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Synthetic process of vinyl isooctoate
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A technology for the synthesis of vinyl isooctanoate, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, organic chemistry, etc., can solve the problems of environmental pollution, difficulty in industrial production, and low yield, and achieve rich sources of raw materials and reduce The effect of simple production cost and synthetic route
Inactive Publication Date: 2018-03-09
PANJIN HONGDING CHEM CO LTD
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Problems solved by technology
Due to the steric hindrance of branched chain fatty acids, it is difficult to complete the reaction, so it is necessary to develop a synthetic process for vinyl isooctanoate suitable for industrial production
The synthesis of vinyl isooctanoate is generally synthesized in organic solvents, which does not meet the technical requirements of green chemistry and easily causes environmental pollution
And generally metal oxides, sulfuric acid, etc. are selected as catalysts. In the production of reagents, there are defects such as expensive reagents, high corrosion, large safety hazards, and low yields, which are not conducive to industrial production.
[0004] It can be seen that the existing synthetic routes are not easy to industrialized production
Method used
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Embodiment 1
[0019] (1) Preparation of solid superacid catalyst.
[0020] Take 100 g TiCl 3 Dissolved in water, then hydrolyzed with dilute ammonia water to become alkaline (PH=9-11), after standing for 36 hours, filtered and washed, a large amount of white precipitate was obtained. The solid was dried at 150 °C and ground into powder. Then it was added to the concentrated sulfuric acid solution of 0.5 M lanthanumsulfate, reacted for 10 h, filtered and dried, and roasted in a muffle furnace to obtain the superacid catalyst SO 4 2- / TiO 2 / Ce.
[0021] (2) Synthesis of vinyl isooctanoate.
[0022] Add vinyl alcohol (150 g) and isooctanoic acid (360 g) into the reaction vessel, then add the catalyst (30 g) prepared in the above step into the reaction vessel, react at a temperature of 230 °C for 10 h, stop the heating after the reaction is completed That is, the crude product is obtained.
[0024] The reaction solution is filtered, and the c...
Embodiment 2
[0026] (1) Preparation of solid superacid catalyst.
[0027] Take 200 g TiCl 3 Dissolved in water, then hydrolyzed with dilute ammonia water to become alkaline (PH=9-11), after standing for 36 hours, filtered and washed, a large amount of white precipitate was obtained. The solid was dried at 180 °C and ground into powder. Then it was added to the concentrated sulfuric acid solution of 0.5 M lanthanumsulfate, reacted for 14 h, filtered and dried, and then roasted in a muffle furnace to obtain the superacid catalyst SO 4 2- / TiO 2 / Ce.
[0028] (2) Synthesis of vinyl isooctanoate.
[0029] Add vinyl alcohol (150 g) and isooctanoic acid (540 g) into the reaction vessel, then add the catalyst (30 g) prepared in the above step into the reaction vessel, react at a temperature of 190 °C for 18 h, stop the heating after the reaction is completed That is, the crude product is obtained.
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Abstract
The invention relates to a method for synthesizing esters, in particular to a method for synthesizing vinyl isooctoate. The preparation method comprises the following steps: preparing a solidsuperacid catalyst; Hydrolyzing a TiCl3 aqueous solution with dilute ammonia water to obtain alkaline solution (pH ranges from 9 to11), standing the solution for 36h, and carrying out filtering and washing toobtain a large amount of white precipitate; drying a solid at a temperature of 150-180 DEG C, and grinding the solid into a powder; then adding the powder into a concentrated sulfuric acid solution of 0.5M lanthanumsulfate to react for 8-14h, carrying out filtering and drying, and carrying out roasting in a muffle furnace to obtain a superacid catalyst SO42- / TiO2 / Ce; adding vinyl alcohol and isooctanoic acid into a reaction vessel, then adding the catalyst prepared in the previous step into the reaction vessel to react for 10-18h at a reaction temperature of 180-230 DEG C, stopping heating after the reaction to obtain a crude product; carrying out post-treatment of the product. The method is simple in synthetic route, mild in condition and easy to control.
Description
technical field [0001] The invention relates to a method for synthesizing esters, in particular to a method for synthesizing vinyl isooctanoate. Background technique [0002] Vinyl isooctanoate has excellent low temperature properties, oil resistance, antistatic properties, etc., and has certain lubricity and other characteristics. Moreover, vinyl isooctanoate is similar to resin in polarity and has good compatibility, so it is a solvent-based plasticizer with good performance. [0003] At present, vinyl isooctanoate is widely used in the preparation of polyvinyl butyral (PVB) safety film, synthetic rubber, polyvinyl chloride (PVC), sealing materials, etc., and has great application value. Due to the steric hindrance of branched chain fatty acids, it is difficult to carry out the reaction completely, so it is necessary to develop a synthesis process suitable for industrialized production of vinyl isooctanoate. The synthesis of vinyl isooctanoate is generally synthesized in...
Claims
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