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Continuous production method of 3-mercaptopropionic acid alkyl ester and 3, 3'-trithiodipropionic acid dialkyl ester

A technology of dialkyl trithiodipropionate and dialkyl dithiodipropionate, which is applied in the field of fine chemicals, can solve the problem of large output of by-products of crystalline sodium thiosulfate, and achieve value-added design , strong combination flexibility and high degree of automation

Pending Publication Date: 2021-06-22
靳浩田
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the significant shortcoming of this method is: relative to the mercapto ester product, the crystalline sodium thiosulfate by-product yield of generation is bigger
However, the route / method adopted by this patent is not aimed at obtaining a relatively pure trithioester product

Method used

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  • Continuous production method of 3-mercaptopropionic acid alkyl ester and 3, 3'-trithiodipropionic acid dialkyl ester
  • Continuous production method of 3-mercaptopropionic acid alkyl ester and 3, 3'-trithiodipropionic acid dialkyl ester

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Prepare ammonium sulfide alkaline aqueous solution: add the ammonia solution (NH 3 The mass concentration is 5.8wt.%). Control the temperature of the ammonia solution at 3°C, and bubble 6.0 parts by mass of hydrogen sulfide gas into the ammonia solution within 30 minutes to obtain an alkaline aqueous solution of ammonium sulfide (pH≤9.5).

[0028] Add 100.0 parts by mass of dimethyl 3,3'-dithiodipropionate to the above alkaline aqueous solution of ammonium sulfide, keep the temperature of the mixture at 20°C, and pour it into the three-necked flask within 5 hours while stirring Slowly feed hydrogen sulfide with a mass fraction of 1.48. After static separation, an organic solution with about 101.4 parts by mass of the lower layer was obtained.

[0029] The organic solution was distilled under reduced pressure at 60° C. under nitrogen protection under a pressure of 2 mm Hg to obtain about 10.1 parts by mass of methyl 3-mercaptopropionate. After chromatographic analysis...

Embodiment 2

[0032]Preparation of potassium hydrosulfide alkaline aqueous solution: add 100.0 mass parts of potassium hydroxide aqueous solution (mass concentration of KOH is 19.1 wt.%) into a three-necked flask. Control the temperature of potassium hydroxide aqueous solution to be 50 DEG C, and in stirring state, in 30 minutes, in the potassium hydroxide aqueous solution, bubbling is passed into the hydrogen sulfide gas that is 15.5 mass parts, obtains the alkaline aqueous solution of potassium hydrogensulfide (pH≤9.5 ).

[0033] Add 100.0 parts by mass of dimethyl 3,3'-dithiodipropionate to the above alkaline aqueous solution of potassium hydrosulfide, keep the temperature of the mixture at 50°C under stirring, and transfer to the three-necked flask within 5 hours 2.3 mass parts of hydrogen sulfide were slowly introduced into the medium. After static separation, an organic solution of about 102.2 mass parts in the lower layer was obtained.

[0034] The organic solution was distilled un...

Embodiment 3

[0037] like figure 1 As shown, the continuous production of methyl 3-mercaptopropionate and dimethyl 3,3'-trithiodipropionate in this example is a diagram of the device. The device includes a feed unit, a reaction unit, a phase separation unit and a distillation unit The reaction unit includes a packed tower 3 and a reactor 4; the phase separation unit includes a first gravity separator 5, an aqueous phase storage tank 6 and an oil phase storage tank 7, and the reactor 4 in the reaction unit is connected with the first gravity separator 5 , the first gravity separator 5 is connected to the water phase storage tank 6 and the oil phase storage tank 7 respectively; the distillation unit is a vacuum still 8, which is connected to the oil phase storage tank 7.

[0038] The bottom liquid in the vacuum kettle 8 is connected to the top of the packed tower 3 through an infusion pump; the one-way liquid infusion device and the mass metering device 2 of the feeding unit are connected to ...

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Abstract

The invention discloses a continuous production method of 3-mercaptopropionic acid alkyl ester and 3, 3'-trithiodipropionic acid dialkyl ester. The method comprises the following steps: reacting 3, 3'-dithiodipropionic acid dialkyl ester with hydrogen sulfide to generate 3-mercaptopropionic acid alkyl ester and 3, 3'-trithiodipropionic acid dialkyl ester; 3-alkyl mercaptopropionate is easy to separate and purify in a reduced pressure distillation mode; continuously reacting the residual 3, 3'-dithiodipropionic acid dialkyl ester with hydrogen sulfide, and continuously converting the residual 3, 3'-dithiodipropionic acid dialkyl ester into 3, 3'-trithiodipropionic acid dialkyl ester, and therefore, the continuous production process of 3-mercaptopropionate and 3, 3'-dialkyl trithiodipropionate is realized through continuous enhanced mass transfer feeding and reaction units of hydrogen sulfide raw materials and liquid raw materials, continuous phase separation units, distillation separation units and feedback control of process products to the reaction units. The synthesis method does not adopt an organic solvent, does not generate inorganic salt byproducts, has no strict requirements on the purity of raw materials, and is easy to industrialize.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a continuous production method of alkyl 3-mercaptopropionate and dialkyl 3,3'-trithiodipropionate. Background technique [0002] Alkyl 3-mercaptopropionate (hereinafter referred to as: mercapto ester) and dialkyl 3,3'-trithiodipropionate (hereinafter referred to as: trithioester) compounds are important additives or organic synthesis intermediate. For example, a series of compounds such as methyl 3-mercaptopropionate and dimethyl 3,3'-trithiodipropionate can be used as passivators for surface processing of germanium-containing semiconductors. In addition, methyl 3-mercaptopropionate and dimethyl 3,3’-trithiodipropionate can also be used to synthesize isothiazolinones. [0003] Usually, mercapto esters use 3-mercaptopropionic acid and alcohol as raw materials, in acid catalyst or trichlorosilane (Liu Yusheng, green synthesis of methyl mercaptopropionate, Fine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/06C07C319/24C07C319/28C07C323/52
CPCC07C319/06C07C319/24C07C319/28C07C323/52
Inventor 靳浩田
Owner 靳浩田
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