CN105585542B - A method of separation epoxychloropropane - Google Patents
A method of separation epoxychloropropane Download PDFInfo
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Abstract
The present invention provides a kind of method of separation epoxychloropropane, this method includes：Will be using chloropropene as raw material, H2O2The reaction mass progress extraction and separation that epoxychloropropane is prepared for the epoxidation of oxidant, obtain raffinate phase and extraction phase；The raffinate phase is sent into Separation of Organic and water in the first distillation system；The extraction phase is sent into separation epoxychloropropane and extractant in the second distillation system；Wherein, first distillation system includes first rectifying column and Second distillation column, and the condition for controlling first rectifying column makes the organic solvent of 1 40 weight % in the raffinate phase be detached from the tower top of the first rectifying column；The condition of control Second distillation column enables the steam that the tower top from the Second distillation column obtains as at least partly heat source of the second distillation system.The steam condensation heat during methanol rectification can be fully utilized in method provided by the invention, and the separating energy consumption that Direct Epoxidation method prepares epoxychloropropane technique is greatly reduced.
Description
Technical field
The present invention relates to a kind of methods of separation epoxychloropropane, more specifically to one kind from hydrogen peroxide and chlorine
Propylene reaction prepares the method that epoxychloropropane is detached in the reaction product of epoxychloropropane.
Background technology
Epoxychloropropane (chloromethyloxirane, abbreviation ECH) is a kind of important Organic Chemicals and fine
Chemical products are widely used in synthetic epoxy resin, glycerine, chlorohydrin rubber, medicine, pesticide, surfactant, fiberglass, ion
Exchanger resin, coating and plasticizer etc..
The industrial process of ECH has three kinds of propylene high-temperature chloridising, allyl acetate method and glycerin chlorination method at present, all
It needs by chlorohydrination and saponification two procedures, there are the corrosion of serious equipment, while generating a large amount of chlorine-contained wastewater.Wherein,
Propylene high-temperature chloridising is main production method, and for domestic, the production capacity of propylene high-temperature chloridising accounts for ECH aggregated capacities
80% or more.Propylene high-temperature chloridising has the advantages that production technology is ripe, stable operation, product is flexible；But there are by-products
The problems such as object is more, material consumption is high, energy consumption is big, and especially wastewater discharge is greatly and a large amount of calcium chloride Solid state fermentations are difficult.
Direct oxidation method produces epoxychloropropane, is Titanium Sieve Molecular Sieve (abbreviation HTS) catalysis chloropropene and hydrogen peroxide (letter
Claim HPO) epoxidation prepares ECH, directly by chloropropene one-step synthesis ECH, eliminate chlorohydrination in existing ECH production technologies and
Two processes of saponification, equipment corrosion and wastewater discharge can significantly decrease, not generate waste residue substantially, belong to the clear of ECH
Clean production technology.Meanwhile the reaction has the characteristics that reaction condition is relatively mild, high selectivity, is the heat researched and developed at present
One of point.
Generally using a large amount of methanol as solvent in the Direct Epoxidation technique of chloropropene and hydrogen peroxide, by excessive chlorine
Propylene is dissolved in methanol solution to be reacted with hydrogen peroxide, to ensure the conversion ratio and epoxychloropropane of higher hydrogen peroxide
Selectivity.Although the reaction of the Direct Epoxidation of chloropropene and hydrogen peroxide has very high selectivity and conversion ratio, reaction product
It is middle to make the product separating energy consumption of Direct Epoxidation technique very high in the presence of a large amount of cycle solvents.Meanwhile using extraction in product purification
Extraction process, the recycling of extractant is taken also to account for the significant portion of plant energy consumption, therefore, the energy consumption for reducing solvent recovery is direct oxygen
Change method technique can large-scale application committed step.
If the method that solvent recovery and extractant recycling are all made of conventional distillation during epoxychloropropane is refined is completed, only it is applicable in
In the little situation of epoxychloropropane production scale.After epoxychloropropane production scale expands, required refined alcohols solvent
Amount and extraction dosage sharply increase, and energy consumption is obviously excessively high.
Invention content
It Direct Epoxidation method can be greatly lowered prepares epoxy chlorine the technical problem to be solved in the present invention is to provide one kind
The method of the separating energy consumption of propane technique.
To realize foregoing purpose, the present invention provides a kind of method of separation epoxychloropropane, this method includes：It will be with chlorine
Propylene is raw material, H2O2The reaction mass progress extraction and separation that epoxychloropropane is prepared for the epoxidation of oxidant, obtain raffinate phase
And extraction phase, wherein the reaction mass contains epoxychloropropane, organic solvent and water, and the boiling point of the organic solvent compares water
Low boiling point, for the boiling point of extractant than the low boiling point of epoxychloropropane, the extraction phase includes epoxychloropropane and extractant, institute
It includes organic solvent and water to state raffinate phase；
The raffinate phase is sent into Separation of Organic and water in the first distillation system；
The extraction phase is sent into separation epoxychloropropane and extractant in the second distillation system；Wherein, first essence
The system of evaporating includes first rectifying column and Second distillation column, and the condition for controlling first rectifying column makes the 1-40 in the raffinate phase heavy
The organic solvent for measuring % is detached from the tower top of the first rectifying column；The condition of control Second distillation column makes from second essence
Evaporating steam that the tower top of tower obtains can be as at least partly heat source of the second distillation system.
The steam condensation heat during methanol rectification can be fully utilized in method provided by the invention, and direct epoxy is greatly reduced
Change method prepares the separating energy consumption of epoxychloropropane technique, and advantage is：
Compared with conventional rectification technology, method provided by the invention can be used when carrying out reaction product separation, refining
Heat source of the methanol vapor as reboiler significantly reduces the energy of device without carrying out distillation operation using additional steam
Consumption, compared with the Direct Epoxidation technique only with direct rectificating method, energy consumption can reduce about 30% or more；Meanwhile it carrying out
When methanol rectification detaches, the methanol vapor of methanol rectification column overhead is cooled down without a large amount of recirculated cooling waters, is not only saved
Plant investment has been saved, the operating cost of device is also reduced, further reduced the energy consumption of device.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Attached drawing is to be used to provide further understanding of the present invention, an and part for constitution instruction, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the flow diagram according to a kind of method of the separation epoxychloropropane of preferred embodiment of the present invention.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
As previously mentioned, the present invention provides a kind of method of separation epoxychloropropane, this method includes：
Will be using chloropropene as raw material, H2O2It prepares the reaction mass of epoxychloropropane for the epoxidation of oxidant and is extracted
Separation, obtains raffinate phase and extraction phase, wherein the reaction mass contains epoxychloropropane, organic solvent and water, described organic
The boiling point of solvent is than the low boiling point of water, and for the boiling point of extractant than the low boiling point of epoxychloropropane, the extraction phase includes epoxy chlorine
Propane and extractant, the raffinate phase include organic solvent and water；The raffinate phase, which is sent into the first distillation system to detach, to be had
Solvent and water；
The extraction phase is sent into separation epoxychloropropane and extractant in the second distillation system；Wherein, first essence
The system of evaporating includes first rectifying column and Second distillation column, and the condition for controlling first rectifying column makes the 1-40 in the raffinate phase heavy
The organic solvent for measuring % is detached from the tower top of the first rectifying column；The condition of control Second distillation column makes from second essence
Evaporating steam that the tower top of tower obtains can be as at least partly heat source of the second distillation system.
With the method for the invention it is preferred to which the condition for controlling first rectifying column makes the weights of the 10-20 in the raffinate phase
The organic solvent for measuring % is detached from the tower top of the first rectifying column.
According to the method for the present invention, make the weights of the 1-40 in the raffinate phase by controlling the condition of first rectifying column
% is measured, the preferably organic solvent of 10-20 weight % is detached from the tower top of the first rectifying column, enabling passes through control second
The condition of rectifying column enables the steam that the tower top from the Second distillation column obtains as the part heat of the second distillation system
Source, or some or all of the second distillation system and the first rectifying column heat source can be used as.
According to the method for the present invention, make the weights of the 10-20 in the raffinate phase by controlling the condition of first rectifying column
The organic solvent for measuring % is detached from the tower top of the first rectifying column, enabling the condition by controlling Second distillation column makes
The steam obtained from the tower top of the Second distillation column can be as the second distillation system and the whole of the first rectifying column
Heat source.
With the method for the invention it is preferred to which second distillation system includes：Third distillation column, the first vacuum column.
With the method for the invention it is preferred to which the operating condition of the third distillation column includes：Tower top pressure be normal pressure extremely
0.5MPaG, theoretical cam curve 10-50, bottom temperature are 40-80 DEG C, reflux ratio 0.5-5.
With the method for the invention it is preferred to which the operating condition of the first vacuum column includes：Tower top pressure is vacuum, theoretical tray
Number is 5-30, and bottom temperature is 80-150 DEG C.
According to a preferred embodiment of the present invention, the condition of preferably control Second distillation column makes from described second
The steam that the tower top of rectifying column obtains can be as whole heat sources of the third distillation column and the first rectifying column.
With the method for the invention it is preferred to which the condition for controlling Second distillation column so that the tower top from the Second distillation column obtains
To steam in organic solvent content more than 90 weight %.
According to the method for the present invention, optional wider range for meeting the operating condition of aforementioned Second distillation column, for this hair
Bright, the operating condition in the preferably described Second distillation column includes：Tower top pressure is 0.3-4.0MPaG, theoretical cam curve 5-60,
Bottom temperature is 110-200 DEG C, reflux ratio 0.5-3.
According to the method for the present invention, the operating condition more preferably in the Second distillation column includes：Tower top pressure is 0.5-
2.0MPaG, theoretical cam curve 10-45, bottom temperature are 145-180 DEG C, reflux ratio 1-2.
According to the method for the present invention, by making the rectifying condition of Second distillation column meet aforementioned claim so that the second essence
The tower top methanol vapor for evaporating tower can be used as the second distillation system and the heat source of the tower bottom reboiler of first rectifying column uses.
According to the method for the present invention, optional wider range for meeting the operating condition of aforementioned first rectifying column, for this hair
Bright, the condition in the preferably described first rectifying column includes：Tower top pressure is normal pressure to 1.0MPaG, theoretical cam curve 5-60, tower
Kettle temperature degree is 40-120 DEG C, reflux ratio 0.5-3.
According to the method for the present invention, the condition more preferably in the first rectifying column includes：Tower top pressure be normal pressure extremely
0.5MPaG, theoretical cam curve 10-45, bottom temperature are 60-100 DEG C, reflux ratio 1-2.
According to the present invention, the condition by controlling first rectifying column makes the 1-40 weight % in the raffinate phase, preferably
The organic solvent of 10-20 weight % is detached from the tower top of the first rectifying column, may make the overhead vapours of Second distillation column just
Meet the heat supply of the second distillation system and the tower bottom reboiler of first rectifying column well.
In the present invention, the tower of the organic solvent of 1-40 weight %, the preferably 10-20 weight % of raffinate phase in first rectifying column
Top is separated, in charging of the aqueous solutions of organic solvent that first rectifying column kettle obtains as Second distillation column.
In the present invention, remaining organic solvent is isolated in Second distillation column tower top, bottom of tower is then organic solvent content pole
Low waste water.In the present invention, pass through the operating condition of preferred first rectifying column and Second distillation column, so as to get cycle it is organic molten
Agent purity is typically larger than 90 weight %, preferably greater than 95 weight %, more preferably greater than 98 weight %, while making Second distillation column
The content of organic solvent is less than 1 weight %, preferably smaller than 0.5 weight %, more preferably less than 0.1 weight % in tower reactor waste water.
With the method for the invention it is preferred to which the organic solvent content in the raffinate phase is 20-70 weight %, preferably
40-50 weight %.
With the method for the invention it is preferred to carry out the epoxidation as follows：Exist in titanium-silicon molecular sieve catalyst
Under, using organic solvent as solvent, chloropropene is contacted with hydrogen peroxide or aqueous hydrogen peroxide solution, obtains the reaction mass.
Wherein, the condition of contact can be the conventional selection of this field, and this is not described in detail here by the present invention.
With the method for the invention it is preferred to which this method further includes：It is condensed after carrying out heat exchange as the steam of heat source
The solvent that at least partly organic solvent arrived is used to contact with hydrogen peroxide or aqueous hydrogen peroxide solution as the chloropropene.
According to the present invention, optional wider range of the type of the organic solvent specifically can be according to epoxidation reaction institute
It needs to determine, for the present invention, the preferably described organic solvent is methanol.
According to the present invention, optional wider range of the type of the extractant, for the present invention, the preferably described extractant is
Chloropropene.
With the method for the invention it is preferred to which the reaction mass contains epoxychloropropane 5-20 weight %, organic solvent 20-
70 weight %, water 5-20 weight %, chloropropene 5-30 weight %, by-product 1-10 weight %.
According to a preferred embodiment of the present invention, then epoxychloropropane is preferably prepared as follows according to this
The method of invention is detached, wherein organic solvent is methanol, and extractant is chloropropene：
(1) hydrogen peroxide and chloropropene mixed dissolution in organic solvent, in epoxidation reactor with Titanium Sieve Molecular Sieve
Catalyst contact carries out epoxidation reaction, obtains the reaction product containing epoxychloropropane, the reaction product includes mainly
Epoxychloropropane, organic solvent and water can also include a small amount of high boiling point by-products produced and complete chloropropene of unreacted；
(2) reaction product from epoxidation reactor enters epoxychloropropane extraction cells, by the addition of extractant,
Isolate the extraction phase (can also claim organic phase) and the raffinate phase (also claiming water phase) so that organic molten in reaction product
Agent and epoxychloropropane are detached；
(3) raffinate phase from extraction cells enters the first distillation system, and first distillation system includes the first rectifying
Tower and Second distillation column, and the condition for controlling first rectifying column makes the organic solvent of the 10-40 weight % in the raffinate phase
It is detached from the tower top of the first rectifying column；The condition of control Second distillation column so that the tower top from the Second distillation column obtains
Steam can isolate organic solvent first alcohol and water as at least partly heat source of the second distillation system, organic solvent cycle
It utilizes；
(4) extraction phase from extraction cells isolates extractant chloropropene, epoxychloropropane into the second distillation system
And high-boiling-point impurity, extractant recycle.
The present invention is described further with reference to Fig. 1.It is only especially preferred embodiment of the invention below, it cannot
It is limited the scope of the invention with this, i.e., it is every with change and modification made by scope of the present invention patent, still belong to of the invention special
The range that profit covers.
In Fig. 1, organic solvent is methanol, and extractant is chloropropene, and raffinate phase 1 (also referred to as water phase 1) is sent into the first rectifying
Tower A1 carries out the separation of water, methanol, obtains methanol 3 (chloropropene containing small part) and methanol aqueous solution 6；The behaviour of first rectifying column A1
Include as condition：Tower top pressure is normal pressure to 1.0MPaG, and theoretical cam curve 5-60, bottom temperature is 40-120 DEG C, reflux ratio
For 0.5-3, preferably tower top pressure is normal pressure to 0.5MPaG, and theoretical cam curve 10-45, bottom temperature is 60-100 DEG C, reflux
Than for 1-2；
Methanol aqueous solution 6 enters back into Second distillation column A2 and is detached.Second distillation column A2 operating conditions include：Tower top pressure
Power is 0.3-4.0MPaG, and theoretical cam curve 5-60, bottom temperature is 110-200 DEG C, reflux ratio 0.5-3, preferably tower top pressure
Power is 0.5-2.0MPaG, and theoretical cam curve 10-45, bottom temperature is 145-180 DEG C, reflux ratio 1-2；So as to control
The temperature of Second distillation column tower top methanol vapor so that it can be as at least partly heat source of the second distillation system；Wherein,
The operating condition of two rectifying columns passes through preferred design, and preferably tower reactor uses pressure to be used as tower for the vapor 12 of 1.0MPaG or more
The heat source of bottom reboiler is more than 90%, preferably greater than 95%, more preferably so as to obtain purity from Second distillation column A2 tower tops
Methanol vapor 5 more than 98% obtains water 2 from Second distillation column A2 tower reactors；
Extraction phase 8 (also referred to as organic phase 8) is sent into the separation that third distillation column A3 carries out chloropropene, epoxychloropropane, is obtained
To extractant chloropropene 9 and epoxychloropropane solution 11, wherein the operating condition of third distillation column A3 includes：Tower top pressure is
Normal pressure to 0.5MPaG, theoretical cam curve 10-50, bottom temperature is 40-80 DEG C, reflux ratio 0.5-5；
Epoxychloropropane solution 11 continue to be fed into the first vacuum column A4 (tower top pressure is vacuum, theoretical cam curve 5-30,
Bottom temperature is 80-150 DEG C) it is detached, obtain epoxychloropropane 14 and chloropropene 13.
, according to the invention it is preferred to the operating condition of Second distillation column and first rectifying column be controlled, to establish suitably again
Boil the cold and hot stream temperature gradient of device so that methanol vapor 5 can supply first rectifying column A1 and third distillation column A3 again simultaneously
Device is boiled as whole heat sources.Methanol vapor 5 obtains after the condensation of the reboiler of first rectifying column A1 and third distillation column A3
Logistics 7 is combined as recycle methanol with logistics 10 and is back to the epoxidation reaction system that epoxidation reaction prepares epoxy chloropropionate alkene.
Embodiment 1
Using technique shown in FIG. 1, the raffinate phase (i.e. methanol aqueous solution) that epoxychloropropane separation and purification unit is obtained
(content of methanol is 45 mass % to 881kg/h, and the content of water is 49 mass %, and chloropropene content is 4 mass %, remaining is miscellaneous
Matter) being sent into first rectifying column, (theoretical cam curve 20, tower top pressure are normal pressure, and bottom temperature is 80 DEG C, reflux ratio 1, and institute
Methanol aqueous solution is stated to feed from the 10th piece of theoretical plate) rectifying separation is carried out, 801kg/h is measured in tower reactor discharging (methanol aqueous solution)
(group becomes：45 mass % of methanol, 54 mass % of water, chloropropene content are 0 mass %, remaining is impurity), it is isolated from tower top
The methanol chloropropene solution 80kg/h that temperature is 40 DEG C, purity is 50 mass %, wherein 10 weight %'s in the raffinate phase
Methanol is detached from the tower top of the first rectifying column；
First rectifying column tower reactor discharging (methanol aqueous solution) 801kg/h feedings Second distillation column (theoretical cam curve 30, and
Methanol aqueous solution is fed from the 15th piece of theoretical plate, tower top pressure 0.5MPa, and bottom temperature is 152 DEG C, reflux ratio 1) into
Row detaches, and is 112 DEG C by Second distillation column top extraction temperature, the methanol vapor that purity is 98 mass %, into first rectifying column
Tower reactor and third distillation column tower reactor reboiler as whole heat sources, after condensation, partial reflux is partly used as recycle methanol
It is back to the epoxidation reaction system that epoxidation reaction prepares epoxy chloropropionate alkene；
Extraction phase from extraction cells is detached into the second distillation system, and the second distillation system includes third rectifying
Tower (tower top pressure is normal pressure, and bottom temperature is 72 DEG C, theoretical cam curve 30, reflux ratio 1.5) and the first vacuum column, separation
Obtain extractant chloropropene, epoxychloropropane and high-boiling-point impurity.
First rectifying column bottom reboiler heat exchange load 80kW, Second distillation column bottom reboiler heat exchange load 292kW, third essence
Evaporate tower bottom reboiler heat exchange load 160kW.
Outer needed for the embodiment to energy consumption is 292kW.
Comparative example 1
According to the method for embodiment 1, the difference is that the process conditions of Second distillation column are different, and the tower top of Second distillation column
Steam is directly used in the solvent returned as reaction member, specifically：
Raffinate phase (i.e. methanol aqueous solution) 880kg/h (wherein, methanol that epoxychloropropane separation and purification unit obtained
Content is 45 mass %, and the content of water is 49 mass %, and chloropropene content is 4 mass %, remaining is impurity etc.) it is sent into the first essence
Evaporating tower, (theoretical cam curve 20, tower top pressure are normal pressure, and bottom temperature is 80 DEG C, and the methanol aqueous solution is managed from the 10th piece
Fed by plate) rectifying separation is carried out, tower reactor discharges, and (discharging group becomes (methanol aqueous solution) amount 800kg/h：45 matter of methanol
Measure %, 54 mass % of water, chloropropene content be 0 mass %, remaining is impurity), from tower top draw temperature be 40 DEG C, purity 50
The flow of quality % is the methanol chloropropene solution of 80kg/h, wherein the methanol of 10 weight % in the raffinate phase is from described
The tower top of first rectifying column detaches；
Wherein, first rectifying column tower reactor discharging (methanol aqueous solution) 800kg/h is sent into Second distillation column (theoretical cam curve is
30, and methanol aqueous solution is fed from the 15th piece of theoretical plate, tower top pressure is normal pressure 0.1MPa, and bottom temperature is 102 DEG C) it carries out
Separation, the methanol purity 99.5% of separation are back to the epoxidation that epoxidation reaction prepares epoxy chloropropionate alkene as recycle methanol
Reaction system；
Extraction phase from extraction cells is detached into the second distillation system, and the second distillation system includes third rectifying
Tower (tower top pressure is normal pressure, and bottom temperature is 72 DEG C, theoretical cam curve 30, reflux ratio 1.5) and the first vacuum column, separation
Obtain extractant chloropropene, epoxychloropropane and high-boiling-point impurity.
First rectifying column bottom reboiler heat exchange load 80kW, Second distillation column bottom reboiler heat exchange load 243kW, third essence
Evaporate tower bottom reboiler heat exchange load 160kW.
According to it is outer needed for the comparative example to energy consumption be 483kW.
It can be seen that method using the present invention, enables to the organic solvent obtained from the tower top of Second distillation column to steam
The heat of gas all efficiently uses, and to which the heat of entire separative element maximumlly be utilized, is effectively saved energy consumption.With only
It is compared using the Direct Epoxidation technique of direct rectificating method, energy consumption can reduce about 30% or more.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, it can be combined by any suitable means.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (11)
1. a kind of method of separation epoxychloropropane, which is characterized in that this method includes：
Will be using chloropropene as raw material, H2O2The reaction mass progress extraction and separation of epoxychloropropane are prepared for the epoxidation of oxidant,
Obtain raffinate phase and extraction phase, wherein the reaction mass contains epoxychloropropane, organic solvent and water, the organic solvent
Boiling point than the low boiling point of water, for the boiling point of extractant than the low boiling point of epoxychloropropane, the extraction phase includes epoxychloropropane
And extractant, the raffinate phase include organic solvent and water；
The raffinate phase is sent into Separation of Organic and water in the first distillation system；
The extraction phase is sent into separation epoxychloropropane and extractant in the second distillation system；
Wherein, first distillation system includes first rectifying column and Second distillation column, and the condition for controlling first rectifying column makes
The organic solvent of 1-40 weight % in the raffinate phase is detached from the tower top of the first rectifying column；
Second distillation system includes：Third distillation column and the first vacuum column, the operating condition of third distillation column include：Tower top
Pressure is normal pressure to 0.5MPaG, and theoretical cam curve 10-50, bottom temperature is 40-80 DEG C, reflux ratio 0.5-5；First is true
The operating condition of void tower includes：Tower top pressure is vacuum, and theoretical cam curve 5-30, bottom temperature is 80-150 DEG C；Control the
The condition of two rectifying columns enable steam that the tower top from the Second distillation column obtains as the third distillation column and
Whole heat sources of the first rectifying column；
Operating condition in the first rectifying column includes：Tower top pressure is normal pressure to 1.0MPaG, theoretical cam curve 5-60,
Bottom temperature is 40-120 DEG C, reflux ratio 0.5-3；
Operating condition in the Second distillation column includes：Tower top pressure is 0.3-4.0MPaG, theoretical cam curve 5-60, tower
Kettle temperature degree is 110-200 DEG C, reflux ratio 0.5-3.
2. according to the method described in claim 1, wherein, the condition for controlling first rectifying column makes 10- in the raffinate phase
The organic solvent of 20 weight % is detached from the tower top of the first rectifying column.
3. method according to claim 1 or 2, wherein the condition for controlling Second distillation column makes from second rectifying
The steam that the tower top of tower obtains can be as the second distillation system and whole heat sources of the first rectifying column.
4. method according to claim 1 or 2, wherein the condition for controlling Second distillation column makes from second rectifying
Organic solvent content is more than 90 weight % in the steam that the tower top of tower obtains.
5. according to the method described in claim 1, wherein, the operating condition in the Second distillation column includes：Tower top pressure is
0.5-2.0MPaG, theoretical cam curve 10-45, bottom temperature are 145-180 DEG C, reflux ratio 1-2.
6. according to the method described in claim 1, wherein, the operating condition in the first rectifying column includes：Tower top pressure is
Normal pressure to 0.5MPaG, theoretical cam curve 10-45, bottom temperature is 60-100 DEG C, reflux ratio 1-2.
7. method according to claim 1 or 2, wherein the organic solvent content in the raffinate phase is 20-70 weights
Measure %.
8. method according to claim 1 or 2, wherein carry out the epoxidation as follows：It is urged in Titanium Sieve Molecular Sieve
In the presence of agent, using organic solvent as solvent, chloropropene is contacted with hydrogen peroxide or aqueous hydrogen peroxide solution, is obtained described anti-
Answer material.
9. according to the method described in claim 8, wherein, this method further includes：After carrying out heat exchange as the steam of heat source
Condense what obtained at least partly organic solvent was used to contact with hydrogen peroxide or aqueous hydrogen peroxide solution as the chloropropene
Solvent.
10. method according to claim 1 or 2, wherein the organic solvent is methanol, and the extractant is chloropropene.
11. method according to claim 1 or 2, wherein the reaction mass contain epoxychloropropane 5-20 weight %,
Organic solvent 20-70 weight %, water 5-20 weight %, chloropropene 5-30 weight %, by-product 1-10 weight %.
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| CN109970683B (en) * | 2017-12-28 | 2020-09-22 | 中国石油化工股份有限公司 | Separation method of epoxy chloropropane |
| CN109966775B (en) * | 2017-12-28 | 2021-05-14 | 中国石油化工股份有限公司 | Liquid-liquid interface control method and application of continuous countercurrent extraction tower |
| CN108530396B (en) * | 2018-06-12 | 2022-01-04 | 山东凯泰科技股份有限公司 | Method for refining chloropropene prepared by epoxidation method |
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| CN112811976B (en) * | 2021-01-12 | 2023-01-13 | 江苏扬农化工集团有限公司 | Method for recovering solvent in aqueous phase of epoxy chloropropane prepared by hydrogen peroxide method |
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