Zeolite membrane, its production method, and separation method using the zeolite membrane

A separation method and zeolite membrane technology, applied in separation methods, semi-permeable membrane separation, dispersed particle separation, etc., can solve the problems of low processing capacity and long separation operation, and achieve excellent acid resistance, high separation performance and processing capacity. , the effect of suppressing the formation of pinholes

Active Publication Date: 2019-12-06
HITACHI ZOSEN CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, when the zeolite membrane having the CHA type crystal structure obtained in this method is intended to be used as a separation membrane, for example, when separately recovering acetic acid or 2-propanol from a water / acetic acid mixture or a water / 2-propanol mixture , due to the low permeation flux (mass of the permeate per unit time and unit area) and the small amount of treatment, there is a problem that it takes a long time for the separation operation

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  • Zeolite membrane, its production method, and separation method using the zeolite membrane
  • Zeolite membrane, its production method, and separation method using the zeolite membrane
  • Zeolite membrane, its production method, and separation method using the zeolite membrane

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preparation example Construction

[0049] According to the preparation method of the present invention, for the zeolite membrane with the CHA type crystal structure formed into a film on the intermediate layer of the porous support with the intermediate layer, the Si / Al (molar ratio) of the CHA type zeolite particles is 9.5~100.5, preferably 10 to 100, more preferably 20 to 80, in the X-ray diffraction pattern obtained by irradiating the surface of the zeolite membrane with X-rays, the peak intensity near 2θ=18° is less than 0.5 times the peak intensity near 2θ=21°, Preferably less than 0.4 times, more preferably less than 0.35 times, most preferably less than 0.25 times, the peak intensity around 2θ=10° is less than 4 times of the peak intensity near 2θ=21°, preferably less than 3 times, more preferably less than 2.5 times, most preferably Preferably less than 0.2 times. The lower limit of (peak intensity around 2θ=18°) / (peak intensity around 2θ=21°) is not limited, and is usually 0.1. The lower limit of (pea...

Embodiment 1

[0065]

preparation example 1

[0068] A cylindrical alumina support (manufactured by Hitachi Zosen, 16 mm in diameter, 60 mm in length, and 10 μm in average pore diameter) with an intermediate layer (thickness about 50 μm, average pore diameter 0.8 μm) on the surface was prepared, and 25 g of / m 2 A CHA-type zeolite was attached as a seed crystal. The average pore diameter of the intermediate layer was measured in accordance with JIS K 3832.

[0069] Using FAU-type zeolite as raw material and N,N,N-trimethyl-1-adamantyl ammonium hydroxide (TMAdaOH) as an organic template, seed crystals were prepared in advance by the following method.

[0070] First, 8.09 g of TMAdaOH aqueous solution (manufactured by SACHEM, 25% by weight) was added to a 50 ml beaker, 0.38 g of sodium hydroxide was added, and the whole was stirred for 5 minutes. Thereafter, 2.1 g of HSZ-360 and 0.9 g of HSZ-390 (manufactured by TOSOH) were added as FAU-type zeolites, respectively, and stirred for 15 minutes. The molar composition of eac...

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Abstract

An object of the present invention is to provide a zeolite membrane which, in separation by the zeolite separation membrane, not only has both practically high enough separation performance and throughput, but also maintains stable separation performance over a long period of time. The Si / Al (molar ratio) of CHA-type zeolite particles is 9.5 to 100.5, and in the X-ray diffraction pattern obtained by irradiating the surface of the zeolite membrane with X-rays, the peak intensity around 2θ=18° is smaller than the peak around 2θ=21° 0.5 times the intensity, and / or the peak intensity around 2θ=10° is less than 4 times the peak intensity around 2θ=21°. When using an aqueous reaction mixture containing Si element source, Al element source, alkali source and organic template to form a zeolite membrane with a CHA-type crystal structure on the middle layer of a porous support by hydrothermal synthesis, use an undealuminized The treated FAU-type zeolite is used as a Si element source and an Al element source.

Description

technical field [0001] The present invention relates to a zeolite membrane, its preparation method and a separation method using the zeolite membrane. The zeolite membrane of the present invention can separate and recover target compounds with high separation performance and throughput, and is especially suitable for dehydration from organic acids containing water and other organic compounds. Background technique [0002] Zeolite has regularly arranged micropores, and usually a zeolite with high heat resistance and stable chemical properties can be obtained in large quantities, so it is used in various fields. Zeolite is an aluminum silicate salt in which a part of Si is replaced by Al. It has fine pores with a molecular order (0.3-1 nm) of an oxygen eight-membered ring to a fourteen-membered ring, and has stereoselective adsorption, so it can be widely used It is used in fields such as liquid separation, steam separation, gas separation, membrane reactor, solid acid cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D69/10B01D69/12B01D71/02C01B39/48
CPCB01D69/10B01D69/12C01B39/48B01D53/22B01D67/0051C01B39/026B01D2256/24B01D2256/245B01D2257/504B01D2257/80B01D2323/12B01D2323/24C01P2004/62C01P2004/64B01D71/028B01J20/18B01J20/3238Y02C20/40Y02P20/151B01D53/228
Inventor 今坂怜史板仓正也长谷川泰久佐藤刚一
Owner HITACHI ZOSEN CORP
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