A continuous production device

Abstract

The present invention discloses a continuous production device for quaternization reaction, including a gas cylinder, a first storage tank, a second storage tank, a third storage tank, a first tubular reactor, a second tubular reactor group, a connecting pipe, a thermometer and / or a pressure gauge and / or a sampling valve arranged on the connecting pipe; the first tubular reactor includes a first shell, a first reaction tube, and a first static mixing unit; the gas cylinder, the first storage tank, and the second storage tank are all connected to the inlet of the first tubular reactor; the second tubular reactor group includes a plurality of second tubular reactors connected in series in sequence, each second tubular reactor includes a second shell, a second reaction tube, and a second static mixing unit; the second storage tank and the third storage tank are respectively connected to the inlet of each second tubular reactor; the connecting pipe is used to connect adjacent tubular reactors. The device of the present invention adjusts the temperature and material concentration separately, adjusts the reaction conditions according to the reaction progress, and can improve the reaction speed in the later stage.

Description

Technical Field

[0001] The invention relates to the technical field of chemical equipment, and in particular to a continuous production device. Background Art

[0002] Continuous tubular reactors are an important type of production equipment in chemical equipment. Traditional continuous tubular reactors include fluidized beds, fixed beds, supergravity, drying towers, distillation towers, etc. In addition, chemical reactions with fast reaction speeds and short times are also achieved using simple tubular reactors. However, most products cannot be produced continuously due to long reaction times, lack of continuous parameters, or the need for intermittent additions. Unfavorable factors such as high human error rates, unstable quality, high amounts of three wastes, and high safety risks in intermittent production have long tormented production managers, so continuous research has almost never stopped, especially in recent years, due to increased environmental protection and safety pressures, continuous research has once again become popular.

[0003] For continuous production of quaternization reaction, all raw materials are usually mixed together before production. Directly adding solvent to the reaction raw materials will cause the concentration of ester tertiary amine monomer and quaternization agent in the reaction to be too low, making the reaction speed slower; at the same time, since ester tertiary amine monomer and quaternization agent are easy to hydrolyze, it will also have a certain negative impact on the reaction.

[0004] Existing continuous production devices generally have the following defects: lack of attention to the process changes of materials in the device. At this time, the reaction conditions should be adjusted according to the progress of the reaction, and the reaction concentration needs to be intervened and the reaction rate (parameters such as temperature or pressure) needs to be adjusted according to the progress; the continuous device needs to have operational flexibility to adapt to the adjustment of product indicators and the change in reaction rate caused by changes in raw material concentration, so as to adapt to or be compatible with a type of reaction; a constant pressure needs to be maintained in the continuous device, especially when easily vaporized raw materials are involved in the reaction. Summary of the invention

[0005] The purpose of the present invention is to provide a continuous production device, which divides the reaction process into multiple sections and has high operation flexibility. By adjusting the temperature and material concentration separately, the reaction conditions are adjusted in real time according to the reaction progress, so that the reaction speed in the later stage can be improved and the reaction time can be further shortened. By adjusting the addition timing and addition amount of the solvent, the concentration of the ester tertiary amine monomer and the quaternary ammonium agent during the reaction is guaranteed, the efficiency of the quaternary ammonium reaction is improved, and the negative impact of the direct addition of the solvent on the quaternary ammonium reaction is avoided.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is:

[0007] A continuous production device for quaternization reaction, comprising:

[0008] A gas cylinder, wherein the gas cylinder is used to store oxygen or air;

[0009] A first storage tank, wherein the first storage tank is used to store ester tertiary amine monomers;

[0010] A second storage tank, the second storage tank is used to store the quaternary ammonium agent;

[0011] A third storage tank, wherein the third storage tank is used to store water and / or alcohol and / or catalyst;

[0012] a first tubular reactor, the first tubular reactor comprising a first shell, a first reaction tube detachably disposed in the first shell, and a first static mixing unit detachably disposed in the first reaction tube; the gas cylinder, the first storage tank, and the second storage tank are all connected to the inlet of the first tubular reactor;

[0013] a second tubular reactor group, wherein the second tubular reactor group comprises a plurality of second tubular reactors connected in series in sequence, each of the second tubular reactors comprises a second shell, a second reaction tube detachably disposed in the second shell, and a second static mixing unit detachably disposed in the second reaction tube; the second storage tank and the third storage tank are respectively connected to the inlet of each second tubular reactor;

[0014] A connecting pipe, the connecting pipe is used to connect the first reaction tube and the second reaction tube located at the inlet of the second tubular reactor group; the connecting pipe is also used to connect two adjacent second reaction tubes;

[0015] A thermometer and / or a pressure gauge and / or a sampling valve is arranged on the connecting pipe.

[0016] Preferably, the first tubular reactor further includes a first heat exchange mechanism disposed in the first shell, and the second tubular reactor further includes a second heat exchange mechanism disposed in the second shell.

[0017] Preferably, the device further comprises a third heat exchange mechanism for exchanging heat for the medium in the first storage tank.

[0018] Preferably, the device further comprises a discharge pipe connected to the outlet of the second tubular reactor group, and a back pressure valve arranged on the discharge pipe.

[0019] Preferably, the device also includes a metering mechanism arranged between the gas cylinder and the first tubular reactor, a first flow regulating mechanism arranged between the first storage tank and the first tubular reactor, a second flow regulating mechanism arranged one-to-one between the second storage tank and the first tubular reactor / the second tubular reactor, and a third flow regulating mechanism arranged one-to-one between the third storage tank and the second tubular reactor.

[0020] Preferably, the first reaction tube comprises a plurality of mutually parallel first straight tubes and a first curved tube connected between two adjacent first straight tubes; the second reaction tube comprises a plurality of mutually parallel second straight tubes and a second curved tube connected between two adjacent second straight tubes.

[0021] Preferably, the inner diameters of the first reaction tube and the second reaction tube are the same, and the ratio of the total length of the first reaction tube and the plurality of second reaction tubes to the inner diameter is less than 2×10 5 .

[0022] More preferably, the ratio of the total length of the first reaction tube and the plurality of the second reaction tubes to the inner diameter is 20-2×10 5 .

[0023] Preferably, the total length of the first reaction tube and the plurality of second reaction tubes is 1-1000 m; the inner diameters of the first reaction tube and the second reaction tube are the same, both of which are 5-50 mm.

[0024] Due to the application of the above technical scheme, the present invention has the following advantages compared with the prior art: a continuous production device of the present invention divides the reaction process into multiple sections and has high operational flexibility. By adjusting the temperature and material concentration separately, the reaction conditions are adjusted in real time according to the reaction progress, which can improve the reaction speed in the later stage and further shorten the reaction time; by adjusting the timing and amount of adding the solvent, the concentration of the ester tertiary amine monomer and the quaternary ammonium agent during the reaction is guaranteed, the efficiency of the quaternary ammonium reaction is improved, and the negative impact of directly adding the solvent on the quaternary ammonium reaction is avoided; the reaction pressure in the reaction tube is controlled by a back pressure valve to maintain a constant reaction pressure so that the easily vaporized raw material can remain in a liquefied state; the reaction tube adopts a straight tube type, which is convenient for installing a static mixing unit, so that the material in the reaction tube is always in a turbulent state, the mixing is strengthened, and the residence time is also shortened; the reaction tube is detachably arranged in the shell, so that it is possible to disassemble and clean it at any time; through these improvements, a continuous production device of the present invention has the advantages of large operational flexibility, strong versatility, high reaction efficiency and low use cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Attached Figure 1 It is a schematic diagram of the structure of the device of the present invention.

[0026] Among them: 1. gas cylinder; 2. first storage tank; 3. second storage tank; 4. third storage tank; 5. first shell; 6. first reaction tube; 7. second shell; 8. second reaction tube; 9. connecting pipe; 10. thermometer; 11. pressure gauge; 12. sampling valve; 13. discharge pipe; 14. back pressure valve; 15. metering mechanism; 16. first flow regulating mechanism; 17. second flow regulating mechanism; 18. third flow regulating mechanism. DETAILED DESCRIPTION

[0027] The technical solution of the present invention is further described below in conjunction with the accompanying drawings.

[0028] See also Figure 1 As shown, the above-mentioned continuous production device is used for quaternization reaction and has the advantages of less backmixing, high volume ratio, easy operation, environmental protection and safety.

[0029] The above-mentioned continuous production device includes a gas cylinder 1 for storing oxygen or air, a first storage tank 2 for storing ester tertiary amine monomers, a second storage tank 3 for storing quaternary ammonium agents, and a third storage tank 4 for storing water and / or alcohol and / or catalysts. Obviously, according to actual production needs, there can be multiple first storage tanks 2, second storage tanks 3 and third storage tanks 4. Since the amount of ester tertiary amine monomers in the reaction in the first storage tank 2 is relatively large, the device also includes a third heat exchange mechanism for heat exchange for the ester tertiary amine monomers in the first storage tank 2. By setting the third heat exchange mechanism, the temperature of the ester tertiary amine monomers can be increased or decreased to the temperature required for the reaction. By setting the gas cylinder 1 to pass air or oxygen into the reactants, the polymerization of the product can be effectively prevented.

[0030] The above-mentioned continuous production device also includes a first tubular reactor, which includes a first shell 5, a first reaction tube 6 detachably arranged in the first shell 5, and a first static mixing unit detachably arranged in the first reaction tube 6. The gas cylinder 1, the first storage tank 2 and the second storage tank 3 are all connected to the inlet of the first tubular reactor. In the present embodiment, the first reaction tube 6 includes a plurality of mutually parallel first straight tubes and a first elbow connected between two adjacent first straight tubes. By setting the first reaction tube 6 as a straight tube, it is convenient to install the first static mixing unit, so that the material in the first reaction tube 6 is always in a turbulent state, the mixing of the material is strengthened, and the residence time is also shortened. Since in the quaternization reaction, the raw materials are easily polymerized into a rubber block in the reaction tube, if there is no flexible detachable structure, once the polymerization is carried out in the reaction tube, the entire continuous production will stop and the equipment will also be scrapped. Therefore, the first reaction tube 6 is set to a detachable structure, which can effectively avoid the occurrence of this problem, not only can the reaction tube with the rubber block be removed in a targeted manner, but also can ensure the continuous production of continuous production, avoiding the problem of equipment scrapping.

[0031] The above-mentioned continuous production device also includes a second tubular reactor group, which includes a plurality of second tubular reactors connected in series, each of which includes a second shell 7, a second reaction tube 8 detachably arranged in the second shell 7, and a second static mixing unit detachably arranged in the second reaction tube 8. The second storage tank 3 and the third storage tank 4 are respectively connected to the inlet of each second tubular reactor. Through this arrangement, only the ester tertiary amine monomer and the quaternary ammonium agent react in the first reaction tube 6, which ensures the concentration of the ester tertiary amine monomer and the quaternary ammonium agent during the reaction, improves the efficiency of the quaternary ammonium reaction, and avoids the negative impact of directly adding solvent on the quaternary ammonium reaction. In this embodiment, the second reaction tube 8 includes a plurality of second straight tubes parallel to each other and a second curved tube connected between two adjacent second straight tubes. By setting the second reaction tube 8 as a straight tube, it is convenient to install the second static mixing unit, so that the material in the second reaction tube 8 is always in a turbulent state, strengthens the mixing of the material, and shortens the residence time. Since the raw materials are easily polymerized into rubber blocks in the reaction tube during the quaternization reaction, if there is no flexibly detachable structure, once the polymerized materials are in the reaction tube, the entire continuous production will stop and the equipment will be scrapped. Therefore, setting the second reaction tube 8 as a detachable structure can effectively avoid the occurrence of this problem. Not only can the reaction tube with rubber blocks be removed in a targeted manner, but also the continuous production can be ensured, thus avoiding the problem of equipment scrapping.

[0032] The above-mentioned continuous production device further comprises a connecting pipe 9, a thermometer 10 and / or a pressure gauge 11 and / or a sampling valve 12 arranged on the connecting pipe 9. Obviously, there are multiple connecting pipes 9. The connecting pipe 9 is used to connect the first reaction tube 6 and the second reaction tube 8 (i.e., Figure 1 The connecting pipe 9 is also used to connect two adjacent second reaction tubes 8, so that all the second reaction tubes 8 in the entire second tubular reactor group are connected in series. In this embodiment, the sampling valve 12 is a needle valve.

[0033] The first tubular reactor further includes a first heat exchange mechanism disposed in the first shell 5, and the second tubular reactor further includes a second heat exchange mechanism disposed in the second shell 7. By providing the first heat exchange mechanism and the second heat exchange mechanism, the materials in the first reaction tube 6 and the second reaction tube 8 can be respectively heat exchanged in real time.

[0034] The above-mentioned continuous production device also includes a metering mechanism 15 disposed between the gas cylinder 1 and the first tubular reactor, a first flow regulating mechanism 16 disposed between the first storage tank 2 and the first tubular reactor, a second flow regulating mechanism 17 disposed one-to-one between the second storage tank 3 and the first tubular reactor / the second tubular reactor, and a third flow regulating mechanism 18 disposed one-to-one between the third storage tank 4 and the second tubular reactor. In this embodiment, the metering mechanism 15 is a flow meter; the first flow regulating mechanism 16, the second flow regulating mechanism 17, and the third flow regulating mechanism 18 are all metering pumps.

[0035] By adjusting the temperature and material concentration in the reaction tube separately and adjusting the reaction conditions in real time according to the progress of the reaction, the reaction speed in the later stage can be increased and the reaction time can be further shortened. The continuous production device of the present invention has operational flexibility, can adapt to the adjustment of product indicators, can adapt to the change of reaction speed caused by the change of raw material concentration, and can therefore adapt to or be compatible with a class of reactions.

[0036] The above-mentioned continuous production device also includes an outlet (i.e. Figure 1 The discharge pipe 13 is connected to the second reaction tube 8 at the top, and the back pressure valve 14 is arranged on the discharge pipe 13. The reaction pressure in the reaction tube is controlled by the back pressure valve 14 to maintain a constant reaction pressure so that the easily vaporizable raw material can remain in a liquefied state.

[0037] The inner diameters of the first reaction tube 6 and the second reaction tube 8 are the same, and the ratio of the total length of the first reaction tube 6 and the plurality of second reaction tubes 8 to the inner diameter is less than 2×10 5 In this embodiment, the ratio of the total length to the inner diameter of the first reaction tube 6 and the plurality of second reaction tubes 8 is 20-2×10 5Since the inner diameter of the reaction tube is less than 5mm, it does not meet the production conditions and cannot meet the characteristics of easy polymerization of the product in this project; at the same time, the inner diameter of the reaction tube is more than 50mm, which will lead to too large production capacity and does not meet the characteristics of this type of product; finally, the length of the reaction tube corresponds to the residence time. In order to ensure the appropriate residence time, the tube length cannot exceed 1-1000 meters. The above ratio parameters are derived from this.

[0038] Specifically, the total length of the first reaction tube 6 and the plurality of second reaction tubes 8 is 1-1000m. Since the length of the reaction tube corresponds to the residence time, if the residence time of the material in the reaction tube is too short, the reaction is incomplete; if the residence time is too long, the material will hydrolyze or polymerize. A suitable flow rate is required to ensure turbulence. The combination of the two gives the above-mentioned range of reaction tube lengths. The inner diameters of the first reaction tube 6 and the second reaction tube 8 are both 5-50mm. If the inner diameter of the reaction tube is too small, the static mixing unit is difficult to install, and once the material is polymerized, it cannot be cleaned. If it is too thin, it has no economic value, and even if it is used for a small test, there is no data significance. If the inner diameter of the reaction tube is too large, it is easy to cause heat exchange to be too late, and the advantages of the tubular reactor cannot be reflected. In addition, the inner diameter of the reaction tube is also related to the production capacity. If the inner diameter is too large, the production capacity exceeds the production capacity of the industry. The above-mentioned range of values ​​is thus obtained.

[0039] In this embodiment, the first static mixing unit and the second static mixing unit are selected from one or more of SV type, SK type, SX type, SL type, SH type, SN type, or other shapes that guide fluid mixing. In this embodiment, SK type is preferred.

[0040] In this embodiment, the first reaction tube 6, the second reaction tube 8, the connecting tube 9, and the discharge pipe 13 are made of one or more of pure titanium material, titanium alloy material, Hastelloy C276 alloy material, austenitic stainless steel material, 2205 duplex stainless steel material, enamel material, and polytetrafluoroethylene material.

[0041] In this embodiment, the connection method between the first reaction tube 6, the second reaction tube 8, the connecting tube 9, the gas cylinder 1, the first storage tank 2, the second storage tank 3, the third storage tank 4, and the metering pump is selected from one or more of flange connection, ferrule connection, thread connection, and welding.

[0042] In actual operation, the temperature of each tubular reactor and the flow rate of each raw material or solvent entering each tubular reactor are adjusted accordingly according to the index of the sample taken out from the sampling valve 12. If the index of the sample in a tubular reactor meets the requirements, the redundant tubular reactor is removed. If the content of the quaternary ammonium agent in the index of the sample in a tubular reactor is lower than the set value or close to complete reaction, part of the pipeline in the tubular reactor needs to be removed.

[0043] Obviously, by adjusting the temperature in each tubular reactor and the flow rate of the corresponding metering pump, the reaction speed can be accelerated and the number of tubular reactors can be further reduced.

[0044] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with this technology to understand the content of the present invention and implement it. They cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A continuous production device for quaternization reaction, characterized in that: The device comprises: A gas cylinder, wherein the gas cylinder is used to store oxygen or air; A first storage tank, wherein the first storage tank is used to store ester tertiary amine monomers; A second storage tank, the second storage tank is used to store the quaternary ammonium agent; A third storage tank, wherein the third storage tank is used to store water and / or alcohol and / or catalyst; a first tubular reactor, the first tubular reactor comprising a first shell, a first reaction tube detachably disposed in the first shell, and a first static mixing unit detachably disposed in the first reaction tube; the gas cylinder, the first storage tank, and the second storage tank are all connected to the inlet of the first tubular reactor; a second tubular reactor group, wherein the second tubular reactor group comprises a plurality of second tubular reactors connected in series in sequence, each of the second tubular reactors comprises a second shell, a second reaction tube detachably disposed in the second shell, and a second static mixing unit detachably disposed in the second reaction tube; the second storage tank and the third storage tank are respectively connected to the inlet of each second tubular reactor; A connecting pipe, the connecting pipe is used to connect the first reaction tube and the second reaction tube located at the inlet of the second tubular reactor group; the connecting pipe is also used to connect two adjacent second reaction tubes; A thermometer and / or a pressure gauge and / or a sampling valve provided on the connecting pipe; The first reaction tube comprises a plurality of mutually parallel first straight tubes and a first curved tube connected between two adjacent first straight tubes; the second reaction tube comprises a plurality of mutually parallel second straight tubes and a second curved tube connected between two adjacent second straight tubes; The first reaction tube is detachable so as to specifically remove the reaction tube with the rubber block to ensure the continuous production; The second reaction tube is detachable so as to specifically remove the reaction tube with the rubber block to ensure the continuous production.

2. A continuous production device according to claim 1, characterized in that: The first tubular reactor further includes a first heat exchange mechanism disposed in the first shell, and the second tubular reactor further includes a second heat exchange mechanism disposed in the second shell.

3. A continuous production device according to claim 1, characterized in that: The device also includes a third heat exchange mechanism for exchanging heat for the medium in the first storage tank.

4. A continuous production device according to claim 1, characterized in that: The device further comprises a discharge pipe connected to the outlet of the second tubular reactor group and a back pressure valve arranged on the discharge pipe.

5. A continuous production device according to claim 1, characterized in that: The device also includes a metering mechanism arranged between the gas cylinder and the first tubular reactor, a first flow regulating mechanism arranged between the first storage tank and the first tubular reactor, a second flow regulating mechanism arranged one-to-one between the second storage tank and the first tubular reactor / the second tubular reactor, and a third flow regulating mechanism arranged one-to-one between the third storage tank and the second tubular reactor.

6. A continuous production device according to claim 1, characterized in that: The first reaction tube and the second reaction tube have the same inner diameter, and the ratio of the total length of the first reaction tube and the plurality of second reaction tubes to the inner diameter is less than 2×10 5 .

7. A continuous production device according to claim 6, characterized in that: The ratio of the total length of the first reaction tube and the plurality of the second reaction tubes to the inner diameter is 20-2×10 5 .

8. A continuous production device according to claim 1, characterized in that: The total length of the first reaction tube and the plurality of second reaction tubes is 1-1000 m; the inner diameters of the first reaction tube and the second reaction tube are the same, both being 5-50 mm.

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