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Preparation method of 2-aminopropanol

An aminopropanol, liquid ammonia technology, applied in the preparation of aminohydroxy compounds, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of large amount of waste water, high equipment requirements, low product selectivity, etc., and achieve the catalyst life. Improve, high atom utilization, reduce the effect of ring-opening polymerization

Active Publication Date: 2022-02-11
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this method are high production cost, large amount of catalyst, low selectivity in the two-step catalytic process, and difficult separation of by-products
The disadvantage of this method is that propylene oxide and hydrochloric acid ring-opening main products are mostly 1-chloro-2-propanol (alpha-chloropropanol), and the product selectivity is low
The disadvantage of this method is that the yield in the reaction process of paraformaldehyde and nitroethane is low, often no more than 65%, and the amount of waste water in the process is large, and 2-nitropropanol is easy to explode when heated to 120 ° C. higher risk
[0008] Patent CN110981738A discloses a method for preparing 2-aminopropanol by catalyzing the reaction of propylene oxide and liquid ammonia with a rare-earth modified catalyst. The hydrogen-type mordenite molecular sieve modified by rare-earth nitrate is used as the catalyst. The disadvantage of the method is that the catalyst high manufacturing cost
[0010] (1) The cost of raw materials and catalysts is high, which limits large-scale industrial production;
[0011] (2) The process is complicated, the utilization rate of atoms is low, the requirements for equipment are high, and the amount of three wastes generated in the production process is large;
[0012] (3) The yield is low, the separation of crude products is difficult, and the product purity is difficult to meet the requirements of the pharmaceutical industry

Method used

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  • Preparation method of 2-aminopropanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] [Preparation Example 1] Preparation of FeCl 3 , AlCl 3 Modified Macroporous Styrenic Strongly Acidic Cation Exchange Resin

[0051] a. Resin pretreatment: wash the macroporous styrene-based strongly acidic cation exchange resin with absolute ethanol for 12 hours, and then wash with deionized water until the effluent is colorless; continuously purge and dry with nitrogen at 70°C until constant weight.

[0052] b. The first modification of Lewis acid:

[0053] The preparation mass concentration is 2% FeCl 3 Ethanol solution, make the pretreated macroporous styrene-based strongly acidic cation exchange resin fully react with it for 12h, the reaction temperature is 50°C, and carry out the first modification; then wash 5 times with deionized water, and then wash 5 times with acetone times, and finally washed with deionized water until chlorine-free (using AgNO with a mass fraction of 1%) 3 The solution was titrated with the cleaning solution, and no precipitation after t...

Embodiment 2-7 and comparative example 1-3

[0067] The other examples and comparative examples were carried out according to the steps substantially the same as in Example 1, the only difference being that the reaction conditions and parameters shown in Table 2 were different.

[0068] Catalyst service life evaluation:

[0069] Catalysts A, F, G, and H were respectively subjected to a continuous catalytic efficiency test according to the operation method in Example 1, and the conversion rate of the raw material and the selectivity of the product were recorded after the catalyst was running for a long time, as shown in Table 4.

[0070] Different reaction conditions and parameters in table 2, each embodiment and comparative examples

[0071]

[0072]

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Abstract

The invention discloses a preparation method of 2-aminopropanol. The preparation method comprises the steps of 1) mixing anhydrous liquid ammonia and epoxypropane, and preheating; 2) feeding the preheated reaction raw materials into a reactor filled with Lewis acid modified strong acid cation exchange resin for reaction, and controlling the reaction temperature to be 60-120 DEG C and the reaction pressure to be 1-8 MPa; (3) after the reaction is completed, feeding reaction liquid into a deamination tower, and separating out unreacted liquid ammonia and epoxypropane; and 4) feeding the tower bottom extract into a rectifying tower, and further rectifying and purifying to obtain the product 2-aminopropanol. According to the method, low-cost epoxypropane and liquid ammonia are used as raw materials, 2-aminopropanol can be synthesized under the catalysis of the modified ion exchange resin under mild reaction conditions. The method has the advantages of being low in raw material cost, high in product purity, mild in process condition, simple in process flow, high in atom utilization rate, small in discharge amount of three wastes and the like.

Description

technical field [0001] The invention relates to a preparation method of 2-aminopropanol, in particular to a preparation method of 2-aminopropanol. Background technique [0002] Ofloxacin, as the third-generation quinolone antibacterial drug, has the advantages of broad antibacterial spectrum, strong antibacterial activity, convenient administration, small adverse reactions, and no cross-resistance with other antibiotics, so it has become the first choice for clinical combination drugs. Surpassing cephalosporin antibiotics, it has become the largest antibacterial drug, and the demand is still growing. At present, 2-aminopropanol is mostly used as the starting material for the industrial production of ofloxacin in China. [0003] At present, the method for synthesizing 2-aminopropanol mainly includes hydroxyacetone ammonolysis method, alanine reduction method, 2-chloro-1-propanol ammonolysis method, nitroethane method and propylene oxide catalytic amination method etc., for e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/04C07C215/08B01J31/10
CPCC07C213/04B01J31/10B01J2231/4283C07C215/08Y02P20/10
Inventor 李昱学张聪颖刘宝现王宁宁刘盼盼迟森森孙淑常
Owner WANHUA CHEM GRP CO LTD
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