CN109772303A - A kind of modified catalyst preparation method promoting noble metal constituent element dispersed homogeneous degree - Google Patents

Abstract

The present invention relates to a kind of modified catalyst preparation methods for promoting noble metal constituent element dispersed homogeneous degree, its innovative point is processing step are as follows: is first put into catalyst carrier particle in the vacuum drier of rotatable vacuum drier, under vacuum conditions, vacuum drier is added in the metal salt solution containing noble metal rapidly；The catalyst carrier particle for not immersing solution is all purged into solution with compressed air again, so that catalyst carrier particle is all flooded by solution；Finally, rotation vacuum drying machine, heats it, vacuumizes, the catalyst granules that surface appends precious metal salt without bright water, suction is made.The present invention has the advantages that catalyst carrier with containing noble metal solution through rotation when come into full contact with absorption and stand when solution in precious metal salt competitive Adsorption balance, it is dehydrated again through heating in vacuum and noble metal catalyst is made, its noble metal constituent element in catalyst carrier on measure, be uniformly dispersed, improve the combined reaction performance of catalyst.

Description

A kind of modified catalyst preparation method promoting noble metal constituent element dispersed homogeneous degree

Technical field

The present invention relates to a kind of modified catalyst preparation methods for promoting noble metal constituent element dispersed homogeneous degree.

Background technique

Noble metal catalyst be petrochemical industry, fine chemistry industry and medication chemistry quoted extensively one kind with expensive Metal component is the catalysis material of active component.Noble metal is obtained in the catalyst there are commonly platinum, palladium, rhodium, silver, ruthenium etc., In it is especially most widely used with platinum, palladium, rhodium.Their electron orbit is all unfilled, the easy adsorption reaction object in surface, and moderate strength, benefit Among being formed " reactive compound ", catalytic activity with higher, while also having high temperature resistant, anti-oxidant, corrosion-resistant etc. comprehensive Good characteristic is closed, most important catalyst material is become.

The impregnation technology of noble metal catalyst is used to the metal salt for containing noble metal being prepared into solution, solution impregnation catalyst Carrier is to make precious metal salt be adsorbed onto a kind of process of catalyst carrier.A kind of method is that liquid excessively impregnates, and is In fixed container, immersion catalyst carrier particle is all flooded with the liquid containing noble metal constituent element, is emptied after a certain period of time It is dry to lead to hot-air for residual liquid；Still an alternative is that rotation dipping, in rotary container, with containing noble metal constituent element Liquid is mixed with catalyst carrier particle, is continued to rotate after a certain period of time, is vacuumized heat drying.Due in noble metal catalyst Bullion content is very low, and using noble metal catalyst made from both methods, there are noble metal constituent elements in catalyst carrier Upper amount, the non-uniform phenomenon of dispersion, to influence the reactivity worth of catalyst.Moreover, your gold remaining contains in the former technique The liquid of category discharges, and recycling is big using difficulty, easily causes the uneven or mutual pollution between batch；In the drying process, when Between it is long, run that damage is big, and product yield is low, energy consumption is high.Kind technique often generates not soaking catalyst carrier primary colors particle afterwards.

Summary of the invention

The technical problem to be solved in the present invention is to provide a kind of modified catalysts for promoting noble metal constituent element dispersed homogeneous degree Preparation method.

In order to solve the above technical problems, the technical solution of the present invention is as follows: a kind of industrial soaking process for noble metal catalyst, Innovative point is processing step are as follows: catalyst carrier particle is put into first in the vacuum drier of rotatable vacuum drier, Under vacuum state of the vacuum degree greater than -0.09Mpa, vacuum drier is added in the metal salt solution containing noble metal rapidly； Only rotation vacuum drying machine, so that the mixing of solution and carrier holding 1 hour or more, stop operating vacuum drier, with compression The catalyst carrier particle for not immersing solution is all purged into solution by air, so that catalyst carrier particle is all by solution It floods；The catalyst granules that will drown out in the solution stands 1-24 hours, and every the solution of agitation in 1-2 hours；Finally, turning Dynamic vacuum drier, and open drying device, carries out it being heated to 70 DEG C -100 DEG C and to be evacuated to vacuum degree simultaneously not small In -0.06Mpa, the above heating vacuumizes holding at least two hours, finally obtained surface without bright water, have precious metal salt Catalyst granules.

Further, the catalyst carrier is aluminium oxide or aluminium oxide and the compound carrier of silica.

Further, the volume of the solution is 1.2 times that catalyst carrier just immerses required liquor capacity in solution To 2 times.

The present invention has the advantages that catalyst carrier is passed through with the solution containing noble metal comes into full contact with absorption when rotating It is balanced with the competitive Adsorption of precious metal salt in solution when standing, then is dehydrated noble metal catalyst, your gold is made through heating in vacuum Belong to constituent element in catalyst carrier on measure, be uniformly dispersed, improve the combined reaction performance of catalyst.

Specific embodiment

Embodiment 1: platinum catalyst dipping

Catalyst carrier particle 200kg containing aluminium oxide is put into the vacuum drier of rotatable vacuum drier, The particle can be strip, spherical, is also possible to other special-shaped particles, vacuumizes 0.5-2 hours, so that in vacuum drier Vacuum degree is greater than -0.09Mpa；

Rotation vacuum impregnator, revolving speed at 0.5 rev/min to 3 revs/min, by the metal salt containing platinum be dissolved in 320 liters it is molten In liquid, solution concentration 0.01% metal salt solution is added in vacuum drier rapidly, at this time under above-mentioned vacuum state Liquor capacity is 1.2 times that catalyst carrier just immerses required liquor capacity in solution.Rotation time is 0.5 hour -2 small When, so that solution is sufficiently mixed repeatedly with catalyst carrier.Later, stop vacuum drier rotation, and blown using compressed gas The catalyst carrier particle in vacuum drier is swept, so that the catalyst carrier particle that part does not immerse solution is all blown into solution In, it is flooded by solution；

The catalyst carrier particle being submerged in solution stands 1-9 hours, every the solution of agitation in 1 hour；

Rotation vacuum drying machine again, carries out it being heated to 70 DEG C -100 DEG C and to be evacuated to vacuum degree simultaneously not small In -0.06Mpa, maintain 2 hours or more, until Pt catalyst granule surface obtained is without bright water.In platinum catalyst vector The content of platinum 0.1% (m) to 0.5% (m) range when, the deviation measured on catalyst granules platinum is in 1%-3%.

Embodiment 2: the dipping of palladium catalyst

Strip catalyst carrier granular 100kg containing aluminium oxide is put into vacuum drier, vacuumizing keeps vacuum dry Vacuum degree in dry machine is greater than -0.09Mpa；

Rotation vacuum impregnator, revolving speed is at 0.5 rev/min to 3 revs/min, the solution for being 2.5g/l by the concentration of palladium It 180 liters, under above-mentioned vacuum state, is pumped into vacuum drier rapidly, liquor capacity is that catalyst carrier just immerses at this time 1.4 times of required liquor capacity in solution；After continuing to rotate -2 hours 0.5 hour, stop vacuum drier rotation, using compression Gas purges the catalyst carrier particle in vacuum drier, so that all catalyst carrier particles all submerge in solution；

The catalyst carrier particle being submerged in palladium solution stands 10-20 hours, every the solution of agitation in 2 hours；

Rotation vacuum drying machine again, it is heated, keep vacuumizing be heated to 70 DEG C -100 DEG C, and simultaneously take out very Sky is to vacuum degree not less than -0.06Mpa maintenance 2 hours or more, until palladium catalyst particle surface obtained is without bright water, palladium For the content of palladium in 0.1% range above, the deviation measured on catalyst granules palladium is no more than 3% in catalyst carrier.

Embodiment 3: the dipping of rhodium catalyst

Strip catalyst carrier granular 100kg containing aluminium oxide and silica is put into vacuum drier, rotation is true Empty drying machine, and vacuum degree is evacuated to greater than -0.09Mpa；

By 200 liters of solution that rhodium content is 5g/l, under above-mentioned vacuum state, it is pumped into vacuum drier rapidly, at this time Liquor capacity is 2 times that catalyst carrier just immerses required liquor capacity in solution；Vacuum drier is continued to rotate, revolving speed exists It after 2 revs/min to 3 revs/min, rotation -2 hours 1 hour, stops operating, using in compressed gas purging vacuum drier Catalyst carrier particle, so that catalyst carrier particle is fully immersed in rhodium dipping solution；

It keeps rhodium dipping solution to submerge all catalyst carrier particles and stands 21-24 hours, it is primary molten every agitation in 2 hours Liquid；

Rotation vacuum drying machine again, it is heated, keep vacuumizing be heated to 70 DEG C -100 DEG C, and simultaneously take out very Sky is to vacuum degree not less than -0.06Mpa maintenance 2 hours or more, until rhodium catalyst particle surface obtained is without bright water, rhodium For the content of rhodium in 0.1% to 2.0% range, the deviation measured on catalyst granules rhodium is no more than 3% in catalyst carrier.

Claims (3)

1. a kind of modified catalyst preparation method for promoting noble metal constituent element dispersed homogeneous degree, it is characterised in that processing step are as follows: Catalyst carrier particle is put into first in the vacuum drier of rotatable vacuum drier, in vacuum degree greater than -0.09Mpa's Under vacuum state, vacuum drier is added in the metal salt solution containing noble metal rapidly；Only rotation vacuum drying machine, so that molten Liquid and mixing in carrier holding 1 hour or more, stop operating vacuum drier, will not immerse the catalyst of solution with compressed air Carrier granular is all purged into solution, so that catalyst carrier particle is all flooded by solution；It will drown out urging in the solution Catalyst particles stand 1-24 hours, and every the solution of agitation in 1-2 hours；Finally, rotation vacuum drying machine, and open drying Device carries out it to be heated to 70 DEG C --- 100 DEG C and while be evacuated to vacuum degree not less than -0.06Mpa, it is described above Heat, vacuumize holding at least two hours, final obtained surface without bright water, have the catalyst granules of precious metal salt.

2. the impregnation technology according to claim 1 for preparing noble metal catalyst, it is characterised in that: the catalyst carrier For aluminium oxide or aluminium oxide and the compound carrier of silica.

3. the impregnation technology according to claim 1 for preparing noble metal catalyst, it is characterised in that: the volume of the solution It is 1.2 times to 2 times that catalyst carrier just immerses required liquor capacity in solution.