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A technology of aminocaproic acid and hydrochloric acid, which is applied in the field of preparation of 6-aminocaproic acid, can solve the problems of low product purity, achieve high product purity, shorten hydrolysis time, and simple operation
Active Publication Date: 2021-03-16
CHANGZHOU LANLING PHARMA
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[0011]
The purpose of the present invention is to solve the problem that the product purity of the existing caprolactam alkaline hydrolysis method is not high, and to provide a method for preparing 6-aminocaproic acid with high reaction yield and high product purity
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Embodiment 1）
[0029] The preparation method of the 6-aminocaproic acid of the present embodiment has the following steps:
[0030] ①Add 5.0g caprolactam, 2.1g sodium hydroxide and 25g demineralized water into a 100mL reaction flask, increase the pressure to 0.2MPa, heat up to 120°C, and carry out an alkaline hydrolysis reaction for 1h.
[0031] ② Cool the material after alkaline hydrolysis in step ① to room temperature, and neutralize it with hydrochloric acid with a concentration of 20wt% to pH=7.7±0.1.
[0032] ③ The material after the neutralization treatment in step ② is pressurized through a reverse osmosis device for desalination treatment, and the chloride ion content in the effluent is less than or equal to 10 mg / L as the end point.
[0033] ④ The material after the desalination treatment in step ③ is first decolorized with activated carbon, filtered, the filtrate is concentrated under reduced pressure at 50~65° C. to dryness, ethanol is added while hot, stirred for crystallization,...
Embodiment 2～ Embodiment 9）
[0036] The preparation method of each embodiment is basically the same as that of embodiment 1, and the difference lies in: the temperature, pressure and time of the alkaline hydrolysis reaction, as shown in Table 1 for details.
Embodiment 10～ Embodiment 11）
[0042] The preparation method of each embodiment is basically the same as that of embodiment 1, and the difference lies in: feeding amount, see Table 2 for details.
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Abstract
The invention discloses a preparation method of 6-aminocaproic acid, which comprises the following steps: by using caprolactam as a raw material, carrying out alkaline hydrolysis, neutralization treatment, desalination treatment and refining treatment to obtain the 6-aminocaproic acid, wherein the alkaline hydrolysis is carried out on caprolactam, sodium hydroxide and water at a certain temperature and under a certain pressure, a certain temperature is 115-125 DEG C, a certain pressure is 0.15-0.3 MPa, and the reaction time of alkaline hydrolysis does not exceed 1.5 hours. According to the alkaline hydrolysis method disclosed by the invention, the hydrolysis time is shortened through pressurization, so that the generation of by-products can be effectively inhibited under the condition of ensuring complete hydrolysis, and therefore, the alkaline hydrolysis method not only has relatively high reaction yield, but also has relatively high product purity.
Description
technical field [0001] The invention belongs to the technical field of pharmaceutical preparation, in particular to a preparation method of 6-aminocaproic acid. Background technique [0002] 6-Aminocaproic acid, molecular formula: C 6 H 13 NO 2 , is an important functional chemical. It is widely used in the medical field as a hemostatic drug at home and abroad. After it dissolves in water, it can hinder the fibrinolytic enzyme, thereby inhibiting the dissolution of fibrin, and can effectively prevent and treat the Bleeding due to increased fibrinolytic activity. [0003] At present, the preparation methods of 6-aminocaproic acid mainly include chemical synthesis method, biosynthesis method and caprolactam hydrolysis method. The disadvantages of the chemical synthesis method are: the synthesis route is long, the raw material cost is high, the by-products are not easy to control, and the yield is low. The disadvantage of the biosynthesis method is that expensive catalytic...
Claims
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