CN102520115A - Fabrication method of carrier catalytic element detection die - Google Patents
Fabrication method of carrier catalytic element detection die Download PDFInfo
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- CN102520115A CN102520115A CN2011104173006A CN201110417300A CN102520115A CN 102520115 A CN102520115 A CN 102520115A CN 2011104173006 A CN2011104173006 A CN 2011104173006A CN 201110417300 A CN201110417300 A CN 201110417300A CN 102520115 A CN102520115 A CN 102520115A
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Abstract
The invention provides a fabrication method of a carrier catalytic element detection die. The fabrication method comprises manufacturing a catalytic element carrier and preparing an impregnation solution; loading the impregnation solution in a suction flask, putting the catalytic element in the impregnation solution, and putting the suction flask in an ultrasonic oscillator; evacuating the suction flask until the vacuum degree reaches 60-100KPa, and keeping the vacuum degree for 5-30min; turning on the ultrasonic oscillator, and restoring the pressure in the suction flask to normal pressure within 5-20min; and taking out the catalytic element carrier, air drying, and decomposing at 500-700 DEG C. The inventive fabrication method has simple process, high practicability, large catalyst loading capacity, high distribution uniformity and prominent loading effects.
Description
Technical field
The present invention relates to a kind of carrier catalyst element, specifically, related to the preparation method that a kind of carrier catalyst element detects tube core.
Background technology
At present, carrier catalyst element is because it is simple in structure, low price, degree of accuracy is higher and be used for the Leak Detection field of inflammable gas in a large number; The load process of catalyzer is one of core technology of preparation carrier catalyst element, and its charge capacity, distribution consistency degree directly influence long-term working stability, the linearity and the anti-activation capability of carrier catalyst element sensitivity.
The existing carrier catalyst element catalyst cupport mode overwhelming majority adopts common impregnation technology; Because carrier has abundant and tortuous micropore; Common impregnation method can not guarantee that catalyzer can be diffused in the micropore in carrier deep; Even adopt the prolongation dip time to make catalyzer be diffused into the carrier deep, also have bigger concentration gradient, and then can influence the efficient of catalyst combustion reaction.
For charge capacity and the dispersion degree that improves catalyzer, industrial circle also has the ultrasonic immersing of employing or vacuum-impregnated technology to handle catalyst support, but effect is still not ideal enough.
Summary of the invention
The objective of the invention is deficiency, thereby the preparation method of the carrier catalyst element detection tube core that a kind of technology is simple, practical, catalyst loadings is big and distribution consistency degree is high, load effect is outstanding is provided to prior art.
To achieve these goals, the technical scheme that the present invention adopted is: a kind of carrier catalyst element detects the preparation method of tube core, and this preparation method may further comprise the steps:
Step 1, making catalysis element carrier and configuration dipping solution;
Step 2, said dipping solution is placed bottle,suction, said catalysis element carrier is placed said dipping solution, more said bottle,suction is placed ultrasonic oscillator; The vacuum tightness of said bottle,suction is extracted into 60～100KPa, kept this vacuum tightness 5～30 minutes;
Step 3, open said ultrasonic oscillator, then, in 5～20 minutes, make the pressure in the said bottle,suction return to normal pressure;
Step 4, the said catalysis element carrier of taking-up after drying, decompose under 500～750 ℃ temperature, promptly get carrier catalyst element and detect tube core.
Based on above-mentioned, in step 1, getting activated alumina powder or high-specific surface area is 50～300m
2The powder of/g adds inorganic adhesive, mixes the back and grinds, and obtains the carrier slurry; Again with said carrier slurry coating on the good platinum filament coil of coiling, form microspheroidal or little ellipsoid shape, then, the sintering temperature moulding at 600～900 ℃ promptly gets the catalysis element carrier; Said powder is at least a in silica powder, tin oxide powder, aluminum silicate powder, thoria powder, the Zinc oxide powder.
Based on above-mentioned, in step 1, it is in 1～10% the hydrochloric acid that platinum chloride and palladium bichloride are dissolved in concentration, obtains catalyzer; In said catalyzer, add catalyst aid again, fully after the dissolving, promptly get dipping solution; Wherein, The weight of contained palladium is 0.5～3 times of weight of institute's platiniferous in the said dipping solution; The general assembly (TW) of said platinum chloride and said palladium bichloride accounts for 5～20% of said dipping solution weight, and the general assembly (TW) of said catalyst aid accounts for 3%～15% of said dipping solution weight; Said catalyst aid is at least a in lanthanum nitrate, cerous nitrate, thorium nitrate, the zirconium nitrate.
The relative prior art of the present invention has outstanding substantive distinguishing features and marked improvement; Specifically; This preparation method is the impregnation catalyst component carrier under vacuum and ultrasound condition; Vacuum condition can guarantee the degree of depth of catalyst soakage, and ultrasonic immersing can guarantee the dispersed homogeneous degree of catalyzer on carrier, the advantage that it has, and technology is simple, practical, catalyst loadings is big and distribution consistency degree is high, load effect is outstanding.
Description of drawings
Fig. 1 is the linearity synoptic diagram of three kinds of catalysis elements.
Embodiment
Through embodiment, technical scheme of the present invention is done further detailed description below.
A kind of carrier catalyst element detects the preparation method of tube core, and this preparation method may further comprise the steps:
Step 1, making catalysis element carrier and configuration dipping solution; Wherein, getting activated alumina powder or high-specific surface area is 50～300m
2The powder of/g adds inorganic adhesive, is ground to certain particle after the mixing, promptly obtains the carrier slurry; Again with said carrier slurry coating on the good platinum filament coil of coiling, form microspheroidal or little ellipsoid shape, then, the sintering temperature moulding at 600～900 ℃ promptly gets the catalysis element carrier; Said powder is at least a in silica powder, tin oxide powder, aluminum silicate powder, thoria powder, the Zinc oxide powder;
It is in 1～10% the hydrochloric acid that platinum chloride and palladium bichloride are dissolved in concentration, obtains catalyzer; In said catalyzer, add catalyst aid again, fully after the dissolving, promptly get dipping solution; Wherein, The weight of contained palladium is 0.5～3 times of weight of institute's platiniferous in the said dipping solution; The general assembly (TW) of said platinum chloride and said palladium bichloride accounts for 5～20% of said dipping solution weight, and the general assembly (TW) of said catalyst aid accounts for 3%～15% of said dipping solution weight; Said catalyst aid is at least a in lanthanum nitrate, cerous nitrate, thorium nitrate, the zirconium nitrate, and said catalyst aid plays the effect of stable carrier material crystal formation and anticatalyst sintering.
Step 2, said dipping solution is placed bottle,suction, said catalysis element carrier is placed said dipping solution, more said bottle,suction is placed ultrasonic oscillator;
Said bottle,suction is connected on the vacuum pump through evacuating valve; And the vacuum tightness of said bottle,suction is extracted into 60～100KPa; In this process; Have considerable bubble and emerge, when the normal pressure dipping is described, exist the part catalyzer of bubble to be difficult to spread in the catalysis element carrier from said catalysis element carrier; Kept this vacuum tightness 5～30 minutes, bubble is fully discharged.
Step 3, open said ultrasonic oscillator, then, close the evacuating valve of said bottle,suction, again vacuum pump cuts out, slowly open the air intake valve of said bottle,suction, in 5～20 minutes, make the pressure in the said bottle,suction return to normal pressure.
Step 4, the said catalysis element carrier of taking-up after drying, decompose under 500～750 ℃ temperature, promptly get carrier catalyst element and detect tube core.
The experiment contrast:
Experimental example: step 1, take by weighing 1g activated alumina powder, add alumina sol, grind after 5 hours, process the carrier slurry as inorganic adhesive; Said carrier slurry coating on the good platinum filament coil of coiling, is formed microspheroidal, after drying,, promptly get the catalysis element carrier 850 ℃ of following sintering 2 hours;
It is in 2% the hydrochloric acid that platinum chloride and palladium bichloride are dissolved in concentration, obtains catalyzer; In said catalyzer, add lanthanum nitrate and cerous nitrate again, fully after the dissolving, promptly get dipping solution; Wherein, the weight of contained palladium is that the weight of institute's platiniferous is identical in the said dipping solution, and the general assembly (TW) of said platinum chloride and said palladium bichloride accounts for 10% of said dipping solution, and the general assembly (TW) of said lanthanum nitrate and said cerous nitrate accounts for 5% of said dipping solution weight.
Step 2, first part of dipping solution placed bottle,suction, said catalysis element carrier is placed first part of dipping solution, more said bottle,suction is placed ultrasonic oscillator; The vacuum tightness of said bottle,suction is extracted into 95KPa, kept this vacuum tightness 20 minutes; Open said ultrasonic oscillator, then, in 20 minutes, make the pressure in the said bottle,suction return to normal pressure; Take out said catalysis element carrier, after drying, under 600 ℃ temperature, decompose, promptly get carrier catalyst element and detect tube core; Again this carrier catalyst element is detected tube core and match, obtain testing catalysis element with the compensation tube core that does not contain catalyzer.
Comparative Examples: with experimental example gained catalysis element carrier and dipping solution, do not vacuumize also without ultrasonic oscillator, dipping is 2 hours under the state of nature, and the same experimental example of all the other steps obtains contrasting catalysis element.
Table 1: catalysis element sensitivity contrast table (catalysis element output unit: mV);
| ? | 0%CH4 | 1%CH4 | 2%CH4 | 3%CH4 | 4%CH4 |
| The |
0 | 29.3 | 57.7 | 86.3 | 114.6 |
| The |
0 | 23.4 | 43.2 | 61.4 | 79.7 |
| Commercially |
0 | 25.7 | 49.3 | 73.3 | 94.7 |
Experiment condition: three kinds of catalysis elements are worked in containing the CH4 environment of variable concentrations, and equal conditions is test down; Be not difficult to find out that by last table in containing the CH4 environment of variable concentrations, the sensitivity of three kinds of catalysis elements has obvious difference, wherein, the sensitivity of experiment catalysis element is the highest; In addition, as shown in Figure 1, under the situation that CH4 concentration changes, the linearity of three kinds of catalysis elements also has bigger difference, and wherein, the linearity of experiment catalysis element is best, approaches straight line.
Table 2: catalysis element anti-poisoning ability contrast table (catalysis element output unit: mV);
| ? | Before poisoning | After poisoning | Attenuation amplitude |
| The experiment catalysis element | 30.7 | 22.1 | -28.0% |
| The contrast catalysis element | 24.2 | 11.4 | -52.9% |
| Commercially available catalysis element | 26.3 | 12.7 | -51.7% |
Experiment condition: three kinds of catalysis elements were all worked 30 minutes in the ethyl orthosilicate atmosphere of 100ppm, and equal conditions is test down; Be not difficult to find out that by last table the anti-poisoning ability of three kinds of catalysis elements has bigger difference, wherein, the antitoxinization attenuation amplitude of experiment catalysis element is minimum, and anti-poisoning ability is the strongest.
This preparation method's advantage: catalysis element and commercially available catalysis element, the normal pressure impregnation catalyst element made with this technology contrast; The catalysis element that this technology is made has remarkable advantages aspect sensitivity, the linearity and antitoxinization; Because catalyst loadings is bigger under this mode of loading, and the carrier deep also can load on catalyzer; When catalysis element places the high concentration inflammable gas; Catalyzer has enough active potential energies that inflammable gas is burnt fully, has guaranteed the linearity of catalysis element in the high concentration inflammable gas, works in the environment that contains sulfide or organosilicon atmosphere and work as catalysis element; Even the catalyzer in the catalysis element carrier skin is poisoned, its inner catalyzer that distributes can also provide suitable active sites to be used to guarantee normally carrying out of catalytic combustion.
Should be noted that at last: above embodiment is only in order to technical scheme of the present invention to be described but not to its restriction; Although with reference to preferred embodiment the present invention has been carried out detailed explanation, the those of ordinary skill in affiliated field is to be understood that: still can specific embodiments of the invention make amendment or the part technical characterictic is equal to replacement; And not breaking away from the spirit of technical scheme of the present invention, it all should be encompassed in the middle of the technical scheme scope that the present invention asks for protection.
Claims (5)
1. a carrier catalyst element detects the preparation method of tube core, and it is characterized in that: this preparation method may further comprise the steps:
Step 1, making catalysis element carrier and configuration dipping solution; Step 2, said dipping solution is placed bottle,suction, said catalysis element carrier is placed said dipping solution, more said bottle,suction is placed ultrasonic oscillator; The vacuum tightness of said bottle,suction is extracted into 60～100KPa, kept this vacuum tightness 5～30 minutes; Step 3, open said ultrasonic oscillator, then, in 5～20 minutes, make the pressure in the said bottle,suction return to normal pressure; Step 4, the said catalysis element carrier of taking-up after drying, decompose under 500～750 ℃ temperature, promptly get carrier catalyst element and detect tube core.
2. carrier catalyst element according to claim 1 detects the preparation method of tube core, and it is characterized in that: in step 1, getting activated alumina powder or high-specific surface area is 50～300m
2The powder of/g adds inorganic adhesive, mixes the back and grinds, and obtains the carrier slurry; Again with said carrier slurry coating on the good platinum filament coil of coiling, form microspheroidal or little ellipsoid shape, then, the sintering temperature moulding at 600～900 ℃ promptly gets the catalysis element carrier.
3. carrier catalyst element according to claim 2 detects the preparation method of tube core, it is characterized in that: said powder is at least a in silica powder, tin oxide powder, aluminum silicate powder, thoria powder, the Zinc oxide powder.
4. detect the preparation method of tube cores according to claim 1 or 2 or 3 described carrier catalyst elements, it is characterized in that: in step 1, it is in 1～10% the hydrochloric acid that platinum chloride and palladium bichloride are dissolved in concentration, obtains catalyzer; In said catalyzer, add catalyst aid again, fully after the dissolving, promptly get dipping solution; Wherein, The weight of contained palladium is 0.5～3 times of weight of institute's platiniferous in the said dipping solution; The general assembly (TW) of said platinum chloride and said palladium bichloride accounts for 5～20% of said dipping solution weight, and the general assembly (TW) of said catalyst aid accounts for 3%～15% of said dipping solution weight.
5. carrier catalyst element according to claim 4 detects the preparation method of tube core, it is characterized in that: said catalyst aid is at least a in lanthanum nitrate, cerous nitrate, thorium nitrate, the zirconium nitrate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105797786A (en) * | 2016-03-28 | 2016-07-27 | 沈阳化工大学 | Ultrasonic vacuum synchronous preparation method of high-dispersion supported catalyst |
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Application publication date: 20120627 |