CN1054955A - Produce the method and the device of aluminium chlorohydroxide from aluminous ore - Google Patents
Produce the method and the device of aluminium chlorohydroxide from aluminous ore Download PDFInfo
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- CN1054955A CN1054955A CN 90101321 CN90101321A CN1054955A CN 1054955 A CN1054955 A CN 1054955A CN 90101321 CN90101321 CN 90101321 CN 90101321 A CN90101321 A CN 90101321A CN 1054955 A CN1054955 A CN 1054955A
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- spray pyrolysis
- pyrolysis polymerization
- breeze
- separator
- aluminium chlorohydroxide
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Abstract
The present invention relates to a kind of method and device of producing aluminium chlorohydroxide from aluminous ore.This method is processed into roasting behind the breeze with aluminous ore, add the aluminum oxide in the direct acidleach stripping of the low-concentration hcl aluminous ore again, the semi-finished product solution employing spray pyrolysis polymerization drying installation of acidleach leachable after separating utilizes superheated vapour, and directly also carrying out spray pyrolysis polymerization and drying simultaneously makes finished product.It is simple that the present invention has technology, and facility investment is few, and cost is low, need not add advantages such as any additives, good product quality.
Description
The present invention relates to the preparation method of aluminum compound, particularly a kind of method and device of producing aluminium chlorohydroxide from aluminous ore with acid system.
Aluminium chlorohydroxide is that polymerize aluminum chloride is a kind of efficient inorganic polymeric flocculant, and its chemical general formula is [Al
2(OH)
nCl
6-n]
m, 1≤n≤5 wherein, m≤10.Aluminium chlorohydroxide generally all adopts traditional production method in the past, promptly with aluminum oxide (Al
2O
3) be the solid alumina pyrolysis method and the neutralisation of raw material, there is following shortcoming in these methods: 1, complex process; 2, the crystallization aluminum chloride that makes of the technology of pyrolysis method by complexity adopts fluidizing furnace to carry out thermolysis, and this facility investment is big, anticorrosion difficult solution, and heat utilization efficiency is lower; 3, neutralisation production acid and alkali consumption amount is big, and the product alumina content reduces, and impurity is many, poor product quality; 4, the neutralisation drying machine adopts steam-heated cal(l)andria, and heat utilization efficiency is low, the product cost height.Also having with industrial residue aluminium ash in addition is " acid-soluble one-step " of raw material, this method because of be subjected to aluminium ash raw materials cost height, few restriction of originating fails to form scale operation.Because the above-mentioned several method production of general at present employing causes the aluminous ore resource of China's abundant to be used on chemical industry seldom.Though the report of producing aluminium chlorohydroxide from aluminum ore is also arranged recently, but not only need operations such as being processed into breeze, roasting, pressurized acid leaching stripping, filtration, pyrolysis polymerization in this kind production technique, and breeze needs activated calcining back to be mixed in proportion to prepare burden with sulfuric acid, fluoride additive to carry out roasting, and to carry out roasting reaction and the stripping of acidleach for several times reaction through repeatedly such batching, again the alumina crystal after heat of stripping is depolymerized and make aluminium chlorohydroxide, thereby complex process, long flow path, pyrolysis rate is slow.
The object of the present invention is to provide a kind of weak point that can overcome above-mentioned preparation method, make full use of the preparation method and the device of the aluminium chlorohydroxide of the abundant aluminous ore resource of China's reserves.
Purpose of the present invention can reach by following measure:
A kind of method of producing aluminium chlorohydroxide from aluminous ore, the aluminous ore raw material is processed into breeze, under the heating and pressurizing condition, directly use hydrochloric acid acidleach stripping aluminum oxide behind the breeze calcination activation, carry out solid-liquid separation again, adopt spray pyrolysis polymerization drying installation to be beneficial to superheated vapo(u)r at last and directly the aluminium chlorohydroxide semi-finished product solution of the low basicity of solid-liquid separation gained is carried out spray pyrolysis polymerization and drying simultaneously and make aluminium chlorohydroxide.
Indication aluminous ore of the present invention can be kaolinite, boehmite, coal gangue, clay pit, gibbsite etc.
A kind of spray pyrolysis polymerization drying installation that is used for producing from aluminous ore aluminium chlorohydroxide is by spray pyrolysis polymerization drying tower, liquid material feed device, opening-closing valve, be communicated with spray pyrolysis polymerization drying tower and provide the dry heat energy of spray pyrolysis polymerization heating plant and on thermometer hole, be communicated with heating plant and feed device and an end puts in superheated vapo(u)r pipeline in the spray pyrolysis polymerization drying tower, be installed in the blanking groove in the spray pyrolysis polymerization drying tower bottom, the finished product exhaust-steam separator, waste gas recovering device, airduct, playing the major portions such as induced draft fan of negative pressure draft effect forms.The part that the superheated vapo(u)r pipeline puts in the spray pyrolysis polymerization drying tower has shower nozzle, being positioned at place, shower nozzle top position in the spray pyrolysis polymerization drying tower has one can make warm air be evenly distributed on the dispersion plate of tower, all be communicated with between blanking groove and the finished product exhaust-steam separator and between finished product exhaust-steam separator and the waste gas recovering device by airduct, airduct is communicated with the appropriate location uncovered suitable for reading that end is positioned at blanking groove with blanking groove, induced draft fan is installed near on the airduct of waste gas recovering device, the discharge port of finished product exhaust-steam separator and blanking groove all is equipped with star-like discharge valve, and this kind valve can play and only allow discharging and do not cause effect in air admission separator and the blanking groove.
Purpose of the present invention can also reach by following measure:
Being processed into the breeze operation can make aluminous ore and hydrochloric acid that contact area preferably be arranged when carrying out solid-liquid phase reaction earlier with the breeze of aluminous ore through the certain particle diameter of break process one-tenth in small, broken bits again.The processing granularity has considerable influence to the solubility rate of aluminum oxide and the separating effect of reaction residues.The breeze particle diameter is more little, and aluminum oxide acidleach solubility rate is high more, but reaction residues is difficult more when separating.Breeze processing granularity of the present invention is generally the 40-80 order.
Calcination activation decomposites the Al of reactive behavior is preferably arranged in acid under the maturing temperature that the breeze after the above processing is suiting
2O
3, maturing temperature with aluminum oxide maturing temperature 600-850 ℃ of the highest solubility rate be good.Roasting time also is one of important factor that influences digesting efficiency of alumina, and roasting time can be 0.5-1 hour.
Add the aluminum oxide in the acidleach stripping breeze behind calcination activation again, its principal reaction is:
Especially hydrochloric acid acidleach under the condition of heating and pressurizing, because the prolongation of time, under the excessive situation of aluminum oxide, reaction continues to move to the stripping direction, and (the Al(H that generates
2O)
6) Cl
3Monomer develops the aluminium chlorohydroxide semi-finished product solution that makes low basicity gradually.
Acidleach stripping reaction is with one of important procedure of aluminous ore raw material production aluminium chlorohydroxide.Outside the Pass the factor that influences digesting efficiency of alumina was removed and to be had with mineral type, particle diameter, roasting condition, major influence factors also had concentration and consumption, the acidleach stripping treatment time etc. of used hydrochloric acid, below division as follows:
1, uses acid concentration.During acidleach stripping reaction, preferably select low-concentration hcl for use, because digesting efficiency of alumina increases and increases with concentration of hydrochloric acid, if but concentration of hydrochloric acid is too high, the hydrochloric acid volatile quantity increases greatly, and operating environment, yield are all had disadvantageous effect, but concentration of hydrochloric acid is too low, digesting efficiency of alumina reduces on the one hand, and the also corresponding reduction of concentration of aluminum chloride on the other hand makes the alumina content in the product not reach target level of product quality.Consider solubility rate and hydrochloric acid volatilization factor, at 110-150 ℃ and 0.7-5Kg/cm
2The heating and pressurizing condition under, concentration of hydrochloric acid selects for use the lower concentration of 15-20% to be advisable.
2, add the acid amount.The acid amount of adding adds acid equivalent than being that the method that is added the ratio of aluminum oxide equivalents in hydrochloric acid equivalents and the breeze in the acidleach stripping is carried out with control.The solubility rate of aluminum oxide increases with the increase that adds the acid equivalent ratio, and the basicity of dissolution fluid then reduces with the increase that adds the acid equivalent ratio.In order to obtain the dissolution fluid of certain amount of alumina solubility rate and basicity content, should be controlled at 0.5-1.0 with adding the acid equivalent ratio.
3, the acidleach stripping reaction times.Digesting efficiency of alumina increases with the growth in acidleach stripping reaction times, but in 1.0 hours the time, and solubility rate is little with the amplitude that the growth in reaction times increases, and in order to improve plant factor, the reaction times selects for use and was advisable in 1-2 hour.
Acidleach stripping reaction solution after filtration with wash the aluminium chlorohydroxide work in-process filtrate of low basicity.Directly also carrying out spray pyrolysis polymerization and drying simultaneously makes the solid aluminium chlorohydroxide to adopt spray pyrolysis polymerization drying installation to utilize superheated vapo(u)r this filtrate.Because of spraying granule is fine, so under 280-300 ℃ of temperature, keep 2-3 can obtain the solid aluminium chlorohydroxide finished product of following index: Al second
2O
3Content 30-35%, basicity 60-80%, pH value 4.0-5.0, water-insoluble 0.5-3%, water-soluble good, outward appearance is good.
The application of aluminium chlorohydroxide except that giving the extensive employing of water treatment, is handled in various industrial sewage at present, has also obtained application in the processing as printing and dyeing water, petroleum wastewater, smelting wastewater, beneficiation wastewater.In addition, aluminium chlorohydroxide has also been opened up new application approach at aspects such as precision casting, papermaking, medicine, process hides, oil treatments.
The present invention compared with prior art has following advantage:
1, technology is simple, roasting and acidleach stripping do not need to carry out repeatedly repeatedly, and need not add sulfuric acid and any additives when carrying out the roasting reaction, do not need the alumina crystal with the acidleach stripping, but will directly adopt superheated vapo(u)r to carry out spray pyrolysis polymerization and drying treatment 2-3 second simultaneously through the low basicity aluminium chlorohydroxide solution after acidleach stripping and the filtration treatment under 280-300 ℃ of condition, speed of response is fast, thereby simplified technology, shortened technical process, labour intensity reduces, and production environment is good.
2, can make full use of abundant, the cheap and easy to get aluminous ore resources such as kaolinite of China's reserves.
3, low-concentration hcl is used in acidleach stripping reaction, can under the situation of the aluminium chlorohydroxide semi-finished product solution pH value lower (pH value about 3) that contains low basicity, produce qualified solid aluminium chlorohydroxide product, recycle but also can utilize the high by-product low-concentration hcl of the rate of recovery to return in the acidleach dissolving-out process, both reduced product cost, prolong the corrosion-resistant cycle of equipment, prevented atmospheric pollution again.
4, owing to adopt spray pyrolysis polymerization drying installation, make the spraying medium, replace pressurized air, can not want air compressor,, be applicable to that especially areas without electricity applies so can save electric energy with superheated vapo(u)r.Spray pyrolysis polymerization drying tower can adopt skeleton construction simultaneously, less investment, and thermal capacity is big, and the pyrolysis polyreaction is comparatively abundant, so the product production height, and quality is good.
The drawing of accompanying drawing is described as follows.
Fig. 1 is the process flow diagram of preparation method of the present invention.
Fig. 2 is a kind of concrete spray pyrolysis polymerization drying installation synoptic diagram that is used for preparation method of the present invention.
1 is spray pyrolysis polymerization drying tower among the figure; 2 is feed device; 3 is opening-closing valve; 4 is heating plant; 5 is the superheated vapo(u)r pipeline; 6 is blanking groove; 7 is the finished product exhaust-steam separator; 8 is waste gas recovering device; 9 is airduct; 10 is induced draft fan; 11 is back blowing machine; 12 is star-like discharge valve; 13 is dispersion plate; 14 is shower nozzle; 15 is thermometer hole; 16 is hand-hole; 17 is cyclonic separator.
The present invention is further detailed in conjunction with the accompanying drawings below.
Embodiment one.As depicted in figs. 1 and 2, employing contains Al
2O
354% kaolinite is a raw material, with jaw crusher block kaolinite ore is broken into the 20-40mm particle diameter earlier, adopts ball mill one-tenth in small, broken bits 40-50 purpose particulate breeze again.Breeze is 800 ℃ of roasting temperatures activation 0.5 hour, again in the hydrochloric acid equivalents: the ratio adding concentration of the equivalents of aluminum oxide in the kaolinite breeze=0.8: 1 is that 15.3% hydrochloric acid is at 120 ℃ of temperature and 1.0Kg/cm
2The breeze of acidleach stripping behind calcination activation is 1 hour under the heating and pressurizing condition of pressure, promptly get the aluminium chlorohydroxide semi-finished product solution that hangs down basicity (basicity is 20%), through filtration and washing after filtrate be that the liquid material is packed in the feed device 2, the superheated vapo(u)r that is provided by the heating plant 4 that feeds in the superheated vapo(u)r pipeline 5 becomes microgranular by shower nozzle 14 at spray pyrolysis polymerization drying tower 1 internal spraying, and under 280 ℃ of temperature, carry out pyrolysis polymerization and dry 3 seconds by the warm air that heating plant 4 provides, promptly get Al
2O
3Content 30.14%, basicity 68.5%, pH value 4.2, water insoluble matter content 2%, the solid aluminium chlorohydroxide finished product that outward appearance is good.Shower nozzle 14 tops in the spray pyrolysis polymerization drying tower 1 have one can make warm air be evenly distributed on the interior dispersion plate 13 of tower.Bottom at tower, portioned product through suitable for reading be uncovered shape, the blanking groove 6 that star-like discharge valve 12 is equipped with in the bottom flows out, most of product is a cloth bag separator in this example of 10 times suction finished products of induced draft fan exhaust-steam separator 7(that plays the negative pressure draft effect then) in, finished product draws off below separator 7 after separating, useless HCl gas is introduced in the waste gas recovering device 8 by airduct 9, reclaims the circulation of gained hydrochloric acid and is used for acidleach stripping reaction.One thermometer hole 15 is arranged on the heating duct of feed device 4, on the pipeline of feed device 2 bottoms and the superheated vapo(u)r pipeline 5 opening-closing valve 3 is arranged.
This routine spray pyrolysis polymerization drying tower 1 is a skeleton construction, and the tower side has the manhole 16 that passes in and out operation for the people.
The back blowing machine 11 that can blow in cloth bag is installed on the airduct 9 that is communicated with cloth bag separator, can blows the finished product that sticks on the cloth bag and draw off off from the cloth bag separator bottom.On the airduct 9 that connects between blanking groove 6 and the finished product exhaust-steam separator 7, increase the cyclonic separator 17 that star-like discharge valve 12 is arranged at a bottom is installed,, thereby can alleviate the burden of cloth bag separator in cyclonic separator 17 so that the big product of particle draws off earlier.
Embodiment two.Employing bauxite is raw material, is processed into particle diameter 80 purpose breezes, and roasting is 1 hour under 650 ℃ of conditions, and in the hydrochloric acid equivalents: it is that 20% hydrochloric acid is at 150 ℃ and 4.0Kg/cm that the ratio of aluminum oxide equivalents in the bauxite=0.5: 1.0 adds concentration
2The heating and pressurizing condition under the breeze of acidleach stripping behind calcination activation must hang down the aluminium chlorohydroxide semi-finished product solution of basicity in 2 hours, after filtration with the dry solid aluminium chlorohydroxide finished product that promptly gets following composition 2.0 seconds of washing rear filtrate spray pyrolysis polymerization under 300 ℃ of temperature: Al
2O
3Content 34.7%, basicity 78%, pH value 4.5, water-insoluble 0.75%, spray pyrolysis polymerization drying installation structure and spray pyrolysis polymerization drying operation step are same as embodiment one.
Claims (5)
1, a kind ofly produce the method for aluminium chlorohydroxide from aluminous ore, aluminium chlorohydroxide is that the chemical general formula of polymerize aluminum chloride is [Al
2(OH)
nCl
6-n]
m, 1≤n≤5 wherein, breeze is processed into the aluminous ore raw material in m≤10, it is characterized in that will be behind the breeze calcination activation under the heating and pressurizing condition directly with hydrochloric acid acidleach stripping aluminum oxide (Al
2O
3), carry out solid-liquid separation again, adopt spray pyrolysis polymerization drying installation to utilize superheated vapo(u)r directly the aluminium chlorohydroxide semi-finished product solution of the low basicity of solid-liquid separation gained to be carried out spray pyrolysis polymerization and drying simultaneously at last and make aluminium chlorohydroxide.
2,, it is characterized in that with the aluminous ore raw material that through fragmentation one-tenth in small, broken bits again 40-80 purpose breeze breeze under 600-850 ℃ of temperature condition calcination activation 0.5-1 hour is then at 110-150 ℃ and 0.7-5Kg/cm according to the described preparation method of claim 1
2The heating and pressurizing condition under to add concentration be the breeze of hydrochloric acid acidleach behind calcination activation of 15-20%, the hydrochloric acid add-on is controlled at the ratio of aluminum oxide equivalents in hydrochloric acid equivalents and the breeze in the scope of 0.5-1.0, acidleach stripping reaction times 1-2 hour, the aluminium chlorohydroxide work in-process filtrate of the low basicity after the acidleach dissolution fluid separates after filtration (basicity 20-40%) adopted spray pyrolysis polymerization drying installation directly to utilize the superheated vapo(u)r dry 2-3 of spray pyrolysis polymerization second under 280-300 ℃ of temperature condition.
3, a kind of spray pyrolysis polymerization drying installation that is used for producing aluminium chlorohydroxide from aluminous ore, it is characterized in that by spray pyrolysis polymerization drying tower 1, liquid material feed device 2, opening-closing valve 3, be communicated with spray pyrolysis polymerization drying tower 1 and provide the dry heat energy of spray pyrolysis polymerization heating plant 4 and on thermometer hole 15, be communicated with heating plant 4 and feed device 2 and an end puts in superheated vapo(u)r pipeline 5 in the spray pyrolysis polymerization drying tower 1, be installed in the blanking groove 6 of spray pyrolysis polymerization drying tower 1 lower interior portion, finished product exhaust-steam separator 7, waste gas recovering device 8, airduct 9, playing the major portions such as induced draft fan 10 of negative pressure draft effect forms, the part that superheated vapo(u)r pipeline 5 puts in the spray pyrolysis polymerization drying tower 1 has shower nozzle 14, being positioned at place, shower nozzle 14 top positions in the spray pyrolysis polymerization drying tower 1 has one can make warm air be evenly distributed on the dispersion plate 13 of tower, all be communicated with between blanking groove 6 and the separator 7 and between separator 7 and the waste gas recovering device 8 by airduct 9, airduct 9 is communicated with the appropriate location uncovered suitable for reading that end is positioned at blanking groove 6 with blanking groove 6, induced draft fan 10 is installed near on the airduct 9 of waste gas recovering device 8, and the discharge port of separator 7 and blanking groove 6 all is equipped with star-like discharge valve 12.
4, device according to claim 3 is characterized in that spray pyrolysis polymerization drying tower 1 is skeleton construction, and the tower side has the hand-hole 16 for people's turnover.
5, according to claim 3 or 4 described devices, it is characterized in that being communicated with increasing on the airduct 9 of blanking groove 6 and finished product exhaust-steam separator 7 cyclonic separator 17 that a bottom has star-like discharge valve 12 is installed, finished product exhaust-steam separator 7 is a cloth bag separator, and the back blowing machine 11 that can blow in cloth bag is installed on the airduct 9 that is communicated with cloth bag separator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90101321 CN1054955A (en) | 1990-03-10 | 1990-03-10 | Produce the method and the device of aluminium chlorohydroxide from aluminous ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90101321 CN1054955A (en) | 1990-03-10 | 1990-03-10 | Produce the method and the device of aluminium chlorohydroxide from aluminous ore |
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|---|---|
| CN1054955A true CN1054955A (en) | 1991-10-02 |
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ID=4877024
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|---|---|---|---|
| CN 90101321 Pending CN1054955A (en) | 1990-03-10 | 1990-03-10 | Produce the method and the device of aluminium chlorohydroxide from aluminous ore |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923746A (en) * | 2012-11-23 | 2013-02-13 | 攀枝花钢城集团有限公司 | Method for preparing polyaluminium chloride (PAC) |
| CN103771344A (en) * | 2014-01-03 | 2014-05-07 | 东北大学 | Device for preparing metallic oxide by jetting and pyrolyzing metal chloride solution |
| CN104743588A (en) * | 2013-12-31 | 2015-07-01 | 重庆蓝洁广顺净水材料有限公司 | Environment-friendly and clean solid polyaluminium chloride production device |
| CN104743590A (en) * | 2013-12-31 | 2015-07-01 | 重庆蓝洁广顺净水材料有限公司 | Environment-friendly clean solid polyaluminium chloride reaction device |
| CN104944548A (en) * | 2015-06-08 | 2015-09-30 | 徐强富 | Polyhydroxy aluminium chloride water treatment agent and production method thereof |
-
1990
- 1990-03-10 CN CN 90101321 patent/CN1054955A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923746A (en) * | 2012-11-23 | 2013-02-13 | 攀枝花钢城集团有限公司 | Method for preparing polyaluminium chloride (PAC) |
| CN104743588A (en) * | 2013-12-31 | 2015-07-01 | 重庆蓝洁广顺净水材料有限公司 | Environment-friendly and clean solid polyaluminium chloride production device |
| CN104743590A (en) * | 2013-12-31 | 2015-07-01 | 重庆蓝洁广顺净水材料有限公司 | Environment-friendly clean solid polyaluminium chloride reaction device |
| CN104743588B (en) * | 2013-12-31 | 2017-10-20 | 重庆蓝洁广顺净水材料有限公司 | The solid polyaluminium chloride process units of environment-protecting clean |
| CN104743590B (en) * | 2013-12-31 | 2017-10-31 | 重庆蓝洁广顺净水材料有限公司 | The solid polyaluminium chloride reaction unit of environment-protecting clean |
| CN103771344A (en) * | 2014-01-03 | 2014-05-07 | 东北大学 | Device for preparing metallic oxide by jetting and pyrolyzing metal chloride solution |
| CN104944548A (en) * | 2015-06-08 | 2015-09-30 | 徐强富 | Polyhydroxy aluminium chloride water treatment agent and production method thereof |
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