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Method for treating acetic acid in acidic DMF and co-producing magnesium acetate and device thereof

A technology of magnesium acetate and crude magnesium acetate, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate, etc., can solve the difficulty of secondary utilization of magnesium hydroxide waste, poor purity and stability of DMF, Affect the quality of sucralose and other issues, to achieve the effect of high industrial application value, improved purity, and low cost

Active Publication Date: 2021-11-26
ANHUI JINGHE IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to solve the problem of poor purity and stability of reclaiming DMF from the DMF mixed solution of the sucralose industry in the prior art, affecting the quality of sucralose and the secondary utilization of magnesium hydroxide waste produced by the ethyl maltol industry Difficult problem, propose a kind of method and device for processing acetic acid in acidic DMF and co-produce magnesium acetate, so that overcome above-mentioned problem

Method used

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  • Method for treating acetic acid in acidic DMF and co-producing magnesium acetate and device thereof

Examples

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Effect test

Embodiment 1

[0028] The components of acidic DMF are shown in Table 1, and the components of magnesium hydroxide waste are shown in Table 2.

[0029] Table 1 Acidic DMF composition:

[0030] components DMF water Acetic acid Mass content / % 65 0 35

[0031] Table 2 Magnesium hydroxide waste composition:

[0032] components Mg(OH) 2

5-Ethyl-2(5H)-furanone Furfural water Mass content / % 89.98 0.01 0.01 10

[0033] A method for processing acetic acid in acidic DMF and co-producing magnesium acetate, the specific implementation steps are as follows:

[0034] Step (1): Add 1000kg of acidic DMF (see Table 1) into the neutralization kettle, the stirring rate is 150r / min, then add 188.0kg of magnesium hydroxide waste (see Table 2), after the addition is completed, the temperature is raised to 100°C, and the temperature is kept 15min; vacuumize after heat preservation, vacuum degree -0.05Mpa, temperature 80°C, remove one-third of DMF an...

Embodiment 2

[0043] The components of acidic DMF are shown in Table 5, and the components of magnesium hydroxide waste are shown in Table 6.

[0044] Table 5 Acidic DMF components

[0045] components DMF water Acetic acid Mass content / % 85 3 15

[0046] Table 6 Composition of magnesium hydroxide waste

[0047] components Mg(OH) 2

5-Ethyl-2(5H)-furanone Furfural water Mass content / % 69.85 0.1 0.05 30

[0048] A method for processing acetic acid in acidic DMF and co-producing magnesium acetate, the specific implementation steps are as follows:

[0049] Step (1): Add 500kg of acidic DMF to the neutralization kettle, the stirring rate is 300r / min, then add 51.9kg of magnesium hydroxide waste, after the addition is completed, the temperature is raised to 50°C, and the temperature is kept for 5min; -0.05Mpa, temperature 40°C, remove one-third of DMF and water, then transfer the material to rake dryer 1 to continue thickening, dryi...

Embodiment 3

[0056] The components of acidic DMF are shown in Table 9, and the components of magnesium hydroxide waste are shown in Table 10.

[0057] Table 9 Acidic DMF composition

[0058] components DMF water Acetic acid Mass content / % 79 1 20

[0059] Table 10 Composition of magnesium hydroxide waste

[0060] components Mg(OH) 2

5-Ethyl-2(5H)-furanone Furfural water Mass content / % 75 0.05 0.02 24.93

[0061] A method for processing acetic acid in acidic DMF and co-producing magnesium acetate, the specific implementation steps are as follows:

[0062] Step (1): Add 700kg of acidic DMF to the neutralization kettle, the stirring rate is 200r / min, then add 90.2kg of magnesium hydroxide waste, after the addition is completed, the temperature is raised to 80°C, and the temperature is kept for 10 minutes; -0.07Mpa, temperature 70°C, remove one-third of DMF and water, then transfer the material to rake dryer 1 to continue thicke...

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Abstract

The invention relates to a method for treating acetic acid and co-producing magnesium acetate in acidic DMF and a device thereof, which are characterized by comprising the following steps: (1) adding magnesium hydroxide waste into an acetic acid-containing DMF solvent, controlling the addition amount of the magnesium hydroxide waste to be 0.8-1 time of the amount of acetic acid substance, and reacting for 5-15 minutes at the speed of 100-300r / min and the temperature of 50-100 DEG C; (2) enabling the solution to enter a neutralization concentration kettle for vacuum concentration, controlling the temperature to be 40-80 DEG C, controlling the vacuum degree to be -0.1 to -0.05 Mpa, transferring the solution into a rake dryer for vacuum concentration drying, wherein the temperature is 80-120 DEG C, and controlling the vacuum degree to be -0.1 to -0.05 Mpa; combining condensate and sending the condensate to refined DMF; (3) adding the concentrated and dried magnesium acetate crude product into a decolorizing kettle containing reuse water for dissolving, adding a decolorizing agent accounting for 1-3% of the mass of the magnesium acetate crude product for heating and decolorizing, and separating by adopting a plate-and-frame filter press; and (4) directly carrying out vacuum concentration drying on the filtrate in a rake dryer, controlling the temperature to be 80-120 DEG C and the vacuum degree to be -0.1 to -0.05 Mpa, and recycling condensate, so as to obtain a solid which is a magnesium acetate refined product. The method has the advantages that by adding the waste magnesium hydroxide generated by the ethyl maltol process, acetic acid in the acidic DMF is converted into magnesium acetate, comprehensive recycling of the two industrial wastes is realized, and the industrial value is high.

Description

technical field [0001] The invention relates to the technical field of chemical product recycling industry, in particular to a method and device for treating acetic acid in acidic DMF and co-producing magnesium acetate. Background technique [0002] Acetic acid, commonly known as glacial acetic acid, is a colorless, irritating organic monobasic acid, and its aqueous solution is weakly acidic and corrosive. High concentration of acetic acid can slowly corrode stainless steel materials and form nickel acetate, an organic salt, which is mainly used as a chemical reagent, and can also be used for nickel plating, metal coloring, catalyst, fabric mordant, etc. Because of its better catalytic activity, in the N,N-dimethylformamide (commonly known as DMF) system, it may cause DMF to form impurities such as tetramethylurea, which is an important factor affecting the quality of DMF recovery in the DMF recovery process. One of factor; Therefore, reduce and reclaim acetic acid, avoid t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/10C07C51/41C07C51/44C07C51/47C07C51/42C07C231/24C07C233/03
CPCC07C51/412C07C51/44C07C51/47C07C51/42C07C231/24C07C53/10C07C233/03Y02P20/584
Inventor 陈永乐郭思雨刘建
Owner ANHUI JINGHE IND
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