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Method and system for preparing 1, 3-butanediol with high selectivity

A high-selectivity, butanediol technology, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, and preparation of organic compounds, etc., can solve problems such as unstable output rate, achieve the effect of reducing side reactions and improving reaction efficiency

Pending Publication Date: 2020-08-25
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the maximum residence time of the material in this method is 24 hours, and the output of 0.51-0.92 tons of 1,3-butanediol per ton of acetaldehyde is unstable.

Method used

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  • Method and system for preparing 1, 3-butanediol with high selectivity

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Experimental program
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Effect test

Embodiment 1

[0045] In this embodiment, the inner diameter of the coiled tube of the coiled tube reactor 1 is 3.0 mm, the wall thickness is 0.8 mm, and the length is 35.0 m.

[0046] The experimental steps are as described above, wherein:

[0047] S1. Preparation of crude 3-hydroxybutyraldehyde: the inorganic base is 10wt% NaOH aqueous solution, and the mass ratio of acetaldehyde and NaOH entering coil reactor 1 is 25:1. The pH of the reaction system was 13.0, and the residence time of the reaction solution was 7.5 minutes. A cooling medium is passed through the interlayer of the heat exchange chamber, and the reaction temperature is controlled to maintain at 3.0±0.8°C.

[0048] S3. Preparation of 1,3-butanediol by hydrogenation: the mass ratio of the skeleton nickel catalyst to the crude 3-hydroxybutyraldehyde solution in the two hydrogenation reactors is 1:6, the reaction temperature is 70°C, and the reaction pressure is 3.5 MPa, the hydrogenation reaction time is 25min.

[0049] Acco...

Embodiment 2

[0051] In this embodiment, the inner diameter of the coiled tube of the coiled tube reactor 1 is 4.0 mm, the wall thickness is 0.9 mm, and the length is 37.5 m.

[0052] The experimental steps are as described above, wherein:

[0053] S1. Preparation of crude 3-hydroxybutyraldehyde: the inorganic base is 10wt% KOH aqueous solution, and the mass ratio of acetaldehyde and KOH entering coil reactor 1 is 35:1. The pH of the reaction system was 13.0, and the residence time of the reaction solution was 6 minutes. A cooling medium is passed through the interlayer of the heat exchange chamber, and the reaction temperature is controlled to maintain at 2.0±0.8°C.

[0054] S3. Preparation of 1,3-butanediol by hydrogenation: the mass ratio of the skeleton nickel catalyst to the crude 3-hydroxybutyraldehyde solution in the two hydrogenation reactors is 1:8, the reaction temperature is 66°C, and the reaction pressure is 4.5 MPa, the hydrogenation reaction time is 30min.

[0055] Accordin...

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Abstract

The invention provides a method and a system for preparing 1, 3-butanediol with high selectivity. According to the scheme, the method comprises the following steps: by taking acetaldehyde as a raw material and inorganic base as a catalyst, carrying out a condensation reaction in a coiled tube type reactor under the condition that the pH value is 11-14; regulating the pH value of the reaction solution to be neutral, and separating unreacted acetaldehyde and a crude 3-hydroxybutyraldehyde solution; and carrying out catalytic hydrogenation at 60-90 DEG C by using a skeleton nickel catalyst to obtain a crude 1, 3-butanediol solution. According to the method and the system, the coiled tube type condensation reactor which is extremely beneficial to heat transfer is adopted, so that the reactiontemperature, the material ratio and the retention time can be accurately controlled. Meanwhile, in the hydrogenation reaction step, a lower hydrogenation temperature and reaction kettles connected inseries are adopted, so that side reactions are effectively reduced. According to the reaction process, the reaction efficiency, the reaction stability and the product selectivity are improved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method and system of 1,3-butanediol. Background technique [0002] 1,3-Butanediol has good hygroscopicity and water solubility, is odorless and low-toxic, and has the reactivity of diols. 1,3-Butanediol has a wide range of uses, and can be used to produce plasticizers, unsaturated polyester resins, industrial dehydrating agents, etc.; it can also be used as moisturizers and softeners for textiles, tobacco and paper, cheese or Antibacterial agent for meat, etc.; it can also be used as a moisturizer in cosmetics. [0003] At present, in the preparation method of 1,3-butanediol, the acetaldehyde condensation method is the mainstream. Its production process is as follows: in a tank reactor, acetaldehyde undergoes condensation reaction in alkaline aqueous solution to generate 3-hydroxybutyraldehyde, and after adding acid to neutralize the reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/152C07C31/20
CPCC07C29/152C07C31/207
Inventor 武金丹刘喆邴威瀚杨光靳权王聪刘新伟杨克俭霍瑜姝梁秀霞
Owner CHINA TIANCHEN ENG
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