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Magnetically recyclable nano magnetic polyacrylic acid microsphere catalyst as well as preparation method and application thereof

A polyacrylic acid microsphere, nano-magnetic technology, applied in catalytic reactions, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve obvious economic and social benefits, good thermodynamic stability, and large reaction area.

Inactive Publication Date: 2020-12-22
江西赣江新区有机硅创新研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above-mentioned technical problems in the preparation of vinyl cyclosiloxane by one-step direct hydrolysis and condensation of existing methyl vinyl dichlorosilane, the present invention provides a magnetically recyclable nano-magnetic polyacrylic acid microsphere catalyst and its preparation method It has the characteristics of more product generation, easy separation of catalyst, recycling of catalyst and unaffected product quality

Method used

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  • Magnetically recyclable nano magnetic polyacrylic acid microsphere catalyst as well as preparation method and application thereof
  • Magnetically recyclable nano magnetic polyacrylic acid microsphere catalyst as well as preparation method and application thereof
  • Magnetically recyclable nano magnetic polyacrylic acid microsphere catalyst as well as preparation method and application thereof

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preparation example Construction

[0040] Such as figure 1 The preparation method of the shown magnetic recyclable nano-magnetic polyacrylic acid microsphere catalyst comprises the following steps,

[0041] (1) Nano-Fe 3 o 4 / HD ferrofluid with as figure 2 Styrene shown, such as image 3 Acrylic as shown, such as Figure 4 p-divinylbenzene as shown, when mixed to form an oily phase;

[0042] (2) deionized water and sodium lauryl sulfate are mixed to form an aqueous phase;

[0043] (3) Under stirring conditions, the oil phase is added dropwise to the water phase to obtain a black suspension;

[0044] (4) Put the black suspension in an ice-water bath, and use a 100-300W cell pulverizer to micro-emulsion for 10-30 minutes to obtain a micro-emulsion;

[0045] (5) Pour the miniemulsion into a new reaction vessel, add K in the reaction vessel 2 S 2 o 8 , under the protection of nitrogen, stirring and polymerizing at a temperature of 60-80°C for 12-24 hours to obtain ethanol demulsification;

[0046] (6) W...

Embodiment 1

[0060] Preparation method of magnetically recyclable nano-magnetic polyacrylic acid microsphere catalyst;

[0061] (1) 10g nanometer Fe 3 o 4 / HD magnetic fluid mixed with 9.1g styrene, 4.4g acrylic acid and 0.45g p-divinylbenzene to form an oil phase, ultrasonically dispersed for 10min, then 300mL deionized water and 1.8g sodium lauryl sulfate were mixed to form a water phase, Under the condition of stirring (300rpm), the oil phase was added dropwise to the water phase, and stirred for 2h to obtain a black suspension;

[0062] (2) Place the black suspension in an ice-water bath, use a 300W cell pulverizer to finely milk 30min to obtain a fine emulsion, then pour the fine emulsion into a reaction vessel, stir at a speed of 300rpm, replace the air with nitrogen for 30min, and add 0.075g K 2 S 2 o 8 , N 2 Stir under protection, raise the temperature to 70°C for constant temperature polymerization for 18 hours, break the emulsification with ethanol, wash with deionized water...

Embodiment 2

[0064] Preparation method of magnetically recyclable nano-magnetic polyacrylic acid microsphere catalyst;

[0065] (1) 7.2g nanometer Fe 3 o 4 / HD magnetic fluid mixed with 3.6g styrene, 1.44g acrylic acid and 0.22g p-divinylbenzene to form an oil phase, ultrasonically dispersed for 10min, then 270mL deionized water and 1.8g sodium lauryl sulfate were mixed to form a water phase, Under the condition of stirring (300rpm), the oil phase was added dropwise to the water phase, and stirred for 2h to obtain a black suspension;

[0066] (2) Place the black suspension in an ice-water bath, use a 300W cell pulverizer to finely milk 30min to obtain a fine emulsion, then pour the fine emulsion into a reaction vessel, stir at a speed of 300rpm, replace the air with nitrogen for 30min, and add 0.055g K 2 S 2 o 8 , N 2 Stir under protection, raise the temperature to 70°C for constant temperature polymerization for 18 hours, break the emulsion with ethanol, wash with deionized water, an...

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Abstract

The invention relates to the technical field of synthesis of a foaming agent, and particularly discloses a magnetically recyclable nano magnetic polyacrylic acid microsphere catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps of (1) mixing nano Fe3O4 / HD magnetic fluid with styrene, acrylic acid and p-divinylbenzene to form an oil phase, (2) mixing deionized water and lauryl sodium sulfate to form a water phase, (3) dropwise adding the oil phase into the water phase to obtain a black suspension, (4) putting the black suspensioninto an ice-water bath, and carrying out fine emulsion for 10-30 minutes by using a 100-300W cell disintegrator to obtain a fine emulsion, (5) pouring the fine emulsion into a new reaction container,adding K2S2O8 into the reaction container, and stirring and polymerizing for 12-24 hours at the temperature of 60-80 DEG C to obtain ethanol demulsified emulsion, and (6) freeze-drying to obtain the nano magnetic polyacrylic acid microsphere catalyst. The method provided by the invention has the characteristics of large product generation amount, easy separation of the catalyst, cyclic utilizationof the catalyst and no influence on product quality.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a magnetically recyclable nano-magnetic polyacrylic acid microsphere catalyst and its preparation method and application. Background technique [0002] Vinylcyclosiloxanes in industrial applications, mainly composed of trimethyltrivinylcyclotrisiloxane, tetramethyltetravinylcyclotetrasiloxane and pentamethylpentavinylcyclopentasiloxane, i.e. D 3 vi 、D 4 vi and D 5 vi . At present, in industrial production, methyl vinyl dichlorosilane is hydrolyzed first, and then the hydrolyzed product is catalytically cracked and rearranged under alkaline conditions to prepare vinyl cyclosiloxane; this indirect synthesis method is generally at high temperature. Cleavage and rearrangement will cause migration and rearrangement of the groups in the organosiloxane, generating a large amount of impurities and increasing the cost of subsequent product separation. [0003] One-step ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/10C07F7/21B82Y40/00C08F212/08C08F220/06C08F212/36
CPCB01J31/1815B01J31/1658B01J31/1691C07F7/21B82Y40/00C08F212/08B01J2531/0241B01J2531/828B01J2231/323B01J35/33B01J35/61C08F220/06C08F212/36Y02P20/584
Inventor 沈显波罗双云李爱民麻培智
Owner 江西赣江新区有机硅创新研究院有限公司