CN103721732A - Catalyst carrier material made of phosphorated and modified pseudo-boehmite and preparation method - Google Patents
Catalyst carrier material made of phosphorated and modified pseudo-boehmite and preparation method Download PDFInfo
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- CN103721732A CN103721732A CN201410029425.5A CN201410029425A CN103721732A CN 103721732 A CN103721732 A CN 103721732A CN 201410029425 A CN201410029425 A CN 201410029425A CN 103721732 A CN103721732 A CN 103721732A
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Abstract
The invention discloses a catalyst carrier material made of phosphorated and modified pseudo-boehmite and a preparation method. After the phosphorated and modified pseudo-boehmite is roasted for 3 hours at the temperature of 600 DEG C, phosphorus pentoxide and aluminium oxide are contained. By adoption of the special preparation method, the phosphorus pentoxide can be dispersed on the surface of the aluminium oxide, and the prepared pseudo-boehmite with large specific surface area and high pore-volume ratio can be prepared, the benefit to improving the activity of the catalyst is achieved and the oxidation-reduction performances are good.
Description
Technical field
The invention belongs to catalyst carrier material technical field, especially relate to a kind of modification boehmite catalyst carrier material and preparation method of phosphorating.
Background technology
Quickening along with diesel oil of vehicle trend in world wide, diesel oil demand is increasing, and in China's diesel oil Oil Product Market, catalytic cracking diesel oil portion has surpassed 1/3rd, and catalytic cracking diesel oil character is poor, main manifestations is that density is large, and the impurity contents such as sulphur and nitrogen are high.Though sulfur content index reduces significantly than before in China's diesel oil, Dan Yu advanced country compares and still has larger gap.
The conventional carrier of industrial diesel oil deep hydrodesulfurizationof catalyst is aluminium oxide, and aluminium oxide has good structural and heat endurance, good mechanical performance, and aperture is suitable.But acidity a little less than, be unfavorable for that catalytic active site forms and performance performance, be difficult to meet the demand of deep desulfuration.Generally with boehmite, through 600 ℃ of roastings, after 3 hours, make in the preparation, the support strength that this method is made by boehmite is low, and specific area is little, pore volume is little, poor catalytic activity, redox property is poor, is difficult to meet the requirement of catalyst depth desulfurization.
Summary of the invention
Object of the present invention is exactly the defect existing for prior art, and a kind of good redox property that has is provided, and can improve a kind of modification boehmite catalyst carrier material that phosphorates of catalyst activity.
Another technical problem to be solved by this invention is to provide a kind of method of preparing the above-mentioned modification boehmite catalyst carrier material that phosphorates.
Its technical scheme is: a kind of modification boehmite catalyst carrier material that phosphorates, the modification boehmite that phosphorates comprises phosphorus pentoxide and aluminium oxide 600 ℃ of roastings after 3 hours, wherein the part by weight of phosphorus pentoxide is 3-5wt%, and the part by weight of aluminium oxide is 95-98wt%.
The part by weight of described material phosphorus pentoxide is 4wt%, and the part by weight of boehmite is 96wt%.
The raw material of described phosphorus pentoxide is phosphoric acid.
The phosphorate preparation method of modification boehmite catalyst carrier material, comprises the steps:
(1) in neutralization reaction still 1, adding alumina concentration is that the aluminum sulfate solution of 45-55g/L and alumina concentration are 200-250g/L, causticity than being the sodium aluminate solution of 1.1-1.3, fixedly the flow of aluminum sulfate solution is 800-1200L/h, control pH value is 6.0-8.0, according to the variation of pH value, regulate the flow of sodium metaaluminate, control reaction temperature at 50-70 ℃;
(2) slurries in neutralization reaction still 1 flow into neutralization reaction still 2 by overflow reaction tube, to adding concentration in neutralization reaction still 2, be simultaneously the sodium carbonate liquor of 100-200g/L, control pH value is 8.5-10, according to the variation of pH value, regulate the flow of sodium carbonate, control reaction temperature at 50-70 ℃;
(3) slurries in neutralization reaction still 2 flow into aging reaction still by overflow reaction tube, slurry temperature in aging reaction still are started to timing after being warming up to 80-95 ℃, aging 2 hours;
(4) according to the quality that drops into aluminium oxide in neutralization reaction still 1 course of reaction, it is the volume of the phosphoric acid solution of 50-150g/L that calculating adds phosphorus pentoxide concentration to aging reaction still, the 3%-5% that the phosphorus pentoxide content that adds phosphoric acid is alumina content;
(5) after aging completing, slurries are transferred to band filter washing, water temperature is controlled at 60-90 ℃;
(6) washed rear filter cake and entered Rotatingandflashstreamingdrier, dry, pulverizing.
The alumina concentration of the aluminum sulfate solution in described step (1) is 50g/L; Described sodium aluminate solution alumina concentration is that 220g/L, causticity ratio are 1.2; The flow of aluminum sulfate is 1000L/h, and pH value is 7.2; Reaction temperature is 60 ℃.
The concentration of described step (2) sodium carbonate is 150g/L; PH value is 8.7; Reaction temperature is 60 ℃.
In described step (3), reaction temperature is 90 ℃.
In described step (4), in phosphoric acid, the concentration of phosphorus pentoxide is 100g/L; The phosphorus pentoxide content of the phosphoric acid adding is 4% of alumina content.
Water temperature in described step (5) is 85 ℃.
The present invention compared with prior art, have the following advantages: by above-mentioned preparation method, can make phosphorus pentoxide be dispersed in alumina surface, can make the boehmite of bigger serface and high pore volume ratio, be conducive to catalyst activity and improve, there is good redox property.
The specific embodiment
Below in conjunction with embodiment, embodiments of the present invention are further described.
Embodiment 1:
In neutralization reaction still 1, adding alumina concentration is that aluminum sulfate solution and the alumina concentration of 50g/L is 22g/L, causticity is than the sodium aluminate solution that is 1.2, fixedly the flow of aluminum sulfate solution is 1000L/h, controlling pH value is 7.2, according to the variation of pH value, regulate the flow of sodium metaaluminate, control reaction temperature at 60 ℃; Slurries in neutralization reaction still 1 flow into neutralization reaction still 2 by overflow reaction tube, to adding concentration in neutralization reaction still 2, be simultaneously the sodium carbonate liquor of 150g/L, controlling pH value is 8.7, regulates the flow of sodium carbonate according to the variation of pH value, controls reaction temperature at 60 ℃; Slurries in neutralization reaction still 2 flow into aging reaction still by overflow reaction tube, slurry temperature in aging reaction still are started to timing after being warming up to 90 ℃, aging 2 hours; According to the quality that drops into aluminium oxide in neutralization reaction still 1 course of reaction, calculate that to aging reaction still, to add phosphorus pentoxide concentration be the volume of the phosphoric acid solution of 100g/L, the phosphorus pentoxide content that adds phosphoric acid is alumina content 4%; After aging completing, slurries are transferred to band filter washing, water temperature is controlled at 85 ℃; Washed rear filter cake and entered Rotatingandflashstreamingdrier, dry, pulverizing.
Comparative example:
Adding alumina concentration is that aluminum sulfate solution and the alumina concentration of 50g/L is 22g/L, causticity is than the sodium aluminate solution that is 1.2, and fixedly the flow of aluminum sulfate solution is 1000L/h, and controlling pH value is 7.2, according to the variation of pH value, regulate the flow of sodium metaaluminate, control reaction temperature at 60 ℃; Slurries in neutralization reaction still 1 flow into neutralization reaction still 2 by overflow reaction tube, to adding concentration in neutralization reaction still 2, be simultaneously the sodium carbonate liquor of 150g/L, controlling pH value is 8.7, regulates the flow of sodium carbonate according to the variation of pH value, controls reaction temperature at 60 ℃; Slurries in neutralization reaction still 2 flow into aging reaction still by overflow reaction tube, slurry temperature in aging reaction still are started to timing after being warming up to 90 ℃, aging 2 hours; After aging completing, slurries are transferred to band filter washing, water temperature is controlled at 85 ℃; Washed rear filter cake and entered Rotatingandflashstreamingdrier, dry, pulverizing.
600 ℃ of roastings of embodiment 1 material are after 3 hours, and alumina content is 96%, and phosphorus pentoxide content is 4%, and specific area is 391g/L, and pore volume is 0.91ml/g.
600 ℃ of roastings of contrast material are after 3 hours, and alumina content is 100%, and specific area is 317g/L, and pore volume is 0.85ml/g.
Hence one can see that, and phosphorus pentoxide is dispersed in alumina surface, can make the boehmite of bigger serface and high pore volume ratio, is conducive to catalyst activity and improves, and has good redox property.
The content that above-described embodiment is illustrated should be understood to these embodiment only for being illustrated more clearly in the present invention, and be not used in, limit the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
Claims (9)
1. the modification boehmite catalyst carrier material that phosphorates, it is characterized in that, the modification boehmite that phosphorates comprises phosphorus pentoxide and aluminium oxide 600 ℃ of roastings after 3 hours, wherein the part by weight of phosphorus pentoxide is 3-5wt%, and the part by weight of aluminium oxide is 95-98wt%.
2. a kind of modification boehmite catalyst carrier material that phosphorates according to claim 1, is characterized in that, the part by weight of described material phosphorus pentoxide is 4wt%, and the part by weight of boehmite is 96wt%.
3. a kind of modification boehmite catalyst carrier material that phosphorates according to claim 1 and 2, is characterized in that, the raw material of described phosphorus pentoxide is phosphoric acid.
4. a preparation method for a kind of modification boehmite catalyst carrier material that phosphorates as claimed in claim 3, is characterized in that, comprises the steps:
In neutralization reaction still 1, adding alumina concentration is that the aluminum sulfate solution of 45-55g/L and alumina concentration are 200-250g/L, causticity than being the sodium aluminate solution of 1.1-1.3, fixedly the flow of aluminum sulfate solution is 800-1200L/h, control pH value is 6.0-8.0, according to the variation of pH value, regulate the flow of sodium metaaluminate, control reaction temperature at 50-70 ℃;
Slurries in neutralization reaction still 1 flow into neutralization reaction still 2 by overflow reaction tube, to adding concentration in neutralization reaction still 2, be simultaneously the sodium carbonate liquor of 100-200g/L, control pH value is 8.5-10, regulates the flow of sodium carbonate according to the variation of pH value, controls reaction temperature at 50-70 ℃;
Slurries in neutralization reaction still 2 flow into aging reaction still by overflow reaction tube, slurry temperature in aging reaction still are started to timing after being warming up to 80-95 ℃, aging 2 hours;
According to the quality that drops into aluminium oxide in neutralization reaction still 1 course of reaction, it is the volume of the phosphoric acid solution of 50-150g/L that calculating adds phosphorus pentoxide concentration to aging reaction still, the 3%-5% that the phosphorus pentoxide content that adds phosphoric acid is alumina content;
After aging completing, slurries are transferred to band filter washing, water temperature is controlled at 60-90 ℃;
Washed rear filter cake and entered Rotatingandflashstreamingdrier, dry, pulverizing.
5. the preparation method of a kind of modification boehmite catalyst carrier material that phosphorates according to claim 4, is characterized in that, the alumina concentration of the aluminum sulfate solution in described step (1) is 50g/L; Described sodium aluminate solution alumina concentration is that 220g/L, causticity ratio are 1.2; The flow of aluminum sulfate is 1000L/h, and pH value is 7.2; Reaction temperature is 60 ℃.
6. the preparation method of a kind of modification boehmite catalyst carrier material that phosphorates according to claim 4, is characterized in that, the concentration of described step (2) sodium carbonate is 150g/L; PH value is 8.7; Reaction temperature is 60 ℃.
7. the preparation method of a kind of modification boehmite catalyst carrier material that phosphorates according to claim 4, is characterized in that, in described step (3), reaction temperature is 90 ℃.
8. the preparation method of a kind of modification boehmite catalyst carrier material that phosphorates according to claim 4, is characterized in that, in described step (4), in phosphoric acid, the concentration of phosphorus pentoxide is 100g/L; The phosphorus pentoxide content of the phosphoric acid adding is 4% of alumina content.
9. the preparation method of a kind of modification boehmite catalyst carrier material that phosphorates according to claim 4, is characterized in that, the water temperature in described step (5) is 85 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105905974A (en) * | 2016-06-27 | 2016-08-31 | 北京化工大学 | Application of phosphorus-modified nano flaky aluminium oxide in removal of cadmium ions in water |
| CN110102250A (en) * | 2019-05-16 | 2019-08-09 | 安庆北化大科技园有限公司 | A kind of preparation method of modified aluminas adsorbent, adsorbent obtained and its application |
| CN110127736A (en) * | 2019-05-28 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of high glutinous macropore boehmite |
| CN111377468A (en) * | 2018-12-28 | 2020-07-07 | 中国石油化工股份有限公司 | Pseudo-boehmite and preparation method thereof |
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| US6638890B2 (en) * | 1999-12-08 | 2003-10-28 | Nippon Shokubai Co. Ltd. | Modified carrier, complex oxide catalyst and process for preparation of acrylic acid |
| CN1488440A (en) * | 2002-10-10 | 2004-04-14 | 中国石油化工股份有限公司 | Phosphor and silicon-containing alumina supporter and preparing method thereof |
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| CN101549300A (en) * | 2008-04-01 | 2009-10-07 | 刘宝珠 | Catalyst for acid and halogen gas treatment and production method thereof |
| CN103357431A (en) * | 2012-03-30 | 2013-10-23 | 中国科学院大连化学物理研究所 | Catalyst for process of producing vehicle fuel through pyrolysis of waste plastic, as well as preparation method and application thereof |
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| US6638890B2 (en) * | 1999-12-08 | 2003-10-28 | Nippon Shokubai Co. Ltd. | Modified carrier, complex oxide catalyst and process for preparation of acrylic acid |
| CN1488440A (en) * | 2002-10-10 | 2004-04-14 | 中国石油化工股份有限公司 | Phosphor and silicon-containing alumina supporter and preparing method thereof |
| CN101069853A (en) * | 2006-05-13 | 2007-11-14 | 林方 | Aluminium oxide carrier containing magnesium and phosphor and preparing method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105905974A (en) * | 2016-06-27 | 2016-08-31 | 北京化工大学 | Application of phosphorus-modified nano flaky aluminium oxide in removal of cadmium ions in water |
| CN111377468A (en) * | 2018-12-28 | 2020-07-07 | 中国石油化工股份有限公司 | Pseudo-boehmite and preparation method thereof |
| CN110102250A (en) * | 2019-05-16 | 2019-08-09 | 安庆北化大科技园有限公司 | A kind of preparation method of modified aluminas adsorbent, adsorbent obtained and its application |
| CN110127736A (en) * | 2019-05-28 | 2019-08-16 | 中国铝业股份有限公司 | A kind of preparation method of high glutinous macropore boehmite |
| CN110127736B (en) * | 2019-05-28 | 2022-02-22 | 中国铝业股份有限公司 | Preparation method of high-viscosity macroporous pseudo-boehmite |
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Application publication date: 20140416 |