CN114315533A - One-step preparation method of high molecular weight alcohol ether - Google Patents
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Abstract
The invention relates to a preparation method of alcohol ether, in particular to a one-step preparation method of high molecular weight alcohol ether. Alkyl alcohol and a catalyst are uniformly mixed to form a homogeneous catalyst alkyl alcohol solution, and then the homogeneous catalyst alkyl alcohol solution and ethylene oxide or propylene oxide enter the microchannel reactor 1 through a feed pump respectively to react; then the mixture enters a micro-channel reactor 2 through a dealcoholization tower and a monoalcohol ether extraction tower, so that the monoalcohol ether reacts with ethylene oxide or propylene oxide to generate glycol ether or glycol ether; then the high-purity triol ether is extracted through a light component removing tower, a diol ether extraction tower and a triol ether extraction tower. The method utilizes the characteristic of good heat transfer and mass transfer performance of the microchannel reactor, realizes the preparation of the molecular weight alcohol ether by one step by accurately controlling the temperature and controlling the molar ratio of materials, simplifies a complex reaction system for producing the molecular weight alcohol ether, and reduces the safety risk brought by production.
Description
Technical Field
The invention relates to a preparation method of alcohol ether, in particular to a one-step preparation method of high molecular weight alcohol ether.
Background
The glycol ethers comprise glycol ethers and propylene glycol ethers, the glycol ethers are prepared by ring-opening addition reaction of alkylene oxides (EO, PO) and various low-carbon alcohols ROH, and comprise glycol ethers with various molecular weights such as ethylene glycol monoether, diethylene glycol monoether, triethylene glycol monoether and the like; the propylene glycol ethers are prepared by ring-opening addition reaction of Propylene Oxide (PO) and various low-carbon alcohols ROH, and comprise multi-molecular-weight alcohol ethers such as propylene glycol monoether, dipropylene glycol monoether, tripropylene glycol monoether and the like; among them, ROH is methanol, ethanol, propanol, allyl alcohol, butanol, hexanol, octanol, phenol, etc., which have both alcohol and ether properties, and dissolve cellulose such as cellulose nitrate, which is known in the industry as cellosolve.
Chinese patent CN111635298A discloses a method and a device for preparing glycol ether, wherein materials are preheated and then sequentially pass through a microchannel reactor, an enhanced heat transfer mixing tube reactor and a heat preservation aging reaction unit, although the method is better than the traditional kettle type reaction in mass and heat transfer, the reaction flow is overlong, and the total reaction time is still longer than 45 min.
Chinese patent CN109134212A discloses a method for preparing dipropylene glycol methyl ether by continuous reaction, which comprises the steps of mixing and preheating 2-methoxy-1-propanol, propylene oxide and a strong base catalyst, then sending into a pipeline reactor for etherification reaction, and finally collecting a target product dipropylene glycol methyl ether from a reaction product. The reaction time is longer and is 1-4h, the molar ratio of the 2-methoxy-1-propanol to the alkylene oxide is 3-8:1, and the subsequent treatment is troublesome.
The reaction of lower alcohols with alkylene oxides (EO and PO) is a strongly exothermic reaction, which creates a greater safety hazard if the heat generated by the reaction cannot be removed in time, and therefore the heat transfer performance requirements of the reactor are extremely high when the production associated with the reaction is carried out. In addition, if the mass transfer effect is poor in the reaction process, more impurities are generated in the reaction of the materials in the flowing process. Taking Propylene Oxide (PO) as an example, one molecule of PO reacts with one molecule of methanol to generate propylene glycol methyl ether, and the heat release amount is 102.9 kj/mol; the 2 molecule PO reacts with one molecule of methanol to generate dipropylene glycol methyl ether with the heat release of 218.4 kj/mol, and the 3 molecule PO reacts with one molecule of methanol to generate tripropylene glycol methyl ether with the heat release of-328.5 kj/mol. It is understood that the higher the molar ratio of alkylene oxide to alcohol, the higher the heat output, and the higher the heat removal capacity of the system.
As is clear from the above patents and the analysis of the heat release amount, the glycol ether having a large molecular weight or the propylene glycol ether having a large molecular weight cannot be produced in one step due to the limitation of the heat transfer capacity of the existing equipment, and the existing diethylene glycol ether, triethylene glycol ether, dipropylene glycol ether and tripropylene glycol ether are mostly obtained by purifying a small amount of by-products in the production process of ethylene glycol methyl ether or propylene glycol methyl ether. The method disclosed in chinese patent CN109134212A is slow in reaction and low in production efficiency, and only the presently disclosed technology can be adopted to obtain a large amount of alcohol ethers with multiple molecular weights.
In addition, in the process of synthesizing propylene glycol methyl ether by reacting propylene oxide and methanol, a certain amount of byproduct 2-methoxy-1-propanol is always generated, the product has certain toxicity and low market value, and needs to be processed on line to be converted into a useful product, and if the product can be converted into dipropylene glycol methyl ether on line, the economic value can be greatly improved.
Therefore, the following major problems exist with respect to the preparation of existing ethylene glycol ethers or propylene glycol ethers:
firstly, limited by the mass transfer and heat transfer capacity of the existing device, the alkylene oxide cannot be greatly excessive, and one-step method synthesis and regulation for producing the alcohol ether with the high molecular weight, such as ethylene glycol methyl ether, diethylene glycol methyl ether and triethylene glycol methyl ether or propylene glycol methyl ether, dipropylene glycol methyl ether and tripropylene glycol methyl ether, cannot be used in a reactor;
secondly, the reaction time of the existing glycol ether or propylene glycol ether process is still long, and the reaction flow is still complex;
and in the synthesis of propylene glycol methyl ether, a byproduct 2-methoxy-1 propanol is generated, and the product has toxicity and low market value and needs to be treated on line.
For convenience of description, it is specified that ethylene glycol monomethyl ether or propylene glycol monomethyl ether and its isomer 2-methoxy-1-propanol may be simply referred to as a glycol ether, diethylene glycol monomethyl ether or dipropylene glycol monomethyl ether may be simply referred to as a glycol ether, and triethylene glycol monomethyl ether or tripropylene glycol monomethyl ether may be simply referred to as a glycol ether.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides the one-step preparation method of the molecular weight alcohol ether, which simplifies the complex reaction system for producing the molecular weight alcohol ether and reduces the safety risk brought by production by accurately controlling the temperature and controlling the molar ratio of materials.
In order to achieve the above object, the present invention is realized by the following technical scheme, a one-step preparation method of a polyol ether, comprising the following steps:
(1) alkyl alcohol and a catalyst are uniformly mixed to form a homogeneous alkyl alcohol catalyst solution, and then the homogeneous alkyl alcohol catalyst solution and ethylene oxide or propylene oxide enter the microchannel reactor 1 through a feed pump respectively to react;
(2) feeding the material from the microchannel reactor 1 into a dealcoholization tower, feeding the tower bottom liquid of the dealcoholization tower into a monoalcohol ether extraction tower, and extracting high-purity monoalcohol ether from the tower top of the monoalcohol ether extraction tower; the tower top liquid of the dealcoholization tower circularly enters the micro-channel reactor 1;
(3) the tower bottom liquid of the mono-alcohol ether extraction tower enters a micro-channel reactor 2, and in the micro-channel reactor 2, the mono-alcohol ether reacts with ethylene oxide or propylene oxide to generate glycol ether or triol ether;
(4) the generated glycol ether or triol ether from the micro-channel reactor 2 enters a lightness-removing tower, the tower bottom material of the lightness-removing tower enters a glycol ether extraction tower, and high-purity glycol ether is extracted from the tower top of the glycol ether extraction tower; the material at the top of the light component removal tower and the supplemented ethylene oxide or propylene oxide circularly enter the micro-channel reactor 2;
(5) the tower bottom liquid of the glycol ether extraction tower enters a triol ether extraction tower, high-purity triol ether is extracted from the tower top material of the triol ether extraction tower, alcohol ether with higher molecular weight is obtained by distilling the tower bottom material, and a product at the bottom of a distillation kettle is a solid catalyst and can be uniformly mixed with alkyl alcohol to be prepared and enter the microchannel reactor 1 for recycling.
Preferably, in the homogeneous catalyst alkyl alcohol solution in the step (1), the catalyst is any one of sodium methoxide, potassium methoxide, sodium tert-butoxide, potassium tert-butoxide, sodium hydroxide and potassium hydroxide, and the alkyl alcohol is any one of methanol, ethanol, propanol, isopropanol and butanol, and the content of the catalyst is 0.1-0.35% of the homogeneous catalyst alkyl alcohol solution by weight percent.
Preferably, in the step (1), the molar ratio of the alkyl alcohol to the ethylene oxide or the propylene oxide is 2.5:1 to 1: 3.5.
Preferably, in the step (1), the reaction temperature in the microchannel reactor 1 is 135-175 ℃, preferably 145-155 ℃; the reaction pressure is 1500KPa-3500KPa, preferably 2500KPa-3000 KPa; the reaction residence time is 2-15min, preferably 4-7.5 min.
Preferably, in the step (2), the operation pressure of the dealcoholization tower is normal pressure, the tower top temperature is 60-64.5 ℃, and the tower kettle temperature is 122-140 ℃; in the step (3), the operating pressure of the pure ether extraction tower is 10KPa to 20KPa, the temperature at the top of the tower is 59 ℃ to 60 ℃, and pure ether with the purity of more than 99.5 percent is extracted from the top of the tower.
Preferably, in the step (3), the molar ratio of the ethylene oxide or the propylene oxide to the mono-alcohol ether is 1:1.1-1:2.0, the reaction pressure is 2500KPa-3000KPa, the reaction temperature is 150-170 ℃, and the reaction time is 4-8 min.
Preferably, in the step (4), the operating pressure of the light component removal tower is 10KPa to 101.3KPa of absolute pressure; the operation pressure of the glycol ether extraction tower is 0.8KPa to 0.92KPa, the temperature at the top of the tower is 64 ℃ to 66 ℃, and the glycol ether with the purity of more than 99.5 percent is obtained at the top of the tower.
Preferably, in the step (5), the operation pressure of the triol ether extraction tower is 0.5KPa to 1KPa absolute pressure.
Preferably, in the step (1), ethylene oxide or propylene oxide is fed simultaneously from a plurality of feed ports of the microchannel reactor 1, so that heat cannot be removed in time, and the yield of the main product can be increased.
Compared with the prior art, the invention has the following outstanding advantages and positive effects:
1. the method utilizes the characteristic of good heat transfer and mass transfer performance of the microchannel reactor, realizes the preparation of the molecular weight alcohol ether by one step through accurately controlling the temperature and controlling the molar ratio of materials, simplifies a complex reaction system for producing the molecular weight alcohol ether, reduces the safety risk brought by production, and can adjust the distribution of products by adjusting reaction process conditions according to the market quotation of the products to increase the benefit.
2. Ethylene oxide or propylene oxide is fed from a plurality of feed inlets of the microchannel reactor 1 simultaneously, which can prevent heat from being removed in time and increase the yield of the main product.
3. In the reaction product obtained by the one-step preparation method, the selectivity of the alcohol ether is 20-100 percent of that of the mono-alcohol ether, the selectivity of the glycol ether product is 0-50 percent, and the selectivity of the triol ether product is 0-40 percent.
Drawings
FIG. 1 is a flow chart of the production process of the present invention;
reference numbers in the figures: 1-catalyst methanol solution tank; 2-microchannel reactor 1; 3-dealcoholizing tower; a 4-monoalcohol ether extraction tower; 5-microchannel reactor 2; 6-light component removal tower; a 7-glycol ether extraction column; 8-triol ether extraction tower.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments and the accompanying drawings of the specification.
A one-step preparation method of a molecular weight alcohol ether comprises the following steps:
(1) alkyl alcohol and a catalyst are uniformly mixed to form a homogeneous alkyl alcohol catalyst solution, and then the homogeneous alkyl alcohol catalyst solution and ethylene oxide or propylene oxide enter the microchannel reactor 1 through a feed pump respectively to react;
(2) feeding the material from the microchannel reactor 1 into a dealcoholization tower, feeding the tower bottom liquid of the dealcoholization tower into a monoalcohol ether extraction tower, and extracting high-purity monoalcohol ether from the tower top of the monoalcohol ether extraction tower; the tower top liquid of the dealcoholization tower circularly enters the micro-channel reactor 1;
(3) the tower bottom liquid of the mono-alcohol ether extraction tower enters a micro-channel reactor 2, and in the micro-channel reactor 2, the mono-alcohol ether reacts with ethylene oxide or propylene oxide to generate glycol ether or triol ether;
(4) the generated glycol ether or triol ether from the micro-channel reactor 2 enters a lightness-removing tower, the tower bottom material of the lightness-removing tower enters a glycol ether extraction tower, and high-purity glycol ether is extracted from the tower top of the glycol ether extraction tower; the material at the top of the light component removal tower and the supplemented ethylene oxide or propylene oxide circularly enter the micro-channel reactor 2;
(5) the tower bottom liquid of the glycol ether extraction tower enters a triol ether extraction tower, high-purity triol ether is extracted from the tower top material of the triol ether extraction tower, alcohol ether with higher molecular weight is obtained by distilling the tower bottom material, and a product at the bottom of a distillation kettle is a solid catalyst and can be uniformly mixed with alkyl alcohol to be prepared and enter the microchannel reactor 1 for recycling.
Example 1
In the microchannel reactor 1: feeding ethylene oxide in three sections, wherein the head of the microchannel reactor 1 is fed with 4mol, the 1/4 section of the microchannel reactor 1 is fed with 3mol, and the 2/4 section of the microchannel reactor 1 is fed with 3 mol; feeding 12mol of catalyst alkyl alcohol homogeneous solution, wherein the alkyl alcohol is methanol, the catalyst is sodium hydroxide, and the mass fraction of the catalyst in the methanol is 0.1%; the reaction temperature is 150 ℃, the pressure is 3MPa, and the reaction time is 5 min.
The discharge composition of the micro-channel reactor 1 is as follows: ethylene glycol monomethyl ether 92.14%, methanol 7.81%, ethylene oxide 0.05%.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: ethylene oxide: 0.64%,; 99.36 percent of methanol. The top of the single alcohol ether extraction tower is composed of ethylene glycol monomethyl ether with the content of more than 99.8 percent. Example 2
In the microchannel reactor 1: ethylene oxide feed 16 mol; feeding 10mol of methanol in the catalyst alkyl alcohol homogeneous solution, wherein the alkyl alcohol is methanol, the catalyst is potassium hydroxide, and the mass fraction of the catalyst in the methanol is 0.15%; the reaction temperature was 150 ℃. The pressure is 3MPa, and the reaction time is 10min
The discharge composition of the micro-channel reactor 1 is as follows: 4.30% of ethylene oxide, 40.82% of ethylene glycol methyl ether, 46.87% of diethylene glycol methyl ether and 8.01% of triethylene glycol methyl ether.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the ethylene oxide content is greater than 99.9%. The top of the single alcohol ether extraction tower is composed of glycol methyl ether with the content more than 99.8 percent;
the operation pressure of the glycol ether extraction tower is 0.81KPa, the temperature at the top of the tower is 60 ℃, and the content of diethylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 104 ℃, and the content of the triethylene glycol methyl ether is more than 99.6%.
Example 3
In the microchannel reactor 1: feeding 10mol of ethylene oxide; 15mol of catalyst alkyl alcohol homogeneous solution is fed, wherein the alkyl alcohol is methanol, the catalyst is potassium methoxide, and the mass fraction of the catalyst in the methanol is 0.2%; the reaction temperature was 150 ℃. The pressure is 3MPa, and the reaction time is 10min
The discharge composition of the micro-channel reactor 1 is as follows: 20.06% of methanol, 70.21% of ethylene glycol methyl ether, 9.13% of diethylene glycol methyl ether and 0.5942% of triethylene glycol methyl ether.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the ethylene oxide content is greater than 99.9%. The top of the single alcohol ether extraction tower is composed of glycol methyl ether with the content more than 99.9 percent;
the operation pressure of the glycol ether extraction tower is 0.81KPa, the temperature at the top of the tower is 60 ℃, and the content of diethylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 104 ℃, and the content of the triethylene glycol methyl ether is more than 99.6%. Example 4
In the microchannel reactor 1: feeding propylene oxide in three sections, wherein the head of a micro-channel reactor 1 is 4mol, the 11/4 sections of the micro-channel reactor are 3mol, and the 12/4 sections of the micro-channel reactor are 3 mol; 15mol of catalyst alkyl alcohol homogeneous solution is fed, wherein the alkyl alcohol is methanol, the catalyst is sodium methoxide, and the mass fraction of the catalyst in the methanol is 0.35%; the reaction temperature was 170 ℃. The pressure is 3MPa, and the reaction time is 5min
The discharge composition of the micro-channel reactor 1 is as follows: propylene oxide: 1.094%, propylene glycol methyl ether: 79.88%%, 2-methoxy-1-propanol: 3.328 percent.
Microchannel reactor 2 feed: propylene oxide: 0.392mol, 2-methoxy-1-propanol: 0.784mol, the reaction temperature is 170 ℃, the pressure is 3MPa, and the reaction time is 7min
Discharging from the microchannel reactor 2: propylene oxide: 0.0244%, 2-methoxy-1-propanol: 38.94%, dipropylene glycol methyl ether: 59.08%, tripropylene glycol methyl ether: 1.73 percent.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the content of the propylene oxide is more than 99.9 percent. The top of the single alcohol ether extraction tower has a propylene glycol methyl ether content of more than 99.9 percent;
the operating pressure of the lightness-removing column is 10KPa, and the temperature at the top of the column is 72 ℃.
The operation pressure of the glycol ether extraction tower is 0.82KPa, the temperature at the top of the tower is 64 ℃, and the content of dipropylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 112 ℃, and the content of the tripropylene glycol methyl ether is more than 99.6 percent.
Example 5
In the microchannel reactor 1: feeding 10mol of propylene oxide at the head of the microchannel reactor 1; feeding 12mol of catalyst alkyl alcohol homogeneous solution, wherein the alkyl alcohol is methanol, the catalyst is sodium methoxide, and the mass fraction of the catalyst in the methanol is 0.1%; the reaction temperature is 170 ℃, the pressure is 3MPa, and the reaction time is 15min
The discharge composition of the micro-channel reactor 1 is as follows: propylene glycol methyl ether: 76.98%%, 2-methoxy-1-propanol: 3.381%, dipropylene glycol methyl ether: 11.13%, tripropylene glycol methyl ether: 0.356 percent.
Microchannel reactor 2 feed: propylene oxide: 0.255mol, 2-methoxy-1-propanol: 0.51mol, the reaction temperature is 170 ℃, the pressure is 3MPa, and the reaction time is 10min
Discharging from the microchannel reactor 2: 2-methoxy-1-propanol: 38.57%, dipropylene glycol methyl ether: 59.7%, tripropylene glycol methyl ether: 1.73 percent.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the content of the propylene oxide is more than 99.9 percent. The top of the single alcohol ether extraction tower has a propylene glycol methyl ether content of more than 99.9 percent;
the operating pressure of the lightness-removing column is 10KPa, and the temperature at the top of the column is 72 ℃.
The operation pressure of the glycol ether extraction tower is 0.82KPa, the temperature at the top of the tower is 64 ℃, and the content of dipropylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 112 ℃, and the content of the tripropylene glycol methyl ether is more than 99.6 percent.
Example 6
In the microchannel reactor 1: feeding 10mol of propylene oxide at the head of the microchannel reactor 1; 15mol of catalyst alkyl alcohol homogeneous solution is fed, wherein the alkyl alcohol is methanol, the catalyst is sodium methoxide, and the mass fraction of the catalyst in the methanol is 0.1%; the reaction temperature is 120 ℃, the pressure is 3MPa, and the reaction time is 5min
The discharge composition of the micro-channel reactor 1 is as follows: propylene glycol methyl ether: 65.88%%, 2-methoxy-1-propanol: 4.014%, methanol: 20.42%, propylene oxide: 9.7 percent.
Microchannel reactor 2 feed: propylene oxide: 0.4728mol, 2-methoxy-1-propanol: 0.9456mol, reaction temperature of 170 ℃, pressure of 3MPa and reaction time of 10min
Discharging from the microchannel reactor 2: 2-methoxy-1-propanol: 38.66%, dipropylene glycol methyl ether: 59.38%, tripropylene glycol methyl ether: 1.947 percent.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the content of the propylene oxide is more than 99.9 percent. The top of the single alcohol ether extraction tower has a propylene glycol methyl ether content of more than 99.9 percent;
the operating pressure of the lightness-removing column is 10KPa, and the temperature at the top of the column is 72 ℃.
The operation pressure of the glycol ether extraction tower is 0.82KPa, the temperature at the top of the tower is 64 ℃, and the content of dipropylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 112 ℃, and the content of the tripropylene glycol methyl ether is more than 99.6 percent.
Comparative example 1
Feeding 10mol of ethylene oxide at the head of the microchannel reactor 1; feeding 12mol of catalyst alkyl alcohol homogeneous solution, wherein the alkyl alcohol is methanol, the catalyst is sodium hydroxide, and the mass fraction of the catalyst in the methanol is 0.1%; the reaction temperature is 150 ℃, the pressure is 3MPa, and the reaction time is 5 min.
The discharge composition of the micro-channel reactor 1 is as follows: methanol 8.816%, ethylene oxide: 0.1068%, ethylene glycol methyl ether: 87.43%, diethylene glycol methyl ether: 3.64 percent.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the ethylene oxide content is greater than 99.9%. The top of the single alcohol ether extraction tower is composed of glycol methyl ether with the content more than 99.9 percent;
the operation pressure of the glycol ether extraction tower is 0.81KPa, the temperature at the top of the tower is 60 ℃, and the content of diethylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 104 ℃, and the content of the triethylene glycol methyl ether is more than 99.6%.
Comparative example 2
In the microchannel reactor 1: feeding 10mol of propylene oxide at the head of the microchannel reactor 1; 15mol of catalyst alkyl alcohol homogeneous solution is fed, wherein the alkyl alcohol is methanol, the catalyst is sodium methoxide, and the mass fraction of the catalyst in the methanol is 0.35%; the reaction temperature is 170 ℃, the pressure is 3MPa, and the reaction time is 5min
The discharge composition of the micro-channel reactor 1 is as follows: propylene oxide: 0.11%, propylene glycol methyl ether: 76.42%, 2-methoxy-1-propanol: 2.54%, methanol: 16.18%, dipropylene glycol methyl ether: 4.74 percent.
Microchannel reactor 2 feed: propylene oxide: 0.3mol, 2-methoxy-1-propanol: 0.6mol, the reaction temperature is 170 ℃, the pressure is 3MPa, and the reaction time is 10min
Discharging from the microchannel reactor 2: propylene oxide: 0.244% mol, 2-methoxy-1-propanol: 38.94%, dipropylene glycol methyl ether: 59.08%, tripropylene glycol methyl ether: 1.73 percent.
The dealcoholization tower is at normal pressure, and the tower top material composition is as follows: the content of the propylene oxide is more than 99.9 percent. The top of the single alcohol ether extraction tower has a propylene glycol methyl ether content of more than 99.9 percent;
the operating pressure of the lightness-removing column is 10KPa, and the temperature at the top of the column is 72 ℃.
The operation pressure of the glycol ether extraction tower is 0.82KPa, the temperature at the top of the tower is 64 ℃, and the content of dipropylene glycol methyl ether at the top of the tower is more than 99.6 percent.
The operation pressure of the triol ether extraction tower is 0.54KPa, the tower top temperature is 112 ℃, and the content of the tripropylene glycol methyl ether is more than 99.6 percent.
Claims (10)
1. The one-step preparation method of the molecular weight alcohol ether is characterized by comprising the following steps:
(1) alkyl alcohol and a catalyst are uniformly mixed to form a homogeneous alkyl alcohol catalyst solution, and then the homogeneous alkyl alcohol catalyst solution and ethylene oxide or propylene oxide enter the microchannel reactor 1 through a feed pump respectively to react;
(2) feeding the material from the microchannel reactor 1 into a dealcoholization tower, feeding the tower bottom liquid of the dealcoholization tower into a monoalcohol ether extraction tower, and extracting high-purity monoalcohol ether from the tower top of the monoalcohol ether extraction tower; the tower top liquid of the dealcoholization tower circularly enters the micro-channel reactor 1;
(3) the tower bottom liquid of the mono-alcohol ether extraction tower enters a micro-channel reactor 2, and in the micro-channel reactor 2, the mono-alcohol ether reacts with ethylene oxide or propylene oxide to generate glycol ether or triol ether;
(4) the generated glycol ether or triol ether from the micro-channel reactor 2 enters a lightness-removing tower, the tower bottom material of the lightness-removing tower enters a glycol ether extraction tower, and high-purity glycol ether is extracted from the tower top of the glycol ether extraction tower; the material at the top of the light component removal tower and the supplemented ethylene oxide or propylene oxide circularly enter the micro-channel reactor 2;
(5) the tower bottom liquid of the glycol ether extraction tower enters a triol ether extraction tower, high-purity triol ether is extracted from the tower top material of the triol ether extraction tower, alcohol ether with higher molecular weight is obtained by distilling the tower bottom material, and a product at the bottom of a distillation kettle is a solid catalyst and can be uniformly mixed with alkyl alcohol to be prepared and enter the microchannel reactor 1 for recycling.
2. The one-step method for preparing a multi-molecular-weight alcohol ether according to claim 1, wherein in the catalyst alkyl alcohol homogeneous solution of step (1), the catalyst is any one of sodium methoxide, potassium methoxide, sodium tert-butoxide, potassium tert-butoxide, sodium hydroxide and potassium hydroxide, the alkyl alcohol is any one of methanol, ethanol, propanol, isopropanol and butanol, and the content of the catalyst is 0.1-0.35% by weight of the catalyst alkyl alcohol homogeneous solution.
3. The one-step process for producing a high molecular weight alcohol ether according to claim 1 or 2, wherein in the step (1), the molar ratio of the alkyl alcohol to the ethylene oxide or propylene oxide is 2.5:1 to 1: 3.5.
4. The one-step process for preparing a molecular weight polyol ether as claimed in claim 1, wherein in said step (1), the reaction temperature in the microchannel reactor 1 is 135-175 ℃, the reaction pressure is 1500-3500 KPa absolute pressure, and the reaction residence time is 2-15 min.
5. The one-step process for preparing a high molecular weight polyol ether according to claim 1, wherein in said step (2), the operating pressure of the dealcoholization column is atmospheric pressure, the temperature at the top of the column is 60 ℃ to 64.5 ℃, and the temperature at the bottom of the column is 122 ℃ to 140 ℃; in the step (3), the operating pressure of the pure ether extraction tower is 10KPa to 20KPa, the temperature at the top of the tower is 59 ℃ to 60 ℃, and pure ether with the purity of more than 99.5 percent is extracted from the top of the tower.
6. The one-step process for preparing polyol ether according to claim 1, wherein in the step (3), the molar ratio of ethylene oxide or propylene oxide to the monomer ether is 1:1.1-1:2.0, the reaction pressure is 2500KPa-3000KPa, the reaction temperature is 150 ℃ to 170 ℃, and the reaction time is 4-8 min.
7. The one-step process for preparing a high molecular weight polyol ether according to claim 1, wherein in said step (4), the operating pressure of the lightness-removing column is 10KPa to 101.3KPa in absolute pressure; the operation pressure of the glycol ether extraction tower is 0.8KPa to 0.92KPa, the temperature at the top of the tower is 64 ℃ to 66 ℃, and the glycol ether with the purity of more than 99.5 percent is obtained at the top of the tower.
8. The one-step process for producing a molecular weight polyol ether according to claim 1, wherein in said step (5), the operation pressure of the triol ether production column is 0.5KPa to 1KPa absolute.
9. The one-step process for producing a high molecular weight alcohol ether according to claim 1, wherein in the step (1), ethylene oxide or propylene oxide is simultaneously fed from a plurality of feed ports of the microchannel reactor 1.
10. The one-step process for preparing a high molecular weight polyol ether according to claim 1, wherein in said step (1), the reaction temperature in the microchannel reactor 1 is 145 ℃ to 155 ℃; the reaction pressure is 2500KPa-3000 KPa; the reaction residence time is 4-7.5 min.
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| CN104326884A (en) * | 2014-09-10 | 2015-02-04 | 百川化工(如皋)有限公司 | Method for producing tripropylene glycol methyl ether |
| CN107162882A (en) * | 2017-07-04 | 2017-09-15 | 中国科学院过程工程研究所 | Spray column disc type reactor, system and technique with its production propylene glycol monomethyl ether |
| CN108033875A (en) * | 2017-12-14 | 2018-05-15 | 中国科学院过程工程研究所 | A kind of system and method for continuous production glycol ether |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326884A (en) * | 2014-09-10 | 2015-02-04 | 百川化工(如皋)有限公司 | Method for producing tripropylene glycol methyl ether |
| CN107162882A (en) * | 2017-07-04 | 2017-09-15 | 中国科学院过程工程研究所 | Spray column disc type reactor, system and technique with its production propylene glycol monomethyl ether |
| CN108033875A (en) * | 2017-12-14 | 2018-05-15 | 中国科学院过程工程研究所 | A kind of system and method for continuous production glycol ether |
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