CN103721681B - The preparation method of protective material for perfluoroisobutyleneand - Google Patents
The preparation method of protective material for perfluoroisobutyleneand Download PDFInfo
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- CN103721681B CN103721681B CN201310596572.6A CN201310596572A CN103721681B CN 103721681 B CN103721681 B CN 103721681B CN 201310596572 A CN201310596572 A CN 201310596572A CN 103721681 B CN103721681 B CN 103721681B
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Abstract
The present invention relates to protective material, it is specially the preparation method of a kind of protective material for perfluoroisobutyleneand, comprise the steps: that (1), described protective material for perfluoroisobutyleneand include the activated carbon as carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 3%～10%(weight) Cu, 0.1%～5%(weight) Zn, 4%～9%(weight) many amine compounds TEDA；By the impregnating agent of active component, the i.e. content according to active component Cu and Zn calculates the amount of basic copper carbonate, zinc carbonate respectively, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 60 80 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 1 2h.The present invention is reasonable in design, and selecting activated carbon is carrier framework material, and load is with metal active constituents such as Cu, Zn, it is provided that its preparation method of a kind of perfluoroisobutylene protection.
Description
Technical field
The present invention relates to protective material, the preparation method of a kind of protective material for perfluoroisobutyleneand.
Background technology
Perfluoroisobutylene (PFIB) has ten times of higher toxicity, about phosgene, under high humidity conditions, penetrates readily through canister respirator it is considered to be the potentiality gas of a kind of great threat.It is the by-product of Organic fluoride industry, source abundance, it is possible to as using by acute toxic agent, therefore suffered from the extensive concern of chemical defence circle.Chemical weapons agreement (CWC) are listed in one of Hazardous Chemical Substances of strict control, also serve as answering acute toxic agent to list in our toxic agent protection pedigree.Therefore, for protection and an important topic of elimination always chemical defence research field of PFlB.
The countries such as Canada have carried out substantial amounts of research to penetrance toxic agent protective carbon (PP charcoal), mainly by activated carbon surface is carried out direct modification, and it is prepared as PP charcoal with organic amine for impregnating agent, it has preferable barrier propterty to perfluoroisobutylene, within 1997, starts filling in protective equipment and uses.
China's existing protective material for perfluoroisobutyleneand PP charcoal, main production is to utilize chlorine to be modified base carbon surface, then impregnates organic amine component.Its technique is loaded down with trivial details and hazardness of to personnel, equipment is bigger.
Summary of the invention
It is an object of the invention to provide the preparation method of the protective material for perfluoroisobutyleneand that a kind of preparation technology is simple, danger coefficient is little, barrier propterty is high.
The present invention adopts the following technical scheme that realization:
The preparation method of a kind of protective material for perfluoroisobutyleneand is as follows:
(1), described protective material for perfluoroisobutyleneand includes the activated carbon as carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 3%～10%(weight) Cu, 0.1%～5%(weight) Zn, 4%～9%(weight) many amine compounds TEDA.Wherein, in bracket, weight refers to the gross weight of protective material for perfluoroisobutyleneand.
Impregnating agent by above-mentioned active component, i.e. basic copper carbonate, zinc carbonate, add in ammonia (consumption of water capacity calculating ammonia that consumption those skilled in the art press absorbent charcoal carrier), add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 60-80 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method (i.e. preparation solution usage and the relation that water capacity is 1:1 of absorbent charcoal carrier), it is mixed homogeneously with activated carbon, and stands 1-2h；
(2), using flowing bed activation method, i.e. utilize ebuillition of heated stove to make impregnated carbon give the process of its catalytic reaction activity under the effect of high-temperature hot air-flow, activation temperature is 140～190 DEG C, soak time 30～40min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls between 60～70 DEG C.
Wherein, Cu derives from basic copper carbonate, generates the coordination compound of cuprammonium in ammonia spirit, it is provided that perfluoroisobutylene (PFIB) is filtered effect.
Zn derives from zinc carbonate, generates the coordination compound of zinc ammonia, it is provided that perfluoroisobutylene (PFIB) is filtered effect in ammonia spirit.
TEDA is solid at normal temperatures, is adsorbed in the top layer of impregnated carbon by heating volatilization, is favorably improved the impregnated carbon protective capacities under high humidity conditions to perfluoroisobutylene (PFIB).
The impregnated carbon prepared by loading various active component on absorbent charcoal carrier realizes the effective protection to perfluoroisobutylene, and its advantage is as follows:
1, the absorbent charcoal carrier that pore structure is reasonably distributed；
2, the kind of load active component mainly includes Cu, Zn and TEDA；
3, on described carrier material, load specified activity component and prepare impregnated carbon, there is the protective capacities to perfluoroisobutylene.
Impregnated carbon the performance test results see table:
The present invention is reasonable in design, and selecting activated carbon is carrier framework material, loaded Cu, Zn and TEDA isoreactivity component, it is provided that a kind of impregnated carbon for the protection of penetrance toxic agent perfluoroisobutylene and preparation method thereof.
Detailed description of the invention
Below the specific embodiment of the present invention is described in detail.
Embodiment
1
A kind of protective material for perfluoroisobutyleneand, including as the activated carbon of carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 5%(weight) Cu, 7%(weight) TEDA, 3%(weight) Zn.
Preparation method is as follows:
(1), by the impregnating agent of above-mentioned active component, the required weight of basic copper carbonate, zinc carbonate is i.e. calculated respectively by the content of active component, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 60 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 2h；
(2), using flowing bed activation method, activation temperature is 185 DEG C, soak time 40min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls at 60 DEG C.
Embodiment
2
A kind of protective material for perfluoroisobutyleneand, including as the cocoanut active charcoal of carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 7%(weight) Cu, 4%(weight) TEDA, 5%(weight) Zn.
Preparation method is as follows:
(1), by the impregnating agent of active component, the required weight of basic copper carbonate, zinc carbonate is i.e. calculated respectively by the content of active component, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 70 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 1.5h；
(2), using flowing bed activation method, activation temperature is 190 DEG C, soak time 35min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls at 70 DEG C.
Embodiment
3
A kind of protective material for perfluoroisobutyleneand, including as the activated carbon of carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 3%(weight) Cu, 8%(weight) TEDA, 0.1%(weight) Zn.
Preparation method is as follows:
(1), by the impregnating agent of active component, the required weight of basic copper carbonate, zinc carbonate is i.e. calculated respectively by the content of active component, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 65 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 2h；
(2), using flowing bed activation method, activation temperature is 180 DEG C, soak time 30min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls at 65 DEG C.
Embodiment
4
A kind of protective material for perfluoroisobutyleneand, including as the activated carbon of carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 10%(weight) Cu, 9%(weight) TEDA, 0.5%(weight) Zn.
Preparation method is as follows:
(1), by the impregnating agent of active component, the required weight of basic copper carbonate, zinc carbonate is i.e. calculated respectively by the content of active component, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 80 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 1h；
(2), using flowing bed activation method, activation temperature is 150 DEG C, soak time 40min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls at 68 DEG C.
Embodiment
5
A kind of protective material for perfluoroisobutyleneand, including as the activated carbon of carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 8%(weight) Cu, 5%(weight) TEDA, 4%(weight) Zn.
Preparation method is as follows:
(1), by the impregnating agent of active component, the required weight of basic copper carbonate, zinc carbonate is i.e. calculated respectively by the content of active component, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 75 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 2h；
(2), using flowing bed activation method, activation temperature is 140 DEG C, soak time 35min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls at 63 DEG C.
Embodiment
6
A kind of protective material for perfluoroisobutyleneand, including as the cocoanut active charcoal of carrier and the impregnating agent of activated carbon adsorption, described impregnating agent includes 6%(weight) Cu, 6%(weight) TEDA, 1%(weight) Zn.
Preparation method is as follows:
(1), by the impregnating agent of active component, the required weight of basic copper carbonate, zinc carbonate is i.e. calculated respectively by the content of active component, add in ammonia, add thermal melting and be configured to impregnation liquid, mixed solution temperature keeps 80 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 1.5h；
(2), using flowing bed activation method, activation temperature is 170 DEG C, soak time 30min；(3), adsorbing many amine compounds TEDA, adsorption temp controls at 65 DEG C.
Claims (1)
1. the preparation method of a protective material for perfluoroisobutyleneand, it is characterised in that: comprise the steps:
(1), protective material for perfluoroisobutyleneand include the cocoanut active charcoal as carrier and cocoanut active charcoal absorption impregnating agent, described impregnating agent includes the Cu of 5% weight, the Zn of 3% weight, many amine compounds TEDA of 7% weight；
By the impregnating agent of active component, the i.e. content according to active component Cu and Zn calculates the amount of basic copper carbonate, zinc carbonate respectively, add in ammonia, heating for dissolving is configured to impregnation liquid, mixed solution temperature keeps 60 DEG C, to be impregnated dose of abundant dissolving, uses equivalent impregnation method, it is mixed homogeneously with activated carbon, and stands 2h；
(2), using flowing bed activation method, activation temperature is 185 DEG C, soak time 40min；
(3), adsorbing many amine compounds TEDA, adsorption temp controls at 60 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4531953A (en) * | 1983-06-21 | 1985-07-30 | Calgon Corporation | Sublimation of amine compounds on activated carbon pore surfaces |
| EP0405404A1 (en) * | 1989-06-23 | 1991-01-02 | Calgon Carbon Corporation | Chromium-free impregnated activated carbon for adsorption of toxic gases and/or vapors |
| WO2006119654A1 (en) * | 2005-05-06 | 2006-11-16 | Dr. P. Pleisch Ag | Filter material for the adsorption of pollutants from breathing gas |
| CN102006929A (en) * | 2007-11-04 | 2011-04-06 | 布吕歇尔有限公司 | Sorption filter material and use thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5462908A (en) * | 1993-06-16 | 1995-10-31 | Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of National Defence | Organic amine impregnated activated carbon |
-
2013
- 2013-11-25 CN CN201310596572.6A patent/CN103721681B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4531953A (en) * | 1983-06-21 | 1985-07-30 | Calgon Corporation | Sublimation of amine compounds on activated carbon pore surfaces |
| EP0405404A1 (en) * | 1989-06-23 | 1991-01-02 | Calgon Carbon Corporation | Chromium-free impregnated activated carbon for adsorption of toxic gases and/or vapors |
| WO2006119654A1 (en) * | 2005-05-06 | 2006-11-16 | Dr. P. Pleisch Ag | Filter material for the adsorption of pollutants from breathing gas |
| CN102006929A (en) * | 2007-11-04 | 2011-04-06 | 布吕歇尔有限公司 | Sorption filter material and use thereof |
Non-Patent Citations (1)
| Title |
|---|
| 活性炭的高温脱氧改性及其床层对全氟异丁烯的吸附动力学研究;叶平伟，等;《高等学校化学学报》;20080531;第29卷(第5期);第954页 * |
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