Trimethylthiopropionaldehyde purification device
By using multiple reflux distillations and polymerization inhibitors in the 3-methylthiopropionaldehyde purification unit, the problems of by-product residue and polymer formation were solved, achieving a highly efficient purification effect.
Patent Information
- Application Number
- CN202422880829.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-26
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2034-11-26
AI Technical Summary
In the existing technology, the purification process of 3-methylthiopropionaldehyde has a large amount of residual by-products, which affects the distillation yield and product purity. Moreover, repeated distillation easily generates polymers, resulting in low purification efficiency.
The process employs separate light and heavy material removal components, which perform multiple reflux distillations through light and heavy material condensers, respectively. During the reflux process, polymerization inhibitors are sprayed to prevent polymer formation. Combined with packing components and a demister, the residence time of the materials is extended, thereby improving purification efficiency.
It improved the distillation yield and product purity of 3-methylthiopropionaldehyde, avoided polymer formation in the column, and improved purification efficiency.
Smart Images
Figure CN223516956U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application relates to the technical field of chemical production, in particular to a trimethylsulfanylpropanal purification device. BACKGROUND
[0002] 3-methylthiopropanal (hereinafter referred to as MMP) is a common perfume and an important intermediate for preparing methionine hydroxyl analogs and methionine and salts thereof. Methionine is a necessary amino acid in animal feed composition, and the hydroxyl analogs and salts of methionine are sources of methionine and are widely used as methionine supplements in animal feed.
[0003] At present, 3-methylthiopropanal is mainly synthesized from propenal and methyl mercaptan. The conventional industrial method is to introduce liquid or gaseous propenal and liquid or gaseous methyl mercaptan into a reactor containing liquid-phase MMP and weak acid salt or weak base salt catalyst. Methyl mercaptan and propenal undergo Michael addition reaction under the action of the catalyst to prepare 3-methylthiopropanal. In the reaction process, various by-products are produced, such as dimethyl sulfide, dimethyl disulfide, xylene benzylamine, allyl acrylate, propenal polymer and 3-methylthiopropanal polymer, and there are dimers and trimers, and a small amount of unreacted methyl mercaptan, dimethyl sulfide, hydrogen sulfide, methanol, acetic acid, acetaldehyde, allyl alcohol, and unreacted propenal and methyl mercaptan. Some of the by-products have a higher boiling point than 3-methylthiopropanal: xylene benzylamine, allyl acrylate, acrylate and 3-methylthiopropanal polymer, and some of the components contained have a lower boiling point than 3-methylthiopropanal: methyl mercaptan, propenal, methyl sulfide, hydrogen sulfide, water, methanol, acetic acid, etc.
[0004] The post-treatment operation of the reaction mixture of 3-methylthiopropanal is to distill the reaction mixture, so as to separate and purify the target product from the mixture. In the current prior art, a light-removing column and a heavy-removing column are mainly used for rectification. Low-boiling-point substances are discharged from the top of the light-removing column, such as hydrogen sulfide, methyl sulfide and the like, 3-methylthiopropanal and high-boiling-point substances are sent from the bottom of the light-removing column to the heavy-removing column, 3-methylthiopropanal is taken from the top of the heavy-removing column, and high-boiling-point by-products are discharged from the bottom of the column, such as propenal polymer, 3-methylthiopropanal polymer and the like. However, this method is prone to residual 3-methylthiopropanal in the high-boiling-point by-products, which is wasteful, and if repeated purification is performed repeatedly, polymers are easily generated in the two columns, thereby affecting the rectification yield and the purity of the product, and thus there are disadvantages. CONTENT OF THE INVENTION
[0005] In order to make up for the above disadvantages, the present application provides a trimethylsulfanylpropanal purification device, which can reduce the content of 3-methylthiopropanal in by-products, improve the purification efficiency, avoid the generation of polymers in the column, and further improve the rectification yield and the purity of the product.
[0006] The application is implemented as follows:
[0007] The light substance removal assembly comprises a light substance removal tower, a light substance condenser and a first polymerization inhibitor, the bottom of the light substance removal tower is fixedly connected with a liquid inlet pipe, the light substance condenser is fixedly connected with the top of the light substance removal tower through a light substance exhaust pipe, the light substance condenser is provided with a first reflux pipe, the first reflux pipe is connected with the top of the light substance removal tower, one end of the first polymerization inhibitor is fixedly connected with the top of the light substance condenser, and the other end of the first polymerization inhibitor is fixedly connected with the first reflux pipe.
[0008] The heavy substance removal assembly comprises a heavy substance removal tower, a heavy substance condenser and a second polymerization inhibitor, the bottom of the heavy substance removal tower is fixedly connected with a feed pipe, the feed pipe is fixedly connected with the bottom of the light substance removal tower, the top of the heavy substance removal tower is fixedly connected with the top of the heavy substance condenser through a distillation exhaust pipe, one side of the top of the heavy substance condenser is fixedly connected with a second reflux pipe, the second reflux pipe is connected with the top of the heavy substance removal tower, one end of the second polymerization inhibitor is fixedly connected with the top of the heavy substance condenser, and the other end of the second polymerization inhibitor is fixedly connected with the second reflux pipe.
[0009] In an embodiment of the application, the light substance removal tower and the heavy substance removal tower are fixedly provided with filler pieces.
[0010] In an embodiment of the application, the filler pieces comprise first filler sections and staggered filler sections, the first filler sections and the staggered filler sections are fixedly connected in sequence in the light substance removal tower and the heavy substance removal tower.
[0011] In an embodiment of the application, the light substance removal tower and the heavy substance removal tower are fixedly connected with a demister below the filler pieces.
[0012] In an embodiment of the application, the first polymerization inhibitor comprises a first shower pipe, a first material conveying pipe and a first polymerization inhibitor tank, the first shower pipe is fixedly connected with the top of the first polymerization inhibitor tank, and the first material conveying pipe is fixedly connected with the bottom of the first polymerization inhibitor tank.
[0013] In an embodiment of the application, the first shower pipe comprises a shower conveying pipe, a spray pipe and a spray nozzle, one end of the shower conveying pipe is fixedly connected with the top of the first polymerization inhibitor tank, the other end of the shower conveying pipe is fixedly connected with the spray pipe, the light substance exhaust pipe is inserted into the spray pipe, there is a gap between the light substance exhaust pipe and the spray pipe, and the spray nozzle is fixedly connected with the spray pipe.
[0014] In an embodiment of the present application, the first polymerization inhibitor device is similar in structure to the second polymerization inhibitor device, the second polymerization inhibitor device comprises a second shower nozzle, a second material conveying pipe and a second polymerization inhibitor tank, the second shower nozzle is fixedly connected to the top end of the second polymerization inhibitor tank, the second material conveying pipe is fixedly connected to the bottom end of the second polymerization inhibitor tank, the distillation exhaust pipe is inserted into the second shower nozzle, and a gap exists between the distillation exhaust pipe and the second shower nozzle.
[0015] In an embodiment of the present application, the heavy substance condenser is fixedly connected with a liquid discharge pipe.
[0016] In an embodiment of the present application, the light substance tower and the heavy substance tower are provided with a bottoming unit at the bottom.
[0017] The present application has the following beneficial effects: when used, the organic liquid generated by the reaction enters the light substance tower through the liquid inlet pipe, and after boiling, the light substance containing trimethylthiopropionaldehyde enters the light substance condenser through the light substance exhaust pipe, and the light substance is repeatedly distilled through the light substance condenser and the first reflux pipe, so that the light substance does not contain trimethylthiopropionaldehyde, thereby improving the yield of trimethylthiopropionaldehyde, wherein the first polymerization inhibitor device sprays the polymerization inhibitor in the light substance condenser and the first reflux pipe respectively during the reflux process, thereby preventing the production of polymers during the repeated distillation in the light substance tower, which affects the distillation yield and the purity of the product of trimethylthiopropionaldehyde, after the light substance is completely separated, trimethylthiopropionaldehyde containing heavy substances enters the heavy substance tower through the feed pipe, the heavy substance tower is used to separate the heavy substance components higher than trimethylthiopropionaldehyde, after boiling, trimethylthiopropionaldehyde and a small amount of heavy substance components are converted into a gas phase, enter the heavy substance condenser through the distillation exhaust pipe, and are repeatedly distilled through the heavy substance condenser and the second reflux pipe, so that trimethylthiopropionaldehyde does not contain heavy substances, thereby improving the yield of trimethylthiopropionaldehyde, wherein the second polymerization inhibitor device sprays the polymerization inhibitor in the heavy substance condenser and the second reflux pipe respectively during the reflux process, thereby preventing the production of polymers during the repeated distillation in the heavy substance tower, which affects the distillation yield and the purity of the product of trimethylthiopropionaldehyde, thereby solving the problems of low distillation yield of trimethylthiopropionaldehyde and easy generation of polymers in the two towers during repeated distillation in the prior art, which affects the distillation yield and the purity of the product. BRIEF DESCRIPTION OF DRAWINGS
[0018] In order to more clearly illustrate the technical scheme of the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope, and for those skilled in the art, other related drawings can also be obtained without creative labor on the basis of these drawings.
[0019] Fig. 1A structural schematic diagram of a trimethylsulfanylpropanal purification device is provided for an embodiment of the present application.
[0020] Fig. 2 A side view of the trimethylsulfanylpropanal purification device is provided for an embodiment of the present application.
[0021] Fig. 3 A structural schematic diagram of a first polymerization inhibitor is provided for an embodiment of the present application.
[0022] In the figure: 100 - light substance removal assembly; 110 - light column; 120 - light substance condenser; 130 - first polymerization inhibitor; 131 - first shower nozzle; 1311 - shower pipe; 1312 - nozzle; 1313 - shower nozzle; 132 - first material conveying pipe; 133 - first polymerization inhibitor tank; 140 - liquid inlet pipe; 150 - light substance exhaust pipe; 160 - first reflux pipe; 170 - filler; 171 - first filler section; 172 - staggered filler section; 180 - demister; 190 - co-boiler; 200 - heavy substance removal assembly; 210 - heavy column; 220 - heavy substance condenser; 230 - second polymerization inhibitor; 231 - second shower nozzle; 232 - second material conveying pipe; 233 - second polymerization inhibitor tank; 240 - feed pipe; 250 - distillation exhaust pipe; 260 - second reflux pipe; 270 - liquid outlet pipe. DETAILED DESCRIPTION
[0023] Some embodiments of the present application will be described in detail below with reference to the accompanying drawings. In the case of no conflict, the following examples and features in the examples can be combined with each other.
[0024] As shown in Figs. 1-3 , a trimethylsulfanylpropanal purification device according to an embodiment of the present application includes:
[0025] The light substance removal assembly 100 includes a light column 110, a light substance condenser 120, and a first polymerization inhibitor 130. The light column 110 is fixedly connected to a liquid inlet pipe 140 at the bottom. The light substance condenser 120 is fixedly connected to the top of the light column 110 through a light substance exhaust pipe 150. The light substance condenser 120 is provided with a first reflux pipe 160, which is in communication with the top end of the light column 110. One end of the first polymerization inhibitor 130 is fixedly connected to the top end of the light substance condenser 120, and the other end is fixedly connected to the first reflux pipe 160.
[0026] The heavy substance removal assembly 200 includes a heavy substance removal tower 210, a heavy substance condenser 220 and a second polymerization inhibitor 230. The bottom of the heavy substance removal tower 210 is fixedly connected with a feed pipe 240, which is fixedly connected with the bottom end of the light substance removal tower 110. The top end of the heavy substance removal tower 210 is fixedly connected with the top end of the heavy substance condenser 220 through a distillation exhaust pipe 250. The top end of the heavy substance condenser 220 is fixedly connected with a second reflux pipe 260, which is connected with the top end of the heavy substance removal tower 210. One end of the second polymerization inhibitor 230 is fixedly connected with the top end of the heavy substance condenser 220, and the other end is fixedly connected with the second reflux pipe 260. In use, the organic liquid generated by the reaction enters the light substance removal tower 110 through the liquid inlet pipe 140. After boiling, the light substance containing trimethylthiopropionaldehyde enters the light substance condenser 120 through the light substance exhaust pipe 150. The light substance containing trimethylthiopropionaldehyde is repeatedly distilled through the light substance condenser 120 and the first reflux pipe 160, so that the light substance does not contain trimethylthiopropionaldehyde, thereby improving the yield of trimethylthiopropionaldehyde. During the reflux process, the first polymerization inhibitor 130 is sprayed in the light substance condenser 120 and the first reflux pipe 160, respectively, to prevent the production of polymers during repeated distillation in the light substance removal tower 110, which affects the distillation yield of trimethylthiopropionaldehyde and the purity of the product. After the light substance is completely removed, the trimethylthiopropionaldehyde containing heavy substance enters the heavy substance removal tower 210 through the feed pipe 240. The heavy substance removal tower 210 is used to remove heavy substance components higher than trimethylthiopropionaldehyde. After boiling, trimethylthiopropionaldehyde and a small amount of heavy substance components are converted into a gas phase, which enters the heavy substance condenser 220 through the distillation exhaust pipe 250. The trimethylthiopropionaldehyde is repeatedly distilled through the heavy substance condenser 220 and the second reflux pipe 260, so that the trimethylthiopropionaldehyde does not contain heavy substance, thereby improving the yield of trimethylthiopropionaldehyde. During the reflux process, the second polymerization inhibitor 230 is sprayed in the heavy substance condenser 220 and the second reflux pipe 260, respectively, to prevent the production of polymers during repeated distillation in the heavy substance removal tower 210, which affects the distillation yield of trimethylthiopropionaldehyde and the purity of the product. Thus, the problem of low distillation yield of trimethylthiopropionaldehyde and easy generation of polymers in the two towers during repeated distillation in the prior art is solved, thereby affecting the distillation yield and the purity of the product.
[0027] As Fig. 2As shown, the packing member 170 is fixedly arranged in the light-removing tower 110 and the heavy-removing tower 210. The packing member 170 is used to prolong the residence time of the substance in the gas phase or liquid phase in the tower. The demister 180 is fixedly connected in the light-removing tower 110 and the heavy-removing tower 210, and is located below the packing member 170. The demister 180 is used to remove the liquid mist entrained in the gas phase. The heavy-substance condenser 220 is fixedly connected with the liquid discharge pipe 270. When the distillation purification is completed, the liquid discharge pipe 270 is used to discharge the condensed trimethylthiopropionaldehyde for collection. The azeotrope boiler 190 is installed at the bottom of the light-removing tower 110 and the heavy-removing tower 210. The azeotrope boiler 190 is used to increase the temperature in the light-removing tower 110 and the heavy-removing tower 210, so that the light-removing tower 110 and the heavy-removing tower 210 can evaporate the light substance or trimethylthiopropionaldehyde at a suitable temperature.
[0028] As shown in the figure, Fig. 3 The packing member 170 includes the first packing section 171 and the staggered packing section 172, which are sequentially and fixedly connected in the light-removing tower 110 and the heavy-removing tower 210. By arranging the first packing section 171 and the staggered packing section 172, the gas phase or liquid phase is subjected to multiple obstacles when passing through, thereby prolonging the residence time in the tower. The first polymerization inhibitor member 130 includes the first shower nozzle 131, the first material conveying pipe 132, and the first polymerization inhibitor tank 133. The first shower nozzle 131 is fixedly connected to the top end of the first polymerization inhibitor tank 133, and the first material conveying pipe 132 is fixedly connected to the bottom end of the first polymerization inhibitor tank 133. The first polymerization inhibitor tank 133 stores the polymerization inhibitor. The first shower nozzle 131 sprays the polymerization inhibitor onto the inner surface of the light-substance condenser 120, so that the substance can fully contact the polymerization inhibitor to prevent the formation of polymers in the light-substance condenser 120. When refluxing, the polymerization inhibitor is input into the substance through the first material conveying pipe 132 to prevent the formation of polymers during repeated distillation. It should be noted that the effective component of the polymerization inhibitor accounts for 0.001% of the total mass of trimethylthiopropionaldehyde. The first shower nozzle 131 includes the conveying shower pipe 1311, the nozzle 1312, and the spray nozzle 1313. One end of the conveying shower pipe 1311 is fixedly connected to the top end of the first polymerization inhibitor tank 133, the other end of the conveying shower pipe 1311 is fixedly connected to the nozzle 1312, the light-substance exhaust pipe 150 is inserted into the nozzle 1312, and there is a gap between the light-substance exhaust pipe 150 and the nozzle 1312. The spray nozzle 1313 is fixedly connected to the nozzle 1312. The polymerization inhibitor is sprayed onto the inner surface of the light-substance condenser 120 through the conveying shower pipe 1311, the nozzle 1312, and the spray nozzle 1313.
[0029] Further, the first polymerization inhibitor 130 and the second polymerization inhibitor 230 are similar in structure, the second polymerization inhibitor 230 comprises a second shower pipe 231, a second material conveying pipe 232 and a second polymerization inhibitor tank 233, the second shower pipe 231 is fixedly connected to the top end of the second polymerization inhibitor tank 233, the second material conveying pipe 232 is fixedly connected to the bottom end of the second polymerization inhibitor tank 233, the distillation exhaust pipe 250 is inserted into the second shower pipe 231, and a gap exists between the distillation exhaust pipe 250 and the second shower pipe 231. The second polymerization inhibitor tank 230 stores the polymerization inhibitor, the second shower pipe 231 sprays the polymerization inhibitor to the inner surface of the heavy material condenser 220, so that the material can fully contact the polymerization inhibitor to prevent the material from generating polymers in the heavy material condenser 220, and the polymerization inhibitor is input into the material through the second material conveying pipe 232 during reflux to prevent the generation of polymers during repeated distillation.
[0030] In summary, the working principle of the trimethylthiopropionaldehyde purification device is as follows: when in use, the organic liquid generated by reaction enters the light-removing tower 110 through the liquid inlet pipe 140, after boiling, the light material containing trimethylthiopropionaldehyde enters the light material condenser 120 through the light material exhaust pipe 150, and the light material containing trimethylthiopropionaldehyde is repeatedly distilled through the light material condenser 120 and the first reflux pipe 160, so that the light material does not contain trimethylthiopropionaldehyde, and the yield of trimethylthiopropionaldehyde is improved, wherein the first shower pipe 131 and the first material conveying pipe 132 spray the polymerization inhibitor in the light material condenser 120 and the first reflux pipe 160 respectively during the reflux process, so as to prevent the production of polymers in the light-removing tower 110 during repeated distillation, which affects the distillation yield and the purity of the product of the subsequent trimethylthiopropionaldehyde, after the light material is completely separated, the trimethylthiopropionaldehyde containing heavy material enters the heavy-removing tower 210 through the feed pipe 240, the heavy-removing tower 210 is used to separate the heavy material components higher than trimethylthiopropionaldehyde, after boiling, the trimethylthiopropionaldehyde and a small amount of heavy material components are converted into gas phase, enter the heavy material condenser 220 through the distillation exhaust pipe 250, and are repeatedly distilled through the heavy material condenser 220 and the second reflux pipe 260, so that the trimethylthiopropionaldehyde does not contain heavy material, and the yield of trimethylthiopropionaldehyde is improved, wherein the second shower pipe 231 and the second material conveying pipe 232 spray the polymerization inhibitor in the heavy material condenser 220 and the second reflux pipe 260 respectively during the reflux process, so as to prevent the production of polymers in the heavy-removing tower 210 during repeated distillation, which affects the distillation yield and the purity of the product of the trimethylthiopropionaldehyde, thereby solving the problems of low distillation yield of trimethylthiopropionaldehyde in the prior art, and the generation of polymers in the two towers during repeated distillation, which affects the distillation yield and the purity of the product.
[0031] The above merely provides examples of the present application, and is not intended to limit the protection scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application. It should be noted that similar reference numerals and letters represent similar items in the following drawings, and therefore once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.
Claims
1. A trimethylthiopropionaldehyde purification apparatus, characterized by, The application relates to a light and heavy substance removal assembly. The light substance removal assembly (100) comprises a light substance removal tower (110), a light substance condenser (120) and a first polymerization inhibitor (130), the bottom of the light substance removal tower (110) is fixedly communicated with a liquid inlet pipe (140), the light substance condenser (120) is fixedly communicated with the top of the light substance removal tower (110) through a light substance exhaust pipe (150), the light substance condenser (120) is provided with a first reflux pipe (160) which is communicated with the top end of the light substance removal tower (110), one end of the first polymerization inhibitor (130) is fixedly communicated with the top end of the light substance condenser (120), and the other end of the first polymerization inhibitor (130) is fixedly communicated with the first reflux pipe (160). The heavy substance removal assembly (200) comprises a heavy substance removal tower (210), a heavy substance condenser (220) and a second polymerization inhibitor (230), the bottom of the heavy substance removal tower (210) is fixedly communicated with a feed pipe (240), the feed pipe (240) is fixedly communicated with the bottom end of the light substance removal tower (110), the top end of the heavy substance removal tower (210) is fixedly communicated with the top end of the heavy substance condenser (220) through a distillation exhaust pipe (250), the top end of the heavy substance condenser (220) is fixedly communicated with a second reflux pipe (260) on one side, the second reflux pipe (260) is communicated with the top end of the heavy substance removal tower (210), one end of the second polymerization inhibitor (230) is fixedly communicated with the top end of the heavy substance condenser (220), and the other end of the second polymerization inhibitor (230) is fixedly communicated with the second reflux pipe (260).
2. A trimethylthiopropionaldehyde purification apparatus according to claim 1, wherein The light substance removal tower (110) and the heavy substance removal tower (210) are fixedly provided with filler pieces (170) therein.
3. A trimethylthiopropionaldehyde purification apparatus according to claim 2, wherein The filler pieces (170) comprise first filler sections (171) and staggered filler sections (172), the first filler sections (171) and the staggered filler sections (172) are fixedly connected in sequence in the light substance removal tower (110) and the heavy substance removal tower (210).
4. A trimethylthiopropionaldehyde purification apparatus according to claim 2, wherein The light substance removal tower (110) and the heavy substance removal tower (210) are fixedly connected with demisters (180) therein, and the demisters (180) are located below the filler pieces (170).
5. A trimethylthiopropionaldehyde purification apparatus according to claim 1, wherein The first polymerization inhibitor (130) comprises a first shower pipe (131), a first material conveying pipe (132) and a first polymerization inhibitor tank (133), the first shower pipe (131) is fixedly connected with the top end of the first polymerization inhibitor tank (133), and the first material conveying pipe (132) is fixedly connected with the bottom end of the first polymerization inhibitor tank (133).
6. A trimethylthiopropionaldehyde purification apparatus according to claim 5, wherein The first shower nozzle (131) comprises a shower pipe (1311), a nozzle (1312) and a shower nozzle head (1313), one end of the shower pipe (1311) is fixedly connected to the top end of the first inhibitor tank (133), the other end of the shower pipe (1311) is fixedly connected to the nozzle (1312), the light substance exhaust pipe (150) is inserted into the nozzle (1312), there is a gap between the light substance exhaust pipe (150) and the nozzle (1312), and the shower nozzle head (1313) is fixedly connected to the nozzle (1312).
7. A trimethylthiopropionaldehyde purification apparatus according to claim 1, wherein The first inhibitor (130) and the second inhibitor (230) are similar in structure, the second inhibitor (230) comprises a second shower nozzle (231), a second material pipe (232) and a second inhibitor tank (233), the second shower nozzle (231) is fixedly connected to the top end of the second inhibitor tank (233), the second material pipe (232) is fixedly connected to the bottom end of the second inhibitor tank (233), and the distillation exhaust pipe (250) is inserted into the second shower nozzle (231), and there is a gap between the distillation exhaust pipe (250) and the second shower nozzle (231).
8. A trimethylthiopropionaldehyde purification apparatus according to claim 1, wherein The heavy substance condenser (220) is fixedly connected with a liquid discharge pipe (270).
9. A trimethylthiopropionaldehyde purification apparatus according to claim 1, wherein The de-light column (110) and the de-heavy column (210) are provided with a azeotrope device (190) at the bottom.