CN104162409B - A kind of effective raising active carbon is to the method for modifying of micro-ammonia absorption property - Google Patents
A kind of effective raising active carbon is to the method for modifying of micro-ammonia absorption property Download PDFInfo
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- CN104162409B CN104162409B CN201410422466.0A CN201410422466A CN104162409B CN 104162409 B CN104162409 B CN 104162409B CN 201410422466 A CN201410422466 A CN 201410422466A CN 104162409 B CN104162409 B CN 104162409B
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Abstract
The present invention relates to a kind of effective raising active carbon to the method for modifying of micro-ammonia absorption property, by the chemical treatment of active carbon through multi-step, the preparation method of this material described is: first active carbon to be modified is placed in reaction vessel, add salpeter solution, stirring reaction under constant temperature; By the activated carbon filtration washing post-drying through preliminary treatment, add and be equipped with in the isothermal reaction container of citric acid solution, after stirring reaction certain hour, filter out active carbon and spend deionized water; Treated active carbon is joined in the reaction vessel of dress butane tetracarboxylic aqueous acid, stirring reaction under constant temperature; By filtering to isolate active carbon, spend deionized water and naturally dry, the active carbon Vacuum Package after having processed is for subsequent use.This activated carbon modified process is simple, and workable, cost is low, and the active carbon prepared in this way effectively can improve the absorption property of active carbon to micro-ammonia in air.
Description
Technical field
The invention belongs to surrounding air field of purification.Be specifically related to a kind of effective raising active carbon to the method for modifying of 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 makes room air pollution be on the rise, wherein the exceeding standard rate of ammonia is higher, occupies the first place of pollution.Indoor ammonia mainly comes out from construction material and finishing material.As the high alkali content expanding admixture in concrete and antifreezing agent etc., the change along with environmental factor can be reduced to ammonia, and discharges from body of wall.In addition in ornamental wood-based planet because of containing urea, cover with paint, lacquer, colour wash, etc. additive and brightening agent because of containing ammoniacal liquor, also ammonia (Liu Xia can be discharged, Li Jing, Xu Fangyuan. passiveness sampling method research [J] of museum's Indoor Micro neutral and alkali gas. environment monitoring management and skill, 2009,21 (2): 13 ~ 17).The quality to residing environmental gas such as special industry it is also proposed higher requirement.The existence of the micro-ammonia in air, often works the mischief to some industries.As: ammonia is as a kind of alkaline gas, and its existence makes the pH of preservation historical relic balance environment be damaged, and affects the life-span of historical relic.As steam, the SO of trace in ammonia and air
2, SO
3or ozone combines, have more for corrosivity necessarily, the color and luster of pigment, animal glue has been had an impact.
Active carbon is a kind of widely used adsorbent, because it has many excellent performances, pore structure as large, excellent in specific area and the surface chemistry of uniqueness, in the separation being widely used in multiple gases and purification process.Normal activated carbon is nonpolar and hydrophobicity, good adsorption effect is had to nonpolar organic matter, but for adsorption effect unsatisfactory (SHaydar, MAFerro-Garcia, the JRivera-Utfilia of formaldehyde, ammonia isopolarity material, etal, Adsorptionofpnitrophenolonanactivatedcarbonwithdifferent oxidations [J], Carbon, 41 (2003), 3,387 ~ 395).Current market exceeds standard for ammonia, main employing is by the active carbon of modification or the purification of other adsorbents, but for low concentration ammonia in room air, commercially available normal activated carbon is limited only by the clean-up effect of physical absorption, is difficult to reach ammonia concentration standard value 0.2mg/m in " Indoor Air Quality standards " (GB/T18883-2002)
3(hourly average), for the requirement that the historical relic's protection environment such as above-mentioned museum are removed micro-ammonia, is difficult to meet more.Therefore, the sorbing material of the removal micro-ammonia that research and development are efficient, applicable, can fill up industry technology blank and have great practical significance.
Summary of the invention
The present invention is directed to current techniques and product exists shortcoming and defect, be intended to solve current various industry to the Environmental capacity problem of low concentration ammonia in air, invented a kind of effective raising active carbon to the method for modifying of micro-ammonia absorption property.
A kind of effective raising active carbon that the present invention proposes, to the method for modifying of micro-ammonia absorption property, is that concrete steps are as follows by the chemical treatment of active carbon through multi-step:
(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, spend deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH value, in less than 100 DEG C oven dry;
(3) active carbon through preliminary treatment that step (2) obtains is added be equipped with in the second reaction vessel of lemon aqueous acid, adopt 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) by filtering to isolate the treated active carbon that step (3) obtains, spend deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH value, in less than 100 DEG C oven dry;
(5) the treated active carbon that step (4) obtains is added be equipped with in the 3rd reaction vessel of butane tetracarboxylic aqueous acid, adopt 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, spend deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH, active carbon dry residing for environment be vacuum, pure nitrogen gas or oxygen purity lower than 5% state, in less than 100 DEG C oven dry.
The scheme that the present invention pollutes with micro-ammonia in existing process air is compared with technology, has following innovation and advantage:
(1) involved in the present invention 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, and by utilizing the distinctive physicochemical properties of this medicament, by oxidation reaction and esterification, effectively improve activated carbon surface acidic-group number, enhanced activity charcoal is to the absorption property of ammonia.
(2) involved in the present invention modifying method of activated carbon advantage is that the activated carbon modified process adopted is simple, and workable, cost is low, has the important feature of environmental protection and splendid market prospects.
(3) the numerous groups contained by active carbon surface can produce certain chemisorbed to ammonia, but the alkaline gas concentration of process highlyer just can reach certain treatment effect.Modified activated carbon involved in the present invention, advantage is that the concentration that can purify containing micro-ammonia (is low to moderate 0.2mg/m
3) air, and purification process non-secondary pollution produce are raw.
Accompanying drawing explanation
Fig. 1 be of the present invention in involved modified activated carbon modification flow chart.
Fig. 2 is modification theory of the present invention diagram.
Detailed description of the invention
Below in conjunction with the instantiation that accompanying drawing and inventor complete according to technical scheme of the present invention, the present invention is described in further detail.
Embodiment 1
Get 150g activated carbon granule, be placed in reaction vessel 1, add the salpeter solution 500mL that mass concentration is 10%, adopt water-bath mode to keep isothermal reaction environment, temperature is 60 DEG C, and the stirring reaction time is 2h; By filtering to isolate treated active carbon, spending deionized water, making the pH of cleaning solution reach 5 ~ 6, then in 80 DEG C of oven dry; Added by active carbon through preliminary treatment in reaction vessel 2, add lemon aqueous acid 500mL in reaction vessel, the mass concentration of citric acid is 10%, and adopt oil bath mode to keep isothermal reaction environment, temperature is 120 DEG C, stirring reaction 4h; Filter out the active carbon through preliminary treatment, spend deionized water, make the pH of cleaning solution reach 5 ~ 6; Added by active carbon in reaction vessel 3, add butane tetracarboxylic aqueous acid 500mL, the mass concentration of BTCA is 10%, and adopt oil bath mode to keep isothermal reaction environment, temperature is 120 DEG C, stirring reaction 4h; By filtering to isolate treated active carbon, spend deionized water, until cleaning solution pH is 5 ~ 6, under vacuum in 80 DEG C of oven dry, the activated carbon sample 1 finished product vacuum preservation obtained is with for subsequent use.
Embodiment 2
Get 150g activated carbon granule, be placed in the first reaction vessel, add the salpeter solution 500mL that mass concentration is 40%, adopt water-bath mode to keep isothermal reaction environment, temperature is 60 DEG C, and the stirring reaction time is 2h; By filtering to isolate treated active carbon, spending deionized water, making the pH of cleaning solution reach 5 ~ 6, then in 80 DEG C of oven dry; Added by active carbon through preliminary treatment in the second reaction vessel, add lemon aqueous acid 500mL in reaction vessel, the mass concentration of citric acid is 10%, and adopt oil bath mode to keep isothermal reaction environment, temperature is 120 DEG C, stirring reaction, 4h; Filter out the active carbon through preliminary treatment, spend deionized water, make the pH of cleaning solution reach 5 ~ 6; Added by active carbon in the 3rd reaction vessel, add butane tetracarboxylic aqueous acid 500mL, the mass concentration of BTCA is 10%, and adopt oil bath mode to keep isothermal reaction environment, temperature is 120 DEG C, stirring reaction 4h; By filtering to isolate treated active carbon, spend deionized water, until cleaning solution pH is 5 ~ 6, under vacuum in 80 DEG C of oven dry, the activated carbon sample 2 finished product vacuum preservation obtained is with for subsequent use.
Embodiment 3
Get 150g activated carbon granule, be placed in the first reaction vessel, add the salpeter solution 500mL that mass concentration is 40%, adopt water-bath mode to keep isothermal reaction environment, temperature is 60 DEG C, and the stirring reaction time is 2h; By filtering to isolate treated active carbon, spending deionized water, making the pH of cleaning solution reach 5 ~ 6, then in 80 DEG C of oven dry; Added by active carbon through preliminary treatment in the second reaction vessel, add lemon aqueous acid 500mL in reaction vessel, the mass concentration of citric acid is 25%, and adopt oil bath mode to keep isothermal reaction environment, temperature is 120 DEG C, stirring reaction, 4h; Filter out the active carbon through preliminary treatment, spend deionized water, make the pH of cleaning solution reach 5 ~ 6; Added by active carbon in the 3rd reaction vessel, add butane tetracarboxylic aqueous acid 500mL, the mass concentration of BTCA is 25%, and adopt oil bath mode to keep isothermal reaction environment, temperature is 120 DEG C, stirring reaction 4h; By filtering to isolate treated active carbon, spending deionized water, until cleaning solution pH is 5 ~ 6, drying under vacuum, the activated carbon sample 3 finished product vacuum preservation obtained is with for subsequent use.
Adopt air tank to store containing the compressed air of certain density ammonia, make to get the active carbon blank sample 4 of obtained activated carbon sample 1, sample 2, sample 3 and non-modified process, carry out Static Adsorption test, to test its clean-up effect.The modified active carbon of primary concern is to the adsorption efficiency of 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.By measuring the concentration by the ammonia before and after adsorption column, calculate removal efficiency, specific experiment data are in table 1.
The purification adsorption efficiency table of the modified active carbon of table 1
Claims (1)
1. effectively improve active carbon to a method of modifying for micro-ammonia absorption property, be by the chemical treatment of active carbon through multi-step, 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 salpeter solution 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, spend deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH value, in less than 100 DEG C oven dry;
(3) active carbon through preliminary treatment that step (2) obtains is added be equipped with in the second reaction vessel of lemon aqueous acid, adopt 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) by filtering to isolate the treated active carbon that step (3) obtains, spend deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH value, in less than 100 DEG C oven dry;
(5) the treated active carbon that step (4) obtains is added be equipped with in the 3rd reaction vessel of butane tetracarboxylic aqueous acid, adopt 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, spend deionized water, washing active carbon is 5 ~ 7 to cleaning solution pH, active carbon dry residing for environment be vacuum, pure nitrogen gas or oxygen purity lower than 5% state, in less than 100 DEG C oven dry.
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| 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 |
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