CN102070168B - Method for reducing sodium oxide in aluminum oxide by using carbon dioxide - Google Patents
Method for reducing sodium oxide in aluminum oxide by using carbon dioxide Download PDFInfo
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- CN102070168B CN102070168B CN 201010579645 CN201010579645A CN102070168B CN 102070168 B CN102070168 B CN 102070168B CN 201010579645 CN201010579645 CN 201010579645 CN 201010579645 A CN201010579645 A CN 201010579645A CN 102070168 B CN102070168 B CN 102070168B
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 40
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 20
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229910001948 sodium oxide Inorganic materials 0.000 title claims abstract description 18
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000011734 sodium Substances 0.000 claims abstract description 36
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 25
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 24
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 238000003837 high-temperature calcination Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 37
- 239000012153 distilled water Substances 0.000 description 21
- 239000003513 alkali Substances 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- 239000012452 mother liquor Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 hardness is large Chemical compound 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a method for reducing sodium oxide in aluminum oxide by using carbon dioxide. The method comprises the following steps of: pre-baking aluminum hydroxide and adding a baked product into water to prepare baked product aqueous solution for later use; introducing CO2 gas into the baked product aqueous solution and fully stirring; adding a small number of sodium removing agents into the baked product aqueous solution into which the CO2 gas is introduced; performing liquid-solid separation; drying to obtain a solid; calcining the solid at a high temperature; and naturally cooling to obtain low-sodium aluminum oxide. By the method, the cost for manufacturing the high-temperature low-sodium aluminum oxide can be reduced, the variation in product performance caused by the sodium removing agent can be reduced, and a new approach is discovered for utilization of the carbon dioxide.
Description
Technical field
The present invention relates to the high temperature alumina production technique, particularly a kind of method of utilizing the carbon dioxide reduction sodium oxide in aluminum oxide.
Background technology
High temperature alumina because of have fusing point high (2040 ℃), the raw materials for production of characteristics are mainly used in refractory materials, automobile spark plug, electronic substrates, cutter, engineering parts and the high alumina ceramic such as hardness is large, unreactiveness is strong, electrical insulating property is excellent, Heat stability is good, wear resistance are strong, its prospect is boundless.
Na
2O content is the important technology index of high temperature alumina, and this is due to pottery and fire resisting material field, Na
2The height of O content directly affects intensity and the resistivity against fire of product, finally affects profile and the use of product.Usually alkali content is higher, α-Al
2O
3The inversion of phases rate is lower, and physical strength is just poorer, further causes distortion and the cracking of alumina article.Take pre-burning aluminium hydroxide as raw material, add the auxiliary agent pre-treatment and reduce sodium oxide content, be the classical pathway of producing low sodium Alpha-alumina in calcining more than 1300 ℃ afterwards.But, the Na that the industrial aluminium hydroxide calcinate carries
2O adds up to 0.26～0.43%, is difficult to by adding the technology such as reagent and calcinate post-processed, sodium oxide content in calcination product be controlled to Na
2O＜0.10%, α-Al
2O
3〉=95% target cause distortion and the cracking of alumina article, and the use of taking off the sodium agent can produce certain side effect, and for example boric acid and compound thereof are in a liquid state and are attached on alumina surface, make its adhesion become piece and the shutoff feed opening.Commercially available low sodium high temperature alumina is mainly with Na in product both at home and abroad
2O content is divided into four grades, sees the following form:
| Grade | Logical product high temperature | Middle sodium high temperature | Low sodium high temperature | Ultralow sodium high temperature |
| Na 2O(％) | 0.3 | 0.15 | ＜0.10 | ≤0.05 |
Find after deliberation Al (OH)
3The occurrence patterns of middle alkali is divided into four classes, as following table:
| Occurrence patterns | Na 2O(％) | Classification |
| (1) particle surface absorption alkali | 0.10 | I mother liquor alkali |
| (2) glomerocryst parcel alkali | 0.1～0.2 | II lattice alkali |
| (3) Na displacement Al (OH) 3In hydrogen atom | 0.05～0.1 | The III combined alkali |
| (4)Na 2O·Al 2O3·2SiO 2·nH 2O | 0.01～0.03 | The IV compound |
Wherein I mother liquor alkali can wash with water and remove; Difficulty is gone in the parcel alkali cleaning, only can partly wash away.II lattice alkali is water insoluble, when only having crystalline network to reset, just can become water-soluble alkali.In addition, a large amount of carbon dioxide of discharging in alumina producing is one of problem that perplexs China's energy-saving and emission-reduction task always.
Summary of the invention
The object of the invention is to provide a kind of can make Na in aluminum oxide
2The method of utilizing the carbon dioxide reduction sodium oxide in aluminum oxide of O＜0.10%.
Provide according to an aspect of the present invention a kind of method of utilizing carbon dioxide gas to reduce sodium oxide in aluminum oxide to comprise:
Aluminium hydroxide is carried out preroasting, and then the roasting after product being added to the water obtains the product of roasting aqueous solution, stand-by;
With the logical CO of the product of roasting aqueous solution
2Gas, and fully stir;
With the mentioned solution solid-liquid separation, add in the gained solid product and take off the sodium agent, the mixing post-drying, then with its high-temperature calcination, namely obtain low sodium high temperature alumina after naturally cooling.
The present invention utilizes the aluminum hydride correlation properties, falls mother liquor alkali and lattice alkali in aluminum oxide by carbon dioxide reaction more than needed, makes sodium oxide in aluminum oxide content reduce by 71%, reach 0.12%, and then save the high-temperature roasting cost, and then add and take off on a small quantity the sodium agent, can reach Na in aluminum hydride
2The requirement of O＜0.10%; Produce the alumina with high temperature and low sodium cost thereby reduce, and reduced and taken off the product performance change that the sodium agent causes.
Description of drawings
Fig. 1 reduces the process flow sheet of the method for sodium oxide in aluminum oxide for the carbon dioxide gas that utilizes that the embodiment of the present invention provides.
The object of the invention, function and advantage are described further with reference to accompanying drawing in connection with embodiment.
Embodiment
As shown in Figure 1, the technical process that the embodiment of the present invention provides, operation as follows:
Embodiment 1
Step 1, with industrial aluminium hydroxide in 600 ℃ of lower preroastings 1 hour, then the roasting after product is joined and get the product of roasting aqueous solution, the liquid-solid ratio L/S=10 of aluminum oxide, i.e. 100g aluminum oxide in distilled water and roasting after product in distilled water, 1.0L distilled water is stand-by;
Step 2, the step 1 product of roasting aqueous solution was stirred 1 hour with the speed of 350r/ minute under 90 ℃ of water bath with thermostatic control conditions.
Step 3, with the above-mentioned CO that passes into
2The aqueous solution solid-liquid separation of gas, add boric acid in the gained solid and do to take off the sodium agent, its addition is 0.15% of amount of solid, first oven dry under 115 ℃, then with it in 1350 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate is less than high-temperature calcination under 1 ℃ of/minute condition, the sodium oxide in aluminum oxide that obtains after naturally cooling＞0.10% (referring to table 1)
Embodiment 2
Step 1, with industrial aluminium hydroxide in 500 ℃ of lower preroastings 1 hour, then the roasting after product is joined in distilled water, the liquid-solid ratio L/S=10 of aluminum oxide in distilled water and roasting after product, i.e. 150g aluminum oxide, 1.5L distilled water, stand-by;
Step 2, with the step 1 product of roasting aqueous solution under 90 ℃ of water bath with thermostatic control conditions with 0.15m
3The flow of/(L hour) passes into CO
2Gas stirred 1 hour with the speed of 350r/ minute simultaneously.
Step 3, with the above-mentioned CO that passes into
2The aqueous solution solid-liquid separation of gas, add aluminum fluoride in the gained solid and do to take off the sodium agent, its addition is 0.05% of amount of solid, first oven dry under 115 ℃, then with it in 1350 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate namely obtains the aluminum oxide (referring to table 1) of sodium oxide＜0.10% less than high-temperature calcination under 1 ℃ of/minute condition after naturally cooling.
Embodiment 3
Step 1, with industrial aluminium hydroxide in 600 ℃ of lower preroastings 1 hour, then the roasting after product is joined in distilled water, the liquid-solid ratio L/S=10 of aluminum oxide in distilled water and roasting after product, i.e. 130g aluminum oxide, 1.3L distilled water, stand-by;
Step 2, with the step 1 product of roasting aqueous solution under 90 ℃ of water bath with thermostatic control conditions with 0.2m
3The flow of/(L hour) passes into CO
2Gas stirred 1 hour with the speed of 350r/ minute simultaneously.
Step 3, with the above-mentioned CO that passes into
2The aqueous solution solid-liquid separation of gas, add boric acid in the gained solid and do to take off the sodium agent, its addition is 0.20% of amount of solid, first oven dry under 115 ℃, then with it in 1350 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate namely obtains the aluminum oxide (referring to table 1) of sodium oxide＜0.10% less than high-temperature calcination under 1 ℃ of/minute condition after naturally cooling.
Embodiment 4
Step 1, with industrial aluminium hydroxide in 600 ℃ of lower preroastings 1 hour, then the roasting after product is joined in distilled water, the liquid-solid ratio L/S=10 of aluminum oxide in distilled water and roasting after product, i.e. 130g aluminum oxide, 1.3L distilled water, stand-by;
Step 2, with the step 1 product of roasting aqueous solution under 90 ℃ of water bath with thermostatic control conditions with 0.25m
3The flow of/(L hour) passes into CO
2Gas stirred 1 hour with the speed of 450r/ minute simultaneously.
Step 3, with the above-mentioned CO that passes into
2The aqueous solution solid-liquid separation of gas, add Neutral ammonium fluoride in the gained solid and do to take off the sodium agent, its addition be in the aqueous solution amount of solid 0.1%, first oven dry under 115 ℃, then with it in 1350 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate namely obtains the aluminum oxide (referring to table 1) of sodium oxide＜0.10% less than high-temperature calcination under 1 ℃ of/minute condition after naturally cooling.
Embodiment 5
Step 1, with industrial aluminium hydroxide in 600 ℃ of lower preroastings 1 hour, then the roasting after product is joined in distilled water, the liquid-solid ratio L/S=8 of aluminum oxide in distilled water and roasting after product, i.e. 162g aluminum oxide, 1.3L distilled water, stand-by;
Step 2, the step 1 product of roasting aqueous solution is passed into CO2 gas with the flow of 0.25m3/ (L hour) under 95 ℃ of water bath with thermostatic control conditions, stirred 1 hour with the speed of 600r/ minute simultaneously.
Step 3, with the above-mentioned aqueous solution solid-liquid separation that passes into CO2 gas, add ammonium chloride in the gained solid and do to take off the sodium agent, its addition is 0.1% of amount of solid, first oven dry under 115 ℃, then with it in 1350 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate namely obtains the aluminum oxide (referring to table 1) of sodium oxide＜0.10% less than high-temperature calcination under 1 ℃ of/minute condition after naturally cooling.
Embodiment 6
Step 1, with industrial aluminium hydroxide in 600 ℃ of lower preroastings 1 hour, then the roasting after product is joined in distilled water, the liquid-solid ratio L/S=20 of aluminum oxide in distilled water and roasting after product, i.e. 65g aluminum oxide, 1.3L distilled water, stand-by;
Step 2, the step 1 product of roasting aqueous solution is passed into CO2 gas with the flow of 0.25m3/ (L hour) under 95 ℃ of water bath with thermostatic control conditions, stirred 1 hour with the speed of 630r/ minute simultaneously.
Step 3, with the above-mentioned aqueous solution solid-liquid separation that passes into CO2 gas, add 0.05% Neutral ammonium fluoride or 0.05% boric acid in the gained solid and do to take off the sodium agent, first oven dry under 115 ℃, then with it in 1350 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate namely obtain the aluminum oxide (referring to table 1) of sodium oxide＜0.10% less than high-temperature calcination under 1 ℃ of/minute condition after naturally cooling.
Embodiment 7
Step 1, with industrial aluminium hydroxide in 600 ℃ of lower preroastings 1 hour, then the roasting after product is joined in distilled water, the liquid-solid ratio L/S=10 of aluminum oxide in distilled water and roasting after product, i.e. 130g aluminum oxide, 1.3L distilled water, stand-by;
Step 2, the step 1 product of roasting aqueous solution is passed into CO2 gas with the flow of 0.1m3/ (L hour) under 90 ℃ of water bath with thermostatic control conditions, stirred 1 hour with the speed of 430r/ minute simultaneously.
Step 3, with the above-mentioned product of roasting aqueous solution solid-liquid separation that passes into CO2 gas, add aluminum fluoride in the gained solid and do to take off the sodium agent, its addition is 0.05% of amount of solid, first oven dry under 115 ℃, then with it in 1450 ℃, greater than 100Pa pressure, dry air atmosphere, heat-up rate namely obtains the aluminum oxide (referring to table 1) of sodium oxide＜0.10% less than high-temperature calcination under 1 ℃ of/minute condition after naturally cooling.Detect the preroasting product, it is the roasting after product of embodiment of the present invention 2-7, wherein Na2O content improves 23%-33%, this is that lattice key due to aluminium hydroxide is come out to greatest extent, become water soluble alkali by insoluble alkali, then the roasting after product is passed into CO2 gas under the water bath with thermostatic control condition, eliminate as far as possible mother liquor alkali and lattice alkali in the Aluminium hydroxide roasting product, make the alkali content in product be down to 0.12% left and right.At last, the requirement that the sodium agent can reach the low desirable Na2O of sodium high temperature alumina industry＜0.10% is taken off in interpolation on a small quantity.
Table 1 test-results
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (6)
1. a method of utilizing carbon dioxide gas to reduce sodium oxide in aluminum oxide, is characterized in that, comprising:
Aluminium hydroxide is carried out preroasting, and then the roasting after product being added to the water obtains the product of roasting aqueous solution; The temperature 350-650 of described preroasting ℃, the time of described preroasting is 1-3 hour;
With the logical CO of the product of roasting aqueous solution
2Gas, and fully stir; The described product of roasting aqueous solution is with 0.1-0.25m under 80-98 ℃ of water bath with thermostatic control condition
3/ (Lh) flow passes into CO
2Gas 0.5-3 hour;
With the mentioned solution solid-liquid separation, to add in the gained solid and take off the sodium agent, the mixing post-drying with its high-temperature calcination, namely obtains low sodium high temperature alumina after naturally cooling; The environment of described high-temperature calcination is 1100-1450 ℃, greater than 100Pa pressure, and dry air atmosphere, heat-up rate is less than the condition of 1 ℃/min; The time of described high-temperature calcination is 1 ~ 3 hour.
2. method according to claim 1 is characterized in that:
Described pre-calcination temperature is 600 ℃, is 1 hour in the time of 600 ℃ of lower preroastings.
3. method according to claim 2 is characterized in that:
The described product of roasting aqueous solution is with 0.25m under 95 ℃ of water bath with thermostatic control conditions
3/ (Lh) flow passes into CO
2Gas 1 hour.
4. method according to claim 1 is characterized in that:
Described aluminium hydroxide is that granularity is less than the aluminium hydroxide of 50 μ m.
5. method according to claim 1 is characterized in that:
Described stirring is the speed stirring with 350-650r/ minute.
6. method according to claim 1 is characterized in that:
Describedly take off the sodium agent and comprise fluorochemicals, chlorine-containing compound or boric acid.
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| CN102320638A (en) * | 2011-08-04 | 2012-01-18 | 中国铝业股份有限公司 | Preparation method of low-sodium fine grain alumina |
| CN103332718B (en) * | 2013-07-10 | 2015-09-30 | 晋城市富基新材料股份有限公司 | A kind of preparation method of ultra-fine, low sodium Alpha-alumina micro mist |
| CN104628023B (en) * | 2015-02-13 | 2016-05-25 | 山东长基化工新材料有限公司 | The preparation method of ultralow sodium high temperature alpha-phase aluminum oxide |
| CN107500324A (en) * | 2017-08-16 | 2017-12-22 | 云南铝业股份有限公司 | The method for preparing high purity aluminium oxide |
| CN108751242B (en) * | 2018-08-27 | 2020-09-01 | 三门峡义翔铝业有限公司 | Low-sodium alumina decomposition process and low-sodium alumina |
| CN109761254A (en) * | 2019-02-02 | 2019-05-17 | 中国铝业股份有限公司 | A method of reducing aluminium hydroxide or sodium oxide in aluminum oxide impurity content |
| CN113233877A (en) * | 2021-05-12 | 2021-08-10 | 中铝山东有限公司 | Sodium removal method for calcining alpha alumina |
| CN114873616B (en) * | 2022-06-13 | 2023-10-03 | 中国铝业股份有限公司 | Low-sodium alumina and preparation method thereof |
| CN114940507B (en) * | 2022-06-22 | 2023-11-14 | 神华准能资源综合开发有限公司 | Method for extracting alumina from fly ash |
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| CN101780969A (en) * | 2009-12-18 | 2010-07-21 | 中国铝业股份有限公司 | Alumina carbon mother liquid processing method |
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| CN101780969A (en) * | 2009-12-18 | 2010-07-21 | 中国铝业股份有限公司 | Alumina carbon mother liquid processing method |
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| 冯国政.高温低钠氧化铝的研制.《矿产保护与利用》.2005,(第5期),第39-43页. * |
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