Recovery device for purifying methyl chloroacetate

Abstract

The utility model belongs to the technical field of purification and recovery of methyl chloroacetate, and discloses a recovery device for purification of methyl chloroacetate, which comprises a bracket, a distillation kettle, a filter, condensing equipment and a storage tank, and gaps are reserved between the baffles of the filter layer and the inner side wall of the filter alternately, so that methyl chloroacetate steam flows in the filter along a Z shape, the contact area between the steam and a filter medium is maximized, and the filter medium can fully absorb impurities of methyl chloroacetate. According to the recovery device for purifying the methyl chloroacetate, the recovery rate of the methyl chloroacetate can be effectively improved, the purification energy consumption of the methyl chloroacetate is reduced, and the purification efficiency is improved. The methyl chloroacetate purification and recovery device is suitable for purification and recovery of methyl chloroacetate.

Description

Technical Field

[0001] The utility model belongs to the technical field of methyl chloroacetate purification and recovery, and relates to a recovery device, in particular to a recovery device for methyl chloroacetate purification. Background Art

[0002] Methyl chloroacetate, molecular formula is C 3 H 5 C1O 2 It is a colorless, transparent liquid with a pungent odor and is slightly soluble in water. It is mainly used as a solvent and is also used in organic synthesis. It is harmful to the body if inhaled, ingested, or absorbed through the skin. Its vapor is toxic and is toxic if inhaled or taken orally. It is highly irritating to the eyes, mucous membranes, and skin. Symptoms of poisoning include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea, and vomiting. It is flammable and may cause combustion and explosion when exposed to open flames, high temperatures, or contact with oxidants. It emits highly toxic fumes when exposed to heat or contact with acids or acid mist.

[0003] In the prior art, methanol and chloroacetic acid are uniformly mixed according to a weight ratio and added to a reactor, stirred and heated to carry out an esterification reaction. The reaction is first put into a second reactor to separate methyl chloroacetate, and then enters a distillation device for distillation. The efficiency of the entire distillation process is relatively low, and the purification effect is poor.

[0004] The invention discloses a high-efficiency distillation and purification device for methyl chloroacetate, which separates crude methyl chloroacetate by distillation and then purifies it by condensation. The application number is: 202022763286.2. The device relates to the technical field of purification devices. A feed port is arranged on the left upper part of the first distillation body, a first steam inlet is arranged on the right lower part of the first distillation body, a first reflux port is arranged on one side of the first distillation body, and the bottom of the first distillation body is connected to the first reflux port through a first reflux pipe. Two distillation tower bodies are arranged, and an overflow weir is arranged in the distillation body. The ordinary high-efficiency distillation and purification device for methyl chloroacetate has too much local temporary storage of materials, which affects the effect of steam on its treatment and also affects the purification effect.

[0005] The application number is: 202320000799.9, a high-efficiency distillation and purification device for methyl chloroacetate, including a distillation body, wherein the upper and lower sides of the distillation body are bolted with a disassembly cover; the upper left part of the distillation body is inlaid with a filling pipe; the middle and upper left part of the distillation body is inlaid with a reflux pipe; the lower end of the reflux pipe is threadedly connected with a delivery pump; the delivery pump is bolted on the disassembly cover, and the delivery pump is arranged at the lower end of the distillation body; the lower right side of the distillation body is inlaid with a steam pipe; the disassembly cover is inlaid with a discharge pipe, and the discharge pipe is arranged at the upper end of the distillation body; the right end of the discharge pipe is threadedly connected with a condenser; the distillation body is supported by an adjustable temporary storage support structure; the outer side of the distillation body is supported by a movable stirring support structure. Although the utility model adjusts the temporary storage support structure to facilitate the lifting and lowering adjustment in conjunction with the lifting baffle, thereby adjusting the temporary storage amount of the material. However, some impurities will still be carried during the purification process, affecting the distillation effect of methyl chloroacetate, and the recovery rate of methyl chloroacetate using the above-mentioned equipment has not been significantly improved. Utility Model Content

[0006] In order to solve the above deficiencies in the prior art, the utility model aims to provide a recovery device for purifying methyl chloroacetate, so as to achieve the purpose of improving the recovery rate of methyl chloroacetate, reducing the energy consumption of purifying methyl chloroacetate, and improving the purification efficiency.

[0007] In order to achieve the above purpose, the technical solution adopted by the utility model is as follows:

[0008] A recovery device for purifying methyl chloroacetate comprises a still, a filter, a condensing device and a storage tank, wherein a stirring paddle is arranged at the inner bottom of the still, a stirring head of the stirring paddle is arranged inside the still, and one end away from the stirring head passes through the bottom of the still and is connected to the power end of a motor; the motor is fixedly arranged at the bottom of the still; a feed port is arranged at one end of the side wall of the top of the still; a filter is arranged at the top of the still, and the bottom of the filter is fixed to the still through a connecting pipe; a first condensing pipe is arranged at the outer side of the side wall of the filter, the first condensing pipe is connected to the filter through a first pipeline, the first pipeline comprises an air outlet pipe and a reflux pipe, one end of the air outlet pipe is connected to the side wall of the filter, and the other end is connected to the side wall of the first condensing pipe, one end of the reflux pipe is connected to the bottom of the first condensing pipe, and the other end is connected to the side wall of the top of the still; the first condensing pipe is connected to the top of the second condensing pipe through a second pipeline, and the bottom of the second condensing pipe leads to the storage tank.

[0009] As a limitation of the present invention, the filter includes at least three groups of filter layers, wherein the first filter layer is a dehydration layer, the second filter layer is a dealcoholization layer, and the third filter layer is an alkalization layer;

[0010] As a further limitation of the present invention, the dehydration layer includes at least one of magnesium sulfate, sodium carbonate, sodium bicarbonate, and potassium carbonate; the dealcoholization layer includes at least one of molecular sieves and activated carbon; and the alkalization layer includes at least one of calcium carbonate, sodium carbonate, and potassium carbonate.

[0011] As a further limitation of the present invention, the three groups of filter layers are, from bottom to top, a first filter layer, a second filter layer and a third filter layer.

[0012] As a further limitation of the present invention, each group of filter layers includes a first baffle, a filter layer and a second baffle; wherein the first baffle is fixed to one end of the filter side wall, and the other end leaves a gap with the other end of the filter; one end of the second baffle is fixed above the corresponding position of the gap between the first baffle and the filter side wall, and the other end leaves a gap with the filter side wall; the filter layer is sandwiched between the first baffle and the second baffle.

[0013] The filter is provided with a filter layer to filter the methyl chloroacetate vapor. The baffle of the filter layer leaves gaps alternately with the inner side wall of the filter, so that the methyl chloroacetate vapor can flow in the filter along a "Z" shape, so that the contact area between the vapor and the filter medium is maximized, so that the filter medium can fully absorb the impurities of the methyl chloroacetate.

[0014] As another limitation of the present invention, a one-way baffle is provided at the connection between the bottom of the first condenser tube and the reflux tube;

[0015] By arranging a one-way baffle at the first condenser tube, it is possible to prevent methyl chloroacetate vapor from directly entering the first condenser tube, and simultaneously prevent excessive condensate from accumulating in the first condenser tube.

[0016] Due to the adoption of the above technical solution, the utility model has the following beneficial effects compared with the prior art:

[0017] (1) The methyl chloroacetate purification recovery device of the utility model has a first filter layer, a second filter layer and a third filter layer from bottom to top, thereby ensuring that the impurity removal order of methyl chloroacetate is first to remove water, then to remove methyl ester, and finally to remove acid, thereby preventing methyl chloroacetate from being hydrolyzed in a steam state.

[0018] (2) The methyl chloroacetate purification recovery device of the utility model filters the methyl chloroacetate vapor by setting a filter layer. The baffles of the filter layer leave gaps alternately with the inner side wall of the filter, allowing the methyl chloroacetate vapor to flow in the filter along a "Z" shape, so that the contact area between the vapor and the filter medium is maximized, so that the filter medium can fully absorb the impurities of the methyl chloroacetate.

[0019] (3) The methyl chloroacetate purification recovery device of the present invention can prevent methyl chloroacetate vapor from directly entering the first condenser tube and prevent excessive condensate from accumulating in the first condenser tube by providing a one-way baffle at the first condenser tube.

[0020] In summary, the recovery device for purifying methyl chloroacetate involved in the utility model can effectively improve the recovery rate of methyl chloroacetate, reduce the energy consumption of purifying methyl chloroacetate, and improve the purification efficiency.

[0021] The utility model is suitable for the purification and recovery of methyl chloroacetate and is used for purifying and recovering methyl chloroacetate. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The present invention is described in further detail below in conjunction with the accompanying drawings and specific embodiments.

[0023] Figure 1 It is a schematic diagram of the structure of an embodiment of the utility model;

[0024] Figure 2 It is a front cross-sectional view of an embodiment of the utility model.

[0025] In the figure: 1. filter; 2. third filter layer; 3. second filter layer; 4. first filter layer; 5-1. first condenser; 5-2. second condenser; 6. second pipeline; 7. one-way baffle; 8. distillation kettle; 9. stirring paddle; 10. storage tank; 11. motor; 12. bracket; 13. feed pipe; 14. feed valve; 15. connecting pipe; 16. outlet pipe; 17. reflux pipe. DETAILED DESCRIPTION

[0026] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and understand the present invention, and are not used to limit the present invention.

[0027] Embodiment A recovery device for purifying methyl chloroacetate

[0028] like Figure 1 to Figure 2As shown, this embodiment includes a bracket 12, a distillation kettle 8, a filter 1, a condensation device and a storage tank 10, wherein a stirring paddle 9 is arranged at the inner bottom of the distillation kettle 8, a stirring head of the stirring paddle 9 is arranged inside the distillation kettle 8, and the end away from the stirring head passes through the bottom of the distillation kettle 8 and is connected to the power end of the motor 11; the motor 11 is fixedly arranged at the bottom of the distillation kettle 8; a feed port is arranged at one end of the top side wall of the distillation kettle 8; a filter is arranged at the top of the distillation kettle 8, and the bottom of the filter 1 is fixed to the distillation kettle 8 through a connecting pipe 15; a first condensation pipe 5-1 is arranged on the outer side wall of the filter 1, The first condenser 5-1 is connected to the filter 1 through a first pipeline, and the first pipeline includes an outlet pipe 16 and a reflux pipe 17. One end of the outlet pipe 16 is connected to the side wall of the filter 1, and the other end is connected to the side wall of the first condenser 5-1. One end of the reflux pipe 17 is connected to the bottom of the first condenser 5-1, and a one-way baffle 7 is provided at the connection between the bottom of the first condenser 5-1 and the reflux pipe 17, and the other end is connected to the top side wall of the distillation kettle 8; the first condenser 5-1 is connected to the top of the second condenser 5-2 through the second pipeline 6, and the bottom of the second condenser 5-2 is connected to the storage tank 10.

[0029] The filter 1 includes at least three groups of filter layers arranged in sequence from bottom to top, each group of filter layers includes a first baffle, a filter layer and a second baffle; wherein the first baffle is fixed to one end of the side wall of the filter 1, and a gap is left between the other end and the other end of the filter 1; one end of the second baffle is fixed above the corresponding position of the gap between the first baffle and the side wall of the filter 1, and a gap is left between the other end and the side wall of the filter 1; the filter layer is sandwiched between the first baffle and the second baffle, wherein the first filter layer 4 is a dehydration layer, which includes at least one of magnesium sulfate, sodium carbonate, sodium bicarbonate, and potassium carbonate; the second filter layer 3 is a dealcoholization layer, which includes at least one of molecular sieves and activated carbon; the third filter layer 2 is an alkalization layer, which includes at least one of calcium carbonate, sodium carbonate, and potassium carbonate.

[0030] When using the present embodiment, the feed valve 14 is opened and the methyl chloroacetate produced or recovered is passed into the still kettle 8 through the feed pipe 13, the motor 11 is started, and the stirring paddle 9 driven by the motor 11 is stirred and distilled to the methyl chloroacetate in the still kettle 8, the methyl chloroacetate steam distilled out passes through the first filter layer 4, the second filter layer 3, and the third filter layer 2 in a "Z" type path from bottom to top, and the methyl chloroacetate steam is dehydrated in the first filter layer 4, demethylated in the second filter layer 3, and dechloroacetic acid is removed in the third filter layer 2, and finally the methyl chloroacetate steam enters the first condenser tube 5-1 through the air outlet pipe 16, and is cooled for the first time, and part of the methyl chloroacetate steam is condensed into condensate and refluxed into the still kettle 8 through the reflux pipe 17 for circulating distillation, and the uncondensed chloroacetic acid steam enters the second condenser tube 5-2 through the second pipeline 6 for secondary condensation, and after being condensed into liquid methyl chloroacetate, it flows into the storage tank 10 for collection.

[0031] It should be noted that the heating equipment used in the distillation process are all conventional heating equipment and can be added to the equipment involved in this application as needed.

[0032] It should be noted that the above is only a preferred embodiment of the utility model and is not intended to limit the utility model. Although the utility model is described in detail with reference to the above embodiments, those skilled in the art can still modify the technical solutions recorded in the above embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model shall be included in the protection scope of the utility model.

Claims

1. A recovery device for purifying methyl chloroacetate, comprising a support (12), a distillation kettle (8), a filter (1), a condensing device and a storage tank (10), characterized in that: A stirring paddle (9) is arranged at the bottom of the inner side of the distillation kettle (8); the stirring head of the stirring paddle (9) is arranged inside the distillation kettle (8), and the end away from the stirring head passes through the bottom of the distillation kettle (8) and is connected to the power end of the motor (11); the motor (11) is fixedly arranged at the bottom of the distillation kettle (8); a feed port is arranged at one end of the top side wall of the distillation kettle (8); a filter (1) is arranged at the top of the distillation kettle (8), and the bottom of the filter (1) is fixed to the distillation kettle (8) through a connecting pipe (15); a first condenser (5-1) is arranged on the outer side wall of the filter (1), and the first condenser (5-1) is arranged on the outer side wall of the filter (1). A condenser (5-1) is connected to the filter (1) via a first pipeline, the first pipeline comprising an outlet pipe (16) and a reflux pipe (17), one end of the outlet pipe (16) is connected to the side wall of the filter (1), and the other end is connected to the side wall of the first condenser (5-1), one end of the reflux pipe (17) is connected to the bottom of the first condenser (5-1), and the other end is connected to the top side wall of the distillation kettle (8); the first condenser (5-1) is connected to the top of the second condenser (5-2) via a second pipeline (6), and the bottom of the second condenser (5-2) leads to a storage tank (10).

2. The methyl chloroacetate purification recovery device according to claim 1, characterized in that: The filter (1) comprises at least three groups of filter layers, wherein the first filter layer (4) is a dehydration layer, the second filter layer (3) is a dealcoholization layer, and the third filter layer (2) is an alkalization layer.

3. The methyl chloroacetate purification recovery device according to claim 2, characterized in that: Each group of the filter layers comprises a first baffle, a filter layer and a second baffle; wherein the first baffle is fixed to one end of the side wall of the filter (1), and the other end of the first baffle is spaced apart from the other end of the filter (1); one end of the second baffle is fixed above a position corresponding to the space between the first baffle and the side wall of the filter (1), and the other end of the second baffle is spaced apart from the side wall of the filter (1); the filter layer is sandwiched between the first baffle and the second baffle.

4. The methyl chloroacetate purification recovery device according to claim 2, characterized in that: The dehydration layer includes at least one of magnesium sulfate, sodium carbonate, sodium bicarbonate, and potassium carbonate; the dealcoholization layer includes at least one of molecular sieves and activated carbon; and the alkalization layer includes at least one of calcium carbonate, sodium carbonate, and potassium carbonate.

5. according to any one of claims 2-4 described methyl chloroacetate purification recovery device, it is characterized in that: The three groups of filter layers are, from bottom to top, a first filter layer (4), a second filter layer (3) and a third filter layer (2).

6. The recovery device for purifying methyl chloroacetate according to claim 1, characterized in that: A one-way baffle (7) is provided at the connection between the bottom of the first condensation tube (5-1) and the reflux tube (17).

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