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Preparation method of 3-methylthiopropionaldehyde

A technology for the crude product of methionaldehyde and methionaldehyde, which is applied in the field of preparation of 3-methylthiopropionaldehyde, can solve the problems of resource waste, impact on yield, and ineffective recovery, and achieve cost savings and enhanced Degree of dissociation, effect of reducing production cost

Pending Publication Date: 2022-02-18
NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problems mentioned in the background technology, the object of the present invention is to provide a kind of preparation method of 3-methylthiopropanal, on the one hand solves the one-way use of catalyst, causes waste of resources, and in the refining and storage of follow-up MMP It leads to instability, so that the polymer generation affects the yield. On the other hand, it solves the problem that the beneficial components MMP, AC and MC light components in the light components are not effectively recovered and increase the cost.

Method used

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  • Preparation method of 3-methylthiopropionaldehyde
  • Preparation method of 3-methylthiopropionaldehyde
  • Preparation method of 3-methylthiopropionaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 1000g of crude MMP prepared by conventional production methods, add 100g of water, keep warm at 30°C, prepare 10 groups, and stir for 10 minutes until the system is white, start timing from the stop of stirring, and take out at 5, 10, 20, 30, and 60 minutes The lower MMP of the two groups of samples, a total of 10 groups, each with a mass of 400g; the remaining 10 groups of upper samples were respectively added with 100g of 99wt% AC and 88.6g of 97.6wt% MC to react at 30°C. When the sum of the mass fractions of MC and AC in the system is less than 1%, the timing is stopped, and the standing separation time and addition reaction time of each group are recorded, see Table 1.

[0029]

[0030] Table 1

Embodiment 2

[0032] Take 1000g of refined MMP (the content of MMP is 99.4wt%, the content of methyl mercaptan is 0.13wt%, and the content of acrolein is 0.05wt%), add 1g of glacial acetic acid and 0.67g of pyridine, prepare 10 groups, and add water to each group 0, 10, 50, 100, 200g, then add 100g 99wt% AC, 88.6g 97.6wt% MC, react at 30°C, the stirring speed is 500r / min, start timing from the addition of MC, until the MC in the system When the sum of the mass fractions of AC and AC is less than 1%, the timing is stopped, and the standing separation time and addition reaction time of each group are recorded, see Table 2.

[0033]

[0034] Table 2

Embodiment 3

[0036] Take MMP10 groups prepared by conventional methods, each group has a mass of 1000g, add 0, 50, 100, 150, and 200g of water to each group, keep stirring at 30°C for 15min until emulsified, let stand for 30min, remove all MMP in the lower layer, and heat at 90°C , Under the relative pressure of -0.01bar, remove the low-boiling point substances until their total mass fraction is less than 1wt%, and detect the heavy component content of the residue. The low-boiling point substances are detected by gas chromatography, and the substances with boiling points lower than MMP are all classified as light components. The test results are shown in Table 3.

[0037]

[0038] table 3

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Abstract

The invention relates to the field of production of 3-methylthiopropionaldehyde, in particular to a preparation method of 3-methylthiopropionaldehyde. According to the invention, water is introduced in synthesis of 3-methylthiopropionaldehyde, wherein AC in MMP is reserved on the upper layer of a system due to absorption of the water on acrolein, the water has an extraction effect, and MMP and MC in the system are layered, so that MC is also reserved on the upper layer of the system; due to the solvation effect of water, the dissociation degree of the catalyst is enhanced, so that the amount of the catalyst can be reduced to be less than half of the original level and still keeps the same reaction rate; and the catalyst can be recovered / partially recovered, the cost is saved, and in the subsequent refining process of MMP, the polymerization degree of MMP is reduced due to reduction of the content of the catalyst; light components removed in the MMP refining process are condensed and absorbed, and MC and MMP are recovered, so that the production cost is further reduced.

Description

technical field [0001] The invention relates to the field of 3-methylthiopropanal production, in particular to a preparation method of 3-methylthiopropanal. Background technique [0002] 3-methylthiopropionaldehyde (MMP) is used in food flavors, and a larger amount is used in 2-hydroxy-4-methylthiobutyric acid (MHA) and 2-amino-4-methylthiobutyric acid (Met) raw material. MMPs are conventionally prepared from acrolein (AC) and methyl mercaptan (MC). [0003] The method of mass production of AC is the partial oxidation of propylene. In addition to the target component AC, there are secondary by-product components such as acrylic acid, formic acid, acetic acid, acetaldehyde, propane, formaldehyde, carbon dioxide, carbon monoxide, allyl alcohol and allyl alcohol Derivatives, in addition to diluent components nitrogen, water. A large amount of MC is prepared by high-temperature dehydration of hydrogen sulfide and methanol. In addition to the main component of methyl mercaptan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/18C07C323/22C07C319/28
CPCC07C319/18C07C319/28C07C323/22
Inventor 曾涛曹华伟刘帮林赵水乙谢绍林袁代强赵丹丹赵二宝
Owner NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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