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Catalyst for synthesizing dodecyl alcohol ester and its preparation method and application

A technology of dodecyl alcohol ester and catalyst, which is applied to the catalyst for synthesizing dodecyl alcohol ester and the field of preparation thereof, can solve the problems of serious corrosion equipment, high production cost, long process route and the like, and achieves less corrosion of reaction equipment and better effect. Good, the effect of process simplification

Active Publication Date: 2019-06-07
RUNTAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patents CN1429809, CN1098712A, EP0317977A2 and US4883906 all use NaOH solution as a catalyst to synthesize dodecyl alcohol esters, but there are problems such as low conversion rate, difficult separation, long reaction time and serious corrosion equipment
Patents CN101838197A and CN101863762A have made some improvements. The aldol condensation reaction is catalyzed by NaOH solution, and then alkali-modified metal oxide or hydrotalcite anionic clay is used as the catalytic material. There is still no corrosion-proof equipment, long process route, and two-stage process operationally complex issues
In the patent CN101948386A, sodium alkoxide is used to catalyze the synthesis, and the reaction of too strong alkalinity is difficult to control. Although the conversion rate can meet the requirements, the corrosion of equipment is more serious, resulting in high production costs and poor economic benefits.

Method used

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  • Catalyst for synthesizing dodecyl alcohol ester and its preparation method and application
  • Catalyst for synthesizing dodecyl alcohol ester and its preparation method and application
  • Catalyst for synthesizing dodecyl alcohol ester and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) KF / γ-Al 2 o 3 Catalyst preparation

[0027] a. 15g γ-Al 2 o 3 Put it into a muffle furnace, calcinate at 300°C in an air atmosphere for 3 hours, cool to room temperature and take it out for later use;

[0028] b. the treated γ-Al in step a 2 o 3 Dissolve in 200mL ethanol solution, add 15g KF and 1g polyethylene glycol PEG6000, stir vigorously at 60°C for 3h to obtain a reaction solution;

[0029] c. Put the obtained reaction solution into a rotary evaporator for rotary evaporation, remove the solvent, and obtain a solid powder;

[0030] d. Vacuum dry the obtained solid powder at 120°C for 10h, cool it to room temperature, place it in a muffle furnace, and bake it at 400°C for 4h to obtain the KF / γ-Al 2 o 3 catalyst.

[0031] (2) Catalytic synthesis of dodecyl alcohol ester

[0032] a. Add 50g isobutyraldehyde and 5g KF / γ-Al to the autoclave with stirring, condensing system, temperature control system and nitrogen filling system 2 o 3 Catalyst, turn on th...

Embodiment 2

[0037] (1) KF / γ-Al 2 o 3 Catalyst preparation

[0038] a. Add 5g γ-Al 2 o 3 Put it into a muffle furnace, calcinate at 300°C in an air atmosphere for 3 hours, cool to room temperature and take it out for later use;

[0039] b. the treated γ-Al in step a 2 o 3 Dissolve in 200mL ethanol solution, add 5g KF and 0.1g polyethylene glycol PEG6000, stir vigorously at 40°C for 2h to obtain a reaction solution;

[0040] c. Put the obtained reaction solution into a rotary evaporator for rotary evaporation, remove the solvent, and obtain a solid powder;

[0041] d. Vacuum dry the obtained solid powder at 100°C for 12h, cool it to room temperature, place it in a muffle furnace, and bake it at 500°C for 3h to obtain the KF / γ-Al 2 o 3 catalyst.

[0042] (2) Catalytic synthesis of dodecyl alcohol ester

[0043] a. Add 50g isobutyraldehyde and 4g KF / γ-Al to the autoclave with stirring, condensing system, temperature control system and nitrogen filling system 2 o 3 Catalyst, turn on ...

Embodiment 3

[0048] (1) KF / γ-Al 2 o 3 Catalyst preparation

[0049] a. 20g γ-Al 2 o 3 Put it into a muffle furnace, calcinate at 300°C in an air atmosphere for 3 hours, cool to room temperature and take it out for later use;

[0050] b. the treated γ-Al in step a 2 o 3 Dissolve in 200mL ethanol solution, add 40g KF and 1.5g polyethylene glycol PEG6000, stir vigorously at 80°C for 5h to obtain a reaction solution;

[0051] c. Put the obtained reaction solution into a rotary evaporator for rotary evaporation, remove the solvent, and obtain a solid powder;

[0052] d. Vacuum dry the obtained solid powder at 150°C for 15h, cool it to room temperature, place it in a muffle furnace, and bake it at 500°C for 3h to obtain the KF / γ-Al 2 o 3 catalyst.

[0053] (2) Catalytic synthesis of dodecyl alcohol ester

[0054] a. Add 20g isobutyraldehyde and 4g KF / γ-Al to the autoclave with stirring, condensing system, temperature control system and nitrogen filling system 2 o 3 Catalyst, turn on ...

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Abstract

The invention discloses a catalyst used for synthesis of n-dodecanol ester, and a preparation method and application thereof. According to the invention, gamma-Al2O3 is used as a carrier, ethanol is used as a solvent, and active components are loaded onto gamma-Al2O3 by using an impregnation method under the action of a surfactant so as to prepare the catalyst; and the loading amount of the active components of the catalyst is 30 to 50 wt%, and the pH value of the catalyst is 35 to 38. Isobutyraldehyde is used as a raw material and is subjected to aldol condensation and a Cannizzaro reaction under the catalysis of the catalyst so as to synthesize n-dodecanol ester. The method provided by the invention overcomes the problem of tedious process flow of a traditional inorganic base two-stage reaction and the problems of high toxicity of catalysis by Ba(OH)2 and severe corrosivity of NaOH to equipment. The catalyst is simple to prepare, easy to separate and recover, repeatedly usable, free of corrosion, mild in reaction conditions, high in the conversion rate of reactants and high in product selectivity and yield.

Description

technical field [0001] The invention belongs to the field of organic synthesis catalysts, in particular to a catalyst for synthesizing dodecyl alcohol esters, a preparation method and application thereof. Background technique [0002] Dodecyl alcohol ester, also known as alcohol ester twelve, scientific name 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, is a water-insoluble high-boiling glycol ester , is often used as an ideal film-forming agent for water-based systems. It has good film-forming effects on emulsion polymer systems and lowers the minimum film-forming temperature. It is suitable for occasions where the product is difficult to form a film, such as a high glass transition temperature. Low ambient temperature, etc.; especially suitable for water-based paint systems such as medium emulsion, latex paint, and adhesives synthesized from methacrylate, styrene, and vinyl acetate. [0003] There are two production methods of dodecyl alcohol esters, the first one: dir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/125B01J27/25B01J31/04B01J31/26C07C67/44C07C69/28
CPCY02P20/584
Inventor 王晓达达海容邱挺叶长燊杨金杯王红星黄智贤杨臣李玲陈锦溢
Owner RUNTAI CHEM CO LTD