Stable synthetic method for TON zeolite

A synthesis method and zeolite technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve problems such as unfavorable industrial production, and achieve the effects of reducing reaction severity, improving synthesis success rate, and reducing production cost

Active Publication Date: 2017-06-16
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this also puts forward high requirements on the stirring material of the reactor, which is not conducive to the actual industrial production.

Method used

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  • Stable synthetic method for TON zeolite
  • Stable synthetic method for TON zeolite
  • Stable synthetic method for TON zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Obtaining Mother Liquor of Primary Crystallization of TON Zeolite

[0038] Refer to the synthesis method of US5783168 patent to prepare TON zeolite molecular sieve, and to recover the mother liquor by primary filtration.

[0039] The specific operation is as follows: under stirring conditions, 0.38g Al 2 (SO 4 ) 3 18H 2 O was dissolved in 30g of water, then 0.9g of KOH was added, and a clear solution A was formed after fully stirring; 2.5g of 1,6-hexanediamine (DAH) was weighed and added to solution A. 10g silica sol (containing SiO 2 30% by mass), after stirring, a uniform gel B is formed; its specific composition is (molar ratio) SiO 2 : 1.00Al 2 o 3 : 14.00K 2 O: 38.60DAH: 3610H 2 O=88.00:1.00:14.00:38.60:3610.

[0040] The gel B was transferred to a 100 mL stainless steel reactor with a polytetrafluoroethylene liner, and the hydrothermal reaction was carried out at 160 °C with a stirring rate of 400 rpm for 48 h. After cooling, the product was filtered at...

Embodiment 2

[0042] 160°C, reaction for 42 hours, 15% mother liquor usage, static synthesis of TON molecular sieve

[0043]Gel B was prepared as described in Example 1. Its specific composition is (molar ratio) SiO 2 : 1.00Al 2 o 3 : 14.00K 2 O: 38.60DAH: 3610H 2 O=88.00:1.00:14.00:38.60:3610. Then, TON zeolite with 15% of the total mass of gel B was added thereto to filter the mother liquor once. After stirring, a uniform gel C is formed. The gel C was transferred to a 100mL stainless steel reactor with a polytetrafluoroethylene liner, and hydrothermally reacted at 160°C for 42h under static conditions. After cooling, the product was filtered at room temperature to obtain 2.6 g of the product. According to XRD characterization, the product is pure TON zeolite molecular sieve. image 3 shown.

Embodiment 3

[0048] 160°C, reaction for 42 hours, 20% mother liquor usage, static synthesis of TON molecular sieve

[0049] Gel B was prepared as described in Example 1, wherein the silicon source was silica and the aluminum source was pseudoboehmite. Its specific composition is (molar ratio) SiO 2 : 1.00Al 2 o 3 : 14.00K 2 O: 38.60DAH: 3610H 2 O=88.00:1.00:14.00:38.60:3610. Then add TON zeolite with 20% of the total mass of gel B to it and filter the mother liquor once. After stirring, a uniform gel C is formed. The gel C was transferred to a 100mL stainless steel reactor with a polytetrafluoroethylene liner, and hydrothermally reacted at 160°C for 42h under static conditions. After cooling, the product was filtered at room temperature to obtain 2.6 g of the product. According to XRD characterization, the product is pure TON zeolite molecular sieve. Figure 5 shown.

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Abstract

The invention relates to a stable synthetic method for TON zeolite. According to the method, zeolite crystallization mother liquor with a TON structure is used as an inductive agent for synthesis of zeolite with the TON structure. The method comprises the following steps: adding the TON zeolite crystallization mother liquor into initial gel in proportion and carrying out a hydro-thermal reaction under sealing conditions so as to obtain a TON zeolite product with a crystallization degree of more than 97%. According to the method, mother liquor produced in primary crystallization of TON zeolite is recovered and utilized; the TON zeolite product with high purity can be obtained in a short period of time under the condition of standing or nonviolent stirring; so the success rate of synthesis of the zeolite is increased, and growth of crystal phases like ZSM-5 and cristobalite is prevented.

Description

technical field [0001] The invention relates to a synthesis method of TON zeolite. Background technique [0002] TON zeolite molecular sieve was reported in US4556477 by Mobil Corporation in 1985. Because it has a one-dimensional 10-ring elliptical mesopore structure, the pore diameter is about 0.46×0.57nm. Because of its excellent selectivity in the selective conversion of olefins, it has been widely used as an important carrier for hydrocarbon isomerization catalysts in heavy oil deisomerization waxing reactions. [0003] Usually TON zeolite is synthesized by SiO 2 、Al 2 o 3 、K 2 O or Na 2 O, H 2 N-(CH 2 ) n -NH 2 (n=2-12) and other organic templates are mixed with water, and are prepared by hydrothermal treatment at 90-200° C. for 3-7 days in a high-pressure reactor. However, this reaction must be stirred at a high speed (300-400rpm) in exchange for the purity of TON molecular sieves, such as US4481177, US4902406, and US4900528, otherwise the synthesis will fail...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 谢彬王新苗翟绪丽高善彬杨晓东张志华胡胜王延飞付凯妹余颖龙张雅琳张瑀健庄梦琪刘彦峰郭金涛
Owner PETROCHINA CO LTD
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