CN106831334A - A kind of continuous production processes of alkaline process petrohol potassium - Google Patents
A kind of continuous production processes of alkaline process petrohol potassium Download PDFInfo
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- CN106831334A CN106831334A CN201710053288.2A CN201710053288A CN106831334A CN 106831334 A CN106831334 A CN 106831334A CN 201710053288 A CN201710053288 A CN 201710053288A CN 106831334 A CN106831334 A CN 106831334A
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- alcohol alkane
- potassium
- distillation column
- reactive distillation
- recovery tower
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 73
- 230000008569 process Effects 0.000 title claims abstract description 53
- 238000010924 continuous production Methods 0.000 title claims abstract description 20
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 16
- 239000011591 potassium Substances 0.000 title claims abstract description 16
- -1 alcohol alkane Chemical class 0.000 claims abstract description 55
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 50
- 238000011084 recovery Methods 0.000 claims abstract description 43
- WQKGAJDYBZOFSR-UHFFFAOYSA-N potassium;propan-2-olate Chemical compound [K+].CC(C)[O-] WQKGAJDYBZOFSR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000066 reactive distillation Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000003513 alkali Substances 0.000 claims abstract description 23
- 238000005516 engineering process Methods 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000005191 phase separation Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims 3
- 230000001476 alcoholic effect Effects 0.000 claims 1
- KVIPHDKUOLVVQN-UHFFFAOYSA-N ethene;hydrate Chemical compound O.C=C KVIPHDKUOLVVQN-UHFFFAOYSA-N 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 7
- 238000010923 batch production Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000002441 reversible effect Effects 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 4
- 238000011105 stabilization Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010533 azeotropic distillation Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropyl acetate Chemical group CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 description 1
- AWDMDDKZURRKFG-UHFFFAOYSA-N potassium;propan-1-olate Chemical compound [K+].CCC[O-] AWDMDDKZURRKFG-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- LMHHRCOWPQNFTF-UHFFFAOYSA-N s-propan-2-yl azepane-1-carbothioate Chemical compound CC(C)SC(=O)N1CCCCCC1 LMHHRCOWPQNFTF-UHFFFAOYSA-N 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940083608 sodium hydroxide Drugs 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/68—Preparation of metal alcoholates
- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a kind of continuous production processes of alkaline process petrohol potassium, the production technology produces potassium isopropoxide by raw material reaction of potassium hydroxide and isopropanol, and device of the present invention includes alcohol alkane solution reservoir, alkali soluble liquid storage tank, measuring pump, reactive distillation column, the condenser of reactive distillation column, Phase separation device, alcohol alkane recovery tower, the condenser of alcohol alkane recovery tower, the reboiler of alcohol alkane recovery tower, the reboiler of reactive distillation column, alcohol alkane solution evaporator.Continuous production processes packed height is calculated with potassium hydroxide reaction rate by isopropanol by power law type reaction kinetics equation, so as to meet the carrying out of potassium isopropoxide continuous prodution positive reaction, potassium isopropoxide using this technique productions meets product requirement, the continuous production processes flow is simple, raw material is cheap and easily-available, safe operation, be easy to monitoring and automated system implementation, be substantially shorter the production time, production capacity is effectively improved, comprehensive energy consumption is reduced.
Description
Technical field
The present invention relates to a kind of continuous production processes of alkaline process petrohol potassium, belong to technical field of fine.
Background technology
Potassium isopropoxide is a kind of strong oxidizer, is also a kind of important organic synthesis intermediate, is mainly used in medicine, agriculture
The industries such as medicine, chemical industry, food, leather.
Can there are metal method and alkaline process with industrialized synthetic method at present.Metal method with metallic potassium with isopropanol as raw material enters
Prepared by row chemical reaction, advantage is that potassium isopropoxide content is high, reliable and stable, free alkali is low, has the disadvantage the valency of metal base simple substance
Lattice are high, are difficult to transport, store, and there is inflammable and explosive potential safety hazard.Alkaline process is reacted with isopropanol using potassium hydroxide
It is prepared, alkali process overcomes the shortcoming of metal method production technology, the security of production is substantially increased, as isopropanol
The main flow synthesis technique of potassium, but the technique has the drawback that this reaction belongs to reversible reaction, and back reaction speed much larger than just
Reaction rate, reaction product water can not be completely eliminated, and free alkali content is higher in causing potassium isopropoxide product, reduce potassium isopropoxide
Product quality.
Therefore, in the alkaline process production technology of potassium isopropoxide, in order to suppress the carrying out of back reaction, it is ensured that potassium isopropoxide is held
Continuous synthesis, it is necessary to remove the water produced in reaction in time.In the alkaline process production technology of potassium isopropoxide, isopropyl alcohol and water belongs to altogether
Boiling thing system, common reactive distillation method can not obtain the relatively low potassium isopropoxide product of free alkali content, industrially frequently with altogether
Boiling method is dehydrated, and does not participate in the entrainer of reaction by adding in the feed, such as benzene, acetone, hexamethylene, makes it in rectifying
New azeotropic mixture is formed with the component such as water in tower and enter vapour phase by mass transfer, depart from from reaction system.
There is in reactor raw material and need by circulating-heating in the batch production process that alkaline process prepares potassium isopropoxide, energy consumption is big,
And it needs the raw material of driving and parking and discontinuity to deliver and product extraction, unit interval production capacity is relatively low；Meanwhile, in the process,
The labour intensity of personnel is big and operating procedure is more, frequent operation, and the mode of operation of different personnel is different, easily causes product quality ripple
Dynamic and easy generation maloperation situation.
Azeotropic reactive distillation is produced in the text of potassium tert-butoxide one, and reaction and azeotropic distillation are combined as a whole using on interface
Technique and the packed tower with bigger serface, obtain the purpose product of strong reversible reaction, but this article to only relate to interval raw
Production. art, it may have the normal of the technique has shortcoming.Using interval in the text of technological design one of sodium-hydroxide method production sodium isopropylate
But preparation technology, can extremely disappear free alkali without acetic acid isopropyl, save raw material, simplify operation also do not refer to that alkaline process synthesizes
Any enlightenment of the continuous production processes of potassium isopropoxide.
The content of the invention
The above mentioned problem that the batch production process of potassium isopropoxide is present is prepared to solve alkaline process, the present invention provides a kind of alkaline process
The continuous production processes of petrohol potassium, the relevant device that it is related to includes alcohol alkane solution reservoir, alkali soluble liquid storage tank, metering
Pump, reactive distillation column, rectifying column condenser, Phase separation device, alcohol alkane recovery tower, recovery tower condenser, recovery tower reboiler, essence
Tower reboiler is evaporated, evaporator, aqueous isopropanol storage tank uses the alkaline process production technology with potassium hydroxide and isopropanol as raw material to close
Into potassium isopropoxide.
Further, it is potassium hydroxide, isopropanol, hexamethylene mixing clear liquid by a certain percentage in above-mentioned alkali soluble liquid storage tank,
Above-mentioned measuring pump is transported to the tower of above-mentioned reactive distillation column in process of production after the clear liquid in above-mentioned alkali soluble liquid storage tank is extracted out
Top.
Further, after the aqueous isopropanol in above-mentioned aqueous isopropanol storage tank is heated through above-mentioned evaporator, in vapour form
The potassium hydroxide solution of liquid film is formed from bottom of towe into above-mentioned reactive distillation column, IPA vapor and in above-mentioned reactive distillation column
Haptoreaction, generates potassium isopropoxide and water.
Further, the hexamethylene for entering from tower top with potassium hydroxide forms ternary azeotropic as water entrainer with water, isopropanol
Thing, product water is taken out from potassium isopropoxide reaction, and suppressing back reaction is carried out, it is ensured that the lasting synthesis of potassium isopropoxide.
Further, packed height is determined by isopropanol with potassium hydroxide reaction rate.
Further, the reaction rate of isopropanol and potassium hydroxide by the content of free alkali in sample, water, total alkali determine it is different
The power law type reaction kinetics equation that potassium propoxide synthesizes at ambient pressure is obtained.
Further, most of potassium isopropoxide from the reactions above rectifying column bottom of towe extraction, a part of potassium isopropoxide is by upper
Above-mentioned reactive distillation column is come back to after stating the heating of rectifying column reboiler, to improve product quality.
Further, the tower top of ternary azeotrope rectifying column from the reactions above is passed through above-mentioned rectifying column condensation as a vapor
Device, condensed liquefied mixture enters above-mentioned Phase separation device.
Further, the light phase (predominantly hexamethylene) that liquefied mixture through above-mentioned Phase separation device separate, from overhead reflux
Recycled to above-mentioned reactive distillation column, heavy phase is aqueous concentration alcohol alkane solution higher, heavy-phase liquid is passed through into above-mentioned alcohol alkane returns
Receiving tower carries out alcohol alkane recovery.
Further, heavy-phase liquid is separated into the alcohol alkane solution and water of low water content, alcohol alkane azeotropic in above-mentioned alcohol alkane recovery tower
Thing enters above-mentioned recovery tower condenser from the tower top of above-mentioned alcohol alkane recovery tower as a vapor, it is condensed after alcohol alkane solution one
Part is transported to above-mentioned alcohol alkane solution reservoir and recycles, and another part passes back into above-mentioned alcohol alkane recovery tower.
Further, the water isolated from heavy-phase liquid is produced from the bottom of towe of above-mentioned alcohol alkane recovery tower, and a part of aqueous solution passes through
Enter above-mentioned alcohol alkane recovery tower after above-mentioned recovery tower reboiler heating, be used to improve the alcohol alkane rate of recovery.
By the technical scheme of the application above, the invention generates following technique effect：
1st, compared with the batch reactive distillation process of potassium isopropoxide, the control parameter at control point during continuous reaction rectification
Stabilization, is conducive to the intelligent operation of production technology, is easy to monitoring.
2nd, continuous process effectively prevent manpower, the energy that each driving and parking process of batch production process is additionally consumed
Source and time, minimize the comprehensive energy consumption of whole technique, material consumption.
3rd, continuous production processes can make production capacity effectively improve, and product quality obtains stabilization and ensures, is conducive to next
The stabilization of operation is carried out, and the technique has the advantages that continuous production, easy to operate.
4th, the continuous production processes set up based on isopropanol and potassium hydroxide reaction mechanism, comprehensive energy consumption is small, the time
Utilization rate is greatly improved, and uses measure control, automation mechanized operation level to be further enhanced technique more, and raw material is not in reactor
Need circulating-heating, it is not necessary to which the raw material of driving and parking and discontinuity is delivered and product extraction.
5th, the present invention by analyze influence that reversible reaction in potassium isopropoxide alkaline process intermittent preparing process synthesizes to it and
The heterogeneous azeotropic removal efficiency of water, it is proposed that a kind of continuous production processes of alkaline process petrohol potassium, the continuous processing bag
Potassium isopropoxide reactive distillation part and alcohol alkane recovery section are included, the batch production process comprehensive energy consumption compared with potassium isopropoxide is low, and produced
Can effectively improve, product quality stabilization；Meanwhile, improve automation and the level of informatization of potassium isopropoxide production process.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of the continuous production processes of alkaline process petrohol potassium of the invention.
1- alcohol alkane solution reservoirs, 2- alkali soluble liquid storage tanks, 3- measuring pumps, 4- reactive distillation columns, 5- rectifying column condensers, 6- liquid
Liquid phase-splitter 7- alcohol alkane recovery towers, 8- recovery tower condensers, 9- recovery tower reboilers, 10- rectifying column reboilers, 11- evaporators,
12- aqueous isopropanol storage tanks.
Specific embodiment
Detailed process of the invention is illustrated by implementation below in conjunction with accompanying drawing.
A kind of continuous production processes of alkaline process petrohol potassium of the invention, its technical characteristics are using azeotropic essence
Method dehydration is evaporated, with hexamethylene as water entrainer, potassium isopropoxide is produced as raw material with hydroxide flake potassium and isopropanol, raw material proportioning is different
Propyl alcohol：Hexamethylene：Potassium hydroxide=6:3:1.
A kind of continuous production processes of alkaline process petrohol potassium, including alcohol alkane solution reservoir 1, alkali soluble liquid storage tank 2, metering
Pump 3, reactive distillation column 4, rectifying column condenser 5, Phase separation device 6, alcohol alkane recovery tower 7, recovery tower condenser 8, recovery tower is again
Boiling device 9, rectifying column reboiler 10, evaporator 11, aqueous isopropanol storage tank 12.
Isopropanol, hexamethylene, the mixture clear liquid of potassium hydroxide, about 13 tons of raw material total amount, hydrogen are placed in alkali soluble liquid storage tank 2
After potassium oxide dissolving, mixeding liquid temperature can reach about 50 DEG C (summer).In process of production, measuring pump 3 is by alkali soluble liquid storage tank 2
Clear liquid extract out after be transported to the tower top of reactive distillation column 4.
Aqueous isopropanol in aqueous isopropanol storage tank 12 enters, isopropyl through evaporator 11 from the bottom of towe of reactive distillation column 4
Alcohol and the potassium hydroxide haptoreaction in the filler of reactive distillation column 4, generate potassium isopropoxide and water.
Reactive distillation column 4 is atmospheric operation, tower top 64 DEG C of temperature of control, tower reactor 72 DEG C of temperature of control.Isopropanol and hydrogen-oxygen
Change nak response speed to be studied by batch production process, uniform sampling is reached up to free alkali and total alkali on an hourly basis from reactor
To product requirement, and measure the content of free alkali in sample, water, total alkali respectively using karl Fischer reagent and acid base titration.
According to the data of experiment measurement, fitting has obtained the power law type reaction kinetics equation that potassium isopropoxide synthesizes at ambient pressure, with this
As the foundation for calculating packed height, not only need to meet reaction time demand but also needs meet separation requirement.The reaction of power law type is dynamic
The formula of mechanical equation is as follows：
In above formula：R is potassium isopropoxide generating rate, molL-1·s-1；C is different solutions concentration, molL-1；T is temperature
Degree, K；T is time, s.
Potassium isopropoxide batch production process filler need to only meet separation requirement, and reactive moieties are carried out in a kettle.,
Its advantage can be to provide the enough reaction time, debug more convenient, be easy to get to qualified products；Shortcoming is similarly obvious, instead
Answering raw material in kettle needs by circulating-heating, and energy consumption is big, and it needs the raw material of driving and parking and discontinuity to deliver and product is produced, list
Position time production capacity is relatively low；Meanwhile, in the process, the labour intensity of personnel is big and operating procedure is more, frequent operation, different personnel
Mode of operation it is different, easily cause product quality fluctuation and maloperation situation easily occur.By contrast, with isopropanol and hydroxide
The continuous production processes set up based on nak response mechanism, comprehensive energy consumption is small, and time availability is greatly improved, using meter more than technique
Amount control, automation mechanized operation level is further enhanced, and is the trend of technique and engineering development.
Hexamethylene from tower top entrance forms ternary azeotrope and enters vapour phase as water entrainer with generation water, isopropanol, will
Product water is taken out from potassium isopropoxide reaction, and suppressing back reaction is carried out, it is ensured that the lasting synthesis of potassium isopropoxide.
Ternary azeotrope is passed through rectifying column condenser 5, condensed liquid as a vapor from the tower top of reactive distillation column 4
State mixture is passed through Phase separation device 6.
Product potassium isopropoxide is produced by the bottom of towe of reactive distillation column 4, by rectifying column reboiler 10, a part of potassium isopropoxide
By coming back to reactive distillation column 4 after heating, to improve product quality.
Light-phase liquid after being separated through Phase separation device 6 is mainly hexamethylene, passes back into reactive distillation column 4 and recycles, weight
Component is mainly water content alcohol alkane solution higher, and heavy constituent is passed through into alcohol alkane recovery tower 7 carries out alcohol alkane recovery.
Heavy constituent isolates the alcohol alkane solution and water of low water content in alcohol alkane recovery tower 7, and the steam of alcohol alkane solution is by alcohol
The overhead extraction of alkane recovery tower 7 is simultaneously passed through recovery tower condenser 8, it is condensed after an alcohol alkane solution part be transported to alcohol alkane solution
Storage tank 1 is recycled, and a part passes back into alcohol alkane recovery tower 7.
The water isolated in alcohol alkane recovery tower 7 is discharged by bottom of towe, and part tower reactor solution is by after the heating of recovery tower reboiler 9
It is circulated, is used to improve the alcohol alkane rate of recovery.
The present invention proposes a kind of continuous production processes of alkaline process petrohol potassium, using potassium hydroxide and isopropanol
Reversible reaction petrohol potassium, because back reaction speed is much larger than positive reaction speed, is carried out instead using the method for azeotropic distillation
The carrying out of the dehydration guarantee positive reaction of thing system is answered, using hexamethylene as entrainer, forms non-equal with the water for removing out reaction system
Phase azeotropic mixture, and hexamethylene solubility in water is low, easily realizes the recycling of hexamethylene, it is ensured that in continuous flow procedure
The band water effect of hexamethylene, while continuous production processes can effectively realize that production capacity is improved, reducing energy consumption improves production process
Automatic control level.
Embodiments above is merely to illustrate the technical scheme being not intended to limit the present invention.Any of spirit of the present invention is not departed from
Modification or local replacement, all should cover in the middle of scope of the presently claimed invention.
Claims (10)
1. a kind of continuous production processes of potassium isopropoxide, the relevant device that it is related to includes alcohol alkane solution reservoir, alkali soluble liquid storage tank,
Measuring pump, reactive distillation column, the condenser of reactive distillation column, Phase separation device, alcohol alkane recovery tower, the condensation of alcohol alkane recovery tower
Device, the reboiler of alcohol alkane recovery tower, the reboiler of reactive distillation column, alcohol alkane solution evaporator, it is characterised in that use with hydrogen-oxygen
It is the alkaline process production technology petrohol potassium of raw material to change potassium and isopropanol.
2. production technology according to claim 1, it is characterised in that the clear liquid of alcoholic caustic potash is placed on aqueous slkali
In storage tank, the top of reactive distillation column is transported to after the clear liquid in alkali soluble liquid storage tank is extracted out with measuring pump.
3. production technology according to claim 1, it is characterised in that the alcohol alkane solution in alcohol alkane solution reservoir is molten through alcohol alkane
Liquid evaporator, enters, isopropanol and the potassium hydroxide haptoreaction in the filler of reactive distillation column from the bottom of towe of reactive distillation column,
Generation potassium isopropoxide and water, product water and hexamethylene, isopropanol form the ternary azeotrope of temperature minimum point again.
4. according to the production technology described in claim 3, it is characterised in that described filler height is reacted by isopropanol and potassium hydroxide
Speed is determined.
5. according to the production technology described in claim 4, it is characterised in that the reaction rate of the isopropanol and potassium hydroxide is by sample
The power law type reaction kinetics equation that the potassium isopropoxide that free alkali, water, the content of total alkali determine in product synthesizes at ambient pressure is calculated
Obtain.
6. production technology according to claim 3, it is characterised in that ternary azeotrope is from the tower top of reactive distillation column steaming
The form of vapour is passed through the condenser of reactive distillation column, and condensed liquefied mixture is passed through Phase separation device.
7. production technology according to claim 1, it is characterised in that product potassium isopropoxide is adopted from the bottom of towe of reactive distillation column
Go out, by the reboiler of reactive distillation column, certain reflux ratio is controlled, to improve product quality.
8. production technology according to claim 6, it is characterised in that the light component after being separated through Phase separation device is mainly
Hexamethylene, passes back into reactive distillation column recycling, and heavy constituent is mainly the mixed liquor of water and isopropanol, also contains a small amount of ring
Hexane, heavy constituent is passed through into alcohol alkane recovery tower carries out alcohol alkane recovery.
9. production technology according to claim 8, it is characterised in that it is molten that heavy constituent is separated into alcohol alkane in alcohol alkane recovery tower
Liquid and water, the steam of alcohol alkane solution by alcohol alkane recovery tower overhead extraction and be passed through the condenser of alcohol alkane recovery tower, it is condensed after
An alcohol alkane solution part be transported to the recycling of alcohol alkane solution reservoir, a part passes back into alcohol alkane recovery tower.
10. production technology according to claim 9, it is characterised in that the water isolated from heavy constituent is by alcohol alkane recovery tower
Bottom of towe is produced, and by the reboiler of alcohol alkane recovery tower, controls certain reflux ratio, is used to improve the alcohol alkane rate of recovery.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299159A (en) * | 2018-03-01 | 2018-07-20 | 浙江大学 | A kind of continuous method for preparing 2- methallyl alkoxide alcoholic solutions |
| CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
| CN112144075A (en) * | 2020-10-09 | 2020-12-29 | 上海漫关越水处理有限公司 | Method for continuously synthesizing potassium tert-butoxide by membrane electrolysis |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004285002A (en) * | 2003-03-24 | 2004-10-14 | Sumitomo Chem Co Ltd | Condensation method |
-
2017
- 2017-01-22 CN CN201710053288.2A patent/CN106831334A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004285002A (en) * | 2003-03-24 | 2004-10-14 | Sumitomo Chem Co Ltd | Condensation method |
Non-Patent Citations (3)
| Title |
|---|
| 朱炳辰 等: "《化学反应工程 第2版》", 《化学反应工程 第2版》 * |
| 王化淳 等: "王化淳 等", 《化学工程》 * |
| 王化淳 等: "用共沸反应精馏制取叔丁醇钾的工艺设备及放大", 《化学工程》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299159A (en) * | 2018-03-01 | 2018-07-20 | 浙江大学 | A kind of continuous method for preparing 2- methallyl alkoxide alcoholic solutions |
| CN108299159B (en) * | 2018-03-01 | 2020-06-12 | 浙江大学 | Method for continuously preparing 2-methyl allyl alcohol solution |
| CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
| CN108950208B (en) * | 2018-06-04 | 2023-09-29 | 山东习尚喜新材料科技股份有限公司 | Continuous production device and process of metal potassium |
| CN112144075A (en) * | 2020-10-09 | 2020-12-29 | 上海漫关越水处理有限公司 | Method for continuously synthesizing potassium tert-butoxide by membrane electrolysis |
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