Preparation method of high-temperature-hole-forming glass hollow fiber membrane
A fiber membrane and hollow technology, which is applied in the field of glass hollow fiber membrane preparation, can solve the problems of membrane performance degradation, porosity decrease, glass melting, etc., achieve permeation flux and separation performance improvement, reduce production cost, and lower calcination temperature Effect
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Embodiment 1
[0018] According to (1) preparation of casting solution, (2) spinning, (3) drying of membrane green body and calcination to make holes to prepare glass hollow fiber membrane, wherein:
[0019] (1) First, wet the glass powder and calcium carbonate in a ball mill for 12 hours, and pass through a 200-mesh sieve after drying to obtain d 50 =1μm solid fine powder. Then polyvinylidene fluoride and N,N-dimethylacetamide with a mass ratio of 8:92 were mixed and stirred for 4 hours to obtain a uniform polymer solution. Add the sieved solid micropowder into the polymer solution, and mechanically stir for 6 hours. The mass ratio of the solid micropowder to the polymer solution is 30:70, and a uniformly dispersed casting solution is obtained.
[0020] (2) Transfer the casting solution to the material tank of the spinning machine, let it stand for degassing for 4 hours, and then, under the pressure of 100KPa nitrogen, let the casting solution enter the water at 50°C through the spinneret,...
Embodiment 2
[0023] According to the steps in Example 1, the casting solution was prepared, spinning, drying and calcining were carried out to form pores, except that the carbonate pore-forming agent used was magnesium carbonate. The particle size of the solid micropowder obtained after ball milling and sieving is d 50 = 5 μm. The polymer is polyvinyl chloride, the solvent is dimethyl sulfoxide, and the mass ratio of polyvinyl chloride to dimethyl sulfoxide is 12:88. The solid micropowder is mixed with the polymer solution to obtain the casting liquid, and its mass ratio is 40:60. The static degassing time is 6 hours, the spinneret core fluid is 50°C deionized water, the coagulation bath is 40°C water, and the green film is soaked in 20°C water for 48 hours. During the sintering process, heat up at 5°C / min, hold at 600°C for 1 hour, then raise the temperature at a rate of 9°C / min to 900°C and hold for 1 hour to decompose magnesium carbonate, and then cool to room temperature with the furna...
Embodiment 3
[0025] According to the steps in Example 1, the casting solution was prepared, spinning, drying and calcining were used to form pores, except that the carbonate pore-forming agent used was a mixture of calcium carbonate and magnesium carbonate in any proportion. The particle size of the solid micropowder obtained after ball milling and sieving is d 50 = 8 μm. The polymer is polyacrylonitrile, the solvent is N,N-dimethylformamide, and the mass ratio of polyacrylonitrile to N,N-dimethylformamide is 20:80. The solid micropowder is mixed with the polymer solution to obtain the casting liquid, and the mass ratio thereof is 50:50. The standing degassing time is 8 hours, the spinneret core fluid is 60°C deionized water, the coagulation bath is 30°C water, and the green film is soaked in 10°C water for 36 hours. During the sintering process, heat up at 4°C / min, hold at 400°C for 1 hour, then raise the temperature at a rate of 10°C / min to 1000°C and hold for 1 hour to decompose calci...
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Abstract
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