A device for synthesizing methyl acetate
By designing a synthesis apparatus that includes a reaction vessel, a filter press, a distillation vessel, a condenser, and a vacuum pump, and by using specific materials and processes, the problems of low yield and high cost in the synthesis of methyl pyruvate were solved, and high-purity and low-cost industrial production was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- HANGZHOU BAIYU BIOTECHNOLOGY CO LTD
- Filing Date
- 2025-07-24
- Publication Date
- 2026-06-26
AI Technical Summary
Existing methods for synthesizing methyl pyruvate suffer from low yield, high production costs, and large equipment investments.
Design a synthesis apparatus including a reaction vessel, a plate and frame filter press, a distillation vessel, a condenser, a product receiving vessel, and a vacuum pump. The apparatus is made of enamel and stainless steel and integrates multiple key pieces of equipment to achieve efficient connection of the entire process. Methyl lactate, dichloromethane, and sodium bicarbonate are used as raw materials. The reaction temperature and vacuum distillation are controlled to improve product purity.
The efficient synthesis of methyl pyruvate was achieved, with a product purity of 99.5%, low production cost, and a short synthetic route, making it suitable for industrial production.
Smart Images
Figure CN224405131U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the technical field of chemical organic synthesis equipment, and specifically relates to a synthesis apparatus for methyl pyruvate. Background Technology
[0002] Methyl pyruvate is used as an intermediate in organic synthesis and pharmaceutical chemistry, primarily in the production and preparation of drug molecules and pesticide chemicals. In organic synthesis transformations, both the ester and ketone carbonyl groups in its structure are highly electrophilic, allowing it to undergo addition reactions with organometallic reagents such as Grignard reagents; it can also be converted into the corresponding diol compounds under the action of strong reducing agents. Furthermore, under appropriate reaction conditions, the ketone carbonyl and ester groups in its structure can undergo selective chemical transformation reactions; for example, in the presence of sodium borohydride, the ester carbonyl group remains unchanged, while the ketone carbonyl group is reduced to an alcohol.
[0003] Currently, there are three methods for synthesizing methyl pyruvate. The first is the lactate oxidation method, which uses liquid bromine and H2O2 as catalysts under light conditions to oxidize methyl lactate, yielding the reaction product. The product is then treated with NaOH and NaHCO3, the powder is neutralized, extracted with dichloromethane, dried with CaCl2, and finally distilled under reduced pressure to obtain the product methyl pyruvate, with a yield of 48%. The second method is the pyruvate-methanol condensation method, which involves mixing a certain amount of pyruvate and methanol, adding benzene and p-toluenesulfonic acid, heating to reflux, and finally distilling under reduced pressure to obtain the product methyl pyruvate, with a yield of 65%. To address the yield issue mentioned above, a method using methyl lactate, dichloromethane, and sodium bicarbonate as main raw materials involves adding a catalyst during the reaction, cooling, adding an oxidant after cooling, maintaining the temperature, filtering, and distilling to obtain methyl pyruvate, with a yield of 90%. This method uses relatively inexpensive raw materials such as dichloromethane and sodium bicarbonate, yields a high product, has a mature process, requires less equipment investment, and is suitable for industrial production. Utility Model Content
[0004] The purpose of this invention is to overcome the shortcomings of the existing technology and provide a synthesis apparatus for methyl pyruvate. Using this synthesis apparatus, the process is advanced and reasonable, the production cost is low, the synthesis route is short, and the product purity is high.
[0005] The technical solution adopted by this utility model to solve its technical problem is as follows: A synthesis apparatus for methyl pyruvate is provided, comprising: a reaction vessel, a plate and frame filter press, a distillation vessel, a condenser, a product receiving vessel, a dichloromethane receiving vessel, and a vacuum pump; the outlet valve at the bottom of the reaction vessel is connected to the inlet end of the plate and frame filter press via a pipeline; the outlet end of the plate and frame filter press is connected to the inlet end of the distillation vessel via a pipeline; the outlet end of the top of the distillation vessel is connected to the inlet end of the stainless steel condenser via a pipeline; the outlet end of the condenser is connected to a T-type control valve; the first outlet end of the T-type control valve is connected to the inlet end of the dichloromethane receiving vessel via a pipeline; the second outlet end of the T-type control valve is connected to the inlet end of the product receiving vessel via a pipeline; and the inlet end of the top of the product receiving vessel is connected to the vacuum pump via a pipeline.
[0006] Furthermore, the inner wall of the reactor is made of enamel; a reactor agitator is installed inside the reactor; and a reactor insulation jacket is installed outside the reactor.
[0007] Furthermore, the plate and frame filter press is made of polypropylene (PP); the product receiving vessel is made of polypropylene (PP); and the dichloromethane receiving vessel is made of polypropylene (PP).
[0008] Furthermore, the inner wall of the distillation vessel is made of enamel; a distillation vessel stirrer is installed inside the distillation vessel; and a distillation vessel insulation jacket is installed outside the distillation vessel.
[0009] Furthermore, the condenser is made of stainless steel.
[0010] Furthermore, the vacuum pump is a rotary vane vacuum pump.
[0011] Furthermore, all pipes and valves in the synthesis unit are made of stainless steel.
[0012] Furthermore, the components in the synthesis apparatus that come into contact with methyl pyruvate are free of iron.
[0013] This utility model has the following beneficial effects:
[0014] The synthesis apparatus of this application is ingeniously designed, integrating a variety of key equipment such as a reaction vessel, filter press, distillation vessel, stainless steel condenser, product receiving vessel, buffer vessel, and vacuum pump, enabling efficient connection of the entire process of methyl pyruvate synthesis. Attached Figure Description
[0015] Figure 1 This is a schematic diagram of the structure of a methyl pyruvate synthesis apparatus according to the present invention;
[0016] The components in the attached diagram are labeled as follows: 2. Reactor; 3. Reactor insulation jacket; 5. Reactor agitator; 9. Distillation vessel insulation jacket; 24. Distillation vessel agitator; 6. Plate and frame filter press; 10. Distillation vessel; 13. Condenser; 16. Dichloromethane receiving vessel; 19. Product receiving vessel; 23. Rotary vane vacuum pump; 1, 4, 7, 8, 11, 12, 14, 15, 17, 18, 20, 21, 22. Switch control valves. Detailed Implementation
[0017] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present utility model.
[0018] Example:
[0019] This embodiment provides an apparatus for synthesizing methyl pyruvate, such as... Figure 1 As shown, the system includes: a reaction vessel 2, a plate and frame filter press 6, a distillation vessel 10, a condenser 13, a product receiving vessel 19, a dichloromethane receiving vessel 16, and a vacuum pump 23; the outlet valve at the bottom of the reaction vessel 2 is connected to the inlet end of the plate and frame filter press 6 via a pipeline; the outlet end of the plate and frame filter press 6 is connected to the inlet end of the distillation vessel 10 via a pipeline; the outlet end of the top of the distillation vessel 10 is connected to the inlet end of the stainless steel condenser 13 via a pipeline; the outlet end of the condenser 13 is connected to a T-type control valve; the first outlet end of the T-type control valve is connected to the inlet end of the dichloromethane receiving vessel 16 via a pipeline; the second outlet end of the T-type control valve is connected to the inlet end of the product receiving vessel 19 via a pipeline; and the inlet end of the top of the product receiving vessel 19 is connected to the vacuum pump 23 via a pipeline. Figure 1 Each pipeline is equipped with a switch control valve.
[0020] Specifically, the inner wall of the reactor 2 is made of enamel; the reactor 2 is equipped with a reactor agitator 5; and the reactor 2 is equipped with a reactor insulation jacket 3 on the outside.
[0021] Specifically, the plate and frame filter press 6 is made of polypropylene (PP); the product receiving vessel 19 is made of polypropylene (PP); and the dichloromethane receiving vessel 16 is made of polypropylene (PP).
[0022] Specifically, the inner wall of the distillation vessel 10 is made of enamel; the distillation vessel 10 is equipped with a distillation vessel stirrer 24; and the distillation vessel 10 is equipped with a distillation vessel insulation jacket 9 on the outside.
[0023] Specifically, the condenser 13 is made of stainless steel.
[0024] Specifically, vacuum pump 23 is a rotary vane vacuum pump.
[0025] Specifically, all pipes and valves in the synthesis unit are made of stainless steel.
[0026] Specifically, the components in the synthesis apparatus that come into contact with methyl pyruvate are free of iron.
[0027] The synthesis process of methyl pyruvate according to this invention is as follows: Methyl lactate, dichloromethane, and sodium bicarbonate are used as main raw materials. Methyl lactate and dichloromethane are pumped sequentially into reactor 2, followed by sodium bicarbonate and a catalyst. Stirring is started. When the temperature inside reactor 2 drops to approximately 14°C, an oxidant is added in batches. The temperature inside reactor 2 is controlled below 18°C. After the oxidant is added, the reaction is maintained at this temperature for 2 hours. After the temperature maintenance, the reaction is monitored in the GC system to check if the raw materials have reacted completely. Once the reaction is complete, the control valve at the bottom of reactor 2 is opened, and the reaction liquid in reactor 2 enters the filter press 6 for filtration. The filtrate is collected. The filtrate is collected in the distillation vessel 10. The rotary vane vacuum pump 23 is turned on, and the distillation is carried out at atmospheric pressure in the distillation vessel 10. Dichloromethane is distilled at atmospheric pressure and flows out through the outlet of the condenser 13. The outlet of the condenser 13 is connected to the inlet of the dichloromethane receiving vessel 16. Dichloromethane flows into the dichloromethane receiving vessel 16. No liquid flows out of the system. The inlet of the dichloromethane receiving vessel 16 is closed, and the rotary vane vacuum pump 23 is turned on again to distill methyl pyruvate under reduced pressure, so that the entire system is in a vacuum state. The distilled product flows into the vessel through the outlet of the condenser 13 and the inlet of the product receiving vessel 19, and a qualified product with a purity of ≥99.5% is obtained.
[0028] This invention relates to a methyl pyruvate synthesis apparatus. Methyl lactate, dichloromethane, and sodium bicarbonate are used as the main raw materials. Methyl lactate and dichloromethane are sequentially pumped into a reaction vessel, followed by the addition of sodium bicarbonate and a catalyst. Stirring is initiated, and when the temperature inside the reaction vessel drops to approximately 14°C, an oxidant is added in batches. The temperature inside the reaction vessel is controlled below 18°C. After the oxidant is added, the reaction is maintained at this temperature for 2 hours. After the maintenance period, the GC control panel monitors whether the raw materials have reacted completely. Once the raw materials have reacted completely, the control valve at the bottom of the reaction vessel is opened, and the reaction liquid enters a filter press. The process begins with pressure filtration, collecting the filtrate in a distillation kettle. A vacuum pump is then activated, and distillation is performed at atmospheric pressure in the kettle, starting with the distillation of dichloromethane. The dichloromethane flows out through the condenser outlet, which is connected to the inlet of the dichloromethane receiving kettle. No liquid flows out of the system. The inlet of the atmospheric pressure dichloromethane receiving kettle is then closed, and the vacuum pump is activated to distill methyl pyruvate under reduced pressure, bringing the entire system to a vacuum state. The distilled product flows into the kettle through the condenser outlet and the product receiving kettle inlet, yielding a qualified product (purity ≥ 99.5%). In summary, the synthesis process of methyl pyruvate using the apparatus described in this invention is advanced and reasonable, reducing production costs, shortening the synthesis route, and resulting in high product purity.
[0029] The above description is merely a preferred embodiment of this utility model. The protection scope of this utility model is not limited to the above embodiments. All technical solutions falling within the scope of this utility model's concept are protected. It should be noted that for those skilled in the art, any improvements and modifications made without departing from the principle of this utility model should also be considered within the protection scope of this utility model.
Claims
1. An apparatus for synthesizing methyl pyruvate, characterized in that, include: The reactor (2), plate and frame filter press (6), distillation vessel (10), condenser (13), product receiving vessel (19), dichloromethane receiving vessel (16) and vacuum pump (23). The outlet valve at the bottom of the reactor (2) is connected to the inlet end of the plate and frame filter press (6) via a pipeline; The outlet end of the plate and frame filter press (6) is connected to the inlet end of the distillation kettle (10) via a pipe; The outlet end of the top of the distillation vessel (10) is connected to the inlet end of the stainless steel condenser (13) via a pipe; The outlet end of the condenser (13) is connected to a T-type control valve; The first outlet of the T-type control valve is connected to the inlet of the dichloromethane receiving vessel (16) via a pipeline; The second outlet of the T-type control valve is connected to the inlet of the product receiving vessel (19) via a pipeline; The inlet end of the top of the product receiving vessel (19) is connected to the vacuum pump (23) via a pipe.
2. The apparatus for synthesizing methyl pyruvate according to claim 1, characterized in that: The inner wall of the reactor (2) is made of enamel. The reactor (2) is equipped with a reactor agitator (5); The reactor (2) is equipped with a reactor insulation jacket (3) on the outside.
3. The apparatus for synthesizing methyl pyruvate according to claim 1, characterized in that: The plate and frame filter press (6) is made of polypropylene (PP); The product receiving vessel (19) is made of polypropylene (PP); The material of the dichloromethane receiving vessel (16) is polypropylene (PP).
4. The apparatus for synthesizing methyl pyruvate according to claim 1, characterized in that: The inner wall of the distillation vessel (10) is made of enamel. The distillation vessel (10) is equipped with a distillation vessel stirrer (24); The distillation vessel (10) is equipped with a distillation vessel insulation jacket (9).
5. The apparatus for synthesizing methyl pyruvate according to claim 1, characterized in that: The condenser (13) is made of stainless steel.
6. The apparatus for synthesizing methyl pyruvate according to claim 1, characterized in that: The vacuum pump (23) is a rotary vane vacuum pump.
7. The apparatus for synthesizing methyl pyruvate according to claim 1, characterized in that: All pipes and valves in the synthesis unit are made of stainless steel.
8. The apparatus for synthesizing methyl pyruvate according to any one of claims 1-7, characterized in that: The components in the synthesis apparatus that come into contact with methyl pyruvate are free of iron.