Carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material and preparation method thereof

A cyclodextrin polymer, carboxymethyl technology, applied in the directions of iron oxide/iron hydroxide, cobalt oxide/cobalt hydroxide, etc., to achieve the effects of high reusability, simple and easy preparation method, and easy realization

Inactive Publication Date: 2014-09-24
ZIBO VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] At present, there are no literature and patent reports about the direct polymerization of

Method used

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  • Carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material and preparation method thereof
  • Carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material and preparation method thereof
  • Carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Step A: take by weighing 11.64g Co(NO 3 ) 2 ﹒ 6H 2 O, 8.08g Fe(NO 3 ) 3 ﹒ 9H 2 Dissolve O in 100ml to remove CO 2 Prepare a mixed salt solution in deionized water, and dissolve another 5.60g NaOH in 50ml to remove CO 2 Alkaline solution prepared in deionized water, at room temperature N 2 Protection Add the mixed salt solution and alkali solution into the four-necked flask by double-drop method, and stir at a stirring speed of 600 rpm. Adjust the pH value to 8 with 0.2mol / L NaOH solution. The resulting slurry was crystallized at 60 °C for 72 h, then the precipitate was filtered, and the CO 2 Washing with water several times until the pH of the washing solution = 7, the hydrotalcite precursor NO 3 -LDHs, whose Co 2+ / Fe 3+ =2.

[0040] Step B: Dissolve 1.0 g of carboxymethyl-β-cyclodextrin (CMCD) solid in 100 mL to remove CO 2 After the deionized water is transferred to the four-necked bottle, add the hydrotalcite precursor NO which is filled with 15.0g st...

Embodiment 2

[0045] Step A: Weigh 9.52g CoCl 2 ﹒ 6H 2 O, 5.40g FeCl 3 ﹒ 6H 2 Dissolve O in 100ml to remove CO 2 deionized water to prepare a mixed salt solution, and another 8.00g NaOH was dissolved in 50ml to remove CO 2 Prepare alkaline solution in water, N at room temperature 2 Protection: Add the salt solution and the alkali solution into the four-necked flask by the double-drop method, and stir at 600 rpm. Adjust the pH value to 10 with 1.0mol / L NaOH solution. The resulting slurry was crystallized at 80 °C for 24 h, then the precipitate was filtered, and the CO 2 Washing with water several times until the pH of the washing solution = 7, the hydrotalcite precursor Cl-LDHs, its Co 2+ / Fe 3+ =2.

[0046] Step B: Dissolve 1.0 g of carboxymethyl-β-cyclodextrin (CMCD) solid in 100 mL to remove CO 2 Transfer the deionized water into the four-necked bottle, and then add the hydrotalcite precursor Cl-LDHs obtained in step A containing 14.0g, N 2 Protected and heated to 80°C, react...

Embodiment 3

[0051] Step A: take by weighing 11.64g Co(NO 3 ) 2 ﹒ 6H 2 O,5.37g Fe(NO 3 ) 3 ﹒ 9H 2 Dissolve O in 100ml to remove CO 2 deionized water to prepare a mixed salt solution, and another 5.60g NaOH was dissolved in 50ml to remove CO 2 Prepare alkaline solution in water, N at room temperature 2Protection The salt solution and the alkali solution were added into the four-necked flask by the double-drop method, and stirred at a stirring speed of 600 rpm. Adjust the pH value to 9 with 0.5mol / L NaOH solution. The resulting slurry was crystallized at 70 °C for 48 h, then the precipitate was filtered, and the CO 2 Washing with water several times until the pH of the washing solution = 7, the hydrotalcite precursor NO 3 -LDHs, whose Co 2+ / Fe 3+ =3.

[0052] Step B: Dissolve 1.0 g of carboxymethyl-β-cyclodextrin (CMCD) solid in 100 mL to remove CO 2 After the deionized water is transferred to the four-necked bottle, then add the hydrotalcite precursor NO which is filled with...

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Abstract

The invention relates to the field of organic-inorganic composites and in particular relates to a carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material and a preparation method thereof. The hydrotalcite material is prepared by the steps of preparing carboxymethyl modified beta-cyclodextrin intercalated cobalt-iron hydrotalcite, fully mixing the hydrotalcite and epichlorohydrin under the condition of strong alkaline, and then carrying out polymerization reaction on interlayer cyclodextrin and the epichlorohydrin to obtain the carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material. A chemical formula of the carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite material is [(Co<2+>)1-x(Fe<3+>)x(OH)2]<x+>(CMCDP<n->)x/n.mH2O, wherein x is equal to 0.25-0.33, m is equal to 3-6 and is an amount of interlayer crystal water molecules, and n is equal to 25-50 and is an amount of negative charges carried by carboxymethyl-beta-cyclodextrin polymer. Compared with monomer cyclodextrin intercalated hydrotalcite, the carboxymethyl-beta-cyclodextrin polymer intercalated hydrotalcite has the advantages of more convenience, stronger stability, higher repeated utilization ratio, larger application range and the like. The preparation method is simple and feasible and is easy to realize.

Description

technical field [0001] The invention relates to the field of organic-inorganic composite materials, in particular to a carboxymethyl-β-cyclodextrin polymer intercalated hydrotalcite material and a preparation method thereof. Background technique [0002] Hydrotalcite (Layered Double Hydroxides, referred to as LDHs), is a class of anionic layered materials, and its chemical composition is [M 2+ 1-x m 3+ x (OH) 2 ] x+ (A n– ) x / n mH 2 O. The material is composed of mutually parallel laminae with a permanent positive charge. m 2+ ,M 3+ That is, divalent and trivalent metal cations with exchangeable anions A between the layers n- to maintain charge balance. The interlayer elements of hydrotalcite have strong covalent bonds, the interlayer anions and the laminates attract each other with electrostatic attraction, and the whole crystal is electrically neutral. Due to the controllability of layered metal ions and interlayer anions, hydrotalcite materials have been wid...

Claims

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Application Information

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IPC IPC(8): C01G51/04C01G49/02
Inventor 刘晓磊
Owner ZIBO VOCATIONAL INST
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