Production device of 5-aminolevulinic acid methyl ester hydrochloride
By designing a methyl 5-aminolevulinate hydrochloride production device containing a mixing tank, reactor, decolorization tank and condenser, the reaction is catalyzed by anhydrous methanol and sulfoxide chloride, combining purified water, activated carbon and condensation. Reflow solves the problems of high ammonia nitrogen wastewater and high cost in the prior art, and achieves high purity, low cost and environmentally friendly production results.
Patent Information
- Application Number
- CN202420907985.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-26
- Publication Date
- 2024-12-24
- Estimated Expiration
- 2034-04-26
AI Technical Summary
There is a problem of high ammonia nitrogen wastewater in the existing 5-aminolevulinate hydrochloride production methods, which affects product quality and environment, and has a high production cost.
A production device including a mixing tank, reactor, decolorizing tank, crystallization tank and condenser was designed. By adding anhydrous methanol and sulfoxide chloride, decolorizing and crystallizing using purified water and activated carbon, combined with condensation reflux and Filters to achieve high purity and low cost production of products.
It improves the purity and color of the product, reduces the production of high ammonia nitrogen wastewater, reduces production costs, and reduces raw material waste and pollution through the recycling of methanol and the effective utilization of activated carbon, and achieves environmental friendliness.
Smart Images
Figure CN222219568U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of 5-aminolevulinic acid methyl ester hydrochloride production, and in particular to a production device for 5-aminolevulinic acid methyl ester hydrochloride. Background Art
[0002] 5-aminolevulinic acid methyl ester hydrochloride (ALA-M for short) is a lipid derivative of ALA, which is widely used in many fields such as medicine, pesticides, cosmetics and photodynamic therapy. Due to its unique biological activity and chemical properties, 5-aminolevulinic acid methyl ester hydrochloride has become one of the hot spots in chemical research and industrial applications.
[0003] Chinese patent CN111517973B discloses a production method for preparing 5-aminolevulinic acid hydrochloride from a fermentation broth. The method uses ammonia water for analysis, which results in a large amount of ammonium ions in the product, which are difficult to remove and affect the product quality. At the same time, a large amount of high-ammonia nitrogen wastewater is generated during resin regeneration, which is difficult to treat, increases the cost of wastewater treatment, and pollutes the environment. Summary of the invention
[0004] The technical problem to be solved by the utility model is: in view of the deficiencies in the prior art, a production device for 5-aminolevulinic acid methyl ester hydrochloride is provided, which has low production cost and is environmentally friendly.
[0005] In order to solve the above technical problems, the technical solution of the utility model is:
[0006] The invention comprises a mixing tank, wherein the inlet of the mixing tank is connected to a 5-aminolevulinic acid hydrochloride tank and a methanol tank through pipelines, the outlet of the mixing tank is connected to a reactor through a pipeline, the inlet of the reactor is connected to a thionyl chloride tank through a pipeline, and the bottom outlet of the reactor is connected to a 5-aminolevulinic acid methyl ester hydrochloride crude product tank through a pipeline.
[0007] As an improved technical solution, the inlet of the reactor is connected to a purified water tank through a pipeline, the outlet of the reactor is connected to a decolorization tank through a pipeline, the inlet of the decolorization tank is connected to an activated carbon tank through a pipeline, the outlet of the decolorization tank is connected to a crystallization tank through a pipeline, and the outlet of the crystallization tank is connected to a 5-aminolevulinic acid methyl ester hydrochloride finished product tank through a pipeline.
[0008] As an improved technical solution, a first automatic regulating valve is provided on the outlet pipe of the hydrochloric acid solution tank, a pH sensor is provided in the reactor, and the first automatic regulating valve and the pH sensor are interlocked to a control system.
[0009] As an improved technical solution, the upper gas phase outlet of the reactor is connected to a condenser through a pipeline, and the lower outlet of the condenser is connected to a recovery tank through a pipeline.
[0010] As an improved technical solution, the outlet of the recovery tank is connected to the methanol tank through a pipeline.
[0011] As an improved technical solution, the outlet of the decolorization tank is connected to a filter through a pipeline, and the liquid phase outlet of the filter is connected to the crystallization tank through a pipeline.
[0012] As a preferred technical solution, a temperature sensor is provided in the crystallization tank, a second automatic regulating valve is provided on the jacket cooling water inlet pipe of the crystallization tank, and the second automatic regulating valve and the temperature sensor are interlocked to a control system.
[0013] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:
[0014] The utility model includes a mixing tank, the inlet of the mixing tank is connected to a 5-aminolevulinic acid hydrochloride tank and a methanol tank through pipelines, the outlet of the mixing tank is connected to a reactor through a pipeline, the inlet of the reactor is connected to a thionyl chloride tank through a pipeline, and the bottom outlet of the reactor is connected to a 5-aminolevulinic acid methyl ester hydrochloride crude product tank through a pipeline. 5-aminolevulinic acid hydrochloride is dissolved by adding anhydrous methanol, and then a thionyl chloride catalyst is added to obtain a 5-aminolevulinic acid methyl ester hydrochloride crude product after reaction, the product purity is higher, and high ammonia nitrogen sewage will not be generated, which is environmentally friendly and reduces production costs.
[0015] The inlet of the reactor of the utility model is connected to a purified water tank through a pipeline, the outlet of the reactor is connected to a decolorizing tank through a pipeline, the inlet of the decolorizing tank is connected to an activated carbon tank through a pipeline, the outlet of the decolorizing tank is connected to a crystallizing tank through a pipeline, and the outlet of the crystallizing tank is connected to a 5-aminolevulinic acid methyl ester hydrochloride finished product tank through a pipeline. Purified water is added to dissolve the crude 5-aminolevulinic acid methyl ester hydrochloride, and then activated carbon is added for decolorization, and the obtained decolorizing solution is crystallized again to obtain the 5-aminolevulinic acid methyl ester hydrochloride finished product, and the product has low chroma and good quality.
[0016] The upper gas phase outlet of the reactor is connected to a condenser through a pipeline, and the lower outlet of the condenser is connected to a recovery tank through a pipeline. Through condensation and reflux, methanol is evaporated and recovered, and a crude product of 5-aminolevulinic acid methyl ester hydrochloride is obtained, which is simple to operate and reduces the waste of raw materials.
[0017] The outlet of the recovery tank is connected to the methanol tank through a pipeline, so that the collected methanol is reused, while also reducing product losses, improving product yields, and reducing raw material costs.
[0018] The outlet of the decolorizing tank is connected to a filter through a pipeline, and the liquid phase outlet of the filter is connected to the crystallizing tank through a pipeline. The activated carbon is filtered out by the filter, thereby improving the purity of the product in the decolorizing liquid.
[0019] A temperature sensor is provided in the crystallizer, and an automatic regulating valve is provided on the cooling water inlet pipe of the jacket of the crystallizer. The automatic regulating valve and the temperature sensor are interlocked to a control system. The control system adjusts the opening of the automatic regulating valve according to the value of the temperature sensor, so that the decolorizing liquid is cooled at a rate of 3-5°C / h, and the crystallization effect is better. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] The utility model is further described below in conjunction with the accompanying drawings and embodiments.
[0021] Figure 1 It is a structural schematic diagram of an embodiment of the utility model;
[0022] Among them: 1. mixing tank; 2. 5-aminolevulinic acid hydrochloride tank; 3. methanol tank; 4. reactor; 5. thionyl chloride tank; 6. 5-aminolevulinic acid methyl ester hydrochloride crude product tank; 7. purified water tank; 8. decolorization tank; 9. activated carbon tank; 10. crystallization tank; 11. 5-aminolevulinic acid methyl ester hydrochloride finished product tank; 12. condenser; 13. recovery tank; 14. filter; 15. temperature sensor; 16. automatic regulating valve. DETAILED DESCRIPTION
[0023] The present invention is further described below in conjunction with the accompanying drawings and embodiments.
[0024] like Figure 1 As shown, a method includes a mixing tank 1, wherein the inlet of the mixing tank 1 is connected to a 5-aminolevulinic acid hydrochloride tank 2 and a methanol tank 3 through pipelines, respectively, the outlet of the mixing tank 1 is connected to a reactor 4 through a pipeline, the inlet of the reactor 4 is connected to a thionyl chloride tank 5 through a pipeline, and the bottom outlet of the reactor 4 is connected to a 5-aminolevulinic acid methyl ester hydrochloride crude product tank 6 through a pipeline. 5-aminolevulinic acid hydrochloride is dissolved by adding anhydrous methanol, and then a thionyl chloride catalyst is added to obtain a crude 5-aminolevulinic acid methyl ester hydrochloride after the reaction, and the product purity is higher, and high ammonia nitrogen wastewater will not be generated, which is environmentally friendly and reduces the production cost.
[0025] The inlet of the reactor 4 is connected to a purified water tank 7 through a pipeline, the outlet of the reactor 4 is connected to a decolorizing tank 8 through a pipeline, the inlet of the decolorizing tank 8 is connected to an activated carbon tank 9 through a pipeline, the outlet of the decolorizing tank 8 is connected to a crystallization tank 10 through a pipeline, and the outlet of the crystallization tank 10 is connected to a 5-aminolevulinic acid methyl ester hydrochloride finished product tank 11 through a pipeline. The crude 5-aminolevulinic acid methyl ester hydrochloride is dissolved by adding purified water, and then activated carbon is added for decolorization, and the obtained decolorized liquid is crystallized again to obtain the 5-aminolevulinic acid methyl ester hydrochloride finished product, and the product has low chroma and good quality.
[0026] The upper gas phase outlet of the reactor 4 is connected to a condenser 12 through a pipeline, and the lower outlet of the condenser 12 is connected to a recovery tank 13 through a pipeline. Through condensation and reflux, methanol is evaporated and recovered, and a crude product of 5-aminolevulinic acid methyl ester hydrochloride is obtained, which is simple to operate and reduces the waste of raw materials.
[0027] The outlet of the recovery tank 13 is connected to the methanol tank 3 through a pipeline, so that the collected methanol is reused, while also reducing the loss of the product, improving the product yield and reducing the raw material cost.
[0028] The outlet of the decolorizing tank 8 is connected to a filter 14 through a pipeline, and the liquid phase outlet of the filter 14 is connected to the crystallization tank 10 through a pipeline. The activated carbon is filtered out by the filter 14, thereby improving the purity of the product in the decolorizing liquid.
[0029] A temperature sensor 15 is provided in the crystallizer 10, and an automatic regulating valve 16 is provided on the cooling water inlet pipe of the jacket of the crystallizer 10. The automatic regulating valve 16 and the temperature sensor 15 are interlocked to the control system. The control system adjusts the opening of the automatic regulating valve 16 according to the value of the temperature sensor 15, so that the decolorizing solution is cooled at a rate of 3-5°C / h, and the crystallization effect is better.
[0030] It should be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the claims attached to this application.
Claims
1. 5-aminolevulinic acid methyl ester hydrochloride production device, characterized in that: The invention comprises a mixing tank, wherein the inlet of the mixing tank is connected to a 5-aminolevulinic acid hydrochloride tank and a methanol tank through pipelines, the outlet of the mixing tank is connected to a reactor through a pipeline, the inlet of the reactor is connected to a thionyl chloride tank through a pipeline, and the bottom outlet of the reactor is connected to a 5-aminolevulinic acid methyl ester hydrochloride crude product tank through a pipeline.
2. The production device of 5-aminolevulinic acid methyl ester hydrochloride as claimed in claim 1, characterized in that: The inlet of the reactor is connected to a purified water tank through a pipeline, the outlet of the reactor is connected to a decolorization tank through a pipeline, the inlet of the decolorization tank is connected to an activated carbon tank through a pipeline, the outlet of the decolorization tank is connected to a crystallization tank through a pipeline, and the outlet of the crystallization tank is connected to a 5-aminolevulinic acid methyl ester hydrochloride finished product tank through a pipeline.
3. The production device of 5-aminolevulinic acid methyl ester hydrochloride as claimed in claim 1, characterized in that: The upper gas phase outlet of the reactor is connected to a condenser through a pipeline, and the lower outlet of the condenser is connected to a recovery tank through a pipeline.
4. The production device of 5-aminolevulinic acid methyl ester hydrochloride as claimed in claim 3, characterized in that: The outlet of the recovery tank is connected to the methanol tank through a pipeline.
5. The production device of 5-aminolevulinic acid methyl ester hydrochloride as claimed in claim 1, characterized in that: The outlet of the decolorizing tank is connected to a filter through a pipeline, and the liquid phase outlet of the filter is connected to the crystallization tank through a pipeline.
6. The production device of 5-aminolevulinic acid methyl ester hydrochloride as claimed in claim 2, characterized in that: A temperature sensor is arranged in the crystallization tank, and an automatic regulating valve is arranged on the cooling water inlet pipe of the jacket of the crystallization tank. The automatic regulating valve and the temperature sensor are interlocked to a control system.