CN109761761A - A kind of preparation method of ethoxy propylene - Google Patents
A kind of preparation method of ethoxy propylene Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of ethoxy propylene, the synthetic method for solving prior art ethoxy propylene has at high cost, and low yield, return is low, reaction route is long, by-product is more and the technical issues of polluting environment.The present invention provides a kind of preparation method of ethoxy propylene, the following steps are included: step S1: the stage of reaction, acetone gas and ethylene gas are passed through in fixed bed type reactor, modified catalyst is provided in the fixed bed type reactor, addition reaction occurs for catalysis ethylene under the conditions of 120-180 DEG C of normal pressure；Step S2: product separation by the gas after fully reacting in step S1, after condensation, separation, recovery processing, obtains ethoxy propylene sterling.The present invention is widely used in technical field of organic synthesis.
Description
Technical field
The present invention relates to technical field of organic synthesis, and in particular to a kind of preparation method of ethoxy propylene.
Background technique
2- ethoxy propylene is a kind of important medicine intermediate, at present at home gradually instead of 2- methoxy propyl
Alkene becomes the key intermediate of synthesis clarithromycin.Clarithromycin category macrolide antibiotics, for treating upper and lower respiratory tract
Infection, the illnesss such as sub-dermal soft tissue infection.
2- ethoxy propylene is simple alkene ether, and there are mainly four types of synthetic methods in the prior art: method one, with acetaldehyde
For raw material, α-chloroethyl ethyl ether, dibromoethyl ethyl ethers, the bromo- 2- ethoxy propane of 1- are obtained with ethyl alcohol, hcl reaction,
Finally obtain product.Method two obtains the chloro- 2- butenoic acid of β-through phosphorus trichloride chlorination using ethyl acetoacetate as raw material, then with second
Sodium alkoxide reacts to obtain β-ethyoxyl -2- butenoic acid, and final high temperature decarboxylation is made.Method three, it is anhydrous using p-methyl benzenesulfonic acid as catalyst
Ethyl alcohol is solvent, and acetone diethyl acetal is made using triethyl orthoformate and condensation of acetone, with phenyl methyl silicon ether etc. for liquid
Phase medium carries out high-temperature liquid-phase cracking to acetone diethyl acetal, or carries out high temperature vapor-phase thermal cracking with solid catalyst and obtain 2- second
Oxygroup propylene.Method four, DEP cracking process are cracked using 2,2- di ethyl propyl ether, slough a molecules of ethanol, obtain 2- ethoxy
Base propylene.Method one and two reaction route of method are long, and side reaction is more in reaction process, cause yield low, and the waste of generation is more, right
Environmental pollution is big.Method three and this two methods of method four are now common method, but raw material primitive nail used in both methods
The cost of triethylenetetraminehexaacetic acid ester and 2,2- di ethyl propyl ether is relatively high, need to invest it is bigger, return it is low.Therefore nowadays compel to be essential
Want a kind of investment small, response path is simple, and yield is relatively high, environmentally friendly method.
Summary of the invention
It is small the object of the invention is in order to overcome the above-mentioned deficiencies of the prior art, provide a kind of investment, response path letter
Single, yield is relatively high, the preparation method of the ethoxy propylene of environmentally friendly method.
The technical proposal for solving the technical problem of the invention is:
A kind of preparation method of ethoxy propylene, comprising the following steps:
Step S1: step S1: acetone gas and ethylene gas are passed through in fixed bed type reactor by the stage of reaction, described
Modified catalyst is provided in fixed bed type reactor, addition reaction occurs for catalysis ethylene under the conditions of 120-180 DEG C of normal pressure；
Step S2: product separation, by the gas after fully reacting in step S1, after condensation, separation, recovery processing,
Obtain ethoxy propylene sterling.
Preferably, in step S1, the mass ratio of acetone gas and ethylene gas is 0.25-2.00:1.
Preferably, in step S1, the mass ratio of acetone gas and ethylene gas is 0.52-1.04:1.
Preferably, in step S1, reaction temperature is 130-170 DEG C.
Preferably, in step S1, reaction time 0.77-1.43h.
Preferably, in step S1, reaction time 1.12-1.43h.
Preferably, modified catalyst is modified porous aluminium oxide, and aluminium oxide is gama-alumina or Alpha-alumina.
Preferably, specific surface area >=200m of modified porous aluminium oxide2/ g, porosity 60-70%.
Preferably, in step S2, it is separated into rectifying separation, condensate liquid obtained will be condensed and carry out rectifying separation, obtain 61-
64 DEG C of fraction, as ethoxy propylene sterling.
Preferably, in step S1, fixed bed type reactor is calandria type fixed bed reactor, calandria type fixed bed reactor
Interior caliber be 32mm.
Beneficial effects of the present invention:
(1) present invention provides a kind of preparation method of 2- ethoxy propylene, and this method is with the most common low price raw material of industry
Ethylene and acetone are starting material, and adding modified catalyst at appropriate temperatures makes ethylene that addition reaction occur, and a step generates second
Oxygroup propylene show that product, yield are received up to 80% with conventional triethyl orthoformate preparation process using distillation operation
Rate (77%) is compared, and is obviously improved about 3%, and simple production process is easy, the three wastes generate less, and environmental protection and energy saving meet current society
The energy-saving and environment friendly theory that can be pursued, is conducive to sustainable development.
(2) using the preparation method of ethoxy propylene of the invention, compared with prior art with following clear superiority: the
One, raw material is cheap is easy to get, and is all starting material for industrial basic low price raw material；The second, simple process, process is short, production
Equipment investment is low, with short production cycle, is easy to commercial introduction；Third, environmental-friendly, raw material availability is high.Therefore, second of the invention
The preparation method of oxygroup propylene is suitble to the production of modern industry.
Detailed description of the invention
Fig. 1 is reaction equation of the invention.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, to help the contents of the present invention are understood.
Method used in the present invention is conventional production method unless otherwise required；Used raw material, such as without special rule
It is fixed, it is conventional commercial product.
Embodiment one
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 65ml acetone and the bottled ethylene gas of 4L as reaction, is 32mm in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of jacketed2/ g, the modification of porosity 60-70% are more
After the gama-alumina of hole, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Distinguish again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened, so that shell and tube is fixed
The porous gama-alumina of modified catalyst in bed reactor is heated to 120 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 120 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 120 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 120 DEG C also by superheater, it is passed through in step S0 and heats
To 120 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 23.8ml/h with the rate of 30ml/h simultaneously
In be heated in 120 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 1.04:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 120 DEG C of temperature, addition reaction occurs, insulation reaction 1.12h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 38.71g, as ethoxy propylene sterling, calculates
Obtaining yield is 50.21%.
Embodiment two
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 65ml acetone and the bottled ethylene gas of 4L as reaction, is 32mm in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of jacketed2/ g, the modification of porosity 60-70% are more
After the gama-alumina of hole, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Distinguish again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened, so that shell and tube is fixed
The porous gama-alumina of modified catalyst in bed reactor is heated to 130 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 130 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 130 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 130 DEG C also by superheater, it is passed through in step S0 and heats
To 130 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 23.8ml/h with the rate of 30ml/h simultaneously
In be heated in 130 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 1.04:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 130 DEG C of temperature, addition reaction occurs, insulation reaction 1.12h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 60.36g, as ethoxy propylene sterling, calculates
Obtaining yield is 78.29%.
Embodiment three
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 65ml acetone and the bottled ethylene gas of 4L as reaction, is 32mm in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of jacketed2/ g, the modification of porosity 60-70% are more
After the gama-alumina of hole, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Distinguish again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened, so that shell and tube is fixed
The porous gama-alumina of modified catalyst in bed reactor is heated to 150 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 150 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 150 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 150 DEG C also by superheater, it is passed through in step S0 and heats
To 150 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 23.8ml/h with the rate of 30ml/h simultaneously
In be heated in 150 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 1.04:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 150 DEG C of temperature, addition reaction occurs, insulation reaction 1.12h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 61.31g, as ethoxy propylene sterling, calculates
Obtaining yield is 79.52%.
Example IV
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 65ml acetone and the bottled ethylene gas of 4L as reaction, is 32mm in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of jacketed2/ g, the modification of porosity 60-70% are more
After the gama-alumina of hole, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Distinguish again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened, so that shell and tube is fixed
The porous gama-alumina of modified catalyst in bed reactor is heated to 170 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 170 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 170 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 170 DEG C also by superheater, it is passed through in step S0 and heats
To 170 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 23.8ml/h with the rate of 30ml/h simultaneously
In be heated in 170 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 1.04:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 170 DEG C of temperature, addition reaction occurs, insulation reaction 1.12h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 61.71g, as ethoxy propylene sterling, calculates
Obtaining yield is 80.03%.
Embodiment five
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 65ml acetone and the bottled ethylene gas of 4L as reaction, is 32mm in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of jacketed2/ g, the modification of porosity 60-70% are more
After the gama-alumina of hole, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Distinguish again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened, so that shell and tube is fixed
The porous gama-alumina of modified catalyst in bed reactor is heated to 200 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 200 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 200 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 200 DEG C also by superheater, it is passed through in step S0 and heats
To 200 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 23.8ml/h with the rate of 30ml/h simultaneously
In be heated in 200 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 1.04:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 200 DEG C of temperature, addition reaction occurs, insulation reaction 0.77-1.43h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 52.96g, as ethoxy propylene sterling, calculates
Obtaining yield is 68.69%.
Embodiment six
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 130ml acetone and the bottled ethylene gas of 4L as reaction, is in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of 32mm jacketed2/ g, porosity 60-70% change
After the porous gama-alumina of property, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened respectively, so that shell and tube
The porous gama-alumina of modified catalyst in fixed bed reactors is heated to 170 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 170 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 170 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 170 DEG C also by superheater, it is passed through in step S0 and heats
To 170 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 47.5ml/h with the rate of 30ml/h simultaneously
In be heated in 170 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 2.08:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 170 DEG C of temperature, addition reaction occurs, insulation reaction 0.77h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 115.89g, as ethoxy propylene sterling, calculates
Obtaining yield is 75.15%.
Embodiment seven
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 162.5ml acetone and the bottled ethylene gas of 4L as reaction, is in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of 32mm jacketed2/ g, porosity 60-70% change
After the porous gama-alumina of property, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened respectively, so that shell and tube
The porous gama-alumina of modified catalyst in fixed bed reactors is heated to 170 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 170 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 170 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 170 DEG C also by superheater, it is passed through in step S0 and heats
To 170 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 59.4ml/h with the rate of 30ml/h simultaneously
In be heated in 170 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 2.6:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 170 DEG C of temperature, addition reaction occurs, insulation reaction 0.67h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 115.89g, as ethoxy propylene sterling, calculates
Obtaining yield is 75.15%.
Embodiment eight
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 65ml acetone and the bottled ethylene gas of 4L as reaction, is 32mm in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of jacketed2/ g, the modification of porosity 60-70% are more
After the gama-alumina of hole, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Distinguish again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened, so that shell and tube is fixed
The porous gama-alumina of modified catalyst in bed reactor is heated to 170 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 170 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 170 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 170 DEG C also by superheater, it is passed through in step S0 and heats
To 170 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 11.9ml/h with the rate of 30ml/h simultaneously
In be heated in 170 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 0.52:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 170 DEG C of temperature, addition reaction occurs, insulation reaction 1.43h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 61.64g, as ethoxy propylene sterling, calculates
Obtaining yield is 79.95%.
Embodiment nine
A kind of method for preparing ethoxy propylene, comprising the following steps:
S0: warm-up phase takes the raw material of 100ml acetone and the bottled ethylene gas of 4L as reaction, is in interior caliber
Specific surface area >=200m of filling 60ml in the calandria type fixed bed reactor of 32mm jacketed2/ g, porosity 60-70% change
After the porous gama-alumina of property, be first passed through 5 minutes nitrogen, by the air displacement in calandria type fixed bed reactor it is complete after；Again
Condensing unit of the heating device on calandria type fixed bed reactor with its lower end close to exit is opened respectively, so that shell and tube
The porous gama-alumina of modified catalyst in fixed bed reactors is heated to 170 DEG C；
S1: acetone soln is transported in coupling exchanger with constant-flux pump and is carried out using 65ml acetone soln by the stage of reaction
Vaporization heating, then is heated to 170 DEG C by superheater, and obtained acetone hot steam is passed through and is heated to 170 DEG C of column in step S0
In tubular fixed-bed reactor, while after ethylene gas is also heated to 170 DEG C also by superheater, it is passed through in step S0 and heats
To 170 DEG C of calandria type fixed bed reactors；
Control acetone hot steam is passed through step S0 with the rate and ethylene gas of 18.3ml/h with the rate of 30ml/h simultaneously
In be heated in 170 DEG C of calandria type fixed bed reactor, controlling acetone and ethylene mass ratio is 0.8:1, normal pressure control reaction
It is catalyzed ethylene under the conditions of 170 DEG C of temperature, addition reaction occurs, insulation reaction 1.24h is carried out, until after fully reacting；
S2: after condensation, rectifying separation: condensation is made for the product after fully reacting in step S1 for product separation
Condensate liquid carry out rectifying separation, recovery processing obtains 61-64 DEG C of fraction 94.08g, as ethoxy propylene sterling, calculates
Obtaining yield is 79.31%.
Summary is further analysed such as to the experimental data of one-embodiment of above embodiments nine and yield statistical result below
Under:
The experimental data and yield statistical form of 1 one-embodiment of embodiment nine of table are as follows:
| Embodiment | Reaction temperature DEG C | Acetone and ethylene mass ratio | Insulation reaction time h | Yield |
| Embodiment one | 120 | 1.04:1 | 1.12 | 50.21% |
| Embodiment two | 130 | 1.04:1 | 1.12 | 78.29% |
| Embodiment three | 150 | 1.04:1 | 1.12 | 79.52% |
| Example IV | 170 | 1.04:1 | 1.12 | 80.03% |
| Embodiment five | 200 | 1.04:1 | 1.12 | 68.69% |
| Embodiment six | 170 | 2.08:1 | 0.77 | 75.15% |
| Embodiment seven | 170 | 2.6:1 | 0.67 | 62.34% |
| Embodiment eight | 170 | 0.52:1 | 1.43 | 79.95% |
| Embodiment nine | 170 | 0.8:1 | 1.24 | 79.31% |
Data result is it is found that reaction temperature, third in the experimental data and yield statistical form of one-embodiment of above embodiments nine
The factors such as ketone and ethylene mass ratio, reaction insulation reaction time all have larger impact to end reaction yield.
Influence of the reaction temperature to reaction yield: acetone and Ethylene mass in the experimental data of one-embodiment of embodiment nine
It is more all the same than, reaction factors such as insulation reaction time, unlike reaction temperature be respectively 120 DEG C, 130 DEG C, 150 DEG C, 170 DEG C
With 200 DEG C, with end reaction yield comparing result it is found that reaction yield be promoted as the temperature rises, but react temperature
After degree is more than 170 DEG C, increases since high temperature generates impurity, cause yield to decline, so reaction temperature should be controlled in 120-180
DEG C, optimal 130-170 DEG C.
The change of acetone and ethylene mass ratio and reaction insulation reaction time influence reaction yield: example IV, implementation
Example six, embodiment seven, embodiment eight, reaction temperature is all the same in the experimental data of embodiment nine, acetone and ethylene mass ratio and
The change of reaction insulation reaction time is on reaction yield the result is that influential, and acetone and ethylene mass ratio become larger or become smaller, i.e.,
Ethylene is in shortage or this excessive reaction of ethylene in there is different degrees of side reaction to generate, cause reaction yield to reduce；And its
The insulation reaction time, too short reaction raw materials conversion was insufficient, and insulation reaction overlong time also has side reaction generation, there is the poly- of itself
Reaction is closed, will also result in reaction yield reduction, so acetone and ethylene mass ratio should be controlled in 0.25-2.00:1, it is optimal
Acetone and ethylene mass ratio are 0.52-1.04:1；The insulation reaction time is 0.77-1.43h, and the peak optimization reaction time is 1.12-
1.43h。
Reaction structure formula of the invention as shown in Figure 1, in the preparation method of ethoxy propylene of the invention, ethylene is being urged
Under the catalytic action of agent, the ketone attack of enolization is by the polarized double bond of hydrogen ion, and double bond is opened and acetone forms chemistry
Key, as ethoxy propylene.Acetone gasification, ethylene gas are warmed to same temperature, then allow ethylene gas and acetone
Gas allows it to react under the catalytic action of catalyst by modified catalyst.Modified catalyst will have great activity,
The effect of this reaction is catalyzed most when wherein modified catalyst is porous gama-alumina convenient for ethylene and acetone haptoreaction
It is good.
The present invention provides a kind of preparation method of 2- ethoxy propylene, and this method is with the most common low price raw material ethylene of industry
It is starting material with acetone, adding modified catalyst at appropriate temperatures makes ethylene that addition reaction occur, and a step generates ethyoxyl
Propylene obtains product using distillation operation, and yield is up to 80%, with conventional triethyl orthoformate preparation process yield
(77%) it compares, is obviously improved about 3%, and simple production process is easy, the three wastes generate less, environmental protection and energy saving meet today's society
The energy-saving and environment friendly theory of pursuit, is conducive to sustainable development.
To sum up, the present invention provides that a kind of input cost is low, and reaction time is short, the preparation of environmental-friendly 2- ethoxy propylene
Method.The process employs the reaction routes before being totally different from, with raw material of industry ethylene and acetone in modified catalyst
Under the conditions of reaction directly generate 2- ethoxy propylene.Using the preparation method of ethoxy propylene of the invention, with prior art phase
Than with following clear superiority: the first, raw material is cheap is easy to get, and is all starting material for industrial basic low price raw material；The second,
Simple process, process is short, and investment of production equipment is low, with short production cycle, is easy to commercial introduction；Third, environmental-friendly, raw material utilize
Rate is high.Therefore, the preparation method of ethoxy propylene of the invention is suitble to the production of modern industry.
The above is only the embodiment of the present invention, such as specific surface area >=200m2The modification of/g, porosity 60-70%
Porous catalyst；Modified porous aluminium oxide is gama-alumina or Alpha-alumina, and ethoxy-c of the invention may be implemented
The preparation method of alkene.
Only as described above, only specific embodiments of the present invention, when the model that cannot be limited the present invention with this and implement
It encloses, it is all according to equivalent changes and modifications within the scope of the patent application of the present invention, it is all covered by the present invention.
Claims (10)
1. a kind of preparation method of ethoxy propylene, which comprises the following steps:
Step S1: acetone gas and ethylene gas are passed through in fixed bed type reactor by the stage of reaction, the fixed-bed type reaction
Modified catalyst is provided in device, addition reaction occurs for catalysis ethylene under the conditions of 120-180 DEG C of normal pressure；
Step S2: product separation obtains the gas after fully reacting in step S1 after condensation, separation, recovery processing
Ethoxy propylene sterling.
2. a kind of preparation method of ethoxy propylene according to claim 1, which is characterized in that in step S1, described third
The mass ratio of ketone gas and ethylene gas is 0.25-2.00:1.
3. a kind of preparation method of ethoxy propylene according to claim 2, which is characterized in that in step S1, described third
The mass ratio of ketone gas and ethylene gas is 0.52-1.04:1.
4. a kind of preparation method of ethoxy propylene according to claim 1, which is characterized in that described anti-in step S1
Answering temperature is 130-170 DEG C.
5. a kind of preparation method of ethoxy propylene according to claim 1, which is characterized in that described anti-in step S1
It is 0.77-1.43h between seasonable.
6. a kind of preparation method of ethoxy propylene according to claim 5, which is characterized in that described anti-in step S1
It is 1.12-1.43h between seasonable.
7. a kind of preparation method of ethoxy propylene according to claim 1, which is characterized in that the modified catalyst is
Modified porous aluminium oxide, the aluminium oxide are gama-alumina or Alpha-alumina.
8. a kind of preparation method of ethoxy propylene according to claim 7, which is characterized in that the modified porous oxygen
Change specific surface area >=200m of aluminium2/ g, porosity 60-70%.
9. a kind of preparation method of ethoxy propylene according to claim 1, which is characterized in that in step S2, described point
Condensation condensate liquid progress rectifying separation obtained is obtained into 61-64 DEG C of fraction, as ethoxy propylene from for rectifying separation
Sterling.
10. a kind of preparation method of ethoxy propylene according to claim 1, which is characterized in that described solid in step S1
Determining hearth reactor is calandria type fixed bed reactor, and the interior caliber of the calandria type fixed bed reactor is 32mm.
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| CN110330412A (en) * | 2019-07-19 | 2019-10-15 | 安徽威驰化工有限责任公司 | A kind of reaction cleavage method of 2- ethyoxyl propylene |
| CN111701539A (en) * | 2020-06-28 | 2020-09-25 | 安徽威驰化工有限责任公司 | 2-ethoxy propylene bed reactor and reaction method |
| CN115490575A (en) * | 2022-10-13 | 2022-12-20 | 辽宁惠风生物医药科技有限公司 | Preparation method of 2-ethoxypropylene |
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| CN1660742A (en) * | 2004-12-30 | 2005-08-31 | 浙江大学 | New technique for synthesizing 2-alkoxyl propylene |
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| CN1660742A (en) * | 2004-12-30 | 2005-08-31 | 浙江大学 | New technique for synthesizing 2-alkoxyl propylene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330412A (en) * | 2019-07-19 | 2019-10-15 | 安徽威驰化工有限责任公司 | A kind of reaction cleavage method of 2- ethyoxyl propylene |
| CN111701539A (en) * | 2020-06-28 | 2020-09-25 | 安徽威驰化工有限责任公司 | 2-ethoxy propylene bed reactor and reaction method |
| CN115490575A (en) * | 2022-10-13 | 2022-12-20 | 辽宁惠风生物医药科技有限公司 | Preparation method of 2-ethoxypropylene |
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