Carboxyl terminated dendritic polymer adsorption material and preparation method thereof

An adsorption material and dendritic technology, which is applied in the field of carboxyl-terminated dendritic polymer adsorption materials and their preparation, can solve the problems of difficult regeneration of adsorption adsorption materials, small adsorption capacity, low bulk density, etc., and achieves wide application range and action efficiency. Increased, less dosage effect

Active Publication Date: 2015-11-04
上海球球云环保科技有限公司
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Problems solved by technology

Commonly used adsorbents mainly include activated carbon, resin, and natural minerals. High-performance adsorbents are mostly synthetic polymer materials. For example, activated carbon is a porous carbon with low bulk density and large specific surface area. The adsorption capacity of some heavy metal ions and organic matter is relatively small, the selectivity is low, and the regeneration of adsorption and adsorption materials is difficult, and there is still a certain distance from the actual industrial application

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  • Carboxyl terminated dendritic polymer adsorption material and preparation method thereof
  • Carboxyl terminated dendritic polymer adsorption material and preparation method thereof
  • Carboxyl terminated dendritic polymer adsorption material and preparation method thereof

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preparation example Construction

[0027] The present invention relates to the preparation method of carboxyl-terminated dendritic polymer adsorption material, comprises the following steps:

[0028] 1) Preparation of hydroxyl-terminated dendrimers:

[0029] The first step: Weigh 5-10mmol of diol and dissolve it in 40-80mL of acetone; according to the molar ratio of diol to cyanuric chloride (3-4):1, dissolve cyanuric chloride in 50 -100mL of acetone or tetrahydrofuran, under the condition of nitrogen protection and ice-water bath, add dropwise to the acetone solution of dihydric alcohol; stir for 1-3h, slowly raise the temperature to 40-50°C, stir for 2-6h, and finally raise the temperature to 85-95°C, stirring and reacting for 3-9h, adding an acid-binding agent continuously during the reaction to maintain a pH of 5-6, and obtaining a crude product of a first-generation hydroxyl-terminated dendritic polymer;

[0030] Step 2: Repeatedly extract and wash the crude product of the first-generation hydroxyl-termin...

Embodiment 1

[0039] 1) Preparation of hydroxyl-terminated dendrimers:

[0040] Step 1: Dissolve 5mmol of dibasic alcohol in 80mL of acetone; Dissolve cyanuric chloride in 100mL of acetone according to the molar ratio of dibasic alcohol and cyanuric chloride to 3:1, store under nitrogen protection and ice Add dropwise to the acetone solution of dibasic alcohol under the condition of water bath; stir for 1 hour, slowly raise the temperature to 50°C, stir for 2 hours, finally raise the temperature to 95°C, stir for 3 hours, keep adding acid-binding agent during the reaction to maintain the pH of 6. Prepare a crude product of a first-generation hydroxyl-terminated dendritic polymer;

[0041] Step 2: Repeatedly extract and wash the crude product of the first-generation hydroxyl-terminated dendrimer with acetone, and vacuum filter to obtain the first-generation hydroxyl-terminated dendritic polymer;

[0042] The third step: with cyanuric chloride as the core and the first generation of hydroxyl...

Embodiment 2

[0049] 1) Preparation of hydroxyl-terminated dendrimers:

[0050] The first step: Weigh 7mmol dihydric alcohol and dissolve it in 60mL acetone; according to the ratio of dihydric alcohol and cyanuric chloride molar ratio of 3.5:1, dissolve cyanuric chloride in 75mL acetone, under nitrogen protection and ice Add dropwise to the acetone solution of dibasic alcohol in a water bath; stir for 2 hours, slowly raise the temperature to 45°C, stir for 4 hours, and finally raise the temperature to 90°C, stir for 6 hours, and keep adding acid-binding agents during the reaction to maintain the pH at 5. Prepare a crude product of a first-generation hydroxyl-terminated dendritic polymer;

[0051]Step 2: Repeatedly extract and wash the crude product of the first-generation hydroxyl-terminated dendrimer with acetone, and vacuum filter to obtain the first-generation hydroxyl-terminated dendritic polymer;

[0052] The third step: with cyanuric chloride as the core and the first generation of h...

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Abstract

The invention relates to a carboxyl terminated dendritic polymer adsorption material and a preparation method thereof. The dendritic polymer has a network spherical three-dimensional structure, and can greatly improve the adsorption efficiency as an adsorption material. The preparation method includes: dissolving cyanuric chloride in acetone or tetrahydrofuran, adding the mixture into an acetone solution of diol to obtain a primary hydroxy terminated dendritic polymer crude product, conducting purification to obtain a primary hydroxy terminated dendritic polymer; taking cyanuric chloride as the core, adopting the primary hydroxy terminated dendritic polymer as the branching unit to prepare a secondary hydroxy terminated dendritic polymer crude product and a tertiary hydroxy terminated dendritic polymer crude product, and carrying out purification; and dispersing the hydroxy terminated dendritic polymer in water, adding maleic anhydride and p-toluenesulfonic acid to prepare a carboxyl terminated dendritic polymer crude product, and conducting purification to obtain the carboxyl terminated dendritic polymer adsorption material. The method provided by the invention has the characteristics of mild conditions, simple process and short production cycle. The product contains a lot of active carboxyl terminal groups, has strong adsorption performance, and is expected to be used in heavy metal ion and organic wastewater treatment and other fields.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a carboxyl-terminated dendritic polymer adsorption material and a preparation method thereof. Background technique [0002] Compared with other water treatment methods, the adsorption method has the advantages of high removal rate, easy operation, and regenerable adsorbent, and is widely used in the treatment of low-concentration wastewater, especially heavy metal ions and organic matter. Commonly used adsorbents mainly include activated carbon, resin and natural minerals, etc. High-performance adsorbents are mostly synthetic polymer materials. For example, activated carbon is a kind of porous carbon with low bulk density and large specific surface area. The adsorption capacity of some heavy metal ions and organic substances is relatively small, the selectivity is low, and the regeneration of adsorption and adsorption materials is difficult, and there is still a c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28
Inventor 强涛涛李小宁赵静任龙芳王学川
Owner 上海球球云环保科技有限公司
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