Synthetic method of 4A molecular sieve

A synthesis method and molecular sieve technology, applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems that do not conform to the development trend of modern green chemical industry, affect the utilization rate of silicon-aluminum species, and seriously pollute the environment , to achieve excellent physical and chemical properties, less pollution, and lower energy consumption

Inactive Publication Date: 2014-12-17
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current activation methods are mainly high-temperature roasting (about 800-1000°C) or alkali-fusion roasting (about 600-800°C). The activation process has high energy consumption, serious environmental pollution, and does not conform to the development trend of modern green chemical industry.
In addition, although high-temperature roasting can activate natural minerals, the activation effect is not good, especially the Si-O bonds in minerals are extremely difficult to be destroyed, which affects the utilization of silicon-aluminum species.

Method used

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  • Synthetic method of 4A molecular sieve
  • Synthetic method of 4A molecular sieve
  • Synthetic method of 4A molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Commercially available kaolin is dried and pulverized into powder (the present invention has no specific requirements on the degree of pulverization, usually pulverized until passing through a 20-mesh sieve). Weigh 10.00g of kaolin powder, mix evenly with 84.00g of sodium hydroxide solution, dry at 200°C, and set aside. Wherein the sodium hydroxide solution is prepared by dissolving 14.00 g of sodium hydroxide solid in 70.00 g of deionized water.

[0042] Weigh 10.44 g of the above dried kaolin powder, add 54.91 g of deionized water, and mix and stir at 40° C. for 12 h. The mixture was poured into a polytetrafluoroethylene-lined stainless steel crystallization kettle, heated to 90°C for static crystallization for 2 h. After the crystallization is completed, cool and filter to remove the mother liquor, wash until neutral, and dry at 120°C to obtain a crystallized product. As determined by XRD, its phase belongs to 4A molecular sieve, the whiteness of 4A molecular sieve...

Embodiment 2

[0044] The pretreatment method of kaolin is with embodiment 1.

[0045] Weigh 8.70 g of the above dried kaolin powder, add 51.48 g of deionized water, and mix and stir at 20° C. for 4 h. The mixture was poured into a stainless steel crystallization kettle lined with polytetrafluoroethylene, heated to 100°C for static crystallization for 6h. After the crystallization is completed, cool and filter to remove the mother liquor, wash until neutral, and dry at 120°C to obtain a crystallized product. As determined by XRD, its phase belongs to 4A molecular sieve, the whiteness of 4A molecular sieve in the product is 92, and the calcium ion exchange capacity is 312mg CaCO 3 / g molecular sieve, its XRD spectrum is shown in image 3 .

Embodiment 3

[0047] The pretreatment method of kaolin is with embodiment 1.

[0048] Weigh 16.73 g of the above dried kaolin powder, add 43.93 g of deionized water, and mix and stir at 60° C. for 8 h. The mixture was poured into a stainless steel crystallization kettle lined with polytetrafluoroethylene, heated to 100°C for static crystallization for 4 hours. After the crystallization is completed, cool and filter to remove the mother liquor, wash until neutral, and dry at 120°C to obtain a crystallized product. According to XRD determination, its phase belongs to 4A molecular sieve, the whiteness of 4A molecular sieve in the product is 94, and the calcium ion exchange capacity is 320mg CaCO 3 / g molecular sieve, its XRD spectrum is shown in Figure 4 .

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Abstract

Provided is a 4A-type molecular sieve synthesis method, comprising: utilizing natural clay mineral to provide all silicon sources and aluminum sources required for molecular sieve synthesis; and after activation, crystallizing the natural clay mineral under a hydrothermal condition to synthesize a 4A-type molecular sieve. The method of the present invention has a simple process and uses inexpensive raw material, and prepares a 4A-type molecular sieve with whiteness being greater than 90%, the calcium ion exchange capacity being not less than 310 mg CaCO3 / g molecular sieve. The present invention enlarges the range of raw materials for preparing molecular sieve material, and the sub-molten salt activation method greatly reduces the production cost of a molecular sieve, and significantly improves greenness of the production process of the molecular sieve material.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis, and in particular relates to a method for synthesizing 4A molecular sieves, in which natural clay minerals activated by sub-molten salts are used as raw materials to provide all silicon and aluminum sources required for synthesizing 4A molecular sieves. Background technique [0002] NaA type molecular sieve, the ideal unit cell composition is Na 96 [(Al 96 Si 96 )O 384 ]·216H 2 O, cubic crystal system, space group Fm-3c, unit cell parameter a=24.61 . The skeleton structure of NaA molecular sieve is that the β cages are placed on the eight vertices of the cube, and they are connected by double four-membered rings, so that an α cage is surrounded by eight β cages, and the α cage is connected with the eight-membered ring. Adjacent α cages are connected, and the eight-membered ring is the main channel of the NaA molecular sieve, with a pore size of 4.2 , so NaA molecular sieve is als...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/18
CPCC01B39/18
Inventor 鲍晓军岳源源李铁森刘海燕石冈杨金彪
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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