Process for producing acetate from p-toluene sulfonic acid

A technology of p-toluenesulfonic acid and acetate, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of acid corrosion, low catalytic reaction temperature and high catalytic activity temperature, and achieve less loss effect

Pending Publication Date: 2018-11-30
南京诺奥新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The catalyst usually used in the direct esterification of acid alcohol is diluted sulfuric acid aqueous solution, and the hydrogen ions ionized by sulfuric acid participate in the esterification reaction in the aqueous solution; although the content of this catalyst aqueous solution in the esterification kettle liquid is only 0.5%~1 %, the catalyst has the characteristics of low catalytic reaction temperature and high catalyst activity, and has always been a type of catalyst commonly used in esterification reactions; but this type of catalyst has the following shortcomings: 1. Acid corrosion is a common problem of acid catalysts; 2. Sulfuric acid catalyst has oxidation effect on reaction raw materials; 3. Sulfuric acid catalyst has dehydration to reaction raw materials; 4. Under certain conditions, sulfuric acid catalyst has a side reaction with raw material alcohol to produce sulfuric acid ester, bisulfate and other products
It is not an acid catalyst. Although it is very less corrosive to equipment, the selectivity of the reaction is also very high, and the side reactions are relatively few, but the catalytic activity temperature is relatively high. For example, the reaction temperature of stannous oxide and titanate catalysts is as high as 180°C The above are generally only suitable for the esterification reaction of high boiling point reaction raw materials

Method used

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  • Process for producing acetate from p-toluene sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Sulfuric acid and p-toluenesulfonic acid were tested for comparison.

[0026] Select 2g of sulfuric acid and 4g of p-toluenesulfonic acid as catalysts respectively, and configure them into 30% aqueous solution through the first and second steps in the above method. The concentration of hydrogen ions in the aqueous solution is about 0.04mol, and the concentration of the catalyst Basically the same.

[0027] Then use the third step and the fourth step in the above method to carry out catalytic reaction, then continue to add acetic acid and n-propanol (n-butanol) reaction mixture, and finally get 2 kg of acetic acid ester crude ester material containing about 86%, stop The results after the reaction are detected as shown in Table 1:

[0028] catalyst

Acetate content

unknown content

Waste liquid volume

Kettle liquid condition

sulfuric acid

85.69%

3.6%

100mL

black sticky

p-toluenesulfonic acid

86.11%

0.17%

5mL ...

Embodiment 2

[0032] P-toluenesulfonic acid is 1% to catalyze the production process of esterification propyl acetate as shown in table 2-3:

[0033] serial number

[0034] serial number

[0035] It can be seen from the above table that when p-toluenesulfonic acid is used as a catalyst for the catalytic reaction, the water separation is close to the theoretical production amount of 60mL, and the reaction effect is excellent.

Embodiment 3

[0037] The production process of p-toluenesulfonic acid catalyzed esterification to produce n-butyl propionate is shown in table 4-5:

[0038] serial number

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Abstract

The invention relates to a process for producing acetate from p-toluene sulfonic acid; a solid p-toluene sulfonic acid catalyst is added into deionized water and stirred to prepare an aqueous solution; the prepared aqueous solution is pressurized for standby use; acetic acid and n-propanol are added into an esterification reactor, the catalyst aqueous solution is pumped into the reactor, the mixture is uniformly mixed and heated to 105-110 DEG C to complete preparation of a reaction base material. The beneficial effects are that the experimental result of corrosiveness of the p-toluene sulfonic acid esterification system is obviously better than the experimental result of corrosiveness of sulfuric acid as a catalyst; the miscibility effect of the p-toluene sulfonic acid with the reaction raw materials is better; the p-toluene sulfonic acid catalyst does not need to be additionally added, and the loss of the catalyst is less; kettle residue of p-toluene sulfonic acid catalysis is stillrelatively clear; and the content of alcohols in crude esters produced by p-toluene sulfonic acid catalytic reaction is less, and the content of unknown substances is 0.17%, which is obviously lower.Waste esterification liquid produced by esterification of the p-toluene sulfonic acid catalytic system is about 5 ml, and the p-toluene sulfonic acid is obviously better than the sulfuric acid.

Description

technical field [0001] The invention relates to the field of esterification catalysis, in particular to a process for producing acetate by using p-toluenesulfonic acid. Background technique [0002] The catalyst usually used in the direct esterification of acid alcohol is diluted sulfuric acid aqueous solution, and the hydrogen ions ionized by sulfuric acid participate in the esterification reaction in the aqueous solution; although the content of this catalyst aqueous solution in the esterification kettle liquid is only 0.5%~1 %, the catalyst has the characteristics of low catalytic reaction temperature and high catalyst activity, and has always been a type of catalyst commonly used in esterification reactions; but this type of catalyst has the following shortcomings: 1. Acid corrosion is a common problem of acid catalysts; 2. The sulfuric acid catalyst has an oxidation effect on the reaction raw materials; 3. The sulfuric acid catalyst has dehydration to the reaction raw m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/14
CPCC07C67/08C07C69/14
Inventor 李宗洲方世银刘玉斌董非非
Owner 南京诺奥新材料有限公司
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