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CD (cyclodextrin) modified starch dye adsorbent and preparation method thereof

A technology of cyclodextrin and adsorbent, which is applied in the direction of chemical instruments and methods, adsorption water/sewage treatment, water pollutants, etc., can solve the problems of high cost, complicated operation, secondary pollution, etc., and achieve less equipment, The effect of simple preparation process and few adsorption conditions

Inactive Publication Date: 2018-12-14
TIANJIN POLYTECHNIC UNIV
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Problems solved by technology

[0004] The existing printing and dyeing wastewater treatment methods include adsorption method, precipitation method, flocculation method, redox method, solvent extraction method, etc., many of which have complex operation, high cost, or in the process of treatment Putting in the treatment agent causes problems such as secondary pollution, which limits its practical application

Method used

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  • CD (cyclodextrin) modified starch dye adsorbent and preparation method thereof
  • CD (cyclodextrin) modified starch dye adsorbent and preparation method thereof
  • CD (cyclodextrin) modified starch dye adsorbent and preparation method thereof

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preparation example Construction

[0025] The present invention simultaneously designs the preparation method (abbreviation preparation method) of γ-cyclodextrin immobilized starch, the preparation method adopts the raw material mass fraction composition and process steps of γ-cyclodextrin immobilized starch of the present invention: corn starch 100 parts; 1000 parts of NaCl aqueous solution (wNaCl%=2.5); 15 parts of γ-CD; 10 parts of ECH.

[0026] (1) Make the cornstarch and NaCl aqueous solution of the stated number into a starch suspension, transfer it to a three-necked flask, and adjust the pH to 10 with 30% NaOH solution. Then add the said number of ECH (drip three times during the reaction), turn on the condensing reflux device, and continue the reaction at 50°C for 6h.

[0027] (2) After the reaction, cool to room temperature, adjust the pH to 6.5-7 with 3N hydrochloric acid solution, precipitate the product with absolute ethanol, and centrifuge to obtain the crude product. Then centrifuge and wash with...

Embodiment 1

[0036] (1) 10g of corn starch is dispersed in 100mL NaCl aqueous solution (w NaCl %=2.5), then add 1.5g γ-CD, adjust pH=10 with 30% NaOH solution. Then a certain amount of ECH was added (dropped three times during the reaction), and the reaction was continued at 50° C. for 6 h.

[0037] (2) After the reaction, cool to room temperature, adjust the pH to 6.5-7 with 3N hydrochloric acid solution, then precipitate the product with 100 mL of absolute ethanol, and centrifuge to obtain the crude product. Then centrifuge and wash three times with 65 / 35 ethanol aqueous solution, vacuum-dry at 50° C., grind and pulverize to obtain CS-γCD.

[0038] Immobilization effect test: refer to the determination method of CS-γCD substitution degree in the previous section to determine relevant parameters. The calculated substitution degree and carboxyl content data in this example are listed in Table 1, and the structural characterization can be found in figure 1 , figure 2 and image 3 .

Embodiment 2

[0040] (1) 10g of corn starch is dispersed in 100mL NaCl aqueous solution (w NaCl %=2.5), then add 1.5g γ-CD, adjust pH=11 with 30% NaOH solution. Then a certain amount of ECH was added (dropped three times during the reaction), and the reaction was continued at 50° C. for 6 h.

[0041] (2) After the reaction, cool to room temperature, adjust the pH to 6.5-7 with 3N hydrochloric acid solution, then precipitate the product with 100 mL of absolute ethanol, and centrifuge to obtain the crude product. Then centrifuge and wash three times with 65 / 35 ethanol aqueous solution, vacuum-dry at 50° C., grind and pulverize to obtain CS-γCD.

[0042] The degree of substitution and reaction efficiency calculated in this embodiment are listed in Table 1.

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Abstract

The invention discloses a natural polymer adsorbent, namely, a gamma-CD (cyclodextrin) immobilized starch adsorbent. The adsorbent is characterized in that starch comprises raw materials by mass as follows: 100 parts of corn starch, 1000 parts of aqueous NaCl solution (wNaCl%=2.5), 15 parts of gamma-CD and 10 parts of ECH. The invention also provides a preparation method of the starch adsorbent. The method adopts the raw material mass composition of the gamma-CD immobilized starch and comprises the following process steps: (1) a starch suspension is prepared from the corn starch and the aqueous NaCl solution in parts and transferred into a three-neck flask, and pH is regulated by a 30% NaOH solution to be 10; then ECH in parts is added (dropwise three times in a reaction process), a refluxcondensation device is connected, and a continuous reaction is performed at 50 DEG C for 6 h; (2) after the reaction, a product is cooled to room temperature, pH is regulated by a 3N hydrochloric acid solution to be 6.5-7, the product is precipitated with absolute ethyl alcohol, and a crude product is obtained by centrifugal separation; the crude product is washed centrifugally three times with 65 / 35 ethanol water, dried in vacuum at 50 DEG C, ground and crushed, and gamma-CD immobilized starch, namely, CS-gamma CD is obtained.

Description

[0001] A method for preparing and using a γ-cyclodextrin-immobilized starch (CS-γCD) dye adsorbent. technical field [0002] The invention relates to the application of modified natural starch in the purification of printing and dyeing wastewater, belonging to the technical field of textile materials. Background technique [0003] Today, with the accelerated process of industrialization and increasing population, China has developed into a major printing and dyeing country. More than 100,000 tons of dye wastewater is discharged directly into the environment without treatment. These water bodies are difficult to rely on the environment for self-healing, and the structure is very stable, which not only destroys the ecological balance of the water body, but also has carcinogenic and teratogenic consequences for aquatic organisms and humans. Therefore, it has become an urgent problem to be solved in the current environmental governance to purify the printing and dyeing wastewat...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F103/30
CPCB01J20/24C02F1/286C02F2101/308C02F2103/30
Inventor 张昊李雅兴张毅李帆孙侨曼
Owner TIANJIN POLYTECHNIC UNIV
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