CN101069853A - Aluminium oxide carrier containing magnesium and phosphor and preparing method - Google Patents
Aluminium oxide carrier containing magnesium and phosphor and preparing method Download PDFInfo
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- CN101069853A CN101069853A CN 200610079765 CN200610079765A CN101069853A CN 101069853 A CN101069853 A CN 101069853A CN 200610079765 CN200610079765 CN 200610079765 CN 200610079765 A CN200610079765 A CN 200610079765A CN 101069853 A CN101069853 A CN 101069853A
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Abstract
The present invention discloses an aluminium oxide carrier which contains magnesium and phosphorus, also can contain potassium and its preparation method. The magnesium, phosphorus and potassium can be added in the process of preparation. Said carrier is low in acidity and has large pore volume and large specific surface area. The catalyst prepared by using said carrier has the features of strong anti-coking property and good stability.
Description
Technical field
The present invention relates to a kind of alumina support and preparation method thereof; Say alumina support that the present invention relates to a kind of P of containing, Mg and possible K and preparation method thereof especially.
Background technology
Hydro carbons such as coal tar light fraction have carbon residue content height (the easy coking of hydro-upgrading process), arene content height, nitrogen content height, (hydrogenation product aquatic products amount is big, water partial pressure is high for the oxygen content height, cause the loss of catalyst activity component easily), characteristics such as sulfur content height, molecule be big, the hydrogenation catalyst that requires hydrocarbons hydrogenation upgrading process such as coal tar light fraction to use possesses strong anti-coking performance, high activity, good stability, big pore volume, big specific area, big aperture.Because carrier property directly influences the overall performance of catalyst consumingly, wherein carrier surface acidity directly influences catalyst coking performance consumingly, for the good hydrocarbons hydrogenation modifying catalysts such as coal tar light fraction of processability, desirable carrier should possess following performance: suitable surface acid alkalescence matter, good heat and hydrothermal stability, higher pore volume, bigger specific area, suitable aperture.
Chinese patent CN1088093C relates to the alumina support of a kind of P of containing, Ti.The adding of Ti has significantly reduced the surface area and the pore volume of carrier, although the adding of P has certain reaming effect, population effect is to have reduced surface area and pore volume.Because have ammonia scrubbing dechlorination step in its preparation process, complicated process of preparation has strengthened preparation cost.
Chinese patent CN1242847C relates to alumina support of a kind of P of containing, Si and preparation method thereof.Its preparation process is: the first step earlier is reacted into glue with sodium metaaluminate and silicon-containing compound solution with carbon dioxide, through aging, filtration.50w% (percentage by weight) silicon-containing compound solution down together in the first step, have only been added; In second step, the filter cake of the remaining silicon-containing compound solution and the first step mixes, and wears out, filters, washs, drying; In the 3rd step, use phosphorus-containing compound and siliceous aluminium oxide mixing, moulding, drying and roasting.The carrier of this invention preparation can reduce the surface acid amount and the acid strength of carrier within the specific limits, and pore volume and the specific area that can regulate carrier within the specific limits, but its acidity is still higher.Because preparation process is to do from sodium metaaluminate, long flow path, process complexity, cost height.
Chinese patent CN1110304A relates to alumina support of a kind of P of containing, Si and preparation method thereof, and CN1242847C is similar with Chinese patent, and its preparation method also is to do from aluminium salt such as aluminium chloride, long flow path, process complexity, cost height.
Chinese patent CN1091427C relates to a kind of preparation method of aluminium oxide, the tens kinds of elements such as can adding P, Mg that just in specification, underdraw, but its preparation method, interpolation quantity and function are not all related to.In addition, the document that adds P, Mg and K in carrier does not appear in the newspapers.
The object of the invention is to provide a kind of anti-coking performance high alumina support, and a kind of simple preparation method of this carrier is provided simultaneously.
Summary of the invention
IIA family elements such as the P of containing of the present invention, Mg, and the alumina support of possible IA family metallic elements such as K is composed as follows: P content is 0.1%～10% (weight), preferred 1%～5% (weight); The content of IIA family element is 0.5%～10% (weight), preferred 1%～5% (weight); The content of IA family metallic element is not more than 10% (weight), preferably is not more than 4% (weight).The pore volume of carrier of the present invention is 0.3～1.0ml/g, preferred 0.6～0.9ml/g; Specific area is 100～450m
2/ g, preferred 150～400m
2/ g; The most probable aperture is 3～30nm.Wherein, the most probable aperture changes with the weight that processes raw material is different: if the processing boiling point less than 200 ℃ naphtha, the most probable aperture is 3.0～5.0nm; If the raw material of being processed is that to do be 360 ℃ distillate, the most probable aperture is 5～10nm; If the raw material of being processed is that to do be 450 ℃ distillate, the most probable aperture is 8～15nm; If the raw material of being processed is that to do be 530 ℃ mink cell focus, then the most probable aperture is 8～15nm and 15～25nm, has double-peak feature.
IIA of the present invention family element is one or more of Be, Mg, Ca, Sr and Ba, and preferred elements is Mg.
IA of the present invention family element is one or more of Li, K, Rb and Cs, and preferred elements is K.
IIA family elements such as the P of containing of the present invention, Mg, and the preparation process of the alumina support of possible IA family metallic elements such as K comprise the steps:
The first step weighs a certain amount of aluminium oxide precursor, adds extrusion aid, mixes; The salt that contains P-compound, IIA family element and possible IA family element of amount of calculation is added in a certain amount of deionized water wiring solution-forming;
In second step, the aluminium oxide precursor that the first step is obtained and the solution of preparation mix pinches into the plastic aftershaping;
The 3rd step is at 80～150 ℃ of down dry 0.5～10h;
In the 4th step,, promptly make carrier of the present invention at 350～850 ℃ of following roasting 0.5～10h.
In the process of preparation carrier, employed aluminium oxide precursor can be a boehmite, also can be boehmite; The P-compound that contains that uses is in phosphoric acid, pyrophosphoric acid, hypophosphorous acid, phosphorous acid, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate (ADP), potassium dihydrogen phosphate and the potassium phosphate one or more; The salt of the IIA family element that uses be nitrate and or hydrochloride, as beryllium nitrate, magnesium nitrate, calcium nitrate and barium nitrate.The salt of the IA family metallic element that uses is one or more in potassium nitrate, potassium phosphate, potassium dihydrogen phosphate, potassium chloride, potash, the lithium nitrate.
The advantage of alumina support of the present invention is:
1. owing to wherein added IA family elements such as IIA family element such as Mg and K, weakened the acidity of carrier, thereby had higher anti-coking performance;
2. owing to added the P that the reaming effect is arranged, have bigger pore volume, feasible catalyst by this preparing carriers has higher appearance charcoal ability;
3. because the synergy of Mg and P has effectively suppressed the interaction of carrier and reactive metal, feasible utilization rate with the active component on the catalyst of this preparing carriers is improved.
Above advantage based on this carrier, Hydrobon catalyst with this preparing carriers possesses strong anti-coking performance, have high activity, good stability, big pore volume, big specific area, big advantages such as aperture simultaneously concurrently, be particularly suitable for having the carbon residue content height, the unifining process of the hydro carbons of characteristics such as arene content height, nitrogen content height, oxygen content height, molecule are big, such as the unifining process of coal tar light fraction.
The specific embodiment
Following examples are understood the present invention specifically, but do not limit the present invention.
Embodiment 1
Weigh aluminum hydroxide solid elastomer powder 100g, add 5g sesbania powder.Magnesium nitrate 30g, phosphatase 11 5g be dissolved in the 80ml water make solution.This solution is joined in the aluminum hydroxide solid elastomer powder that contains the sesbania powder, mix pinch into uniform paste plastic after, being extruded into diameter is the cloverleaf pattern bar of 1.2mm.In drying box,, move into then in the muffle furnace, make the alumina support A that contains magnesium, phosphorus 550 ℃ of following roastings 4 hours in 110 ℃ of dryings 4 hours.
Embodiment 2
Weigh aluminum hydroxide solid elastomer powder 100g, add 5g sesbania powder.Magnesium nitrate 7.42g, phosphoric acid 5.5g be dissolved in the 80ml water make solution.This solution is joined in the aluminum hydroxide solid elastomer powder that contains the sesbania powder, mix pinch into uniform paste plastic after, being extruded into diameter is the cloverleaf pattern bar of 1.2mm.In drying box,, move into then in the muffle furnace, make the alumina support B that contains magnesium, phosphorus 550 ℃ of following roastings 4 hours in 110 ℃ of dryings 4 hours.
Embodiment 3
Weigh 100g aluminum hydroxide solid elastomer powder, add 5g sesbania powder, magnesium nitrate 14.8g, potassium nitrate 1.8g, phosphoric acid 8.3g are dissolved in the 80ml water make solution.Above-mentioned mixing of materials is even, mix and pinch into plastic material, being extruded into diameter is the cloverleaf pattern bar of 1.2mm, 120 ℃ of following dry 2h, 650 ℃ of following roasting 4h make the alumina support C that contains magnesium, phosphorus, potassium.
Embodiment 4
Weigh 100g aluminum hydroxide solid elastomer powder, add 5g sesbania powder, magnesium nitrate 29.7g, ammonium dihydrogen phosphate (ADP) 10.4g are dissolved in the 80ml water make solution.Above-mentioned mixing of materials is even, mix and pinch into plastic material, being extruded into diameter is the cloverleaf pattern bar of 1.2mm, 130 ℃ of following dry 2h, 650 ℃ of following roasting 4h make the alumina support D that contains magnesium, phosphorus.
Embodiment 5
Weigh 100g aluminum hydroxide solid elastomer powder, add 5g sesbania powder, magnesium nitrate 14.8g, potassium nitrate 1.8g, diammonium hydrogen phosphate 11.9g are dissolved in the 80ml water make solution.Above-mentioned mixing of materials is even, mix and pinch into plastic material, being extruded into diameter is the cloverleaf pattern bar of 1.2mm, 120 ℃ of following dry 2h, 750 ℃ of following roasting 4h make the alumina support E that contains magnesium, phosphorus, potassium.
Embodiment 6
Weigh 100g aluminum hydroxide solid elastomer powder, add 5g sesbania powder, magnesium nitrate 7.4g, potassium nitrate 3.6g, phosphatase 11 1.1g are dissolved in the 80ml water make solution.Above-mentioned mixing of materials is even, mix and pinch into plastic material, being extruded into diameter is the cloverleaf pattern bar of 1.2mm, 130 ℃ of following dry 4h, 800 ℃ of following roasting 4h make the alumina support F that contains magnesium, phosphorus, potassium.
Comparative Examples 1
Press the embodiment 1 among the Chinese patent CN1088093C, make carrier G.
Comparative Examples 2
Press the embodiment 1 among the Chinese patent CN1242847C, make carrier H.
Chemical composition and the surface nature of carrier A, B, C, D, E, F, G and H are listed in subordinate list.
By subordinate list as can be seen, the surface acid amount of carrier of the present invention is significantly less than the comparative example, has big pore volume, big specific area simultaneously concurrently.
The main character of subordinate list carrier
| Carrier | A | B | C | D | E | F | G | H |
| Chemical composition, w% | ||||||||
| Mg | 3.35 | 0.93 | 1.77 | 3.43 | 1.75 | 0.87 | ||
| K | - | - | 0.89 | - | 0.87 | 1.74 | ||
| P | 4.81 | 1.99 | 2.85 | 3.46 | 3.51 | 3.75 | 3.23 | 2.5 |
| Physico-chemical property | ||||||||
| Pore volume, ml/g | 0.55 | 0.48 | 0.42 | 0.45 | 0.41 | 0.38 | 0.58 | 0.54 |
| Specific area, m 2/g | 320 | 340 | 310 | 300 | 305 | 280 | 280 | 300 |
| Side pressure strength, N/cm | 129 | 128 | 138 | 140 | 145 | 152 | - | - |
| The surface acid amount, μ mol/g | 0.13 | 0.15 | 0.06 | 0.11 | 0.05 | 0.03 | - | 0.35 |
| Acid amount relatively, % | 37 | 43 | 17 | 31 | 14 | 8.6 | - | 100 |
Claims (21)
1, a kind of alumina support is characterized in that containing IIA family element in P, the periodic table of elements.With the carrier is benchmark, and the content of P is 0.1%～10% (weight), and the content of IIA family element is 0.5%～10% (weight).
2,, it is characterized in that containing IA family element according to the described carrier of claim 1.With the carrier is benchmark, and the content of IA family element is lower than 10% (weight).
3,, it is characterized in that described IIA family element is one or more of Be, Mg, Ca, Sr and Ba according to the described carrier of claim 2.
4,, it is characterized in that described IA family element is one or more of Li, K, Rb and Cs according to the described carrier of claim 2.
5,, it is characterized in that described IIA family element is Mg according to the described carrier of claim 2.
6,, it is characterized in that described IA family element is K according to the described carrier of claim 2.
7, according to the described carrier of claim 2, it is characterized in that described IIA family element is Mg, described IA family element is K.
8,, it is characterized in that the content (is benchmark with the carrier) of described P is 1%～5% (weight) according to the described carrier of claim 2.
9, according to the described carrier of claim 5, the content of described Mg (is benchmark with the carrier) is 1%～5% (weight).
10,, it is characterized in that the content (is benchmark with the carrier) of described K is lower than 4% (weight) according to the described carrier of claim 6.
11, according to claim 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 described carriers, its preparation method may further comprise the steps:
The first step weighs a certain amount of aluminium oxide precursor, adds extrusion aid, mixes; The salt that contains P-compound, IIA family element and possible IA family element of amount of calculation is added in a certain amount of deionized water wiring solution-forming;
In second step, the aluminium oxide precursor that the first step is obtained and the solution of preparation mix pinches into the plastic aftershaping;
The 3rd step is at 80～150 ℃ of down dry 0.5～10h;
In the 4th step,, promptly make carrier of the present invention at 350～850 ℃ of following roasting 0.5～10h.
12, according to the described preparing carriers method of claim 11, it is characterized in that described baking temperature is 100～130 ℃, be 2～6h drying time.
13, according to the described preparing carriers method of claim 11, it is characterized in that described sintering temperature is 450～750 ℃, roasting time is 2～6h.
14,, it is characterized in that the described P-compound that contains is in phosphoric acid, hypophosphorous acid, pyrophosphoric acid, phosphorous acid, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate (ADP), potassium dihydrogen phosphate and the potassium phosphate one or more according to the described preparing carriers method of claim 11.
15, according to the described preparing carriers method of claim 11, the salt that it is characterized in that described IIA family element is nitrate and or hydrochloride.
16, according to the described preparing carriers method of claim 11, the salt that it is characterized in that described IA family element is one or more in nitrate, hydrochloride, phosphate and the carbonate.
17, according to claim 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8 or 9 or 10 described carriers, it is characterized in that its physical property is: pore volume is that 0.3～1.0ml/g, specific area (BET) are 100～450m
2/ g, most probable aperture are 3～30nm.
18,, it is characterized in that the most probable aperture is 3～5nm according to the described carrier of claim 17.
19,, it is characterized in that the most probable aperture is 5～10nm according to the described carrier of claim 17.
20,, it is characterized in that the most probable aperture is 8～15nm according to the described carrier of claim 17.
21,, it is characterized in that the most probable aperture is 8～15nm and 15～25nm, has double-peak feature according to the described carrier of claim 17.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610079765 CN101069853A (en) | 2006-05-13 | 2006-05-13 | Aluminium oxide carrier containing magnesium and phosphor and preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610079765 CN101069853A (en) | 2006-05-13 | 2006-05-13 | Aluminium oxide carrier containing magnesium and phosphor and preparing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101069853A true CN101069853A (en) | 2007-11-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610079765 Pending CN101069853A (en) | 2006-05-13 | 2006-05-13 | Aluminium oxide carrier containing magnesium and phosphor and preparing method |
Country Status (1)
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| CN103230798A (en) * | 2013-04-26 | 2013-08-07 | 沈阳三聚凯特催化剂有限公司 | Hydrogen desulfurization catalyst and preparation method thereof |
| CN103331177A (en) * | 2013-03-29 | 2013-10-02 | 广西民族大学 | A carried-type aluminium dihydrogen tripolyphosphate catalyst and a preparation method thereof |
| CN103418388A (en) * | 2012-05-24 | 2013-12-04 | 中国石油化工股份有限公司 | Fischer-Tropsch synthesis catalyst and preparation and applications thereof |
| CN103480337A (en) * | 2012-06-08 | 2014-01-01 | 中国石油化工股份有限公司 | Hydrate alumina forming product, production method thereof, alumina forming product, applications thereof, catalyst, preparation method thereof, and hydrogenation processing method |
| CN103721732A (en) * | 2014-01-23 | 2014-04-16 | 山东允能催化技术有限公司 | Catalyst carrier material made of phosphorated and modified pseudo-boehmite and preparation method |
| CN104324723A (en) * | 2013-07-22 | 2015-02-04 | 中国石油化工股份有限公司 | Hydrogenation protection catalyst, and preparation method and application thereof |
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| CN106732692A (en) * | 2016-11-15 | 2017-05-31 | 中国海洋石油总公司 | A kind of preparation method of modified aluminium oxide supports |
| CN106807420A (en) * | 2017-03-17 | 2017-06-09 | 钦州学院 | A kind of catalyst and preparation method for petroleum naphtha hydrogenation dearsenification |
| CN108949287A (en) * | 2018-08-08 | 2018-12-07 | 桂林桂特板业有限公司 | A method of biomass molding fuel ash softening point is improved using porous ceramics |
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| CN111744485A (en) * | 2019-03-29 | 2020-10-09 | 中国石油化工股份有限公司 | Modified alumina, preparation method of modified alumina and catalyst containing modified alumina |
| CN113559889A (en) * | 2020-04-28 | 2021-10-29 | 中国石油化工股份有限公司 | Modified phosphorus-containing pseudo-boehmite, preparation method thereof, modified phosphorus-containing alumina and hydrogenation catalyst |
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-
2006
- 2006-05-13 CN CN 200610079765 patent/CN101069853A/en active Pending
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| CN103480337B (en) * | 2012-06-08 | 2016-01-13 | 中国石油化工股份有限公司 | Hydrated alumina forming matter and preparation method and aluminium oxide article shaped and application and catalyst and preparation method and hydrotreating method |
| CN103480337A (en) * | 2012-06-08 | 2014-01-01 | 中国石油化工股份有限公司 | Hydrate alumina forming product, production method thereof, alumina forming product, applications thereof, catalyst, preparation method thereof, and hydrogenation processing method |
| CN103331177A (en) * | 2013-03-29 | 2013-10-02 | 广西民族大学 | A carried-type aluminium dihydrogen tripolyphosphate catalyst and a preparation method thereof |
| CN103331177B (en) * | 2013-03-29 | 2014-12-03 | 广西民族大学 | A carried-type aluminium dihydrogen tripolyphosphate catalyst and a preparation method thereof |
| CN103230798A (en) * | 2013-04-26 | 2013-08-07 | 沈阳三聚凯特催化剂有限公司 | Hydrogen desulfurization catalyst and preparation method thereof |
| CN104324723A (en) * | 2013-07-22 | 2015-02-04 | 中国石油化工股份有限公司 | Hydrogenation protection catalyst, and preparation method and application thereof |
| CN104324723B (en) * | 2013-07-22 | 2016-06-29 | 中国石油化工股份有限公司 | A kind of hydrogenation protecting catalyst and preparation method and application |
| CN103721732A (en) * | 2014-01-23 | 2014-04-16 | 山东允能催化技术有限公司 | Catalyst carrier material made of phosphorated and modified pseudo-boehmite and preparation method |
| CN104927911A (en) * | 2014-03-21 | 2015-09-23 | 中国石油化工股份有限公司 | Hydrotreatment method of hydrocarbon oil raw material with high content of iron and calcium |
| CN104927911B (en) * | 2014-03-21 | 2017-01-18 | 中国石油化工股份有限公司 | Hydrotreatment method of hydrocarbon oil raw material with high content of iron and calcium |
| CN106732692B (en) * | 2016-11-15 | 2020-02-18 | 中国海洋石油集团有限公司 | Preparation method of modified alumina carrier |
| CN106732692A (en) * | 2016-11-15 | 2017-05-31 | 中国海洋石油总公司 | A kind of preparation method of modified aluminium oxide supports |
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| CN113559889B (en) * | 2020-04-28 | 2023-09-05 | 中国石油化工股份有限公司 | Modified phosphorus-containing pseudo-boehmite, preparation method thereof, modified phosphorus-containing alumina and hydrogenation catalyst |
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Open date: 20071114 |