CN111747828B - 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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- CN111747828B CN111747828B CN202010718384.6A CN202010718384A CN111747828B CN 111747828 B CN111747828 B CN 111747828B CN 202010718384 A CN202010718384 A CN 202010718384A CN 111747828 B CN111747828 B CN 111747828B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- Y02P20/50—Improvements relating to the production of bulk chemicals
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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:
comprising the following steps: the normal propyl alcohol and the ethylene oxide react under the action of a catalyst to synthesize a crude ethylene glycol monopropyl ether product; and the crude product is subjected to vacuum rectification to obtain a finished product of ethylene glycol monopropyl ether. The preparation system 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, wherein the material steam outlet is connected with a rectification inlet of a rectification tower, a rectification inlet and a rectification outlet are arranged on the rectification tower, 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 less byproducts.
Description
Technical Field
The invention belongs to the technical field of synthesis of organic compounds, and particularly relates to a preparation method and a system of ethylene glycol monopropyl ether.
Background
Ethylene glycol monopropyl ether is also called propoxyl ethanol, is colorless transparent liquid, and can be dissolved in organic solvents such as ethanol, acetone and the like, and is mixed with water. The ethylene glycol monopropyl ether has very strong dissolving capacity, and its kauri-butanol value (KB value) is 5 times that of aromatic hydrocarbon solvent and 17 times that of aliphatic hydrocarbon solvent, so that it is an excellent solvent and can be extensively used in the fields of nitrocellulose, industrial coating material, etc. The ethylene glycol monopropyl ether has a relatively low evaporation rate, and has obvious effects of improving the gloss of varnish, preventing peeling and the like, so that the ethylene glycol monopropyl ether can be used as a diluent in quick-drying paint and enamel paint, and the adhesiveness between paint and wood and between paint and metal is improved. Meanwhile, the ethylene glycol monopropyl ether can also be used as a raw material for synthesizing the pesticide herbicide pretilachlor.
The current synthetic process route of ethylene glycol monopropyl ether is a polymerization method: the n-propanol and the ethylene oxide react under the action of a catalyst, wherein the catalyst mainly comprises a Lewis acid catalyst and an alkali metal catalyst. By Lewis acids, e.g. BF 3 The catalyst has the characteristics of high catalytic activity and low catalytic temperature, but has more side reactions, high content of byproducts such as dioxane, diethylene glycol and the like, and is not easy to remove. The alkali metal catalyst such as KOH is easy to produce byproducts such as glycol, diethylene glycol and the like, the reaction products are widely distributed, the conversion rate of target products of glycol monopropyl ether is low, and the content of byproducts such as diethylene glycol monopropyl ether, triethylene glycol monopropyl ether and the like is high. Therefore, there is a need for a process for synthesizing ethylene glycol monopropyl etherThe route is optimized to solve the problems of low purity of the synthesized crude product, more byproducts, complex procedures, high production cost and the like in the existing synthetic process route.
In order to solve the problems of low purity, more byproducts, complex procedures, high production cost and the like of the synthesized crude products in 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, fewer byproducts, easy operation and high efficiency.
Disclosure of Invention
The invention provides a preparation method and a system for ethylene glycol monopropyl ether, which are high in catalytic selectivity, low in production cost, less in byproducts, easy to operate and efficient, and aim to solve the problems of low purity of a synthesized crude product, more byproducts, complex procedures, high production cost and the like in the existing ethylene glycol monopropyl ether synthesis process route. The technical scheme of the invention is as follows:
in a first aspect, the invention provides a preparation system of ethylene glycol monopropyl ether, which 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, wherein the material steam outlet is connected with a rectifying inlet of the rectifying tower; the rectifying tower is provided with the rectifying inlet and the rectifying outlet, and is also connected with a vacuum device.
Further, the reaction discharge port is also connected with the reaction feed port through a return pipeline, and a filter and a material conveying pump are arranged on the return pipeline.
Further, a stirring device is arranged in the reaction kettle main body.
Furthermore, 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 and rectification integrated reaction kettle.
In a second aspect, the present invention provides a method for preparing ethylene glycol monopropyl ether, which adopts the above system and the following reaction equation:
comprising the following steps: the normal propyl alcohol and the ethylene oxide react under the action of a catalyst to synthesize a crude ethylene glycol monopropyl ether product; and the crude product is subjected to vacuum rectification to obtain a finished product of ethylene glycol monopropyl ether.
Further, the preparation method comprises the following steps: mixing N-propanol with catalyst, N 2 Adding ethylene oxide under protection for reaction; separating out the catalyst after the reaction is finished to obtain a crude ethylene glycol monopropyl ether product; and (3) 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 to the reaction process, and the kettle bottom liquid can be directly used for producing the n-propanol polyether surfactant product.
Further, the catalyst is one or two of zinc methylsulfonate 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 specific process of the reduced pressure rectification comprises the following steps: vacuumizing the addition and rectification integrated reaction kettle to-0.05 MPa, controlling the vacuum degree to be unchanged, heating up the crude ethylene glycol monopropyl ether in the reaction kettle body, opening rectification for condensation, controlling the temperature of the kettle substrate material to be 65-80 ℃ and the temperature of the top of the kettle to be 50-65 ℃, firstly carrying out total reflux for 30min, then starting to receive n-propanol, and vacuumizing to improve the vacuum degree in the kettle to be more than or equal to-0.098 MPa when the temperature of the top of the kettle is reduced to normal temperature after the n-propanol is completely collected; heating the material in the kettle again, controlling the temperature of the material at 80-100 ℃ and the temperature of the top of the kettle at 50-65 ℃, carrying out total reflux for 30min,and then receiving the mixture of ethylene glycol monopropyl ether and n-propanol, and controlling the reflux ratio to be 5:1, detecting the ethylene glycol monopropyl ether content in the mixture by taking liquid in the period, when the ethylene glycol monopropyl ether content in the receiving liquid is more than or equal to 99.7%, starting to independently receive the ethylene glycol monopropyl ether finished product, and when the ethylene glycol monopropyl ether purity in the fraction is less than or equal to 99.7%, stopping receiving, and finishing rectification. Cooling the bottom solution of the kettle to 40+/-2 ℃ and filling N 2 And (3) placing the kettle bottom liquid into a packaging barrel until the pressure of the reaction kettle is 0.00-0.04MPa, and producing other n-propanol polyether.
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 less byproducts.
2. The preparation method has the advantages of simple process, mild reaction condition, 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 into a whole, 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, the material transfer is not needed, the material pollution probability is avoided, and the product quality can be ensured.
Drawings
FIG. 1 is a schematic diagram of a manufacturing system according to the present invention.
Fig. 2 is a schematic structural diagram of the rectifying tower of the present invention.
In fig. 1 and 2, 1: ethylene oxide reservoir, 2: material transfer pump, 3: catalyst filter, 4: reaction kettle main body, 5: rectifying column, 6: n-propanol reservoir, 7: ethylene glycol monopropyl ether tank, 8: the vacuum pipeline, 9, branch pipeline, 10, reaction feed inlet, 11, reaction discharge outlet, 12, temperature control steam outlet/cooling water inlet, 13, protection gas port, 14, rectification inlet, 15, rectification outlet, 16, stirring device, 17, interlayer, 18, control valve, 19, vacuum pumping port on the storage tank, 20, protection gas port on the storage tank, 21, sampling port, 22, storage tank material outlet, 23, 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 the specific conditions are not specified in the examples, and the description is performed under the conventional conditions or the conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention will now be described in further detail with reference to the drawings and to specific examples, which are given by way of illustration and not limitation.
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 is clean, and heating N 2 Purging and drying the main body of the reaction kettle, the rectifying tower and the storage tank, and cooling to normal temperature for standby.
Example 1
As shown in fig. 1 and 2, the embodiment provides a preparation system of ethylene glycol monopropyl ether, which comprises an addition and rectification integrated reaction kettle, wherein the addition and rectification integrated reaction kettle comprises a reaction kettle main body 4, and a rectification tower 5 is connected above the reaction kettle main body 4. The reaction kettle body 4 is provided with an interlayer 17 for introducing a temperature control medium, such as: steam, cooling water (the steam and cooling water inlet and outlet are just opposite), oil, etc. The reaction kettle body 4 comprises a reaction feed inlet 10, a reaction discharge outlet 11, a protection air port 13 and a material steam outlet, wherein the reaction feed inlet 10 and the reaction discharge outlet 11 are respectively arranged at the top and the bottom of the reaction kettle body 4, and a control valve 18 is arranged on the reaction feed inlet 10 and the reaction discharge outlet 11; the reaction discharge port 11 is also connected with the reaction feed port 10 through a feed back pipeline 23, and the feed back pipeline 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; the reaction kettle body 4 is also internally provided with a pressure sensor and a temperature sensor which are respectively used for monitoring the pressure and the temperature in the reaction kettle body 4. The rectifying tower 5 is a tray type rectifying tower, the bottom is provided with a rectifying inlet 14, the top 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 inlet 14 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, the two branch pipelines 9 are respectively used for collecting the rectified n-propanol and the rectified ethylene glycol monopropyl ether, and a control valve 18 and a check valve 27 are arranged on the two branch pipelines 9; a 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 respectively provided with a vacuumizing port 19, a protection air port 20 and a material outlet 22. The vacuum line 8 is also provided with a plurality of control valves 18. The vacuum pipeline 8 is also provided with a sampling port 21 for sampling and detecting components of the rectification liquid so as to control the purity of different distillates. The preparation system further comprises an ethylene oxide storage tank 1, the ethylene oxide storage tank 1 is connected with a reaction feed inlet 10 of the reaction kettle main body 4, a vacuum pumping port 19 and a protection gas port 20 are also arranged on the ethylene oxide storage tank 1, and a material inlet 24 and a material outlet 22 are also arranged.
Example 2
Adding 60kg of N-propanol and 0.4%o (the proportion of the N-propanol and the ethylene oxide is the same as the following) of zinc methylsulfonate catalyst into an addition reaction and rectification integrated kettle, vacuumizing by a vacuum pump, and adopting N 2 And (3) replacing air in the reaction kettle for three times, wherein the evacuation degree is more than or equal to-0.096 MPa, and heating to 100 ℃ while adding ethylene oxide. The reaction temperature is controlled between 165 and 180 ℃, and the total addition amount of the ethylene oxide is controlled to be 14kg. After the addition of ethylene oxide, the reaction is continued with heat preservation until the pressure no longer drops. Cooling to 50 ℃ after the reaction is finished, and filling N 2 And (3) sampling and detecting crude components until the pressure reaches 0.02MPa, opening a feed back pipeline, a reaction discharge port and a reaction feed inlet 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 kettle materials while maintaining the vacuum degree, and opening a rectifying tower condenser; controlling the temperature of the bottom material of the kettle to be 65-80 ℃ and the temperature of the top of the tower to be 50-65 ℃, carrying out total reflux for 30min, opening a control valve of an n-propanol storage tank when the total reflux time is upReceiving n-propanol; controlling the vacuum degree to be-0.05 MPa, closing a control valve of an n-propanol storage tank when the temperature of the top of the kettle is reduced to normal temperature, vacuumizing to be more than-0.098 MPa, heating the bottom of the kettle to be 80-100 ℃, performing total reflux for 30min at the temperature of the top of the kettle at 50-65 ℃, opening the n-propanol storage tank to receive a mixture of n-propanol and ethylene glycol monopropyl ether, sampling and detecting fraction components at an indefinite time, closing the control valve of the n-propanol storage tank when the fraction ethylene glycol monopropyl ether is more than or equal to 99.7%, opening the control valve of the ethylene glycol monopropyl ether storage tank to receive ethylene glycol monopropyl ether, performing random sampling and detecting of the fraction components, and closing the control valve of the ethylene glycol monopropyl ether storage tank when the fraction ethylene glycol monopropyl ether is less than 99.7%. Cooling the substrate material of the kettle to 40 ℃ and filling N 2 And (5) discharging the bottom material of the kettle to the normal pressure, and packaging the bottom material of the kettle for producing other n-propanol polyethers. The purity detection method adopts gas chromatography calibrated by a standard substance, and is the same as the following.
Comparative example 1
Adding 60kg of normal propyl alcohol and 0.4 permillage KOH catalyst into an addition reaction and rectification integrated kettle, vacuumizing by a vacuum pump, and adopting N 2 And (3) replacing air in the reaction kettle for three times, wherein the evacuation degree is more than or equal to-0.096 MPa, and heating to 150 ℃ after adding ethylene oxide, heating. The reaction temperature is controlled between 165 and 180 ℃, and the total addition amount of the ethylene oxide is controlled to be 14kg. After the addition of ethylene oxide, the reaction is continued with heat preservation until the pressure no longer drops. Cooling to 50 ℃ after the reaction is finished, and filling N 2 To 0.02MPa, sampling and detecting crude components.
Comparative example 2
Adding 60kg of n-propanol and 0.4 permillage of BF into an addition reaction and rectification integrated kettle 3 Diethyl ether catalyst, vacuum pump, N 2 And (3) replacing air in the reaction kettle for three times, wherein the evacuation degree is more than or equal to-0.096 MPa, and after the temperature is raised to 100 ℃, starting to add ethylene oxide for reaction. The reaction temperature is controlled between 100 ℃ and 120 ℃, and the total addition amount of the ethylene oxide is controlled to be 14kg. After the addition of ethylene oxide, the reaction is continued with heat preservation until the pressure no longer drops. Cooling to 50 ℃ after the reaction is finished, and filling N 2 To 0.02MPa, sampling and detecting crude components.
Effect verification experiment
1. Comparison of the merits of different technologies
Examples 3-7 raw materials n-propanol, ethylene oxide, types and amounts of catalysts, reaction temperatures were adjusted, and other process conditions were the same as in example 1; comparative examples 3 to 7 the raw materials n-propanol, ethylene oxide, the kind and amount of catalyst, and the reaction temperature were adjusted, and other process conditions were the same as those of examples; the crude product is shown in Table 1 for specific index (gas chromatography calibrated by standard, the same applies hereinafter).
Table 1 crude conditions and indices for examples and comparative examples
Note that: the catalyst amount is the proportion of the total weight of the n-propanol and the ethylene oxide; the "zinc methyldisulfonate: zinc p-toluenesulfinate=1:1 mixture" having a heavy catalyst type is a mixture catalyst in which the weight ratio of zinc methyldisulfonate to zinc p-toluenesulfinate is 1:1, and the weight ratio is the same as in example 6 and example 7.
As can be seen from the data in Table 1, under the conditions that the dosage of the n-propanol and the ethylene oxide is constant, the dosage of the catalyst is consistent or similar, and the reaction temperature is consistent, the crude product synthesized by the catalyst (zinc methylsulfonate and zinc paratoluenesulfonate) of the invention is compared with the crude product synthesized by the prior art KOH, naOH, CH 3 The content of crude ethylene glycol monopropyl ether synthesized by strong alkaline catalysts such as ONa, sodium n-propoxide and the like is 22% -150%, the higher the weight ratio of ethylene oxide to n-propanol is, the more obvious the difference is, the maximum ethylene glycol monopropyl ether content can be higher by approximately 149% (the comparison of the example 6 and the comparative example 6), and the residual unreacted n-propanol is less; the ratio of the by-products such as diethylene glycol monopropyl ether, triethylene glycol monopropyl ether and the like to the by-products adopting the prior art KOH, naOH, CH 3 Crude products synthesized by strong alkaline catalysts such as ONa, sodium n-propoxide and the like are obviously lowIt is 1/3 or less. Compared with BF 3 The byproducts such as diethylene glycol monopropyl ether, triethylene glycol monopropyl ether and the like are below 15% of the catalyst, and the target product ethylene glycol monopropyl ether is above 18% of the catalyst. It can be seen that the catalyst selection of the present invention represents a significant substantial advance over the prior art.
2. Product rectification index: the final product index after rectification in examples 2 to 7 is shown in Table 2.
Table 2 examples 2 to 7 end product index
As shown in the data of Table 2, the ethylene glycol monopropyl ether content of the product prepared by the rectification method is more than 99.85%, the n-propanol is less than 0.002%, and the diethylene glycol monopropyl ether content is less than 0.003%.
3. Catalyst sleeve
The synthesis reaction conditions were the same as those in example 3, and the catalyst types and the catalyst application times were changed (the catalyst recovery sleeve amount was not enough to slightly supplement the new catalyst), and zinc methyldisulfonate and zinc p-toluenesulfonate were used as examples, but the method is not limited thereto. The specific index of the crude product is shown in tables 3 and 4.
TABLE 3 parameters and crude index for zinc methyldisulfonate catalyst set
TABLE 4 parameters and crude index for zinc p-toluenesulfonate catalyst set
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.
4. Recycling normal propyl alcohol
The synthesis reaction conditions were the same as those in example 3, and the number of times of the n-propanol recycle was changed (the amount of n-propanol recycle was insufficient, and the same amount was supplemented with new n-propanol), but the synthesis reaction was not limited thereto. The specific index of the crude product is shown in Table 5.
TABLE 5 parameters for normal propanol jacket and crude product index
The data in Table 5 shows that the recovered n-propanol of the present invention was reused 8 times without significant change in catalytic effect, indicating that the recovered n-propanol of the present invention was reusable. Since this example examined only 8 times of the effect of the application of n-propanol, it was inferred from the result that n-propanol could be applied at least 8 times or more without affecting the experimental effect.
5. Kettle bottom liquid application example
And (3) using the kettle base solution for synthesizing and producing the n-propanol polyether surfactant: adding the bottom solution into a clean and dry condensation kettle, adding KOH catalyst with the weight of 0.8% of the bottom solution, and adopting N 2 And (3) replacing air in the kettle, heating to 105 ℃, adding different amounts of ethylene oxide for reaction (3 batches of reaction are carried out, namely, application example 1, application example 2 and application example 3), controlling the reaction temperature to be 100-120 ℃, obtaining crude n-propanol polyether after the reaction is finished, cooling the crude n-propanol polyether to 60-70 ℃, transferring the crude n-propanol polyether to a post-treatment kettle, adding deionized water and 85% phosphoric acid with the weight of 2.1 times of KOH for hydrolysis and neutralization, adding polyether adsorbent with the amount of 0.5% of the crude n-propanol polyether, and finally heating to 100-120 ℃ for dehydration. After dehydration, cooling to 55-65 ℃ and filtering to obtain the n-propanol polyether tableAnd (5) a surfactant finished product. Example data is shown in table 6.
TABLE 6 index of finished products of n-propanol polyether produced from bottom solution of kettle
The production data in Table 6 show that the product n-propanol polyether produced by adopting the kettle base solution completely meets the relevant requirement index (color is less than or equal to 50 Pt-Co) of the surfactant, and can be used for producing the surface active n-propanol polyether.
In summary, the preparation method of the ethylene glycol monopropyl ether takes weak acid solid catalysts such as zinc methyldisulfonate, zinc methylsulfonate or zinc p-toluenesulfonate as catalysts, and compared with strong alkaline catalysts such as KOH, naOH, sodium methoxide, sodium n-propoxide and the like and BF 3 The Lewis acid-like catalyst has good reaction selectivity, high purity of ethylene glycol monopropyl ether, few byproducts, mild and safe reaction, reusable catalyst, low cost and few three wastes. Compared with two kettles, namely a synthesis reaction kettle and a rectifying kettle, required by the existing equipment of ethylene glycol monopropyl ether, the integrated reaction kettle for the synthesis reaction and the rectifying operation reduces one reaction kettle, reduces equipment investment, reduces equipment cost and reduces the use of the production area; meanwhile, materials are not required to be transferred to other kettles from the synthesis reaction to the rectifying 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 pressure reduction and accurate control: the whole process adopts reduced pressure rectification, so that the separation temperature of materials is reduced, the temperature is only 65-80 ℃ in the stage of separating n-propanol, and the heat energy requirement of the materials required by rectification is reduced; through monitoring the process fraction components, the purity of the required ethylene glycol monopropyl ether finished product is accurately controlled to be more than or equal to 99.8 percent.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (4)
1. A preparation method of ethylene glycol monopropyl ether is characterized in that: the preparation system of ethylene glycol monopropyl ether is adopted, and the following reaction equation is adopted:
the preparation system of ethylene glycol monopropyl ether 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, wherein the material steam outlet is connected with a rectifying inlet of the rectifying tower; the rectifying tower comprises the rectifying inlet and the rectifying outlet, and is also connected with a vacuum device; the method comprises the following steps: the normal propyl alcohol and the ethylene oxide react under the action of a catalyst to synthesize a crude ethylene glycol monopropyl ether product; rectifying the crude product to obtain a finished product of ethylene glycol monopropyl ether; the preparation method comprises the following steps: mixing N-propanol with catalyst, N 2 Adding ethylene oxide under protection for reaction; separating out the catalyst after the reaction is finished to obtain a crude ethylene glycol monopropyl ether product; 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 to the reaction process, and the kettle bottom liquid can be directly used for producing an n-propanol polyether surfactant product; the catalyst is one or two of zinc methylsulfonate and zinc paratoluenesulfonate; 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; 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; the specific process of the vacuum rectification comprises the following steps: adding the saidVacuum pumping of the rectification integrated reaction kettle to minus 0.05MPa, controlling the vacuum degree unchanged, heating up the crude ethylene glycol monopropyl ether in the reaction kettle, opening rectification for condensation, controlling the temperature of the kettle substrate material to be 65-80 ℃, controlling the temperature of the top of the kettle to be 50-65 ℃, firstly carrying out total reflux for 30min, then starting to receive n-propanol, and vacuumizing to improve the vacuum degree in the kettle to be more than or equal to minus 0.098MPa when the temperature of the top of the kettle is reduced to normal temperature after the n-propanol is collected; heating the materials in the kettle again, controlling the temperature of the materials at 80-100 ℃ and the temperature of the top of the kettle at 50-65 ℃, performing total reflux for 30min, starting to receive the mixture of ethylene glycol monopropyl ether and n-propanol, and controlling the reflux ratio to be 5:1, taking liquid in the period to detect the ethylene glycol monopropyl ether content in the mixture, when the ethylene glycol monopropyl ether content in the receiving liquid is more than or equal to 99.7%, starting to independently receive an ethylene glycol monopropyl ether finished product, and when the ethylene glycol monopropyl ether purity in the fraction is less than or equal to 99.7%, stopping receiving, and finishing rectification; cooling the bottom solution of the kettle to 40+/-2 ℃ and filling N 2 And (3) placing the kettle bottom liquid into a packaging barrel until the pressure of the reaction kettle is 0.00-0.04MPa, and producing other n-propanol polyether.
2. The method for preparing ethylene glycol monopropyl ether according to claim 1, wherein the method comprises the following steps: the reaction discharge port is also connected with the reaction feed port through a return pipeline, and a filter and a material conveying pump are arranged on the return pipeline.
3. The method for preparing ethylene glycol monopropyl ether according to claim 1, wherein the method comprises the following steps: the reaction kettle is provided with an interlayer, and the interlayer is used for introducing a temperature control medium.
4. The method for preparing ethylene glycol monopropyl ether according to claim 1, wherein the method comprises the following steps: 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 and rectification integrated reaction kettle.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010718384.6A CN111747828B (en) | 2020-07-23 | 2020-07-23 | Preparation method and system of ethylene glycol monopropyl ether |
| PCT/CN2021/106809 WO2022017286A1 (en) | 2020-07-23 | 2021-07-16 | Preparation method and system for ethylene glycol monopropyl ether |
Applications Claiming Priority (1)
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| CN111747828B (en) * | 2020-07-23 | 2023-05-26 | 浙江皇马科技股份有限公司 | Preparation method and system of ethylene glycol monopropyl ether |
| CN114367259B (en) * | 2021-12-17 | 2023-05-23 | 江苏春江润田农化有限公司 | Methyl trifluoroalkynoate apparatus for producing with batching automatically regulated is put in function |
| 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 |
| CN115301173A (en) * | 2022-07-18 | 2022-11-08 | 临沂金朗化工有限公司 | Preparation device and method of sodium tert-butoxide |
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