A method for preparing 3-methylthiopropanol by catalytic hydrogenation

A technology for the catalytic hydrogenation of methylthiopropanol, which is applied in the chemical industry, can solve the problems of complex preparation process, dangerous raw materials, high equipment and operation requirements, and achieve clean and simple reaction raw materials, easy-to-operate and controllable reaction conditions, and easy operation and low equipment requirements

Active Publication Date: 2020-09-22
LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method realizes the simple and direct method of producing alcohol from aldehyde, the reductant used is highly active and dangerous, and the reductant needs to be slowly added dropwise at sub-zero temperature for reaction. The control of reaction conditions is relatively harsh, and the requirements for equipment and operation are high. The cost of the reducing agent used is high and the remaining saline waste liquid needs to be treated, so there are many unfavorable factors in industrialization
[0005] In summary, the traditional addition route to prepare 3-methylthiopropanol has problems such as complicated preparation process, difficult to remove impurities, and low yield. However, direct reduction of 3-methylthiopropanol using borohydride and lithium aluminum hydride The cost of preparing 3-methylthiopropanol from aldehydes is relatively high, the reaction conditions are harsh, and the raw materials are dangerous to a certain extent, which is not conducive to large-scale industrial production. Therefore, it is necessary to provide a simple, direct, safe and stable, easy to operate and control, and environmentally friendly. Continuous new method with more characteristics of industrialized mass production to realize efficient and sustainable preparation of 3-methylthiopropanal to 3-methylthiopropanol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Preparation of ultrafine amorphous catalyst (CoFeB)

[0030] 1 mol of analytically pure dark red cobalt acetate and 0.01 to 0.3 mol of ferric chloride were dissolved in 2.5 times the volume of ethanol, and stirred vigorously at 20 to 30°C until all of them were dissolved to obtain a brown-red clear solution. Slow down the stirring, start the ultrasonic wave to cover the reaction liquid under the ultrasonic atmosphere, the ultrasonic frequency is 20~40Hz, and at the same time, use a peristaltic pump to drip fresh 2mol / L potassium borohydride into the reaction liquid at a flow rate of 1~3ml / min. A large amount of hydrogen gas bubbles and black solid powder precipitated out of the solution at the same time, continue to slowly add potassium borohydride until the dripping is complete, continue to stir and react under ultrasonic atmosphere for 10 to 30 minutes, after the reaction is completed, suction filtration, repeated washing with deionized water to remove The salt...

Embodiment 2

[0032] Example 2 Mixed alcohol ratio experiment (ethanol:glycerol=6:1)

[0033] 1 mol of 3-methylthiopropionaldehyde with a purity greater than 99% and a monomer content greater than 95% is added to a mixed solution of ethanol and glycerin to prepare a 3-methylthiopropionaldehyde mixed alcohol solution with a concentration of 10 to 90% by weight. Ethanol in mixed alcohol solution: glycerol = 6:1. The mixed solution was transferred to the reactor, and the ultrafine amorphous CoFeB catalyst prepared in Example 1 was added with 1 to 30 wt% relative to the raw material, stirred at 40 to 50°C and injected with hydrogen at a pressure of 1 to 3Mpa for reaction for 30 to 180 minutes. At the end of the reaction, the reaction solution was transferred out under reduced pressure distillation, ethanol and 3-methylthiopropanol were recovered respectively, and glycerin was transferred out directly from the bottom of the kettle. The 3-methylthiopropanol with a purity of more than 99% is obtaine...

Embodiment 3

[0035] Example 3 Mixed alcohol ratio experiment (ethanol:glycerol=4:1)

[0036] 1 mol of 3-methylthiopropionaldehyde with a purity greater than 99% and a monomer content greater than 95% is added to a mixed solution of ethanol and glycerin to prepare a 3-methylthiopropionaldehyde mixed alcohol solution with a concentration of 10 to 90% by weight. . Ethanol in mixed alcohol solution: glycerol = 4:1. The mixed solution was transferred to the reactor, and the ultrafine amorphous CoFeB catalyst prepared in Example 1 was added with 1 to 30 wt% relative to the raw material, stirred at 40 to 50°C and injected with hydrogen at a pressure of 1 to 3Mpa for reaction for 30 to 180 minutes. At the end of the reaction, the reaction solution was transferred out under reduced pressure distillation, ethanol and 3-methylthiopropanol were recovered respectively, and glycerin was transferred out directly from the bottom of the kettle. The 3-methylthiopropanol with a purity of more than 99% is obta...

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Abstract

The invention discloses a method for preparing 3-methylthiopropanol by efficiently catalyzing 3-methylthiopropanal for carrying out hydrogenation reduction by using superfine amorphous boron series metallic compounds at lower temperature. According to the method disclosed by the invention, by adopting hierarchical alcohol mixtures with high and low boiling points and high and low viscosities as diluting solvents, the problems of raw material polymerization and product separation are effectively solved. The catalytic hydrogenation activity and efficiency of the superfine amorphous boron seriesmetallic compound catalyst are excellent at the relatively low temperature near normal temperature, and the purity of the obtained 3-methylthiopropanol is greater than 99 percent; no negative substances such as by-product salt, toxic raw materials, wastewater and the like are generated in the whole preparation process, and therefore, the method is clean, environmentally-friendly and sustainable.

Description

Technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for preparing 3-methylthiopropanol by catalytic hydrogenation. Background technique [0002] 3-Methylthiopropanol, commonly known as pinapple alcohol, is a spice ingredient naturally found in foods such as apples, tomatoes, bacon, wine, soy sauce and fermented foods. It has a strong sweet aroma, meat or broth-like aroma at low concentration. It is widely used in the blending of meat flavors and the aroma adjustment of fruits, vegetables, sauces, wines, etc. It is included in the national standard (GB 2760-2011 National Food Safety Standard Food Additive Use Standard", No. S0687) safe edible spices. [0003] With the continuous improvement of people's living standards, the market demand for 3-methylthiopropanol is increasing. Due to cost and technology constraints, the current industrial production of 3-methylthiopropanol is mainly chemical synthesis. Generally, the tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/20C07C319/28C07C323/12B01J23/75B01J23/835
CPCB01J23/75B01J23/835C07C319/20C07C319/28C07C323/12
Inventor 周荣超彭启明廖常福
Owner LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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