CN102398914A - Method for modifying Bayer process, processing low-grade diaspore bauxite and producing alumina - Google Patents
Method for modifying Bayer process, processing low-grade diaspore bauxite and producing alumina Download PDFInfo
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Abstract
The invention provides a method for modifying a Bayer process, processing low-grade diaspore bauxite and producing alumina. The method comprises steps that: (1) silicon is chemically pre-removed, wherein the low-grade bauxite is immersed into a sodium aluminate solution containing a stabilizing agent, such that a slurry containing dissolved silica is obtained; (2) obtained high-silicon sodium aluminate solution is processed through desilication, wherein desilication crystal seeds are added to the slurry processed through filtration, such that desilication is carried out; (3) the sodium aluminate solution is processed through seed precipitation, wherein aluminum hydroxide crystal seeds are added to the sodium aluminate solution processed through desilication, such that seed precipitation is carried out; (4) the obtained aluminum hydroxide product is baked, such that an alumina product is obtained; (5) a high-pressure dissolution process is carried out, wherein the obtained seed precipitation mother liquor is processed through evaporation and alkali supplementation, and is used in high-pressure dissolution of a concentrate obtained in the step (2); a stabilizing agent is added to the obtained sodium aluminate solution, the sodium aluminate solution is then used for processing the next batch of bauxite, and the steps (1) to (4) are repeated. The method provided by the invention is suitable to be used for processing low-grade diaspore bauxite. With the method, a silicon scaling problem in alumina industries can be effectively solved, energy consumption can be substantially improved, and the quality of the finished product alumina can be improved.
Description
Technical field
The present invention relates to the bauxite process field, particularly, the present invention relates to a kind of improvement Bayer process processing low-grade diaspore type bauxite production method of alumina.
Background technology
At present in alumina producing, that realizes suitability for industrialized production mainly contains Bayer process, sintering process and mixed combining method.Wherein Bayer process has the advantage that energy consumption is low, flow process is simple, production cost is low; But the employing alumina producing Bayer process is strict to raw material; Its alumina silica ratio of general requirement is greater than 8, is specially adapted to the alumina producing that three high water-type bauxite raw materials of alumina silica ratio carry out.And the bauxite of China is alumina silica ratio (Al in the bauxite more than 80%
2O
3And SiO
2Mass ratio) 4～8 middle low-grade diasporite type; Because the dioxide-containing silica of this bauxite is high; Therefore can not directly apply in the low pure bayer process of production cost, and have to adopt sintering process or the mixed combining method technology that flow process is long, energy consumption is higher, construction investment is bigger.How according to this situation, developing the alumina producing novel process that flow process is simple, energy consumption is lower, can effectively reduce cost, is the strategic problem that China aluminum oxide enterprise must solve.
Along with alumina silica ratio greater than 8 monohydrated bauxite reduce day by day and cut down the consumption of energy, the needs of production cost, utilize low-grade diasporite type bauxite to be the alumina producing raw material, adopting alumina producing Bayer process is an important topic of aluminum oxide industry.People have carried out a large amount of research for this reason, and one of them approach improves the pure Bayer process of tradition exactly.
Traditional Bayer process essence is reflected at hocketing under the different condition below being exactly:
To be bauxite through alkaline solution press boils stripping and handles, and makes aluminum oxide wherein get into liquid phase.Some impurity components in the mineral are deleterious to reaction in this course, and are wherein maximum to the influence degree of reaction with the silicon composition.Silicon composition in the conventional Bayer process process in leaching ore pulp and alkaline reaction generate and contain sodium aluminosilicate of water, and its molecular formula roughly is equivalent to Na
2OAl
2O
31.7SiO
2NH
2O, wherein Al
2O
3With SiO
2Be equal in weight, promptly A/S is 1, if the whole SiO in the ore
2Be converted into this sodium aluminosilicate of water that contains, every 1kg SiO
2Will cause 1kg Al
2O
3With 0.608kg Na
2The O loss.Make under pressure is boiled condition the SiO in the ore
2Generate with alkali reaction and to contain sodium aluminosilicate of water, discharge flow process, make alkaligenous chemical loss and have to reclaim again, strengthened production energy consumption, make the production cost rising with the agglomerating method with the residue red mud.It has been generally acknowledged that the low bauxite of alumina silica ratio can cause quite high alkaline consumption in Bayer process is produced, and make production cost too high.Generally believe that at present A/S is not just suitable to conventional Bayer process production below 7～8.
For reducing alkaline consumption, energy consumption and more efficient use China bauxite resource, traditional Bayer process many improvement have been carried out, like new production processes such as Liquor of Ore Dressing Bayer process, lime bayer method, series process, Bayer aquation method, hydrothermal methods.In above-mentioned production technique, still there are some problems, used chemical agent, and cause a large amount of mine tailings to utilize, be unfavorable for effective utilization of China's bauxite like Liquor of Ore Dressing Bayer process; Though lime bayer method has reduced alkaline consumption, exist the alumina recovery rate low, problem such as the silicon fouling is serious; Though series process can improve the utilization ratio of resource, also there is sintering process in it, and energy consumption is still bigger; Bayer aquation method, hydrothermal method can improve the recovery of aluminum oxide, can reduce alkaline consumption, energy consumption again; Handling middle-low bauxite has greater advantage, but exists high causticity ratio's solution to be difficult to obtain, and high causticity ratio's solution decomposes difficult; Perhaps adopt the method for heavy aluminium to handle; Exist heavy filter residue more again, can not efficient recovery etc. problem, therefore be difficult to realize industriallization.
In addition, apply for a patent 20041004691, proposed " symmetrical Bayer process " for effectively handling high-silica diaspore ore.It uses lower concentration causticity sodium hydroxide solution unlike traditional Bayer process; And be to use highly concentrated solution stripping bauxite; After stripping is accomplished, the concentration of the causticity sodium oxide the when concentration of causticity sodium oxide is greater than the common thermodynamic(al)equilibrium of hydrated alumina (bauxite) under the stripping temperature and sodium aluminate (or sodium aluminate hydrate) in the solution.The balance of stripping system like this, is the dissolution-crystallization balance between sodium aluminate solution and sodium aluminate crystal by the bauxite and the equilibrium conversion between the sodium aluminate solution of traditional Bayer process.Therefore, gipsite no matter, boehmite still is that diaspore all can not stable existence.But this method need adopt higher alkali concn, is difficult for the realization filtering separation, and is relatively stricter to equipment requirements, and a large amount of moisture of requirements of process evaporation, and it is also relatively more difficult to reclaim alkali from the stripping slag.Chinese patent CN1807251A discloses a kind of " from high-silica diaspore ore, extracting method of alumina "; This method is that symmetrical Bayer process and high pressure water chemical method are combined; Utilize symmetrical Bayer process directly to handle high-silica diaspore ore; Extract aluminum oxide, adopt high pressure water chemical Treatment red mud again, reclaim wherein by SiO
2Bonded Al
2O
3, the solution that obtains needn't be handled again, directly send symmetrical Bayer process system stripping next batch ore deposit, and the hydrated sodium silicate calcium that is generated reclaims alkali wherein through hydrolysis.But the alkali concn that the high pressure water chemical part of this method adopts is higher, and liquid-solid separation is difficulty comparatively, and the flow process relative complex, and is not easy to operate.
Prior art is when processing low-grade diaspore type bauxite stone; Or energy consumption height, complex process, cost are high and unstable product quality, or added chemical reagent, the alumina recovery rate is low, and causes a large amount of mine tailings to utilize; Or the alkali concn that adopts is higher; Make liquid-solid separation comparatively difficult, flow process relative complex, unfavorable operation or the like deficiency.For being the aluminum oxide industry of main raw material with the low-grade diasporite type at present, develop the new process of production that flow process is simple, energy consumption is lower, can effectively reduce cost, produce the aluminum oxide industry for China and can produce huge promoter action.
Summary of the invention
The object of the present invention is to provide a kind of improvement Bayer process processing low-grade diaspore type bauxite production method of alumina, successful solution an above-mentioned difficult problem.
Improvement Bayer process processing low-grade diaspore type bauxite production method of alumina provided by the invention may further comprise the steps:
1) chemistry desiliconization in advance: the low-grade diasporite type bauxite immersion of granularity less than 0.098mm contained in the sodium aluminate solution of stablizer; Contact; Make the active silica dissolving in the diaspore type bauxite and be stabilized in the slurries, obtain being dissolved with the slurries of silicon-dioxide;
2) desiliconization of high sodium aluminosilicate solution: the slurries of gained filtration step 1); Obtain the sodium aluminate solution and the high aluminium silicon ratio concentrate of high silicon content; Desiliconization is carried out in sodium aluminate solution dilution and adding desiliconization crystal seed; Obtain sodium aluminate solution, washing high aluminium silicon ratio concentrate, washing water are used as the diluent of high sodium silicoaluminate;
The sodium aluminate solution of the desiliconization that 3) the kind branch of sodium aluminate solution: with step 2) obtains adds aluminium hydroxide crystal seed and carries out the seed decomposition; Obtain white lake coarse-grain and seed precipitation solution after the separation; Sufficient crystallising white lake is through washing, behind recovery incidental aluminum oxide of white lake and the sodium oxide; Obtain the white lake finished product, washings turns back to seed precipitation solution;
4) Aluminium hydroxide roasting: the white lake finished product roasting that step 3) is obtained obtains alumina product;
5) high pressure stripping: the seed precipitation solution that step 3) is obtained is used for step 2 through evaporation, after mending alkali) the high pressure stripping of gained concentrate; Obtain sodium aluminate solution and red mud after the dissolution fluid filtering separation; Said sodium aluminate solution is used to handle next batch bauxite after adding stablizer; Repeating step 1)～4), said red mud gets into red mud dump after washing, and washing lotion turns back to step 2) be used for the dilution of high sodium silicoaluminate.
According to improvement Bayer process processing low-grade diaspore type bauxite production method of alumina of the present invention; Said low-grade diasporite type bauxite is 70～130 ℃ with the temperature that contacts of the sodium aluminate solution that contains stablizer; Be preferably 80～105 ℃; Be 2～10h duration of contact, is preferably 4～8h.
According to improvement Bayer process processing low-grade diaspore type bauxite production method of alumina of the present invention; Stablizer in the described step 1) is a kind of in potassium hydrogenphosphate, ATMP, ethylene diamine tetra methylene phosphonic acid sodium, the PAPE, and concentration is not higher than 0.1g/L; The add-on of bauxite is 100～400g/L, is preferably 200～300g/L, and concentration sodium hydroxide in the sodium aluminate solution (in NaOH) is 200g/L～500g/L, preferably is higher than 300g/L, and alumina concentration is (with Al
2O
3Meter) is 200g/L～400g/L, preferably is higher than 250g/L; After desiliconization was handled in advance through chemistry, dissolving and stable silica volume were 6-25g/L, be preferably to be higher than 8g/L, and the aluminum oxide that from raw material, digests were lower than 20%, preferably is lower than 8%.
According to improvement Bayer process processing low-grade diaspore type bauxite production method of alumina of the present invention, described step 2) in desiliconization be with the dilution filtrating at 150～170 ℃ of following desiliconization 4～10h, crystal seed is red mud or sodium white residue or kaolinite; Or at 90～120 ℃ of following red mud or sodium white residue or kaolinite desiliconization 4～8h of adding; The quicklime, terra alba, calcium aluminate, the carbon calcium aluminate that add 5～20g/L under this temperature, a kind of 0.5～4h of desiliconization again in the preferably water talcum (like Friedel salt and Kuzel salt); The alumina silica ratio of the high aluminium silicon ratio concentrate that obtains through desiliconization is 7～20, is preferably more than 9.
According to improvement Bayer process processing low-grade diaspore type bauxite production method of alumina of the present invention; The seed decomposition condition is for decomposing 60～75 ℃ of initial temperature in the described step 3); Decompose warm 40～50 ℃ eventually, the resolving time is 40～70h, more than the preferred 50h; Seed load is 50～300g/L, is preferably more than the 150g/L.
According to improvement Bayer process processing low-grade diaspore type bauxite production method of alumina of the present invention, roasting is at 1000～1200 ℃ of following roasting 30s～30min in the described step 4), is preferably more than the 10min.
According to improvement Bayer process processing low-grade diaspore type bauxite production method of alumina of the present invention; The temperature of the high pressure stripping workshop section in the described step 5) is 220～280 ℃, is preferably 260～280 ℃, pressure 3～6MPa; Dissolution time 30～120min; Be preferably more than the 45min, the concentrate addition is 200-400g/L, is preferably more than the 250-300g/L.
The present invention is different with prior art, and in the prior art, bauxite contacted the short time with leaching liquid after, desiliconization product (DSP) precipitated very soon, and silicon-dioxide stable very poor in solution do not have the competent time to carry out solid/liquid separation.Technology of the present invention is that low-grade bauxite is contacted with the high-concentration sodium aluminate solution that contains stablizer, can make in the low-grade bauxite most active silica get in the slurries and reaches high density, is typically 10g/L.In addition, method of the present invention can make dissolved silicon-dioxide in slurries, can stablize for some time, for example more than 2 hours, avoids the deposition absorption of DSP on bauxite surface simultaneously.Making like this has the time enough dissolve silica and from ore pulp, isolates the sodium aluminate solution of high-content silicon-dioxide and the concentrate of high aluminium silicon ratio (A/S).
In silicon-dioxide dissolving, minimizing of alumina dissolution is that sodium aluminate solution by high alumina content and low stabiliser content causes.In the process of lytic activity silicon-dioxide; Use contains high-alumina or near the saturated sodium aluminate solution of aluminum oxide; This solution is under the leaching temperature that the present invention proposes; Limited the ability of its dissolved oxygen aluminium, guaranteed the stripping from bauxite of the least possible aluminum oxide thus, improved the purpose of bauxite aluminium-silicon than (A/S) thereby reach.
In traditional Bayer process technology, the solution after the high pressure stripping enters into crystallization workshop section after the dilution desiliconization, and the mother liquor after the crystallization is used to handle next batch bauxite behind evaporative fill alkali, thereby realizes the circulation of Bayer process.And the present invention is sent to crystallization workshop section with the high sodium aluminosilicate solution after the preparatory desiliconization of chemistry after the dilution desiliconization; Mother liquor after the crystallization is the gained concentrate after being used for handling the preparatory desiliconization of chemistry behind the evaporative fill alkali; The high pressure dissolution fluid enters in advance desiliconization workshop section of chemistry, is used for handling next batch bauxite, and the purpose of doing like this is that the leach liquor with high aluminium content is used for chemistry desiliconization in advance; Satisfy the condition of chemical preparatory desiliconization, also realized haveing suffered simultaneously the circulation of flow process.
The key of the inventive method is chemistry desiliconization workshop section in advance; Use the sodium aluminate solution of the high density that contains the few stable agent in the desiliconization process; This sodium aluminate solution fluid power that contains the high density of few stable agent makes active silica (being mainly derived from the kaolinite in the bauxite) dissolving fast in the low-grade bauxite; Dissolved silicon-dioxide can be kept stable in slurries for a long time and have time enough to carry out solid/liquid separation; Avoid the deposition of the preceding DSP of solid/liquid separation, thereby obtain the bauxite concentrate of high aluminium silicon ratio (A/S).
Through using the high-concentration sodium aluminate solution that contains stablizer among the present invention to the desiliconization in advance of bauxite contact carrying out chemistry; Can make the stable existence of dissolved silicon-dioxide; Do not separate out on the aluminous surface; After adding the desiliconization crystal seed, can remove by successful most of silicon-dioxide, and obtain the high concentrate of alumina silica ratio, realized the application in the Bayer process low-grade bauxite in the low-grade bauxite; Use the gained concentrate after being used for handling the preparatory desiliconization of chemistry behind the evaporative fill alkali of the mother liquor after the crystallization among the present invention in addition, the sodium aluminate solution of high pressure stripping turns back to chemistry desiliconization workshop section in advance, carries out the processing of next batch aluminium ore, has realized haveing suffered the circulation of flow process.
Compare with art methods, the technical characterstic of the inventive method is embodied in the following aspects:
1) the inventive method adopts high-concentration sodium aluminate solution can make the most of active silica in the low-grade bauxite get into solution, and being removed of 50～85% silicon-dioxide arranged in the low-grade bauxite.
2) the inventive method is through adding a spot of stablizer in sodium hydroxide solution or sodium aluminate solution; Strengthened the stability of silicon-dioxide in slurries; Avoid dissolved silicon-dioxide to change desiliconization product (DSP) into and get into solid phase again, the solution (6～12SiO of high silicon dioxide content
2G/L) can stablize the sufficiently long time, for example more than 2 hours, thereby guarantee the solid/liquid separation of ore pulp.
3) the inventive method can change higher-grade concentrate (A/S>=9) into low-grade diasporite type bauxite (A/S≤5), thereby realizes the comprehensive utilization of China's low-grade bauxite.
4) the present invention can reduce alkaline consumption, reduces the silicon fouling, improves reactor drum, particularly autoclave efficient.
5) compare with existing sintering process, the present invention can significantly cut down the consumption of energy, and improves the quality of the finished product aluminum oxide.
6) the present invention can also accurately control the desiliconization of high sodium aluminosilicate solution, and obtain feed and form consistent pure siliceous product, and can be to its further processing, in order to reclaim caustic soda or to be used for other purpose or sale.
Description of drawings
Fig. 1 is an improvement bayer process schema of the present invention.
Embodiment
Embodiment 1
With certain low-grade diasporite type bauxite (place of production Jin Jiang River; Composition is seen table 1) grind to sieve and obtain breeze; Wherein granularity accounts for 80% less than the breeze of 0.074mm in the breeze; In the silicon-dioxide dissolution vessel, add the breeze 100g that obtains after grinding is sieved, the sodium aluminate solution that makes low-grade diasporite type bauxite and contain stablizer is (by NaOH and Al (OH)
3Adding water preparation and obtain sodium aluminate solution) 500ml mixes, and wherein, the stabilizer concentration that contains in the sodium aluminate solution of stablizer (potassium hydrogenphosphate) is 0.1g/L, and NaOH concentration is 400g/L, Al
2O
3Concentration is 300g/L; Leaching temperature is 130 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 6～8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 65wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
Table 1: the wt% of unit
| Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
| 60.5 | 11.9 | 6.3 | 2.8 | - | 5.1 |
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 9.9, and dioxide-containing silica is 10.12g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add CaO 20g in 160 ℃ of following desiliconizations solid-liquid separation after 3 hours, the siliceous modulus in the filtrating reaches 264.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 60 ℃ of decomposition temperatures, resolving time 60h carries out seed and decomposes under the seed load 300g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 43.8%.Aluminum hydroxide crystals is through washing, and drying is calcined 10min down at 1050 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 21.37g, gained concentrate 78g, CaO5g is at 260 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 375g/L through detecting NaOH concentration, Al
2O
3Concentration is 304g/L, SiO
20.84g/L the content 12mg/L of iron, the solubility rate of aluminium are 89.3%.
Get above-mentioned high pressure dissolution fluid 500ml and mix, and add stablizer ATMP 0.05g with the Jin Jiang River bauxite that ground; Leaching temperature is 130 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 6～8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 70wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 11.88, and dioxide-containing silica is 13.05g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add Friedel salt (3CaOAl
2O
3CaCl
210H
2O) 20g is in 120 ℃ of following desiliconizations solid-liquid separation after 3 hours, and the siliceous modulus in the filtrating reaches 228.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 60 ℃ of decomposition temperatures, resolving time 45h carries out seed and decomposes under the seed load 300g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 42.8.%.Aluminum hydroxide crystals is through washing, and drying is calcined 20min down at 1050 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 25.82g, gained concentrate 78g, CaO 5g is at 260 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 342g/L through detecting NaOH concentration, Al
2O
3Concentration is 318g/L, SiO
20.88g/L the content 23mg/L of iron, the solubility rate of aluminium are 90.4%.
Embodiment 2
Certain low-grade diasporite type bauxite (is derived from Cayman, Sanmenxia Gorge Aluminum; Composition is seen table 2) grind to sieve and obtain breeze; Wherein granularity accounts for 80% less than the breeze of 0.074mm in the breeze; In the silicon-dioxide dissolution vessel, add the breeze 100g that obtains after grinding is sieved, the sodium aluminate solution that makes low-grade diasporite type bauxite and contain stablizer is (by NaOH and Al (OH)
3Adding water preparation and obtain sodium aluminate solution) 500ml mixes, and wherein, the stabilizer concentration that contains in the sodium aluminate solution of stablizer (ATMP) is 0.1g/L, and NaOH concentration is 400g/L, Al
2O
3Concentration is 300g/L; Leaching temperature is 90 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 6～8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 72wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
Table 2: the wt% of unit
| Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
| 62.3 | 11.47 | 6.29 | 2.8 | - | 5.43 |
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 11.56, and dioxide-containing silica is 12.12g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add CaO 20g in 160 ℃ of following desiliconizations solid-liquid separation after 3 hours, the siliceous modulus in the filtrating reaches 285.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 60 ℃ of decomposition temperatures, resolving time 45h carries out seed and decomposes under the seed load 400g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 46.5%.Aluminum hydroxide crystals is through washing, and drying is calcined 20min down at 1050 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 18.75g, gained concentrate 78g, CaO 5g is at 260 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 382g/L through detecting NaOH concentration, Al
2O
3Concentration is 315g/L, SiO
20.92g/L the content 18mg/L of iron, the solubility rate of aluminium are 91.2%.
Get above-mentioned high pressure dissolution fluid 500ml and mix, and add stablizer ATMP 0.05g with the Cayman bauxite that ground; Leaching temperature is 90 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 6～8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 78wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 12.03, and dioxide-containing silica is 12.78g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add Friedel salt (3CaOAl
2O
3CaCl
210H
2O) 20g is in 120 ℃ of following desiliconizations solid-liquid separation after 3 hours, and the siliceous modulus in the filtrating reaches 245.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 60 ℃ of decomposition temperatures, resolving time 45h carries out seed and decomposes under the seed load 350g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 44.5%.Aluminum hydroxide crystals is through washing, and drying is calcined 20min down at 1050 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 22.75g, gained concentrate 78g, CaO 5g is at 260 ℃ of following stirring reaction 2.5h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 375g/L through detecting NaOH concentration, Al
2O
3Concentration is 321g/L, SiO
20.88g/L the content 21mg/L of iron, the solubility rate of aluminium are 92.4%.
Embodiment 3
Somewhere, Guizhou low-grade diasporite type bauxite (composition is seen table 3) ground to sieve obtain breeze; Wherein granularity accounts for 80% less than the breeze of 0.074mm in the breeze; In the silicon-dioxide dissolution vessel, add the breeze 100g that obtains after grinding is sieved, the sodium aluminate solution that makes low-grade diasporite type bauxite and contain stablizer is (by NaOH and Al (OH)
3Adding water preparation and obtain sodium aluminate solution) 500ml mixes, and wherein, the stabilizer concentration that contains in the sodium aluminate solution of stablizer (ethylene diamine tetra methylene phosphonic acid sodium) is 0.1g/L, and NaOH concentration is 400g/L, Al
2O
3Concentration is 300g/L; Leaching temperature is 90 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 6～8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 78wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
Table 3: the wt% of unit
| Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
| 62.65 | 13 | 2.58 | 2.95 | - | 4.82 |
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 10.38, and dioxide-containing silica is 10.24g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add calcium aluminate 20g in 160 ℃ of following desiliconizations solid-liquid separation after 3 hours, the siliceous modulus in the filtrating reaches 235.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 65 ℃ of decomposition temperatures, resolving time 45h carries out seed and decomposes under the seed load 300g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 44.68%.Aluminum hydroxide crystals is through washing, and drying is calcined 30min down at 1000 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 24.5g, gained concentrate 90g, CaO 5g is at 240 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 362g/L through detecting NaOH concentration, Al
2O
3Concentration is 298g/L, SiO
21.14g/L the content 17mg/L of iron, the solubility rate of aluminium are 88.5%.
Get above-mentioned high pressure dissolution fluid 500ml and mix, and add stablizer ethylene diamine tetra methylene phosphonic acid sodium 0.05g with the Guizhou bauxite that ground; Leaching temperature is 90 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 82wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 11.58, and dioxide-containing silica is 12.15g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add calcium aluminate 20g in 170 ℃ of following desiliconizations solid-liquid separation after 3 hours, the siliceous modulus in the filtrating reaches 245.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 60 ℃ of decomposition temperatures, resolving time 45h carries out seed and decomposes under the seed load 320g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 45.2%.Aluminum hydroxide crystals is through washing, and drying is calcined 20min down at 1050 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 24.82g, gained concentrate 78g, CaO 5g is at 280 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 372g/L through detecting NaOH concentration, Al
2O
3Concentration is 338g/L, SiO
20.74g/L the content 18mg/L of iron, the solubility rate of aluminium are 93.1%.
Embodiment 4
Yangquan, Shanxi low-grade diasporite type bauxite (composition is seen table 4) ground to sieve obtain breeze; Wherein granularity accounts for 80% less than the breeze of 0.074mm in the breeze; In the silicon-dioxide dissolution vessel, add the breeze 100g that obtains after grinding is sieved, the sodium aluminate solution that makes low-grade diasporite type bauxite and contain stablizer is (by NaOH and Al (OH)
3Adding water preparation and obtain sodium aluminate solution) 500ml mixes, and wherein, the stabilizer concentration that contains in the sodium aluminate solution of stablizer (PAPE) is 0.1g/L, and NaOH concentration is 400g/L, Al
2O
3Concentration is 300g/L; Leaching temperature is 100 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 6～8 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 68wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
Table 4: the wt% of unit
| Al 2O 3 | SiO 2 | Fe 2O 3 | TiO 2 | H 2O | A/S |
| 60.34 | 17.16 | 5.61 | 2.15 | - | 3.5 |
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 9.12, and dioxide-containing silica is 10.04g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add CaO 20g in 170 ℃ of following desiliconizations solid-liquid separation after 3 hours, the siliceous modulus in the filtrating reaches 218.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 65 ℃ of decomposition temperatures, resolving time 50h carries out seed and decomposes under the seed load 300g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 47.68%.Aluminum hydroxide crystals is through washing, and drying is calcined 10min down at 1100 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 27.5g, gained concentrate 90g, CaO 5g is at 250 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 382g/L through detecting NaOH concentration, Al
2O
3Concentration is 302g/L, SiO
21.02g/L the content 21mg/L of iron, the solubility rate of aluminium are 91.2%.
Get above-mentioned high pressure dissolution fluid 500ml and mix, and add stablizer PAPE 0.05g with Yangquan, the Shanxi bauxite that ground; Leaching temperature is 100 ℃.In the silicon-dioxide dissolution vessel; Sodium aluminate solution soaked diaspore type bauxite 7 hours; Sodium aluminate solution is with the dissolving of the silicon-dioxide of the 65wt% in the diaspore type bauxite and be stabilized in the slurries; And do not have tangible sodium aluminum silicate (DSP) deposition to be adsorbed on raw material diaspore type bauxite surface, obtain being dissolved with the slurries of silicon-dioxide.
The slurries that are dissolved with silicon-dioxide that to from the silicon-dioxide dissolution vessel, discharge feed in the solid/liquid separator, obtain solid concentrate alumina silica ratio (A/S) after the separation and reach 9.95, and dioxide-containing silica is 10.72g/L in the gained filtrating.Get filtrating 375ml, add water 225ml, add calcium aluminate 20g in 160 ℃ of following desiliconizations solid-liquid separation after 3 hours, the siliceous modulus in the filtrating reaches 224.
The sodium aluminate solution 500ml that gets after the desiliconization adds aluminium hydroxide crystal seed, and 60 ℃ of decomposition temperatures, resolving time 45h carries out seed and decomposes under the seed load 350g/L, obtain the aluminum hydroxide crystals and the about 450ml of seed precipitation solution of white, rate of decomposition 46.8%.Aluminum hydroxide crystals is through washing, and drying is calcined 30min down at 1050 ℃ and obtained alumina product.
The seed precipitation solution of gained is evaporated to 300ml is placed in the autoclave, add NaOH 28.16g, gained concentrate 78g, CaO 5g is at 260 ℃ of following stirring reaction 2h after-filtration.Filter residue discards, filtrates to be sodium aluminate solution, and be 366g/L through detecting NaOH concentration, Al
2O
3Concentration is 313g/L, SiO
20.94g/L the content 23mg/L of iron, the solubility rate of aluminium are 90.8%.
Claims (12)
1. one kind is improved Bayer process processing low-grade diaspore type bauxite production method of alumina, it is characterized in that this method may further comprise the steps:
1) chemistry desiliconization in advance: the low-grade diasporite type bauxite immersion of granularity less than 0.098mm contained in the sodium aluminate solution of stablizer; Contact; Make the active silica dissolving in the diaspore type bauxite and be stabilized in the slurries, obtain being dissolved with the slurries of silicon-dioxide;
2) desiliconization of high sodium aluminosilicate solution: the slurries of gained filtration step 1); Obtain the sodium aluminate solution and the high aluminium silicon ratio concentrate of high silicon content; Desiliconization is carried out in sodium aluminate solution dilution and adding desiliconization crystal seed; Obtain sodium aluminate solution, washing high aluminium silicon ratio concentrate, washing water are used as the diluent of high sodium silicoaluminate;
The sodium aluminate solution of the desiliconization that 3) the kind branch of sodium aluminate solution: with step 2) obtains adds aluminium hydroxide crystal seed and carries out the seed decomposition; Obtain white lake coarse-grain and seed precipitation solution after the separation; Sufficient crystallising white lake is through washing, behind recovery incidental aluminum oxide of white lake and the sodium oxide; Obtain the white lake finished product, washings turns back to seed precipitation solution;
4) Aluminium hydroxide roasting: the white lake finished product roasting that step 3) is obtained obtains alumina product;
5) high pressure stripping: the seed precipitation solution that step 3) is obtained is used for step 2 through evaporation, after mending alkali) the high pressure stripping of gained concentrate; Obtain sodium aluminate solution and red mud after the dissolution fluid filtering separation; Said sodium aluminate solution is used to handle next batch bauxite after adding stablizer; Repeating step 1)～4), said red mud gets into red mud dump after washing, and washing lotion turns back to step 2) be used for the dilution of high sodium silicoaluminate.
2. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1; It is characterized in that; Low-grade diasporite type bauxite is 70～130 ℃ with the temperature that contacts of the sodium aluminate solution that contains stablizer in the described step 1), and be 2～10h duration of contact.
3. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 2; It is characterized in that; Low-grade diasporite type bauxite is 80～105 ℃ with the temperature that contacts of the sodium aluminate solution that contains stablizer in the described step 1), and be 4～8h duration of contact.
4. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1; It is characterized in that; Stablizer in the described step 1) is a kind of in potassium hydrogenphosphate, ATMP, ethylene diamine tetra methylene phosphonic acid sodium, the PAPE, and concentration is less than or equal to 0.1g/L.
5. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1; It is characterized in that; The add-on of bauxite is 100～400g/L in the described step 1); Concentration sodium hydroxide is 200g/L～500g/L in the sodium aluminate solution, and alumina concentration is 200g/L～400g/L.
6. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 5; It is characterized in that; The add-on of bauxite is 200～300g/L in the described step 1); Concentration sodium hydroxide is greater than 300g/L in the sodium aluminate solution, and alumina concentration is greater than 250g/L.
7. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1; It is characterized in that; Described step 2) desiliconization in be with the dilution filtrating at 150～170 ℃ of following desiliconization 4～10h, crystal seed is red mud or sodium white residue or kaolinite; Or add down red muds or sodium white residue or kaolinite desiliconization 4～8h at 90～120 ℃, add a kind of 0.5～4h of desiliconization again in quicklime, terra alba, calcium aluminate, carbon calcium aluminate or the hydrotalcite of 5～20g/L under this temperature.
8. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1; It is characterized in that; The seed decomposition condition is for decomposing 60～75 ℃ of initial temperature in the described step 3); Decompose warm 40～50 ℃ eventually, the resolving time is 40～70h, and seed load is 50～300g/L.
9. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 8 is characterized in that the seed decomposition condition is greater than 50h in the described step 3), and seed load is greater than 150g/L.
10. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1 is characterized in that roasting is at 1000～1200 ℃ of following roasting 30s～30min in the described step 4).
11. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 1; It is characterized in that; The temperature of described step 5) mesohigh stripping workshop section is 220～280 ℃; Pressure 3～6MPa, dissolution time 30～120min, concentrate addition are 200-400g/L.
12. improvement Bayer process processing low-grade diaspore type bauxite production method of alumina according to claim 11; It is characterized in that; The temperature of described step 5) mesohigh stripping workshop section is 260～280 ℃; Pressure 5～6MPa, dissolution time are greater than 45min, and the concentrate addition is 250-300g/L.
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