CN103706393A - Preparation method of wear-resistant catalyst microspheres for producing low-carbon olefin - Google Patents
Preparation method of wear-resistant catalyst microspheres for producing low-carbon olefin Download PDFInfo
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- CN103706393A CN103706393A CN201310719176.8A CN201310719176A CN103706393A CN 103706393 A CN103706393 A CN 103706393A CN 201310719176 A CN201310719176 A CN 201310719176A CN 103706393 A CN103706393 A CN 103706393A
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Abstract
The invention discloses a preparation method of wear-resistant catalyst microspheres for producing low-carbon olefin. The preparation method comprises the steps of dispersing a molecular sieve and a base material in deionized water, adding a synthesized molecular sieve after homogeneous stirring to obtain a mother solution, and continuously stirring to obtain mixture slurry; grinding the mixture slurry in a colloid milling machine, then performing spray drying on the mixture slurry to obtain catalyst microspheres, and roasting to obtain the wear-resistant catalyst microspheres for a reaction for preparing olefin from methanol. The preparation method disclosed by the invention has the advantages that no pollution is generated, the abrasion resistance index of the catalyst is reduced to be less than 0.5%/h<-1>, and the preparation is simple.
Description
Technical field
The invention belongs to a kind of preparation method of catalyst, be specifically related to a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene.
Background technology
Methanol-to-olefins technology (being called for short MTO technology) is the high-end core technology in world energy sources chemical field.It take the methyl alcohol that coal or natural gas make is raw material, becomes important industrial chemicals-light olefin (ethene and propylene), and then derive numerous olefines chemical products through MTO technology process change.For the national conditions of China's " rich coal of oil starvation weak breath ", this is the revolutionary industrial technology realizing with coal petroleum replacing.Become the core technology of national great energy strategy.Yet the core of this type of technology is catalyst, because methanol to olefins reaction carries out in fluidized-bed reactor, therefore, the activity of catalyst and wearability are particularly important.
There have been many patent Introductions for the method for preparing catalyst of MTO reaction, wherein US Patent No. 4440871 and US5279810 have described the SAPO-34 molecular sieve preparation method with CHA topological structure, and this molecular sieve can be used as the active component of MTO catalysts.
US4987110 patent discloses take the molecular sieve molded method of SAPO-34 that kaolin is binding agent as carrier, Ludox, CN102284302A patent discloses a kind of methanol-to-olefins catalyst microspheres preparation method equally, and the patent CN101121148.2008 of Dalian Chemiclophysics Inst., Chinese Academy of Sciences discloses a kind of direct forming method of fluidized reaction catalyst containing molecular sieve.In order further to improve the intensity of MTO catalyst, researcher has carried out again a large amount of exploratory experiments both at home and abroad, for example, US7214844 B2.2007 patent discloses the forming method that improves MTO catalyst scuff resistance, and the method is by each component proportion in optimization preparation, to reduce to greatest extent the abrasion index of preformed catalyst; In the patent CN1341584 A. 2002 of Praxair Technology, Inc's application, disclose a kind of scuff resistance that improves catalyst by reducing the method for active component consumption, the shortcoming of the method has been to limit greatly the usefulness of catalyst in reaction; Same in US Patent No. 20070249885A1.2007, point out by after binding agent, carrier and molecular sieve mixed pulp under gentle condition burin-in process certain hour, can suitably improve the scuff resistance of preformed catalyst, but its abrasion index is generally still greater than 1%h
-1.
Summary of the invention
The object of this invention is to provide the super-high wear-resistant catalyst microspheres for methanol to olefins reaction that a kind of scuff resistance is high and become preparation method.
Guarantee that its abrasion index is minimum when making catalyst performance maximum efficiency, preparation moulding catalyst microspheres of the present invention binding agent used is taken from the aluminium phosphate sol of synthesis of molecular sieve in mother liquid obtained,, calcination process dry through spraying after this colloidal sol and molecular sieve and matrix bonding, can effectively improve the scuff resistance of catalyst microspheres, catalyst prepared by the method, its abrasion index is at 0.5%/h
-1below.
Preparation method of the present invention comprises the steps:
(1) molecular sieve and matrix are dispersed in deionized water, homogeneous stirs after 1～3 hour and adds synthesis of molecular sieve mother liquid obtained, continues to stir within 1～5 hour, to obtain mixture paste;
(2) step (1) mixture paste is ground 1～5 hour through rubber mill, ground gained mixture paste and be dried through spraying, obtain catalyst microspheres;
(3) by the roasting of step (2) catalyst microspheres process, obtain the wear-resistant catalyst microballoon for methanol to olefins reaction.
As mentioned above, the concentration of molecular sieve in decentralized medium deionized water is 200～700 g/L; The concentration of matrix in decentralized medium deionized water is 100～600 g/L; The concentration of the mother liquid obtained middle aluminum phosphate of synthesis of molecular sieve in decentralized medium deionized water is 10～100 g/L.
As mentioned above, the solid content in step (1) gained mixture paste is at 30～60wt%.
As mentioned above, step (2) mixture paste is viscosity 100cps～30000cps after glue mill, preferably at 3000～20000 cps.
As mentioned above, molecular sieve refers to sial phosphorus SAPO-34; Synthesis of molecular sieve is mother liquid obtained is that separation obtains mother liquor from synthesis of molecular sieve finishes, and effective ingredient refers to the aluminum phosphate obtaining in mother liquor.
As mentioned above, matrix can be selected sesbania powder, kaolin or halloysite.
As mentioned above, preformed catalyst microballoon is 320～380 ℃ of spray dryer inlet temperatures, 90～150 ℃ of outlet temperatures, control rate of drying is 0.1～0.3Kg/ (Kgh), through the dry gained of centrifugal atomizing, the dry microballoon granularity obtaining of spraying is 20～200 μ m, preferably 40～150 μ m.
As mentioned above, spraying is dry obtains microballoon 500～750 ℃ of roastings 1～10 hour, preferably 550 ℃～650 ℃ roastings 3～6 hours.
The present invention is applicable to the preparation of the catalyst that all molecular sieves and matrix, binding agent form, can be for the production of other reactions such as low-carbon alkene reactions.
Advantage of the present invention and good effect are to have utilized the mother liquor producing in sieve synthesis procedure to prepare moulding catalyst microspheres as binding agent, mother liquor has reduced pollutant emission significantly when obtaining utilizing, the more important thing is, in mother liquor, the cementation of aluminium phosphate sol has improved much catalyst microspheres scuff resistance, under the prerequisite that guarantees catalyst effective active, makes attrition of catalyst index drop to 0.5%/h
-1below.Catalyst prepared by the present invention is for realizing environmental friendliness, economically feasible, extensively the success of applicable methanol to olefins reaction course of industrialization provides powerful guarantee.
Accompanying drawing explanation
Fig. 1 is the abrasion resistance index measurement result of the embodiment of the present invention and comparative example.
The specific embodiment
Below in conjunction with embodiment, technology contents of the present invention is described further; Embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
(1). by 300 grams of SAPO-34 molecular sieves and 280 grams of Dispersion of Kaolins, in the deionized water of 450 grams, homogeneous adds 250 gram molecules sieve mother liquors (aluminum phosphate mass content 10.2%) after stirring half an hour, continues to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 47wt%.
(2). said mixture is ground 2.5 hours through rubber mill, and recording mixture viscosity is 5000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 350 ℃ of spray dryer inlet temperatures, 120 ℃ of outlet temperatures, and control rate of drying is 0.15Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 580 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 3 hours, and identified as samples is designated as A, sample D
50be 65 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 2
(1). 260 grams of SAPO-34 molecular sieves and 320 grams of halloysites (85wt%) are dispersed in the deionized water of 400 grams, homogeneous stir about adds 320 gram molecule sieve mother liquors (aluminum phosphate mass content 8.6%) after 2 hours, continue to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 43wt%.
(2). said mixture is ground 5 hours through rubber mill, and recording mixture viscosity is 8000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 380 ℃ of spray dryer inlet temperatures, 150 ℃ of outlet temperatures, and control rate of drying is 0.18Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 600 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 2 hours, and identified as samples is designated as B, sample D
50be 85 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 3
(1). 290 grams of SAPO-34 molecular sieves and 300 grams of sesbania powder are dispersed in the deionized water of 450 grams, homogeneous stir about adds 300 gram molecules sieve mother liquors (aluminum phosphate mass content 8.0%) after 1 hour, continue to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 46wt%.
(2). said mixture is ground 4 hours through rubber mill, and recording mixture viscosity is 7000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 320 ℃ of spray dryer inlet temperatures, 100 ℃ of outlet temperatures, and control rate of drying is 0.10Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 630 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 5 hours, and identified as samples is designated as C, sample D
50be 60 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 4
(1). by 300 grams of SAPO-34 molecular sieves and 260 grams of Dispersion of Kaolins, in the deionized water of 420 grams, homogeneous stir about adds 340 gram molecules sieve mother liquors (aluminum phosphate mass content 9.7%) after half an hour, continues to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 45wt%.
(2). said mixture is ground 3.5 hours through rubber mill, and recording mixture viscosity is 10000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 360 ℃ of spray dryer inlet temperatures, 130 ℃ of outlet temperatures, and control rate of drying is 0.25Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 600 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 4 hours, and identified as samples is designated as D, sample D
50be 70 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 5
(1). 260 grams of SAPO-34 molecular sieves and 360 grams of halloysites (85wt%) are dispersed in the deionized water of 430 grams, homogeneous adds 350 gram molecule sieve mother liquors (aluminum phosphate mass content 7.8%) after stirring for 3 half an hour, continues to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 42wt%.
(2). said mixture is ground 6 hours through rubber mill, and recording mixture viscosity is 15000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 330 ℃ of spray dryer inlet temperatures, 120 ℃ of outlet temperatures, and control rate of drying is 0.28Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 550 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 6 hours, and identified as samples is designated as E, sample D
50be 80 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 6
(1). by 380 grams of SAPO-34 molecular sieves and 350 grams of Dispersion of Kaolins, in the deionized water of 480 grams, homogeneous stir about adds 360 gram molecules sieve mother liquors (aluminum phosphate mass content 8.9%) after 2 hours, continues to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 48wt%.
(2). said mixture is ground 5 hours through rubber mill, and recording mixture viscosity is 9000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 370 ℃ of spray dryer inlet temperatures, 140 ℃ of outlet temperatures, and control rate of drying is 0.26Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 650 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 4.5 hours, and identified as samples is designated as F, sample D
50be 70 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 7(comparative example)
(1). 260 grams of SAPO-34 molecular sieves and 360 grams of halloysites (85wt%) are dispersed in the deionized water of 530 grams, homogeneous stir about adds 108 gram molecules sieve Ludox (mass content 25%) after half an hour, continue to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 47wt%.
(2). said mixture is ground 6 hours through rubber mill, and recording mixture viscosity is 15000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 350 ℃ of spray dryer inlet temperatures, 120 ℃ of outlet temperatures, and control rate of drying is 0.21Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 550 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 6 hours, and identified as samples is designated as G, sample D
50be 75 microns, its abrasion resistance index is shown in Fig. 1.
Embodiment 8(comparative example)
(1). by 320 grams of SAPO-34 molecular sieves and 280 grams of Dispersion of Kaolins, in the deionized water of 560 grams, homogeneous stir about adds 220 gram molecule aluminium colloidal sols (mass content 12%) after half an hour, continues to stir within 1 hour, to obtain mixture; Solid content in thing slurry is 45wt%.
(2). said mixture is ground 4.5 hours through rubber mill, and recording mixture viscosity is 8000 cps, has ground rear mixture through the dry gained catalyst microspheres of spraying; Preformed catalyst microballoon is 370 ℃ of spray dryer inlet temperatures, 130 ℃ of outlet temperatures, and control rate of drying is 0.18Kg/ (Kgh), through the dry gained of centrifugal atomizing.
(3). the roasting at 600 ℃ of above-mentioned catalyst microspheres obtains the wear-resistant catalyst microballoon that can be used for methanol to olefins reaction for 4 hours, and identified as samples is designated as H, sample D
50be 65 microns, its abrasion resistance index is shown in Fig. 1.
Claims (13)
1. for the production of a wear-resistant catalyst method for preparing microsphere for low-carbon alkene, it is characterized in that comprising the steps:
(1) molecular sieve and matrix are dispersed in deionized water, homogeneous stirs after 1～3 hour and adds synthesis of molecular sieve mother liquid obtained, continues to stir within 1～5 hour, to obtain mixture paste;
(2) step (1) mixture paste is ground 1～5 hour through rubber mill, ground gained mixture paste and be dried through spraying, obtain catalyst microspheres;
(3) by the roasting of step (2) catalyst microspheres process, obtain the wear-resistant catalyst microballoon for methanol to olefins reaction.
2. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, is characterized in that the concentration of described molecular sieve in decentralized medium deionized water is 200～700 g/L; The concentration of matrix in decentralized medium deionized water is 100～600 g/L; The concentration of the mother liquid obtained middle aluminum phosphate of synthesis of molecular sieve in decentralized medium deionized water is 10～100 g/L.
3. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, is characterized in that solid content in described step (1) gained mixture paste is at 30～60wt%.
4. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, is characterized in that described step (2) mixture paste viscosity after glue mill is 100cps～30000cps.
5. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 4, is characterized in that described step (2) mixture paste viscosity after glue mill is 3000～20000 cps.
6. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, is characterized in that described molecular sieve is sial phosphorus SAPO-34.
7. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, it is characterized in that synthesis of molecular sieve mother liquid obtained be that separation obtains mother liquor from synthetic SAPO-34 molecular sieve finishes, effective ingredient is the aluminum phosphate in mother liquor.
8. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, is characterized in that described matrix is sesbania powder, kaolin or halloysite.
9. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, it is characterized in that described spray-dired condition is 320～380 ℃ of inlet temperatures, 90～150 ℃ of outlet temperatures, control rate of drying is 0.1～0.3Kg/ (Kgh).
10. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as described in claim 1 or 9, is characterized in that the microballoon granularity through the dry gained of centrifugal atomizing is 20～200 μ m.
11. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 10, is characterized in that the microballoon granularity through the dry gained of centrifugal atomizing is 40～150 μ m.
12. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 1, is characterized in that described roasting is 500～750 ℃ of roastings 1～10 hour.
13. a kind of wear-resistant catalyst method for preparing microsphere for the production of low-carbon alkene as claimed in claim 12, is characterized in that described roasting is 550 ℃～650 ℃ roastings 3～6 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104162448A (en) * | 2014-09-03 | 2014-11-26 | 太原大成环能化工技术有限公司 | Microsphere catalyst for producing low carbon olefin and preparation method of microsphere catalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4987110A (en) * | 1987-05-07 | 1991-01-22 | Union Oil Company Of California | Attrition resistant cracking catalyst |
| CN1341584A (en) * | 2000-07-13 | 2002-03-27 | 环球油品公司 | Abrasion-resisting catalyst for producing light olefin |
-
2013
- 2013-12-24 CN CN201310719176.8A patent/CN103706393B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4987110A (en) * | 1987-05-07 | 1991-01-22 | Union Oil Company Of California | Attrition resistant cracking catalyst |
| CN1341584A (en) * | 2000-07-13 | 2002-03-27 | 环球油品公司 | Abrasion-resisting catalyst for producing light olefin |
Non-Patent Citations (1)
| Title |
|---|
| 狄秋雨 等: "用于快速流化床反应器的甲醇制烯烃催化剂制备和性能研究", 《第十七届全国分子筛学术大会》, 29 August 2013 (2013-08-29), pages 743 - 744 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104162448A (en) * | 2014-09-03 | 2014-11-26 | 太原大成环能化工技术有限公司 | Microsphere catalyst for producing low carbon olefin and preparation method of microsphere catalyst |
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