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Preparation method of porous aluminum phosphate block

A technology of aluminum phosphate block and phosphoric acid, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry and other directions, can solve the problems that do not involve the preparation of aluminum phosphate block materials, etc., and achieve the effects of low equipment and simple process

Active Publication Date: 2014-03-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the aluminum phosphate prepared by these methods is only aimed at its molecular sieve system, that is, aluminum phosphate itself, and does not involve the preparation of aluminum phosphate block materials with a co-continuous porous structure.

Method used

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  • Preparation method of porous aluminum phosphate block

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1. A method for preparing a porous aluminum phosphate block, using aluminum chloride hexahydrate as an aluminum source, phosphoric acid as a phosphorus source, a mixture of deionized water and anhydrous methanol as a solvent, and propylene oxide as a condensate Adhesive accelerator, polyethylene oxide (average molecular weight 1×10 4 ) is a phase separation inducer; the following steps are carried out in sequence:

[0023] 1) Put 1.0g of aluminum chloride hexahydrate and 46mg of polyethylene oxide into the reaction bottle, add 1.0ml of deionized water, 1.0ml of anhydrous methanol and 0.3ml of phosphoric acid in turn, and stir until the polyethylene oxide (PEO) completely dissolved;

[0024] 2) Under ice bath conditions, evenly mix 2.00ml of propylene oxide into the solution obtained in the above step 1), and continue to stir vigorously (rotating at 400 rpm) until the propylene oxide is completely dissolved;

[0025] 3) Seal the reaction bottle and place it ...

Embodiment 2

[0030] Change the amount of propylene oxide in Step 2) of Example 1 from 2.00ml to 2.50ml; the rest is the same as Example 1.

[0031] In this embodiment 2, with respect to embodiment 1, the addition amount of PEO is kept constant, and the amount of propylene oxide (PO) is increased to 2.50ml. The porous aluminum phosphate block prepared in Example 2 began to form a bicontinuous pore structure, and the amount of PEO added was sufficient to cause phase separation of the sample, but the pores inside the sample were not uniform, and some pores were discontinuous. This is due to the fact that the gel time is earlier than the phase separation time due to the increase of PO addition, resulting in the formation of a porous structure with independent pores distributed on the continuous gel phase inside the sample. The sample is macroscopically opaque. According to the pore size distribution diagram of mesopores, the specific surface area (BET) = 39m 2 / g, total pore volume=0.12cc / g....

Embodiment 3

[0034] Change the amount of polyethylene oxide used in step 1) of Example 1 from 46 mg to 44 mg; the rest is the same as in Example 1.

[0035] Example 3 is compared with Example 1, the PO content is kept constant, and the amount of PEO is changed to 44 mg. The SEM photos show that the interior does not form a porous structure, and it is still a flocculent aluminum phosphate aggregate. It should be that the addition of PEO is too small, resulting in phase separation later than the gel. The macroscopic appearance of the sample is translucent, not pure white. According to the pore size distribution diagram of mesopores, the specific surface area (BET) = 37m 2 / g, total pore volume=0.03cc / g. Large pores basically do not exist, and the pore size is mainly distributed in the range of 200-300nm; the bulk density of the block is 1.24g / cm 3 ; The porosity is 35.6%.

[0036] It was concluded that reducing the amount of polyethylene oxide would reduce the pore size and form a nanopo...

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Abstract

The invention discloses a preparation method of a porous aluminum phosphate block. According to the preparation method, aluminum chloride hexahydrate is taken as an aluminum source, phosphoric acid is taken as a phosphorus source, a mixture of deionized water and absolute methanol is taken as a solvent, propylene epoxide is taken as a gel accelerator, and polyoxyethylene is taken as a phase separation inductive agent; the following steps are sequentially performed: 1), aluminum chloride hexahydrate and polyoxyethylene are put in a reaction flask, deionized water, absolute methanol and phosphoric acid are doped, and stirring is performed until polyoxyethylene is dissolved completely; 2), under the condition of ice bath, propylene epoxide is doped into a solution obtained in step 1), stirring is continuously performed until propylene epoxide is dissolved completely; 3), the reaction flask is sealed and aged, then a lid is opened, and drying is performed; and 4), obtained xerogel is processed for 1.5-2.5 hours at the temperature of 1,050-1,150 DEG C so as to obtain the porous aluminum phosphate block. The porous aluminum phosphate block can be directly applied to the fields of catalysis, separation, absorption, extraction, degradation, curing and the like.

Description

technical field [0001] The invention relates to a method for preparing a porous aluminum phosphate block, in particular to a method for preparing a porous aluminum phosphate block by a wet chemical method. Background technique [0002] Aluminum phosphate, as a catalyst carrier and molecular sieve, is composed of aluminum-oxygen polyhedron and phosphorus-oxygen tetrahedron. Because of its high specific surface area, good thermal stability and unique surface acid-base characteristics, it has attracted widespread attention. Especially in terms of being used as a catalyst carrier, it has demonstrated superior characteristics, and the incorporation of transition metals into the aluminum phosphate skeleton can also be applied to the oxidation reaction of alkanes, cycloalkanes and phenols. [0003] The synthesis method of aluminum phosphate molecular sieve mainly adopts the hydrothermal synthesis method. Various synthetic methods such as in-system synthesis. At the same time, in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/36
Inventor 郭兴忠杨辉徐晨阳李文彦王应恺
Owner ZHEJIANG UNIV
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