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Ester-containing quaternary ammonium salt modified montmorillonite and preparation method thereof

The technology of ester quaternary ammonium salt and montmorillonite is applied in the direction of fibrous filler, dyed low-molecular-weight organic compound treatment, etc., can solve the problems of high reaction temperature, single modification effect, complicated method, etc., and achieves simple preparation method, The effect of improving compatibility and good degradability

Active Publication Date: 2015-04-22
河南天海合聚新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The quaternary ammonium salt modified montmorillonites that have been reported so far include: Allyl quaternary ammonium salt modified montmorillonite [Gao Dangge, Ma Jianzhong, Lu Bin, Guo Haiqing. Modified montmorillonite containing diallyl quaternary ammonium salt Preparation method of soil [P]. Chinese patent: 101597067, 20091209], the modification method is simple and effective, but the modification effect is single; hyperbranched quaternary ammonium salt modified montmorillonite [Wang Jincheng, Yang Ke, Zheng Xiaoyu. Hyperbranched quarter Ammonium salt organically modified montmorillonite and its preparation method [P]. Chinese patent 101717090A, 20100602]. This modification method can effectively open the distance between montmorillonite layers, but the method is relatively complicated and the reaction temperature is high

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  • Ester-containing quaternary ammonium salt modified montmorillonite and preparation method thereof
  • Ester-containing quaternary ammonium salt modified montmorillonite and preparation method thereof
  • Ester-containing quaternary ammonium salt modified montmorillonite and preparation method thereof

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Embodiment 1

[0029] The preparation method step of present embodiment containing ester group quaternary ammonium salt modified montmorillonite is as follows:

[0030] 1) Add 100mL of deionized water to a 250mL three-necked flask, then add 3.00g of montmorillonite powder, stir well to obtain a dispersion with a concentration of 30g / L, and calculate according to the ion exchange capacity (CEC) of 90mmol / 100g of montmorillonite , add C16 diester-based quaternary ammonium salt surfactant, gradually increase the temperature and stabilize at 70°C, fully stir and condense and reflux for 2 hours to obtain a uniform white suspension;

[0031] 2) Ultrasonic disperse the above white suspension for 15min, then centrifuge at 10000r / min for 20min, remove the supernatant to obtain a white precipitate, wash the white precipitate twice with deionized water and ethanol respectively, and then incubate at 80°C Dry it under vacuum for 24 hours to obtain a white flaky solid, and then grind it to obtain the este...

Embodiment 2

[0034] The preparation method step of present embodiment containing ester group quaternary ammonium salt modified montmorillonite is as follows:

[0035] 1) Add 100mL of deionized water to a 250mL three-neck flask, then add 4.00g of montmorillonite powder, stir well to obtain a dispersion with a concentration of 40g / L, and calculate the ion exchange capacity (CEC) as 90mmol / 100g of montmorillonite , add C16 diester-based quaternary ammonium salt surfactant, gradually increase the temperature and stabilize it at 75°C, fully stir and condense and reflux for 3 hours to obtain a uniform white suspension;

[0036] 2) Ultrasonic disperse the above white suspension for 20min, then centrifuge at 11000r / min for 20min, remove the supernatant to obtain a white precipitate, wash the white precipitate twice with deionized water and ethanol respectively, and then incubate at 80°C Dry it under vacuum for 24 hours to obtain a white flaky solid, and then grind it to obtain the ester group-cont...

Embodiment 3

[0038] The preparation method step of present embodiment containing ester group quaternary ammonium salt modified montmorillonite is as follows:

[0039] 1) Add 100mL of deionized water to a 250mL three-neck flask, then add 6.00g of montmorillonite powder, stir well to obtain a dispersion with a concentration of 60g / L, and calculate the ion exchange capacity (CEC) as 90mmol / 100g of montmorillonite , add C12 diester-based quaternary ammonium salt surfactant, gradually increase the temperature and stabilize it at 80°C, fully stir and condense and reflux for 3 hours to obtain a uniform white suspension;

[0040] 2) Ultrasonic disperse the above white suspension for 25min, then centrifuge at 11000r / min for 20min, remove the supernatant to obtain a white precipitate, wash the white precipitate with deionized water and ethanol three times respectively, and then incubate at 80°C Dry it under vacuum for 24 hours to obtain a white flaky solid, and then grind it to obtain the ester grou...

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Abstract

The invention relates to ester-containing quaternary ammonium salt modified montmorillonite and a preparation method thereof. The ester-containing quaternary ammonium salt modified montmorillonite is prepared by the following steps: 1) adding montmorillonite powder into deionized water, sufficiently stirring to obtain 30-60g / L dispersion liquid, adding an ester-containing quaternary ammonium salt surfactant, heating to 70-85 DEG C, sufficiently stirring and performing reflux condensation reaction for 2-4 hours to obtain uniform suspension; and 2) performing uniform ultrasonic dispersion of the suspension, performing centrifugal separation to remove supernatant liquid to obtain a precipitate, washing the obtained precipitate and drying to obtain a lamellar solid, and grinding to obtain the ester-containing quaternary ammonium salt modified montmorillonite. The method provided by the invention is easy to operate and can effectively open the interlamellar spacing of montmorillonite; and due to the ester group, the ester-containing quaternary ammonium salt modified montmorillonite has good organic compatibility and degradability.

Description

technical field [0001] The invention relates to the technical field of montmorillonite modification, in particular to an ester group-containing quaternary ammonium salt modified montmorillonite and a preparation method thereof. Background technique [0002] Montmorillonite is a kind of fine-grained clay, which can be used in textile, light industry, petroleum, metallurgy, desertification control, sewage treatment, biological supply, food, medicine and other industries. It is known as "universal material" because of its wide range of uses. . However, the performance of natural montmorillonite in practical applications is often not ideal, because of its strong hydrophilicity and poor organic compatibility, it needs to be modified to improve the performance and expand the application field. [0003] The most organic modification method of montmorillonite is surfactant modification, and cationic surfactant is often used. The modification mechanism is: exchangeable cations (main...

Claims

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Application Information

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IPC IPC(8): C09C1/42C09C3/08
Inventor 刘治田李洋张旗王成李超
Owner 河南天海合聚新材料有限公司
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