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CN-122006809-A - Preparation method and synthesis method of catalyst for preparing 1-methyl hexyl acetate by adding n-heptene and acetic acid

CN122006809ACN 122006809 ACN122006809 ACN 122006809ACN-122006809-A

Abstract

The invention relates to a preparation method of a catalyst for preparing 1-methyl hexyl acetate by adding n-heptene and acetic acid, which comprises the following steps of impregnating carrier sulfo strong acid resin into a heteropolyacid solution, stirring for 8-24 hours at 20-50 ℃, wherein the mass ratio of the sulfo strong acid resin to the heteropolyacid solution is 10:1-1:3, filtering after stirring, and drying the filtered solid at 80-140 ℃ to obtain a finished product. The invention also provides a method for synthesizing the 1-methyl hexyl acetate by using the catalyst. The supported solid acid catalyst can be recovered and reused from the reaction slurry by simple liquid-solid separation means such as filtration, centrifugation and the like, and better product selectivity can be obtained.

Inventors

  • SHAO YEWEI
  • ZHANG QIAN
  • CHEN PEIYU

Assignees

  • 江苏恒兴新材料科技股份有限公司

Dates

Publication Date
20260512
Application Date
20251230

Claims (6)

  1. 1. The preparation method of the catalyst for preparing the 1-methyl hexyl acetate by adding n-heptene and acetic acid is characterized by comprising the following steps of: (1) Immersing carrier sulfonic acid group strong acid resin into a heteropoly acid solution, and stirring for 8-24 hours at 20-50 ℃, wherein the mass ratio of the sulfonic acid group strong acid resin to the heteropoly acid solution is 10:1-1:3; (2) And stirring, filtering, and drying the solid obtained after filtering at 80-140 ℃ to obtain a finished product.
  2. 2. The method for producing a catalyst for the addition of n-heptene to acetic acid to 1-methyl hexyl acetate according to claim 1, wherein the sulfonic acid group strongly acidic resin comprises one of a polystyrene-divinylbenzene sulfonic acid resin and an acrylic sulfonic acid resin.
  3. 3. The method for preparing a catalyst for preparing 1-methyl hexyl acetate by adding n-heptene to acetic acid according to claim 1, wherein the polystyrene-divinylbenzene sulfonic acid resin comprises one of Amberlyst-36 resin, amberlyst-45 resin and D005-II resin.
  4. 4. The method for producing a catalyst for the addition of n-heptene to acetic acid to produce hexyl 1-methylacetate according to claim 1, wherein the heteropolyacid in the heteropolyacid solution comprises one or more of phosphotungstic acid (HPW), silicotungstic acid (HSiW), phosphomolybdic acid (HPMo).
  5. 5. The method for preparing a catalyst for preparing 1-methyl hexyl acetate by adding n-heptene to acetic acid according to claim 1, wherein the concentration of the heteropolyacid solution is 10-40 wt%.
  6. 6. The method for synthesizing 1-methyl hexyl acetate by using the catalyst according to any one of claims 1-5, wherein the reaction temperature is 60-180 ℃, the reaction time is 4-20 h, the molar ratio of n-heptene to acetic acid is 1:2-1:20, the reaction pressure is 0.1-5 MPa, and the mass of n-heptene of the catalyst is 5-40 wt%.

Description

Preparation method and synthesis method of catalyst for preparing 1-methyl hexyl acetate by adding n-heptene and acetic acid Technical Field The invention belongs to the field of preparation of 1-methyl hexyl acetate, and particularly relates to a preparation method and a synthesis method of a catalyst for preparing 1-methyl hexyl acetate by adding n-heptene and acetic acid. Background The industrial production of simple esters mostly adopts traditional alkyd esterification reactions, such as ethyl acetate, butyl acetate and the like. The core disadvantage of this process stems from the nature of its reversible reaction, which results in an inherent limitation of its reaction efficiency. As water is continuously produced during the reaction, the chemical equilibrium must be broken by continuously removing the moisture, and the use of a water separator or dehydrating agent during the production directly increases the complexity and energy consumption of the process. The reaction is usually carried out under the conditions of strong acid (concentrated sulfuric acid is adopted in industrial application) catalysis and heating reflux, which not only brings equipment corrosion and safety risks, but also obviously increases the production cost due to high energy consumption and long reaction time. More importantly, strong acidic and high temperature conditions are extremely prone to initiate a series of side reactions such as dehydration of alcohols, decomposition of carboxylic acids, etc., resulting in poor product selectivity, reduced yields, and rendering substrates containing acid sensitive or readily dehydrated functional groups unsuitable. The complicated purification process after the reaction, including neutralization, washing, distillation and the like, has more steps, large product loss and serious environmental protection pressure caused by a large amount of acid wastewater which is difficult to treat. The mode of formation of water as a by-product of this reaction also means that the atom utilization rate is low from the viewpoint of atom economy. Ester production by the enoate addition method presents significant advantages over conventional alkyd esterification reactions in multiple dimensions. The process is usually carried out under milder conditions, and solid acid is adopted to replace liquid strong acid as a catalyst, so that not only is the energy consumption greatly reduced, but also the corrosion to equipment and the pollution to the environment are reduced, and the byproduct is few, thereby conforming to the development direction of green chemistry. The method follows the principle of atom economy, almost all reactant atoms are converted into target products, so that the utilization efficiency of raw materials is fundamentally improved, and the separation and purification burden caused by the generation of water byproducts in the traditional method is avoided. Meanwhile, from the economical point of view, the sources of olefin and carboxylic acid raw materials are wide, and the simplified post-treatment and lower equipment requirements make the technical path more competitive in comprehensive cost. Thus, the enoate addition method represents a new way of synthesizing esters with higher efficiency, cleanliness and controllability. However, the current research on the addition reaction of olefine acid is mainly focused on short-chain olefins such as ethylene and propylene, and a method for synthesizing corresponding carboxylic esters by adding dilute ethylene, dilute propylene and acetic acid is reported in patent CN109456179A, CN 102757341A. Compared with short-chain olefin, the reaction of heptene and other long-chain olefin with acetic acid has the problems of low reaction activity, complex product, low yield and the like, and the relevant reports on a catalytic reaction system and a reaction process are fresh. Disclosure of Invention The invention aims to overcome the defects in the prior art and provides a preparation method of a catalyst for preparing 1-methyl hexyl acetate by adding n-heptene and acetic acid. The invention also provides a method for synthesizing the 1-methyl hexyl acetate by using the catalyst. A preparation method of a catalyst for preparing 1-methyl hexyl acetate by adding n-heptene and acetic acid comprises the following steps: (1) Immersing carrier sulfonic acid group strong acid resin into a heteropoly acid solution, and stirring for 8-24 hours at 20-50 ℃, wherein the mass ratio of the sulfonic acid group strong acid resin to the heteropoly acid solution is 10:1-1:3; (2) And stirring, filtering, and drying the solid obtained after filtering at 80-140 ℃ to obtain a finished product. Further, the sulfonic acid group strong acid resin comprises one of polystyrene-divinylbenzene sulfonic acid resin and acrylic sulfonic acid resin. Further, the polystyrene-divinylbenzene sulfonic acid resin comprises one of Amberlyst-36 resin, amberlyst-45 resin and D005-II resin. Furth