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Process for preparing 1,3-propanediol

A technology of propylene glycol and alcohol solution, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc.

Inactive Publication Date: 2019-11-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

From the examples listed in this patent document, it can be seen that the single-pass yield of its 1,3-propanediol is about 50%, and there is still room for improvement

Method used

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  • Process for preparing 1,3-propanediol
  • Process for preparing 1,3-propanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 24.16g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 196 mL deionized water at room temperature, 20% ammonium bicarbonate was added dropwise under vigorous stirring, and then silica gel (SiO 2 ), aging at 40°C for 4 hours; heating up and distilling ammonia to PH=7; filtering and washing with water; drying at 120°C for 12 hours, and roasting at 450°C for 4 hours; tableting, grinding, and sieving to obtain 20-60 mesh particles. Denoted as catalyst A.

Embodiment 2

[0035] 24.16g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 196mL deionized water at room temperature, 25% ammonia water was added dropwise under vigorous stirring, and then silica gel (SiO 2 ), aging at 40°C for 4 hours; heating up and distilling ammonia to PH=7; filtering and washing with water; drying at 120°C for 12 hours, and roasting at 450°C for 4 hours; tableting, grinding, and sieving to obtain 20-60 mesh particles. Denoted as Catalyst B.

Embodiment 3

[0037] 24.16g Cu(NO 3 ) 2 ·3H 2 O, 7.16g 50% Mn(NO 3 ) 2 Dissolve the aqueous solution in 196mL deionized water at room temperature, add 20% ammonium carbonate dropwise under vigorous stirring, then add silica gel, age at 40°C for 8 hours; heat up and distill ammonia to PH=7; filter and wash with water; dry at 100°C for 12 hours, and roast at 500°C 5h; tablet, grind, and sieve out 20-60 mesh particles. Denoted as catalyst C.

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Abstract

The invention relates to a method for preparing 1,3-propylene glycol by dialkyl malonates through catalytic hydrogenation (reduction). The method comprises the following steps: under existence condition of a catalyst, a target object is prepared by dialkyl malonates through hydrogenation reduction; the catalyst is the supported catalyst, by taking the total weight of the supported catalyst as 100%, the supported catalyst comprises 10-40 wt% of metal copper and / or its oxide, 0-15 wt% of a cocatalyst component, and 60-90 wt% of a carrier; the cocatalyst component is a boron and / or its oxide, a zinc and / or its oxide, or manganese and / or its oxide; and the carrier is silica gel or / and a mesoporous molecular sieve. Due to selection of the appropriate catalyst, the product (1,3-propylene glycol)yield is high.

Description

technical field [0001] The invention relates to a method for preparing 1,3-propanediol, in particular to a method for preparing 1,3-propanediol from dialkyl malonate through catalytic hydrogenation (reduction). Background technique [0002] 1,3-propanediol, as an important chemical raw material, can be used in ink, printing and dyeing, paint, medicine, lubricant, antifreeze, and can also be used as a monomer of polyester and polyurethane for the production of polyol polyester and As a carbon chain extender. The main reason for the rapid development of 1,3-propanediol is that it is an important monomer for the synthesis of polytrimethylene terephthalate (PTT). PTT is a synthetic fiber material that realizes industrial scale after polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), and is a new type of polyester material with great development prospects. [0003] Ethylene oxide carbonylation method (US 5304686 and WO 02102754 etc.), acrolein hydration hydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/149C07C31/20
CPCC07C29/149C07C31/205
Inventor 田恒水丁同梅魏永梅李峰
Owner EAST CHINA UNIV OF SCI & TECH