[go: up one dir, main page]

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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
activated carbon
ammonia
carbon
water
preparing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010236412.0A
Other languages
Chinese (zh)
Inventor
裴佩
安丽花
金彦任
郭军军
王德周
胡元宏
魏志凤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanxi Xinhua Chemical Industry Co Ltd
Original Assignee
Shanxi Xinhua Chemical Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanxi Xinhua Chemical Industry Co Ltd filed Critical Shanxi Xinhua Chemical Industry Co Ltd
Priority to CN202010236412.0A priority Critical patent/CN111389361A/en
Publication of CN111389361A publication Critical patent/CN111389361A/en
Pending legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid 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
    • B01J20/0233Compounds of Cu, Ag, Au
    • B01J20/0237Compounds of Cu
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid 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
    • B01J20/0274Solid 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
    • B01J20/0281Sulfates of compounds other than those provided for in B01J20/045
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3214Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating

Landscapes

  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • 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

Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon
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
Figure DEST_PATH_IMAGE001
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.
CN202010236412.0A 2020-03-30 2020-03-30 Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon Pending CN111389361A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010236412.0A CN111389361A (en) 2020-03-30 2020-03-30 Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010236412.0A CN111389361A (en) 2020-03-30 2020-03-30 Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon

Publications (1)

Publication Number Publication Date
CN111389361A true CN111389361A (en) 2020-07-10

Family

ID=71416615

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010236412.0A Pending CN111389361A (en) 2020-03-30 2020-03-30 Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon

Country Status (1)

Country Link
CN (1) CN111389361A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
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

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1036433A (en) * 1962-02-16 1966-07-20 Gen Electric Co Ltd Improvements in or relating to the formation of a copper layer on an electrically non-conducting support
US3630958A (en) * 1968-12-19 1971-12-28 Miles Lab Test composition and method for detecting reducing sugars in aqueous fluids
US5300271A (en) * 1990-08-23 1994-04-05 Air Products And Chemicals, Inc. Method for separation of carbon monoxide by highly dispersed cuprous compositions
CN102120176A (en) * 2010-12-11 2011-07-13 山西新华化工有限责任公司 Preparation method of asphalt ball impregnation carbon for protecting H2S and NH3
CN102580742A (en) * 2012-02-05 2012-07-18 淮北师范大学 Activated carbon-loaded cuprous oxide photocatalyst and preparation method thereof
CN103071497A (en) * 2012-12-31 2013-05-01 天津大学 Activated carbon load single valence state cuprous oxide chloride-free catalyst, preparation method, and application in oxidate oxo synthesis dimethyl carbonate
US20170203281A1 (en) * 2016-01-19 2017-07-20 Bharat Petroleum Corporation Ltd. Method of preparation of mixed metal oxide using glucose oxidation assisted precipitation
CN110482604A (en) * 2019-07-25 2019-11-22 广东工业大学 A kind of Cu2V2O7Nanometer rods kalium ion battery positive electrode, kalium ion battery and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1036433A (en) * 1962-02-16 1966-07-20 Gen Electric Co Ltd Improvements in or relating to the formation of a copper layer on an electrically non-conducting support
US3630958A (en) * 1968-12-19 1971-12-28 Miles Lab Test composition and method for detecting reducing sugars in aqueous fluids
US5300271A (en) * 1990-08-23 1994-04-05 Air Products And Chemicals, Inc. Method for separation of carbon monoxide by highly dispersed cuprous compositions
CN102120176A (en) * 2010-12-11 2011-07-13 山西新华化工有限责任公司 Preparation method of asphalt ball impregnation carbon for protecting H2S and NH3
CN102580742A (en) * 2012-02-05 2012-07-18 淮北师范大学 Activated carbon-loaded cuprous oxide photocatalyst and preparation method thereof
CN103071497A (en) * 2012-12-31 2013-05-01 天津大学 Activated carbon load single valence state cuprous oxide chloride-free catalyst, preparation method, and application in oxidate oxo synthesis dimethyl carbonate
US20170203281A1 (en) * 2016-01-19 2017-07-20 Bharat Petroleum Corporation Ltd. Method of preparation of mixed metal oxide using glucose oxidation assisted precipitation
CN110482604A (en) * 2019-07-25 2019-11-22 广东工业大学 A kind of Cu2V2O7Nanometer rods kalium ion battery positive electrode, kalium ion battery and preparation method thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
KAKARLA RAGHAVA REDDY ET AL: "A new one-step synthesis method for coating multi-walled carbon nanotubes with cuprous oxide nanoparticles", 《SCRIPTA MATERIALIA》 *
LIANG, SH ET AL: "Adsorption of HCN onto Copper@Copper-oxide Core-Shell Nanoparticle Systems", 《ADSORPTION SCIENCE & TECHNOLOGY 》 *
秦浩正 总主编: "《中学生学习辞典 化学卷》", 30 September 2012, 世界图书上海出版公司 *
郭红梅 等: "采用炭基复合材料降解卷烟烟气中有害成分", 《山东化工》 *
闫冰: "氧化羰基合成碳酸酯炭材料负载铜基催化剂的研究", 《中国优秀博硕士学位论文全文数据库(博士)工程科技I辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
US2511288A (en) Preparation of a protective adsorbent carbon
US2920050A (en) Whetlerite product and process
CN111389362B (en) Nickel-loaded impregnated carbon for protecting HCN and CNCl and preparation method thereof
CN110773156A (en) Transition metal monatomic catalyst, preparation method and application thereof
CN105107498A (en) Method for preparing carbon-loaded gold catalyst and application of catalyst
CN111389361A (en) Method for preparing ammonia-free impregnated carbon by using Fehling reagent loaded with activated carbon
CN104841466B (en) A kind of biological oil base oxygenatedchemicals hydrogenation deoxidation catalyst and preparation method thereof
CN110161097B (en) Preparation of ferric oxide-silver modified tin dioxide nano material for gas sensor, product and application
CN109574008A (en) A kind of preparation method and application of ammonium thiocyanate modified activated carbon
Wang et al. Yeast‐raised polyamidoxime hydrogel prepared by ice crystal dispersion for efficient uranium extraction from Seawater
CN102151573A (en) Preparation method of low-mercury catalyst for preparing vinyl chloride
CN102441409B (en) Composite low mercury catalyst used for synthesizing vinyl chloride
CN102009969A (en) Method for treating anode material lithium iron phosphate of lithium ion battery
CN103394324A (en) Load-type dearsenic agent and preparation method
CN105036108B (en) A kind of method that utilizes corn leaf to prepare electrode carbon material of sodium ion battery
CN113477216A (en) Method for preparing adsorbent for protecting cyanide by adding organic acid
CN100402140C (en) Sulfur-proof deoxidizing agent and its preparing and use
CN113501895A (en) Preparation method of catalyst for mercury-free synthesis of polyvinyl chloride
WO2024037662A1 (en) Preparation method for and use of bismuth ion filter membrane
CN116773302A (en) Detection method for adsorbing heavy metal mercury in micro-plastic
CN109833879A (en) A kind of residual oil hydrocatalyst and preparation method thereof
CN114602487A (en) Sulfur-tolerant deoxygenation catalyst and preparation method and application thereof
CN107597144A (en) Protect the preparation method of arsenic hydride impregnated carbon
CN116747890B (en) Preparation and application of electrochemical catalysts of BN-loaded doped and modified metal oxides
CN115121221A (en) Loaded CeO 2 Preparation method of CuO ammonia-free system activated carbon

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20200710

RJ01 Rejection of invention patent application after publication