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CN-116351334-B - MNMP production device and production method

CN116351334BCN 116351334 BCN116351334 BCN 116351334BCN-116351334-B

Abstract

The invention discloses a MNMP production device and a production method, which relate to the technical field of MNMP production, and comprise a reaction box, wherein a pair of material injection mechanisms are arranged above the reaction box, a connecting hose is arranged on one side of the material injection mechanisms, a feeding mechanism is arranged in the material injection mechanisms, a heating plate is fixedly connected in the reaction box, a sealing moving plate is arranged in the heating plate, a sealing ring is fixedly connected to the outer wall of the sealing moving plate, the outer wall of the sealing ring is in interference fit with the inner wall of the sealing ring, the selective improvement of a target product MNMP is attempted by increasing hydrogen pressure, the product purification treatment is facilitated greatly, and the hydrogen pressure, the temperature, the time, the raw material levulinate and methylamine are added in the hydrogenation process, so that the high-selectivity preparation of MNMP can be realized through process optimization.

Inventors

  • KE ZHUO
  • ZHAO JIA
  • GAO YING

Assignees

  • 安徽利科新材料科技有限公司

Dates

Publication Date
20260508
Application Date
20221214

Claims (7)

  1. The MNMP production device comprises a reaction box (1) and is characterized in that a pair of material injection mechanisms (3) are arranged above the reaction box (1), a connecting hose (4) is arranged on one side of each material injection mechanism (3), a feeding mechanism (5) is arranged inside each material injection mechanism (3), a heating plate (6) is fixedly connected inside each reaction box (1), a sealing moving plate (18) is arranged inside each heating plate (6), a sealing ring (19) is fixedly connected to the outer wall of each sealing moving plate (18), the outer wall of each sealing ring (19) is in interference fit with the inner wall of the reaction box (1), a filter screen plate (16) is fixedly connected to the upper side of each reaction box (1), an extension port (17) is formed in a penetrating mode on one side of the upper end face of each filter screen plate (16), an exhaust pipe (13) and a hydrogen pipe (14) are symmetrically arranged on the upper end face of each filter screen plate (16), one ends, far away from the connecting pipes (13) and the hydrogen pipes (14), of the corresponding exhaust pipes (13) penetrate through the corresponding filter screen plates (16) and the corresponding sealing moving plates (18), and the corresponding hydrogen pipes (14) are fixedly connected with the corresponding sealing moving plates (18); The material injection mechanism (3) comprises a material box (301) fixedly connected to the upper end face of a filter screen plate (16), a scale plate (302) is fixedly connected to the outer wall of the material box (301), a grid plate (303) is fixedly connected to the upper end face of the material box (301), a supporting block (310) is fixedly connected to the lower portion of an inner cavity of the material box (301), an injection pipe (305) is fixedly connected to the upper end face of the supporting block (310), a light floating plate (307) is slidably connected to the outer wall of the injection pipe (305), a silica gel ring (312) is fixedly connected to the outer wall of the light floating plate (307), and a plurality of communication holes (311) communicated with the inside of the injection pipe (305) are formed in the outer wall of the lower end of the injection pipe (305); The upper end face of the grid plate (303) is provided with a connecting port (304) in a penetrating manner, the upper end of the injection pipe (305) extends out of the connecting port (304), the upper end of the injection pipe (305) is fixedly connected with a funnel frame (306), a water outlet pipe (308) communicated with the lower part of the end face of the material box (301) away from the scale plate (302) is fixedly connected with, a combined pipe (309) is fixedly connected between the two water outlet pipes (308), and the connecting hose (4) is fixedly connected with the combined pipe (309) and communicated with each other; Feeding mechanism (5) including running through sealed fixed pipe (501) of movable plate (18) and with sealed movable plate (18) fixed connection, the lower terminal surface fixedly connected with of fixed pipe (501) is fixed plate (503) of intercommunication each other, the below of fixed plate (503) is equipped with drainage board (504), peripheral fixedly connected with fixed frame (505) between fixed plate (503) and the drainage board (504), slot (506) have been seted up to the lateral wall of drainage board (504), the inside activity grafting of slot (506) has picture peg (507), one end fixedly connected with a pair of connecting block (508) of drainage board (507) are kept away from to picture peg (507), one end fixedly connected with arc cover (509) of connecting block (508), the inside movable joint of arc cover (509) has ball-type head (510).
  2. 2. The MNMP production device according to claim 1, wherein the lower end surface of the reaction tank (1) is fixedly connected with a plurality of brackets (2), one side of the lower end surface of the reaction tank (1) is fixedly connected with a discharging pipe (12) which is communicated with the lower end surface, a stirring rod (10) is arranged below the inside of the reaction tank (1), a motor (11) is fixedly connected to the central position of the bottom of the reaction tank (1), and the output end of the motor (11) extends into the inside of the reaction tank (1) and is fixedly connected with the stirring rod (10).
  3. 3. The MNMP production device according to claim 2, wherein the upper end surface of the heating plate (6) is fixedly connected with a first limit ring (7), the lower end surface of the heating plate (6) is fixedly connected with a second limit ring (8), one side of the upper end surface of the second limit ring (8) is provided with a connecting groove (9) in a penetrating way, and the other ends of the exhaust pipe (13) and the hydrogen pipe (14) are fixedly connected with a connecting pipe (15).
  4. 4. A MNMP production device according to claim 3, wherein the upper end surface of the fixed pipe (501) is fixedly connected with a sealing valve (502) which is communicated with each other, the sealing valve (502) is fixedly connected with a connecting hose (4) and communicated with each other, a plurality of springs (511) are fixedly connected inside the slot (506), and the springs (511) are fixedly connected with the inserting plate (507).
  5. 5. A method of manufacturing an MNMP production device according to claim 4, comprising the steps of: step one, using a hydrogen source for catalyzing levulinic acid to prepare MNMP through reductive amination, carrying out catalyst-free comparison reaction, and reacting at 160 ℃ under normal pressure hydrogen condition for 6 h; step two, performing a catalyst-containing comparative reaction, and adding a catalyst to react at 160 ℃ under normal pressure hydrogen to obtain a reaction product 6 h; step three, carrying out hydrogenation comparison reaction with a catalyst, and adding the catalyst under the hydrogen conditions of different pressures for reaction; and step four, analyzing the conversion rate of levulinic acid and the MNMP selectivity, wherein the catalyst is Raney nickel.
  6. 6. The method according to claim 5, wherein in the third step, the control method for performing hydrogen conditions of different pressures is as follows: Injecting the proportioning liquid of the production reactants into the injection pipe (305) through the funnel frame (306), discharging the proportioning liquid through a plurality of communication holes (311) at the bottom of the injection pipe (305), jacking up the light floating plate (307) while the water level of the proportioning liquid rises, controlling the proportion of the proportioning liquid in the two scale plates (302) through observing the scale plates (302), installing a connecting pipe (15) on the exhaust pipe (13) on the exhaust pump after the proportioning liquid is injected, installing the connecting pipe (15) on the hydrogen pipe (14) on the hydrogen cylinder, starting the exhaust pump firstly, pumping the air in the reaction box (1) by the operation of the exhaust pump, reducing the air in the reaction box (1), moving the sealing moving plate (18) in the reaction box (1) towards the inside of the second limit ring (8) until the sealing moving plate (18) contacts the second limit ring (8), and completely vacuumizing the inside of the reaction box (1) below the second limit ring (8), wherein the inner cavity of the reaction box (1) is a liquid reaction cavity; Starting a heating plate (6) on the inner wall of the reaction box (1), wherein the heating plate (6) is in working release heat, a sealing valve (502) is fixedly connected with a connecting hose (4) and a fixed pipe (501) respectively, the connecting hose (4) is connected with a combined pipe (309), the sealing valve (502) is opened, under the action of negative pressure, the proportioning liquid in the two material boxes (301) can be sucked into the fixed pipe (501), the proportioning liquid can fall onto a drainage plate (504) along the fixed pipe (501), one end of the drainage plate (504) is movably inserted with a plugboard (507), a connecting block (508) and an arc sleeve (509) are fixed on the plugboard (507), a spherical head (510) in the arc sleeve (509) is in contact with the inner wall of the reaction box (1) so that the plugboard (507) and the inner wall of the reaction box (1) have a certain distance, the proportioning liquid flows into the bottom of the reaction box (1) along the inner wall of the drainage plate (504) and prevents the electromotor from entering the water outlet pipe (11) until the electromotor is completely inserted into the liquid cavity (307), and then the air outlet pipe (11) is prevented from entering the working space (11) to completely, and the air outlet pipe (11) is prevented from entering the bottom of the reaction box (1), the output rotates and drives puddler (10) to rotate, puddler (10) rotates and makes the ratio liquid fully fuse, afterwards open the hydrogen bottle, the inside that hydrogen entered into reaction tank (1), inside sealed movable plate (18) of reaction tank (1) moves to the inside of first spacing collar (7), until sealed movable plate (18) contact first spacing collar (7), the inside that hydrogen is full of reaction tank (1), thereby take place the reaction, sealed movable plate (18) remove and drive feeding mechanism (5) and remove, when picture peg (507) remove to hot plate (6) inside, ball-type head (510) and hot plate (6) inner wall contact, the inside of slot (506) is got into to the one end of picture peg (507), spring (511) shrink.
  7. 7. A production method according to claim 6, characterized in that between the reactions of the steps, the residues in the reaction tank (1) need to be removed by the following method: And (3) opening an air valve on the air pump to discharge hydrogen, then opening a discharge pipe (12) below the reaction box (1) to discharge reaction residues, cleaning the reaction box (1), repeating the operations from the first step to the fourth step, and recharging for production.

Description

MNMP production device and production method Technical Field The invention relates to the technical field of MNMP production, in particular to a MNMP production device and a production method. Background In order to avoid the situation that the system pressure is too high due to the fact that formic acid is used as a hydrogen source to decompose and generate CO2, the industrialized preparation of 1, 5-dimethyl-2-pyrrolidone is realized, and the hydrogen method hydrogenation process is also the cheapest hydrogenation mode in industry, so that the preparation of MNMP by using the hydrogen source catalytic hydrogenation process is attempted, and the hydrogenation catalyst source is an industrialized large-scale application hydrogenation catalyst and can be obtained in a large amount. The prior art has the following problems: The hydrogen pressure adding amount is only at a lower pressure level in the process fumbling stage, but the poor product selectivity brings great difficulty to the subsequent product purification, meanwhile, the tightness of the device is not very good, and the air inlet can influence the production result. Disclosure of Invention The invention aims to solve the problem that the production effect of the existing MNMP production device and production method is not very good, and provides the MNMP production device and production method. In order to solve the technical problems, the MNMP production device and the production method adopt the following technical scheme that the MNMP production device comprises a reaction box, a pair of material injection mechanisms are arranged above the reaction box, a connecting hose is arranged on one side of the material injection mechanisms, a feeding mechanism is arranged inside the material injection mechanisms, a heating plate is fixedly connected inside the reaction box, a sealing moving plate is arranged inside the heating plate, a sealing ring is fixedly connected to the outer wall of the sealing moving plate, the outer wall of the sealing ring is in interference fit with the inner wall of the sealing ring, a filter screen plate is fixedly connected to the upper side of the inner part of the reaction box, an extension opening is formed in one side of the upper end face of the filter screen plate in a penetrating way, an exhaust pipe and a hydrogen pipe are symmetrically arranged on the upper end face of the filter screen plate, one ends of the exhaust pipe and the hydrogen pipe, which are far away from a connecting pipe, respectively penetrate the filter screen plate and the sealing moving plate, and the exhaust pipe and the hydrogen pipe are fixedly connected with the sealing moving plate. Preferably, the lower terminal surface fixedly connected with a plurality of supports of reaction tank, one side fixedly connected with of terminal surface is linked together down to the reaction tank, the below of reaction tank inside is equipped with the puddler, the central point of reaction tank bottom puts fixedly connected with motor, the output of motor extends into the inside of reaction tank and with puddler fixed connection, the up end fixedly connected with first spacing collar of hot plate, the lower terminal surface fixedly connected with second spacing collar of hot plate, the spread groove has been seted up in one side of second spacing collar terminal surface, the equal fixedly connected with connecting pipe of the other end of exhaust tube and hydrogen pipe. Preferably, the material injection mechanism comprises a material box fixedly connected to the upper end face of the filter screen plate, a scale plate is fixedly connected to the outer wall of the material box, a grid plate is fixedly connected to the upper end face of the material box, a supporting block is fixedly connected to the lower portion of an inner cavity of the material box, an injection pipe is fixedly connected to the upper end face of the supporting block, a light floating plate is slidably connected to the outer wall of the injection pipe, a silica gel ring is fixedly connected to the outer wall of the light floating plate, a plurality of communication holes communicated with the inside of the injection pipe are formed in the outer wall of the lower end of the injection pipe, a connecting port is formed in the upper end face of the grid plate in a penetrating mode, a connecting port extends out of the upper end of the injection pipe, a funnel frame is fixedly connected to the upper end of the injection pipe, a water outlet pipe communicated with the lower end face of the material box, a combination pipe is fixedly connected between the two water outlet pipes, and the connection hose is fixedly connected to the combination pipe. Preferably, the feeding mechanism comprises a fixed pipe penetrating through the sealing moving plate and fixedly connected with the sealing moving plate, a fixed plate communicated with each other is fixedly connected to the lower end face of the fixe