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Preparation method of macroporous strong-acidity resin and application of macroporous strong-acidity resin

A strong acid resin and reaction technology, which is applied in the field of macroporous strong acid resin preparation to achieve the effects of expanding the scope of application, being easy to recycle and reuse, and increasing bond energy.

Active Publication Date: 2018-11-13
天门润诚生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Can be used repeatedly

Method used

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  • Preparation method of macroporous strong-acidity resin and application of macroporous strong-acidity resin
  • Preparation method of macroporous strong-acidity resin and application of macroporous strong-acidity resin
  • Preparation method of macroporous strong-acidity resin and application of macroporous strong-acidity resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation method of macroporous strongly acidic resin, concrete steps are as follows:

[0030] Step 1: Weigh p-nitrostyrene, divinylbenzene, toluene and azobisisoheptanonitrile with a mass ratio of 1:0.05:0.05:0.005, wherein the selected p-nitrostyrene has a mass of 7.458g. Mix p-nitrostyrene and divinylbenzene, wash twice with 5% (mass fraction, the same below) NaOH solution, and then wash twice with water to remove the hydroquinone inhibitor. Absolute pressure, the same below) and vacuum distillation at 45°C to obtain a purified mixture of p-nitrostyrene and divinylbenzene. Add toluene and azobisisoheptanonitrile to the mixture of p-nitrostyrene and divinylbenzene, stir and mix evenly, and then pour it into three mouthfuls of 30ml 0.2% (mass fraction, the same below) methylcellulose solution in the flask;

[0031] Step 2: Control the rotating speed to raise the temperature to 65°C under the condition of 1000r / min, and keep it for 1h; then raise the tempe...

Embodiment 2

[0034] A kind of preparation method of macroporous strongly acidic resin, concrete steps are as follows:

[0035] Step 1: Weigh p-nitrostyrene, divinylbenzene, paraffin oil and dibenzoyl peroxide with a mass ratio of 1:0.3:1.5:0.03, wherein the selected p-nitrostyrene has a mass of 7.458g. Wash twice with 5% NaOH aqueous solution, then wash twice with water to remove the hydroquinone inhibitor, and distill under reduced pressure at 10Pa and 45°C to obtain purified p-nitrostyrene and divinyl Benzene mixture. After adding paraffin oil and dibenzoyl peroxide (BPO) to the mixture of p-nitrostyrene and divinylbenzene, pour it into a three-necked flask filled with 30ml of 1.5% methylcellulose solution;

[0036] Step 2: Control the rotating speed to raise the temperature to 65°C under the condition of 4000r / min, and keep it for 3 hours; then raise the temperature to 75°C, keep it for 8 hours; then raise the temperature to 90°C, and keep it for 2 hours. Cool, filter, wash with water...

Embodiment 3

[0039] A kind of preparation method of macroporous strongly acidic resin, concrete steps are as follows:

[0040] Step 1: Weigh p-nitrostyrene, divinylbenzene, paraffin oil and dimethyl azobisisobutyrate with a mass ratio of 1: 0.16: 0.75: 0.015, wherein the quality of p-nitrostyrene selected is 7.458g. Mix p-nitrostyrene and divinylbenzene, wash twice with 5% NaOH solution, and then wash twice with water to remove the hydroquinone inhibitor, and distill under reduced pressure at 10Pa and 45°C to obtain Purified mixture of p-nitrostyrene and divinylbenzene. After adding paraffin oil and dimethyl azobisisobutyrate into the mixture of p-nitrostyrene and divinylbenzene, pour it into a three-necked flask equipped with 30ml of 0.85% polyvinyl alcohol solution;

[0041] Step 2: Control the rotational speed to raise the temperature to 65°C under the condition of 2500r / min, and keep it for 2h; then raise the temperature to 75°C, and keep it for 6h; then raise the temperature to 90°C...

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Abstract

The invention relates to a preparation method of macroporous strong-acidity resin and application of the macroporous strong-acidity resin. The preparation method comprises the following steps: performing coreaction on p-nitrostyrene serving as a main monomer raw material, divinylbenzene serving as a crosslinking agent, a dispersing agent, an initiator and a pore-forming agent to prepare microspheres of p-nitrostyrene-divinylbenzene, and performing sulfonation reaction through chlorosulfonic acid to prepare the macroporous strong-acidity resin. The prepared macroporous strong-acidity resin hashigh heat stability and can serve as an efficient catalyst as the following system: reaction of isoamylene and methanol is catalyzed to synthesize t-amyl-methyl ether (TAME), reaction of isoamylene and ethanol is catalyzed to synthesize ethyl tert-amyl ether (ETBE), and reaction of cyclopentene and methanol is catalyzed to synthesize cyclopentyl methyl ether (CPME); and extremely high catalytic activity on reaction such as synthesis of a loxoprofen sodium precursor and loxolfonic acid is achieved. In addition, the macroporous strong-acidity resin can be recovered and reused after catalytic reaction and is a green and environmentally-friendly efficient catalytic material.

Description

technical field [0001] The invention belongs to the technical field of polymer resins, and in particular relates to a preparation method of a macroporous strongly acidic resin and an application thereof. Background technique [0002] Ion exchange resins are widely used in industrial water treatment, pharmaceutical and food industries, pesticides, dyes, paints, detergents and other fine chemical industries, mineral processing and environmental protection and other fields. In the field of organic synthesis, strongly acidic ion exchange resins can be used as catalysts for organic reactions such as epoxidation reactions, addition reactions, and esterification reactions. In the paper "Ce 4+ Modified cation exchange resin catalyzed epoxidation reaction" (Zhou Jie, Ren Qinggong, Pan Jingjing, et al. Ce 4+ Research on epoxidation reaction catalyzed by modified cation exchange resin[J]. Ion Exchange and Adsorption, 2015(4):359-369.), a Ce 4+ The modified cation exchange resin is u...

Claims

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Application Information

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IPC IPC(8): C08F8/36C08F212/14C08F212/36C08J9/28C07C41/06C07C43/04C07C43/184C07C51/38C07C65/36C07C51/09
CPCB01J31/10B01J2231/32C07C41/06C07C51/09C07C51/38C08F8/36C08F212/14C08F2800/20C08J9/28C08J2201/0502C08J2325/18C07C2601/06C08F212/36C07C43/046C07C43/184C07C65/36
Inventor 程正载曾胜刘盼盼胡海李光要王涵鼎唐然王云丁玲李文兵马里奥·高斯尔
Owner 天门润诚生物科技股份有限公司
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