CN104162409A - Modification method for effectively improving adsorption performance of activated carbon on trace ammonia - Google Patents
Modification method for effectively improving adsorption performance of activated carbon on trace ammonia Download PDFInfo
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- CN104162409A CN104162409A CN201410422466.0A CN201410422466A CN104162409A CN 104162409 A CN104162409 A CN 104162409A CN 201410422466 A CN201410422466 A CN 201410422466A CN 104162409 A CN104162409 A CN 104162409A
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Abstract
The invention relates to a modification method for effectively improving the adsorption performance of activated carbon on trace ammonia. The activated carbon is treated in a chemical way by adopting a plurality of steps; the preparation method of a material comprises the steps of putting the activated carbon to be modified into a reaction vessel, feeding a nitric acid solution into the reaction vessel, and carrying out mixing reaction under the constant temperature condition; after primary treatment, filtering and washing the activated carbon, and drying to obtain dried activated carbon; putting the dried activated carbon into a constant temperature reaction vessel filled with a citric acid solution, stirring and carrying out reaction for a period of time; filtering out the activated carbon and washing the activated carbon by deionized water so as to obtain treated activated carbon; feeding the treated activated carbon into a reaction vessel filled with a butane-tetracarboxylic acid water solution, and carrying out stirring reaction under the constant temperature condition; separating the activated carbon in a filtering manner, washing the separated activated carbon by deionized water, and naturally drying so as to obtain dried activated carbon; and carrying out vacuum encapsulation on the dried activated carbon for later use. The activated carbon modification process is simple, high in operability and low in cost; the activated carbon prepared by adopting the method is capable of effectively improving the adsorption performance of the activated carbon on the trace ammonia in the air.
Description
Technical field
The invention belongs to surrounding air field of purification.Be specifically related to the method for modifying of a kind of effective raising active carbon to micro-ammonia absorption property.
Background technology
Along with expanding economy, pursuit work, quality of life become the focus that people are concerned about day by day.And the introducing of the rise of interior decoration and all kinds of Modern Live articles for use is on the rise room air pollution, wherein the exceeding standard rate of ammonia is higher, occupies the first place of pollution.Indoor ammonia is mainly to come out from construction material and finishing material.As high alkali content expanding admixture and antifreezing agent etc. in concrete, along with the variation of environmental factor can be reduced to ammonia, and discharge from body of wall.In addition in ornamental wood-based planet because containing urea, cover with paint, lacquer, colour wash, etc. additive and brightening agent because containing ammoniacal liquor, also can discharge ammonia (Liu Xia, Li Jing, Xu Fangyuan. the passiveness sampling method research [J] of museum's Indoor Micro neutral and alkali gas. environmental monitoring management and skill, 2009,21 (2): 13 ~ 17).Special industries etc. are also had higher requirement to the quality of environmental gas of living in.The existence of airborne micro-ammonia, often works the mischief to some industries.As: ammonia is as a kind of alkaline gas, and its existence is damaged the pH balance environment of preserving historical relic, affects the life-span of historical relic.As steam, the SO of trace in ammonia and air
2, SO
3or ozone combination, have more for corrosivity necessarily, the color and luster of pigment, animal glue is exerted an influence.
Active carbon is a kind of widely used adsorbent, because it has many good performances, pore structure as large, good in specific area and unique surface chemistry, be widely used in the separation and purification process of multiple gases.Common active carbon is nonpolar and hydrophobicity, nonpolar organic matter is had to good adsorption effect, but the adsorption effect for formaldehyde, ammonia isopolarity material unsatisfactory (S Haydar, M A Ferro-Garcia, J Rivera-Utfilia, etal, Adsorption of pnitrophenol on an activated carbon with different oxidations[J], Carbon, 41 (2003), 3,387 ~ 395).Currently exceed standard for ammonia on the market, main employing by active carbon or other adsorbents of modification purifies, but for low concentration ammonia in room air, commercially available common active carbon is only limited by the clean-up effect of physical absorption, is difficult to reach ammonia concentration standard value 0.2mg/m in " IAQ standard " (GB/T 18883-2002)
3(hourly average), the requirement of micro-ammonia being removed for historical relic's protection environment such as above-mentioned museums, is difficult to meet more.Therefore, research and develop the sorbing material of efficient, applicable removal micro-ammonia, can fill up industry technology blank and there is great practical significance.
Summary of the invention
The present invention is directed to current techniques and product existent defect and deficiency, be intended to solve the pollution control problem of current various industry to low concentration ammonia in air, invented the method for modifying of a kind of effective raising active carbon to micro-ammonia absorption property.
The method of modifying of a kind of effective raising active carbon that the present invention proposes to micro-ammonia absorption property, is the chemical treatment through multi-step by active carbon, and concrete steps are as follows:
(1) get active carbon and be placed in the first reaction vessel, and add salpeter solution, adopt water-bath mode stirring reaction under constant temperature; The mass ratio of active carbon and nitric acid is 1:2 ~ 1:5, and the mass concentration of nitric acid is 10% ~ 50%, and under constant temperature, reaction temperature is 50 ~ 80 DEG C, reaction time 1 ~ 3h, and course of reaction fully stirs;
(2) by filtering to isolate treated active carbon, with deionized water washing, washing active carbon is 5 ~ 7 to cleaning solution pH value, in 100 DEG C of following oven dry;
(3) active carbon through preliminary treatment step (2) being obtained adds in the second reaction vessel that lemon aqueous acid is housed, and adopts oil bath mode stirring reaction under constant temperature; The mass ratio of active carbon and lemon aqueous acid is 1:2 ~ 1:5, and the mass concentration of citric acid is 10% ~ 40%, and isothermal reaction temperature is 100 ~ 170 DEG C, reaction 2 ~ 6h, and course of reaction fully stirs;
(4) the treated active carbon obtaining by filtering to isolate step (3), with deionized water washing, washing active carbon is 5 ~ 7 to cleaning solution pH value, in 100 DEG C of following oven dry;
(5) treated active carbon step (4) being obtained adds in the 3rd reaction vessel that butane tetracarboxylic aqueous acid is housed, and adopts stirring reaction under oil bath mode constant temperature; The mass ratio of active carbon and butane tetracarboxylic aqueous acid is 1:2 ~ 1:5, and the mass concentration of BTCA is 10% ~ 45%, and isothermal reaction temperature is 100 ~ 170 DEG C, reaction 2 ~ 6h, and course of reaction fully stirs;
(6) by filtering to isolate treated active carbon, wash by deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH, and it is vacuum, pure nitrogen gas or oxygen purity lower than 5% state that active carbon is dried residing environment, in 100 DEG C of following oven dry.
The present invention compares with technology with the scheme that micro-ammonia in existing processing air pollutes, and has following innovation and advantage:
(1) in the present invention, related modifying method of activated carbon innovation is that the material modified of employing is active carbon, and improved chemical is nitric acid, citric acid and BTCA.Improved chemical is simple and easy to get, by utilizing the distinctive physicochemical properties of this medicament, by oxidation reaction and esterification, effectively improves activated carbon surface acidic-group number, the absorption property of enhanced activity charcoal to ammonia.
(2) in the present invention, related modifying method of activated carbon advantage is that the activated carbon modified process adopting is simple, workable, and cost is low, has the important feature of environmental protection and splendid market prospects.
(3) the contained numerous groups of common activated carbon surface can produce certain chemisorbed to ammonia, just can reach certain treatment effect but the alkaline gas concentration of processing is higher.Related modified activated carbon in the present invention, the concentration that advantage is to purify containing micro-ammonia (is low to moderate 0.2 mg/m
3) air, and purification process non-secondary pollution deposits yields.
Brief description of the drawings
Fig. 1 be of the present invention in related modified activated carbon modification flow chart.
Fig. 2 is modification theory diagram of the present invention.
Detailed description of the invention
Comply with below in conjunction with accompanying drawing and inventor the instantiation that technical scheme of the present invention completes, the present invention is described in further detail.
Embodiment 1
Get 150g activated carbon granule, be placed in reaction vessel 1, adding mass concentration is 10% salpeter solution 500mL, adopts water-bath mode to keep isothermal reaction environment, and temperature is 60 DEG C, and the stirring reaction time is 2h; By filtering to isolate treated active carbon, with deionized water washing, make the pH of cleaning solution reach 5 ~ 6, then in 80 DEG C of oven dry; Active carbon through preliminary treatment is added in reaction vessel 2, in reaction vessel, add lemon aqueous acid 500mL, the mass concentration of citric acid is 10%, adopts oil bath mode to keep isothermal reaction environment, and temperature is 120 DEG C, stirring reaction 4h; Filter out the active carbon through preliminary treatment, with deionized water washing, make the pH of cleaning solution reach 5 ~ 6; Active carbon is added in reaction vessel 3, add butane tetracarboxylic aqueous acid 500mL, the mass concentration of BTCA is 10%, adopts oil bath mode to keep isothermal reaction environment, and temperature is 120 DEG C, stirring reaction 4h; By filtering to isolate treated active carbon, with deionized water washing, until cleaning solution pH is 5 ~ 6, under vacuum condition, in 80 DEG C of oven dry, the activated carbon sample 1 finished product vacuum preservation obtaining is with for subsequent use.
Embodiment 2
Get 150g activated carbon granule, be placed in the first reaction vessel, adding mass concentration is 40% salpeter solution 500mL, adopts water-bath mode to keep isothermal reaction environment, and temperature is 60 DEG C, and the stirring reaction time is 2h; By filtering to isolate treated active carbon, with deionized water washing, make the pH of cleaning solution reach 5 ~ 6, then in 80 DEG C of oven dry; Active carbon through preliminary treatment is added in the second reaction vessel, in reaction vessel, add lemon aqueous acid 500mL, the mass concentration of citric acid is 10%, adopts oil bath mode to keep isothermal reaction environment, and temperature is 120 DEG C, stirring reaction, 4h; Filter out the active carbon through preliminary treatment, with deionized water washing, make the pH of cleaning solution reach 5 ~ 6; Active carbon is added in the 3rd reaction vessel, add butane tetracarboxylic aqueous acid 500mL, the mass concentration of BTCA is 10%, adopts oil bath mode to keep isothermal reaction environment, and temperature is 120 DEG C, stirring reaction 4h; By filtering to isolate treated active carbon, with deionized water washing, until cleaning solution pH is 5 ~ 6, under vacuum condition, in 80 DEG C of oven dry, the activated carbon sample 2 finished product vacuum preservations that obtain are with for subsequent use.
Embodiment 3
Get 150g activated carbon granule, be placed in the first reaction vessel, adding mass concentration is 40% salpeter solution 500mL, adopts water-bath mode to keep isothermal reaction environment, and temperature is 60 DEG C, and the stirring reaction time is 2h; By filtering to isolate treated active carbon, with deionized water washing, make the pH of cleaning solution reach 5 ~ 6, then in 80 DEG C of oven dry; Active carbon through preliminary treatment is added in the second reaction vessel, in reaction vessel, add lemon aqueous acid 500mL, the mass concentration of citric acid is 25%, adopts oil bath mode to keep isothermal reaction environment, and temperature is 120 DEG C, stirring reaction, 4h; Filter out the active carbon through preliminary treatment, with deionized water washing, make the pH of cleaning solution reach 5 ~ 6; Active carbon is added in the 3rd reaction vessel, add butane tetracarboxylic aqueous acid 500mL, the mass concentration of BTCA is 25%, adopts oil bath mode to keep isothermal reaction environment, and temperature is 120 DEG C, stirring reaction 4h; By filtering to isolate treated active carbon, with deionized water washing, until cleaning solution pH is 5 ~ 6, under vacuum condition, to dry, the activated carbon sample 3 finished product vacuum preservations that obtain are with for subsequent use.
Adopt air tank to store the compressed air containing certain density ammonia, make to get the active carbon blank sample 4 of the activated carbon sample 1, sample 2, sample 3 and the non-modified processing that make, carry out Static Adsorption test, to test its clean-up effect.Mainly consider active carbon after the modification adsorption efficiency to Ammonia in Air gas.Adsorption column is of a size of 35mm × 150mm, and air draught amount is 110mL/min, and experimental temperature is 30 ~ 35 DEG C.Pass through the concentration of the ammonia before and after adsorption column by mensuration, calculate removal efficiency, specific experiment data are in table 1.
The purification adsorption efficiency table of active carbon after table 1 modification
Claims (1)
1. effectively improving the method for modifying of active carbon to micro-ammonia absorption property, is the chemical treatment through multi-step by active carbon, it is characterized in that concrete steps are as follows:
(1) get active carbon and be placed in the first reaction vessel, and add salpeter solution, adopt water-bath mode stirring reaction under constant temperature; The mass ratio of active carbon and nitric acid is 1:2 ~ 1:5, and the mass concentration of nitric acid is 10% ~ 50%, and under constant temperature, reaction temperature is 50 ~ 80 DEG C, reaction time 1 ~ 3h, and course of reaction fully stirs;
(2) by filtering to isolate treated active carbon, with deionized water washing, washing active carbon is 5 ~ 7 to cleaning solution pH value, in 100 DEG C of following oven dry;
(3) active carbon through preliminary treatment step (2) being obtained adds in the second reaction vessel that lemon aqueous acid is housed, and adopts oil bath mode stirring reaction under constant temperature; The mass ratio of active carbon and lemon aqueous acid is 1:2 ~ 1:5, and the mass concentration of citric acid is 10% ~ 40%, and isothermal reaction temperature is 100 ~ 170 DEG C, reaction 2 ~ 6h, and course of reaction fully stirs;
(4) the treated active carbon obtaining by filtering to isolate step (3), with deionized water washing, washing active carbon is 5 ~ 7 to cleaning solution pH value, in 100 DEG C of following oven dry;
(5) treated active carbon step (4) being obtained adds in the 3rd reaction vessel that butane tetracarboxylic aqueous acid is housed, and adopts stirring reaction under oil bath mode constant temperature; The mass ratio of active carbon and butane tetracarboxylic aqueous acid is 1:2 ~ 1:5, and the mass concentration of BTCA is 10% ~ 45%, and isothermal reaction temperature is 100 ~ 170 DEG C, reaction 2 ~ 6h, and course of reaction fully stirs;
(6) by filtering to isolate treated active carbon, wash by deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH, and it is vacuum, pure nitrogen gas or oxygen purity lower than 5% state that active carbon is dried residing environment, in 100 DEG C of following oven dry.
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| CN104162409B CN104162409B (en) | 2016-04-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574008A (en) * | 2018-12-03 | 2019-04-05 | 昆明理工大学 | A kind of preparation method and application of ammonium thiocyanate modified activated carbon |
| CN111821944A (en) * | 2020-07-07 | 2020-10-27 | 美埃(中国)环境科技股份有限公司 | Active carbon modification method for removing ammonia gas in air |
| CN114763264A (en) * | 2021-01-11 | 2022-07-19 | 中国石油化工股份有限公司 | Process for preparing activated carbon by alkali activation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63178822A (en) * | 1987-01-20 | 1988-07-22 | Matsushita Electric Ind Co Ltd | Filter for cleaning air |
| CN102627277A (en) * | 2012-04-11 | 2012-08-08 | 太原理工大学 | Modified active carbon and method for removing ammonia gas in intensive livestock farm |
-
2014
- 2014-08-26 CN CN201410422466.0A patent/CN104162409B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63178822A (en) * | 1987-01-20 | 1988-07-22 | Matsushita Electric Ind Co Ltd | Filter for cleaning air |
| CN102627277A (en) * | 2012-04-11 | 2012-08-08 | 太原理工大学 | Modified active carbon and method for removing ammonia gas in intensive livestock farm |
Non-Patent Citations (1)
| Title |
|---|
| 盛丽丽 等: ""改性活性炭对氨气吸附性能研究"", 《林产化学与工业》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574008A (en) * | 2018-12-03 | 2019-04-05 | 昆明理工大学 | A kind of preparation method and application of ammonium thiocyanate modified activated carbon |
| CN109574008B (en) * | 2018-12-03 | 2022-03-08 | 昆明理工大学 | Preparation method and application of ammonium thiocyanate modified activated carbon |
| CN111821944A (en) * | 2020-07-07 | 2020-10-27 | 美埃(中国)环境科技股份有限公司 | Active carbon modification method for removing ammonia gas in air |
| CN114763264A (en) * | 2021-01-11 | 2022-07-19 | 中国石油化工股份有限公司 | Process for preparing activated carbon by alkali activation method |
| CN114763264B (en) * | 2021-01-11 | 2024-05-03 | 中国石油化工股份有限公司 | Process for preparing active carbon by alkali activation method |
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