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Phthalate type plasticizer hydrogenated catalyst preparation method thereof and application

A technology of phthalates and catalysts, which is applied in the preparation of carboxylate esters, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of complex preparation, high requirements for hydrogenation process conditions, and easy deactivation, and achieve the goal of preparing Simple, no by-products, mild reaction conditions

Inactive Publication Date: 2017-07-28
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, phthalate hydrogenation catalysts have problems such as complex preparation, easy deactivation, and high requirements for hydrogenation process conditions. Therefore, we have invented a phthalate hydrogenation to produce cyclohexanedicarboxylate Compared with the prior art, the present invention has the characteristics of simple catalyst preparation, mild reaction conditions, high product yield, and no by-products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for preparing a catalyst for hydrogenation of phthalate plasticizers to produce cyclohexane dicarboxylate, the specific steps are as follows:

[0023] Weigh 1 g of sodium bicarbonate to prepare 5% sodium bicarbonate solution, use it to treat 10 g of alumina, stir evenly at room temperature, overnight at 110°C, dry, and grind; weigh 0.027 g of RuCl 3 ·xH 2 O (about 37% Ru), 0.382 g of Cu(NO 3 ) 2 ·3H 2 O was dissolved in 20 g of distilled water, and after it was completely dissolved, the treated carrier was sprayed into the impregnation solution, stirred for 2 h, immersed for 6 h, overnight at 110 °C, dried, ground, and washed 4 times with water to remove Cl - , overnight at 110 °C, dried, and ground to obtain the catalyst precursor; the prepared catalyst precursor was activated in a hydrogen atmosphere under normal pressure at a temperature of 100 °C for 10 h. Wherein the active component accounts for 0.1% by mass of the total catalyst, and the auxiliary ag...

Embodiment 2

[0025] A method for preparing a catalyst for hydrogenation of phthalate plasticizers to produce cyclohexane dicarboxylate, the specific steps are as follows:

[0026] Weigh 1 g of sodium carbonate to prepare 2% sodium carbonate solution, use it to treat 10 g of zirconia, stir evenly at room temperature, dry at 110 °C overnight, and grind; weigh 0.932 g of RuCl 3 ·xH 2 O (about 37% Ru), 5.244 g of Mn(NO 3 ) 2 4H 2 O was dissolved in 50 g of distilled water, and after it was completely dissolved, the treated carrier was sprayed into the impregnation solution, stirred for 2 h, immersed for 7 h, overnight at 110 °C, dried, ground, and washed 4 times with water to remove Cl - , overnight at 110 °C, dried, and ground to obtain the catalyst precursor; the prepared catalyst precursor was activated in a hydrogen atmosphere at normal pressure at a temperature of 150 °C for 4 h. Wherein the active component accounts for 3% by mass of the total catalyst, and the auxiliary agent accoun...

Embodiment 3

[0028] A method for preparing a catalyst for hydrogenation of phthalate plasticizers to produce cyclohexane dicarboxylate, the specific steps are as follows:

[0029] Weigh 1 g of sodium carbonate to prepare 5% sodium carbonate solution, use it to treat 10 g of silica, stir evenly at room temperature, overnight at 110°C, dry and grind; weigh 0.030 g of RuCl 3 ·xH 2 O (about 37% Ru), 2.000 g of Ni(NO 3 ) 2 ·6H 2 O and 5.434 g of Cr(NO 3 ) 3 9H 2 O was dissolved in 20 g of distilled water, and after it was completely dissolved, the treated carrier was sprayed into the impregnation solution, stirred for 2 h, immersed for 7 h, overnight at 110 °C, dried, ground, and washed 4 times with water to remove Cl - , overnight at 110°C, dried, and ground to obtain the catalyst precursor; the catalyst precursor was activated in a hydrogen atmosphere under normal pressure at a temperature of 200°C for 4 hours. Wherein the active component accounts for 0.1% by mass of the total catalys...

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PUM

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Abstract

The invention discloses a phthalate type plasticizer hydrogenated catalyst preparation method thereof and an application, and belongs to the field of catalytic hydrogenation. The catalyst consists of active component, assistant and carrier, wherein the active component is 0.1-3% of total content of catalyst by mass, assistant is 1-10% of total content of catalyst by mass, and the rest is carrier. The active component of the catalyst is precious metal element ruthenium; assistants are copper, manganese, cobalt, nickel, iron, chromium and tin; the carrier is zirconia, titanium oxide, alumina, silica, silicon carbide, zinc oxide, magnesium oxide, activated carbon, diatomite, aluminosilicate, molecular sieve. Compared with the prior art, the catalyst preparation method is simple in preparation, gentle in reaction condition, high in product yield, and free from side product.

Description

technical field [0001] The invention belongs to the field of catalytic hydrogenation, in particular to a preparation method and application of a catalyst for producing cyclohexanedicarboxylate by hydrogenation of phthalate plasticizers. Background technique [0002] With the rapid development of polyvinyl chloride (PVC) industry and petroleum industry, plasticizers are widely demanded. Among them, phthalates (PAEs) compounds are currently the most widely used and the largest output of the main plasticizers, which have good comprehensive performance, light color, good electrical properties, low volatility, and low odor. Consumption accounts for about 80% of the total consumption of plasticizers. PAEs plasticizers can enter the human body through many ways, and the toxicity research of its benzene ring structure has attracted extensive attention of scholars. With the deepening of environmental protection, green and non-toxic concepts, PAEs plasticizers are no longer suitab...

Claims

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Application Information

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IPC IPC(8): B01J23/656B01J23/89B01J29/00C07C67/303C07C69/75
CPCB01J23/8926B01J23/6562B01J23/8966B01J23/8993B01J29/00C07C67/303C07C69/75
Inventor 何明阳曹芮钱俊峰孙富安陈群
Owner CHANGZHOU UNIV
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