CN111978165B - Method for improving acetone recovery rate in condensation process of producing pseudo ionone - Google Patents
Method for improving acetone recovery rate in condensation process of producing pseudo ionone Download PDFInfo
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- CN111978165B CN111978165B CN202010781210.4A CN202010781210A CN111978165B CN 111978165 B CN111978165 B CN 111978165B CN 202010781210 A CN202010781210 A CN 202010781210A CN 111978165 B CN111978165 B CN 111978165B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/51—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition
- C07C45/55—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition of oligo- or polymeric oxo-compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The invention relates to a method for improving the recovery rate of acetone in the condensation process for producing pseudo ionone, which comprises the following steps: standing and layering a product mixed solution prepared from pseudo ionone by an Aldol condensation reaction process, wherein the obtained organic phase is subjected to organic phase atmospheric distillation and organic phase vacuum distillation in turn to obtain acetone in the organic phase; and adding an alkaline solution into the obtained water phase, and sequentially carrying out water phase atmospheric distillation and water phase reduced pressure distillation to obtain the acetone in the water phase. Compared with the prior art, the invention adds alkaline solution into the layered water phase product of pseudo ionone prepared by the Aldol condensation reaction process and heats the product to decompose the diacetone alcohol in the water phase into acetone and water, thereby improving the recovery rate of the acetone on one hand by the subsequent modes of normal pressure fractionation and reduced pressure fractionation and avoiding the problem of environmental pollution caused by direct discharge of the diacetone alcohol along with the water phase on the other hand.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and relates to a method for improving acetone recovery rate in a condensation process for producing pseudo ionone.
Background
The method for recovering acetone in the pseudo ionone condensation process mainly comprises the following steps: firstly, standing and layering reaction products, taking an upper organic phase, heating and evaporating at normal pressure, taking a fraction with a boiling range of 55-60 ℃, reducing the pressure to about 50% of vacuum degree, taking a fraction with a boiling range of 45-50 ℃, and obtaining an acetone recovery rate of about 65% (deducting the acetone consumed by the reaction). Wherein, the water phase at the lower layer is usually directly discharged after neutralization during standing and layering, so that the waste of residual acetone in the water phase is caused, the recovery rate of the acetone is reduced, and the reduction of the production cost is not facilitated; in addition, the water phase also contains a large amount of organic matters, mainly including diacetone alcohol generated by the reaction of acetone and water in an alkaline environment, and the substances have high water solubility and are easy to cause serious environmental pollution when being directly discharged.
Disclosure of Invention
The invention aims to provide a method for improving the recovery rate of acetone in the condensation process of producing pseudo-ionone, which is used for solving the technical problem of lower recovery rate of acetone in the process of preparing pseudo-ionone by an Aldol condensation reaction process.
The purpose of the invention can be realized by the following technical scheme:
a method for increasing acetone recovery in a condensation process for producing pseudoionone, the method comprising: standing and layering a product mixed solution prepared from pseudo ionone by an Aldol condensation reaction process, wherein the obtained organic phase is subjected to organic phase atmospheric distillation and organic phase vacuum distillation in turn to obtain acetone in the organic phase; and adding an alkaline solution into the obtained water phase, and sequentially distilling the water phase under normal pressure and the water phase under reduced pressure to obtain the acetone in the water phase.
Further, the alkaline solution is NaOH solution.
Further, the NaOH solution is added into the water phase in a dropwise manner.
Further, the concentration of the NaOH solution is 30-40wt%.
Further, the concentration of the NaOH solution is 30wt%.
Furthermore, the addition amount of the NaOH solution is 2-5% of the volume of the water phase.
Further, the NaOH solution was added in an amount of 5% by volume of the aqueous phase.
Further, in the aqueous atmospheric distillation, the boiling range of the fraction is 55-60 ℃.
Furthermore, in the water phase reduced pressure distillation, the vacuum degree is 40-60%, and the boiling range of the extracted fraction is 45-50 ℃.
Furthermore, the acetone in the water phase is dried by anhydrous magnesium sulfate and can be directly used for preparing the pseudo ionone by an Aldol condensation reaction process.
Compared with the prior art, the method has the advantages that the alkaline solution is added into the layered water phase product of the pseudo ionone prepared by the Aldol condensation reaction process and is heated, so that the diacetone alcohol in the water phase is decomposed into acetone and water, on one hand, the recovery rate of the acetone is improved by the subsequent normal-pressure fractionation and reduced-pressure fractionation, on the other hand, the problem of environmental pollution caused by the direct discharge of the diacetone alcohol with the water phase is avoided, and the method has the advantages of simple operation method, mild conditions, high raw material utilization rate, environmental protection and the like.
Detailed Description
The present invention will be described in detail with reference to specific examples.
A method for increasing acetone recovery in a condensation process for producing pseudoionone, comprising: standing and layering a product mixed solution prepared from pseudo ionone by an Aldol condensation reaction process, wherein the obtained organic phase is heated and evaporated under normal pressure, a fraction with a boiling range of 55-60 ℃ is taken, then the pressure is reduced to about 50% of vacuum degree, and a fraction with a boiling range of 45-50 ℃ is taken to obtain acetone in the organic phase; adding 30-40wt% of NaOH solution dropwise into the obtained water phase, wherein the addition amount of NaOH solution is 2-5% of the volume of the water phase, heating and evaporating under normal pressure, collecting fraction with boiling range of 55-60 deg.C, reducing pressure to vacuum degree of 40-60%, collecting fraction with boiling range of 45-50 deg.C, and collecting acetone in the water phase.
The acetone in the organic phase and the acetone in the water phase are dried by anhydrous magnesium sulfate and can be directly used for preparing the pseudo ionone by the Aldol condensation reaction process.
The following examples are given in detail to illustrate the embodiments and specific procedures of the present invention, but the scope of the present invention is not limited to the following examples.
Comparative example:
taking the mixed solution of the product obtained in the same example 1 to carry out standing and layering, heating and evaporating the obtained organic phase under normal pressure, taking the fraction with the boiling range of 55-60 ℃, then decompressing to about 50 percent of vacuum degree, taking the fraction with the boiling range of 45-50 ℃ to obtain acetone in the organic phase; the obtained water phase is directly discharged after being neutralized. The total acetone recovery was 65%.
Example 1:
taking a product mixed solution of pseudo ionone prepared by an Aldol condensation reaction process in a certain factory, standing and layering, heating and evaporating the obtained organic phase under normal pressure, taking a fraction with a boiling range of 55-60 ℃, reducing the pressure to about 50% of vacuum degree, taking a fraction with a boiling range of 45-50 ℃, and obtaining acetone in the organic phase; and (3) firstly, dropwise adding 40wt% of NaOH solution into the obtained water phase, mixing, wherein the adding amount of the NaOH solution is 2% of the volume of the water phase, then heating and evaporating under normal pressure, taking fractions with the boiling range of 55-60 ℃, reducing the pressure to 50% of vacuum degree, taking fractions with the boiling range of 45-50 ℃, and obtaining the acetone in the water phase.
The acetone in the organic phase and the acetone in the water phase are dried by anhydrous magnesium sulfate and can be directly used for preparing the pseudo ionone by the Aldol condensation reaction process. Compared with the comparative example, the recovery rate of the total acetone is improved by 20 percent and reaches 85 percent by recovering the acetone in the water phase.
Example 2:
taking the mixed solution of the products in the same example 1 to stand and layer, heating and evaporating the obtained organic phase at normal pressure, taking the fraction with the boiling range of 55-60 ℃, then decompressing to about 50 percent of vacuum degree, taking the fraction with the boiling range of 45-50 ℃ to obtain acetone in the organic phase; and (3) dropwise adding 30wt% of NaOH solution into the obtained water phase, mixing, wherein the addition amount of the NaOH solution is 5% of the volume of the water phase, heating and evaporating under normal pressure, taking fractions with the boiling range of 55-60 ℃, reducing the pressure to 50% of vacuum degree, and taking fractions with the boiling range of 45-50 ℃ to obtain acetone in the water phase.
The acetone in the organic phase and the acetone in the water phase are dried by anhydrous magnesium sulfate and can be directly used for preparing the pseudo ionone by the Aldol condensation reaction process. Compared with the comparative example, the recovery rate of the total acetone is improved by 25 percent and reaches 90 percent by recovering the acetone in the water phase.
The embodiments described above are intended to facilitate a person of ordinary skill in the art in understanding and using the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. A method for increasing acetone recovery in a condensation process for producing pseudoionone, the method comprising: standing and layering a product mixed solution prepared from pseudo ionone through an Aldol condensation reaction process, and sequentially carrying out organic phase atmospheric distillation and organic phase vacuum distillation on an obtained organic phase to obtain acetone in the organic phase; the method is characterized in that 30-40wt% of NaOH solution is added into the obtained water phase, the water phase is subjected to normal pressure distillation in sequence, fractions with the boiling range of 55-60 ℃ are taken, the water phase is subjected to reduced pressure distillation under the vacuum degree of 40-60%, and fractions with the boiling range of 45-50 ℃ are taken, so that acetone in the water phase is obtained.
2. The method of claim 1, wherein the NaOH solution is added dropwise to the aqueous phase.
3. The method of claim 1, wherein the concentration of NaOH solution is 30wt% for improving acetone recovery in the condensation process for the production of pseudoionone.
4. The method of claim 3, wherein the NaOH solution is added in an amount of 2-5% by volume of the aqueous phase.
5. The method of claim 4, wherein the NaOH solution is added in an amount of 5% by volume of the aqueous phase.
6. The method for improving the recovery rate of acetone in the condensation process for producing pseudoionone according to claim 1, wherein the acetone in the aqueous phase is dried by anhydrous magnesium sulfate and then directly used in an Aldol condensation reaction process to prepare pseudoionone.
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