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Polycarboxyl silicon dioxide nanoparticles and preparation method thereof

A technology of hydroxy silica and nanoparticles, which is applied in the treatment of dyed organic silicon compounds, dyed low-molecular organic compounds, and fibrous fillers. The effect of high content, mild reaction conditions, and simple preparation process

Active Publication Date: 2015-05-20
JIANGSU HUAJIA SILK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the strong acidity and acylation ability of chloroacetic acid during the treatment process, the side reaction of chloroacetamide will be generated during the reaction process, which seriously affects the degree of carboxylation

Method used

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  • Polycarboxyl silicon dioxide nanoparticles and preparation method thereof
  • Polycarboxyl silicon dioxide nanoparticles and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Hydroxy silica nanoparticles surface treatment

[0028] Add 100 g of tetrahydrofuran (THF) and 10 g of hydroxy silica nanoparticles (commercially available) with a particle size of 300 nm in a 1000 mL three-necked flask, and ultrasonically disperse the suspension for 10 min, then add 22.1 g of 3-aminopropyl triethoxy A solution of silane (APTES) dissolved in 20 g of tetrahydrofuran. After the mixture was refluxed at 60°C for 6 hours, the reaction was stopped, cooled to room temperature, centrifuged, and dried at 90°C for 1 hour to obtain amino silica nanoparticles.

[0029] (2) Carboxylation treatment

[0030] Add 30 g of tetrahydrofuran and 23.4 g of butane tetracarboxylic acid to a 500 mL three-necked flask in sequence, under nitrogen protection, dropwise add 16.2 g N,N' - A solution formed by dissolving carbonyldiimidazole (CDI) in 50 gTHF, and the dropping time was controlled within 1.5 hours. After the addition, react at room temperature for 5 h, then add t...

Embodiment 2

[0038] (1) Hydroxy silica nanoparticles surface treatment

[0039]Add 150g of tetrahydrofuran (THF) and 10g of hydroxylated silica nanoparticles with a particle size of 50nm in a 1000mL three-necked flask. The suspension is ultrasonically dispersed for 15min, and then 26.5g of aminoethylaminopropyltriethoxysilane is added and dissolved in 20g solution in tetrahydrofuran. After the mixture was refluxed at 65°C for 5 hours, the reaction was stopped, cooled to room temperature, centrifuged, and dried at 92°C for 1 hour to obtain amino silica nanoparticles.

[0040] (2) Carboxylation treatment

[0041] Add 50 g tetrahydrofuran and 46.8 g butane tetracarboxylic acid successively to a 500 mL three-necked flask, and under nitrogen protection, add 32.4 g N,N' - A solution formed by dissolving carbonyldiimidazole (CDI) in 70 gTHF, and the dropping time was controlled within 2 hours. After the addition, react at room temperature for 5 h, then add the above-mentioned aminoethylaminop...

Embodiment 3

[0051] (1) Hydroxy silica nanoparticles surface treatment

[0052] Add 120g of 1,4-dioxane and 8 g of hydroxylated silica nanoparticles with a particle size of 100nm in a 1000mL three-necked flask, and ultrasonically disperse the suspension for 15min, then add 26.5g of aminoethylaminopropyltrimethoxysilane A solution formed by dissolving in 25 g of 1,4-dioxane. After the mixture was refluxed at 58°C for 5 hours, the reaction was stopped, cooled to room temperature, centrifuged, and dried at 90°C for 1 hour to obtain amino silica nanoparticles.

[0053] (2) Carboxylation treatment

[0054] Add 60 g of 1,4-dioxane and 46.8 g of butane tetracarboxylic acid in sequence to a 500 mL three-necked flask, and add 31.9 g of N,N' - A solution formed by dissolving carbonyldiimidazole (CDI) in 65 g of 1,4-dioxane, and the dropping time was controlled within 1.5 hours. After the addition, react at room temperature for 5 h, then add the above-mentioned aminoethylaminopropyl silica nanopa...

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Abstract

The invention discloses polycarboxyl silicon dioxide nanoparticles and a preparation method thereof. The preparation method comprises the following steps: by using hydroxy silicon dioxide nanoparticles as the initial raw material, treating with an aminosilane coupling agent to introduce reactive amino or amine group, and reacting with N,N-carbonyldiimidazole-activated butane tetrabasic carboxylic acid under very mild conditions to introduce 3,4,5-tricarboxylvaleryl group onto the surface of the hydroxy silicon dioxide nanoparticles, thereby obtaining the surface-polycarboxylated modified silicon dioxide nanoparticles. By using the butane tetrabasic carboxylic acid to perform carboxylation modification on the hydroxy silicon dioxide nanospheres, the polycarboxyl silicon dioxide nanoparticles have the advantages of high carboxyl content and controllable carboxyl content; and since the reaction conditions for the N,N-carbonyldiimidazole-activated butane tetrabasic carboxylic acid and amino group are very mild, the reaction is easy to perform and is complete. The method disclosed by the invention has the advantages of simple preparation technique and accessible raw materials, and is easy for industrial production and popularization.

Description

technical field [0001] The invention relates to a carboxylated silica nanoparticle, in particular to a polycarboxylated silica nanoparticle and a preparation method thereof, and belongs to the field of synthesis of composite materials and fine chemicals. Background technique [0002] Silica nanoparticles have been widely used in modern industry. The introduction of carboxyl groups on the surface of silica nanoparticles can not only improve the interfacial compatibility between small spherical particles and matrix materials, but more importantly, the wide reaction range of carboxyl groups and easy The ionization characteristic endows the particles with high reactivity, so that they can be widely used in polymer material modifiers, water treatment agents, catalysts and carrier materials, microcapsule embedding and other fields. [0003] There have been many reports on the method of introducing carboxyl groups in hydroxyl silica nanoparticles. Most of them first use aminosilane...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/12C09C3/08
Inventor 张丽洁蒋碧玉张娇莉李惠刘锦臧雄李战雄眭建华
Owner JIANGSU HUAJIA SILK
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