CN105236454A - Method and apparatus for synthesizing hydrotalcite-like material by using coal gasification furnace residue as aluminum source - Google Patents
Method and apparatus for synthesizing hydrotalcite-like material by using coal gasification furnace residue as aluminum source Download PDFInfo
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- CN105236454A CN105236454A CN201510583221.0A CN201510583221A CN105236454A CN 105236454 A CN105236454 A CN 105236454A CN 201510583221 A CN201510583221 A CN 201510583221A CN 105236454 A CN105236454 A CN 105236454A
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- hydrotalcite
- slag
- coal gasification
- gasification furnace
- aluminium source
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Abstract
The invention relates to a method and an apparatus for synthesizing a hydrotalcite-like material by using coal gasification furnace residue as an aluminum source, and belongs to hydrotalcite-like material synthesis method and hydrotalcite-like material synthesis apparatus. The preparation method comprises: placing gasification furnace residue in a drying oven, drying for 72 h, grinding into powder with a particle size of less than 80 mesh by using a coal mill, calcining through a muffle furnace, and pre-treating the gasification furnace residue, wherein the coking of the calcining process can be effectively prevented through the pre-treating process; carrying out a complete stirring reaction on the calcined gasification furnace residue and 30% nitric acid for 6 h at a temperature of 80 DEG C, and filtering to obtain the filtrate, ie., the aluminum source for synthesizing the hydrotalcite-like material; adding a magnesium source to the filtrate, and carrying out double titration co-precipitation on the obtained solution and an alkali solution under a constant pH value of 9-10, wherein the magnesium source is a magnesium nitrate solution; and finally obtaining a mud compound, washing, filtering, and drying so as to obtain the hydrotalcite-like compound. According to the present invention, the coal gasified waste gasification furnace residue is adopted as the raw material so as to reduce the hydrotalcite-like production cost, and the experiment apparatus and the process are simple so as to achieve the high added value utilization of the coal gasification furnace and the low cost production of the hydrotalcite-like material.
Description
Technical field
The present invention relates to a kind of method and device of synthesis hydrotalcite-like material material, particularly a kind of utilize slag of coal gasification to be aluminium source synthesis hydrotalcite-like material material method and device.
Background technology
Slag of coal gasification is the primary solids waste of Coal Chemical Engineering Project, and fully utilizing it is the important factor that whole Coal Chemical Engineering Project realizes recycling economy.The composition of gasifier slag mainly comprises SiO
2, Al
2o
3, CaO and carbon residue etc.
At present, slag of coal gasification Land use systems is also more single, is mainly used in building materials, builds work, the blended feedstock such as road and stemming operation, and added value is lower.Therefore coal chemical industry is also at the diversification utilization actively inquiring into slag, such as, be raw material production high temperature ceramic material with gasifier slag, but is applied in by slag of coal gasification in the technique of synthesis hydrotalcite-like material and also rarely has people to study.
Houghite is a kind of laminated dihydroxy composite metal hydroxide (LayeredDoubleHydroxides is called for short LDHs), is a kind of important inorganic functional material.
Its chemical constitution can be expressed as [M
2+ 1-xm
3+ x(OH)
2]
x+[(A
n-)
x/nmH
2o]
x-, wherein M
2+for Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+deng divalent metal; M
3+for A1
3+, Cr
3+, Fe
3+, Sc
3+deng trivalent metal cation; A
n-for negatively charged ion, as CO
3 2-, NO
3 -, Cl
-, OH
-, SO
4 2-, PO
4 3-, C
6h
4(COO)
2 2-etc. inorganic and organic ion and complexing ion.Typical magnesia-alumina hydrotalcite molecular formula is Mg
6a1
2(OH)
16cO
34H
2o, has and is similar to brucite [Mg (OH)
2] regular octahedron structure.
Houghite has a series of excellent properties, and as the Modulatory character, interlayer anion interchangeability, memory effect etc. of laminate chemical constitution, be widely used in the fields such as polymer composite, catalytic material, environmental improvement, demand also increases year by year.But because houghite compound synthesis material cost is higher, still cannot realize large-scale cheap production at present, directly affect it and apply widely.
Summary of the invention
The object of the invention is to provide a kind of raw material to be easy to get, with low cost, environmental friendliness and be applicable to the method utilizing slag of coal gasification to be aluminium source synthesis hydrotalcite-like material material and the device of scale operation.
The object of the present invention is achieved like this: the preparation method of houghite: gasifier slag is placed in the dry 72h of loft drier, <80 object powder is worn into again with coal pulverizer, use retort furnace roasting again, carry out pre-treatment to gasifier slag, preprocessing process effectively prevents roasting process coking; By the gasifier slag that burnt and 30% nitric acid abundant stirring reaction 6h at 80 DEG C, the aluminium source of the filtrate that reaction mixture obtains after filtering and synthesis hydrotalcite-like material material; Add in filtrate by magnesium source, under constant pH 9-10 condition, carry out two titration coprecipitation reaction with alkaline solution, magnesium source is wherein magnesium nitrate solution; Finally obtain mud synthetics, after washing, filtration, drying, obtain houghite compound.
PH value in reaction is controlled by the NaOH solution of 1M in reaction.
The aluminium source of synthesis hydrotalcite-like material, from slag of coal gasification, is reacted and is carried out in water bath with thermostatic control, and constantly stirs in dropping process, controls bath temperature.
Dropping process in the reactor answers the period within 1h.
Crystallization temperature is 70 DEG C, and keeps this temperature crystallization 48h.
Special purpose device comprises: magnetic stirring apparatus and four-hole boiling flask, and four-hole boiling flask is placed on magnetic stirring apparatus, and a bite of four-hole boiling flask places pH meter, and insert mechanical stirring rod flatly, other two mouthfuls respectively connect constant pressure funnel.
Beneficial effect, owing to have employed such scheme, pretreated slag of coal gasification is selected to be aluminium source, adopt two titration Co deposited synthesis houghite, by Special experimental apparatus, the pH value in reaction process can be controlled constantly, significantly reduce production cost, simplify production technique, fully realize the Appropriate application of solid waste, decrease environmental pollution.Houghite synthesized by the present invention has that complete layered crystal structure, crystalline form are single, epigranular.Reach object of the present invention.
Accompanying drawing illustrates:
Fig. 1 is the special purpose device figure of the houghite that the present invention synthesizes.
Embodiment
Pretreated slag of coal gasification is adopted to be aluminium source in the invention process example.
Embodiment 1: first by slag of coal gasification dry 72h in loft drier, worn into coal pulverizer and be less than 80 object powder, this process effectively prevents coking in roasting process, puts it into roasting in retort furnace, obtains pretreatment product.Pretreated gasifier slag is got 20g interpolation 8gNaCl and be placed on 700 DEG C of roasting 3h in retort furnace, measure the constituent content in above-mentioned product of roasting with ICP-AES.Product of roasting is added in the nitric acid of 30wt%, stir 6h with the rotating speed 80 DEG C of 210r/min and obtain aluminium source.Take the magnesium nitrate hexahydrate (mol ratio: Mg of 51.2g
2+/ Al
3+=2) to add in the aluminium source solution that slag of coal gasification obtains to obtain A liquid, the sodium hydroxide of preparation 1M is B liquid, A, B liquid 25 DEG C is carried out two titration and obtains co-precipitation slurries, keep pH to be 9,70 DEG C of thermostatical crystallization 48h, filter, washing is to neutral, and 80 DEG C of dry 72h obtain houghite powder.
Special purpose device comprises: magnetic stirring apparatus and four-hole boiling flask, and four-hole boiling flask is placed on magnetic stirring apparatus, and a bite of four-hole boiling flask places pH meter, inserts mechanical stirring rod flatly, and other two mouthfuls respectively connect a constant pressure funnel.
Embodiment 2: first by slag of coal gasification dry 72h in loft drier, is worn into coal pulverizer and is less than 80 object powder (this process effectively prevents coking in roasting process), put it into retort furnace roasting, obtain pretreatment product.Pretreated gasifier slag is got 20g to add 8gNaCl and be placed in retort furnace 700 DEG C of roasting 3h, measure the constituent content in above-mentioned product of roasting with ICP-AES.Product of roasting is added in the nitric acid of 30wt%, stir 6h with the rotating speed 80 DEG C of 210r/min and obtain aluminium source.Take the magnesium nitrate hexahydrate (mol ratio: Mg of 51.2g
2+/ Al
3+=2) to add in the aluminium source solution that slag of coal gasification obtains to obtain A liquid, the sodium hydroxide of preparation 1M is B liquid, A, B liquid 70 DEG C is carried out two titration and obtains co-precipitation slurries, keep pH to be 9,70 DEG C of thermostatical crystallization 48h, filter, washing is to neutral, and 80 DEG C of dry 72h obtain houghite powder.
Other and enforcement are together.
Embodiment 3: first by slag of coal gasification dry 72h in loft drier, then worn into <80 object powder (this process effectively prevents roasting process coking) with coal pulverizer, then use retort furnace roasting, obtain pretreatment product.Pretreated gasifier slag is got 20g to add 8gNaCl and be placed in retort furnace 700 DEG C of roasting 3h, measure the constituent content in above-mentioned product of roasting with ICP-AES.Product of roasting is added in the nitric acid of 30wt%, stir 6h with the rotating speed 80 DEG C of 210r/min and obtain aluminium source.Take the magnesium nitrate hexahydrate (mol ratio: Mg of 51.2g
2+/ Al
3+=2) to add in the aluminium source solution that slag of coal gasification obtains to obtain A liquid, the sodium hydroxide of preparation 1M is B liquid, A, B liquid 25 DEG C is carried out two titration and obtains co-precipitation slurries, keep pH to be 10,70 DEG C of thermostatical crystallization 48h, filter, washing is to neutral, and 80 DEG C of dry 72h obtain houghite powder.
Other and enforcement are together.
Embodiment 4: first by slag of coal gasification dry 72h in loft drier, then worn into <80 object powder (this process effectively prevents roasting process coking) with coal pulverizer, then use retort furnace roasting, obtain pretreatment product.Pretreated gasifier slag is got 20g to add 8gNaCl and be placed in retort furnace 700 DEG C of roasting 3h, measure the constituent content in above-mentioned product of roasting with ICP-AES.Product of roasting is added in the nitric acid of 30wt%, stir 6h with the rotating speed 80 DEG C of 210r/min and obtain aluminium source.Take the magnesium nitrate hexahydrate (mol ratio: Mg of 51.2g
2+/ Al
3+=2) to add in the aluminium source solution that slag of coal gasification obtains to obtain A liquid, the sodium hydroxide of preparation 1M is B liquid, A, B liquid 70 DEG C is carried out two titration and obtains co-precipitation slurries, keep pH to be 10,70 DEG C of thermostatical crystallization 48h, filter, washing is to neutral, and 80 DEG C of dry 72h obtain houghite powder.
Other and enforcement are together.
Claims (6)
1. one kind utilizes slag of coal gasification for the method for aluminium source synthesis hydrotalcite-like material material, it is characterized in that: the preparation method of houghite is for be placed in the dry 72h of loft drier by gasifier slag, worn into coal pulverizer and be less than 80 object powder, put it into roasting in retort furnace, pre-treatment is carried out to gasifier slag, effectively prevents coking in roasting process; By the gasifier slag that burnt and 30% nitric acid in 80
oabundant stirring reaction 6h under C, the aluminium source of the filtrate that reaction mixture obtains after filtering and synthesis hydrotalcite-like material material; Add in filtrate by magnesium source, under constant pH 9-10 condition, carry out two titration coprecipitation reaction with alkaline solution, wherein magnesium source is magnesium nitrate solution; Finally obtain slurry mixture, after washing, filtration, drying, obtain houghite compound.
2. the slag of coal gasification that utilizes according to claim 1 is for the method for aluminium source synthesis hydrotalcite-like material material, it is characterized in that: control pH value in reaction by the NaOH solution of 1M in reaction.
3. the slag of coal gasification that utilizes according to claim 1 is for the method for aluminium source synthesis hydrotalcite-like material material, it is characterized in that: the aluminium source of synthesis hydrotalcite-like material is from slag of coal gasification, reaction is carried out in water bath with thermostatic control, and constantly stirs in dropping process, controls bath temperature.
4. the slag of coal gasification that utilizes according to claim 3 is for the method for aluminium source synthesis hydrotalcite-like material material, it is characterized in that: dropping process in the reactor answers the period within 1h.
5. the slag of coal gasification that utilizes according to claim 3 is for the method for aluminium source synthesis hydrotalcite-like material material, it is characterized in that: crystallization temperature is 70
oc, and keep this temperature crystallization 48h.
6. the slag of coal gasification that utilizes according to claim 1 is for the device of aluminium source synthesis hydrotalcite-like material MATERIALS METHODS, it is characterized in that: special purpose device comprises: magnetic stirring apparatus and four-hole boiling flask, four-hole boiling flask is placed on magnetic stirring apparatus, a bite of four-hole boiling flask places pH meter, insert mechanical stirring rod flatly, other two mouthfuls respectively connect a constant pressure funnel.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107847923A (en) * | 2016-03-18 | 2018-03-27 | 株式会社Lg化学 | The preparation method of oxidative dehydrogenation catalyst |
| CN110586622A (en) * | 2019-09-24 | 2019-12-20 | 新疆天业（集团）有限公司 | Method for comprehensively utilizing gasification furnace slag resources |
-
2015
- 2015-09-14 CN CN201510583221.0A patent/CN105236454A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 寇鹏: "镁铝水滑石的制备及在印染废水处理中的应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107847923A (en) * | 2016-03-18 | 2018-03-27 | 株式会社Lg化学 | The preparation method of oxidative dehydrogenation catalyst |
| CN107847923B (en) * | 2016-03-18 | 2020-08-07 | 株式会社Lg化学 | Method for preparing catalyst for oxidative dehydrogenation |
| US10926246B2 (en) | 2016-03-18 | 2021-02-23 | Lg Chem, Ltd. | Method of preparing catalyst for oxidative dehydrogenation |
| CN110586622A (en) * | 2019-09-24 | 2019-12-20 | 新疆天业（集团）有限公司 | Method for comprehensively utilizing gasification furnace slag resources |
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