CN101574655A - Supported catalyst of potassium perchlorate used for fireworks and crackers and preparation method thereof - Google Patents

Abstract

The invention relates to a supported catalyst of potassium perchlorate used for fireworks and crackers, belonging to the field of fireworks and crackers. By the mass percentage, the supported catalyst comprises the following compositions of: 33%-38% of transitional metal oxide and 62%-67% of carrier; the method comprises the following steps of: firstly adding the carrier in a transitional metal water-soluble salt solution, mixing the solution at a constant temperature so that the solution is dispersed sufficiently; under the mixing condition, gradually adding NaOH solution in the mixed solution; subsequently utilizing ammonia to adjust the pH value to 7.5-8.0; mixing the solution subsequently at the constant temperature, filtering the solution and washing the deposition by distilled water, drying and grinding the depositions and screening the depositions by a sieve of 100 meshes; finally baking the depositions at the temperature of 300-400 DEG C in an environment without oxygen, thus obtaining the target product. The supported catalyst can be directly mixed in the pyrotechnic compositions containing the potassium perchlorate, has little usage amount and simple preparation process, and can greatly improve the reaction rate of the potassium perchlorate-contained pyrotechnic compositions.

Description

Loaded catalyst of potassium perchlorate used for fireworks and crackers and preparation method thereof

Technical field

The present invention relates to a kind of loaded catalyst of potassium perchlorate used for fireworks and crackers, belong to the fireworks and firecrackers field.

Background technology

Potassium chlorate is important raw material in fireworks and firecrackers and other firework medicaments.Potassium chlorate is a kind of strong oxidizer.Scholars such as Zhuo Nan point out that in its article " development of modification potassium chlorate " potassium chlorate has characteristics such as decomposition temperature is low, hygroscopicity is little, explosion property is good, stability in storage is good, production technology is simple, cost is low.But mechanical sensitivities such as the friction of chloracid potassium class fireworks and firecrackers medicament, bump are too high, in production, the transportation security incident take place very easily.Because existing, potassium chlorate is unfavorable for the drawback of keeping the safety in production having occurred advocating to eliminate potassium chlorate or look for the cry of substitute both at home and abroad.Potassium hyperchlorate is that potassium chlorate commonly used in the firework medicament substitutes one of oxidant.But the view that can the scholar replace potassium chlorate for potassium hyperchlorate comprehensively is disunity also, even far from each other.Present most of potassium chlorate substitute all is as one of key component of firecracker oxidant with potassium hyperchlorate.Therefore, the oxidation susceptibility of potassium hyperchlorate has significant effects for the overall performance of firework medicament.By adding suitable catalyst, can improve the reaction rate that contains the potassium hyperchlorate firework medicament, improve the oxidation susceptibility of potassium hyperchlorate, reduce oxidant cost by reducing its consumption, for the exploitation of new type of safe oxidant lays the foundation.

Summary of the invention

The objective of the invention is for a kind of loaded catalyst of potassium perchlorate used for fireworks and crackers is provided, the potassium hyperchlorate oxidation susceptibility that the solution fireworks and firecrackers is used is poor, and the reaction rate that contains the potassium hyperchlorate firework medicament waits problem slowly.

The objective of the invention is to be achieved through the following technical solutions:

A kind of potassium perchlorate used for fireworks and crackers loaded catalyst of the present invention, the mass percent of its each component is as follows:

Transition metal oxide 33%～38%

Carrier 62%～67%

Wherein, described transition metal oxide is the oxide of iron or copper; Carrier is CNT, active carbon.

The preparation method of a kind of potassium perchlorate used for fireworks and crackers loaded catalyst of the present invention, its concrete preparation process is as follows:

1) carrier that will cross 100 mesh sieves joins in the transition metal water-soluble salt solution that concentration is 0.05～0.1mol/L, stirs more than the 30min at 30～40 ℃ of following constant temperature, and it is fully disperseed;

Wherein, described transition metal water soluble salt is ferric sulfate, iron chloride, ferric nitrate, copper sulphate, copper chloride or copper nitrate; Carrier is CNT, active carbon; The mass ratio of carrier and transition metal water soluble salt is 1: 1～1: 1.2;

2) stir down, in above-mentioned mixed solution, dropwise add mass percent and be 1～5% the NaOH aqueous solution, adjusting its pH value with ammoniacal liquor then makes it 7.5～8.0,30～40 ℃ of constant temperature stir more than the 3h, filter, more than 3 times, 100 mesh sieves were ground in the sediment oven dry with the distilled water washing precipitate.

Wherein the molar ratio range of transition metal water soluble salt and NaOH is 1: 2～1: 3.

3) 300～400 ℃ down will on sediment starvation roasting 1.5～2h of making of step, obtain target product.

Beneficial effect: the present invention can directly be mixed in the firework medicament that contains potassium hyperchlorate, and consumption is few, and preparation technology is simple.This loaded catalyst can improve the reaction rate that contains the potassium hyperchlorate firework medicament greatly.

Description of drawings

Fig. 1 is embodiment 1 gained Fe ₂O ₃The SEM figure of/active carbon;

Fig. 2 contains potassium hyperchlorate firework medicament reaction rate---time graph for what add embodiment 1 gained supported catalyst; Wherein: the 1-catalyst-free; The activated carbon supported Fe of 2- ₂O ₃)

The specific embodiment

Embodiment 1

1) with iron chloride (FeCl ₃) be mixed with the aqueous solution of matter 0.06mol/L, measure 50mL, in solution, add the active carbon that 0.5g can mistake 100 mesh sieves, under 40 ℃ of constant temperature, stir 30min, it is fully disperseed;

2) stir down, in above-mentioned mixed solution, dropwise add mass percent and be 1% NaOH weak solution 24mL, adjust its pH value with ammoniacal liquor at last to make it 8; 40 ℃ of constant temperature stir 3h, filter, and use distilled water washing precipitate 3 times, and 100 mesh sieves were ground in the sediment oven dry;

3) 400 ℃ down will on the sediment starvation roasting 2h that makes of step, obtain loaded catalyst.

The result:

Electron spectrum shows that the mass percent of activated carbon surface Fe element is 8.92%, shows Fe ₂O ₃Have at activated carbon surface and to adhere to.Add the firework medicament that contains potassium hyperchlorate of catalyst, its apparent activation energy has reduced by 20.6%, and maximum reaction rate has improved 73.8%.

Embodiment 2

1) with copper chloride (CuCl ₂) be mixed with the aqueous solution of matter 0.06mol/L, measure 50mL, in solution, add the active carbon that 0.5g can mistake 100 mesh sieves, under 30～40 ℃ of constant temperature, stir 30min, it is fully disperseed;

2) stir down, in above-mentioned mixed solution, dropwise add mass percent and be 1% NaOH weak solution 36mL, adjust its pH value with ammoniacal liquor at last to make it 8; 40 ℃ of constant temperature stir 3h, filter, and use distilled water washing precipitate 3 times, and 100 mesh sieves were ground in the sediment oven dry;

3) 400 ℃ down will on the sediment starvation roasting 1.5h that makes of step, obtain loaded catalyst.

The result:

Electron spectrum shows that the mass percent of activated carbon surface Cu element is 63.82%, shows that CuO has at activated carbon surface to adhere to.Add the firework medicament that contains potassium hyperchlorate of catalyst, its apparent activation energy has reduced by 27.0%, and maximum reaction rate has improved 91.0%.

Embodiment 3

1) with iron chloride (FeCl ₃) be mixed with the aqueous solution of matter 0.06mol/L, measure 50mL, in solution, add the CNT that 0.5g can cross 100 mesh sieves, under 30～40 ℃ of constant temperature about stirring 30min, it is fully disperseed;

2) stir down, in above-mentioned mixed solution, dropwise add mass percent and be 1% NaOH weak solution 24mL; Adjusting its pH value with ammoniacal liquor at last makes it 8; 40 ℃ of constant temperature stir about 3h, filter, and use distilled water washing precipitate 3 times, and 100 mesh sieves were ground in the sediment oven dry;

3) 350 ℃ down will on the starvation roasting 2h that makes of step, obtain loaded catalyst.

The result:

Electron spectrum shows that the mass percent of activated carbon surface Fe element is 56.24%, shows Fe ₂O ₃Have at activated carbon surface and to adhere to.Add the firework medicament that contains potassium hyperchlorate of catalyst, its apparent activation energy has reduced by 27.0%, and maximum reaction rate has improved 74.3%.

Embodiment 4

1) with copper chloride (CuCl ₂) be mixed with the aqueous solution of matter 0.06mol/L, measure 50mL, the 0.5g that adds in solution can cross the CNT of 100 mesh sieves, stirs 30min under 340 ℃ of constant temperature, and it is fully disperseed;

2) stir down, in above-mentioned mixed solution, dropwise add mass percent and be 1% NaOH weak solution 36mL; Adjusting its pH value with ammoniacal liquor at last makes it 8; 40 ℃ of constant temperature stir about 3h, filter, and use distilled water washing precipitate 3 times, and 100 mesh sieves were ground in the sediment oven dry;

3) 400 ℃ down will on sediment starvation roasting 1.5～2h of making of step, obtain loaded catalyst.

The result:

Electron spectrum shows that the mass percent of activated carbon surface Cu element is 46.41%, shows that CuO has at activated carbon surface to adhere to.Add the firework medicament that contains potassium hyperchlorate of catalyst, its apparent activation energy has reduced by 27.0%, and maximum reaction rate has improved 74.2%.

Claims (2)

1, potassium perchlorate used for fireworks and crackers loaded catalyst is characterized in that the mass percent of each component is as follows:

Transition metal oxide 33%～38%

Carrier 62%～67%

Wherein, described transition metal oxide is the oxide of iron or copper; Carrier is CNT, active carbon.

2, the preparation method of potassium perchlorate used for fireworks and crackers loaded catalyst is characterized in that concrete preparation process is as follows:

1) carrier that will cross 100 mesh sieves is in the transition metal water-soluble salt solution of 0.05～0.1mol/L to concentration, stirs more than the 30min at 30～40 ℃ of following constant temperature, and it is fully disperseed;

Wherein, described transition metal water soluble salt is ferric sulfate, iron chloride, ferric nitrate, copper sulphate, copper chloride or copper nitrate; Carrier is CNT, active carbon; The mass ratio of carrier and transition metal water soluble salt is 1: 1～1: 1.2;

2) stir down, in above-mentioned mixed solution, dropwise add mass percent and be 1～5% the NaOH aqueous solution, adjusting its pH value with ammoniacal liquor then makes it 7.5～8.0,30～40 ℃ of constant temperature stir more than the 3h, filter, more than 3 times, 100 mesh sieves were ground in the sediment oven dry with the distilled water washing precipitate;

Wherein the molar ratio range of transition metal water soluble salt and NaOH is 1: 2～1: 3;

3) 300～400 ℃ down will on sediment starvation roasting 1.5～2h of making of step, obtain target product.

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