CN110585994B - Device and method for synthesizing 2-methoxy-3, 4-dihydropyran - Google Patents
Device and method for synthesizing 2-methoxy-3, 4-dihydropyran Download PDFInfo
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- CN110585994B CN110585994B CN201910858007.XA CN201910858007A CN110585994B CN 110585994 B CN110585994 B CN 110585994B CN 201910858007 A CN201910858007 A CN 201910858007A CN 110585994 B CN110585994 B CN 110585994B
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- C07D309/28—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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Abstract
The invention provides a device for synthesizing 2-methoxy-3, 4-dihydropyran, which is provided with a recovery tank, so that acrolein and vinyl methyl ether gas in a reaction kettle can enter the recovery tank and be condensed, and the condition that the acrolein gas in the reaction kettle influences the body health of staff and peripheral staff when the reaction kettle is required to be dredged can be avoided; a second jacket is sleeved on the periphery of the reaction kettle, the reaction kettle is subjected to steam heating by the second jacket, and the temperature of the reaction kettle is uniformly increased by the steam heating; the invention also provides a method for synthesizing 2-methoxy-3, 4-dihydropyran, the device of the invention is used for synthesizing 2-methoxy-3, 4-dihydropyran, acrolein and vinyl methyl ether gases which do not react in the reaction kettle enter the recovery tank and are condensed, then the acrolein and vinyl methyl ether gases enter the reaction kettle again for further reaction, and the device is used for synthesizing 2-methoxy-3, 4-dihydropyran, so that the raw materials can be fully utilized, and the production yield is improved.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a device and a method for synthesizing 2-methoxy-3, 4-dihydropyran.
Background
Glutaraldehyde is the most widely used product for killing bacteria and viruses in recent years, and the process of hydrolyzing and synthesizing the glutaraldehyde by 2-methoxy-3, 4-dihydropyran is the lowest-cost production method at present. The existing method for synthesizing 2-methoxy-3, 4-dihydropyran is to directly place acrolein, vinyl methyl ether and polymerization inhibitor in a pipeline reactor for reaction, thus having the following disadvantages: the polymer produced during the reaction often blocks the reactor, so that the pipes are dredged, however, the raw material acrolein which is not completely reacted is often used in the reaction, and the toxic odor strongly stimulated by the acrolein can influence the health of staff and people around the staff.
Based on the above risks, there is a need for an improvement of the existing apparatus for synthesizing 2-methoxy-3, 4-dihydropyran.
Disclosure of Invention
In view of the above, the invention provides a device for synthesizing 2-methoxy-3, 4-dihydropyran, which can avoid acrolein gas in a reaction kettle from influencing the health of staff when the reaction kettle needs to be dredged.
In one aspect, the invention provides a device for synthesizing 2-methoxy-3, 4-dihydropyran, which comprises a reaction kettle, a recovery tank, a communicating pipe and a first valve, wherein the reaction kettle is provided with a feed pipe and a discharge pipe, the recovery tank is communicated with the reaction kettle through the communicating pipe, and the first valve is arranged on the communicating pipe.
On the basis of the technical scheme, the automatic control system is preferable and further comprises a condenser, a first pipeline, a second pipeline and a second valve, wherein the inlet of the condenser is communicated with the recovery tank through the first pipeline, the outlet of the condenser is communicated with the recovery tank through the second pipeline, and the first pipeline and the second pipeline are both provided with the second valve.
On the basis of the technical scheme, the reactor is preferably further provided with a first jacket, a third pipeline and a third valve, the first jacket is hollow, one end of the first jacket is closed, the first jacket is sleeved on the periphery of the recovery tank, a liquid inlet is formed in the first jacket, one end of the third pipeline is communicated with the reaction kettle, the other end of the third pipeline penetrates through the closed end of the first jacket and is communicated with the recovery tank, and the third valve is arranged on the third pipeline.
Preferably, the reactor further comprises a second jacket, the second jacket is hollow, one end of the second jacket is closed, the second jacket is sleeved on the periphery of the reactor, a steam inlet is formed in the second jacket, and the discharge pipe penetrates out of the closed end of the second jacket.
On the basis of above technical scheme, preferred, still include an inlet tube, the inlet tube is located in reation kettle, outside the reation kettle was stretched out respectively to the end of intaking, the play water end of inlet tube, the part that the inlet tube is located reation kettle is snakelike bending.
Further preferably, the reaction kettle further comprises a gas storage tank, wherein the gas storage tank is communicated with the reaction kettle, and inert gas or nitrogen is stored in the gas storage tank.
In another aspect, the present invention also provides a method for synthesizing 2-methoxy-3, 4-dihydropyran, which comprises the following steps:
s1, adding acrolein, vinyl methyl ether and a polymerization inhibitor into the reaction kettle through a feeding pipe, opening a gas storage tank, and introducing gas into the reaction kettle to enable the pressure in the reaction kettle to be 0.1-9 Mpa;
s2, introducing steam into the second jacket through a steam inlet, keeping the temperature in the reaction kettle at 60-200 ℃, maintaining for 2-5 hours, and stopping introducing the steam;
s3, opening a first valve on the communicating pipe, introducing low-temperature liquid into the first jacket through the liquid inlet to maintain the materials in the recovery tank in a liquid state, then opening second valves on the first pipeline and the second pipeline, simultaneously opening a third valve on the third pipeline, opening a gas storage tank, and introducing gas into the reaction kettle to enable the pressure in the reaction kettle to be 0.1-9 Mpa; and introducing steam into the second jacket through a steam inlet to keep the temperature in the reaction kettle at 60-200 ℃, maintaining for 2-5 h, stopping introducing the steam, and opening a discharge pipe to obtain the 2-methoxy-3, 4-dihydropyran.
On the basis of the technical scheme, preferably, the polymerization inhibitor comprises one of 2, 6-di-tert-butyl-4-methylphenol, hydroquinone, p-methoxyphenol and phenothiazine.
On the basis of the technical scheme, the mass ratio of the acrolein to the vinyl methyl ether to the polymerization inhibitor is preferably 1 (1-3) to 0.001-0.003.
On the basis of the technical scheme, preferably, when steam is introduced into the second jacket from the steam inlet in the S2, cooling water with the temperature of 5-10 ℃ is introduced into the water inlet pipe through the water inlet end, so that the temperature in the reaction kettle is increased to 90-160 ℃ within 8-10 hours.
Compared with the prior art, the device for synthesizing the 2-methoxy-3, 4-dihydropyran has the following beneficial effects:
(1) the recovery tank is arranged, so that acrolein and vinyl methyl ether gas in the reaction kettle can enter the recovery tank and be condensed, and the phenomenon that the acrolein gas in the reaction kettle influences the body health of staff and peripheral staff when the reaction kettle needs to be dredged can be avoided;
(2) a second jacket is sleeved on the periphery of the reaction kettle, the reaction kettle is subjected to steam heating by the second jacket, and the temperature of the reaction kettle is uniformly increased by the steam heating;
(3) the device is utilized to synthesize the 2-methoxy-3, 4-dihydropyran, the unreacted acrolein and vinyl methyl ether gas in the reaction kettle enters the recovery tank and is condensed, and then enters the reaction kettle again to further react, so that the 2-methoxy-3, 4-dihydropyran is synthesized through the device, the raw materials can be fully utilized, and the production yield is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for synthesizing 2-methoxy-3, 4-dihydropyran according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
As shown in FIG. 1, the present invention provides an apparatus for synthesizing 2-methoxy-3, 4-dihydropyran, comprising: the system comprises a reaction kettle 1, a recovery tank 2, a condenser 3, a first pipeline 4, a second pipeline 5, a first jacket 6, a third pipeline 7, a second jacket 8 and a water inlet pipe 9.
The reaction kettle 1 provides a place for synthesizing 2-methoxy-3, 4-dihydropyran, specifically, a feed pipe 11 and a discharge pipe 12 are arranged on the reaction kettle 1, and synthetic raw materials are added into the reaction kettle 1 through the feed pipe 11: acrolein, vinyl methyl ether and polymerization inhibitor, and controlling the reaction conditions to obtain the 2-methoxy-3, 4-dihydropyran.
And a condenser 3 for further condensing a part of the uncondensed gas in the recovery tank 2.
A first conduit 4 for communicating the inlet of the condenser 3 with the recovery tank 2.
And a second pipe 5 for communicating the outlet of the condenser 3 with the recovery tank 2.
Specifically, most of the gas entering the recovery tank 2 is condensed into liquid, and a part of the gas is not condensed, at this time, the second valve 41 on the first pipeline 4 is opened, a part of the gas which is not condensed enters the condenser 3 for condensation, then the second valve 41 on the second pipeline 5 is opened, and the condensed gas enters the recovery tank 2 again.
The second presss from both sides cover 8, and it is used for carrying out steam heating to reation kettle 1, and is concrete, and the second presss from both sides inside cavity and one end of cover 8 and seals, and reation kettle 1 periphery is located to the second cover 8 cover, and the second presss from both sides and has seted up steam inlet 81 on the cover 8, presss from both sides the interior steam that lets in of cover 8 to the second through steam inlet 81, can heat reation kettle 1 through steam to control the temperature in the reation kettle 1.
The reaction kettle is characterized by further comprising a gas storage tank 10, wherein the gas storage tank 10 is used for introducing gas into the reaction kettle 1 to maintain the reaction pressure in the reaction kettle 1, specifically, the gas storage tank 10 is communicated with the reaction kettle 1, inert gas or nitrogen is stored in the gas storage tank 10, the gas storage tank 10 is started, and the gas in the gas storage tank 10 enters the reaction kettle 1, so that the pressure in the reaction kettle 1 can be maintained.
The synthesis of 2-methoxy-3, 4-dihydropyran using the above apparatus is exemplified below.
Example 1
A method for synthesizing 2-methoxy-3, 4-dihydropyran, comprising the following steps:
s1, adding 1.5 tons of acrolein, 1.5 tons of vinyl methyl ether and 3 kilograms of polymerization inhibitor hydroquinone into a reaction kettle through a feeding pipe, opening a gas storage tank, and introducing nitrogen into the reaction kettle to enable the pressure in the reaction kettle to be 1 Mpa;
s2, introducing steam into the second jacket through the steam inlet, and simultaneously introducing cooling water with the temperature of 8 ℃ into the water inlet pipe through the water inlet end at proper time to heat the inside of the reaction kettle to 160 ℃ within 9 hours and keep the temperature for 2 hours;
s3, opening a first valve on a communicating pipe, enabling unreacted acrolein and vinyl methyl ether gas in the reaction kettle to enter a recovery tank, simultaneously introducing low-temperature liquid such as liquid nitrogen into a first jacket through a liquid inlet, reducing the temperature in the recovery tank after introducing the low-temperature liquid, so that the acrolein and vinyl methyl ether gas entering the reaction kettle are condensed, then opening second valves on a first pipeline and a second pipeline, enabling part of uncondensed gas in the recovery tank to enter a condenser for further condensation, and then flowing into the recovery tank again, opening a third valve on a third pipeline again, enabling the condensed raw material in the recovery tank to return to the reaction kettle further, then opening a gas storage tank again, and introducing nitrogen into the reaction kettle to continuously enable the pressure in the reaction kettle to be 1 Mpa; and introducing steam into the second jacket through a steam inlet to keep the temperature in the reaction kettle at 160 ℃, maintaining for 2h, opening a discharge pipe to obtain 2-methoxy-3, 4-dihydropyran, and synthesizing the 2-methoxy-3, 4-dihydropyran by the device, so that raw materials can be fully utilized, and the production yield is improved.
Example 2
A method for synthesizing 2-methoxy-3, 4-dihydropyran, comprising the following steps:
s1, adding 1 ton of acrolein, 1 ton of vinyl methyl ether and 1 kg of polymerization inhibitor phenothiazine into a reaction kettle through a feed pipe, starting a gas storage tank, and introducing nitrogen into the reaction kettle to enable the pressure in the reaction kettle to be 3 Mpa;
s2, introducing steam into the second jacket through the steam inlet, and introducing cooling water with the temperature of 5 ℃ into the water inlet pipe through the water inlet end at proper time to heat the inside of the reaction kettle to 120 ℃ within 9 hours and keep the temperature for 2 hours;
s3, opening a first valve on a communicating pipe, enabling unreacted acrolein and vinyl methyl ether gas in the reaction kettle to enter a recovery tank, simultaneously introducing low-temperature liquid such as liquid nitrogen into a first jacket through a liquid inlet, reducing the temperature in the recovery tank after introducing the low-temperature liquid, so that the acrolein and vinyl methyl ether gas entering the reaction kettle are condensed, then opening second valves on a first pipeline and a second pipeline, enabling part of uncondensed gas in the recovery tank to enter a condenser for further condensation, and then flowing into the recovery tank again, opening a third valve on a third pipeline again, enabling the condensed raw material in the recovery tank to return to the reaction kettle further, then opening a gas storage tank again, and introducing nitrogen into the reaction kettle to continuously enable the pressure in the reaction kettle to be 3 Mpa; and introducing steam into the second jacket through a steam inlet to keep the temperature in the reaction kettle at 120 ℃, maintaining for 2h, opening a discharge pipe to obtain 2-methoxy-3, 4-dihydropyran, and synthesizing the 2-methoxy-3, 4-dihydropyran by the device, so that raw materials can be fully utilized, and the production yield is improved.
Example 3
A method for synthesizing 2-methoxy-3, 4-dihydropyran, comprising the following steps:
s1, adding 2 tons of acrolein, 2 tons of vinyl methyl ether and 4 kilograms of polymerization inhibitor p-methoxyphenol into a reaction kettle through a feeding pipe, opening a gas storage tank, and introducing nitrogen into the reaction kettle to enable the pressure in the reaction kettle to be 5 Mpa;
s2, introducing steam into the second jacket through the steam inlet, and simultaneously introducing cooling water with the temperature of 8 ℃ into the water inlet pipe through the water inlet end at proper time to heat the inside of the reaction kettle to 100 ℃ within 9 hours and keep the temperature for 2 hours;
s3, opening a first valve on a communicating pipe, enabling unreacted acrolein and vinyl methyl ether gas in the reaction kettle to enter a recovery tank, simultaneously introducing low-temperature liquid such as liquid nitrogen into a first jacket through a liquid inlet, reducing the temperature in the recovery tank after introducing the low-temperature liquid, so that the acrolein and vinyl methyl ether gas entering the reaction kettle are condensed, then opening second valves on a first pipeline and a second pipeline, enabling part of uncondensed gas in the recovery tank to enter a condenser for further condensation, and then flowing into the recovery tank again, opening a third valve on a third pipeline again, enabling the condensed raw material in the recovery tank to return to the reaction kettle further, then opening a gas storage tank again, and introducing nitrogen into the reaction kettle to continuously enable the pressure in the reaction kettle to be 5 Mpa; and introducing steam into the second jacket through a steam inlet to keep the temperature in the reaction kettle at 100 ℃, maintaining for 2h, opening a discharge pipe to obtain 2-methoxy-3, 4-dihydropyran, and synthesizing the 2-methoxy-3, 4-dihydropyran by the device, so that raw materials can be fully utilized, and the production yield is improved.
Comparative example 1
A method for synthesizing 2-methoxy-3, 4-dihydropyran, comprising the following steps:
s1, adding 1.5 tons of acrolein, 1.5 tons of vinyl methyl ether and 3 kilograms of polymerization inhibitor hydroquinone into a pipeline reactor, and reacting for 2 hours at the temperature of 160 ℃ and the pressure of 1 Mpa.
The yields of 2-methoxy-3, 4-dihydropyran synthesized in examples 1 to 3 and comparative example 1 were calculated, respectively, and the results are shown in table 1 below.
TABLE 1 yield of 2-methoxy-3, 4-dihydropyran synthesized in different examples
| Example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Yield (%) | 93.8 | 94.1 | 93.3 | 85.3 |
As can be seen from the above Table 1, the yields of the methods for synthesizing 2-methoxy-3, 4-dihydropyran according to the present invention are all greater than those of the comparative examples, because the acrolein and vinyl methyl ether gases which do not react in the reaction kettle are condensed and then enter the recovery tank, and enter the reaction kettle again to participate in the reaction, thereby increasing the yield.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method for synthesizing 2-methoxy-3, 4-dihydropyran is characterized in that: the method comprises the following steps:
s1, adding acrolein, vinyl methyl ether and a polymerization inhibitor into the reaction kettle through a feeding pipe, opening a gas storage tank, and introducing gas into the reaction kettle to enable the pressure in the reaction kettle to be 0.1-9 Mpa;
s2, introducing steam into the second jacket through a steam inlet, keeping the temperature in the reaction kettle at 60-200 ℃, maintaining for 2-5 hours, and stopping introducing the steam;
s3, opening a first valve on the communicating pipe, introducing low-temperature liquid into the first jacket through the liquid inlet to maintain the materials in the recovery tank in a liquid state, then opening second valves on the first pipeline and the second pipeline, simultaneously opening a third valve on the third pipeline, opening a gas storage tank, and introducing gas into the reaction kettle to enable the pressure in the reaction kettle to be 0.1-9 Mpa; introducing steam into the second jacket through a steam inlet to keep the temperature in the reaction kettle at 60-200 ℃, maintaining for 2-5 h, stopping introducing the steam, and opening a discharge pipe to obtain 2-methoxy-3, 4-dihydropyran;
the device for synthesizing the 2-methoxy-3, 4-dihydropyran comprises a reaction kettle (1), a recovery tank (2), a communicating pipe (21) and a first valve (22), wherein the reaction kettle (1) is provided with a feeding pipe (11) and a discharging pipe (12), the recovery tank (2) is communicated with the reaction kettle (1) through the communicating pipe (21), and the first valve (22) is arranged on the communicating pipe (21);
the device is characterized by further comprising a condenser (3), a first pipeline (4), a second pipeline (5) and a second valve (41), wherein an inlet of the condenser (3) is communicated with the recovery tank (2) through the first pipeline (4), an outlet of the condenser (3) is communicated with the recovery tank (2) through the second pipeline (5), and the first pipeline (4) and the second pipeline (5) are respectively provided with the second valve (41);
the reaction kettle further comprises a first jacket (6), a third pipeline (7) and a third valve (71), wherein the first jacket (6) is hollow, one end of the first jacket is closed, the first jacket (6) is sleeved on the periphery of the recovery tank (2), a liquid inlet (61) is formed in the first jacket (6), one end of the third pipeline (7) is communicated with the reaction kettle (1), the other end of the third pipeline penetrates through the closed end of the first jacket (6) and is communicated with the recovery tank (2), and the third valve (71) is arranged on the third pipeline (7);
the reaction kettle further comprises a second jacket (8), the second jacket (8) is hollow, one end of the second jacket (8) is closed, the second jacket (8) is sleeved on the periphery of the reaction kettle (1), a steam inlet (81) is formed in the second jacket (8), and the discharge pipe (12) penetrates out of the closed end of the second jacket (8);
still include a gas holder (10), gas holder (10) intercommunication reation kettle (1), store inert gas in gas holder (10).
2. The process for the synthesis of 2-methoxy-3, 4-dihydropyran according to claim 1, characterized in that: still include an inlet tube (9), in reation kettle (1) was located in inlet tube (9), outside reation kettle (1) was stretched out respectively to the end of intaking, the play water end of inlet tube (9), the part that inlet tube (9) are located reation kettle is snakelike bending.
3. The process for the synthesis of 2-methoxy-3, 4-dihydropyran according to claim 1, characterized in that: the polymerization inhibitor comprises one of 2, 6-di-tert-butyl-4-methylphenol, hydroquinone, p-methoxyphenol and phenothiazine.
4. The process for the synthesis of 2-methoxy-3, 4-dihydropyran according to claim 1, characterized in that: the mass ratio of the acrolein to the vinyl methyl ether to the polymerization inhibitor is 1 (1-3) to 0.001-0.003.
5. The process for the synthesis of 2-methoxy-3, 4-dihydropyran according to claim 1, characterized in that: when steam is introduced into the second jacket from the steam inlet in the S2, cooling water with the temperature of 5-10 ℃ is introduced into the water inlet pipe through the water inlet end, and the temperature in the reaction kettle is raised to 90-160 ℃ within 8-10 hours.
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