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Method for separating gas-liquid/liquid mixtures through pervaporation and vapor permeation by SAPO-34 molecular sieve membrane
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A technology of SAPO-34, gas-liquid mixture, applied in molecular sieves and alkali exchange compounds, separation methods, separation/purification of hydroxyl compounds, etc., to achieve high separation coefficient, large economic value, and low energy consumption
Active Publication Date: 2016-10-05
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI +2
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However, at present, molecular sieve membranes are mainly used for the dehydration of organic matter, while the separation of MeOH / DMC mixtures, especially the application of high-temperature vapor phase separation, has rarely been reported.
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Embodiment 1
[0050] SAPO-34 molecular sieve membrane separation methanol / dimethyl carbonate under different feed concentrations of embodiment 1
[0051] Step 1: Add 2.46 g of deionized water to 31.13 g of tetraethylammonium hydroxide solution (TEAOH, 35 wt%), then weigh 7.56 g of aluminum isopropoxide and add it to the aforementioned solution, and stir at room temperature for 2-3 hours; then , add dropwise 1.665g silica sol (40wt%), stir for 1 hour; Finally, slowly add dropwise 8.53g phosphoric acid solution (H 3 PO 4 , 85wt%), stirring overnight (such as stirring for 12 hours). Microwave heating was used for crystallization at 180°C for 7 hours. After the product is taken out, it is centrifuged, washed and dried to obtain SAPO-34 molecular sieve seed crystals. Among them, the SEM image of the seed crystal is shown as figure 1 shown. The XRD pattern of the seed crystal, such as figure 2 shown. It can be seen from the SEM image that the size of the seed crystal is about 300 nm×300 n...
Embodiment 2
[0062] SAPO-34 molecular sieve membrane separation methanol / dimethyl carbonate under different operating temperatures in embodiment 2
[0063] The difference from Example 1 is that the feed concentration MeOH / DMC in step 5 is 90 / 10, and the operating temperatures are 100°C, 110°C, 120°C, 130°C, and 140°C, respectively. All the other steps are the same as in Example 1.
[0064] The MeOH / DMC vapor phase permeation separation test result of table 2 embodiment 2
[0065]
[0066] It can be seen from Table 2 that at different operating temperatures (100-140° C.), the SAPO-34 molecular sieve membrane synthesized under the fluoride system has very high methanol selectivity. As the operating temperature increases, the methanol permeation flux increases gradually, which is due to the increase of methanol partial pressure.
Embodiment 3
[0067] SAPO-34 molecular sieve membrane separation methanol / dimethyl carbonate under different feed pressures of embodiment 3
[0068] The difference from Example 1 is that the feed concentration MeOH / DMC in step 5 is 90 / 10, and the feed pressures are 0.3MPa, 0.4MPa, 0.5MPa, 0.6MPa respectively. All the other steps are the same as in Example 1.
[0069] The MeOH / DMC pervaporation separation test result of table 3 embodiment 3
[0070]
[0071]It can be seen from Table 3 that under different feed pressures, the SAPO-34 molecular sieve membrane synthesized under the fluoride system has very high methanol selectivity; and as the system pressure increases, the permeation flux gradually increases. When the pressure reaches 0.5MPa, the flux of methanol is flat.
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Abstract
The invention discloses a method for separating gas-liquid / liquid mixtures through pervaporation and vapor permeation by an SAPO-34 molecular sieve membrane. The method comprises the steps: (1) mixing and dissolving an aluminum source, ammonium tetraethylhydroxide, water, a silicon source and a phosphorus source, then, carrying out hydrothermal crystallization, carrying out centrifugation, carrying out washing, and carrying out drying, so as to obtain an SAPO-34 molecular sieve seed crystal; (2) coating the internal surface of a porous support tube with the SAPO-34 molecular sieve seed crystal; (3) synthesizing an SAPO-34 molecular sieve membrane tube; (4) roasting the SAPO-34 molecular sieve membrane tube, so as to obtain an SAPO-34 molecular sieve membrane; and (5) separating the gas-liquid mixtures or liquid mixtures by using the SAPO-34 molecular sieve membrane obtained in the step (4) by adopting a pervaporation separation process or vapor permeation separation process. According to the method, methanol selectivity and permeation flux are very high, and pervaporation or vapor permeation separation is an efficient and energy-saving separation method.
Description
technical field [0001] The invention relates to a method for separating a mixture by using a SAPO-34 molecular sieve membrane, in particular to a method for separating a gas-liquid or a liquid mixture by pervaporation and vapor phase permeation of a SAPO-34 molecular sieve membrane. Background technique [0002] Dimethyl carbonate (DMC), the molecular formula is CO (OCH 3 ) 2 , is a good solvent, low volatility, toxicity value similar to absolute ethanol, and can be completely biodegradable, is an environmentally friendly chemical, has a wide range of applications in the fields of medicine, chemical industry, energy and so on. The molecular oxygen content of DMC reaches 53%, which is three times that of methyl tert-butyl ether (MTBE). It can be used as a gasoline additive to increase the octane number and suppress the emission of carbon monoxide and hydrocarbons. Its chemical properties are very active, and it is an important intermediate and starting material for organic ...
Claims
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