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Continuous production method of propyl acetate

A technology of n-propyl acetate and n-propanol, which is applied in the field of continuous production of n-propyl acetate, can solve the problems of a large amount of organic solvents, high energy consumption, and a large amount of total waste liquid, and achieve simple preparation process and product selectivity Good, simple synthesis method

Inactive Publication Date: 2011-04-06
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (2) n-propyl acetate has a higher yield in the traditional process, at the cost of a large amount of head fraction returning to the reactor of the esterification tower, because the head fraction contains a high proportion of n-propyl acetate, thereby reducing the The conversion rate of the reaction;
[0008] (3) Since the whole process is operated intermittently, waste acid and neutralized waste liquid are discharged in each operation, and the total waste liquid is relatively large, which increases the operating cost
In 2002, foreign countries reported the method of utilizing ionic liquid to catalyze esterification. The ionic liquid used in this method is complex to synthesize, and needs a large amount of organic solvent, and the conversion rate of esterification is not high. +BF4-catalyzed preparation of esters
However, this method also has the disadvantages of large amount of ionic liquid, cumbersome catalyst post-treatment steps, high energy consumption, etc., and cannot be industrialized.

Method used

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  • Continuous production method of propyl acetate
  • Continuous production method of propyl acetate
  • Continuous production method of propyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Attached figure 1 The process flow is carried out, in the figure 1-glacial acetic acid, 2-n-propanol, 3-catalyst, 4-esterification tank, 5-esterification tower, 6-layer device, 7-distributor,

[0026] Glacial acetic acid 1 100g, n-propanol 2 100g and FeCl 3 3.33 g with 1-methylimidazolium fluoroborate [Hmim] + BF4 - Add 16.67g of the prepared ionic liquid catalyst 3 into the esterification kettle 4 for heating and esterification reaction. The reaction temperature is 80°C. After the reaction starts to distill, continue to inject glacial acetic acid into the esterification kettle at a speed of 20g / h 100g of mixed raw materials with 100g of n-propanol is pumped into the esterification tank, the reaction product is separated in the esterification tower 5, and the unreacted raw materials are returned from the bottom of the esterification tower to continue the reaction in the esterification tank. The temperature at the top of the tower should be controlled at 80±10°C, the...

Embodiment 2

[0030] With the technical process of embodiment 1, glacial acetic acid 100g, n-propanol 110g, SnCl4 9.69 g and 1-ethylimidazolium fluoroborate [Heim] + BF4 - The ionic liquid catalyst that 32.31g makes is added in the esterification kettle and carries out heating esterification reaction, and reaction temperature is 85 ℃, after the reaction starts back distillation, then continuously inject glacial acetic acid 100g with the speed of 20g / h in the esterification kettle The mixed raw materials of n-propanol 110g ratio are pumped into the esterification tank, the reaction product is separated in the esterification tower, and the unreacted raw materials are returned from the bottom of the esterification tower to the esterification tank to continue the reaction, and the esterification tower top The temperature should be controlled at 80±10°C, the reflux ratio at the top of the esterification tower is 1:1.5, the acetic acid content of the distilled product at the top of the tower is ...

Embodiment 3

[0035] With the technological process of embodiment 1, glacial acetic acid 100g, n-propanol 110g, AlCl 3 16.33 g and 1-butylimidazolium fluoroborate [Hbim] + BF4 - The ionic liquid catalyst that 46.67g makes is added in the esterification kettle and carries out heating esterification reaction, and reaction temperature is 90 ℃, after the reaction starts back distillation, inject 100g of glacial acetic acid and 100g of glacial acetic acid and The mixed raw materials of n-propanol 110g ratio are pumped into the esterification tank, the reaction product is separated in the esterification tower, and the unreacted raw materials are returned from the bottom of the esterification tower to the esterification tank to continue the reaction, and the esterification tower top The temperature should be controlled at 80±10°C, the reflux ratio at the top of the esterification tower is 1:1.5, the acetic acid content of the distilled product at the top of the tower is less than 0.1%, and the n...

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Abstract

The invention relates to a continuous production method of propyl acetate, and is characterized by comprising the following steps: adding ionic liquid dissolving inorganic compound of the Lewis acid into the glacial acetic acid and the normal propyl alcohol as the catalyst; heating the components in an esterification kettle for esterification reaction; adding the mixed raw material of the glacial acetic acid and the normal propyl alcohol with the same proportion into the esterification kettle continuously after the reaction begins to reflux; separating the propyl acetate generated in the reaction in an esterification tower, and sending the unreacted raw materials back to the esterification kettle from the bottom of the kettle to continue the reaction; steaming the water and part of the normal propyl alcohol from the tower top; after the cooling, refluxing one part of the steam to the tower top, and sending the other part of the steam to a stratifying device at the tower top; refluxing part of the aqueous phase at the lower layer to the esterification tower through a reflux ratio distributor, and recovering the other part of the aqueous phase; and sending the ester phase at the upper layer to the production purification stage for the further separation to obtain the propyl acetate product. The method of the invention has simple process, high esterification conversion rate, good product selectivity, recyclable catalyst, no device corrosion, environmental protection, simple synthesis method of the selected ionic liquid catalyst, and better solubility of the acid inorganic compound.

Description

technical field [0001] The present invention relates to a kind of processing method of n-propyl acetate, more specifically, it is a kind of processing method that utilizes ionic liquid to be the continuous production of n-propyl acetate as catalyst. Background technique [0002] N-propyl acetate is a colorless, transparent liquid with aromatic odor, flammable and volatile, miscible with various organic solvents such as alcohol, ketone, ether, etc., and has excellent solubility for various synthetic resins. It is an ethyl fiber An effective solvent for many synthetic resins such as cellulose, nitrocellulose, polystyrene, and methacrylate resins. It is often used in organic synthesis process and as a solvent for coatings, printing inks, etc. It is also a commonly used dehydrating agent in industry. [0003] N-propyl acetate is usually prepared by reacting glacial acetic acid and n-propanol under the catalysis of concentrated sulfuric acid. The specific steps are to add glaci...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/08B01J31/30B01J31/26B01J31/02
CPCY02P20/584
Inventor 姚志龙李翠清赵如松翟彦青任绍梅朱超
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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