Solidifying method in two steps for preparing carbon membrane of phenol-formaldehyde resin

Abstract

A process for preparing phenlic resin-base carbon film with different pore diameters by two-step solidification includes pre-solidifying the thermoplastic phenolic resin in air by adding hexamethylenetetramine, pulverizing by 120 meshes, mixing with adhesive, water and hexamethylenetetramine, kneading, extruding out for shaping, drying, solidifying in air again, and carbonizing in inertial gas for 30-120 min.

Description

technical field

[0001] The invention belongs to the key membrane preparation technical field in membrane separation, and relates to a method for preparing carbon membranes with different apertures by using thermoplastic phenolic resin. Background technique

[0002] Carbon membrane is a new type of inorganic separation membrane, which usually refers to a separation membrane composed of carbon materials. Compared with traditional organic membranes, carbon membranes have the advantages of high separation capacity, high temperature resistance, good chemical stability, uniform pore size, large adjustable range, and high mechanical strength. The average pore size of the carbon membrane is in the range of a few angstroms to more than ten microns. According to the different pore sizes, the carbon membrane can be used for liquid separation, gas separation and membrane reactors. Adjusting the pore size of the carbon membrane is the key to the preparation of the carbon membrane. [00...

Examples

Embodiment 1

[0018] Add 3wt% hexamethylenetetramine to the thermoplastic phenolic resin powder (particle size ≤ 200 mesh), place it in an oven, keep the temperature at 150°C for 60 minutes, and cool to room temperature to obtain a primary solidified block. Crush to less than 250 mesh, add 6wt% cellulose, 80wt% water, 8wt% hexamethylenetetramine, knead and extrude to form a raw material film, dry the raw material film at room temperature for 3 days, and place it in carbonization Secondary curing in the furnace, heating rate 0.5°C / min, curing temperature 120°C, curing time 60min, carbonization under the protection of Ar gas after secondary curing, carbonization temperature 850°C, heating rate 1°C / min, constant temperature time 60min, cooling After obtaining the carbon membrane product, use the bubble point method to measure its average pore size and pore size distribution, with N 2 To permeate gas, cyclohexanol is used as permeate liquid, the average pore size of the carbon membrane is 0.1 μ...

Embodiment 2

[0020] 1 wt% hexamethylenetetramine was added during primary curing, and 10 wt% hexamethylenetetramine was added during molding. Other conditions were the same as in Example 1, and the maximum pore size of the carbon membrane was 0.15 μm.

Embodiment 3

[0022] 5wt% hexamethylenetetramine was added during primary curing, and 6wt% hexamethylenetetramine was added during molding. Other conditions were the same as in Example 1. The average pore size of the carbon membrane was 0.28 μm, and the maximum pore size was 0.79 μm.

technical field

[0001] The invention belongs to the key membrane preparation technical field in membrane separation, and relates to a method for preparing carbon membranes with different apertures by using thermoplastic phenolic resin. Background technique

[0002] Carbon membrane is a new type of inorganic separation membrane, which usually refers to a separation membrane composed of carbon materials. Compared with traditional organic membranes, carbon membranes have the advantages of high separation capacity, high temperature resistance, good chemical stability, uniform pore size, large adjustable range, and high mechanical strength. The average pore size of the carbon membrane is in the range of a few angstroms to more than ten microns. According to the different pore sizes, the carbon membrane can be used for liquid separation, gas separation and membrane reactors. Adjusting the pore size of the carbon membrane is the key to the preparation of the carbon membrane. [00...

Examples

Embodiment 1

[0018] Add 3wt% hexamethylenetetramine to the thermoplastic phenolic resin powder (particle size ≤ 200 mesh), place it in an oven, keep the temperature at 150°C for 60 minutes, and cool to room temperature to obtain a primary solidified block. Crush to less than 250 mesh, add 6wt% cellulose, 80wt% water, 8wt% hexamethylenetetramine, knead and extrude to form a raw material film, dry the raw material film at room temperature for 3 days, and place it in carbonization Secondary curing in the furnace, heating rate 0.5°C / min, curing temperature 120°C, curing time 60min, carbonization under the protection of Ar gas after secondary curing, carbonization temperature 850°C, heating rate 1°C / min, constant temperature time 60min, cooling After obtaining the carbon membrane product, use the bubble point method to measure its average pore size and pore size distribution, with N 2 To permeate gas, cyclohexanol is used as permeate liquid, the average pore size of the carbon membrane is 0.1 μ...

Embodiment 2

[0020] 1 wt% hexamethylenetetramine was added during primary curing, and 10 wt% hexamethylenetetramine was added during molding. Other conditions were the same as in Example 1, and the maximum pore size of the carbon membrane was 0.15 μm.

Embodiment 3

[0022] 5wt% hexamethylenetetramine was added during primary curing, and 6wt% hexamethylenetetramine was added during molding. Other conditions were the same as in Example 1. The average pore size of the carbon membrane was 0.28 μm, and the maximum pore size was 0.79 μm.