CN111747828A - Preparation method and system of ethylene glycol monopropyl ether - Google Patents
Preparation method and system of ethylene glycol monopropyl ether Download PDFInfo
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- CN111747828A CN111747828A CN202010718384.6A CN202010718384A CN111747828A CN 111747828 A CN111747828 A CN 111747828A CN 202010718384 A CN202010718384 A CN 202010718384A CN 111747828 A CN111747828 A CN 111747828A
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- C07C41/01—Preparation of ethers
- C07C41/02—Preparation of ethers from oxiranes
- C07C41/03—Preparation of ethers from oxiranes by reaction of oxirane rings with hydroxy groups
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Abstract
The invention provides a preparation method and a system of ethylene glycol monopropyl ether, wherein the preparation method adopts the following reaction equation:
the method comprises the following steps: n-propanol and ethylene oxide react under the action of a catalyst to synthesize a crude product of ethylene glycol monopropyl ether; and carrying out reduced pressure rectification on the crude product to obtain a finished product of the ethylene glycol monopropyl ether. The preparation system comprises an addition and rectification integrated reaction kettle, the addition and rectification integrated reaction kettle comprises a reaction kettle main body, and a rectification tower is connected above the reaction kettle main body; inverse directionThe reactor main body comprises a reaction feed inlet, a reaction discharge outlet and a material steam outlet, the material steam outlet is connected with a rectification inlet of a rectification tower, the rectification tower is provided with a rectification inlet and a rectification outlet, and the rectification tower is also connected with a vacuum device. The ethylene glycol monopropyl ether prepared by the method has high purity (more than or equal to 99.8 percent) and few byproducts.
Description
Technical Field
The invention belongs to the technical field of organic compound synthesis, and particularly relates to a preparation method and a system of ethylene glycol monopropyl ether.
Background
The ethylene glycol monopropyl ether is also called propoxyethanol, is colorless transparent liquid, can be dissolved in organic solvents such as ethanol and acetone, and is miscible with water. The ethylene glycol monopropyl ether has very high dissolving capacity, and has kauri-butanol value (KB value) 5 times that of aromatic hydrocarbon solvent and 17 times that of aliphatic hydrocarbon solvent, so that ethylene glycol monopropyl ether is excellent solvent and may be used widely in nitric acid fiber, industrial paint, etc. Because the evaporation speed of the ethylene glycol monopropyl ether is relatively slow, the ethylene glycol monopropyl ether has obvious effects of improving the gloss of varnish, preventing peeling and the like, and can be used as a diluent in quick-drying paint and enamel paint to increase the adhesion of the paint to wood and metal. Meanwhile, the ethylene glycol monopropyl ether can also be used as a raw material for synthesizing a pesticide herbicide pretilachlor.
The current synthesis process route of ethylene glycol monopropyl ether is polymerization: the catalyst mainly comprises Lewis acid catalyst and alkali metal catalyst. With Lewis acids, e.g. BF3The catalyst has the characteristics of high catalytic activity and low catalytic temperature, but has more side reactions, high contents of by-products such as dioxane, diethylene glycol and the like, and is not easy to remove. The alkali metal catalyst such as KOH catalyst is easy to produce by-products such as ethylene glycol, diethylene glycol and the like, reaction products are widely distributed, the conversion rate of a target ethylene glycol monopropyl ether product is low, and the content of by-products such as diethylene glycol monopropyl ether, triethylene glycol monopropyl ether and the like is high. Therefore, the existing synthesis process route of ethylene glycol monopropyl ether is necessary to be carried outThe method is optimized to solve the problems of low purity of the synthesized crude product, more byproducts, complex working procedures, high production cost and the like in the existing synthesis process route.
In order to solve the problems of low purity of a synthetic crude product, more byproducts, complex working procedures, high production cost and the like of the existing synthetic process route, the invention provides the preparation method of the ethylene glycol monopropyl ether, which has the advantages of high catalytic selectivity, low production cost, less byproducts, easy operation and high efficiency.
Disclosure of Invention
In order to solve the problems of low purity of a synthesized crude product, more byproducts, complex working procedures, high production cost and the like in the existing synthesis process route of the ethylene glycol monopropyl ether, the invention provides a preparation method and a system of the ethylene glycol monopropyl ether, which have the advantages of high catalytic selectivity, low production cost, less byproducts, easy operation and high efficiency. The technical scheme of the invention is as follows:
the invention provides a preparation system of ethylene glycol monopropyl ether, which comprises an addition rectification integrated reaction kettle, wherein the addition rectification integrated reaction kettle comprises a reaction kettle main body, and a rectification tower is connected above the reaction kettle main body; the reaction kettle main body comprises a reaction feed inlet, a reaction discharge outlet and a material steam outlet, and the material steam outlet is connected with a rectification inlet of the rectification tower; the rectifying tower is provided with the rectifying inlet and the rectifying outlet and is also connected with a vacuum device.
Furthermore, the reaction discharge hole is connected with the reaction feed hole through a material return pipeline, and a filter and a material conveying pump are arranged on the material return pipeline.
Further, a stirring device is also arranged in the reaction kettle main body.
Further, the reaction kettle is provided with an interlayer, and the interlayer is used for introducing a temperature control medium.
Further, the preparation system also comprises a raw material storage tank and a product storage tank, wherein the raw material storage tank and the product storage tank are respectively connected with the addition rectification integrated reaction kettle.
In a second aspect, the present invention provides a method for preparing ethylene glycol monopropyl ether, which uses the above system and the following reaction equation:
the method comprises the following steps: n-propanol and ethylene oxide react under the action of a catalyst to synthesize a crude product of ethylene glycol monopropyl ether; and carrying out reduced pressure rectification on the crude product to obtain a finished product of the ethylene glycol monopropyl ether.
Further, the preparation method comprises the following steps: mixing N-propanol with a catalyst, N2Adding ethylene oxide under protection to react; separating out the catalyst after the reaction is finished to obtain a crude product of ethylene glycol monopropyl ether; and (2) carrying out reduced pressure rectification on the ethylene glycol monopropyl ether crude product, respectively collecting free n-propanol, an ethylene glycol monopropyl ether finished product and kettle bottom liquid, wherein the separated catalyst and the free n-propanol can be recycled and applied to the reaction process, and the kettle bottom liquid can be directly used for producing an n-propanol polyether surfactant product.
Further, the catalyst is one or a mixture of two of zinc methanesulfonate and zinc p-toluenesulfonate.
Further, the mass ratio of the n-propanol to the ethylene oxide is as follows: 60: (13.2-44), wherein the dosage of the catalyst is 0.3-5 per mill of the total weight of the n-propanol and the ethylene oxide.
Preferably, the reaction temperature of the n-propanol and the ethylene oxide under the catalysis of the catalyst is 110-180 ℃, and the reaction pressure is-0.05-0.60 MPa.
Further, the vacuum rectification specific process comprises the following steps: vacuumizing the addition rectification integrated reaction kettle to-0.05 MPa, controlling the vacuum degree to be constant, heating the ethylene glycol monopropyl ether crude product in the reaction kettle main body, opening rectification and condensation, controlling the temperature of the material at the bottom of the kettle to be 65-80 ℃, controlling the temperature at the top of the kettle to be 50-65 ℃, carrying out total reflux for 30min, then starting to receive the n-propanol, vacuumizing to improve the vacuum degree in the kettle to be more than or equal to-0.098 MPa when the n-propanol is completely collected and the temperature at the top of the kettle is reduced to the normal temperature; heating the materials in the kettle again, controlling the temperature of the materials at the bottom of the kettle to be 80-100 ℃, controlling the temperature at the top of the kettle to be 50-65 ℃, carrying out total reflux for 30min, and then beginning to receive ethylene glycol monopropylEther and n-propanol mixture, controlling reflux ratio at 5: 1, taking liquid during the period to detect the content of ethylene glycol monopropyl ether in the mixture, starting to receive the finished product of ethylene glycol monopropyl ether alone when the content of ethylene glycol monopropyl ether in the receiving liquid is more than or equal to 99.7 percent, stopping receiving when the purity of ethylene glycol monopropyl ether in the fraction is less than or equal to 99.7 percent, and finishing rectification. Cooling the bottom liquid to 40 + -2 deg.C, charging N2And (3) putting the kettle bottom liquid into a packaging barrel for producing other n-propanol polyether until the pressure of the reaction kettle is 0.00-0.04 MPa.
Compared with the prior art, the method has the following outstanding advantages and positive effects:
1. the ethylene glycol monopropyl ether prepared by the method has high purity (more than or equal to 99.8 percent) and few byproducts.
2. The preparation method has the advantages of simple process, mild reaction conditions, good selectivity, short production period, low energy consumption, repeated utilization of the catalyst and less three wastes.
3. The preparation system integrates the addition reaction and the rectification process, and the rectification step is directly carried out in the same reaction kettle after the addition reaction is finished, so that the equipment requirement is reduced, the cost is reduced, material transfer is not needed, the material pollution probability is avoided, and the product quality can be ensured.
Drawings
FIG. 1 is a schematic view of the structure of a production system of the present invention.
Fig. 2 is a schematic structural view of a rectifying column of the present invention.
In fig. 1 and 2, 1: ethylene oxide storage tank, 2: material transfer pump, 3: catalyst filter, 4: reaction kettle main body, 5: rectifying tower, 6: n-propanol storage tank, 7: ethylene glycol monopropyl ether reservoir, 8: vacuum pipeline, 9, branch pipeline, 10, reaction feed inlet, 11, reaction discharge outlet, 12, temperature-control steam outlet/cooling water inlet, 13, protective gas port, 14, rectification inlet, 15, rectification outlet, 16, stirring device, 17, interlayer, 18, control valve, 19, vacuumizing port on the storage tank, 20, protective gas port on the storage tank, 21, sampling port, 22, storage tank material outlet, 23, material return pipeline, 24, storage tank material inlet, 25 condenser, 26, temperature-control steam inlet/cooling water outlet, 27, check valve, 28 and vacuum device.
Detailed Description
In the description of the present invention, it is to be noted that those whose specific conditions are not specified in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present invention will now be described in further detail with reference to the following figures and specific examples, which are intended to be illustrative, but not limiting, of the invention.
Preparation of the reaction kettle before implementation: washing the main body of the reaction kettle, the rectifying tower, the raw material storage tank and the product storage tank with distilled water for several times until the main body, the rectifying tower, the raw material storage tank and the product storage tank are clean, and heating N2And blowing and drying the reaction kettle main body, the rectifying tower and the storage tank, and cooling to normal temperature for later use.
Example 1
As shown in fig. 1 and 2, this embodiment provides a system for preparing ethylene glycol monopropyl ether, including an addition rectification integrated reaction kettle, where the addition rectification integrated reaction kettle includes a reaction kettle main body 4, and a rectification tower 5 is connected above the reaction kettle main body 4. The reaction kettle main body 4 is provided with an interlayer 17 for introducing a temperature control medium, such as: steam, cooling water (the inlet and outlet of the steam and the cooling water are just opposite), oil and the like. The reaction kettle main body 4 comprises a reaction feed inlet 10, a reaction discharge outlet 11, a protective gas port 13 and a material steam outlet, the reaction feed inlet 10 and the reaction discharge outlet 11 are respectively arranged at the top and the bottom of the reaction kettle main body 4, and the reaction feed inlet 10 and the reaction discharge outlet 11 are provided with control valves 18; the reaction discharge hole 11 is also connected with the reaction feed hole 10 through a return pipe 23, and the return pipe 23 is provided with a catalyst filter 3, a material conveying pump 2 and a control valve 18. A stirring device 16 is arranged in the reaction kettle main body 4; still be equipped with pressure sensor and temperature sensor in the reation kettle main part 4, be used for monitoring reation kettle main part 4 pressure and temperature respectively. The rectifying tower 5 is a plate-type rectifying tower, the bottom of the rectifying tower is provided with a rectifying inlet 14, the top of the rectifying tower is provided with a rectifying outlet 15, the rectifying inlet 14 is connected with a material steam outlet of the reaction kettle main body 4, and a control valve 18 is arranged between the rectifying tower and the material steam outlet. The top of the rectifying tower 5 is communicated with a condenser 25, the condenser 25 is connected with a vacuum device 28 through a vacuum pipeline 8, the rectifying tower 5 is directly connected with two branch pipelines 9, one branch pipeline 9 is connected with an n-propanol storage tank 6, the other branch pipeline 9 is connected with an ethylene glycol monopropyl ether storage tank 7 and is respectively used for collecting rectified n-propanol and ethylene glycol monopropyl ether, and the two branch pipelines 9 are respectively provided with a control valve 18 and a check valve 27; the vacuum line 8 is also connected to the two branch lines 9. The n-propanol storage tank 6 and the ethylene glycol monopropyl ether storage tank 7 are both provided with a vacuumizing port 19 and a protective gas port 20, and are also provided with a material outlet 22. The vacuum line 8 is also provided with a plurality of control valves 18. The vacuum pipe 8 is also provided with a sampling port 21 for sampling and detecting the components of the distillate so as to control the purities of different distillates. The preparation system also comprises an ethylene oxide storage tank 1, wherein the ethylene oxide storage tank 1 is connected with a reaction feeding hole 10 of the reaction kettle main body 4, a vacuumizing hole 19 and a protective gas hole 20 are also arranged on the ethylene oxide storage tank 1, and a material inlet 24 and a material outlet 22 are also arranged on the ethylene oxide storage tank 1.
Example 2
Adding 60kg of N-propanol and 0.4 per mill (the proportion of the total material of N-propanol and ethylene oxide, the same below) of zinc methanesulfonate catalyst into an integrated kettle for addition reaction and rectification, vacuumizing by using a vacuum pump, and adopting N2Displacing air in the reaction kettle, after three times of displacement, the degree of evacuation is more than or equal to-0.096 MPa, heating to 100 ℃, and adding ethylene oxide while heating. The reaction temperature was controlled at 165 ℃ and 180 ℃ and the total amount of ethylene oxide added was controlled at 14 kg. After the addition of ethylene oxide, the reaction is continued while maintaining the temperature until the pressure does not decrease any more. After the reaction is finished, the temperature is reduced to 50 ℃, and N is filled2Sampling to 0.02MPa, detecting the crude product components, opening a material return pipeline, a reaction discharge hole and a reaction feed hole control valve, and filtering to recover the catalyst. After the catalyst is recovered, closing a reaction discharge port and a reaction feed port control valve, opening a control valve between the reaction kettle main body and the rectifying tower and a control valve between the rectifying tower and a vacuum pump, vacuumizing to-0.05 MPa, heating the kettle material while maintaining the vacuum degree, and opening a rectifying tower condenser; controlling the temperature of the bottom material of the kettle at 65-80 ℃, the temperature of the top of the kettle at 50-65 ℃, carrying out total reflux for 30min, opening a control valve of an n-propanol storage tank to receive the n-propanol when the total reflux time is up; controlThe vacuum degree is-0.05 MPa, the bottom material of the kettle is 65-80 ℃, when the temperature of the top of the tower is reduced to normal temperature, a control valve of an n-propanol storage tank is closed, the normal-0.098 MPa is vacuumized, the bottom material of the kettle is heated to 80-100 ℃, the temperature of the top of the tower is 50-65 ℃ for total reflux for 30min, when the total reflux time is up, the n-propanol storage tank is opened to receive the mixture of n-propanol and ethylene glycol monopropyl ether, the components of fractions are sampled and detected at random, when the content of the ethylene glycol monopropyl ether in the fractions is more than or equal to 99.7%, the control valve of the n-propanol storage tank is closed, the control valve of the ethylene glycol monopropyl ether storage tank is opened to receive the ethylene glycol monopropyl ether, the components are sampled and detected at random. Cooling the kettle bottom material to 40 ℃, and charging N2Discharging the kettle bottom material to normal pressure, and packaging for producing other n-propanol polyether. The method for detecting purity adopts gas chromatography calibrated by standard substance, the same as below.
Comparative example 1
Adding 60kg of N-propanol and 0.4 per mill of KOH catalyst into an integrated kettle for addition reaction and rectification, vacuumizing by using a vacuum pump, and adopting N2Displacing air in the reaction kettle, after three times of displacement, the degree of evacuation is more than or equal to-0.096 MPa, heating to 150 ℃, and adding ethylene oxide while heating. The reaction temperature was controlled at 165 ℃ and 180 ℃ and the total amount of ethylene oxide added was controlled at 14 kg. After the addition of ethylene oxide, the reaction is continued while maintaining the temperature until the pressure does not decrease any more. After the reaction is finished, the temperature is reduced to 50 ℃ and N is filled2Sampling to 0.02MPa, and detecting the crude product components.
Comparative example 2
60kg of n-propanol and 0.4 per mill of BF are added into the kettle integrating the addition reaction and the rectification3Diethyl ether catalyst, vacuum pumping with vacuum pump, using N2Displacing air in the reaction kettle, after three times of displacement, the degree of evacuation is more than or equal to-0.096 MPa, and after the temperature is raised to 100 ℃, adding ethylene oxide for reaction. The reaction temperature is controlled at 100 ℃ and 120 ℃, and the total addition of the ethylene oxide is controlled at 14 kg. After the addition of ethylene oxide, the reaction is continued while maintaining the temperature until the pressure does not decrease any more. After the reaction is finished, the temperature is reduced to 50 ℃ and N is filled2Sampling to 0.02MPa, and detecting the crude product components.
Effect testing experiment
Comparing the merits of different processes
Examples 3 to 7 the raw materials of n-propanol, ethylene oxide, the kind and amount of the catalyst, and the reaction temperature were adjusted, and other process conditions were the same as those in example 1; comparative examples 3 to 7 were carried out by adjusting the kinds and amounts of the raw materials of n-propanol, ethylene oxide, catalyst, and reaction temperature, and other process conditions were the same as those of the examples; the specific index of the crude product (gas chromatography using standard standards, the same applies below) is shown in Table 1.
TABLE 1 crude conditions and indices for examples and comparative examples
Note: the catalyst amount is the proportion of the total weight of the n-propanol and the ethylene oxide; the catalyst type "zinc methyldisulfonate: zinc p-toluenesulfonate ═ 1:1 mixture" means that the weight ratio of zinc methyldisulfonate to zinc p-toluenesulfonate in the mixture catalyst was 1:1, and the same applies to example 6 and example 7.
As can be seen from the data in Table 1, under the conditions of constant usage of n-propanol and ethylene oxide, consistent or similar usage of catalyst, and consistent reaction temperature, the crude product synthesized by using the catalyst (zinc methanesulfonate, zinc p-toluenesulfonate) of the invention is more preferable than the crude product synthesized by using KOH, NaOH, CH of the prior art3The content of crude ethylene glycol monopropyl ether synthesized by strong alkaline catalysts such as ONa and sodium n-propoxide is 22-150 percent higher, the difference is more obvious when the weight ratio of ethylene oxide to n-propanol is higher, the maximum ethylene glycol monopropyl ether content can be close to 149 percent (comparing example 6 with comparative example 6), and the residual unreacted n-propanol is less; the ratio of byproducts such as diethylene glycol monopropyl ether, triethylene glycol monopropyl ether and the like in the prior art is compared with KOH, NaOH and CH3The crude product synthesized by strong alkaline catalysts such as ONa, sodium n-propoxide and the like is remarkably low and is below 1/3. Inventive phase comparison of BF3Lewis acids such as diethyl etherIn the catalytic process, byproducts such as diethylene glycol monopropyl ether and triethylene glycol monopropyl ether are below 15%, and the ratio of ethylene glycol monopropyl ether to the target product is higher than 18%. It can be seen that the catalyst selection of the present invention represents a significant substantial advance over the prior art.
Secondly, the product rectification index: the indexes of the finished products after rectification in examples 2 to 7 are shown in Table 2.
TABLE 2 EXAMPLES 2 TO 7 indexes of finished products
The data in table 2 show that the content of ethylene glycol monopropyl ether in the product prepared by the rectification method is more than 99.85%, the content of n-propanol is less than 0.002%, and the content of diethylene glycol monopropyl ether is less than 0.003%.
Third, the catalyst uses mechanically
The synthesis reaction conditions are the same as those in example 3, only the type of the catalyst and the number of times of catalyst application (the amount of the catalyst recovery kit is not enough and a new catalyst is slightly supplemented) are changed, and zinc methanedisulfonate and zinc p-toluenesulfonate are taken as examples for application and are not limited to the above actually. The crude specific indices are shown in tables 3 and 4.
TABLE 3 Zinc methyldi-sulfonate catalyst application parameters and crude product index
TABLE 4 application parameters and crude index of zinc p-toluenesulfonate catalyst
The data in tables 3 and 4 show that the catalyst of the invention can be repeatedly used for more than 8 times without obvious reduction of the catalytic effect, which indicates that the catalyst of the invention can be recycled.
Fourthly, the normal propyl alcohol is recycled
The synthesis reaction conditions are the same as those in example 3, and the method is not limited to the above only by changing the application times of the n-propanol (the recovery application amount of the n-propanol is not enough, and the new n-propanol is supplemented to the same amount). The specific index of the crude product is shown in Table 5.
TABLE 5 n-propanol parameters and crude index
The data in table 5 show that the recovered n-propanol of the present invention was repeatedly used for 8 times without significant change in catalytic effect, indicating that the recovered n-propanol of the present invention can be recycled. In the embodiment, only the effect of using n-propanol for 8 times is considered, but according to the result, the n-propanol can be used for at least 8 times without affecting the experimental effect.
Fifth, application example of bottom liquid of autoclave
The kettle bottom liquid is used for synthesizing and producing the n-propanol polyether surfactant: putting the bottom liquid into a clean and dry condensation kettle, adding a catalyst KOH with the weight of 0.8 percent of the bottom liquid of the kettle, and adopting N2Replacing air in the kettle, heating to 105 ℃, adding different amounts of ethylene oxide for reaction (3 batches of reaction are carried out, see application example 1, application example 2 and application example 3), controlling the reaction temperature at 120 ℃ of 100-. After the dehydration is finished, the temperature is reduced to 55 to 65 ℃ and the n-propanol polyether surfactant finished product is obtained after filtration. The data of the examples are shown in Table 6.
TABLE 6 finished product index of n-propanol polyether production from kettle bottom liquid
The production data in Table 6 show that the product n-propanol polyether produced by adopting the kettle bottom liquid completely meets the related requirement indexes (the color is less than or equal to 50Pt-Co) of the surfactant, and can be used for producing the surface active n-propanol polyether.
In summary, the method for preparing ethylene glycol monopropyl ether of the present invention uses weak acidic solid catalyst such as zinc methanedisulfonate, zinc methanesulfonate or zinc p-toluenesulfonate as catalyst, and uses strong basic catalyst such as KOH, NaOH, sodium methoxide or sodium n-propoxide and BF3The Lewis acid-like catalyst has the advantages of good reaction selectivity, high purity of ethylene glycol monopropyl ether, less byproducts, mild and safe reaction, reutilization of the catalyst, low cost and less three wastes. Compared with the prior synthesis reaction kettle and the rectification kettle which are required by the prior equipment for ethylene glycol monopropyl ether, the integrated reaction kettle for synthesis reaction and rectification operation reduces one reaction kettle, equipment investment, equipment cost and production area; meanwhile, materials are not required to be transferred to other kettles from a synthesis reaction to a rectification section, so that the pollution of the materials in the transfer process is reduced, and the product quality is ensured. The invention adopts a rectification method with reduced pressure and accurate control, which comprises the following steps: the whole process adopts reduced pressure rectification, the separation temperature of the materials is reduced, the temperature is only 65-80 ℃ in the stage of separating the n-propanol, and the heat energy requirement of the materials required by rectification is reduced; the purity of the ethylene glycol monopropyl ether finished product is more than or equal to 99.8% by accurately controlling the process fraction component monitoring.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation system of ethylene glycol monopropyl ether is characterized in that: the device comprises an addition and rectification integrated reaction kettle, wherein the addition and rectification integrated reaction kettle comprises a reaction kettle main body, and a rectification tower is connected above the reaction kettle main body; the reaction kettle main body comprises a reaction feed inlet, a reaction discharge outlet and a material steam outlet, and the material steam outlet is connected with a rectification inlet of the rectification tower; the rectifying tower comprises a rectifying inlet and a rectifying outlet, and is also connected with a vacuum device.
2. The system for preparing ethylene glycol monopropyl ether according to claim 1, wherein: the reaction discharge hole is also connected with the reaction feed hole through a material return pipeline, and a filter and a material conveying pump are arranged on the material return pipeline.
3. The system for preparing ethylene glycol monopropyl ether according to claim 1, wherein: the reaction kettle is provided with an interlayer, and the interlayer is used for introducing a temperature control medium.
4. The system for producing ethylene glycol monopropyl ether according to any one of claims 1 to 3, characterized in that: the preparation system also comprises a raw material storage tank and a product storage tank, wherein the raw material storage tank and the product storage tank are respectively connected with the addition rectification integrated reaction kettle.
5. A preparation method of ethylene glycol monopropyl ether is characterized in that: the preparation system of any one of claims 1 to 4 is used with the following reaction equation:
the method comprises the following steps: n-propanol and ethylene oxide react under the action of a catalyst to synthesize a crude product of ethylene glycol monopropyl ether; and rectifying the crude product to obtain a finished product of the ethylene glycol monopropyl ether.
6. A process according to claim 5The preparation method of the ethylene glycol monopropyl ether is characterized by comprising the following steps: the preparation method comprises the following steps: mixing N-propanol with a catalyst, N2Adding ethylene oxide under protection to react; separating out the catalyst after the reaction is finished to obtain a crude product of ethylene glycol monopropyl ether; and (2) carrying out reduced pressure rectification on the ethylene glycol monopropyl ether crude product, respectively collecting free n-propanol, an ethylene glycol monopropyl ether finished product and kettle bottom liquid, wherein the separated catalyst and the free n-propanol can be recycled and applied to the reaction process, and the kettle bottom liquid can be directly used for producing an n-propanol polyether surfactant product.
7. The method for preparing ethylene glycol monopropyl ether according to claim 5 or 6, characterized in that: the catalyst is one or a mixture of zinc methanesulfonate and zinc p-toluenesulfonate.
8. The method for preparing ethylene glycol monopropyl ether according to claim 5 or 6, characterized in that: the mass ratio of the n-propanol to the ethylene oxide is as follows: 60: (13.2-44), wherein the dosage of the catalyst is 0.3-5 per mill of the total weight of the n-propanol and the ethylene oxide.
9. The method for preparing ethylene glycol monopropyl ether according to claim 5 or 6, characterized in that: the reaction temperature of the n-propanol and the ethylene oxide under the catalysis of the catalyst is 110-180 ℃, and the reaction pressure is-0.05-0.60 MPa.
10. The method for preparing ethylene glycol monopropyl ether according to claim 5 or 6, characterized in that: the vacuum rectification specific process comprises the following steps: vacuumizing the addition rectification integrated reaction kettle to-0.05 MPa, controlling the vacuum degree to be constant, heating the ethylene glycol monopropyl ether crude product in the reaction kettle, opening rectification for condensation, controlling the temperature of the material at the bottom of the kettle to be 65-80 ℃ and the temperature at the top of the kettle to be 50-65 ℃, carrying out total reflux for 30min, then starting to receive the n-propanol, vacuumizing to improve the vacuum degree in the kettle to be more than or equal to-0.098 MPa when the n-propanol is completely collected and the temperature at the top of the kettle is reduced to normal temperature; kettle capable of raising temperature againControlling the temperature of the inner material at the bottom of the kettle to be 80-100 ℃, controlling the temperature at the top of the kettle to be 50-65 ℃, carrying out total reflux for 30min, and then starting to receive the mixture of ethylene glycol monopropyl ether and n-propanol, wherein the reflux ratio is controlled to be 5: 1, taking liquid during the period to detect the content of ethylene glycol monopropyl ether in the mixture, starting to receive the finished product of ethylene glycol monopropyl ether alone when the content of ethylene glycol monopropyl ether in the receiving liquid is more than or equal to 99.7 percent, stopping receiving when the purity of ethylene glycol monopropyl ether in the fraction is less than or equal to 99.7 percent, and finishing rectification. Cooling the bottom liquid to 40 + -2 deg.C, charging N2And (3) putting the kettle bottom liquid into a packaging barrel for producing other n-propanol polyether until the pressure of the reaction kettle is 0.00-0.04 MPa.
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| WO2022017286A1 (en) * | 2020-07-23 | 2022-01-27 | 浙江皇马科技股份有限公司 | Preparation method and system for ethylene glycol monopropyl ether |
| CN114367259A (en) * | 2021-12-17 | 2022-04-19 | 江苏春江润田农化有限公司 | Trifluoro acetylenic acid methyl ester apparatus for producing with batching automatically regulated puts in function |
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| CN114950297B (en) * | 2022-03-30 | 2024-02-23 | 浙江诺亚氟化工有限公司 | Device and process for producing hydrofluoroether |
| CN115106365B (en) * | 2022-06-28 | 2024-01-12 | 四川国纳科技有限公司 | Recovery method and recovery device for degradable medical supplies |
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