CN111389361A - Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon - Google Patents
Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon Download PDFInfo
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- CN111389361A CN111389361A CN202010236412.0A CN202010236412A CN111389361A CN 111389361 A CN111389361 A CN 111389361A CN 202010236412 A CN202010236412 A CN 202010236412A CN 111389361 A CN111389361 A CN 111389361A
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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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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0281—Sulfates of compounds other than those provided for in B01J20/045
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3214—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
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- Chemical Kinetics & Catalysis (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for preparing ammonia-free impregnated carbon by using a Fehling reagent loaded with activated carbon, which comprises the following steps: (1) preparing a liquid A: weighing deionized water according to 100% of the water capacity of the activated carbon, weighing 5-20% (weight) of sodium hydroxide and 15-40% (weight) of potassium sodium tartrate, heating the deionized water to 40-80 ℃, and sequentially adding and uniformly mixing; (2) and preparing a solution B: deionized water is measured according to 100% of the water capacity of the activated carbon, 10% -30% (by weight) of copper sulfate is weighed, and the copper sulfate is added at the water temperature of 40-80 ℃ and is fully dissolved. The ammonia-free impregnated carbon is prepared by loading a Fehling reagent and glucose on active carbon, does not generate toxic and harmful substances in the preparation process, abandons common ammonia water as a solvent, replaces the solvent with water, and has the advantages of easily obtained active components, simple preparation method and low cost.
Description
Technical Field
The invention relates to the technical field of impregnated carbon preparation, in particular to a method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded activated carbon.
Background
Currently, the production of impregnated carbon in various countries in the world mainly uses ammonia water as a solvent to impregnate active components of metal compounds, and the common method is to firstly dissolve the metal compounds by using the ammonia water to prepare impregnation liquid, fully impregnate an active carbon carrier, and calcine the impregnated carbon at high temperature after impregnation to obtain the impregnated carbon. The loaded metal ammonia complex is decomposed in the high-temperature calcination process to generate metal oxide, and ammonia is removed at the same time. Is applied to gas masks, canister and canister of gas collecting equipment, and is used up to now.
However, in some regions, due to high temperature and high humidity of climate environment, ammonia smell can escape when the impregnated carbon in the canister is used after being stored for a long time, and uncomfortable symptoms such as lacrimation, pharyngalgia, cough and the like can occur after the impregnated carbon is inhaled by a human body, so that the health of users is affected.
Disclosure of Invention
The invention aims to provide a method for preparing ammonia-free impregnated carbon by using a Fehling reagent loaded with activated carbon. The preparation process does not involve ammonia substances, and the ammonia odor cannot escape when the ammonia odor-free hydrogen cyanide protective agent is applied to gas masks and canister and has a certain protection effect on hydrocyanic acid.
The invention is realized by adopting the following technical scheme:
a method for preparing ammonia-free impregnated carbon by using a Fehling reagent loaded with activated carbon comprises the steps of weighing a certain weight of activated carbon and adopting an excess impregnation method. The method comprises the following steps:
(1) preparing a liquid A: weighing deionized water according to 100% of the water capacity of the activated carbon, weighing 5-20% (weight) of sodium hydroxide and 15-40% (weight) of potassium sodium tartrate, heating the deionized water to 40-80 ℃, and sequentially adding and uniformly mixing;
(2) and preparing a solution B: deionized water is measured according to 100% of the water capacity of the activated carbon, 10% -30% (by weight) of copper sulfate is weighed and added at the water temperature of 40-80 ℃, and the activated carbon is fully dissolved;
(3) mixing the solution A and the solution B, pouring the mixture on an equal amount of activated carbon carriers, continuously stirring, soaking for 3-5 hours under magnetic stirring after full impregnation, then adding 5-20 wt% of glucose, standing for 1-2 hours after complete reaction, and calcining and drying at 80-150 ℃ to obtain the ammonia-free impregnated carbon.
Currently, the commercially available impregnated carbon mainly uses activated carbon as a carrier, and different active components are loaded in ammonia water to achieve the purpose of protective performance, but ammonia odor can escape when the impregnated carbon is used under the conditions of high temperature and high humidity. The ammonia-free impregnated carbon is prepared by loading a Fehling reagent and glucose on active carbon, does not generate toxic and harmful substances in the preparation process, abandons common ammonia water as a solvent, replaces the solvent with water, and has the advantages of easily obtained active components, simple preparation method and low cost.
Detailed Description
The following provides a detailed description of specific embodiments of the present invention.
The embodiment of the invention selects coal-based activated carbon as a carrier material, adopts an excess impregnation method to load a Fehling reagent, and the balance of activated carbon, and is soaked for a period of time under magnetic stirring, and then dextrose is added. Wherein, the fibulin reagent is mainly prepared by mixing a solution A consisting of sodium hydroxide and sodium potassium tartrate, and a solution B consisting of copper sulfate and sulfuric acid, and the dextrose is derived from glucose.
Example 1
Firstly, preparing a Fehling reagent:
liquid A: weighing 100ml of deionized water, weighing 10g of sodium hydroxide and 34.6g of potassium sodium tartrate, heating the deionized water to 40-80 ℃, and sequentially adding and uniformly mixing.
B, liquid B: weighing 100ml of deionized water, weighing 17.3g of copper sulfate, adding 1-2 drops of sulfuric acid deionized water by a dropper, heating to 40-80 ℃, and adding for full dissolution.
And mixing the solution A and the solution B in equal volume, adding 100g of activated carbon, soaking for 4 hours under magnetic stirring, adding 11g of glucose, standing for 2 hours after complete reaction, and calcining and drying at 100-130 ℃ to obtain the ammonia-free impregnated carbon.
Example 2
Firstly, preparing a Fehling reagent:
liquid A: weighing 100ml of deionized water, weighing 15g of sodium hydroxide and 52g of potassium sodium tartrate, heating the deionized water to 40-80 ℃, and sequentially adding and uniformly mixing.
B, liquid B: weighing 100ml of deionized water, weighing 26g of copper sulfate, adding 1-2 drops of sulfuric acid deionized water by a dropper, heating to 40-80 ℃, and adding for full dissolution.
And mixing the solution A and the solution B in equal volume, adding 100g of activated carbon, soaking for 4 hours under magnetic stirring, adding 16.5g of glucose, standing for 2 hours after complete reaction, and calcining and drying at 100-130 ℃ to obtain the ammonia-free impregnated carbon.
The protection effect of the ammonia-free impregnated carbon prepared by the embodiment of the invention on hydrocyanic acid is shown in the following table 1:
TABLE 1 protection time of non-ammonia impregnated carbon against hydrocyanic acid
As can be seen from table 1: the ammonia-free impregnated carbon samples (example 1 and example 2) prepared in the embodiment of the invention can achieve effective protection of hydrocyanic acid (more than or equal to 30 min) by referring to a GJB6239.18-2008 test method, and compared with commercially available impregnated carbon, the protection performance is not greatly different.
The fibhlin reagent in the above embodiments can be replaced by banbury reagent, glucose can be replaced by dextrose, and activated carbon can be replaced by adsorption material such as zeolite, ceramic, etc. Firstly preparing excessive Fehling reagent, then adding activated carbon and stirring, and finally adding dextrose to fully react, wherein brick red precipitate is generated in the reaction process. And placing for a period of time, calcining and drying to obtain the ammonia-free impregnated carbon. The impregnated carbon has the advantages of easily obtained materials and active components, simple preparation method, low cost, no escape of ammonia smell in the use process, and no harm to human body. The prepared ammonia-free impregnated carbon has a good elimination effect on the hydrocyanic acid gas, and the preparation method is simple, low in cost and high in feasibility.
Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention.
Claims (1)
1. A method for preparing ammonia-free impregnated carbon by using a Fehling reagent loaded with activated carbon is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a liquid A: weighing deionized water according to 100% of the water capacity of the activated carbon, weighing 5-20% (weight) of sodium hydroxide and 15-40% (weight) of potassium sodium tartrate, heating the deionized water to 40-80 ℃, and sequentially adding and uniformly mixing;
(2) and preparing a solution B: deionized water is measured according to 100% of the water capacity of the activated carbon, 10% -30% (by weight) of copper sulfate is weighed and added at the water temperature of 40-80 ℃, and the activated carbon is fully dissolved;
(3) mixing the solution A and the solution B, pouring the mixture on an equal amount of activated carbon carriers, continuously stirring, soaking for 3-5 hours under magnetic stirring after full impregnation, then adding 5-20 wt% of glucose, standing for 1-2 hours after complete reaction, and calcining and drying at 80-150 ℃ to obtain the ammonia-free impregnated carbon.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113477216A (en) * | 2021-07-19 | 2021-10-08 | 山西新华防化装备研究院有限公司 | Method for preparing adsorbent for protecting cyanide by adding organic acid |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113477216A (en) * | 2021-07-19 | 2021-10-08 | 山西新华防化装备研究院有限公司 | Method for preparing adsorbent for protecting cyanide by adding organic acid |
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