# US 2018/0022648 A1 · Method for preparing support of molecular sieve membrane

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 2018/0022648 A1
- Document ID: US20180022648A1
- Status: Published application
- Kind: A1
- Application number: 15/542,648
- Filed: 2016-07-22
- Published: 2018-01-25
- Earliest claimed: 2015-12-25
- Assignees: Shandong Guiyuan Advanced Ceramics Co., Ltd
- Applicants: Shandong Guiyuan Advanced Ceramics Co., Ltd
- Inventors: Fanpeng Meng; Zhenkun Fan; Jian Zhang; Chao Zhang
- Web page: https://patentgrep.com/patent/US20180022648A1

## CPC

- C04B 35/195: Alkaline earth aluminosilicates, e.g. cordierite {or anorthite}
- B01D 67/00411: {by sintering}
- B01D 69/105: {Support pretreatment}
- C04B 35/624: Sol-gel processing
- C04B 35/6264: {Mixing media, e.g. organic solvents}
- C04B 35/62655: {Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying}
- C04B 35/62807: {Silica or silicates}
- C04B 35/62815: {Rare earth metal oxides}
- C04B 35/62886: {by wet chemical techniques}
- C04B 35/62892: {with a coating layer consisting of particles}
- C04B 35/62897: {Coatings characterised by their thickness}
- C04B 35/6365: {Cellulose or derivatives thereof}
- C04B 35/64: Burning or sintering processes (C04B33/32 takes precedence {; powder metallurgy B22F})
- C04B 38/00: Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof (treating slag with gases or gas generating material C04B5/06 {; expanded graphite C04B35/536})
- C04B 41/009: {characterised by the material treated}
- C04B 41/5042: {Zirconium oxides or zirconates; Hafnium oxides or hafnates}
- C04B 41/87: Ceramics
- C04B 2111/00801: {Membranes; Diaphragms}
- C04B 2235/3227: Lanthanum oxide or oxide-forming salts thereof
- C04B 2235/3481: Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
- C04B 2235/444: Halide containing anions, e.g. bromide, iodate, chlorite
- C04B 2235/483: Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
- C04B 2235/5436: micrometer sized, i.e. from 1 to 100 micron
- C04B 2235/602: Making the green bodies or pre-forms by moulding
- C04B 2235/6562: Heating rate
- C04B 2235/6567: Treatment time
- C04B 2235/77: Density
- C04B 2235/96: Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)

## Abstract

A method for preparing a support of a molecular sieve membrane is provided and relates to a technical field of support preparation, including steps of: according to a molar ratio of magnesium, aluminum and silicon in cordierite, preparing a nanometer composite sol of magnesium, aluminum, silicon and lanthanum serving as a sintering aid through a sol-gel method, enveloping and bonding the sol on a surface of dispersed nano-sized cordierite powders, and transforming the sol into nanometer composite oxides through presintering; mixing the cordierite powders, a binder and water, forming mud, extruding the mud, forming the mud into a green body, and sintering the green body into a cordierite support; coating a layer of film on the cordierite support with an aqueous dispersant of zirconia, then sintering, and obtaining a support of a molecular sieve membrane, composited by a cordierite main support layer and a zirconia film layer.

## Claims

### Claim 1

A method for preparing a support of a molecular sieve membrane, comprising steps of:
(1) adding ethyl alcohol and a first weight of water into a reaction kettle, then adding cordierite powders, and uniformly stirring; adding a first dispersant, then adding tetraethoxysilane, aluminum salt, magnesium salt and lanthanum salt, stirring and dissolving, and obtaining a mixed liquid; increasing a temperature of the mixed liquid to 65-80° C., then adding ammonium hydroxide into the mixed liquid, and adjusting a pH value thereof to 5-6; reacting for 2-12 hours, and generating a mixed sol of silicon, aluminum, magnesium and lanthanum, wherein a proportion of silicon, aluminum and magnesium in the mixed sol is the same as that in a composition of cordierite; further adjusting the pH value to 8-9, reacting for 2-6 hours, and aging the mixed sol; pouring an obtained mixture into a container, standing and generating precipitates; washing the precipitates with reverse osmosis (RO) water, sucking and filtering liquid out, and drying the precipitates; heating the dried precipitates, keeping a temperature of the precipitates, and obtaining cordierite particles enveloped by composite nanometer oxides which are prepared according to a composition proportion of the cordierite;
(2) uniformly mixing and stirring the cordierite particles, a binder, a second weight of water and a humectant, and forming mud; preparing the mud into a green body, drying the green body, and sintering the green body into a cordierite support; and
(3) adding zirconia into a third weight of water, adjusting a pH value thereof to 2.5-3 with nitric acid, and uniformly stirring; then adding a second dispersant and a viscosity modifier, uniformly stirring, and obtaining a film coating solution; coating the film coating solution on an outer layer of the cordierite support, drying and sintering the cordierite support, and obtaining the cordierite support with the outer layer coated by a zirconia film layer.

### Claim 2 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (1), a weight ratio of the ethyl alcohol and the water is 0.85-1.15:1; a median particle diameter D50 of the cordierite powders is 2-5 μm, and a weight of the cordierite powders is 25-35% of a total weight of the ethyl alcohol and the water; the first dispersant is a polyethylene glycol dispersant or a polyvinyl alcohol (PVA) dispersant, and a weight of the added first dispersant is 2-5% of the weight of the cordierite powders.

### Claim 3 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (1), a total weight of the tetraethoxysilane, the aluminum salt, the magnesium salt and the lanthanum salt is 3-8% of a weight of the cordierite powders; and a molar ratio of silicon in the tetraethoxysilane, aluminum in the aluminum salt, magnesium in the magnesium salt and lanthanum in the lanthanum salt is 5-5.2:4:2-2.2:0-3.

### Claim 4 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (1), the aluminum salt comprises at least one member selected from a group consisting of aluminum nitrate, aluminum chloride and aluminum sulfate; the magnesium salt comprises at least one member selected from a group consisting of magnesium nitrate, magnesium chloride and magnesium sulfate; and the lanthanum salt comprises at least one member selected from a group consisting of lanthanum nitrate, lanthanum chloride and lanthanum sulfate.

### Claim 5 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (1), a heating temperature is 450-650° C. and kept for 1-6 hours.

### Claim 6 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (2), the binder is methylcellulose or hydroxypropyl methyl cellulose, and a weight of the added binder is 4-10% of a weight of the cordierite particles; the second weight of the water is 20-40% of the weight of the cordierite particles; the humectant is glycerinum, and a weight of the added humectant is 1.5-3.5% of the weight of the cordierite particles.

### Claim 7 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (2), the green body is a circular tubular green body having a single hole, three holes or four holes.

### Claim 8 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (2), a sintering temperature is 950-1150° C. and a sintering time is 1-6 hours.

### Claim 9 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (3), a median particle diameter D50 of the zirconia is 0.25-0.6 μm, and a weight of the added zirconia is 10-20% of the third weight of water in the film coating solution; the second dispersant is a polyethylene glycol dispersant, and a weight of the added second dispersant is 2-5% of the weight of the zirconia; the viscosity modifier is hydroxypropyl methyl cellulose, and a weight of the added viscosity modifier is 0.65-1.5% of the third weight of water in the film coating solution; and a weight of the film coating solution is 6-12% of a weight of the cordierite support.

### Claim 10 (depends on 1)

The method for preparing the support of the molecular sieve membrane, as recited in claim 1, wherein: in the step (3), a sintering temperature is 950-1150° C. and a sintering time is 2-4 hours.