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Novel methods for producing type A molecular sieve film in current system

A molecular sieve and system technology, which is applied in the field of preparing A-type molecular sieve membranes, can solve the problems of difficulty in forming dense and continuous molecular sieve membranes, uneven crystallization on the surface of molecular sieve membranes, etc.

Inactive Publication Date: 2009-04-08
中科院嘉兴中心成都有机所分中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under normal hydrothermal synthesis conditions, as time progresses and crystals grow, the density of the sol in the bulk phase increases, and due to the effect of gravity, a large concentration gradient will be formed in the axial and radial directions of the reactor. , resulting in uneven crystallization on the surface of the molecular sieve membrane, making it difficult to form a dense and continuous molecular sieve membrane

Method used

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  • Novel methods for producing type A molecular sieve film in current system
  • Novel methods for producing type A molecular sieve film in current system
  • Novel methods for producing type A molecular sieve film in current system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: the preparation of NaA type molecular sieve membrane

[0018] Sodium silicate, sodium aluminate, sodium hydroxide and distilled water are used as raw materials to configure the precursor sol of NaA molecular sieve. The molar ratio of each component in the sol is: SiO 2 :Al 2 o 3 :Na 2 O:H 2 O=2:1:2:120, fully stirred and mixed evenly at room temperature. The two ends of the aluminum oxide film tube (commercially available, average pore diameter 1.5 μm, porosity 38%, outer diameter 13 mm, inner diameter 8 mm, length 350 mm) with NaA molecular sieve seed crystallization pre-coated with PTFE rods were fixed on the figure 1 in the synthesis reactor shown. After heating the molecular sieve precursor sol to 100°C in the raw material storage tank, pump it into the synthesis reactor at a speed of 30ml / min with a slurry pump. The outside of the synthesis reactor is wrapped with a heating belt, and the temperature is kept at 100°C. During the whole reaction pr...

Embodiment 2

[0019] Embodiment 2: Pervaporation separation performance of NaA molecular sieve membrane

[0020] figure 2 It is a schematic diagram of the molecular sieve membrane pervaporation separation device in the present invention. The molecular sieve membrane tube is placed in a stainless steel assembly, one end is connected to a small section of polytetrafluoroethylene rod, the other end is connected to a vacuum system, and the two ends are respectively sealed with a silicone rubber tube and a thermoplastic tube in turn, and the outside of the assembly is wrapped with a heating tape. The raw material liquid heated to a certain temperature in the constant temperature tank is circulated and supplied in the module through the liquid pump, and liquid N is used for permeating steam. 2 Condensation is recovered, and two cold traps are switched to ensure continuous measurement. The permeate collected by condensation is weighed with an electronic balance, and the concentrations of the ra...

Embodiment 3

[0022] Embodiment 3: NaA molecular sieve membrane is to THF / H 2 Pervaporation Separation of O System

[0023] THF is a very important organic solvent widely used in pharmaceutical, chemical, electronic and other industries. Due to the high price of THF, its separation and recovery are very important for the effective utilization of resources and environmental protection. THF and H 2 O forms an azeotropic composition when the content is 95 wt%, and the azeotropic point is 63.4°C. At present, the commonly used separation methods are azeotropic distillation and extractive distillation with salt addition, etc., which have high energy consumption, and the addition of entrainer and extractant will cause serious pollution to the environment and products. With 200ml of mixed solution containing THF 50wt% as raw material, the A-type molecular sieve membrane pervaporation method prepared in Example 1 is used to separate THF / H 2 O mixture, pervaporation separation results see image...

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Abstract

The invention provides a novel method for preparing an A-type molecular sieve membrane, which adopts preparation of the molecular sieve membrane in a flow system. The method comprises the following steps: a silicon source, an aluminum source, an alkali source and deionized water are prepared into precursor sol of A-type molecular sieve according to certain proportion first; a vector membrane tube which is precoated with A-type molecular sieve crystal seeds is fixed inside a synthesis reactor; the molecular sieve precursor sol which is heated to a given temperature is conveyed into the synthesis reactor through a slurry pump, and the precursor sol is driven to flow and circulate on the surface of an outer membrane of the vector membrane tube; and the A-type molecular sieve membrane can be obtained after flowing, circulating and crystallization for a definite time at the given temperature. The preparation method provided by the invention has the advantages that the preparation method can basically solve the problem of concentration gradient during the synthetic process of he molecular sieve, is favorable to the preparation of the uniform, continuous and compact molecular sieve membrane with superior separation performance, and is particularly suitable for preparing the molecular sieve membrane for industrial application.

Description

technical field [0001] The invention provides a new method for preparing A-type molecular sieve membrane in a flow system, and belongs to the technical field of inorganic membrane material preparation. Background technique [0002] Pervaporation (PV) is a new type of membrane separation technology, which is a new process with high efficiency, low energy consumption and low investment. Its separation principle is not limited by thermodynamic equilibrium, mainly depends on the interaction between the membrane and the permeate components, especially suitable for the separation of near-boiling point, azeotropic point mixtures and isomers that are difficult or impossible to separate by distillation . Compared with traditional rectification separation, pervaporation membrane separation can save energy by 1 / 2 to 1 / 3, the operating cost is 50% of the traditional distillation process, and can avoid product and environmental pollution, dehydration of organic solvents, The removal of...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D69/04
Inventor 张小明吕高孟雷骞索继栓
Owner 中科院嘉兴中心成都有机所分中心
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