Production method of aliphatic carboxylic acid ester

Patent metadata

Field	Value
Publication number	US-10919836-B2
Application number	US-201816639932-A
Country	US
Kind code	B2
Filing date	Sep 3, 2018
Priority date	Sep 5, 2017
Publication date	Feb 16, 2021
Grant date	Feb 16, 2021

Abstract

In a method for producing an aliphatic carboxylic acid ester by reacting an aliphatic carboxylic acid having from 1 to 5 carbon atoms and an olefin having from 2 to 4 carbon atoms in a gas phase by use of a solid acid catalyst, a solid acid catalyst in which a heteropolyacid or a salt thereof is supported on a silica carrier obtainable by kneading fumed silica obtained by a combustion method, silica gel obtained by a gel method, and colloidal silica obtained by a sol-gel method or a water glass method, molding the resulting kneaded product, and calcining the resulting molded body, is used.

First claim

The invention claimed is:

1. A method for producing an aliphatic carboxylic acid ester comprising the steps of:
1) kneading fumed silica obtained by a combustion method, silica gel obtained by a gel method, and colloidal silica obtained by a sol-gel method or a water glass method, molding the resulting kneaded product, and calcining the resulting molded body to obtain a silica carrier;
2) supporting a heteropolyacid or a salt thereof on the silica carrier to obtain a solid acid catalyst; and
3) reacting an aliphatic carboxylic acid having from 1 to 5 carbon atoms and an olefin having from 2 to 4 carbon atoms in a gas phase by use of the solid acid catalyst.

2. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein, in step 1), the blending amount of fumed silica is from 4.0 to 52.6 mass %, the blending amount of silica gel is from 33.3 to 90.0 mass %, and the blending amount of the solid content of colloidal silica is from 3.4 to 40.0 mass %, provided that the total amount of the fumed silica, the silica gel, and the solid content of the colloidal silica is 100 mass %.

3. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein the calcining temperature is from 300 to 1,000° C. in step 1).

4. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein the silica carrier obtained in step 1) has, in the measurement of pore size distribution, mesopores with a pore size of 2 to 50 nm and macropores with a pore size of more than 50 nm and 1,000 nm or less.

5. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein in the pore size distribution by mercury intrusion porosimetry, the pore volume of macropores of the silica carrier is from 0.05 to 0.50 cc/g.

6. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein the BET specific surface area of the silica carrier is from 200 to 500 m 2 /g.

7. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein the bulk density of the silica carrier is from 300 to 700 g/L.

8. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein the average pore size of mesopores by the BJH method of the silica carrier is from 3 to 16 nm.

9. The method for producing an aliphatic carboxylic acid ester according to claim 1 , wherein the particle diameter of the silica carrier is from 2 to 8 mm.

Assignees

• Showa Denko Kk

Inventors

• Itagaki Shintaro
• Yamashita Katsuhiko
• Takahashi Taku

Classifications

• B01J35/51

  Spheres · CPC title

• B01J35/32

  Bulk density · CPC title

• B01J35/40

  characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77) · CPC title

• B01J27/188

  with chromium, molybdenum, tungsten or polonium · CPC title

• B01J37/0018

  Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat) · CPC title