CN104671266A - Process for preparing ultrafine aluminum hydroxide by seed crystal precipitation method - Google Patents
Process for preparing ultrafine aluminum hydroxide by seed crystal precipitation method Download PDFInfo
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- CN104671266A CN104671266A CN201310613172.1A CN201310613172A CN104671266A CN 104671266 A CN104671266 A CN 104671266A CN 201310613172 A CN201310613172 A CN 201310613172A CN 104671266 A CN104671266 A CN 104671266A
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Abstract
The invention provides a process for preparing ultrafine aluminum hydroxide. Alumina crude ore or crude aluminum hydroxide is dissolved in alkali lye so that a meta-aluminate solution is prepared, and the meta-aluminate solution and seed slurry are mixed and crystallize in a stator-rotor reactor so that the ultrafine aluminum hydroxide is prepared. The process has a low production cost and no pollution. The ultrafine aluminum hydroxide has good performances and can be used as an industrial additive and a fire retardant.
Description
Technical field
The present invention relates to a kind of producing and manufacturing technique of ultrafine aluminium hydroxide material, its feature, for adopting fixed-rotor reaction equipment as core crystalline reactor, is a kind of process for cleanly preparing process of low-cost and pollution-less.
Background technology
Aluminium hydroxide is the maximum and most widely used inorganic fire-retarded additive of consumption.Aluminium hydroxide can not only be fire-retardant as fire retardant, and can prevent from being fuming, do not produce dropping, do not produce toxic gas.Therefore, obtain and apply more widely, usage quantity is also increasing year by year.For fire-retardant in the industries such as thermosetting resin, thermoplastics, synthetic rubber, coating and building materials of being everlasting.
Aluminium hydroxide size directly affects its flame retardant resistance and fillibility.Increase the surface-area of aluminum hydroxide particles, make particle surface water vapor pressure increase, be conducive to the raising of flame retardant resistance.Along with granularity attenuates, the oxygen index of material improves.This is because the performance of fire retardation arranged by chemical reaction, so the fire retardant of equivalent, its particle diameter is less, and specific surface area is larger, and flame retardant effect is better.
The ultrafine aluminium hydroxide particle diameter that current domestic and international market is commonly used is many between 0.5 micron to 3 microns, and except flame-retardant additive, abrasive material, pottery, industrial adsorbents and catalytic carrier also have a large amount of demands to aluminium hydroxide.In existing ultrafine aluminium hydroxide production technique, the product cut size that chemical method is produced is comparatively homogeneous, and purity performance is superior, and wherein in industry, topmost method has two kinds: acid-base neutralisation method and traditional Bayer process.
The technique of acid-base neutralisation method mainly adopts highly basic dissolved oxygen aluminium rough, adopt acidic solution (adopting carbon dioxide, i.e. carbon method) more after rear refining and edulcoration, while producing aluminium hydroxide, obtain byproduct sodium carbonate, normal with waste liquid byproduct, technique also has the space of improving.Also crystal seed can be used in the production technique of tradition Bayer process, but crystal seed many employings chemical precipitation method obtains.Prepare in the factory of aluminium hydroxide in employing Bayer process, because the processing method gap of JZPD capsule method and major product is comparatively large, production equipment and process is not general, improves the overall cost of production, has the space of improvement yet.
Summary of the invention
The invention provides a kind of production technique of ultrafine aluminium hydroxide, have employed rotor-stator reactor (patent No. ZL200410042631.6) in processing condition, material internal recycle in process, without discharge, and cost is lower.
The technical process that invention adopts is as shown in Figure of description 1:
The process flow sheet (Figure of description 1) that the present invention adopts, its detailed process step is as follows:
(1) at 100 ~ 300 DEG C of temperature, adopt that aluminum oxide is rough is dissolved in the high alkali liquid of mass concentration 20 ~ 40%, make dense meta-aluminate saturated solution.
(2) by dense meta-aluminate saturated solution and seed slurry at 10 ~ 110 DEG C of temperature, 3:1 ~ 1:4 mixed cycle crystallization in proportion in rotor-stator reactor.
(3) determine-rotor device speed range is 300 ~ 3000rpm.
(4) mixed reaction solution under rotor-stator reactor Circulation through the crystallization process of 6 ~ 96h.
(5), after the reacting liquid filtering after crystallization being separated the solid phase prod employing process water washing obtained, at 100 ~ 120 DEG C, dry 24h obtains ultrafine aluminium hydroxide product.
(6) liquid that obtains is filtered through evaporation concentration, the evaporation condensed water of gained is for configuring seed slurry for rotor-stator reactor mixing step (established technology process the 2nd step), and the alkaline mother liquor after concentrating can be reused for dissolving crude aluminum ore deposit (established technology process the 1st step).
Wherein, the crystal seed in seed slurry adopts following processing step to synthesize:
(I) at 100 ~ 200 DEG C of temperature, adopt the rough or rough aluminium hydroxide of aluminum oxide to be dissolved in high alkali liquid, make the dense meta-aluminate saturated solution that mass concentration is 20% ~ 40%;
(II) at 10 ~ 90 DEG C of temperature, by dense meta-aluminate saturated solution and process water with the ratio of volume ratio 3:1 ~ 1:4 short mix in rotor-stator reactor;
(III) mixed reaction solution crystallization 12 ~ 120h under agitation;
(IV) reacting liquid filtering after crystallization is separated the solid phase prod obtained and adopts process water washing, at 100 ~ 120 DEG C, obtain crystal seed after dry 24h.
(V) filter the liquid that obtains through evaporation concentration, the evaporation condensed water of gained is used for rotor-stator reactor mixing step (Step II), and concentrated after alkaline mother liquor can be reused for and dissolve crude aluminum ore deposit (step I).
Beneficial effect of the present invention:
Seed production technique is close with major product production technique, and equipment is identical, can coproduction to reduce costs;
Adopt the production technique of material internal recycle, pollution-free, the simple cost of raw material is low;
The ultrafine aluminium hydroxide product degree of crystallinity of producing is good, can be used for industrial additive and fire retardant, excellent performance.
Accompanying drawing explanation
Fig. 1 is the technological process of production schematic diagram that kind of point-score prepares ultrafine aluminium hydroxide.
Fig. 2 is the XRD spectra of aluminium hydroxide crystal seed prepared by embodiment 1.
Fig. 3 is the XRD spectra of ultrafine aluminium hydroxide product prepared by embodiment 3.
Embodiment
Below enumerate embodiment and illustrate method for manufacturing aluminium hydroxide of the present invention and processing condition.But the present invention is not limited to following embodiment.
JZPD capsule example
Embodiment 1
At 100 DEG C of temperature, adopt that aluminum oxide is rough is dissolved in the high alkali liquid of mass concentration 25%, make dense meta-aluminate saturated solution.By strong solution and distilled water at 40 DEG C of temperature, 3:1 short mix in proportion in rotor-stator reactor, fixed-rotor speed is 300rpm.Mixed reaction solution is under continuous stirring through the crystallization process of 120h.Reacting liquid filtering after crystallization is separated the solid phase prod obtained and adopts process water washing 3 ~ 4 times, at 100 DEG C, dry 24h obtains the crystal seed for the preparation of ultrafine aluminium hydroxide.Filtrate carries out dissolving circulation technique again by concentrated solution after evaporation recovery process water.
Obtained aluminium hydroxide crystal seed carries out XRD sign, sees Figure of description 2.
Embodiment 2
At 200 DEG C of temperature, adopt that aluminum oxide is rough is dissolved in the high alkali liquid of mass concentration 40%, make dense meta-aluminate saturated solution.By strong solution and distilled water at 90 DEG C of temperature, 1:4 short mix in proportion in rotor-stator reactor, fixed-rotor speed is 3000rpm.Mixed reaction solution is under continuous stirring through the crystallization process of 12h.Reacting liquid filtering after crystallization is separated the solid phase prod obtained and adopts process water washing 3 ~ 4 times, at 120 DEG C, dry 24h obtains the crystal seed for the preparation of ultrafine aluminium hydroxide.Filtrate carries out dissolving circulation technique again by concentrated solution after evaporation recovery process water.
Ultrafine aluminium hydroxide prepares example
Embodiment 3
At 100 DEG C of temperature, adopt rough aluminium hydroxide to be dissolved in the high alkali liquid of mass concentration 25%, make dense meta-aluminate saturated solution.The crystal seed prepare embodiment 1 and process water are made into seed slurry, dense meta-aluminate saturated solution and seed slurry at 40 DEG C of temperature, 3:1 short mix in proportion in rotor-stator reactor, fixed-rotor speed is 3000rpm.The mixed reaction solution 40h that circulates in rotor-stator reactor carries out crystallization.At reacting liquid filtering after crystallization being separated latter 100 DEG C of the solid phase prod employing process water washing obtained, dry 24h obtains ultrafine aluminium hydroxide product.Filtrate for evaporating recovery process water preparation seed slurry, the filtrate after concentrated be reused for dissolve rough aluminium hydroxide or aluminum oxide rough.
Obtained aluminium hydroxide carries out XRD sign, sees Figure of description 3.
Embodiment 4
At 240 DEG C of temperature, adopt that aluminum oxide is rough is dissolved in the high alkali liquid of mass concentration 40%, make dense meta-aluminate saturated solution.The crystal seed prepare embodiment 1 and process water are made into seed slurry, dense meta-aluminate saturated solution and seed slurry at 100 DEG C of temperature, 1:2 short mix in proportion in rotor-stator reactor, fixed-rotor speed is 3000rpm.The mixed reaction solution 20h that circulates in rotor-stator reactor carries out crystallization.At reacting liquid filtering after crystallization being separated latter 100 DEG C of the solid phase prod employing process water washing obtained, dry 24h obtains ultrafine aluminium hydroxide product.Filtrate for evaporating recovery process water preparation seed slurry, the filtrate after concentrated be reused for dissolve rough aluminium hydroxide or aluminum oxide rough.
Claims (4)
1. prepare a production technique for ultrafine aluminium hydroxide, it is characterized in that adopting following steps:
(A) in a heated condition, adopt the rough or rough aluminium hydroxide of aluminum oxide to be dissolved in high alkali liquid, make dense meta-aluminate saturated solution;
(B) by dense meta-aluminate saturated solution and seed slurry at a certain temperature, in rotor-stator reactor, crystallization is mixed;
(C) in mixing process and mixed solution circulate in rotor-stator reactor crystallization for some time;
(D), after the reacting liquid filtering after crystallization being separated the solid phase prod employing process water washing obtained, ultrafine aluminium hydroxide product is obtained after drying;
(E) filter the liquid that obtains through evaporation concentration, after the evaporation condensed water of gained adds crystal seed mixing, be mixed with seed slurry, i.e. step B; And the alkaline mother liquor after concentrating can be reused for dissolving crude aluminum ore deposit or rough aluminium hydroxide, i.e. steps A.
2. production technique according to claim 1, is characterized in that adopting following processing condition:
A in () processing step A, heating temperature range is 100 ~ 300 DEG C, alkali lye mass concentration scope is 20 ~ 40%;
B in () processing step B, blend temperature range is 10 ~ 110 DEG C, the blending ratio scope of dense meta-aluminate saturated solution and seed slurry is volume ratio 3:1 ~ 1:4;
Fixed in (c) processing step B and processing step C-rotor device speed range is 300 ~ 3000rpm;
D the time range adopting fixed-rotor circulation crystallization in () processing step C is 6 ~ 96h;
E in () processing step D, drying conditions is dry 24h at 100 ~ 120 DEG C.
3. production technique according to claim 1, is characterized in that adopting following processing step to synthesize for the crystal seed preparing seed slurry in processing step B and step e:
(I) in a heated condition, adopt the rough or rough aluminium hydroxide of aluminum oxide to be dissolved in high alkali liquid, make dense meta-aluminate saturated solution;
(II) by dense meta-aluminate saturated solution and process water at a certain temperature, short mix in rotor-stator reactor;
(III) mixed reaction solution is through the crystallization process of certain hour;
(IV) reacting liquid filtering after crystallization is separated after the solid phase prod obtained adopts process water washing drying and obtains ultrafine aluminium hydroxide product;
(V) filter the liquid that obtains through evaporation concentration, the evaporation condensed water of gained is used for rotor-stator reactor mixing step, i.e. Step II; And the alkaline mother liquor after concentrating can be reused for dissolving crude aluminum ore deposit or rough aluminium hydroxide, i.e. step I.
4. production technique according to claim 3, is characterized in that adopting following processing condition to synthesize for the crystal seed preparing seed slurry in processing step B and step e:
I in () processing step I, heating temperature range is 100 ~ 200 DEG C, alkali lye mass concentration scope is 20 ~ 40%;
(ii) in processing step II, blend temperature range is 10 ~ 90 DEG C, and the blending ratio scope of dense meta-aluminate saturated solution and water is volume ratio 3:1 ~ 1:4;
(iii) determine in processing step II-rotor device speed range is 300 ~ 3000rpm;
(iv) in processing step III, the condition of crystallization process is the lower crystallization 12 ~ 120h of stirring;
V in () processing step IV, drying conditions is dry 24h at 100 ~ 120 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104893365A (en) * | 2015-06-18 | 2015-09-09 | 淄博鹏丰铝业有限公司 | Production method for aluminum hydroxide micro-powder subjected to surface coating and modification |
| CN111807392A (en) * | 2020-06-28 | 2020-10-23 | 山东泰星新材料股份有限公司 | Preparation method of submicron-grade superfine aluminum hydroxide, product and application thereof |
| CN116102041A (en) * | 2023-01-30 | 2023-05-12 | 中铝山东有限公司 | Preparation method of low-sodium low-oil-absorption superfine aluminum hydroxide |
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| CN1528668A (en) * | 2003-10-09 | 2004-09-15 | 淄博博洋化工有限公司 | Method for preparing fine grained active alumina |
| CN101348272A (en) * | 2008-08-29 | 2009-01-21 | 河南未来铝业（集团）有限公司 | Application process for drying aluminium hydroxide fines |
| CN101746796A (en) * | 2009-12-18 | 2010-06-23 | 中国铝业股份有限公司 | Method for preparing low-sodium aluminum hydroxide by decomposing sodium aluminate solution |
| CN102838148A (en) * | 2011-06-23 | 2012-12-26 | 中国石油化工股份有限公司 | Reactor and method used for preparing aluminum hydroxide |
| CN102992366A (en) * | 2012-11-19 | 2013-03-27 | 贵州省新材料研究开发基地 | Process method for preparing aluminum hydroxide micropowder |
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| CN1528668A (en) * | 2003-10-09 | 2004-09-15 | 淄博博洋化工有限公司 | Method for preparing fine grained active alumina |
| CN101348272A (en) * | 2008-08-29 | 2009-01-21 | 河南未来铝业（集团）有限公司 | Application process for drying aluminium hydroxide fines |
| CN101746796A (en) * | 2009-12-18 | 2010-06-23 | 中国铝业股份有限公司 | Method for preparing low-sodium aluminum hydroxide by decomposing sodium aluminate solution |
| CN102838148A (en) * | 2011-06-23 | 2012-12-26 | 中国石油化工股份有限公司 | Reactor and method used for preparing aluminum hydroxide |
| CN102992366A (en) * | 2012-11-19 | 2013-03-27 | 贵州省新材料研究开发基地 | Process method for preparing aluminum hydroxide micropowder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104893365A (en) * | 2015-06-18 | 2015-09-09 | 淄博鹏丰铝业有限公司 | Production method for aluminum hydroxide micro-powder subjected to surface coating and modification |
| CN104893365B (en) * | 2015-06-18 | 2017-06-13 | 淄博鹏丰铝业有限公司 | A kind of production method of surface coating modification aluminium hydroxide micro powder |
| CN111807392A (en) * | 2020-06-28 | 2020-10-23 | 山东泰星新材料股份有限公司 | Preparation method of submicron-grade superfine aluminum hydroxide, product and application thereof |
| CN116102041A (en) * | 2023-01-30 | 2023-05-12 | 中铝山东有限公司 | Preparation method of low-sodium low-oil-absorption superfine aluminum hydroxide |
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