Glyphosate continuous rectification device
By designing a continuous distillation unit for glyphosate, and adopting gas-phase inlet and stepwise distillation, the problems of high cost and low automation in the treatment of glyphosate desolvation products were solved, and a highly efficient separation and safe and reliable production process was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- HENAN HDF CHEM CO LTD
- Filing Date
- 2025-06-06
- Publication Date
- 2026-05-12
AI Technical Summary
Existing glyphosate desolvation product treatment processes are characterized by high costs, low automation, poor separation efficiency, and potential safety hazards and errors.
Design a continuous distillation unit including a methyl acetal distillation column and a methanol distillation column. Employ a vapor-phase feed method and combine online measuring equipment and a reboiler to achieve stepwise distillation, reduce preheating requirements, and improve automation and control precision.
It achieves efficient and thorough separation, reduces heating costs and equipment investment, improves automation, and reduces safety hazards and errors caused by human operation.
Smart Images
Figure CN224220769U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of chemical technology, specifically relating to a glyphosate continuous distillation device. Background Technology
[0002] Glyphosate possesses superior performance due to its high efficiency, low toxicity, broad spectrum, and non-selective nature. Domestically, glyphosate is primarily produced via the alkyl ester method. Specifically, this involves the addition and condensation of glycine, dimethyl phosphite, and paraformaldehyde as raw materials to prepare a synthetic solution. This solution is then fed into a hydrolysis reactor, where hydrolysis and solvent removal are performed using hydrochloric acid. Finally, alkali is added for crystallization. In the solvent removal process, the most common method involves condensing the product in a condenser to form acidic methanol, which is then further neutralized before being separated in a methyl acetal distillation column and a methanol distillation column. This method is used in specific applications... During operation, the liquid entering the tower is at a low temperature, requiring the installation of preheaters and other equipment for preheating, which increases the cost. Furthermore, due to the low level of automation in existing equipment, manual on-site operation and sampling are often required during the adjustment of tower efficiency and flow rate, which poses certain risks and errors. Therefore, in order to improve the separation and treatment of glyphosate desolvation products and solve the problems of high consumption costs, low automation, and poor separation effect in the treatment of desolvation products, it is necessary to develop a glyphosate continuous distillation unit with a highly efficient and reasonable overall design and good performance. Utility Model Content
[0003] The purpose of this invention is to overcome the shortcomings of the prior art and provide a glyphosate continuous distillation device with an efficient and reasonable overall design and good performance.
[0004] The purpose of this utility model is achieved as follows: A continuous glyphosate distillation device includes a methylal distillation column and a methanol distillation column. The methylal distillation column has a gas inlet pipe connected to the middle of its side end, a reboiler a connected to its bottom, and a first condenser connected to its top. The upper and lower ends of the reboiler a are each equipped with a first packing layer. An online gas flow meter, a gas composition analyzer, and a control valve are installed on the gas inlet pipe. A methylal measuring device is installed on the connecting pipe between the reboiler a and the methylal distillation column. The reboiler a has a steam inlet pipe at its lower left end, a steam outlet pipe at its upper right end, and a material outlet pipe at its bottom, connected to a buffer tank. An exhaust pipe is located on the upper right side of the first condenser, connected to a chloromethane purification device. A first reflux tank is connected to the lower end of the first reflux tank. A first reflux pipe is located on the lower left side of the first reflux tank, and a methylal outlet pipe is located on the lower right side of the first reflux tank. The first reflux pipe is connected to the top of the methyl acetal distillation column via a circulation pump; a transfer pump is installed on the side of the buffer tank, and the transfer pump connects the buffer tank to the feed inlet at the middle of the side of the methanol distillation column; reboilers b are installed on both sides of the bottom of the methanol distillation column, and a second condenser is connected to the top. The upper and lower ends of the reboiler b are provided with a second packing layer. The reboiler b has the same structure as the reboiler a, and a wastewater outlet pipe is provided at the bottom of the reboiler b. A methanol measuring device, a COD measuring device, and an acidity measuring device are installed sequentially on the connecting pipe between the reboiler b and the methanol distillation column; a tail gas pipe is provided on the right side of the upper end of the second condenser, and the tail gas pipe is connected to a tail gas treatment device. A second reflux tank is connected to the lower end of the second reflux tank. A second reflux pipe is installed on the left side of the lower end of the second reflux tank, and a methanol outlet pipe is installed on the right side of the lower end. The second reflux pipe is connected to the top of the methanol distillation column via a circulation pump.
[0005] Furthermore, both the methyl acetal distillation column and the methanol distillation column are fitted with an insulation layer.
[0006] Furthermore, both the methyl acetal distillation column and the methanol distillation column are equipped with demisters at their top ends.
[0007] Furthermore, online thermometers are installed at the bottom, middle, and top of both the methyl acetal distillation column and the methanol distillation column.
[0008] Furthermore, a gas composition measuring device is installed on the exhaust pipe.
[0009] Furthermore, a methyl acetal content analyzer is installed at the upper end of the first reflux tank.
[0010] Furthermore, a methanol content analyzer is installed at the upper end of the second reflux tank.
[0011] Furthermore, the first condensing device and the second condensing device have the same structure, both consisting of multiple sets of tubular condensers, and the condensing medium inside is chilled brine.
[0012] The beneficial effects of this invention are as follows: By setting up a methyl acetal distillation column and a methanol distillation column, the gas generated during desolventizing is first injected into the methyl acetal distillation column to separate chloromethane and methyl acetal. Then, the bottom liquid of the methyl acetal distillation column is injected into the methanol distillation column to separate methanol and water. By using a stepwise distillation process, the separation is more thorough and the purity of the separated products is improved. At the same time, this invention adopts a gas phase inlet method, which reduces the preheating of materials and saves heating costs and equipment investment. Furthermore, by setting up two reboilers b, this invention can improve the distillation efficiency of the methanol distillation column.
[0013] This invention, through the setup of a methylal measuring device, a gas composition measuring device, a methylal content measuring instrument, a methanol measuring device, a COD measuring device, an acidity measuring device, an online thermometer, an online gas flow meter, a gas composition analysis device, and control valves, allows for real-time measurement and analysis of reaction process data through various online measuring devices. While achieving a high degree of automation, it also improves the accuracy of control and adjustment, and reduces the safety hazards and errors associated with human sampling. Overall, this invention has the advantages of efficient and reasonable overall design and good performance. Attached Figure Description
[0014] Figure 1 This is a flowchart illustrating the structure of this utility model.
[0015] Figure 2 This is a structural connection diagram of the methyl acetal distillation column, reboiler a, first condenser, first reflux tank, buffer tank and transfer pump in this utility model.
[0016] Figure 3 This is a structural connection diagram of the transfer pump, methanol distillation column, reboiler b, second condenser and second reflux tank in this utility model.
[0017] In the diagram: 1. Methyl acetal distillation column; 11. Gas inlet pipe; 12. First packing layer; 2. Methanol distillation column; 21. Second packing layer; 3. Reboiler a; 31. Methyl acetal measuring device; 32. Material outlet pipe; 4. First condenser; 41. Exhaust pipe; 42. Gas composition measuring device; 5. Buffer tank; 51. Transfer pump; 6. First reflux tank; 61. First reflux pipe; 62. Methyl acetal content analyzer; 7. Reboiler b; 71. Wastewater outlet pipe; 72. Methanol measuring device; 73. COD measuring device; 74. Acidity measuring device; 8. Second condenser; 81. Tail gas pipe; 9. Second reflux tank; 91. Second reflux pipe; 92. Methanol content analyzer; 0. Demister. Detailed Implementation
[0018] The present invention will be further described below with reference to the accompanying drawings.
[0019] Example: Figure 1 , Figure 2 , Figure 3As shown, a glyphosate continuous distillation apparatus includes a methylal distillation column 1 and a methanol distillation column 2. The methylal distillation column 1 has a gas inlet pipe 11 connected to the middle of its side end, a reboiler a3 connected to its bottom, and a first condenser 4 connected to its top. The upper and lower ends of the column are each provided with a first packing layer 12. An online gas flow meter, a gas composition analyzer, and control valves are installed on the gas inlet pipe 11. A methylal measuring device is installed on the connecting pipe between the reboiler a3 and the methylal distillation column 1. The reboiler a3 is equipped with a steam inlet pipe at its lower left end, a steam outlet pipe at its upper right end, and a material outlet pipe 32 at its bottom. A buffer tank 5 is connected to the material outlet pipe 32. An exhaust pipe 41 is located on the upper right side of the first condensing device 4, and is connected to a chloromethane purification device. A first reflux tank 6 is connected to the lower end of the first reflux tank 6. A first reflux pipe 61 is located on the lower left side of the first reflux tank 6, and a formaldehyde outlet pipe is located on the lower right side of the first reflux tank 6. The buffer tank 5 is connected to the top of the methyl acetal distillation column 1 via a circulating pump; a transfer pump 51 is installed on the side of the buffer tank 5, which connects it to the feed inlet at the middle of the side of the methanol distillation column 2; reboilers b7 are installed on both sides of the bottom of the methanol distillation column 2, and a second condenser 8 is connected to the top. A second packing layer 21 is provided at the upper and lower ends of the reboiler b7. The reboiler b7 has the same structure as the reboiler a3, and a wastewater outlet pipe 71 is provided at the bottom of the reboiler b7. A methanol measuring device 72, a COD measuring device 73, and an acidity measuring device 74 are sequentially installed on the connecting pipe between the methanol distillation columns 2; a tail gas pipe 81 is provided on the right side of the upper end of the second condensation device 8, and the tail gas pipe 81 is connected to a tail gas treatment device. A second reflux tank 9 is connected to the lower end of the second reflux tank 9. A second reflux pipe 91 is provided on the left side of the lower end of the second reflux tank 9, and a methanol discharge pipe is provided on the right side of the lower end. The second reflux pipe 91 is connected to the top of the methanol distillation column 2 through a circulation pump.
[0020] Both the methyl acetal distillation column 1 and the methanol distillation column 2 are externally fitted with insulation layers; both the methyl acetal distillation column 1 and the methanol distillation column 2 are equipped with demisters 0 at their top interiors; both the methyl acetal distillation column 1 and the methanol distillation column 2 are equipped with online thermometers at their bottom, middle, and top; a gas composition measuring device 42 is installed on the exhaust pipe 41; a methyl acetal content analyzer 62 is installed at the top of the first reflux tank 6; a methanol content analyzer 92 is installed at the top of the second reflux tank 9; the first condensing device 4 and the second condensing device 8 have the same structure, both consisting of multiple sets of tubular condensers, and the internal condensing medium is chilled brine.
[0021] In use, this invention first injects the gas generated from solvent removal into the interior of the methyl acetal distillation column 1 via the gas phase inlet pipe 11. Then, with the combined action of the reboiler a3 and the methyl acetal distillation column 1, the gas generated from solvent removal is subjected to distillation. The mixed gas of methyl acetal and chloromethane produced during distillation is injected into the first condenser 4 through the gas phase outlet at the top of the methyl acetal distillation column 1. The methyl acetal and chloromethane are then separated by the condensation action of the first condenser 4. During this process, the chloromethane gas is sent to the chloromethane purification treatment device via the exhaust pipe 41 for further cooling. The condensed methylal is injected into the first reflux tank 6. Then, the methylal content in the solution inside the first reflux tank 6 is detected using a methylal content analyzer 62, and the methylal is purified using the first reflux pipe 61. After the methylal content in the solution is deemed acceptable, the methylal is discharged through the methylal discharge pipe. Simultaneously, the bottom liquid of the methylal distillation column 1 is injected into the methanol distillation column 2 via the material collection pipe 32 and buffer tank 5, driven by the transfer pump 51. Finally, the liquid is discharged through the reboiler b7 and the methanol distillation column 2. Under the combined action of the two systems, the solution injected into the methanol distillation column 2 undergoes a distillation operation. The methanol gas produced during distillation is injected into the second condenser 8 through the gas phase outlet at the top of the methanol distillation column 2, where it is condensed to form a methanol solution. This methanol solution is then injected into the second reflux tank 9. Using a methanol content analyzer 92 and the second reflux pipe 91, the methanol is purified. Once the methanol content in the solution meets the requirements, the methanol is discharged through the methanol discharge pipe. Simultaneously, during the distillation process in the methanol distillation column 2... The bottom liquid of the column is sent to the sewage treatment plant for treatment through the wastewater collection pipe. This utility model adopts this structure, which uses the combination of methyl acetal distillation column 1 and methanol distillation column 2. First, the gas generated by desolventizing is injected into the methyl acetal distillation column 1 to separate chloromethane and methyl acetal. Then, the bottom liquid of the methyl acetal distillation column 1 is injected into the methanol distillation column 2 to separate methanol and water. In this way, the separation is more thorough and the purity of the separated products is improved by using a stepwise distillation process. In addition, the use of gas phase inlet reduces the preheating of materials and saves heating costs and equipment investment.
[0022] This invention, through the setup of a methylal measuring device 31, a gas composition measuring device 42, a methylal content measuring instrument 62, a methanol measuring device 72, a COD measuring device 73, an acidity measuring device 74, a methanol content measuring instrument 92, an online thermometer, an online gas flow meter, a gas composition analysis device, and control valves, allows for real-time measurement and analysis of reaction process data through various online measuring devices. This high degree of automation improves the accuracy of control and adjustment, and reduces the safety hazards and errors associated with manual sampling. Overall, this invention boasts the advantages of efficient and reasonable overall design and excellent performance.
[0023] The above embodiments are only used to illustrate the technical solution of this utility model and are not intended to limit it. Although the utility model has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of this utility model without departing from the spirit and scope of this utility model. Any modifications or equivalent substitutions should be covered within the scope of the claims of this utility model.
Claims
1. A glyphosate continuous distillation apparatus, comprising a methyl acetal distillation column (1) and a methanol distillation column (2), characterized in that: The methyl acetal distillation column (1) has a gas inlet pipe (11) connected to the middle of its side end, a reboiler a (3) connected to its bottom, and a first condenser device (4) connected to its top. The upper and lower ends of the column are each equipped with a first packing layer (12). An online gas flow meter, a gas composition analyzer, and control valves are installed on the gas inlet pipe (11). A methyl acetal measuring device (31) is installed on the connecting pipe between the reboiler a (3) and the methyl acetal distillation column (1). A steam inlet pipe is located at the lower left end of the reboiler a (3), and a steam inlet pipe is located at the upper right end. The steam outlet pipe is provided with a material outlet pipe (32) at the bottom and a buffer tank (5) is connected to the material outlet pipe (32). An exhaust pipe (41) is provided on the right side of the upper end of the first condensing device (4), and the exhaust pipe (41) is connected to a chloromethane purification treatment device. A first reflux tank (6) is connected to the lower end. A first reflux pipe (61) is provided on the left side of the lower end of the first reflux tank (6), and a methylal discharge pipe is provided on the right side of the lower end. The first reflux pipe (61) is connected to the top of the methylal distillation column (1) through a circulating pump. The buffer tank (5) is equipped with a transfer pump (51) on its side, and the transfer pump (51) connects it to the feed inlet at the middle of the side of the methanol distillation column (2); both sides of the bottom of the methanol distillation column (2) are equipped with reboilers b (7), and the top is connected to a second condenser (8). The upper and lower ends of the interior are equipped with a second packing layer (21). The reboiler b (7) has the same structure as the reboiler a (3), and the bottom of the reboiler b (7) is equipped with a wastewater outlet pipe (71), which connects it to the methanol distillation column (2). A methanol measuring device (72), a COD measuring device (73), and an acidity measuring device (74) are installed sequentially on the connecting pipe; a tail gas pipe (81) is provided on the right side of the upper end of the second condensing device (8), and the tail gas pipe (81) is connected to a tail gas treatment device, and a second reflux tank (9) is connected to the lower end. A second reflux pipe (91) is provided on the left side of the lower end of the second reflux tank (9), and a methanol discharge pipe is provided on the right side of the lower end. The second reflux pipe (91) is connected to the top of the methanol distillation tower (2) through a circulating pump.
2. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: Both the methyl acetal distillation column (1) and the methanol distillation column (2) are covered with an insulation layer.
3. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: Demisters (0) are installed at the top of both the methyl acetal distillation column (1) and the methanol distillation column (2).
4. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: Online thermometers are installed at the bottom, middle and top of the methyl acetal distillation column (1) and the methanol distillation column (2).
5. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: A gas composition measuring device (42) is installed on the exhaust pipe (41).
6. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: The upper end of the first reflux tank (6) is equipped with a formaldehyde content analyzer (62).
7. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: A methanol content analyzer (92) is installed at the upper end of the second reflux tank (9).
8. The glyphosate continuous distillation apparatus as described in claim 1, characterized in that: The first condensing device (4) and the second condensing device (8) have the same structure, both consisting of multiple sets of tubular condensers, and the condensing medium inside is frozen brine.