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Method for preparing intercalation alpha-titanium phosphate through ion exchange method

An ion exchange method, titanium phosphate technology, applied in the field of green chemistry, can solve the problems of slow method, unable to complete the intercalation reaction, unable to take effect, etc., to achieve the effect of inhibiting hydrolysis

Active Publication Date: 2018-08-10
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method cannot be effective without the addition of organic amines, that is, the organic amine hydrochloride itself cannot complete the intercalation reaction
Whether it is the aqueous solution method of amine or the method of combining salt with amine, it is faced with the problem that the non-polarity of the amine is gradually increased, and it is difficult to dissolve in water. At this time, only the slow steam method can be used, which greatly reduces the production efficiency.

Method used

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  • Method for preparing intercalation alpha-titanium phosphate through ion exchange method
  • Method for preparing intercalation alpha-titanium phosphate through ion exchange method
  • Method for preparing intercalation alpha-titanium phosphate through ion exchange method

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Stir and mix butyl titanate and phosphoric acid solution (5-10mol / L) (Ti / P molar ratio is 1:38), transfer the mixed solution into a polytetrafluoroethylene-lined stainless steel reaction kettle, and put it in a constant temperature Dry in a drying oven at 180°C for 6 hours, cool to room temperature, centrifuge, fully wash until neutral, and dry at 70°C overnight to obtain the finished product of α-titanium phosphate.

Embodiment 2

[0019] In the phosphoric acid solution (5mol / L), add tetraethyl orthosilicate (containing an equal volume of absolute ethanol), CTAB and butyl titanate, the reaction temperature is 140°C, stir vigorously for 8h, cool to room temperature, centrifuge, and fully Wash until neutral, and dry at 70°C overnight to obtain the finished product of α-titanium phosphate. Among them, the molar ratio of butyl titanate, phosphoric acid, ethyl orthosilicate and CTAB is 1:4:3.93:0.018.

Embodiment 3

[0021] Add 0.05mol n-butylamine dropwise to 50ml phosphoric acid aqueous solution with a concentration of 0.538mol / L at 35°C, stir to prepare a solution with a pH value of 6.0-6.5 with an n-butylamine ion concentration of 1mol / L. Put 0.5 g of α-titanium phosphate powder into the above solution, stir and react at 50°C for 200 minutes, centrifuge after the reaction, wash the precipitate, dry at 70°C overnight, and pulverize to obtain α-titanium phosphate intercalated with n-butylamine. The product was measured by powder X-ray diffraction (XRD) and the proportion of completion of the intercalation reaction was measured, and the spectral position of the ammonium ion contained was observed by Fourier transform infrared spectroscopy (IR). The interlayer spacing of the intercalated α-titanium phosphate obtained by this method is calculated as 1.89nm according to the XRD spectrogram, and the intercalation completion ratio is 97.8%, and the ammonium ion is in the infrared spectrogram (a...

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Abstract

The invention provides a method for preparing intercalation alpha-titanium phosphate through an ion exchange method. The method comprises the following steps: adding a substance B, alpha-titanium phosphate and a solvent into a reactor; then stirring a mixed solution at 45 to 55 DEG C and reacting for 200 to 500min; after finishing reaction, centrifuging and washing sediment after the temperature is reduced to room temperature; drying to obtain the intercalation alpha-titanium phosphate, wherein the substance B is phosphate, phosphite, sulfite, malate or citrate of a substance A, the substanceA is organic amine or organic alkali and the organic amine or the organic alkali is n-butylamine, n-hexylamine, cyclohexylamine or pyridine. The method provided by the invention can finish intercalation reaction with relatively short time, the production efficiency is improved and the production cost is reduced.

Description

technical field [0001] The invention relates to the technical field of green chemistry. The intercalated alpha-titanium phosphate is prepared by ion exchange operation without additional additives. The method is simple, fast and versatile, and is suitable for industrial production. Background technique [0002] α-Titanium phosphate (α-TiP) is a typical cationic layered compound, which has a wide range of applications in adsorption, catalysis, and electrochemistry. α-titanium phosphate can realize ion exchange reaction by exchanging interlayer hydrogen ions with foreign guest cations, but due to the small interlayer distance, many large cations cannot directly enter the interlayer. The commonly used method is to bond organic bases such as amines (or alcohols, which are rare) to interlayer hydrogen ions through lone pair electrons on heteroatoms ( Acid-base neutralization reaction) is introduced into the interlayer, so that the guests such as amine can stay in the layered st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/372C01P2002/72C01P2002/82
Inventor 程庆彦王春扬王延吉
Owner HEBEI UNIV OF TECH
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