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Method for preparing 2,2,4-trimethyl-1,3-pentanediol single-isobutyrate

A technology of pentanediol monoisobutyrate and trimethyl, which is applied in the field of organic chemical industry, can solve the problems of non-conformity with the concept of green environmental protection, highly toxic substances, and large equipment corrosion, so as to achieve easy separation and recovery, and low equipment corrosion , the effect of simple operation

Inactive Publication Date: 2010-09-22
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However Ba(OH) 2 ·8H 2 O or Ba(OH) 2 ·H 2 O are all highly toxic substances, which do not conform to the concept of green environmental protection
CN1098712A uses NaOH as a catalyst, which causes great corrosion to equipment and many by-products

Method used

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  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol single-isobutyrate
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol single-isobutyrate
  • Method for preparing 2,2,4-trimethyl-1,3-pentanediol single-isobutyrate

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Experimental program
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Effect test

Embodiment 1

[0020] (1), preparation of KF / MgO catalyst

[0021] Step 1 Vector Pretreatment

[0022] 50g of MgAc 2 , in a muffle furnace at 500 ° C, under an air atmosphere, calcined for 5 hours under a temperature-programmed condition, and then cooled to room temperature and taken out to obtain MgO powder.

[0023] Step 2 Solid Phase Grinding

[0024] Take 6g MgO powder and a certain amount of KF·2H 2 O (the mass of converted KF is 30% of MgO), grind and mix in a mortar for 30min.

[0025] Step 3 Dry

[0026] Dry the KF / MgO obtained in the second step in an oven at 80° C. for 12 h. After cooling to room temperature, the catalyst KF / MgO-80 is obtained.

[0027] Step 4 Catalyst Treatment

[0028] Put the KF / MgO-80 obtained in the third step in a muffle furnace, and calcinate it under air atmosphere at 500°C for 5 hours under a temperature-programmed condition, then cool to room temperature and take it out to obtain the catalyst KF / MgO-500.

[0029] Other catalysts such as K 2 CO 3...

Embodiment 2

[0039] a, with stirring, in the 100mL tank reactor of condensing system and thermometer, add 30g of 2% NaOH solution, in N 2 Under the condition of protection and stirring, 30g of isobutyraldehyde was slowly added dropwise, and the aldol condensation reaction was carried out at 30°C; the reaction was stopped, washed with water, left standing for 8h, liquid separation, and the oil layer and the water layer were separated.

[0040] b, put the separated oil layer in a in N 2 Under protection, heat up to 90°C, add KF / γ-Al whose weight is 3% of oil layer weight 2 o 3 , magnetic stirring, continue to react 10h.

[0041] c., settle the reaction mixture obtained in b, filter and separate the catalyst, and distill the filtrate under reduced pressure to obtain the product 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, the product Yield = 50.8% by GC analysis.

Embodiment 4-5

[0043] with K 2 CO 3 / MgO, K 2 CO 3 / γ-Al 2 o 3 Be catalyzer, other conditions are identical with embodiment 1, and reaction result is as follows:

[0044]

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PUM

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Abstract

The invention discloses a method for preparing 2,2,4-trimethyl-1,3-pentanediol single-isobutyrate, which comprises the step of performing an intra-molecular Cannizzaro reaction on an aldol condensation product, which is prepared from isobutyraldehyde at a low temperature, under the action of a catalyst to synthesize the 2,2,4-trimethyl-1,3-pentanediol single-isobutyrate, wherein the catalyst is ametallic oxide heterogeneous catalyst modified by KF, K2CO3 or KOAc which is used as an active center base. The catalyst in the method is simple and easy to prepare, is easy to separate and reclaim and has small corrosion to equipment; and the method is simple to operate and has a mild reaction condition.

Description

technical field [0001] The invention belongs to the field of organic chemical industry and relates to the heterogeneous catalytic synthesis of alkali-modified metal oxides to synthesize 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate. Background technique [0002] In recent years, the rapid development of my country's real estate industry has greatly increased the demand for high-end architectural coatings. As one of the decorative materials, the quality of water-based high-end latex coatings has attracted more and more people's attention. The film-forming and environmental performance of coatings directly affect the use of coatings. Effect and construction performance. Therefore, coalescents have become the most critical raw materials for high-grade environmentally friendly coatings. [0003] The chemical name is 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate and the molecular formula is C 12 h 24 o 3 , whose structure is, [0004] [0005] It is a kind of non-water...

Claims

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Application Information

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IPC IPC(8): C07C69/28C07C67/44
Inventor 杨建国朱娟
Owner EAST CHINA NORMAL UNIVERSITY
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