CN109776287A - A kind of preparation method of acetone dimethyl acetal - Google Patents
A kind of preparation method of acetone dimethyl acetal Download PDFInfo
- Publication number
- CN109776287A CN109776287A CN201711169986.5A CN201711169986A CN109776287A CN 109776287 A CN109776287 A CN 109776287A CN 201711169986 A CN201711169986 A CN 201711169986A CN 109776287 A CN109776287 A CN 109776287A
- Authority
- CN
- China
- Prior art keywords
- acetone
- methanol
- tower
- method described
- section
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HEWZVZIVELJPQZ-UHFFFAOYSA-N 2,2-dimethoxypropane Chemical compound COC(C)(C)OC HEWZVZIVELJPQZ-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 123
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 83
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 230000002378 acidificating effect Effects 0.000 claims abstract description 15
- 239000002808 molecular sieve Substances 0.000 claims abstract description 13
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 238000005192 partition Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 43
- 239000000463 material Substances 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 18
- 238000004821 distillation Methods 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 230000029936 alkylation Effects 0.000 claims description 8
- 238000005804 alkylation reaction Methods 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 8
- 239000011973 solid acid Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000000994 depressogenic effect Effects 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 2
- 229920001429 chelating resin Polymers 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 6
- 239000003456 ion exchange resin Substances 0.000 description 6
- 229920003303 ion-exchange polymer Polymers 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000004702 methyl esters Chemical class 0.000 description 3
- SPEUIVXLLWOEMJ-UHFFFAOYSA-N 1,1-dimethoxyethane Chemical compound COC(C)OC SPEUIVXLLWOEMJ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910000474 mercury oxide Inorganic materials 0.000 description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- MWWATHDPGQKSAR-UHFFFAOYSA-N propyne Chemical compound CC#C MWWATHDPGQKSAR-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- NKLCNNUWBJBICK-UHFFFAOYSA-N Dess-Martin periodinane Substances C1=CC=C2I(OC(=O)C)(OC(C)=O)(OC(C)=O)OC(=O)C2=C1 NKLCNNUWBJBICK-UHFFFAOYSA-N 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- -1 dewaterer Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012971 dimethylpiperazine Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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 present invention relates to a kind of preparation methods of acetone dimethyl acetal, using methanol and acetone as reaction raw materials, and methanol is divided into two parts addition, and reaction raw materials are reacted in the presence of acidic resins and molecular sieve catalyst, and reaction product is separated using partition wall type rectifying column.Compared with prior art, it is of the invention have the advantages that catalyst activity is high, reaction yield is high, separation efficiently and low energy consumption.
Description
Technical field
The present invention relates to field of organic compound preparation more particularly to a kind of preparation method of acetone dimethyl acetal.
Background technique
Acetone dimethyl acetal is also known as 2,2-dimethoxypropane, is abbreviated as DMP, is a kind of important organic intermediate.
DMP can be used as hydroxy-protecting agent, condensing agent, cyclizing agent, dewaterer, Insecticides (tech) & Herbicides (tech) etc., in medicine, pesticide, natural products
Have in the development and industrialized production of equal fine chemical products and has been widely used.
The synthetic method of DMP has propine and methanol synthesis, methanol and acetone method, ortho acid methyl esters and acetone method etc. at present,
Wherein propine and methanol synthesis usually require that a certain amount of mercury oxide is added, reaction yield is lower, and using being more toxic
Mercury oxide；Ortho acid methyl esters and the raw material ortho acid methyl esters price in acetone method are higher, it is difficult to carry out industrialized production.Methanol and acetone
Its process flow of method is simple, and raw material is cheap and easy to get, is conducive to industrialized production.
However, there is catalyst activities that low, product separates that difficult, rectification efficiency is low, yield is low, energy for methanol and acetone method
Consume higher disadvantage.For there are drawbacks described above, need to develop that a kind of catalyst activity is high and reaction yield is high and energy consumption at present
Low DMP preparation method.
Summary of the invention
It is an object of the invention to overcome the shortcomings of methanol in the prior art and acetone method, it is high to provide a kind of catalyst activity
And reaction yield height and the DMP each method that low energy consumption.
What the invention is realized by the following technical scheme: a kind of preparation method of acetone dimethyl acetal, including following process:
1) methanol (A), acetone (B) from tank field storage tank are in molar ratio 3.2-4.0: 1 pumped in dosage bunker；
2) methanol, acetone mixture are pumped up in built-in steam pipe coil and distillation still with destilling tower in dosage bunker；
Kettle is warming up to 65-70 DEG C, and tower top begins with reflux；Pressure≤0.020Mpa, bottom temperature≤85 DEG C in control tower, tower top control
Certain reflux ratio；Material a part is back in distillation still in reflux condenser, and remainder is cooled to through first-stage condenser
Material-heat-exchanging that 45-50 DEG C, first-class heat exchanger and rear step alkalization device come out and the freezing for being cooled to 30-35 DEG C, secondary condenser
Brine-cooled enters alkylation reactor to -15 DEG C to -20 DEG C after cooling；The another part in methanol measuring tank
Methanol (C) and the outlet material from first-stage condenser enter from the same entrance of first-class heat exchanger together；
3) alkylation reactor is fixed bed reactors, wherein built-in solid acid catalyst, reaction temperature -15 DEG C to -
20 DEG C, pressure≤0.015Mpa, the solid acid catalyst are the combination of acidic resins and acidic molecular sieve, acidic resins and acid
Mass ratio 3-5: 1 of property molecular sieve；
4) enter alkalization device from the material that reactor comes out, built-in basic resin in the device that alkalizes, temperature is -15 in the device that alkalizes
DEG C to -20 DEG C, pressure≤0.015Mpa；From alkalization device come out material first through process 2) in first-class heat exchanger heat exchange, heating
To 28-32 DEG C, exchange heat using secondary heat exchanger to after 65-70 DEG C, return to process 2) in distillation still circulation, until acetone in kettle
When dimethyl acetal content reaches 60-65%, reaction terminates, and material is depressed into crude product slot with pressure itself in kettle；
5) material in crude product slot is sent into from the middle part of partition wall type rectifying column, tower reactor is warming up to 70-78 DEG C, and rectifying tower top is adopted
Acetone and part acetone is flowed back out, side take-off methanol, the DMP product that tower lower end produces concentration >=99% is simultaneously condensed laggard
Enter product receiving slit, tower bottom recovered water removes waste water after hot water storgae is collected.
Further, process 1) in methanol (A), acetone (B) molar ratio be 3.5-3.8: 1.
Further, process 2) in methanol (C) and acetone (B) molar ratio be 0.2-0.5: 1.
Further, process 3) in acidic resins be acidity in ion exchange resin；Molecular sieve be selected from HZSM-5,
One of HMCM-22, SAPO-34, preferably SAPO-34.
Further, process 4) in secondary heat exchanger heat source be process 2) or process 5) in heat exchange recycling 70-75
DEG C hot water.
Further, process 5) in partition wall type rectifying column be divided into four regions, including rectifying section (I), stripping section (II),
Side line rectifying section (III) and public stripping section (IV)；Next door is the setting of eccentric or center, makes stripping section (II) and side line rectifying section
(III) cross-sectional area ratio is 1: 1~10: 1, and the number of plates of rectifying section (I) is 8-10 block, and the number of plates of stripping section (II) is
10-15 block, the number of plates of side line rectifying section (III) are 10-15 block, and the number of plates of public stripping section (IV) is 3-5 block, and is mentioned
It is identical as the number of plates of side line rectifying section (III) to evaporate section (II).
Further, process 5) in produce acetone and methanol return to process 1) in dosage bunker in recycle.
Compared with the prior art, the present invention has the following advantages:
(1) reactivity is improved as catalyst using the combination of acidic resins and molecular sieve, and molecular sieve is simultaneously
It can play the role of dehydrating agent, be integrally improved reaction yield, product yield is up to 83.6%；
(2) product separation is carried out using partition wall type rectifying column, overcomes the separation that methanol, acetone, DMP three's azeotropic occur
Difficult problem, and it is easy to operate；
(3) methanol, which is divided into two parts addition, ensure that the raw material into reactor is in best proportion, improves the receipts of reaction
Rate；
(4) heat exchange utilization sufficiently is carried out to the heat of technical process, effectively reduces energy consumption.
Detailed description of the invention
Fig. 1 is partition wall type rectifying tower structure schematic diagram of the invention.
In figure: I- rectifying section, II- stripping section, III- side line rectifying section, the public stripping section of IV-.
Specific embodiment
The present invention will now be described in detail with reference to examples, and the examples are only preferred embodiments of the present invention,
It is not limitation of the invention.
Embodiment 1
1) methanol (A), acetone (B) from tank field storage tank are in molar ratio 3.5: 1 pumped in dosage bunker；
2) methanol, acetone mixture are pumped up in built-in steam pipe coil and distillation still with destilling tower in dosage bunker；
Kettle is warming up to 65 DEG C, and tower top begins with reflux；Pressure≤0.015Mpa, bottom temperature≤80 DEG C in control tower, tower top control one
Fixed reflux ratio；Material a part is back in distillation still in reflux condenser, and remainder is cooled to 45- through first-stage condenser
Material-heat-exchanging that 50 DEG C, first-class heat exchanger and rear step alkalization device come out and the chilled brine for being cooled to 30-35 DEG C, secondary condenser
- 15 DEG C to -20 DEG C are cooled to, alkylation reactor is entered after cooling；The another part methanol in methanol measuring tank
(C) enter together from the same entrance of first-class heat exchanger with the outlet material from first-stage condenser；Methanol (C) and acetone (B)
Molar ratio is 0.5: 1
3) alkylation reactor is fixed bed reactors, wherein built-in solid acid catalyst, reaction temperature is in -15 DEG C, pressure
Power≤0.015Mpa, the solid acid catalyst are the combination of ion exchange resin and acidic molecular sieve SAPO-34 in acidity,
The mass ratio 5: 1 of ion exchange resin and acidic molecular sieve SAPO-34 in acidity；
4) enter alkalization device from the material that reactor comes out, built-in basic resin in the device that alkalizes, temperature is -15 in the device that alkalizes
DEG C, pressure≤0.015Mpa；From alkalization device come out material first through process 2) in first-class heat exchanger heat exchange, be warming up to 28-32
DEG C, exchange heat using secondary heat exchanger to after 65-70 DEG C, return to process 2) in distillation still circulation, until acetone contracting diformazan in kettle
When alcohol content reaches 60-65%, reaction terminates, and material is depressed into crude product slot with pressure itself in kettle；
5) material in crude product slot is sent into from the middle part of partition wall type rectifying column, partition wall type rectifying column is divided into four regions, wraps
It includes rectifying section (I), stripping section (II), side line rectifying section (III) and public stripping section (IV)；Next door makes stripping section (II) and side line
The cross-sectional area ratio of rectifying section (III) is 1: 1, and the number of plates of rectifying section (I) is 8 pieces, and the number of plates of stripping section (II) is 15 pieces,
The number of plates of side line rectifying section (III) is 15 pieces, and the number of plates of public stripping section (IV) is 5 pieces；Tower reactor is warming up to 70-78 DEG C,
Rectifying tower top extraction acetone simultaneously flows back part acetone, and side take-off methanol, tower lower end produces the DMP product of concentration >=99% simultaneously
Enter product receiving slit after condensing, tower bottom recovered water removes waste water after hot water storgae is collected.
Using acetone dosage as calculating benchmark, the yield of product DMP is 80.7%, purity 99.3%.
Embodiment 2
1) methanol (A), acetone (B) from tank field storage tank are in molar ratio 3.8: 1 pumped in dosage bunker；
2) methanol, acetone mixture are pumped up in built-in steam pipe coil and distillation still with destilling tower in dosage bunker；
Kettle is warming up to 65 DEG C, and tower top begins with reflux；Pressure≤0.015Mpa, bottom temperature≤80 DEG C in control tower, tower top control one
Fixed reflux ratio；Material a part is back in distillation still in reflux condenser, and remainder is cooled to 45- through first-stage condenser
Material-heat-exchanging that 50 DEG C, first-class heat exchanger and rear step alkalization device come out and the chilled brine for being cooled to 30-35 DEG C, secondary condenser
- 15 DEG C to -20 DEG C are cooled to, alkylation reactor is entered after cooling；The another part methanol in methanol measuring tank
(C) enter together from the same entrance of first-class heat exchanger with the outlet material from first-stage condenser；Methanol (C) and acetone (B)
Molar ratio is 0.2: 1
3) alkylation reactor is fixed bed reactors, wherein built-in 12g solid acid catalyst, reaction temperature -15 DEG C,
Pressure≤0.015Mpa, the solid acid catalyst are the group of ion exchange resin and acidic molecular sieve SAPO-34 in acidity
It closes, the mass ratio 5: 1 of ion exchange resin and acidic molecular sieve SAPO-34 in acidity；
4) enter alkalization device from the material that reactor comes out, built-in basic resin in the device that alkalizes, temperature is -15 in the device that alkalizes
DEG C, pressure≤0.015Mpa；From alkalization device come out material first through process 2) in first-class heat exchanger heat exchange, be warming up to 28-32
DEG C, exchange heat using secondary heat exchanger to after 65-70 DEG C, return to process 2) in distillation still circulation, until acetone contracting diformazan in kettle
When alcohol content reaches 60-65%, reaction terminates, and material is depressed into crude product slot with pressure itself in kettle；
5) material in crude product slot is sent into from the middle part of partition wall type rectifying column, partition wall type rectifying column is divided into four regions, wraps
It includes rectifying section (I), stripping section (II), side line rectifying section (III) and public stripping section (IV)；Next door makes stripping section (II) and side line
The cross-sectional area ratio of rectifying section (III) is 5: 1, and the number of plates of rectifying section (I) is 8 pieces, and the number of plates of stripping section (II) is 15 pieces,
The number of plates of side line rectifying section (III) is 15 pieces, and the number of plates of public stripping section (IV) is 5 pieces；Tower reactor is warming up to 70-78 DEG C,
Rectifying tower top extraction acetone simultaneously flows back part acetone, and side take-off methanol, tower lower end produces the DMP product of concentration >=99% simultaneously
Enter product receiving slit after condensing, tower bottom recovered water removes waste water after hot water storgae is collected.
Using acetone dosage as calculating benchmark, the yield of product DMP is 83.6%, purity 99.5%.
Comparative example 1
In addition to use 12g acidity in ion exchange resin be catalyst other than, remaining is identical as example 2.
Using acetone dosage as calculating benchmark, the yield of product DMP is 68.9%, purity 99.3%.
Comparative example 2
In addition to use 12g acidic molecular sieve SAPO-34 be catalyst other than, remaining is identical as example 2.
Using acetone dosage as calculating benchmark, the yield of product DMP is 63.3%, purity 99.1%.
Comparative example 3
In addition to methanol is disposably in process 1) in be added, in process 2) in do not add methanol, and methanol and acetone mole
Except 4: 1, remaining is identical as example 2.
Using acetone dosage as calculating benchmark, the yield of product DMP is 77.6%, purity 99.2%.
Comparative example 4
In addition to process 5) in use routine rectifying column (number of plates is 28 piece) other than, remaining is identical as example 2.
It handles identical inventory and reaches the DMP product requirement of tower lower end extraction concentration >=99%, rectifying separates the used time
It is 4.5 hours, and the rectifying in embodiment 2 separates the used time 2 hours.
The present invention can be summarized with others without prejudice to the concrete form of spirit or essential characteristics of the invention.Of the invention
Above-described embodiment can only all be considered the description of the invention rather than limit that all substantial technologicals according to the present invention are to above
Any subtle modifications, equivalent variations and modifications, belong in the range of technical solution of the present invention made by embodiment.
Claims (8)
1. a kind of preparation method of acetone dimethyl acetal, it is characterised in that: including following process:
1) methanol (A), acetone (B) from tank field storage tank are in molar ratio 3.2-4.0: 1 pumped in dosage bunker；
2) methanol, acetone mixture are pumped up in built-in steam pipe coil and distillation still with destilling tower in dosage bunker；Kettle liter
For temperature to 65-70 DEG C, tower top begins with reflux；Pressure≤0.020Mpa, bottom temperature≤85 DEG C in control tower, tower top control are certain
Reflux ratio；Material a part is back in distillation still in reflux condenser, and remainder is cooled to 45-50 through first-stage condenser
DEG C, the material-heat-exchanging that comes out of first-class heat exchanger and rear step alkalization device and be cooled to 30-35 DEG C, the chilled brine of secondary condenser it is cold
But -15 DEG C to -20 DEG C are arrived, alkylation reactor is entered after cooling；Another part methanol (C) in methanol measuring tank
Enter together from the same entrance of first-class heat exchanger with the outlet material from first-stage condenser；
3) alkylation reactor is fixed bed reactors, wherein built-in solid acid catalyst, reaction temperature -15 DEG C to -20 DEG C,
Pressure≤0.015Mpa, the solid acid catalyst are the combination of acidic resins and acidic molecular sieve, acidic resins and acidity point
Mass ratio 3-5: 1 of son sieve；
4) enter alkalization device from the material that reactor comes out, built-in basic resin in the device that alkalizes, temperature is at -15 DEG C in the device that alkalizes
To -20 DEG C, pressure≤0.015Mpa；From alkalization device come out material first through process 2) in first-class heat exchanger heat exchange, be warming up to
28-32 DEG C, exchange heat using secondary heat exchanger to after 65-70 DEG C, return to process 2) in distillation still circulation, until in kettle acetone contract
When diformazan alcohol content reaches 60-65%, reaction terminates, and material is depressed into crude product slot with pressure itself in kettle；
5) material in crude product slot is sent into from the middle part of partition wall type rectifying column, tower reactor is warming up to 70-78 DEG C, rectifying tower top extraction third
Ketone simultaneously flows back part acetone, side take-off methanol, and tower lower end produces the product of concentration >=99% and enters product after condensing
Receiving slit, tower bottom recovered water remove waste water after hot water storgae is collected.
2. according to the method described in claim 1, it is characterized in that process 1) in methanol (A), acetone (B) molar ratio be 3.5-
3.8∶1。
3. according to the method described in claim 1, it is characterized in that process 2) in methanol (C) and acetone (B) molar ratio be 0.2-
0.5∶1。
4. according to the method described in claim 1, it is characterized in that process 3) in acidic resins be acid mesoporous amberlite
Rouge；Molecular sieve is selected from one of HZSM-5, HMCM-22, SAPO-34, preferably SAPO-34.
5. according to the method described in claim 1, it is characterized in that process 4) in the heat source of secondary heat exchanger be process 2) or
Process 5) in heat exchange recycling 70-75 DEG C of hot water.
6. according to the method described in claim 1, it is characterized in that process 5) in partition wall type rectifying column be divided into four regions, wrap
It includes rectifying section (I), stripping section (II), side line rectifying section (III) and public stripping section (IV)；Next door (5) is that eccentric or center is set
It sets, makes the cross-sectional area ratio 1: 1~10: 1 of stripping section (II) Yu side line rectifying section (III).
7. according to the method described in claim 6, it is characterized in that the number of plates of rectifying section (I) is 8-10 block, stripping section (II)
The number of plates be 10-15 block, the number of plates of side line rectifying section (III) is 10-15 block, and the number of plates of public stripping section (IV) is 3-
5 pieces, and stripping section (II) is identical as the number of plates of side line rectifying section (III).
8. according to the method described in claim 1, it is characterized in that process 5) in the acetone that produces and methanol return to process 1)
In dosage bunker in recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711169986.5A CN109776287A (en) | 2017-11-15 | 2017-11-15 | A kind of preparation method of acetone dimethyl acetal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711169986.5A CN109776287A (en) | 2017-11-15 | 2017-11-15 | A kind of preparation method of acetone dimethyl acetal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109776287A true CN109776287A (en) | 2019-05-21 |
Family
ID=66495513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711169986.5A Pending CN109776287A (en) | 2017-11-15 | 2017-11-15 | A kind of preparation method of acetone dimethyl acetal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109776287A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724038A (en) * | 2019-11-06 | 2020-01-24 | 安徽华甬新材料股份有限公司 | Preparation method of methyl isopropenyl ether |
| CN113999092A (en) * | 2021-09-30 | 2022-02-01 | 宿迁盛基医药科技有限公司 | Method and device for recycling byproducts in production of statins intermediates |
| CN114213223A (en) * | 2021-12-08 | 2022-03-22 | 浙江胡涂硅有限公司 | Production process and production device of 2, 2-dimethoxypropane |
| CN115536504A (en) * | 2022-09-19 | 2022-12-30 | 江苏道尔顿石化科技有限公司 | Bulkhead catalytic reaction method and device for synthesizing polymethoxy dimethyl ether |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810753A (en) * | 2006-02-28 | 2006-08-02 | 上海华谊丙烯酸有限公司 | Acid zeolite catalyzed process to synthesize acetal (ketal) |
| CN101357887A (en) * | 2008-07-31 | 2009-02-04 | 中国石油大学(华东) | Ethyl acetate synthetic process and apparatus thereof |
| CN101367724A (en) * | 2008-09-18 | 2009-02-18 | 中国石油大学(华东) | Method and apparatus for synthesis of isopropyl acetate |
| CN102070417A (en) * | 2011-01-06 | 2011-05-25 | 福州大学 | Dimethoxym ethane catalytic distillation production process and production equipment thereof |
| CN102584513A (en) * | 2012-02-27 | 2012-07-18 | 江西师范大学 | Method for preparing ketal by catalysis of ionic liquid and dehydration of acid-resistant molecular sieve membrane |
| CN103058837A (en) * | 2013-01-29 | 2013-04-24 | 福建师范大学福清分校 | Method and equipment for producing acetal through catalytic distillation |
| CN103772167A (en) * | 2014-01-08 | 2014-05-07 | 浙江胡涂硅有限公司 | Preparation method of 2, 2-dimethoxypropane |
| CN104193598A (en) * | 2014-08-13 | 2014-12-10 | 山东滨州新天阳化工有限责任公司 | Multi-reflux environment-friendly dimethoxymethane preparation process |
| CN104326888A (en) * | 2014-09-27 | 2015-02-04 | 安徽华甬新材料有限公司 | Preparation method of 2,2-dimethoxyl propane |
| CN105693687A (en) * | 2016-03-10 | 2016-06-22 | 天津大学 | Efficient reactive distillation method and device for glycol acetal/ketone reaction |
| CN106146265A (en) * | 2015-04-24 | 2016-11-23 | 衷晟 | A kind of 2, the synthetic method of 2-dialkoxy propane |
| CN106220499A (en) * | 2016-08-03 | 2016-12-14 | 中国石油大学(华东) | A kind of Apparatus and method for producing dimethyl adipate |
-
2017
- 2017-11-15 CN CN201711169986.5A patent/CN109776287A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810753A (en) * | 2006-02-28 | 2006-08-02 | 上海华谊丙烯酸有限公司 | Acid zeolite catalyzed process to synthesize acetal (ketal) |
| CN101357887A (en) * | 2008-07-31 | 2009-02-04 | 中国石油大学(华东) | Ethyl acetate synthetic process and apparatus thereof |
| CN101367724A (en) * | 2008-09-18 | 2009-02-18 | 中国石油大学(华东) | Method and apparatus for synthesis of isopropyl acetate |
| CN102070417A (en) * | 2011-01-06 | 2011-05-25 | 福州大学 | Dimethoxym ethane catalytic distillation production process and production equipment thereof |
| CN102584513A (en) * | 2012-02-27 | 2012-07-18 | 江西师范大学 | Method for preparing ketal by catalysis of ionic liquid and dehydration of acid-resistant molecular sieve membrane |
| CN103058837A (en) * | 2013-01-29 | 2013-04-24 | 福建师范大学福清分校 | Method and equipment for producing acetal through catalytic distillation |
| CN103772167A (en) * | 2014-01-08 | 2014-05-07 | 浙江胡涂硅有限公司 | Preparation method of 2, 2-dimethoxypropane |
| CN104193598A (en) * | 2014-08-13 | 2014-12-10 | 山东滨州新天阳化工有限责任公司 | Multi-reflux environment-friendly dimethoxymethane preparation process |
| CN104326888A (en) * | 2014-09-27 | 2015-02-04 | 安徽华甬新材料有限公司 | Preparation method of 2,2-dimethoxyl propane |
| CN106146265A (en) * | 2015-04-24 | 2016-11-23 | 衷晟 | A kind of 2, the synthetic method of 2-dialkoxy propane |
| CN105693687A (en) * | 2016-03-10 | 2016-06-22 | 天津大学 | Efficient reactive distillation method and device for glycol acetal/ketone reaction |
| CN106220499A (en) * | 2016-08-03 | 2016-12-14 | 中国石油大学(华东) | A kind of Apparatus and method for producing dimethyl adipate |
Non-Patent Citations (1)
| Title |
|---|
| 兰州石油机械研究所, 中国石化出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724038A (en) * | 2019-11-06 | 2020-01-24 | 安徽华甬新材料股份有限公司 | Preparation method of methyl isopropenyl ether |
| CN113999092A (en) * | 2021-09-30 | 2022-02-01 | 宿迁盛基医药科技有限公司 | Method and device for recycling byproducts in production of statins intermediates |
| CN114213223A (en) * | 2021-12-08 | 2022-03-22 | 浙江胡涂硅有限公司 | Production process and production device of 2, 2-dimethoxypropane |
| CN114213223B (en) * | 2021-12-08 | 2024-02-02 | 浙江胡涂硅有限公司 | Production process and production device of 2, 2-dimethoxy propane |
| CN115536504A (en) * | 2022-09-19 | 2022-12-30 | 江苏道尔顿石化科技有限公司 | Bulkhead catalytic reaction method and device for synthesizing polymethoxy dimethyl ether |
| CN115536504B (en) * | 2022-09-19 | 2024-04-05 | 江苏道尔顿石化科技有限公司 | Partition wall catalytic reaction method and device for polymethoxy dimethyl ether synthesis |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109776287A (en) | A kind of preparation method of acetone dimethyl acetal | |
| CN103030622B (en) | Method for preparing glyceride carbonate by using loop reaction device | |
| CN103506171B (en) | Modification acid cation exchange resin and uses thereof | |
| CN104209003B (en) | Industrial process based on methyl ether-boron trifluoride complex Separation of boron isotopes product | |
| CN102267972B (en) | Method for producing 1,3-dioxolame based on reaction-separation coupling | |
| CN107353188A (en) | A kind of method for preparing anhydrous gaseous formaldehyde | |
| CN110294675B (en) | Method and system for preparing methyl acetoacetate by adopting tubular continuous flow reactor | |
| CN104803958A (en) | Preparation technique for florosa | |
| CN109438196B (en) | Method for preparing 2, 2-dimethoxypropane | |
| CN102516044A (en) | Preparation method for 3,4'dichloro diaryl ether | |
| CN106380383B (en) | A kind of synthetic method of 2- hexenoic aldehyde | |
| CN102351713A (en) | Industrialized production method of 2,6-difluoroaniline | |
| CN110256397B (en) | Method for extracting biuret in process of preparing cyclic carbonate by reacting urea with polyhydric alcohol | |
| CN105622366B (en) | A kind of device and method for producing polymethoxy dimethyl ether DMM3 5 | |
| CN104355977A (en) | Synthesis process of raspberry ketone | |
| CN106518620B (en) | A kind of method and device preparing sec-butyl alcohol | |
| CN101735019A (en) | Process for producing resorcinol by continuously hydrolyzing m-phenylenediamine | |
| CN101676252A (en) | Method for preparing acetal by using glyoxal | |
| CN110437044A (en) | Prepare the method and device of polymethoxy dimethyl ether | |
| CN102399189B (en) | Synthesizing method of 3,4-dimethylpyrazole phosphate (DMPP) | |
| CN102206145A (en) | Continuous catalysis and rectification technology for synthesizing diethoxymethane | |
| CN106316792B (en) | The device and method of methanol and ethyl alcohol is recycled from stalk sugar hydrocrackates | |
| CN101337868A (en) | Method for preparing 3-phenoxy-benzaldehyde | |
| CN101220006B (en) | Buflomedil production method | |
| CN103483151A (en) | Ebanol preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190521 |
|
| WD01 | Invention patent application deemed withdrawn after publication |