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Method for synthesizing 3-amido-1,2-propanediol by pipe reactor

A technology of pipeline reactor and propylene glycol, which is applied in chemistry/physics/physicochemistry fixed reactor, preparation of functional groups substituted with amino groups, organic chemistry, etc., can solve the problems of poor reaction selectivity and many by-products, and achieve high yield The effect of high rate and short reaction time

Active Publication Date: 2008-08-27
ZHEJIANG HAIZHOU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its disadvantage is also that the reaction selectivity is not good, and there are many by-products.

Method used

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  • Method for synthesizing 3-amido-1,2-propanediol by pipe reactor
  • Method for synthesizing 3-amido-1,2-propanediol by pipe reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1, a kind of pipeline reactor synthetic 3-amino-1, the method for 2-propanediol, carry out following steps successively:

[0024] 1), ammoniation, namely the preparation of the mixed solution of 3-amino-1,2-propanediol and ammoniacal liquor:

[0025] The liquid phase chloroglycerol 55g (0.5mol) in the storage tank I 1 and the ammoniacal liquor of 40%wt in the storage tank II 2 are premixed earlier in the mixer 3 to form a reactant, and the mol ratio of chloroglycerin and ammonia is 1:10, mixer 3 is a static mixer. Then reactant is sent into pipeline reactor 4 with metering pump 10 and reacts, 70 ℃ of temperature of reaction, reaction pressure 4Mpa, pipeline reactor 4 is that an internal diameter is 4mm, the length is the cylindrical reactor of 30m; Control The flow rate of the metering pump 10 makes the flow rate of the reactant in the pipeline reactor 4 be 3.2l / h, even if the reaction time is about 7min; finally obtain the mixed solution of 3-amino-1,2-prop...

Embodiment 2

[0030] Embodiment 2, a method for synthesizing 3-amino-1,2-propanediol in a pipeline reactor, the device used is the same as in Example 1, and the following steps are carried out in sequence:

[0031] 1), ammoniation, namely the preparation of the mixed solution of 3-amino-1,2-propanediol and ammoniacal liquor:

[0032] After fully mixing chloroglycerin 55g (0.5mol) and ammonia water (80%wt) with a molar ratio of 1:15 (the molar ratio of chloroglycerin and ammonia), the reaction is carried out at a reaction temperature of 90°C and a reaction pressure of 6Mpa. The flow rate in the pipeline reactor 4 is 2.3 l / h, that is, the reaction time is controlled to be about 10 minutes; a mixed solution of 3-amino-1,2-propanediol and ammonia water is obtained.

[0033] 2), purification, i.e. the preparation of 3-amino-1,2-propanediol:

[0034] The above-mentioned mixed solution is returned to deamination through decompression flash evaporation; then the liquid obtained after the above-men...

Embodiment 3

[0035] Embodiment 3, a method for synthesizing 3-amino-1,2-propanediol in a pipeline reactor, the device used is the same as in Example 1, and specifically proceeds in the following steps:

[0036] 1), ammoniation, namely the preparation of the mixed solution of 3-amino-1,2-propanediol and ammoniacal liquor:

[0037] After fully mixing chloroglycerin 55g (0.5mol) and ammonia water (40%wt) with a molar ratio of 1:30 (the molar ratio of chloroglycerin and ammonia), the reaction is carried out at a reaction temperature of 80°C and a reaction pressure of 4Mpa. The flow rate in the pipeline reactor 4 is about 1.9 l / h, that is, the reaction time is controlled to be 12 minutes; a mixed solution of 3-amino-1,2-propanediol and ammonia water is obtained.

[0038] 2), purification, i.e. the preparation of 3-amino-1,2-propanediol:

[0039] The above-mentioned mixed solution is returned to deamination through decompression flash evaporation; then the liquid obtained after the above-mentio...

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Abstract

The invention discloses a method for synthesizing 3-amino-1, 2-propanediol via a tubular reactor, which comprises (1) ammoniation such as premixing liquid chlorine glycerol and ammonia water via a mixer, and reacting in a tubular reactor while the reaction temperature is 60-100DEG C, the pressure is 3-6MPa and the time is 6-12min, and obtain the mixture solution of 3-amino-1, 2-propanediol and ammonia water, (2) purification such as treating the mixture solution by depressurizing, flash evaporation and deamination, and treating the liquid after the deamination by adding alkali to neutralize, dehydrating, depressurizing and distilling, to obtain 3-amino-1, 2-propanediol. The synthesized 3-amino-1, 2-propanediol has the advantages of high yield.

Description

technical field [0001] The invention relates to a method for synthesizing compounds using a pipeline reactor, in particular to a pipeline synthesis method for 3-amino-1,2-propanediol. Background technique [0002] [0003] CH 2 ClCHOHCH 2 OH+NH 3 —→CH 2 NH 2 CHOHCH 2 Oh [0004] CH 2 NH 2 CHOHCH 2 OH+CH 2 ClCHOHCH 2 OH—→(CH 2 OHCHOHCH 2 ) 2 NH [0005] S-2 [0006] 3-Amino-1,2-propanediol with a molecular formula as shown in S-1 is widely used in the fields of pesticides and medicine, and is an important intermediate for the synthesis of non-ionic contrast agents. 3-Amino-1,2-propanediol is mainly obtained by ammoniation of chloroglycerin, and the reaction formula is shown in S-2. From the reaction point of view, in addition to the target product 3-amino-1,2-propanediol in the amination reaction of chloroglycerol, there are also side reactions in series to generate by-product bis(2,3-dihydroxypropyl)amine and even tertiary ( 2,3-D...

Claims

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Application Information

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IPC IPC(8): C07C215/10C07C209/08B01J19/24
Inventor 陈新志张海江钱超
Owner ZHEJIANG HAIZHOU PHARMA CO LTD
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