction tower is sent into reaction tower and decomposed in parsing section
Obtain the temperature at the top and bottom of formaldehyde and isooctanol, the parsing section to control respectively in 150 ± 5 DEG C and 180 ± 5 DEG C, parse
Obtained formaldehyde gas is ramped up into reactive distillation section, parsing obtain isooctanol liquid decline and analytically tower bottom it is different pungent
Alcohol outlet is produced；The dimethoxym ethane is sent into from tower top dimethoxym ethane entrance simultaneously, the temperature of the top and bottom of control reactive distillation section
Degree is in 80 ± 5 DEG C and 150 ± 5 DEG C, and the formaldehyde gas with rising is in solid acid catalysis resin down from upper spray for the dimethoxym ethane
Surface carry out polymerisation and obtain the alkyl polyoxyether DMMn products of different polymerization degree, the at the same time alkyl of different polymerization degree
Polyoxyether DMMn products carry out rectifying in reactive distillation section, and produce mouth and DMM2 extraction mouth extraction DMM3-5 from DMM3-5 respectively
Product and DMM2 products, the temperature range of DMM3-5 extraction mouths and DMM2 the extraction mouth is respectively 110~120 DEG C and 90~95
℃；Again boil section of the material liquid comprising dimethoxym ethane and hemiacetal not reacted completely in tower body bottom passes through reboiler cycle gasification
Reactive distillation section into upper strata continues polymerisation and rectifying, the restructuring sub-export of the heavy constituent of the degree of polymerization more than 5 from bottom
Extraction.
Claims (5)
1. a kind of alkyl polyoxyether DMMn reaction tower, it is characterised in that：Including tower body, wrapped successively from bottom to up in the tower body
Include and boil section, parsing section, reactive distillation section and tower top section again, the tower body parsing section is provided with the top of hemiacetal entrance, the tower body
Provided with dimethoxym ethane entrance, the reactive distillation section is provided with multistage rectification section and is mounted with solid acid catalysis resin, and in reaction essence
Evaporate section and be sequentially provided with DMM3-5 extraction mouths and DMM2 extraction mouths from bottom to up, the bottom of the parsing section is exported provided with isooctanol,
Reboiler is also associated with outside the tower for boiling section again of the tower body bottom, the bottom that section is boiled again is provided with restructuring sub-export.
2. alkyl polyoxyether DMMn reaction tower according to claim 1, it is characterised in that：The parsing section is bubble cap plate
Section.So as to which the formaldehyde gas rapid increase being beneficial to enough free air spaces after parsing avoids the auto polymerization of formaldehyde from blocking circulation
Path.
3. a kind of alkyl polyoxyether DMMn manufacturing technique methods based on reaction tower described in claim 1, are contracted with hemiacetal and first
Aldehyde is reaction raw materials, and hemiacetal is sent into reaction tower and decomposed in parsing section by the hemiacetal entrance for parsing section by reaction tower
Obtain the temperature at the top and bottom of formaldehyde and isooctanol, the parsing section to control respectively in 150 ± 5 DEG C and 180 ± 5 DEG C, parse
Obtained formaldehyde gas is ramped up into reactive distillation section, parsing obtain isooctanol liquid decline and analytically tower bottom it is different pungent
Alcohol outlet is produced；The dimethoxym ethane is sent into from tower top dimethoxym ethane entrance simultaneously, the temperature of the top and bottom of control reactive distillation section
Degree is in 80 ± 5 DEG C and 150 ± 5 DEG C, and the formaldehyde gas with rising is in solid acid catalysis resin down from upper spray for the dimethoxym ethane
Surface carry out polymerisation and obtain the alkyl polyoxyether DMMn products of different polymerization degree, the at the same time alkyl of different polymerization degree
Polyoxyether DMMn products carry out rectifying in reactive distillation section, and produce mouth and DMM2 extraction mouth extraction DMM3-5 from DMM3-5 respectively
Product and DMM2 products, the temperature range of DMM3-5 extraction mouths and DMM2 the extraction mouth is respectively 110~120 DEG C and 90~95
℃；Again boil section of the material liquid comprising dimethoxym ethane and hemiacetal not reacted completely in tower body bottom passes through reboiler cycle gasification
Reactive distillation section into upper strata continues polymerisation and rectifying, the restructuring sub-export of the heavy constituent of the degree of polymerization more than 5 from bottom
Extraction.
4. alkyl polyoxyether DMMn manufacturing technique methods according to claim 3, it is characterised in that：The hemiacetal is by formaldehyde
Unstripped gas extracts the hemiacetal organic phase that upper strata is obtained in 80~100 DEG C with isooctanol by reaction, and by stratification.
5. alkyl polyoxyether DMMn manufacturing technique methods according to claim 3, it is characterised in that：The tower top is additionally provided with
Gas component is exported, and sends reaction tower top back to by condensing reflux.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710572049.8A CN107285999A (en) | 2017-07-13 | 2017-07-13 | A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710572049.8A CN107285999A (en) | 2017-07-13 | 2017-07-13 | A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107285999A true CN107285999A (en) | 2017-10-24 |
Family
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Family Applications (1)
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| CN201710572049.8A Pending CN107285999A (en) | 2017-07-13 | 2017-07-13 | A kind of alkyl polyoxyether DMMn reaction tower and manufacturing technique method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109173310A (en) * | 2018-08-29 | 2019-01-11 | 张家港市科华化工装备制造有限公司 | Dimethoxym ethane rectifying column |
| CN109277056A (en) * | 2018-11-15 | 2019-01-29 | 凯瑞环保科技股份有限公司 | Azeotropic catalytic tower |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109277056B (en) * | 2018-11-15 | 2024-04-16 | 凯瑞环保科技股份有限公司 | Azeotropic catalytic reaction tower |
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Effective date of registration: 20200622 Address after: No.117, YINGSHANHONG Road, gugugukou, Huangdao District, Qingdao, Shandong Province Applicant after: Qingdao Zhuohui Chuang Neng New Energy Technology Co.,Ltd. Address before: East Lake new technology development zone of Hubei Province, Wuhan city Hongshan District 430070 Luoyu Road shops along the Street No. 490-518 Optics Valley world city B block 1 Building 2 unit 8 room 20 Applicant before: HUBEI SANLIFENGXIANG TECHNOLOGY Co.,Ltd. |
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Application publication date: 20171024 |
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