CN102847562A - Catalyst and preparation method thereof - Google Patents
Catalyst and preparation method thereof Download PDFInfo
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- CN102847562A CN102847562A CN2012103716372A CN201210371637A CN102847562A CN 102847562 A CN102847562 A CN 102847562A CN 2012103716372 A CN2012103716372 A CN 2012103716372A CN 201210371637 A CN201210371637 A CN 201210371637A CN 102847562 A CN102847562 A CN 102847562A
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Abstract
The invention provides catalyst and a preparation method thereof. The preparation method comprises following steps that S1, molecular screen, catalyst carrier raw materials, auxiliary materials and catalyst fine powder with grain size being less than 40 micrometers are dissolved into deionized water to form mixed slurry, wherein the content by weight percent of the catalyst fine powder in the mixed slurry is 10 to 35 percent; S2, the mixed slurry is atomized and granulated into catalyst precursors, and the catalyst precursors comprise catalyst fine powder and catalyst semifinished products; and S3, the catalyst semifinished products are baked to obtain the catalyst finished products. The catalyst fine powder and the molecular screen are collectively dissolved into the deionized water to form the mixed slurry, the mixed slurry is atomized and granulated to form the catalyst semifinished products and the catalyst fine powder, and the addition of the catalyst fine powder is free from increasing the content of the catalyst fine powder in the catalyst precursor, so that the repeated utilization of the catalyst fine powder can be realized.
Description
Technical field
The present invention relates to the Catalyst Production field, in particular to a kind of Catalysts and its preparation method.
Background technology
At present, catalyst is synthetic general to be adopted the molecular sieve after dried molecular sieve or the roasting and molecular sieve carrier such as kaolin etc. are dissolved in and forms slurry in the deionized water, then the slurry spray granulating and drying is obtained the catalyst semi-finished product, further the catalyst semi-finished product are carried out roasting and obtain the catalyst finished product.But, in the mist projection granulating process, formed the qualified catalyst semi-finished product of a part of catalyst grain size, made the catalyst finished product through roasting and carry out commercial Application, the catalyst fines of particle diameter below 40 μ m of the gross weight about 35% that can account at most catalyst precarsor still also arranged, because the particle diameter of catalyst fines is too little, abrasion index is also larger, is not suitable for further carrying out commercial Application, therefore, catalyst fines is difficult to be utilized effectively, and causes the wasting of resources.
Summary of the invention
The present invention aims to provide a kind of Catalysts and its preparation method, has realized the effective utilization to catalyst fines.
To achieve these goals, according to an aspect of the present invention, a kind of preparation method of catalyst is provided, the preparation method comprises: S1, molecular sieve, catalyst carrier raw material, auxiliary material and particle diameter be dissolved in less than the catalyst fines of 40 μ m form mixed slurry in the deionized water, the weight percentage of catalyst fines is 10～35% in the mixed slurry; S2, mixed slurry is carried out mist projection granulating obtain catalyst precarsor, catalyst precarsor comprises catalyst fines and catalyst semi-finished product; And S3, the roasting of catalyst semi-finished product is obtained the catalyst finished product.
Further, the weight percentage of catalyst fines is 20～30% in the above-mentioned mixed slurry.
Further, the weight percentage of catalyst fines is 25% in the above-mentioned mixed slurry.
Further, above-mentioned steps S2 comprises: S21, the dry and granulation with mixed slurry of employing centrifugal spray method obtain catalyst semi-finished product and catalyst fines; S22, employing cyclone separator recovery of catalyst fines.
Further, the catalyst fines that obtains of above-mentioned steps S22 returns step S1 and reuses.
According to a further aspect in the invention, provide a kind of catalyst, this catalyst is the catalyst finished product that above-mentioned preparation method obtains.
The present invention is with the catalyst fines and the molecular sieve that reclaim, catalyst carrier raw material and auxiliary material together are dissolved in and form mixed slurry in the deionized water, then this mixed slurry is carried out forming catalyst semi-finished product and the less fine powder of granularity behind the mist projection granulating, and this fine powder inventory proportion is with not add the shared inventory ratio of the catalyst fines that obtains behind the slurry drying of catalyst fines suitable, that is to say and add the content that catalyst fines can not increase catalyst fines in the catalyst precarsor, avoid the accumulation of catalyst fines, realized the recycling to catalyst fines.And the proportion of catalyst fines in mixed slurry should not be too large, avoids causing the bulk density of molecular sieve finished product too large, abrasion are too large; The proportion of catalyst fines in mixed slurry should not be too little simultaneously, avoids reusing effectively fully catalyst fines.
Description of drawings
The Figure of description that consists of the application's a part is used to provide a further understanding of the present invention, and illustrative examples of the present invention and explanation thereof are used for explaining the present invention, do not consist of improper restriction of the present invention.In the accompanying drawings:
Fig. 1 shows the XRD spectra of the catalyst finished product of embodiment 1 to 6 and Comparative Examples 1.
The specific embodiment
Need to prove, in the situation that do not conflict, embodiment and the feature among the embodiment among the application can make up mutually.Describe below with reference to the accompanying drawings and in conjunction with the embodiments the present invention in detail.
In a kind of typical embodiment of the present invention, a kind of preparation method of catalyst is provided, this preparation method comprises S1, molecular sieve, catalyst carrier raw material and auxiliary material and particle diameter are dissolved in less than the catalyst fines of 40 μ m form mixed slurry in the deionized water, and the weight percentage of catalyst fines described in the described mixed slurry is 10～35%; S2, mixed slurry is carried out drying obtain catalyst semi-finished product and catalyst fines S3, the roasting of catalyst semi-finished product is obtained the catalyst finished product.
The present invention is with the catalyst fines and the molecular sieve that reclaim, catalyst carrier raw material and auxiliary agent and particle diameter are dissolved in less than the catalyst fines of 40 μ m and form mixed slurry in the deionized water, then this mixed slurry is carried out forming catalyst semi-finished product and catalyst fines behind the mist projection granulating, and this fine powder inventory proportion is with not add the shared inventory ratio of the catalyst fines that obtains behind the slurry drying of catalyst fines suitable, that is to say and add the content that catalyst fines can not increase catalyst fines in the catalyst precarsor, avoid the accumulation of catalyst fines, realized the recycling to catalyst fines.And the proportion of catalyst fines in mixed slurry should not be too large, avoids causing the bulk density of molecular sieve finished product too large, abrasion are too large; The proportion of catalyst fines in mixed slurry should not be too little simultaneously, avoids reusing effectively fully catalyst fines.
Can be used for molecular sieve of the present invention can be through the molecular sieve filter cake after purifying, filter, washing, also can be the molecular sieve semi-finished product that obtain behind the molecular sieve filtration cakes torrefaction, it also can be the molecular sieve finished product that obtains after the roasting of molecular sieve semi-finished product, and, those skilled in the art can in conjunction with prior art under guidance of the present invention, be dissolved in according to certain proportioning and form mixed slurry in the deionized water with corresponding catalyst carrier raw material, auxiliary material take molecular sieve filter cake, molecular sieve semi-finished product or molecular sieve finished product as raw material.Can be used for catalyst carrier raw material of the present invention and include but not limited to kaolin, aluminium oxide, Bio-sil, diatomite, can be used for auxiliary material of the present invention and include but not limited to aluminium oxide, SB powder.
In a kind of preferred embodiment of the present invention, the weight percentage of catalyst fines is 20～30% in the mixed slurry.Through inventor's test of many times, when finding between the weight percentage of catalyst fines in the mixed slurry is controlled at 20～30%, the half-finished bulk density of the catalyst that obtains, abrasion index all have preferably performance.
In a kind of specific embodiment of the present invention, the weight percentage of catalyst fines is 25% in the mixed slurry.When the weight percentage of catalyst fines in the mixed slurry was 25%, the half-finished bulk density of the catalyst that obtains was between 0.70～0.80g/ml, and abrasion index is less than 2%.
The drying means of above-mentioned mixed slurry has multiple, such as vacuum filtration, spray-drying, centrifugal drying etc., preferred steps S2 of the present invention comprises: S21, the dry and granulation with mixed slurry of employing centrifugal spray method obtain catalyst semi-finished product and catalyst fines S22, adopt the cyclone separator recovery of catalyst fines.
The centrifugal spray drying method is applicable to the large-scale production of catalyst, and in the centrifugal spray drying process, catalyst fines can be realized separating with the catalyst semi-finished product, is convenient to the recovery to catalyst fines; After the gas that is entrained with catalyst fines adopted the processing of cyclone separator, catalyst fines was collected in the bottom of cyclone separator, has realized the quickly and easily purpose of collection catalyst fine powder.
Used catalyst fines of the present invention can adopt the existing catalyst fines of having accumulated, and the catalyst fines that above-mentioned steps S22 obtains returns step S1 and reuses, and has avoided the further accumulation in the molecular sieve long-term production process.
In the another kind of typical embodiment of the present invention, a kind of catalyst also is provided, this catalyst is the catalyst finished product that above-mentioned preparation method obtains.Adopt the preparation method's of the present invention catalyst that obtains, its bulk density, particle size and abrasion index all can satisfy the demand of commercial Application.
Below with reference to embodiment and Comparative Examples, further specify beneficial effect of the present invention.
The present invention is with the example that is prepared as of MTO (methanol-to-olefins) catalyst, will be through purifying, behind the SAPO molecular sieve Washing of Filter Cake that obtains after the filtration with kaolin, aluminium oxide jointly is dissolved in and forms slurry in the deionized water, this slurry and the MTO catalyst fines that contains the SAPO molecular sieve are mixed to get the mixed slurry of embodiment 1 to 6 according to proportioning in the table 1, adopt drying machine with centrifugal spray to carry out drying the mixed slurry of embodiment 1 to 6, the rotary speed of drying machine with centrifugal spray is 15000 rev/mins, the temperature of hot-air is 300～380 ℃, and be recovered to particle diameter greater than the MTO catalyst meal of 40 μ m in the bottom of drying machine with centrifugal spray, along with tail gas enters cyclone separator, the MTO catalyst fines focuses in the barrel of cyclone separator bottom particle diameter less than the MTO catalyst fines of 40 μ m.
Comparative Examples 1 will directly be carried out spray-drying through jointly being dissolved in the slurry that forms in the deionized water with kaolin after the SAPO molecular sieve filter cake flushing that obtains after purifying, filtering, the condition of work of centrifugal atomizer is identical with the condition of work of above-described embodiment 1 to 6, and the particle diameter that obtains is greater than the MTO catalyst semi-finished product of 40 μ m and the particle diameter MTO catalyst fines less than 40 μ m.
The half-finished bulk density of MTO catalyst, average grain diameter, abrasion index that mensuration embodiment 1 to 6 and Comparative Examples 1 obtain are measured, wherein, the measurement result of bulk density, particle diameter, abrasion index sees Table 1, and, but listed size that roasting direct forms MTO catalyst half-finished bulk density of MTO catalyst and abrasion index in the table 1 as with reference to value; And the MTO catalyst finished product that MTO catalyst semi-finished product obtain after 600 ℃ of roastings is carried out X-ray diffraction test, the XRD spectra that obtains is seen Fig. 1.
Table 1
Can be found out by the data in the table 1, the half-finished bulk density of embodiment 1 to 6 resulting catalyst is in reference value, and, therefore the half-finished abrasion index of catalyst of embodiment 1 to 4 gained also in reference value, proves that the catalyst finished product that forms after the catalyst semi-finished product roasting of embodiment 1 to 4 gained can be applied to industrial production.Compare with Comparative Examples 1, the percentage by weight of catalyst fines is all below 30% in the catalyst precarsor of embodiment 1 to 6 gained, proof is added catalyst fines and not only can not brought more fine powder to product thus, makes on the contrary catalyst fines content in the product maintain original level and has realized effective utilization to catalyst fines.
And, can be found out by the XRD spectra among Fig. 1, no matter be the catalyst finished product of embodiment or the catalyst finished product of Comparative Examples, complete in crystal formation and the peak intensity of molecular sieve wherein are more or less the same, especially the XRD spectra of embodiment 4 and Comparative Examples 1 is almost completely consistent, therefore, the interpolation that catalyst fines is described does not have a negative impact to degree of crystallinity and the crystal formation of the molecular sieve in the catalyst finished product.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. the preparation method of a catalyst is characterized in that, described preparation method comprises:
S1, molecular sieve, catalyst carrier raw material, auxiliary material and particle diameter be dissolved in less than the catalyst fines of 40 μ m form mixed slurry in the deionized water, the weight percentage of catalyst fines described in the described mixed slurry is 10～35%;
S2, described mixed slurry is carried out mist projection granulating obtain described catalyst precarsor, described catalyst precarsor comprises catalyst fines and catalyst semi-finished product; And
S3, the roasting of described catalyst semi-finished product is obtained the catalyst finished product.
2. preparation method according to claim 1 is characterized in that, the weight percentage of catalyst fines described in the described mixed slurry is 20～30%.
3. preparation method according to claim 2 is characterized in that, the weight percentage of catalyst fines described in the described mixed slurry is 25%.
4. each described preparation method in 3 according to claim 1 is characterized in that, described step S2 comprises:
S21, the dry and granulation with described mixed slurry of employing centrifugal spray method obtain described catalyst semi-finished product and described catalyst fines;
S22, employing cyclone separator reclaim described catalyst fines.
5. preparation method according to claim 4 is characterized in that, the described catalyst fines that described step S22 obtains returns described step S1 and reuses.
6. a catalyst is characterized in that, described catalyst is the catalyst finished product that each described preparation method obtains in the claim 1 to 5.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015109587A1 (en) * | 2014-01-21 | 2015-07-30 | 万华化学集团股份有限公司 | Method for preparing catalyst used for preparing chlorine, catalyst and method for preparing chlorine |
| CN106334586A (en) * | 2016-08-19 | 2017-01-18 | 山东东岳化工有限公司 | Method for recycling debris and dust during production process of gaseous phase fluorination catalyst |
| CN107185538A (en) * | 2017-05-27 | 2017-09-22 | 兖矿榆林精细化工有限公司 | A kind of method that high efficiente callback utilizes fine powder in Low Temperature Fischer Tropsch synthesis iron base catalyst |
| CN107971043A (en) * | 2016-10-21 | 2018-05-01 | 中国石油化工股份有限公司 | The method and a kind of method of catalytic cracking catalyst production that a kind of beaded catalyst crushes |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2015109587A1 (en) * | 2014-01-21 | 2015-07-30 | 万华化学集团股份有限公司 | Method for preparing catalyst used for preparing chlorine, catalyst and method for preparing chlorine |
| US10226758B2 (en) | 2014-01-21 | 2019-03-12 | Wanhua Chemical Group Co., Ltd. | Method for preparing catalyst used for preparing chlorine, catalyst and method for preparing chlorine |
| CN106334586A (en) * | 2016-08-19 | 2017-01-18 | 山东东岳化工有限公司 | Method for recycling debris and dust during production process of gaseous phase fluorination catalyst |
| CN107971043A (en) * | 2016-10-21 | 2018-05-01 | 中国石油化工股份有限公司 | The method and a kind of method of catalytic cracking catalyst production that a kind of beaded catalyst crushes |
| CN107185538A (en) * | 2017-05-27 | 2017-09-22 | 兖矿榆林精细化工有限公司 | A kind of method that high efficiente callback utilizes fine powder in Low Temperature Fischer Tropsch synthesis iron base catalyst |
| CN107185538B (en) * | 2017-05-27 | 2020-04-03 | 兖矿榆林精细化工有限公司 | Method for efficiently recycling fine powder in low-temperature Fischer-Tropsch synthesis iron-based catalyst |
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