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Method for preparing and purifying propyl acetate

A technology of propyl acetate and n-propyl acetate, which is applied in the field of preparation and purification of propyl acetate, can solve the problems of separation and purification difficulty of esterification liquid, and achieve the effect of continuous separation and purification and continuous esterification reaction

Inactive Publication Date: 2006-02-15
SHANGHAI WUJING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the existence of a multi-component azeotropic system between esters, alcohols and water, it brings certain difficulties to the separation and purification of esterification liquid.

Method used

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  • Method for preparing and purifying propyl acetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Acetic acid, n-propanol and concentrated sulfuric acid are preset in the esterification kettle, and the temperature is raised for reaction. To stabilize the temperature at the top of the esterification tower at 82°C, control the reflux ratio to 4-5. Then, acetic acid, n-propanol and sulfuric acid pass through the pre-reactor continuously according to the ratio, and then enter the esterification tank for esterification. Add about 100ml of about 95% crude ester obtained from the top of the esterification tower and distilled water into a 250ml stoppered Erlenmeyer flask, put it in a constant temperature water bath shaker at 25°C, shake for 0.5-1 hour, and analyze the ester phase after standing still for 0.5 hours and water phase. Add a certain amount of saturated magnesium chloride salt solution to the ester phase, put it into a constant temperature water bath shaker at 25°C, shake for 0.5 to 1 hour, stand still for 0.5 hour, and analyze the ester phase and the water phas...

Embodiment 2

[0019] Acetic acid, n-propanol and concentrated sulfuric acid are preset in the esterification kettle, and the temperature is raised for reaction. To stabilize the temperature at the top of the esterification tower at 82°C, control the reflux ratio to 4-5. Then, acetic acid, n-propanol and sulfuric acid pass through the pre-reactor continuously according to the ratio, and then enter the esterification tank for esterification. Obtain about 95% crude ester from the top of the esterification tower as the dispersed phase, use 65% potassium acetate solution extractant as the continuous phase, the solvent ratio is 1:1, the diameter of entering the tower is 50 mm, the height of the tower is 1200 mm, and the number of rotating discs It is a 30-piece liquid-liquid rotary disk extraction tower, the crude ester flow rate is controlled at 40ml / min, and the rotation speed is controlled at 300, 500, and 700r / min respectively. After extraction, the ester phase is rectified by a rectificatio...

Embodiment 3

[0022] Acetic acid, n-propanol and concentrated sulfuric acid are preset in the esterification kettle, and the temperature is raised for reaction. To stabilize the temperature at the top of the esterification tower at 82°C, control the reflux ratio to 4-5. Then, acetic acid, n-propanol and sulfuric acid pass through the pre-reactor continuously according to the ratio, and then enter the esterification tank for esterification. Obtain about 95% crude ester from the top of the esterification tower as the dispersed phase, use 65% potassium acetate solution extractant as the continuous phase, the solvent ratio is 2:1, the diameter of entering the tower is 50 mm, the height of the tower is 1200 mm, and the number of rotating discs It is a 30-piece liquid-liquid rotary disk extraction tower, the crude ester flow is controlled at 40ml / min, and the rotation speeds are 300, 500, and 700r / min respectively. After extraction, the ester phase is rectified by a rectification tower to obtain...

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Abstract

The invention relates to a method for preparing and purifying propyl acetate, which comprises charging quantitative acetic acid, n-propanol (or isopropanol) and acidic homogeneous catalyst continuously into a pre-reactor, loading into esterification tower, obtaining crude ester on the top of the tower, loading the crude ester into a liquid-liquid rotating disc extraction tower, extracting and purifying with aqueous solution extracting agent of salts, recycling the extract phase and loading into rectifying tower for continuous distillation, thus obtaining n-propyl acetate or isopropyl acetate whose content is above 99.5% on the bottom of the tower.

Description

1. Technical field: [0001] The invention relates to a method for preparing propyl acetate, in particular discloses a method for preparing and purifying propyl acetate. 2. Background technology: [0002] Propyl acetate is a fine chemical raw material. Among them, n-propyl acetate is used as a mild and quick-drying agent for elastic printing inks and gravure printing inks, especially for polyolefin and polyamide film printing. It can also be used as a solvent for nitrocellulose, chlorinated rubber and thermoreactive phenolic plastics. It has a slightly fruity aroma and is therefore also used in spices. [0003] At present, the production of propyl acetate in China adopts the traditional esterification method: that is, the esterification synthesis method of acetic acid and n-propanol under the condition of concentrated sulfuric acid as a catalyst. The production process of batch method is usually adopted: acetic acid and n-propanol are catalyzed by concentrated sulfuric acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/08C07C67/58
Inventor 孙粤昌曹智龙李彩云陈艳咸燕美陆鑫华
Owner SHANGHAI WUJING CHEM
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