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Method for recovering free template in molecular sieve slurry or filtrated stock

A technology for filtering mother liquor and molecular sieves, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of miscellaneous crystals, steam pollution, high energy consumption, etc., and achieve the effect of improving recovery rate

Active Publication Date: 2015-07-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, too many times of mother liquor reuse will easily lead to the formation of miscellaneous crystals, and recovery methods such as flash evaporation have high energy consumption and are likely to cause steam pollution, which is not an ideal recovery method for mother liquor templating agent

Method used

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  • Method for recovering free template in molecular sieve slurry or filtrated stock
  • Method for recovering free template in molecular sieve slurry or filtrated stock

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The silicon source, aluminum source, alkali source, and deionized water used in Example 1 are the same as those in Comparative Example 1, except that HMI and aniline are used as composite templates.

[0037] The colloidal molar ratio of the mixture is: 0.18NaOH:SiO 2 :0.033Al 2 o 3 :0.10HMI: 0.20 Aniline: 15H 2 O, the crystallization temperature is 145°C, under autogenous pressure, crystallize at a stirring speed of 300 rpm for 72 hours, take out the product after cooling, filter, wash and dry, and roast at 550°C for 10 hours to obtain a sample. Test its XRD diffraction pattern, the 2θ angle is 0 to 35°, the product is MCM-22 molecular sieve, the specific surface is 508m 2 / g, the relative crystallinity is 105%.

[0038] Wet base molecular sieve B is obtained after direct filtration (without washing with water). After the mother liquor is allowed to stand for stratification, the upper layer is the aniline phase. After the liquid separation operation, the aniline pha...

Embodiment 2-7

[0040] This example illustrates the recovery method provided by the present invention.

[0041] The wet-based molecular sieve A in Comparative Example 1 was extracted with aniline aqueous solution. The results of different extraction times, mass ratio of aniline to mother liquor, water / wet-based molecular sieve mass ratio and extraction temperature are listed in Table 1.

[0042] Table 1 The experimental results of treating wet base molecular sieve A

[0043]

Embodiment 8-13

[0045] This example illustrates the recovery method provided by the present invention.

[0046] The wet-based molecular sieve B prepared in Example 1 was extracted with an aniline aqueous solution. The results of different extraction times, aniline / mother liquor mass ratio, water / wet-based molecular sieve mass ratio and extraction temperature are listed in Table 2.

[0047] Table 2 Experimental results of treating wet base molecular sieve B

[0048]

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Abstract

The invention discloses a method for recovering a free template in molecular sieve slurry or filtrated stock. The method is characterized by comprising carrying out crystallization on mixture colloid comprising a silicon source, an aluminum source, an alkali source, a main template, an optional auxiliary template and deionized water under the hydro-thermal conditions, carrying out extraction on molecular sieve slurry or filtrated stock by the auxiliary template, extracting the free main template in the molecular sieve slurry or filtrated stock into an organic phase, and recovering the main template in the organic phase, wherein the auxiliary template is a substance of which the solubility is substantially improved with temperature increasing. The method substantially improves a main template recovery rate.

Description

technical field [0001] The present invention relates to a method for recovering free template agent in molecular sieve slurry or filtered mother liquor, and more particularly to a method for recovering free template agent in molecular sieve slurry or filtered mother liquor in the synthesis of a MWW structure molecular sieve. Background technique [0002] MCM-22 molecular sieve is a representative molecular sieve of MWW structure molecular sieve. MCM-22 molecular sieve has two sets of independent pore systems that are not directly connected to each other: a ten-membered ring channel with a pore diameter of 0.40×0.59 nm in the layer; a twelve-membered ring supercage with a 0.40 nm diameter between layers. The opening of the ten-membered ring of ×0.54nm communicates with the outside world. On the crystal surface of MCM-22 molecular sieve, there are some twelve-membered ring holes, which are half of the supercage, and the depth is about 0.71nm (Science, 1994, 264:1910). Theref...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 邢恩会谢文华刘强慕旭宏罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP