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Resin catalyst for synthesizing mibk and preparation method thereof

A catalyst and chelating resin technology, applied in catalyst activation/preparation, carbon-based compound preparation, chemical instruments and methods, etc., can solve problems such as difficult to effectively control product quality, difficult to control solution acidity and alkalinity, insufficient catalyst acidity, etc. Achieve the effect of improving activity and use stability, firm palladium loading, high conversion rate and selectivity

Active Publication Date: 2022-02-18
丹东明珠特种树脂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the method of first chelating palladium and then adsorbing, the adsorption process takes up the active site on the sulfonic acid group, resulting in insufficient acidity and activity of the catalyst; moreover, in the palladium chelation treatment in advance, the acidity and alkalinity of the solution is difficult to control, which will cause The palladium precipitates out, and the pre-chelated palladium cannot be completely adsorbed on the catalyst during the adsorption process, resulting in a large amount of palladium loss and a very large change in palladium loading, making it difficult to effectively control product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Catalyst A:

[0029] ①. Copolymerization: Add water, alum, and hydroquinone to a stainless steel stirred tank with a reflux condensing device, heat and stir to dissolve completely, and obtain an aqueous phase; by weight, the components of the aqueous phase are:

[0030] 2000 parts of water,

[0031] 20 parts of alum,

[0032] 20 parts of hydroquinone;

[0033] Raise the temperature to 40°C, add the oil phase, and by weight, the same as below, the ratio of the water phase to the oil phase is 2040:1105, stir and heat up to 80°C, react for 8 hours, and the stirring speed is 100r / min to obtain a copolymer White ball; described oily phase comprises o-chlorostyrene, divinylbenzene, methyl isobutyl ketone and benzoyl peroxide, also by weight, each component is:

[0034] 500 parts of o-chlorostyrene,

[0035] 100 parts of divinylbenzene,

[0036] 500 parts of methyl isobutyl ketone,

[0037] 5 parts of benzoyl peroxide;

[0038] ②. Pore structure purification: The filter...

Embodiment 2

[0044] Catalyst B:

[0045] ①. Copolymerization: Add water, alum, and hydroquinone to a stainless steel stirred tank with a reflux condensing device, heat and stir to dissolve completely, and obtain an aqueous phase; by weight, the components of the aqueous phase are:

[0046] 2500 parts of water,

[0047] 50 parts of alum,

[0048] 50 parts of hydroquinone;

[0049] Raise the temperature to 50°C, add the oil phase, and by weight, the same as below, the ratio of the water phase to the oil phase is 2600:1520, stir and heat up to 90°C, react for 10 hours, and the stirring speed is 140r / min to obtain a copolymer white ball; the oil phase includes o-chlorostyrene, divinylbenzene, methyl isobutyl ketone and benzoyl peroxide, and each component is:

[0050] 600 parts of o-chlorostyrene,

[0051] 300 parts of divinylbenzene,

[0052] 600 parts of methyl isobutyl ketone,

[0053] 20 parts of benzoyl peroxide;

[0054] ②. Pore structure purification: The filtered copolymer white...

Embodiment 3

[0060] Catalyst C:

[0061] ①. Copolymerization: Add water, alum, and hydroquinone to a stainless steel stirred tank with a reflux condensing device, heat and stir to dissolve completely, and obtain an aqueous phase; by weight, the components of the aqueous phase are:

[0062] 2200 parts of water,

[0063] 30 parts of alum,

[0064] 30 parts of hydroquinone;

[0065] Raise the temperature to 45°C, add the oil phase, and by weight, the same as below, the ratio of the water phase to the oil phase is 2260:1310, stir the temperature to 85°C, react for 9 hours, and the stirring speed is 120r / min to obtain a copolymer white ball; the oil phase includes o-chlorostyrene, divinylbenzene, methyl isobutyl ketone and benzoyl peroxide, and each component is:

[0066] 550 parts of o-chlorostyrene,

[0067] 200 parts of divinylbenzene,

[0068] 550 parts of methyl isobutyl ketone,

[0069] Benzoyl peroxide 10 parts;

[0070] ②. Pore structure purification: The filtered copolymer white...

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PUM

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Abstract

This patent application provides a resin catalyst for synthesizing MIBK and its preparation method. The preparation method of the catalyst is: using o-chlorostyrene and divinylbenzene as monomers and methyl isobutyl ketone as the porogen, It includes suspension copolymerization in the presence of a dispersant. The copolymer white balls are purified by boiling distilled water, chloroacylated with methyl chloride, and then loaded with palladium after chelation reaction with aminodiacetic acid. The palladium is reduced and solidified and then sulfonated. This technical solution has the technical advantages of firm palladium loading, better stability, high activity, long service life, high single-pass acetone conversion rate and high MIBK selectivity.

Description

technical field [0001] This patent application relates to resin catalyst preparation and its application. Background technique [0002] Methyl isobutyl ketone, referred to as MIBK, is an important organic solvent used in paints, resins, coatings and other industries. It is also an important raw material for organic synthesis. [0003] The manufacturing methods of MIBK mainly include one-step method and three-step method. The three-step method has been gradually replaced by the one-step method due to technical problems such as long production process route, difficult purification of intermediates, and low yield. There are two main types of catalysts used in the one-step preparation of MIBK: one is Pd / Al 2 o 3 And Pd molecular sieve catalyst, the other is Pd-loaded resin catalyst. The former is due to the water produced in the preparation process of MIBK, which will rapidly reduce the strength of the inorganic catalyst when it encounters water, making it impossible to use ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C07C45/73C07C49/04C08F212/14C08F212/36C08J9/26C08F8/32C08F8/18
CPCB01J31/069B01J37/0018C07C45/73C08F212/14C08J9/26C08F8/32C08F8/18C08J2201/0422
Inventor 王义成冷东斌张伟吕晓东彭慧敏吴万春王英杰段宏毅管秀明
Owner 丹东明珠特种树脂有限公司