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A kind of preparation method of cosapo-11 molecular sieve
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A technology of cosapo-11 and molecular sieve, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of unstable product quality, low acid site density of molecular sieve, etc., and achieve high stability and wide application foreground effect
Inactive Publication Date: 2014-10-29
HEILONGJIANG UNIV
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[0003] The present invention aims to solve the problems of low acid site density and unstable product quality of molecular sieves prepared at present, and provides a preparation method of CoSAPO-11 molecular sieves
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specific Embodiment approach 1
[0022] Specific embodiment one: the preparation method of a kind of CoSAPO-11 molecular sieve of this embodiment, specifically is prepared according to the following steps:
[0023] 1. Perform ion exchange between X-type molecular sieve and cobalt nitrate solution, or between X-type molecular sieve and cobalt acetate solution, control the ion exchange temperature at 50-80°C, ion exchange time at 0.5-4h, and exchange times at 1-20°C 4 times to obtain Co / X molecular sieve;
[0024] 2. Add phosphoric acid with a mass concentration of 85%, pseudoboehmite, Co / X molecular sieve and di-n-butylamine obtained in step 1 into deionized water in sequence, control the speed at 1000-1500r / min, and stir for 1-2 hours , to prepare the initial gel, wherein the ratio of phosphoric acid, pseudo-boehmite, di-n-butylamine, Co / X molecular sieve obtained in step 1 and deionized water is 1:1~9.134:0.800~7.000:1 ~5.726:7.000~56.484;
[0025] 3. Put the initial gel obtained in step 2 into a crystalli...
specific Embodiment approach 2
[0026] Embodiment 2: This embodiment differs from Embodiment 1 in that in step 1, the X-type molecular sieve is ion exchanged with cobalt nitrate solution, the ion exchange temperature is controlled at 60° C., and the number of exchanges is 2 times. Others are the same as in the first embodiment.
specific Embodiment approach 3
[0027] Embodiment 3: This embodiment differs from Embodiment 1 in that in step 1, the X-type molecular sieve is ion-exchanged with the cobalt acetate solution, the ion exchange temperature is controlled at 70° C., and the number of exchanges is 2 times. Others are the same as in the first embodiment.
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Abstract
The invention provides a preparation method of a CoSAPO-11 molecular sieve, relates to a preparation method of a molecular sieve and aims to solve the problems of a prepared molecular sieve such as low acid site density and unstable product quality in the prior art. The method comprises the following steps: 1, preparing a Co / X molecular sieve; 2, preparing an initial gel; and 3, crystallizing, and drying. According to the invention, the method combines ion exchange and isomorphous replacement, and realizes the modulation of two acid sites by changing the silicon-cobalt ratio; more acid sites can be formed in comparison with simply introducing cobalt and other heteroatoms; and higher stability is achieved. The invention is used for preparation of a CoSAPO-11 molecular sieve.
Description
technical field [0001] The invention relates to a method for preparing molecular sieves. Background technique [0002] In 1982, a new type of aluminum phosphate molecular sieve was developed by UCC Corporation of the United States. Due to its AlO 4 and PO 4 Tetrahedrons are composed of strictly ordered and alternating arrangements on the molecular sieve framework, so they are electrically neutral, have no ion exchange performance, and have weak surface acidity. The synthesis of SAPO-11 with mild acidity usually uses di-n-propylamine as a template, and uses silica sol and pseudo-boehmite or aluminum isopropoxide as a source of silicon and aluminum (US P4440871). However, due to di-n-propylamine When used as a template, it can guide the formation of more than eight crystal phases such as SAPO-11, SAPO-5, SAPO-31 and SAPO-41, and it is very easy to form mixed crystals of multiple crystal phases during the synthesis of SAPO-11 molecular sieves. Moreover, the crystallinity of...
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