CN111943198A - Preparation method of coconut shell carbon molecular sieve with high specific surface area - Google Patents
Preparation method of coconut shell carbon molecular sieve with high specific surface area Download PDFInfo
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- CN111943198A CN111943198A CN202010829901.7A CN202010829901A CN111943198A CN 111943198 A CN111943198 A CN 111943198A CN 202010829901 A CN202010829901 A CN 202010829901A CN 111943198 A CN111943198 A CN 111943198A
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- molecular sieve
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/04—Purification or separation of nitrogen
- C01B21/0405—Purification or separation processes
- C01B21/0433—Physical processing only
- C01B21/045—Physical processing only by adsorption in solids
- C01B21/0455—Physical processing only by adsorption in solids characterised by the adsorbent
- C01B21/0461—Carbon based materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- Analytical Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a preparation method of a coconut shell carbon molecular sieve with high specific surface area, which adopts coconut shells, coal and phenolic resin to be fully mixed as raw materials, so that the raw materials have low cost, realize the waste utilization of the coconut shells, have low ash content, and are beneficial to the subsequent treatment; in particular, in the carbonization process, the particle material contains micro-nano-scale raw vermiculite powder which has the characteristic of thermal expansion of 18-25 times, and interlayer water molecules are gradually evaporated in the heating process. Compared with the traditional coconut shell carbon molecular sieve, the coconut shell carbon molecular sieve with high specific surface area prepared by the invention has the advantages that the specific surface area is increased by 50 percentAnd the aperture is uniform. The nitrogen-producing carbon molecular sieve of the invention has the nitrogen production concentration of 99.9 percent and the specific surface area of 3000-2/g。
Description
Technical Field
The invention relates to a preparation method of a molecular sieve, belongs to the field of carbon materials, and particularly relates to a preparation method of a coconut shell carbon molecular sieve with a high specific surface area.
Background
The nitrogen-producing carbon molecular sieve is a novel activated carbon containing almost only uniform micropores with a diameter of several angstroms. The pore characteristics can endow the nitrogen-producing carbon molecular sieve with selective adsorption performance according to the pore size and the size and shape of molecules of gas to be adsorbed. By utilizing this characteristic, nitrogen-producing carbon molecular sieves are widely used in various gas separation processes. The raw materials which can be used for preparing the carbon molecular sieve are very wide, and the carbon molecular sieve can be prepared from natural products to high molecular polymers. The most important of them are coal, husk, etc.
Through retrieval, the disclosure of carbon molecular sieve using coconut shell as raw material is also disclosed, for example, chinese patent application No. 200580029160.8 discloses a method for preparing carbon molecular sieve using coconut shell as raw material and using the carbon molecular sieve for nitrogen separation. Chinese patent application No. 201510498117.1 discloses a method for preparing a carbon molecular sieve from coconut shells, and the purity of nitrogen produced by the molecular sieve prepared by the method is 99.6%. However, the specific surface area of the carbon molecular sieve prepared by the above method needs to be improved, and the gas yield has a larger bottleneck, so that a preparation method of the coconut shell carbon molecular sieve with high specific surface area needs to be researched.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a coconut shell carbon molecular sieve with high specific surface area.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of a coconut shell carbon molecular sieve with high specific surface area comprises the following steps:
a. proportioning raw materials; crushing coconut shells into a powdery material, drying and grinding the powdery material into a micro-powdery material, uniformly mixing coconut shell powder, coal and phenolic resin, and heating for 6-8h at the temperature of 300-400 ℃ under the protection of nitrogen;
b. planetary ball milling the sample, and crushing to 120 meshes;
c. adding phenolic resin and micro-nano-scale vermiculite powder into a sample, kneading, extruding and forming into particles;
d. placing the sample in a furnace pipe, heating to 1300-;
e. adding a sample into a potassium hydroxide solution, uniformly stirring, carrying out ball milling, filtering, carrying out filter pressing, and drying;
f. placing the sample in a converter, heating to 600-650 ℃ under the protection of nitrogen, and activating for 5-6h under the protection of nitrogen;
g. and (3) carrying out hydrochloric acid pickling on the sample, then washing the sample to be neutral, and drying the sample to obtain the carbon molecular sieve.
Preferably, in the step a, the particle size of the micro-powder coconut husk powder is 10-50 μm.
Preferably, in the step a, the raw materials comprise 80-120 parts of coconut shell powder, 15-25 parts of coal and 18-30 parts of phenolic resin.
Preferably, in the step c, the particle size of the micro-nano-scale raw vermiculite powder is 0.5-5 μm.
Preferably, in the step c, the added phenolic resin and the micro-nano-scale raw vermiculite powder account for 6-8% and 0.1-0.2% of the weight of the particles.
Preferably, in the step d, the temperature rising speed is 15-20 ℃/min; preserving the heat for 20-25 min.
Preferably, in the step f, the temperature rise speed is 3-5 ℃/min.
Preferably, in the step g, in the acid washing process, the concentration of the hydrochloric acid is 0.1-0.2mol/L, the acid washing time is 20-30min, and the stirring speed is 600-800 rpm.
The invention has the beneficial effects that: compared with the prior art, the coconut shell, the coal and the phenolic resin are fully mixed as the raw materials, so that the cost of the raw materials is low, the waste utilization of the coconut shell is realized, and the ash content of the raw materials is low, thereby being beneficial to the subsequent treatment; in particular, in the carbonization process, the particle material contains micro-nano-scale raw vermiculite powder which has the characteristic of thermal expansion of 18-25 times, and interlayer water molecules are gradually evaporated in the heating process. Compared with the traditional coconut shell carbon molecular sieve, the coconut shell carbon molecular sieve with high specific surface area prepared by the invention has the advantages that the specific surface area is increased by more than 50 percent, and the aperture is uniform. The nitrogen-producing carbon molecular sieve of the invention has the nitrogen production concentration of 99.9 percent and the specific surface area of 3000-2/g。
Detailed Description
Example 1:
a preparation method of a coconut shell carbon molecular sieve with high specific surface area comprises the following steps:
a. proportioning raw materials; crushing coconut shells into a powdery material, drying and grinding the powdery material into a micro-powdery material, uniformly mixing coconut shell powder, coal and phenolic resin, and heating for 7 hours at 380 ℃ under the protection of nitrogen;
b. planetary ball milling the sample, and crushing to 120 meshes;
c. adding phenolic resin and micro-nano-scale vermiculite powder into a sample, kneading, extruding and forming into particles;
d. putting the sample in a furnace pipe, heating to 1320 ℃ under the protection of nitrogen, and carbonizing;
e. adding a sample into a potassium hydroxide solution, uniformly stirring, carrying out ball milling, filtering, carrying out filter pressing, and drying;
f. putting the sample into a converter, heating to 620 ℃ under the protection of nitrogen, and activating for 5.5 hours under the protection of nitrogen;
g. and (3) carrying out hydrochloric acid pickling on the sample, then washing the sample to be neutral, and drying the sample to obtain the carbon molecular sieve.
In the step a, the particle size of the micro-powder coconut husk powder is 10-50 μm.
In the step a, the raw materials comprise 100 parts of coconut shell powder, 18 parts of coal and 25 parts of phenolic resin.
In the step c, the particle size of the micro-nano-scale raw vermiculite powder is 0.5-5 μm; the added phenolic resin and micro-nano-scale vermiculite powder account for 6.5 percent and 0.15 percent of the weight of the particles.
In the step d, the temperature rising speed is 18 ℃/min; and keeping the temperature for 22 min.
In the step f, the temperature rise speed is 4 ℃/min.
In the step g, in the acid washing process, the concentration of hydrochloric acid is 0.18mol/L, the acid washing time is 25min, and the stirring speed is 750 rpm.
Example 2:
a preparation method of a coconut shell carbon molecular sieve with high specific surface area comprises the following steps:
a. proportioning raw materials; crushing coconut shells into a powdery material, drying and grinding the powdery material into a micro-powdery material, uniformly mixing coconut shell powder, coal and phenolic resin, and heating for 6 hours at 400 ℃ under the condition of nitrogen protection;
b. planetary ball milling the sample, and crushing to 120 meshes;
c. adding phenolic resin and micro-nano-scale vermiculite powder into a sample, kneading, extruding and forming into particles;
d. putting the sample in a furnace pipe, heating to 1350 ℃ under the protection of nitrogen, and carbonizing;
e. adding a sample into a potassium hydroxide solution, uniformly stirring, carrying out ball milling, filtering, carrying out filter pressing, and drying;
f. putting the sample into a converter, heating to 600 ℃ under the protection of nitrogen, and activating for 6 hours under the protection of nitrogen;
g. and (3) carrying out hydrochloric acid pickling on the sample, then washing the sample to be neutral, and drying the sample to obtain the carbon molecular sieve.
In the step a, the particle size of the micro-powder coconut husk powder is 10-50 μm.
In the step a, the raw materials comprise 80 parts of coconut shell powder, 25 parts of coal and 18 parts of phenolic resin.
In the step c, the particle size of the micro-nano-scale raw vermiculite powder is 0.5-5 μm; the added phenolic resin and micro-nano-scale raw vermiculite powder account for 8 percent and 0.2 percent of the weight of the particles.
In the step d, the temperature rising speed is 15 ℃/min; and keeping the temperature for 25 min.
In the step f, the temperature rise speed is 3 ℃/min.
In the step g, in the acid washing process, the concentration of hydrochloric acid is 0.2mol/L, the acid washing time is 20min, and the stirring speed is 800 rpm.
Example 3:
a preparation method of a coconut shell carbon molecular sieve with high specific surface area comprises the following steps:
a. proportioning raw materials; crushing coconut shells into a powdery material, drying and grinding the powdery material into a micro-powdery material, uniformly mixing coconut shell powder, coal and phenolic resin, and heating for 8 hours at 300 ℃ under the condition of nitrogen protection;
b. planetary ball milling the sample, and crushing to 120 meshes;
c. adding phenolic resin and micro-nano-scale vermiculite powder into a sample, kneading, extruding and forming into particles;
d. putting the sample in a furnace pipe, heating to 1300 ℃ under the protection of nitrogen, and carbonizing;
e. adding a sample into a potassium hydroxide solution, uniformly stirring, carrying out ball milling, filtering, carrying out filter pressing, and drying;
f. putting the sample into a converter, heating to 650 ℃ under the protection of nitrogen, and activating for 5 hours under the protection of nitrogen;
g. and (3) carrying out hydrochloric acid pickling on the sample, then washing the sample to be neutral, and drying the sample to obtain the carbon molecular sieve.
In the step a, the particle size of the micro-powder coconut husk powder is 10-50 μm.
In the step a, the raw materials comprise 120 parts of coconut shell powder, 15 parts of coal and 30 parts of phenolic resin.
In the step c, the particle size of the micro-nano-scale raw vermiculite powder is 0.5-5 μm; the added phenolic resin and micro-nano-scale raw vermiculite powder account for 6 percent and 0.1 percent of the weight of the particles.
In the step d, the temperature rising speed is 20 ℃/min; and preserving the temperature for 20 min.
In the step f, the temperature rise speed is 5 ℃/min.
In the step g, in the acid washing process, the concentration of hydrochloric acid is 0.1mol/L, the acid washing time is 30min, and the stirring speed is 600 rpm.
Comparative example 1
The micro-nano-scale vermiculite powder in the example 1 is removed, and other preparation conditions are unchanged, so that the carbon molecular sieve is obtained.
Comparative example
The carbon molecular sieve obtained in the Chinese patent with the application number of 201510498117.1 in example 1.
The specific surface areas and nitrogen-making purities of the molecular sieves of examples 1-3 and comparative example 1 and the comparative example were tested, and the specific data are as follows:
table 1: molecular sieve test results of examples 1-3 and comparative example 1 and comparative example;
example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example | |
Specific surface area (m)2/g) | 3181 | 3157 | 3195 | 1755 | 2082 |
Purity of nitrogen (%) | 99.95 | 99.94 | 99.94 | 99.18 | 99.66 |
The above embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the scope of the present invention, and all equivalent substitutions or changes according to the technical solutions and the inventive concepts of the present invention should be covered by the scope of the present invention.
Claims (8)
1. A preparation method of a coconut shell carbon molecular sieve with high specific surface area is characterized by comprising the following steps:
a. proportioning raw materials; crushing coconut shells into a powdery material, drying and grinding the powdery material into a micro-powdery material, uniformly mixing coconut shell powder, coal and phenolic resin, and heating for 6-8h at the temperature of 300-400 ℃ under the protection of nitrogen;
b. planetary ball milling the sample, and crushing to 120 meshes;
c. adding phenolic resin and micro-nano-scale vermiculite powder into a sample, kneading, extruding and forming into particles;
d. placing the sample in a furnace pipe, heating to 1300-;
e. adding a sample into a potassium hydroxide solution, uniformly stirring, carrying out ball milling, filtering, carrying out filter pressing, and drying;
f. placing the sample in a converter, heating to 600-650 ℃ under the protection of nitrogen, and activating for 5-6h under the protection of nitrogen;
g. and (3) carrying out hydrochloric acid pickling on the sample, then washing the sample to be neutral, and drying the sample to obtain the carbon molecular sieve.
2. The method for preparing the coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in the step a, the particle size of the micro-powder coconut shell powder is 10-50 μm.
3. The preparation method of the coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in the step a, the raw material mixture ratio is 80-120 parts of coconut shell powder, 15-25 parts of coal and 18-30 parts of phenolic resin.
4. The method for preparing a coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in step c, the particle size of the micro-nano-sized vermiculite powder is 0.5-5 μm.
5. The method for preparing coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in step c, the phenolic resin and micro-nano-scale raw vermiculite powder are added in an amount of 6-8% and 0.1-0.2% by weight of the particles.
6. The method for preparing the coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in the step d, the temperature rising speed is 15-20 ℃/min; preserving the heat for 20-25 min.
7. The method for preparing the coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in step f, the temperature rising speed is 3-5 ℃/min.
8. The method for preparing coconut shell carbon molecular sieve with high specific surface area as claimed in claim 1, wherein in step g, the concentration of hydrochloric acid is 0.1-0.2mol/L, the acid washing time is 20-30min, and the stirring speed is 600-800 rpm.
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CN112721364A (en) * | 2021-01-20 | 2021-04-30 | 嘉兴市博尔新材料有限公司 | Mildew-proof wear-resistant environment-friendly PVC artificial leather and preparation method thereof |
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