CN114700037A - Active carbon composite material and process - Google Patents
Active carbon composite material and process Download PDFInfo
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- CN114700037A CN114700037A CN202210305999.5A CN202210305999A CN114700037A CN 114700037 A CN114700037 A CN 114700037A CN 202210305999 A CN202210305999 A CN 202210305999A CN 114700037 A CN114700037 A CN 114700037A
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- 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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
Abstract
The invention discloses an active carbon composite material and a process thereof, the active carbon composite material comprises an active carbon layer and an organic layer wrapped outside the active carbon layer, and copper hydroxide layers are wrapped outside the active carbon layer and the organic layer. A process for preparing an activated carbon composite material comprises the following steps: preparing a graphene aqueous solution for later use; weighing an iron salt solution, adding the iron salt solution into the prepared graphene aqueous solution until the iron salt solution is uniformly mixed for later use; weighing the crude bran and the terephthalic acid, sequentially adding the crude bran and the terephthalic acid into the prepared mixed solution, and uniformly stirring; obtaining activated carbon; placing the mixture in a closed reaction kettle; and filtering and centrifuging the mixed solution after the reaction is finished and the mixed solution is cooled to carry out solid-liquid separation to obtain the iron/crude bran/activated carbon composite material. The invention has the advantages of easily obtained raw materials, low price, high quality and easy recovery, and the prepared active carbon composite material has stronger adsorbability; meanwhile, the mesoporous structure of the activated carbon can be optimized, the specific surface area of the activated carbon is improved, and the material has more excellent performance.
Description
Technical Field
The invention relates to a composite material and a process, in particular to an active carbon composite material and a process.
Background
The activated carbon is an excellent adsorbent, has the advantages of porous structure, large adsorption capacity, high speed, high physical adsorption and chemical adsorption functions, high efficiency, good removal effect and the like, and has the biggest characteristic of cyclic utilization and desorption regeneration after saturation; can be used for adsorbing toxic gas and harmful substances. In recent years, with the increase of severe weather such as haze and the like, the application of gas masks is becoming more and more common, and the adsorption effect of common activated carbon for gas masks sometimes does not meet the requirement. Based on the above situation, finding a novel active carbon adsorbent for toxic gas and harmful substances, which has larger adsorption capacity, faster absorption and desorption speed and good stability, becomes the key point for the research of technical personnel. The activated carbon for the gas mask in the market at present has low adsorption efficiency, so that the canister matched with the gas mask for use has large volume and cannot meet the requirements of light weight and long-time use.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides an activated carbon composite material and a process thereof.
In order to solve the technical problems, the invention adopts the technical scheme that: an active carbon composite material comprises an active carbon layer and an organic layer wrapped outside the active carbon layer, wherein the active carbon layer and the organic layer are wrapped with copper hydroxide layers.
Preferably, the specific surface area of the activated carbon layer is 2310-2410m2/g。
Preferably, the organic layer consists of crude bran, iron salts and terephthalic acid.
A process for preparing an activated carbon composite material comprises the following steps:
(1) dissolving graphene in deionized water, stirring and performing ultrasonic treatment to obtain a graphene aqueous solution with the mass concentration of 3.05-4% for later use;
(2) according to the weight ratio of iron: the graphene is 1-2: 1, adding the ferric salt solution into the graphene aqueous solution prepared in the step (1), uniformly stirring, dripping alkaline solution, adjusting the pH of the mixed solution to be 8-10, and continuously stirring for more than 40min until the mixed solution is uniformly mixed for later use;
(3) weighing the crude bran and the terephthalic acid according to the mass ratio of 10:1-20, sequentially adding the crude bran and the terephthalic acid into the mixed solution prepared in the step (2), heating to 350 ℃, and uniformly stirring;
(4) weighing activated carbon and graphene-hydrogen peroxide according to the mass ratio of 2:9, soaking the activated carbon in the graphene-hydrogen peroxide mixed solution to obtain activated carbon, adding the activated carbon into the mixed solution prepared in the step (3), and uniformly stirring;
(5) placing the mixed solution prepared in the step (4) in a closed reaction kettle, and carrying out hydrothermal reaction for 6-9h at the temperature of 200-300 ℃;
(6) and (3) taking out the mixed solution after the reaction in the step (5) is finished and cooled, filtering and centrifuging to perform solid-liquid separation, soaking the separated solid in a soaking agent containing ammonia and copper hydroxide, and drying to obtain the iron/crude bran/activated carbon composite material.
Preferably, the activated carbon is powder, and the mesh number is 500-600 meshes.
Preferably, the ferric salt is one or more of ferric nitrate, ferric sulfate and ferric chloride.
Preferably, the alkaline solution is: one or more of NaOH solution, KOH solution and ammonia water solution.
Preferably, in the graphene-hydrogen peroxide mixed solution, the mass fraction of hydrogen peroxide is 3-12%, and the mass fraction of graphene is 0.03-0.7%.
Preferably, the mass fraction of ammonia in the impregnating agent is 20-25%.
Preferably, the preparation method of the impregnation agent comprises the following steps: adding ammonia water and copper hydroxide dispersion liquid into water, and uniformly mixing, wherein the mass fraction of the ammonia water is 65-75%, the mass fraction of the copper hydroxide dispersion liquid is 25-35%, and the mass fraction of the water is 3-12%.
According to the invention, by using the crude bran, the ferric salt and the graphene, not only are the raw materials easily available, cheap and excellent in quality and easy to recover, but also the prepared activated carbon composite material has stronger adsorbability, and the iron particles are uniformly dispersed by adding the graphene, so that the catalytic activity of the activated carbon composite material is realized; meanwhile, the mesoporous structure of the activated carbon can be optimized, the specific surface area of the activated carbon is improved, and the material has more excellent performance. The invention has the advantages of easily obtained materials, low cost, easy recovery and environmental protection, not only meets the requirement of practical application, but also improves the high value-added utilization of agricultural and forestry wastes. In addition, the method has simple process and easy operation, and can be widely popularized and used.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples.
Example one
As shown in fig. 1, the activated carbon composite material comprises an activated carbon layer 1 and an organic layer 2 wrapped outside the activated carbon layer 1, wherein a copper hydroxide layer 3 is wrapped outside the activated carbon layer 1 and the organic layer 2. The specific surface area of the activated carbon layer 1 was 2310m2(ii) in terms of/g. The organic layer 2 consists of crude bran, iron salts and terephthalic acid.
A process for preparing an activated carbon composite material comprises the following steps:
(1) dissolving graphene in deionized water, stirring and carrying out ultrasonic treatment to obtain a graphene aqueous solution with the mass concentration of 3.05% for later use;
(2) according to the weight ratio of iron: the graphene is 1: 1, adding the ferric nitrate solution into the graphene aqueous solution prepared in the step (1), uniformly stirring, dripping NaOH solution, adjusting the pH of the mixed solution to be 8, and continuously stirring for more than 40min until the mixed solution is uniformly mixed for later use;
(3) weighing the crude bran and the terephthalic acid according to the mass ratio of 10:1, sequentially adding the crude bran and the terephthalic acid into the mixed solution prepared in the step (2), heating to 350 ℃, and uniformly stirring;
(4) weighing activated carbon and graphene-hydrogen peroxide according to the mass ratio of 2:9, soaking the activated carbon in the graphene-hydrogen peroxide mixed solution to obtain activated carbon, adding the activated carbon into the mixed solution prepared in the step (3), and uniformly stirring; the active carbon is powder with 500 meshes.
In the graphene-hydrogen peroxide mixed solution, the mass fraction of hydrogen peroxide is 3%, and the mass fraction of graphene is 0.03%.
(5) Placing the mixed solution prepared in the step (4) in a closed reaction kettle, and carrying out hydrothermal reaction for 6h at the temperature of 200 ℃;
(6) and (3) taking out the mixed solution after the reaction in the step (5) is finished and cooled, filtering and centrifuging to perform solid-liquid separation, soaking the separated solid in a soaking agent containing ammonia and copper hydroxide, and drying to obtain the iron/crude bran/activated carbon composite material.
Wherein, in the dipping medicament, the mass fraction of ammonia is 20%. The preparation method of the dipping medicament comprises the following steps: adding ammonia water and copper hydroxide dispersion liquid into water, and uniformly mixing, wherein the mass fraction of the ammonia water is 65%, the mass fraction of the copper hydroxide dispersion liquid is 25%, and the mass fraction of the water is 3%.
Example two
An activated carbon composite material comprises an activated carbon layer 1 and an organic layer 2 wrapped outside the activated carbon layer 1, wherein a copper hydroxide layer 3 is wrapped outside the activated carbon layer 1 and the organic layer 2. The specific surface area of the activated carbon layer 1 was 2410m2(ii) in terms of/g. The organic layer 2 consists of crude bran, iron salts and terephthalic acid.
A process for preparing an activated carbon composite material comprises the following steps:
(1) dissolving graphene in deionized water, stirring and performing ultrasonic treatment to obtain a graphene aqueous solution with the mass concentration of 4% for later use;
(2) according to the weight ratio of iron: the graphene is 2: 1, adding a ferric sulfate solution into the graphene aqueous solution prepared in the step (1), uniformly stirring, dripping a KOH solution, adjusting the pH of the mixed solution to 10, and continuously stirring for more than 40min until the mixed solution is uniformly mixed for later use;
(3) weighing the crude bran and the terephthalic acid according to the mass ratio of 1:2, sequentially adding the crude bran and the terephthalic acid into the mixed solution prepared in the step (2), heating to 350 ℃, and uniformly stirring;
(4) weighing activated carbon and graphene-hydrogen peroxide according to the mass ratio of 2:9, soaking the activated carbon in the graphene-hydrogen peroxide mixed solution to obtain activated carbon, adding the activated carbon into the mixed solution prepared in the step (3), and uniformly stirring; the active carbon is powder with 600 meshes.
In the mixed solution of graphene and hydrogen peroxide, the mass fraction of hydrogen peroxide is 12%, and the mass fraction of graphene is 0.7%.
(5) Placing the mixed solution prepared in the step (4) in a closed reaction kettle, and carrying out hydrothermal reaction for 9 hours at the temperature of 300 ℃;
(6) and (3) taking out the mixed solution after the reaction in the step (5) is finished and cooled, filtering and centrifuging to perform solid-liquid separation, soaking the separated solid in a soaking agent containing ammonia and copper hydroxide, and drying to obtain the iron/crude bran/activated carbon composite material.
Wherein, in the dipping medicament, the mass fraction of ammonia is 25%. The preparation method of the dipping medicament comprises the following steps: adding ammonia water and copper hydroxide dispersion liquid into water, and uniformly mixing, wherein the mass fraction of the ammonia water is 75%, the mass fraction of the copper hydroxide dispersion liquid is 35%, and the mass fraction of the water is 12%.
EXAMPLE III
An activated carbon composite material comprises an activated carbon layer 1 and an organic layer 2 wrapped outside the activated carbon layer 1, wherein a copper hydroxide layer 3 is wrapped outside the activated carbon layer 1 and the organic layer 2. The specific surface area of the activated carbon layer 1 was 2340m2(ii) in terms of/g. The organic layer 2 consists of crude bran, iron salts and terephthalic acid.
A process for preparing an activated carbon composite material comprises the following steps:
(1) dissolving graphene in deionized water, stirring and carrying out ultrasonic treatment to obtain a graphene aqueous solution with the mass concentration of 3.35% for later use;
(2) according to the weight ratio of iron: graphene is 1.3: weighing ferric chloride solution according to the mass ratio of 1, adding the ferric chloride solution into the graphene aqueous solution prepared in the step (1), uniformly stirring, dripping ammonia aqueous solution, adjusting the pH of the mixed solution to 9, and continuously stirring for more than 40min until the mixture is uniformly mixed for later use;
(3) weighing the crude bran and the terephthalic acid according to the mass ratio of 10:7, sequentially adding the crude bran and the terephthalic acid into the mixed solution prepared in the step (2), heating to 350 ℃, and uniformly stirring;
(4) weighing activated carbon and graphene-hydrogen peroxide according to the mass ratio of 2:9, soaking the activated carbon in the graphene-hydrogen peroxide mixed solution to obtain activated carbon, adding the activated carbon into the mixed solution prepared in the step (3), and uniformly stirring; the active carbon is powder with 530 meshes.
In the graphene-hydrogen peroxide mixed solution, the mass fraction of hydrogen peroxide is 6%, and the mass fraction of graphene is 0.23%.
(5) Placing the mixed solution prepared in the step (4) in a closed reaction kettle, and carrying out hydrothermal reaction for 7 hours at the temperature of 230 ℃;
(6) and (3) taking out the mixed solution after the reaction in the step (5) is finished and cooled, filtering and centrifuging to perform solid-liquid separation, soaking the separated solid in a soaking agent containing ammonia and copper hydroxide, and drying to obtain the iron/crude bran/activated carbon composite material.
Wherein, in the dipping medicament, the mass fraction of ammonia is 22%. The preparation method of the dipping medicament comprises the following steps: adding ammonia water and copper hydroxide dispersion liquid into water, and uniformly mixing, wherein the mass fraction of the ammonia water is 68%, the mass fraction of the copper hydroxide dispersion liquid is 25-358%, and the mass fraction of the water is 6%.
Example four
An active carbon composite material comprises an active carbon layer and an organic layer wrapped outside the active carbon layer, wherein the active carbon layer and the organic layer are wrapped with copper hydroxide layers. The specific surface area of the activated carbon layer is 2370m2(iv) g. The organic layer consisted of crude bran, iron salt and terephthalic acid.
A process for preparing an activated carbon composite material comprises the following steps:
(1) dissolving graphene in deionized water, stirring and carrying out ultrasonic treatment to obtain a graphene aqueous solution with the mass concentration of 3.65% for later use;
(2) according to the weight ratio of iron: graphene is 1.6: weighing ferric nitrate solution according to the mass ratio of 1, adding the ferric nitrate solution into the graphene aqueous solution prepared in the step (1), uniformly stirring, dripping NaOH solution into the solution, adjusting the pH of the mixed solution to 9, and continuously stirring for more than 40min until the mixture is uniformly mixed for later use;
(3) weighing the crude bran and the terephthalic acid according to the mass ratio of 10:13, sequentially adding the crude bran and the terephthalic acid into the mixed solution prepared in the step (2), heating to 350 ℃, and uniformly stirring;
(4) weighing activated carbon and graphene-hydrogen peroxide according to the mass ratio of 2:9, soaking the activated carbon in the graphene-hydrogen peroxide mixed solution to obtain activated carbon, adding the activated carbon into the mixed solution prepared in the step (3), and uniformly stirring; the active carbon is powder with 560 meshes.
In the graphene-hydrogen peroxide mixed solution, the mass fraction of hydrogen peroxide is 9%, and the mass fraction of graphene is 0.43%.
(5) Placing the mixed solution prepared in the step (4) in a closed reaction kettle, and carrying out hydrothermal reaction for 8 hours at the temperature of 260 ℃;
(6) and (4) taking out the mixed solution after the reaction in the step (5) is finished and cooled, filtering and centrifuging to perform solid-liquid separation, soaking the separated solid in a soaking agent containing ammonia and copper hydroxide, and drying to obtain the iron/coarse bran/active carbon composite material.
Wherein, in the dipping medicament, the mass fraction of ammonia is 24 percent. The preparation method of the dipping medicament comprises the following steps: adding ammonia water and copper hydroxide dispersion liquid into water, and uniformly mixing, wherein the mass fraction of the ammonia water is 71%, the mass fraction of the copper hydroxide dispersion liquid is 31%, and the mass fraction of the water is 9%.
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make variations, modifications, additions or substitutions within the technical scope of the present invention.
Claims (10)
1. An activated carbon composite characterized by: the activated carbon coating comprises an activated carbon layer (1) and an organic layer (2) wrapped outside the activated carbon layer (1), wherein a copper hydroxide layer (3) is wrapped outside the activated carbon layer (1) and the organic layer (2).
2. The activated carbon composite of claim 1, wherein: the specific surface area of the activated carbon layer (1) is 2310-2410m2/g。
3. The activated carbon composite of claim 1, wherein: the organic layer (2) is composed of crude bran, iron salt and terephthalic acid.
4. A process of preparing the activated carbon composite material according to any one of claims 1 to 3, wherein: the process comprises the following steps:
(1) dissolving graphene in deionized water, stirring and performing ultrasonic treatment to obtain a graphene aqueous solution with the mass concentration of 3.05-4% for later use;
(2) according to the weight ratio of iron: the graphene is 1-2: weighing an iron salt solution according to the mass ratio of 1, adding the iron salt solution into the graphene aqueous solution prepared in the step (1), uniformly stirring, dripping an alkaline solution, adjusting the pH of the mixed solution to 8-10, and continuously stirring for more than 40min until the solution is uniformly mixed for later use;
(3) weighing the crude bran and the terephthalic acid according to the mass ratio of 10:1-20, sequentially adding the crude bran and the terephthalic acid into the mixed solution prepared in the step (2), heating to 350 ℃, and uniformly stirring;
(4) weighing activated carbon and graphene-hydrogen peroxide according to the mass ratio of 2:9, soaking the activated carbon in the graphene-hydrogen peroxide mixed solution to obtain activated carbon, adding the activated carbon into the mixed solution prepared in the step (3), and uniformly stirring;
(5) placing the mixed solution prepared in the step (4) in a closed reaction kettle, and carrying out hydrothermal reaction for 6-9h at the temperature of 200-300 ℃;
(6) and (3) taking out the mixed solution after the reaction in the step (5) is finished and cooled, filtering and centrifuging to perform solid-liquid separation, soaking the separated solid in a soaking agent containing ammonia and copper hydroxide, and drying to obtain the iron/crude bran/activated carbon composite material.
5. The process of activated carbon composite of claim 4, wherein: the active carbon is powder, and the mesh number is 500-600 meshes.
6. The process of activated carbon composite of claim 4, wherein: the ferric salt is one or more of ferric nitrate, ferric sulfate and ferric chloride.
7. The process of activated carbon composite of claim 4, wherein: the alkaline solution is as follows: one or more of NaOH solution, KOH solution and ammonia water solution.
8. The process of activated carbon composite of claim 4, wherein: in the graphene-hydrogen peroxide mixed solution, the mass fraction of hydrogen peroxide is 3-12%, and the mass fraction of graphene is 0.03-0.7%.
9. The process of activated carbon composite of claim 4, wherein: in the dipping medicament, the mass fraction of ammonia is 20-25%.
10. The process of activated carbon composite of claim 4, wherein: the preparation method of the impregnation medicament comprises the following steps: adding ammonia water and copper hydroxide dispersion liquid into water, and uniformly mixing, wherein the mass fraction of the ammonia water is 65-75%, the mass fraction of the copper hydroxide dispersion liquid is 25-35%, and the mass fraction of the water is 3-12%.
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