CN1313200C - Magnesium aluminium spinel activated adsorbent - Google Patents
Magnesium aluminium spinel activated adsorbent Download PDFInfo
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- CN1313200C CN1313200C CNB2005100784325A CN200510078432A CN1313200C CN 1313200 C CN1313200 C CN 1313200C CN B2005100784325 A CNB2005100784325 A CN B2005100784325A CN 200510078432 A CN200510078432 A CN 200510078432A CN 1313200 C CN1313200 C CN 1313200C
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 24
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 20
- 239000011029 spinel Substances 0.000 title claims abstract description 20
- 229910052749 magnesium Inorganic materials 0.000 title description 9
- 239000011777 magnesium Substances 0.000 title description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title 1
- 229910052782 aluminium Inorganic materials 0.000 title 1
- 239000004411 aluminium Substances 0.000 title 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 17
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 16
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910003158 γ-Al2O3 Inorganic materials 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 239000005995 Aluminium silicate Substances 0.000 claims description 9
- 235000012211 aluminium silicate Nutrition 0.000 claims description 9
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical group O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 9
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 229910003112 MgO-Al2O3 Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical group [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 20
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 239000011148 porous material Substances 0.000 abstract description 11
- 229910021529 ammonia Inorganic materials 0.000 abstract description 10
- 239000000428 dust Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 7
- 239000002817 coal dust Substances 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract 3
- 239000000853 adhesive Substances 0.000 abstract 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- -1 Magnesium aluminate Chemical class 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- 239000003245 coal Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000010802 sludge Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000010779 crude oil Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000003034 coal gas Substances 0.000 description 2
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical group O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention discloses a magnesium-aluminum spinel activated adsorbent which prepared from 5 to 20 wt% of light MgO, 30 to 70 wt% of gamma-Al2O3, 5 to 20 wt% of alpha-Al2O3 and SiO2 as the rest. 3 to 30 wt% of adhesive agents and 5 to 20 wt% of accelerating agents are added to the components to be sintered at high temperature to obtain the activated adsorbent having a spatial mesh micropore structure, large pore volume and bulk gap. The activated adsorbent can sufficiently adsorb dust and liquid water, prevent the dust and the liquid water from being mutually slimed, and ensure the normal operation of a reaction device. The activated adsorbent can be used in devices for making synthetic ammonia, methanol, hydrogen, etc. to eliminate the dust and the liquid water in gas, can improve the conversion rate of the dry coal dust, can reduce the production cost, and can improve the economic benefit of an enterprise.
Description
Technical Field
The invention relates to an adsorbent, in particular to a magnesia-alumina spinel active adsorbent used on a device for synthesizing ammonia from coal.
Background
At present, with the continuous and great increase of the price of crude oil in the market, domestic chemical enterprises are carrying out technical transformation on a gas making system of synthetic ammonia so as to meet the technical requirement of carrying out synthetic ammonia production by replacing crude oil with coal, reduce the production cost of the synthetic ammonia and improve the economic benefit of the enterprises. In the ammonia production process technology using coal instead of crude oil, the conversion of carbon monoxide by coal has two modes: firstly, coal water slurry is converted into carbon monoxide by a Dongting nitrogen fertilizer plant in Hunan province and an Anhui province and an Anqing fertilizer plant in China, the conversion rate is only 50-55%, and the conversion rate is low; secondly, if the foreign U.S. shell company directly converts the dry coal dust into carbon monoxide, the conversion rate is over 65%, but the conversion rate is high, but the direct conversion of the dry coal dust into carbon monoxide has the following problems: although the coal gas is dedusted by the cloth bag, the coal gas still contains a small amount of dust, and the dust is easily deposited in a converter and a pre-converter in the ammonia synthesis device to form sludge after being mixed with water vapor, so that blockage is caused, the normal operation of the ammonia synthesis device is influenced, the service life of a conversion catalyst is shortened, the production cost is increased, and the economic benefit is reduced.
Technical content
Aiming at the problems that sludge deposition is easy to form and the normal operation of a conversion device is influenced in the process of directly converting dry coal dust into carbon monoxide in the prior art, the invention provides the magnesia-alumina spinel active adsorbent which can be filled in a conversion furnace and a pre-conversion furnace and is used for adsorbing dust and liquid water in gas, preventing the dust and the liquid water from interacting with each other to form sludge and ensuring the normal operation of a synthetic ammonia conversion device.
The object of the invention is achieved by using light MgO, gamma-Al2O3、α-Al2O3、SiO2The composition comprises the following material components in percentage by weight: light MgO: 5-20% of gamma-Al2O3：30-70％、α-Al2O3: 5-20%, the rest is: SiO 22。
In order to improve the content of the magnesia-alumina spinel in the active adsorbent and increase the pore volume and the adsorption activity, a promoter is added into the mixture of the material components, wherein the promoter can be boehmite, aluminum hydroxide or alumina with higher activity, and the addition amount of the promoter is 2-20% of the total amount of the material components.
In order to ensure that the material components have certain viscosity and toughness after being mixed and be convenient for production, molding and pressing, the mixture is also added with a binder, the addition amount of the binder is 3-30% of the total amount of the material components, the binder can be kaolin or an organic binder, and the main chemical component of the kaolin is Al2O3And SiO2。
The forming mechanism of the invention is as follows: light MgO and gamma-Al2O3And α -Al2O3Reacting at 1200-1450 ℃ to generate magnesia-alumina spinelA primary crystalline phase having the chemical reaction formula: in the main crystal phase MgO.2Al2O3In, Al2O340-90% of gamma-Al2O335-80% of MgO, 5-30% of MgO and the balance of SiO2。
The preparation method of the magnesium aluminate spinel active adsorbent comprises the following steps:
1. mixing light MgO and gamma-Al in percentage by weight2O3、α-Al2O3、SiO2Uniformly mixing;
2. adding a binder accounting for 3-30% of the total weight and an accelerant accounting for 2-20% of the total weight into the mixed material, and uniformly mixing to form a dry material;
3. grinding the dry materials in a ball mill, and then sending the ground dry materials into a vibrator for magnetic iron removal and sieving;
4. adding the iron-removed and screened dry materials into a pug mill, adding a proper amount of water, and then mixing and grinding to ensure that the materials have certain toughness;
5. adding the material from the pugging machine into a model, and pressing into various shapes;
6. and (3) feeding the formed material into a calcining furnace, heating to 1200-1450 ℃, preserving heat for 6-8 hours, cooling along with the furnace, and discharging to obtain the magnesia-alumina spinel active adsorbent.
After the invention is prepared, the main technical indexes are as follows through detection:
specific pore volume is not less than 0.1ml/g pore diameter of 20-500 Å
Porosity: the stacking porosity is more than or equal to 20 percent: not less than 45 percent
Compressive strength: more than or equal to 100N/particle heat-resistant rapid denaturation: not less than 500 deg.C
Bulk density: not less than 1.0g/cm3Adsorption activity: not less than 20 percent
Maximum scale capacity: not less than 300kg/m3
The light MgO, gamma-Al of the invention2O3、α-Al2O3、SiO2(ii) a Kaolin or an organic binder; the raw materials of the pseudoboehmite, the aluminum hydroxide or the aluminum oxide with larger activity can be purchased in the chemical industry market.
The main crystal phase of the active adsorbent is magnesia-alumina spinel which has a spatial reticular microporous structure, has larger pore volume and stacked gaps, and the surface of the main crystal is microscopic alkaline, so that dust and liquid water can be fully adsorbed, the dust and the liquid water are prevented from interacting to form sludge, and the normal operation of an ammonia synthesis device is ensured.
Detailed Description
Example 1
The proportion of the magnesium aluminate spinel active adsorbent is as follows: it is made of light MgO and gamma-Al2O3、α-Al2O3、、SiO2The composition comprises the following material components in percentage by weight: light MgO: 8% of gamma-Al2O3：70％、α-Al2O3: 8 percent, and the balance: SiO 22The kaolin accounts for 15% of the total amount of the materials, and the aluminum hydroxide accounts for 10% of the total amount of the materials. The manufacturing method comprises the following steps:
1. mixing light MgO and gamma-Al according to the weight percentage2O3、α-Al2O3、SiO2Uniformly mixing;
2. adding kaolin accounting for 15 percent of the total weight and aluminum hydroxide accounting for 10 percent of the total weight into the mixed material, and uniformly mixing to form a dry material;
3. grinding the dry materials in a ball mill, and then sending the ground dry materials into a vibrator for magnetic iron removal and sieving;
4. adding the iron-removed and screened dry materials into a pug mill, adding a proper amount of water, and then mixing and grinding to ensure that the materials have certain toughness;
5. adding the material from the pugging machine into a model, and pressing into various shapes;
6. and (3) feeding the formed material into a calcining furnace, heating to 1400 ℃, preserving heat for 8 hours, cooling along with the furnace, and discharging to obtain the magnesia-alumina spinel active adsorbent.
The magnesium aluminate spinel active adsorbent manufactured in embodiment 1 of the invention has the following main technical indexes:
specific pore volume of 0.15ml/g pore diameter of 220 Å
Porosity: 35% bulk porosity: 55 percent of
Compressive strength: 105N/particle heat shock resistance: 560 ℃ C
Bulk density: 1.1g/cm3Adsorption activity: 35 percent of
Maximum scale capacity: 320kg/m3
Example 2
The proportion of the magnesium aluminate spinel active adsorbent is as follows: it is made of light MgO and gamma-Al2O3、α-Al2O3、SiO2The composition comprises the following material components in percentage by weight: light MgO: 15% of gamma-Al2O3：50％、α-Al2O3: 15% and the balance: SiO 22The organic binder accounts for 25% of the total amount of the material components, and the pseudoboehmite accounts for 5% of the total amount of the material components. The manufacturing method comprises the following steps:
1. mixing light MgO and gamma-Al according to the weight percentage2O3、α-Al2O3、SiO2Uniformly mixing;
2. adding organic binder accounting for 25% of the total amount and pseudoboehmite accounting for 5% of the total amount into the mixed material, and uniformly mixing to form a dry material;
3. grinding the dry materials in a ball mill, and then sending the ground dry materials into a vibrator for magnetic iron removal and sieving;
4. adding the iron-removed and screened dry materials into a pug mill, adding a proper amount of water, and then mixing and grinding to ensure that the materials have certain toughness;
5. adding the material from the pugging machine into a model, and pressing into various shapes;
6. and (3) feeding the formed material into a calcining furnace, heating to 1350 ℃, preserving heat for 7 hours, cooling along with the furnace, and discharging to obtain the magnesia-alumina spinel active adsorbent.
The magnesium aluminate spinel active adsorbent manufactured in embodiment 2 of the invention has the following main technical indexes:
specific pore volume of 0.12ml/g pore diameter of 300 Å
Porosity: 50% bulk porosity: 65 percent of
Compressive strength: 110N/particle thermal shock resistance: 550 deg.C
Bulk density: 1.2g/cm3Adsorption activity: 50 percent of
Maximum scale capacity: 370kg/m3
Example 3
The proportion of the magnesium aluminate spinel active adsorbent is as follows: it is made of light MgO and gamma-Al2O3、α-Al2O3、、SiO2The composition comprises the following material components in percentage by weight: light MgO: 20% of gamma-Al2O3：40％、α-Al2O3: 20%, the rest is: SiO 22The kaolin accounts for 5% of the total amount of the materials, and the aluminum hydroxide accounts for 20% of the total amount of the materials. The manufacturing method comprises the following steps:
1. mixing light MgO and gamma-Al according to the weight percentage2O3、α-Al2O3、SiO2Uniformly mixing;
2. adding kaolin accounting for 5 percent of the total amount and aluminum hydroxide accounting for 20 percent of the total amount into the mixed material, and uniformly mixing to form a dry material;
3. grinding the dry materials in a ball mill, and then sending the ground dry materials into a vibrator for magnetic iron removal and sieving;
4. adding the iron-removed and screened dry materials into a pug mill, adding a proper amount of water, and then mixing and grinding to ensure that the materials have certain toughness;
5. adding the material from the pugging machine into a model, and pressing into various shapes;
6. and (3) feeding the formed material into a calcining furnace, heating to 1250 ℃, preserving heat for 6 hours, cooling along with the furnace, and discharging to obtain the magnesia-alumina spinel active adsorbent.
The magnesium aluminate spinel active adsorbent manufactured in embodiment 3 of the invention has the following main technical indexes:
specific pore volume of 0.16ml/g pore diameter of 250 Å
Porosity: 30% bulk porosity: 50 percent of
Compressive strength: 100N/particle thermal shock resistance: 530 deg.C
Bulk density: 1.05g/cm3Adsorption activity: 40 percent of
Maximum scale capacity: 350kg/m3
Claims (1)
1. A magnesia-alumina spinel active adsorbent is characterized in that: light MgO and gamma-Al are adopted2O3、α-Al2O3、SiO2The promoter and the binder are raw materials, wherein the promoter is pseudo-boehmite or aluminum hydroxide, the binder is kaolin or an organic binder, and the main component of the kaolin is Al2O3And SiO2(ii) a And is prepared by adopting the following method:
(1) light MgO and gamma-Al2O3、α-Al2O3And SiO2The four raw materials are uniformly mixed to form a mixture, and the weight percentage of the materials in the mixture is as follows: MgO: 5-20% of gamma-Al2O3：30-70％、α-Al2O3: 5-20% and the balance of SiO2；
(2) Respectively adding an accelerant accounting for 2-20 wt% of the total weight of the mixture and a binder accounting for 3-30 wt% of the total weight of the mixture into the mixture, and uniformly mixing to form a dry material;
(3) grinding the dry materials in a ball mill, and then sending the ground dry materials into a vibrator for magnetic iron removal and sieving;
(4) adding the dry material subjected to grinding, iron removal and sieving into a pug mill, adding a proper amount of water, and mixing and grinding to ensure that the material has certain toughness;
(5) adding the material discharged by the pug mill into a model, and pressing into various shapes;
(6) and feeding the formed material into a calcining furnace, heating to 1200-1450 ℃, preserving heat for 6-8 hours, cooling along with the furnace, and discharging to obtain the magnesia-alumina spinel active adsorbent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100784325A CN1313200C (en) | 2005-06-10 | 2005-06-10 | Magnesium aluminium spinel activated adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100784325A CN1313200C (en) | 2005-06-10 | 2005-06-10 | Magnesium aluminium spinel activated adsorbent |
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| Publication Number | Publication Date |
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| CN1724140A CN1724140A (en) | 2006-01-25 |
| CN1313200C true CN1313200C (en) | 2007-05-02 |
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| CNB2005100784325A Expired - Fee Related CN1313200C (en) | 2005-06-10 | 2005-06-10 | Magnesium aluminium spinel activated adsorbent |
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| CN105170074B (en) * | 2015-10-08 | 2018-01-05 | 萍乡市石化填料有限责任公司 | A kind of preparation method of magnesium aluminate spinel base hypersober |
| CN109589912B (en) * | 2019-01-29 | 2021-09-17 | 山东奥福环保科技股份有限公司 | Concentrated rotating wheel adsorption material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1336148A (en) * | 1970-06-09 | 1973-11-07 | Ici Ltd | Mixed oxide material |
| CN1011229B (en) * | 1988-09-26 | 1991-01-16 | 冶金工业部洛阳耐火材料研究院 | Method for synthesizing magnesium aluminate spinel |
| CN1086799A (en) * | 1992-11-10 | 1994-05-18 | 冶金工业部洛阳耐火材料研究院 | A kind of method of synthetic MgAl spinal |
| CN1382665A (en) * | 2001-04-26 | 2002-12-04 | 河南省登封市第二耐火材料总厂 | Synthetic magnesium aluminate spinel and preparation method thereof |
| CN1464037A (en) * | 2002-06-12 | 2003-12-31 | 中国石化集团齐鲁石油化工公司 | Low cost sulfur transformation resistant deoxidizing agent and process for preparing the same |
-
2005
- 2005-06-10 CN CNB2005100784325A patent/CN1313200C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1336148A (en) * | 1970-06-09 | 1973-11-07 | Ici Ltd | Mixed oxide material |
| CN1011229B (en) * | 1988-09-26 | 1991-01-16 | 冶金工业部洛阳耐火材料研究院 | Method for synthesizing magnesium aluminate spinel |
| CN1086799A (en) * | 1992-11-10 | 1994-05-18 | 冶金工业部洛阳耐火材料研究院 | A kind of method of synthetic MgAl spinal |
| CN1382665A (en) * | 2001-04-26 | 2002-12-04 | 河南省登封市第二耐火材料总厂 | Synthetic magnesium aluminate spinel and preparation method thereof |
| CN1464037A (en) * | 2002-06-12 | 2003-12-31 | 中国石化集团齐鲁石油化工公司 | Low cost sulfur transformation resistant deoxidizing agent and process for preparing the same |
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| CN1724140A (en) | 2006-01-25 |
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