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Decarburization filtering device and method for preparing aminolevulinic acid hydrochloride

A technology of aminolevulinic acid hydrochloride and filtration device, which is applied in the direction of filtration loop, filtration separation, separation method, etc., can solve the problems of slow speed, poor filtration efficiency, affecting progress, etc., and achieve a short process, good quality, and improved efficiency. Effect

Active Publication Date: 2020-06-09
SHANGHAI WANXIANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Since the level of the feed inlet is lower than that of the discharge outlet, the mixed solution to be treated entering the feed inlet will have a lower filtration efficiency due to its own gravity due to the filtering operation from bottom to top. Poor, slow speed, this time will inevitably affect the entire progress, so it is necessary to propose a new technical solution to solve the above problems

Method used

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  • Decarburization filtering device and method for preparing aminolevulinic acid hydrochloride
  • Decarburization filtering device and method for preparing aminolevulinic acid hydrochloride
  • Decarburization filtering device and method for preparing aminolevulinic acid hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: a kind of decarbonization filtering device, such as figure 1 As shown, it includes a frame 1, and a casing 2 fixedly installed on the frame 1 with an open upper end and a hollow interior. The casing 2 is in the form of a cylindrical barrel, and a cover 3 is detachably connected to the opening. The above-mentioned cover body 3 can be sealed and closed on the casing 2, and the casing 2 is provided with a material inlet 5 and a material outlet 6 sequentially from bottom to top.

[0049] Such as figure 1 As shown, in order to increase the retention of activated carbon, a filter plate 7 arranged horizontally is rotatably connected to the housing 2 . The filter plate 7 is disc-shaped, and there is a gap between it and the inner wall of the housing 2 . There is a filter cavity 8 between the filter plate 7 and the feed port 5. The filter plate 7 communicates with a central tube 9 on the side away from the filter cavity 8, and the central tube 9 communicates with ...

Embodiment 2

[0056] Embodiment 2: a kind of method for preparing aminolevulinic acid hydrochloride comprises the following steps:

[0057] Step 1. Add 5-phthalimide levulinic acid to 400ml of 5mol / L hydrochloric acid solution, reflux for 4 hours, cool slightly, add activated carbon, and decolorize through the decarbonization filter device of Example 1 at 80°C. Cool to 5°C and filter. Concentrate the filtrate, cool at 5°C, precipitate crystals, filter, and vacuum-dry the filter cake for 4 hours under a vacuum of 0.8 MPa to obtain the crude product.

[0058] Wherein, the molecular formula of 5-phthalimide levulinic acid: C13H11O5N, its chemical structural formula is as follows:

[0059]

[0060] Step 2, finishing: add the water (60 ℃) of the same quantity as crude product feed to dissolve crude product, filter, add the acetone of 50wt% of crude product feed rate, cool to room temperature (20 ℃), place 4 ℃, after 3 hours put The solid-liquid mixture was filtered, and the obtained crystal...

Embodiment 3

[0063] Embodiment 3: a kind of method for preparing aminolevulinic acid hydrochloride comprises the following steps:

[0064] Step 1. Add 5-phthalimide levulinic acid into 500ml of 8mol / L hydrochloric acid solution, reflux for 8 hours, cool slightly, add activated carbon, and decolorize through the decarbonization filter device of Example 1 at 90°C. Cool to 15°C and filter. Concentrate the filtrate, cool at 15°C, precipitate crystals, filter, and vacuum-dry the filter cake for 5 hours under a vacuum of 1.0 MPa to obtain the crude product.

[0065] Step 2, finishing: add the water (75 ℃) of the same quantity as crude product feed to dissolve crude product, filter, add the acetone of 50wt% of crude product feed rate, cool to room temperature (20 ℃), place 8 ℃, after 4 hours put The solid-liquid mixture was filtered, and the obtained crystal was vacuum-dried for 15 hours to obtain the fine product of aminolevulinic acid hydrochloride.

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Abstract

The invention relates to a decarburization filtering device and a method for preparing aminolevulinic acid hydrochloride, and belongs to the technical field of aminolevulinic acid hydrochloride production. The decarburization filtering device comprises a shell and a cover body, the shell is provided with a filter plate and a central pipe, and the central pipe is communicated with a plurality of first filter elements. A bracket, a clamping ring rotationally connected with the central pipe and a motor are arranged on the inner wall of the shell, and an output shaft of the motor coincides with the central axis of the central pipe. The shell is provided with a baffle connected with the central pipe through a bearing, and the baffle is fixedly arranged on the inner wall of the shell. Second filter elements are arranged in the shell and communicated with a main pipe, one end of the main pipe is sealed, and the other end of the main pipe is connected to a discharge port. The preparation method comprises the following steps: adding 5-phthalimide levulinic acid into a hydrochloric acid solution for reflux, slightly cooling, adding activated carbon for decolorization, and filtering; and cooling the concentrated filtrate, separating out crystals, filtering, carrying out vacuum drying on the filter cake, and recrystallizing with acetone / water to obtain a fine aminolevulinic acid hydrochloride product. Filtration is accelerated by virtue of centrifugal force, the decarburization efficiency is high, and the obtained aminolevulinic acid hydrochloride is high in yield and good in quality.

Description

technical field [0001] The invention relates to the technical field of production of aminolevulinic acid hydrochloride, more specifically, it relates to a decarbonization filter device and a method for preparing aminolevulinic acid hydrochloride. Background technique [0002] Aminolevulinic acid hydrochloride (abbreviation: 5-ALA, ALA), is a second-generation photosensitizer developed in recent years, and is a precursor of hemoglobin synthesis in vivo. [0003] A study conducted by several authoritative institutions in China shows that the treatment of genital warts with aminolevulinic acid hydrochloride can effectively reduce the recurrence rate of the disease while obtaining a high cure rate. The study was jointly carried out by 5 medical institutions including Peking University First Hospital. During the 1-year study period, a total of 453 patients with condyloma acuminatum were included. The results showed that the wart removal rate of ALA was 98.44%, and there were no ...

Claims

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Application Information

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IPC IPC(8): B01D36/02B01D15/00C07C227/18C07C229/22
CPCB01D15/00B01D36/02C07C227/18C07C229/22
Inventor 袁相富胡志奇张崇东
Owner SHANGHAI WANXIANG PHARMA