CN103657594A - Preparation method of tiny hole type multihole clay heterogeneous material - Google Patents

Abstract

The invention discloses a preparation method of a micro-hole type multihole clay heterogeneous material. The method comprises the following steps: uniformly mixing tetraethoxysilane and diphenyl dimethyldiethoxylsilane at a mass ratio of 1:(0.1-100) to form a mixing solution; fully uniformly mixing lauryl amine, organobentonite and the mixing solution at a mass ratio of (1-40);1:120 to obtain a front body solution; carrying out water bath reaction on the front body solution at 30-70 DEG C for 6-18 hours, carrying out suction filtration, naturally blowing or drying the obtained solid, placing the solid in a muffle furnace at 450-650 DEG C, and calcining for 2-6 hours to obtain the micro-hole type multihole clay heterogeneous material. The prepared material provided by the invention has the advantages that the adsorptive property of an indoor organic pollutant is better than that of the PCH material synthetized by the traditional method, and the material has wide application prospect.

Description

A kind of preparation method of pore type adobe isomery material

Technical field

The invention belongs to adsorbent technical field, be specifically related to a kind of preparation method of pore type adobe isomery material.

Background technology

Room air pollution serious harm human health, its purification techniques is subject to people and more and more pays close attention to.Absorption method has that efficiency is high, cost is low, nonhazardous, the advantage such as be easy to commercially produce, and is widely used in indoor air purification.Wherein common sorbing material has active carbon and molecular sieve etc., and active carbon is usually used in removing hydrophobic organic pollutant, but is difficult to effectively remove polarity organic pollution.Molecular sieve can be used for adsorption cleaning hydrophily organic pollution, but cost is high.Adobe isomery material (being called for short PCH) is a kind of porous material of surface hydrophilic, can be used for adsorption cleaning hydrophily organic pollution, and cost is significantly lower than molecular sieve.But traditional PCH material is as a kind of mesopore sorbing material (aperture >2nm), its adsorption effect to light concentration organic pollutant in room air is difficult to reach real requirement, thereby need to develop the abundant novel PC H material of micropore (aperture <2nm).

Summary of the invention

For solving the few deficiency of conventional P CH micro content, the present invention adopts diphenyl diethoxy silane as pore former, and low temperature has synthesized and contained the novel PC H material that enriches micropore.

The inventive method comprises the following steps:

Step (1). in bentonite, add softex kw to mix, obtain organobentonite; The addition of softex kw is one times of bentonite cation exchange capacity (CEC) CEC;

Step (2). by ethyl orthosilicate with diphenyl diethoxy silane by 1:(0.1～100) mass ratio mix formation mixed liquor;

Step (3). the mixed liquor that the synthetic organobentonite of lauryl amine, step (1) and step (2) are obtained fully mixes by the mass ratio of (1～40): 1:120, obtains precursor solution;

Step (4). the precursor solution that step (3) is obtained after 30～70 ℃ of water-bath 6～18h hours and suction filtration, the solid natural air drying or the oven dry that obtain;

Step (5). the drying solid that step (4) is obtained is put into 450～650 ℃ of calcining 2～6h of Muffle furnace and is obtained micropore PCH material.

The present invention adopts diphenyl diethoxy silane as pore former, makes the material micropore size <2nm that finally prepares, can reach better the adsorption effect of light concentration organic pollutant in room air.

Material prepared by the present invention all has obvious lifting than conventional P CH material in the parameters such as aperture, specific area, micropore specific area, and the adsorption capacity of low concentration pollutant is significantly strengthened.

The synthetic material of the present invention can be applicable to indoor air purification, for example: the material of take is prepared clean air package as core, is installed on air purifier, can effectively remove the pollutant producing as finishing, smoking etc.; Be installed on air-conditioning equipment, can realize in the process of Air conditioner air exchange and remove indoor pollutant, effectively reduce the indoor healthy risk causing due to new wind deficiency; Material preparation is become to coating, can realize the adsorption cleaning to being indoor air pollutants.This materials'use place is extensive, and as indoor in resident, hospital, school and factory etc., be with a wide range of applications in light concentration gas field of purification.

Accompanying drawing explanation

Fig. 1 is the pore-size distribution comparison diagram of the prepared micropore PCH material of embodiment 1 and conventional P CH material.

The specific embodiment

Below in conjunction with the drawings and specific embodiments, the present invention is further analyzed.

Comparative example.

2g organobentonite and 40g lauryl amine are mixed, and 50 ℃ are stirred 30min; 240g ethyl orthosilicate is added, and 35 ℃ are stirred 12h; Gained solid natural air drying after suction filtration; Muffle furnace is with 2 ℃/min temperature programming to 600 ℃, and keeps obtaining conventional P CH material after 4h, is designated as PCH0.

Embodiment 1.

180g ethyl orthosilicate and 60g diphenyl diethoxy silane are mixed to formation 240g mixed liquor, 2g organobentonite and 40g lauryl amine are mixed, 50 ℃ are stirred 30min, then add 240g mixed liquor, and 35 ℃ are stirred 12h; Gained solid natural air drying after suction filtration; Muffle furnace is with 2 ℃/min temperature programming to 600 ℃, and keeps obtaining micropore PCH material after 4h, is designated as PCH25.

As shown in table 1, Fig. 1, the specific area of PCH25 and micropore specific area are all greater than PCH0; PCH25 compares with PCH0, and its micro content significantly increases, and mesopore content obviously reduces, and illustrates that the absorption potential of PCH25 is than the obvious enhancing of PCH0.

Specific area and the micropore specific area of the different PCH sorbing materials of table 1

Sorbing material	Specific area m 2g -1	Micropore specific surface m 2g -1
			PCH0	855	732
PCH25	963	875

Embodiment 2.

120g ethyl orthosilicate and 120g diphenyl diethoxy silane are mixed to formation 240g mixed liquor, 2g organobentonite and 40g lauryl amine are mixed, 50 ℃ are stirred 30min, then add 240g mixed liquor, and 35 ℃ are stirred 12h, obtain precursor solution; By gained solid natural air drying after precursor solution suction filtration; Muffle furnace is with 2 ℃/min temperature programming to 600 ℃, and keeps obtaining micropore PCH material after 600 ℃ of calcining 4h.

Embodiment 3.

60g ethyl orthosilicate and 180g diphenyl diethoxy silane are mixed to formation 240g mixed liquor, 2g organobentonite and 40g lauryl amine are mixed, 70 ℃ are stirred 30min, then add 240g mixed liquor, and 35 ℃ are stirred 12h, obtain precursor solution; By 70 ℃ of oven dry of gained solid after precursor solution suction filtration; Muffle furnace is with 2 ℃/min temperature programming to 600 ℃, and keeps obtaining micropore PCH material after 600 ℃ of calcining 4h.

Embodiment 4.

218.2g ethyl orthosilicate and 21.8g diphenyl diethoxy silane are mixed to formation 240g mixed liquor, 2g organobentonite and 2g lauryl amine are mixed, 50 ℃ are stirred 30min, then add 240g mixed liquor, and 35 ℃ are stirred 12h, obtain precursor solution; By gained solid natural air drying after precursor solution suction filtration; Muffle furnace is with 2 ℃/min temperature programming to 450 ℃, and keeps obtaining micropore PCH material after 450 ℃ of calcining 6h.

Embodiment 5.

2.4g ethyl orthosilicate and 237.6g diphenyl diethoxy silane are mixed to formation 240g mixed liquor, 2g organobentonite and 80g lauryl amine are mixed, 70 ℃ are stirred 30min, then add 240g mixed liquor, and 35 ℃ are stirred 12h, obtain precursor solution; By 70 ℃ of oven dry of gained solid after precursor solution suction filtration; Muffle furnace is with 2 ℃/min temperature programming to 650 ℃, and keeps obtaining micropore PCH material after 650 ℃ of calcining 2h.

Above-described embodiment organobentonite used is in bentonite, to add softex kw to mix to form; The addition of softex kw is one times of bentonite cation exchange capacity (CEC) CEC.

Above embodiment is only described further invention, and scope of the present invention is not limited to by illustrated embodiment.

Claims (1)

1. a preparation method for pore type adobe isomery material, is characterized in that the method comprises the following steps:

Step (1). in bentonite, add softex kw to mix, obtain organobentonite; The addition of softex kw is one times of bentonite cation exchange capacity (CEC) CEC;

Step (2). by ethyl orthosilicate with diphenyl diethoxy silane by 1:(0.1～100) mass ratio mix formation mixed liquor;

Step (3). the mixed liquor that the synthetic organobentonite of lauryl amine, step (1) and step (2) are obtained fully mixes by the mass ratio of (1～40): 1:120, obtains precursor solution;

Step (4). the precursor solution that step (3) is obtained after 30～70 ℃ of water-bath 6～18h hours and suction filtration, the solid natural air drying or the oven dry that obtain;

Step (5). the drying solid that step (4) is obtained is put into 450～650 ℃ of calcining 2～6h of Muffle furnace and is obtained pore type adobe isomery material.

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