CN212954957U - Production equipment of methyl hypophosphite - Google Patents
Production equipment of methyl hypophosphite Download PDFInfo
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- CN212954957U CN212954957U CN202021238112.8U CN202021238112U CN212954957U CN 212954957 U CN212954957 U CN 212954957U CN 202021238112 U CN202021238112 U CN 202021238112U CN 212954957 U CN212954957 U CN 212954957U
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Abstract
The utility model relates to a production facility of methyl hypophosphite, including have be used for letting in methyl phosphine dichloride's first entry and be used for letting in the continuous flow reactor of the second entry of alcohol, with the continuous flow reactor export the evaporimeter that is linked together, with the export of evaporimeter be linked together be used for collecting the first groove of receiving of methyl hypophosphite. The utility model has the advantages of simple structure, the side reaction is few, can reduce the production of noxious material, and the aftertreatment is with low costs, and production efficiency is high, and yield and purity are high, and the security is good, is fit for the industrial production.
Description
Technical Field
The invention belongs to the field of organic chemical synthesis, and particularly relates to production equipment of methylphosphinic acid ester.
Background
In the prior art, methylphosphinic acid ester is prepared by a reaction tower, such as CN106674275B, but the preparation by the reaction tower has the defects of long reaction time, low production efficiency, easy disproportionation reaction, toxic substance generation and complex post-treatment.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a synthetic method of methylphosphinic acid ester with high production efficiency and simple post-treatment and production equipment.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model discloses an aspect provides a synthetic method of methyl hypophosphite, it uses methyl phosphine dichloride and alcohol as the raw materials and reacts and makes, the reaction goes on in continuous flow reactor.
Preferably, the continuous flow reactor is a microchannel reactor, a pipeline reactor or a flat-plate reactor, such as a G1 reactor, AFR reactor, etc. of Corning.
Preferably, the continuous flow reactor comprises a plurality of reaction parts which are connected in series in sequence, the alcohol is introduced from the first reaction part of the continuous flow reactor, and the methyl phosphine dichloride is introduced from the second reaction part of the continuous flow reactor and is mixed and reacted with the alcohol.
Preferably, the continuous flow reactor comprises a first preheating part for introducing the methyl phosphine dichloride, a second preheating part for introducing the alcohol, and a plurality of reaction parts which are communicated with the first preheating part and the second preheating part and are connected in series in sequence.
Preferably, the flow rate of the methyl phosphine dichloride is controlled to be 5-50 g/min, preferably 5-35 g/min, and more preferably 5-10 g/min.
Preferably, the flow rate of the alcohol is controlled to be 5-100 g/min, preferably 10-70 g/min, and more preferably 10-15 g/min.
Preferably, the residence time of the raw materials in the continuous flow reactor is controlled to be 15 s-30 min, preferably 1-5 min.
Preferably, the reaction temperature in the continuous flow reactor is controlled to be 0-150 ℃.
Preferably, the molar ratio of the methyl phosphine dichloride to the alcohol is 1: 2-50, preferably 1: 5-10, and more preferably 1: 3.1 to 10.
Preferably, the discharge from said continuous flow reactor is passed through an evaporator to separate said methylphosphinic acid esters from said by-products.
Further preferably, the degree of vacuum of the vaporization chamber in the evaporator is controlled to be-0.095 MPa to 100Pa, preferably 100Pa to 300 Pa.
Further preferably, the temperature in the evaporator is controlled to be 0-100 ℃, preferably 35-100 ℃, and further preferably 60-100 ℃.
Further preferably, after the byproduct is condensed by a cold air cooler, hydrogen chloride is collected by an absorption tower, and the rest byproduct is collected by a receiving groove.
The second aspect of the utility model is to provide a methyl hypophosphite production facility, including having the continuous flow reactor that is used for letting in methyl phosphine dichloride's first entry and is used for letting in the second entry of alcohol, with the export of continuous flow reactor communicate with the evaporimeter, with the export of evaporimeter communicate with be used for collecting methyl hypophosphite first groove.
Preferably, the continuous flow reactor is a microchannel reactor, a pipeline reactor or a flat-plate reactor, such as a G1 reactor, AFR reactor, etc. of Corning.
Preferably, said continuous flow reactor comprises a plurality of reaction sections connected in series, said first inlet being disposed on a second of said reaction sections and said second inlet being disposed on a first of said reaction sections.
Preferably, the continuous flow reactor comprises a first preheating part provided with the first inlet, a second preheating part provided with the second inlet, and a plurality of reaction parts which are communicated with the first preheating part and the second preheating part and are sequentially connected in series.
Preferably, said production apparatus further comprises a first intermediate tank disposed between said continuous flow reactor and said evaporator, and a pump installed on a pipe of said first intermediate tank and said evaporator.
Further preferably, a liquid level meter is arranged on the first middle groove.
Preferably, the inlet of the evaporator is located at the upper part of the evaporator, and the outlet of the evaporator is located at the lower part of the evaporator.
Preferably, the production equipment further comprises a condenser communicated with the evaporator, a second receiving groove communicated with the condenser and used for collecting byproducts, a vacuum pump communicated with the second receiving groove, and an absorption tower communicated with the vacuum pump.
Further preferably, the first receiving groove and the second receiving groove are provided with liquid level meters.
Further preferably, the production equipment further comprises a second intermediate tank, wherein the upper part of the second intermediate tank is respectively communicated with the lower part of the evaporator and the inlet of the condenser, and the lower part of the second intermediate tank is communicated with the first receiving tank or a pipeline between the first receiving tank and the evaporator.
Further preferably, the top of the first receiving tank is communicated with the condenser.
Preferably, the evaporator comprises a falling film evaporator or a wiped film evaporator.
Due to the adoption of the technical scheme, compared with the prior art, the utility model have the following advantage:
the utility model discloses a process flow is simple, and the side reaction is few, can reduce the production of noxious material, and the aftertreatment is with low costs, and production efficiency is high, and yield and purity are high, and the security is good, is fit for the industrial production.
Drawings
FIG. 1 is a schematic configuration diagram of a production apparatus of example 1;
FIG. 2 is a schematic structural view of a production apparatus of example 2;
wherein, 1, a continuous flow reactor; 2. a first intermediate tank; 3. an evaporator; 4. a pump; 5. a first receiving groove; 6. a second intermediate tank; 7. a condenser; 8. a second receiving groove; 9. a vacuum pump; 10. a liquid level meter; 11. a reaction section; 12. a first preheating section; 13. a second preheating part.
Detailed Description
The technical solution of the present invention will be further described below with reference to specific embodiments, but the present invention is not limited to the following embodiments. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
The apparatus for producing methylphosphinic acid ester as shown in FIGS. 1 and 2 comprises a continuous flow reactor 1 having a first inlet for introducing methylphosphine dichloride and a second inlet for introducing alcohol, a first intermediate tank 2 having a top communicating with an outlet of the continuous flow reactor 1, an evaporator 3 having a top communicating with a bottom of the first intermediate tank 2, a pump 4 installed on a pipe of the first intermediate tank 2 and the evaporator 3, a first receiving tank 5 communicating with a bottom of the evaporator 3 for collecting methylphosphinic acid ester, a second intermediate tank 6 with the upper part communicated with the lower part of the evaporator 3, a condenser 7 with the top part communicated with the upper part of the second intermediate tank 6, a second receiving tank 8 with the top part communicated with the bottom part of the condenser 7 and used for collecting byproducts (alkyl chloride and alcohol), a vacuum pump 9 communicated with the top part of the second receiving tank 8, and an absorption tower communicated with the vacuum pump 9. The bottom of the second intermediate tank 6 is communicated with the top of the first intermediate tank 2 or the pipeline between the first intermediate tank 2 and the evaporator 3, and the top of the first receiving tank 5 is communicated with the top of the condenser 7. The first intermediate tank 2, the first receiving tank 5 and the second receiving tank 8 are respectively provided with a liquid level meter 10.
Wherein the continuous flow reactor 1 is a microchannel reactor, a pipeline reactor or a flat-plate reactor, such as a G1 reactor, an AFR reactor, etc. of Corning Corp. The evaporator 3 includes a falling film evaporator or a wiped film evaporator.
Example 1 (as shown in fig. 1), the continuous flow reactor 1 includes a first preheating section 12 having a first inlet, a second preheating section 13 having a second inlet, and a plurality of reaction sections 11 connected in series in order to communicate with the first preheating section 12 and the second preheating section 13.
Example 2 (as shown in fig. 2), the continuous flow reactor 1 comprises a plurality of reaction sections 11 connected in series in sequence, a first inlet is provided on the second reaction section 11, and a second inlet is provided on the first reaction section 11.
The reaction part and the preheating part in the utility model have the same structure and are only named differently.
When the equipment is adopted for production, the methyl phosphine dichloride enters from the first inlet at a certain flow rate, the alcohol enters from the second inlet at a certain flow rate and is preheated, the methyl phosphine dichloride and the alcohol are mixed and reacted in the continuous flow reactor 1, and the residence time of reactants in the continuous flow reactor 1 can be controlled by controlling the number of the reaction parts 11 which are connected in series; the reaction liquid from the continuous flow reactor 1 passes through an intermediate tank and then rapidly enters an evaporator 3, byproducts such as chloroalkane, alcohol and hydrogen chloride are rapidly gasified in the evaporator 3 through the blowing-off of hot nitrogen, the methyl hypophosphite product is discharged from the bottom of the evaporator 3 to a first receiving tank 5, the byproducts such as chloroalkane, alcohol and hydrogen chloride pass through a second intermediate tank 6 and then enter a condenser 7 for condensation, wherein the methyl hypophosphite product blown off along with the byproducts is liquefied from the second intermediate tank 6 and then flows back to the first receiving tank 5, the byproducts brought in the first receiving tank 5 are gasified and then enter the condenser 7 from the first receiving tank 5, the chloroalkane and the alcohol condensed by an air cooler are collected in the second receiving tank 8, the hydrogen chloride gas discharged from the top of the second receiving tank 8 is pumped to an absorption tower for treatment through a vacuum pump 9, the absorption tower can be sprayed with water to obtain hydrochloric acid, neutralization treatment with alkali may also be employed.
A specific example of the production of methylphosphinic acid esters using the apparatus of example 2 is as follows:
example 1:
synthesis of ethyl methylphosphinate
Ethanol is preheated to 60 ℃ through the 1 st plate at the flow rate of 15g/min, the methyl phosphine dichloride is mixed with the ethanol at the 2 nd plate at the flow rate of 5g/min, the mixture enters a vaporization chamber after the mixture stays for 2 minutes, the temperature of the vaporization chamber is 60 ℃, the negative pressure is-0.095 MPa, the ethyl chloride, the ethanol and the hydrogen chloride are collected for 5 minutes, 23.5g of products are discharged from the bottom of the vaporization chamber, the purity is 96 percent, and the yield is 98.6 percent.
Example 2:
synthesis of ethyl methylphosphinate
Ethanol is preheated to 80 ℃ through the 1 st plate at the flow rate of 15g/min, the methyl phosphine dichloride is mixed with the ethanol at the 2 nd plate at the flow rate of 10g/min, the mixture enters a vaporization chamber after the mixture stays for 2 minutes, the temperature of the vaporization chamber is 80 ℃, the negative pressure is minus 0.095MPa, the ethyl chloride, the ethanol and the hydrogen chloride are collected for 5 minutes, 42g of product is discharged from the bottom of the vaporization chamber, the purity is 96 percent, and the yield is 88 percent.
Example 3:
synthesis of n-butyl methylphosphinate
Butanol alcohol is preheated to 75 ℃ through the 1 st plate at the flow rate of 15g/min, methyl phosphine dichloride is mixed with ethanol at the 2 nd plate at the flow rate of 5g/min, after the mixture stays for 2 minutes, the mixture enters a vaporization chamber, the temperature of the vaporization chamber is 75 ℃, the negative pressure is-0.095 MPa, chlorobutane, butanol and hydrogen chloride are collected for 5 minutes, 29.7g of product is discharged from the bottom of the vaporization chamber, the purity is 96 percent, and the yield is 99 percent.
Example 4:
synthesis of n-butyl methylphosphinate
Butanol is preheated to 100 ℃ through the 1 st plate at the flow rate of 25g/min, methyl phosphine dichloride is mixed with ethanol at the 2 nd plate at the flow rate of 5g/min, after the mixture stays for 2 minutes, the mixture enters a vaporization chamber, the temperature of the vaporization chamber is 100 ℃, the negative pressure is-0.095 MPa, chlorobutane, butanol and hydrogen chloride are collected for 5 minutes, 32.2g of product is discharged from the bottom of the vaporization chamber, the purity is 89%, and the yield is 99%.
Example 5:
synthesis of n-butyl methylphosphinate
Butanol is preheated to 100 ℃ through the 1 st plate at the flow rate of 10g/min, methyl phosphine dichloride is mixed with ethanol at the 2 nd plate at the flow rate of 5g/min, the mixture enters a vaporization chamber after the mixture stays for 1 minute, the temperature of the vaporization chamber is 100 ℃, the negative pressure is-0.095 MPa, chlorobutane, butanol and hydrogen chloride are collected for 5 minutes, 30g of product is discharged from the bottom of the vaporization chamber, the purity is 95 percent, and the yield is 99 percent.
Example 6:
synthesis of n-butyl methylphosphinate
Butanol is preheated to 100 ℃ through the 1 st plate at the flow rate of 70g/min, methyl phosphine dichloride is mixed with ethanol at the 2 nd plate at the flow rate of 30g/min, after the mixture stays for 1 minute, the mixture enters a vaporization chamber at the temperature of 100 ℃ and the negative pressure of-0.095 MPa, chlorobutane, butanol and hydrogen chloride are collected for 2 minutes, 67.67g of product is discharged from the bottom of the vaporization chamber, the purity is 92 percent, and the yield is 90 percent.
The present invention has been described in detail, and it is intended to enable those skilled in the art to understand the contents and practice the present invention, and the scope of the present invention should not be limited thereto, and the present invention is not limited to the above-mentioned embodiments.
Claims (12)
1. A production facility of methyl hypophosphite, its characterized in that: comprises a continuous flow reactor (1) with a first inlet for introducing the methyl phosphine dichloride and a second inlet for introducing the alcohol, an evaporator (3) communicated with the outlet of the continuous flow reactor (1), and a first receiving tank (5) communicated with the outlet of the evaporator (3) and used for collecting the methyl hypophosphite.
2. The apparatus for producing methylphosphinic acid ester according to claim 1, wherein: the continuous flow reactor (1) is a micro-channel reactor, a pipeline reactor or a flat-plate reactor.
3. The apparatus for producing methylphosphinic acid ester according to claim 1 or 2, wherein: the continuous flow reactor (1) comprises a plurality of reaction parts (11) which are connected in series in sequence, wherein the first inlet is arranged on the second reaction part (11), and the second inlet is arranged on the first reaction part (11).
4. The apparatus for producing methylphosphinic acid ester according to claim 1 or 2, wherein: the continuous flow reactor (1) comprises a first preheating part (12) provided with the first inlet, a second preheating part (13) provided with the second inlet, and a plurality of reaction parts (11) which are communicated with the first preheating part (12) and the second preheating part (13) and are sequentially connected in series.
5. The apparatus for producing methylphosphinic acid ester according to claim 1, wherein: the production plant also comprises a first intermediate tank (2) arranged between the continuous flow reactor (1) and the evaporator (3), and a pump (4) mounted on the pipeline of the first intermediate tank (2) and the evaporator (3).
6. The apparatus for producing methylphosphinic acid ester according to claim 5, wherein: the first middle groove (2) is provided with a liquid level meter (10).
7. The apparatus for producing methylphosphinic acid ester according to claim 1, wherein: the inlet of the evaporator (3) is positioned at the upper part of the evaporator (3), and the outlet of the evaporator (3) is positioned at the lower part of the evaporator (3).
8. The apparatus for producing methylphosphinic acid ester according to claim 1, wherein: the production equipment also comprises a condenser (7) communicated with the evaporator (3), a second receiving groove (8) communicated with the condenser (7) and used for collecting byproducts, a vacuum pump (9) communicated with the second receiving groove (8), and an absorption tower communicated with the vacuum pump (9).
9. The apparatus for producing methylphosphinic acid ester according to claim 8, wherein: the first receiving groove (5) and the second receiving groove (8) are provided with liquid level meters (10).
10. The apparatus for producing methylphosphinic acid ester according to claim 8, wherein: the production equipment also comprises a second middle tank (6), wherein the upper part of the second middle tank (6) is respectively communicated with the lower part of the evaporator (3) and the inlet of the condenser (7), and the lower part of the second middle tank (6) is communicated with the first receiving tank (5) or a pipeline between the first receiving tank (5) and the evaporator (3).
11. The apparatus for producing methylphosphinic acid ester according to claim 8, wherein: the top of the first receiving groove (5) is communicated with the condenser (7).
12. The apparatus for producing methylphosphinic acid ester according to claim 1, wherein: the evaporator (3) comprises a falling film evaporator or a wiped film evaporator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021238112.8U CN212954957U (en) | 2020-06-30 | 2020-06-30 | Production equipment of methyl hypophosphite |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021238112.8U CN212954957U (en) | 2020-06-30 | 2020-06-30 | Production equipment of methyl hypophosphite |
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