CN105836865B - A kind of preparation process of aluminium polychloride - Google Patents
A kind of preparation process of aluminium polychloride Download PDFInfo
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- CN105836865B CN105836865B CN201610389486.1A CN201610389486A CN105836865B CN 105836865 B CN105836865 B CN 105836865B CN 201610389486 A CN201610389486 A CN 201610389486A CN 105836865 B CN105836865 B CN 105836865B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A kind of preparation process of aluminium polychloride, comprises the following steps：BB acid mother liquors, be added in enamel reactor by S1, and is slowly added to hydrogen peroxide in backward BB acid mother liquors, and is stirred continuously, and stops adding after no longer gas is produced；S2, the calcium powder for weighing certain mass are added in the BB acid mother liquors in S1；Suitable water is added in S3, the BB acid mother liquors into S2, controls the temperature of enamel reactor at 60 DEG C~70 DEG C, and keep 1h~2h；S4, after the completion for the treatment of S3 reactions, 100 DEG C~110 DEG C are increased to by the temperature that enamel reacts, and keep the temperature 2.5h~4h, obtain light yellow floccule；S5, carry out light yellow floccule press filtration, wash, blot again successively, finally obtains finished product.The preparation process can not only effectively improve the utilization rate of resource, and can also improve the purity of finished product, avoid the materials such as phthalic anhydride and benzene and be mixed into finished product, and secondary pollution is caused to handled water body, meanwhile the step of preparing aluminium polychloride is decreased, improve production efficiency.
Description
Technical field
The present invention relates to aluminum chloride flocculant production technical field, more particularly to a kind of preparation process of aluminium polychloride.
Background technology
Aluminium polychloride is a kind of water-purifying material, inorganic polymer coagulant, and is called poly-aluminium for short, and english abbreviation is
PAC, the molecular weight that is produced due to the polymerization of the bridging action and multivalent anions of hydroxide ion is larger, electric charge is higher
Inorganic polymer water treatment agent.Morphologically two kinds of solid and liquid can be divided into again.Solid is divided into again by color is different
Sepia, ecru, golden yellow and white, liquid can be rendered as water white transparency, is yellowish, light yellow to yellowish-brown.It is different
The aluminium polychloride of color also has larger difference in application and production technology.
Be used to prepare in the prior art the raw material of liquid aluminium polychloride mainly have aluminium skimmings, aluminium ash and aluminium slag, aluminium hydroxide,
Aluminium chloride and aluminum-containing mineral etc..In addition, in order to improve the utilization rate of resource and implement the theory of Green Chemistry, it is therefore, existing
There is partial oxidation aluminium manufacturing enterprise to be used as raw material with mother liquor remaining in BB acid production processes, its main reaction
Principle is：(Al3++SO4 2-+Cl-+H2+)+NH3·H2O→Al(OH)3↑+NH4 ++SO2 4-+Cl-；(1)Al(OH)3+HCl→Aln
(OH)mCl3n-m, (2) Al (OH)3+(Al3 ++SO2 4-+Cl-+H+)→[Al2(OH)NCl6-N]M·(SO4)x.Due to the reaction principle
Need to first pass through addition ammonium hydroxide to neutralize the acidity in mother liquor, and backward will be into a taking-up precipitate A l (OH)3Inside adds hydrochloric acid
Aluminium polychloride is made again after carrying out polymerization curing, so as to cause a large amount of wastes that hydrochloric acid uses, and environment can also be made
Into pollution, and due to also containing the organic substances such as phthalic anhydride, benzene in BB acid mother liquors, so the final purity to aluminium polychloride
It can affect.
The content of the invention
It is an object of the invention to provide a kind of material waste and high aluminium polychloride of alumina leaching amount of reducing
Preparation process.
The present invention above-mentioned purpose technical scheme is that：A kind of preparation work of aluminium polychloride
Skill, comprises the following steps：
BB acid mother liquors, be added in enamel reactor by S1, and is slowly added to hydrogen peroxide in backward BB acid mother liquors, and constantly
Stirring, stops adding after no longer gas is produced；
S2, the calcium powder for weighing certain mass are added in the BB acid mother liquors in S1；
Suitable water is added in S3, the BB acid mother liquors into S2, controls the temperature of enamel reactor at 60 DEG C~70 DEG C, and
Keep 1h~2h；
S4, after the completion for the treatment of S3 reactions, 100 DEG C~110 DEG C are increased to by the temperature that enamel reacts, and keep the temperature 2.5h~4h,
Obtain light yellow floccule；
S5, carry out light yellow floccule press filtration, wash, blot again successively, finally obtains finished product.
By the Organic Ingredients that left behind in BB acid mother liquors containing phthalic anhydride, benzene when being used to prepare BB acid, and generally
Water is insoluble in, last in reaction be difficult to be washed away with water, therefore, when producing polyaluminium by the use of BB acid mother liquors as raw material
When aluminium finished product, the surface of finished product will carry phthalic anhydride and benzene, so as to be purified by the use of the aluminium polychloride as flocculant
New noxious material will be brought into when water body in water body, so as to will result in the secondary pollution of water body.And hydrogen peroxide exists
There is very strong oxidisability under conditions of acidity, its can by phthalic anhydride with benzene oxidatoin into carbon dioxide, carbon monoxide and water so that
Be conducive to improve the purity of aluminium polychloride.
And hydrogen ion is originally contained in BB acid mother liquors Central Plains, therefore, there is no need to from extraneous individually addition acid to BB acid mother liquors
In, meanwhile, decrease the input amount that postorder is used for neutralizing alkaline material needed for BB acid mother liquors.
In addition, calcium powder, that is, calcium carbonate is put into BB acid mother liquors, primarily to making the aluminium ion and carbon in BB acid mother liquors
Polymeric and aging reactions generation aluminium polychloride occurs for sour calcium, is so precipitated compared to addition ammonium hydroxide, then recycles brine
For the operation cured, operating procedure is greatly reduced.Also, calcium carbonate also advantageously improves the alkali of aluminium polychloride
Degree, the polymer poly that such aluminium ion hydrolyzes to form is right higher, the charge neutrality ability and bonding bridge formation energy of its active ingredient
Power is stronger, so flocculating property is better.
Preferably, the mass fraction of the hydrogen peroxide in S1 is 20%~30%.
Preferably, the speed of the addition of hydrogen peroxide in S1 is 500mL/min~1000mL/min.
Hydrogen peroxide is added using high concentration, low speed, primarily to the number of hydrogen peroxide addition is reduced, and can also
Avoid hydrogen peroxide input amount excessive and caused by waste, so as to substantially increase dioxygen water use efficiency.
Preferably, during S1 adds hydrogen peroxide, the gas produced in enamel is outwards arranged using air exhausting device
Remove.
Since hydrogen peroxide is when the organic matter such as phthalic anhydride and benzene is aoxidized, it can produce carbon dioxide and carbon monoxide, and
Inherently a kind of poisonous gas of carbon monoxide, therefore by air exhausting device by the carbon dioxide in enamel reactor and an oxygen
Change carbon discharge, be on the one hand conducive to avoid the pressure in enamel reactor excessive and cause security risk, on the other hand can also
Carbon monoxide is avoided to pollute production environment so that toxic hazard occurs for staff.
Preferably, after the completion for the treatment of S1, the temperature of enamel is increased to 50 DEG C~60 DEG C, and keep 15min~30min.
Since the low hydrogen peroxide of concentration will decompose at normal temperatures, when the temperature of enamel is increased to 50 DEG C~60 DEG C
When, the decomposition rate of hydrogen peroxide will be accelerated, and in the range of the temperature, continue to keep the temperature 15min~30min, so that
Only have less than 5% hydrogen peroxide it is undecomposed complete, be so conducive to avoid hydrogen peroxide concentration excessive and ensuing operation made
Into influence.
Preferably, the mass ratio of the BB acid mother liquors and calcium powder in S2 is 1: 0.1~0.2.
Preferably, the mass ratio of the BB acid mother liquors and calcium powder in S2 is 1: 0.16.
When the mass ratio of calcium powder and BB acid mother liquors is more than 0.2, the basicity for the aluminium polychloride produced
Will be more than 90%.At this time, since basicity is excessive, the hydroxyl in polymer can be caused to tend to saturation, generates the hydrogen-oxygen of indissoluble
Compound micelle, product are difficult to be stabilized, while influence the flocculating property of product.And calcium powder and the mass ratio of BB acid mother liquors
Most suitable scope is 0.16.
Preferably, the water used in S3 is to wash the washings after light yellow floccule in S5.
Dosed in S3 using raw material is used as with the washings after the light yellow floccule of washing in S5, so not only improved
The utilization ratio of water resource, meanwhile, under being washed on light yellow floccule again can be with for the chlorion, the aluminium ion etc. that are utilized
It is re-used, and then substantially increases the utilization rate of each element in whole system, therefore, is close to this reason of Green Chemistry
Read.
In conclusion the invention has the advantages that：
1. with phthalic anhydride and benzene in hydrogen peroxide oxidation BB acid mother liquors, can so avoid phthalic anhydride and benzene is attached on product and
Secondary pollution is caused to the water body purified；
2. carrying out Polymeric and aging reactions production aluminium polychloride to BB mother liquors using calcium carbonate, behaviour is so greatly saved
The step of making, improves the efficiency of operation；
Reacted 3. being used as raw material using the washings for washing light yellow floccule and being added in enamel reactor, this
Sample substantially increases the utilization rate of water resource, calcium ion and chlorion etc., so as to more be close to the environmental protection reason of Green Chemistry
Read.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of aluminium polychloride.
Embodiment
The present invention is described in further detail below in conjunction with attached drawing 1.
Embodiment 1,
A kind of preparation process of aluminium polychloride, step 1：The BB acid mother liquors of 100kg are added in enamel reactor,
And mass fraction is slowly added to as 20% hydrogen peroxide using the speed of 500mL/min~1000mL/min in backward BB acid mother liquors,
And be stirred continuously, stop adding hydrogen peroxide after no longer gas is produced；Step 2：Enamel is warming up to 50 DEG C~60 DEG C, and is protected
Warm 15min~30min；Step 3：Weigh in the BB acid mother liquors that 10kg calcium powders are added in step 1, and add suitable washing
Water, meanwhile, the temperature of enamel reactor is controlled at 60 DEG C~70 DEG C, and keeps 1h~2h；Step 4：Treat that step 3 reaction is completed
Afterwards, the temperature that enamel reacts is increased to 100 DEG C, and keeps the temperature 2.5h, obtain light yellow floccule；Step 5：To light yellow wadding
Shape thing carries out press filtration, washs, blots again successively, final to obtain liquid aluminium polychloride finished product, the aluminium oxide obtained after detection
Content is 15.3%.
Embodiment two,
A kind of preparation process of aluminium polychloride, step 1：The BB acid mother liquors of 100kg are added in enamel reactor,
And mass fraction is slowly added to as 30% hydrogen peroxide using the speed of 500mL/min~1000mL/min in backward BB acid mother liquors,
And be stirred continuously, stop adding hydrogen peroxide after no longer gas is produced；Step 2：Enamel is warming up to 50 DEG C~60 DEG C, and is protected
Warm 15min~30min；Step 3：Weigh in the BB acid mother liquors that 20kg calcium powders are added in step 1, and add suitable washing
Water, meanwhile, the temperature of enamel reactor is controlled at 60 DEG C~70 DEG C, and keeps 1h~2h；Step 4：Treat that step 3 reaction is completed
Afterwards, the temperature that enamel reacts is increased to 110 DEG C, and keeps the temperature 4h, obtain light yellow floccule；Step 5：To light yellow cotton-shaped
Thing carries out press filtration, washs, blots again successively, final to obtain liquid aluminium polychloride finished product, and the aluminium oxide obtained after detection contains
Measure as 16.4%.
Embodiment three,
A kind of preparation process of aluminium polychloride, step 1：The BB acid mother liquors of 100kg are added in enamel reactor,
And mass fraction is slowly added to as 25% hydrogen peroxide using the speed of 500mL/min~1000mL/min in backward BB acid mother liquors,
And be stirred continuously, stop adding hydrogen peroxide after no longer gas is produced；Step 2：Enamel is warming up to 50 DEG C~60 DEG C, and is protected
Warm 15min~30min；Step 3：Weigh in the BB acid mother liquors that 16kg calcium powders are added in step 1, and add suitable washing
Water, meanwhile, the temperature of enamel reactor is controlled at 60 DEG C~70 DEG C, and keeps 1h~2h；Step 4：Treat that step 3 reaction is completed
Afterwards, the temperature that enamel reacts is increased to 105 DEG C, and keeps the temperature 3.2h, obtain light yellow floccule；Step 5：To light yellow wadding
Shape thing carries out press filtration, washs, blots again successively, final to obtain liquid aluminium polychloride finished product, the aluminium oxide obtained after detection
Content is 16.9%.
Example IV,
A kind of preparation process of aluminium polychloride, step 1：The BB acid mother liquors of 100kg are added in enamel reactor,
And mass fraction is slowly added to as 20% hydrogen peroxide using the speed of 500mL/min~1000mL/min in backward BB acid mother liquors,
And be stirred continuously, stop adding hydrogen peroxide after no longer gas is produced；Step 2：Enamel is warming up to 50 DEG C~60 DEG C, and is protected
Warm 15min~30min；Step 3：Weigh in the BB acid mother liquors that 20kg calcium powders are added in step 1, and add suitable washing
Water, meanwhile, the temperature of enamel reactor is controlled at 60 DEG C~70 DEG C, and keeps 1h~2h；Step 4：Treat that step 3 reaction is completed
Afterwards, the temperature that enamel reacts is increased to 110 DEG C, and keeps the temperature 2.5h, obtain light yellow floccule；Step 5：To light yellow wadding
Shape thing carries out press filtration, washs, blots again successively, final to obtain liquid aluminium polychloride finished product, the aluminium oxide obtained after detection
Content is 17.2%.
Embodiment five,
A kind of preparation process of aluminium polychloride, step 1：The BB acid mother liquors of 100kg are added in enamel reactor,
And mass fraction is slowly added to as 30% hydrogen peroxide using the speed of 500mL/min~1000mL/min in backward BB acid mother liquors,
And be stirred continuously, stop adding hydrogen peroxide after no longer gas is produced；Step 2：Enamel is warming up to 50 DEG C~60 DEG C, and is protected
Warm 15min~30min；Step 3：Weigh in the BB acid mother liquors that 10kg calcium powders are added in step 1, and add suitable washing
Water, meanwhile, the temperature of enamel reactor is controlled at 60 DEG C~70 DEG C, and keeps 1h~2h；Step 4：Treat that step 3 reaction is completed
Afterwards, the temperature that enamel reacts is increased to 110 DEG C, and keeps the temperature 4h, obtain light yellow floccule；Step 5：To light yellow cotton-shaped
Thing carries out press filtration, washs, blots again successively, final to obtain liquid aluminium polychloride finished product, and the aluminium oxide obtained after detection contains
Measure as 16.5%.
Embodiment six,
A kind of preparation process of aluminium polychloride, step 1：The BB acid mother liquors of 100kg are added in enamel reactor,
And mass fraction is slowly added to as 25% hydrogen peroxide using the speed of 500mL/min~1000mL/min in backward BB acid mother liquors,
And be stirred continuously, stop adding hydrogen peroxide after no longer gas is produced；Step 2：Enamel is warming up to 50 DEG C~60 DEG C, and is protected
Warm 15min~30min；Step 3：Weigh in the BB acid mother liquors that 16kg calcium powders are added in step 1, and add suitable washing
Water, meanwhile, the temperature of enamel reactor is controlled at 60 DEG C~70 DEG C, and keeps 1h~2h；Step 4：Treat that step 3 reaction is completed
Afterwards, the temperature that enamel reacts is increased to 105 DEG C, and keeps the temperature 3.2h, obtain light yellow floccule；Step 5：To light yellow wadding
Shape thing carries out press filtration, washs, blots again successively, final to obtain liquid aluminium polychloride finished product, the aluminium oxide obtained after detection
Content is 17.1%.
Comparative example,
Step 1：The BB acid mother liquors of 100kg are added in enamel reactor, ammonium hydroxide is configured to 3~5mol/L solution
It is quantitatively adding in enamel with kettle, unlatching stirring is slowly added to BB acid mother liquors, with cooling water control reaction temperature≤45 DEG C, neutralizes
Terminal pH=6.5~7；Step 2：By Al (OH)3Gel mixture pressure filtration washing；Step 3：By the Al (OH) after washing and filter pressing3
Gel is transferred in reaction kettle, and is added mass fraction with the speed of 500mL/min~1000mL/min and be less than 10%~20%
Dilute hydrochloric acid solution 1kg, finally obtain uniform thin liquid pasty material；Step 4：Open stirring, with 250mL/min~
500mL/min constant speed adds 10%~20% dilute hydrochloric acid solution 1.5kg, and 90~105 DEG C of controlling reaction temperature, pressure is normal
Pressure, 3~4h of reaction time, obtains light floccule；Step 5：Light floccule is carried out to pressure again, washs and blots to obtain
The aluminium polychloride finished product of liquid, detects the content of aluminium oxide 15.2%~16.9%.
By that can obtain the analysis to aluminium polychloride finished product such as the data in table 1 below：
It can be drawn by upper table 1, it is obtained by BB acid mother liquors and calcium carbonate as raw material come the aluminium polychloride for preparing
The residue of phthalic anhydride and benzene in aluminium polychloride will well below by prepared by BB acid mother liquors, ammonium hydroxide and hydrochloric acid out
Aluminium polychloride.
Also, embodiment one is to the basicity of obtained aluminium polychloride done in embodiment six and the basicity of comparative example
It is essentially identical, it disclosure satisfy that the national standard of polyaluminium chlorine.Moreover, in the production process of whole aluminium polychloride, implement
Example one will be less than the water consumption of comparative example far away to the water consumption between embodiment six, so substantially increasing the profit of water resource
With rate.
This specific embodiment is only explanation of the invention, it is not limitation of the present invention, people in the art
Member as needed can make the present embodiment the modification of no creative contribution after this specification is read, but as long as at this
All protected in the right of invention be subject to Patent Law.
Claims (8)
1. a kind of preparation process of aluminium polychloride, comprises the following steps：
BB acid mother liquors, be added in enamel reactor by S1, and is slowly added to hydrogen peroxide in backward BB acid mother liquors, and constantly stirs
Mix, stop adding after no longer gas is produced；
S2, the calcium powder for weighing certain mass are added in the BB acid mother liquors in S1；
Suitable water is added in S3, the BB acid mother liquors into S2, controls the temperature of enamel reactor at 60 DEG C~70 DEG C, and keep
1h~2h；
S4, after the completion for the treatment of S3 reactions, 100 DEG C~110 DEG C are increased to by the temperature of enamel reactor, and keep the temperature 2.5h~4h, are obtained
Obtain light yellow floccule；
S5, carry out light yellow floccule press filtration, wash, blot again successively, finally obtains finished product.
A kind of 2. preparation process of aluminium polychloride according to claim 1, it is characterised in that：The matter of hydrogen peroxide in S1
It is 20%~30% to measure fraction.
A kind of 3. preparation process of aluminium polychloride according to claim 2, it is characterised in that：Hydrogen peroxide in S1 plus
The speed entered is 500mL/min~1000mL/min.
A kind of 4. preparation process of aluminium polychloride according to claim 3, it is characterised in that：Hydrogen peroxide is added in S1
During, the gas produced in enamel reactor is outwards excluded using air exhausting device.
A kind of 5. preparation process of aluminium polychloride according to claim 4, it is characterised in that：After the completion for the treatment of S1, it will ward off
The temperature of porcelain reactor is increased to 50 DEG C~60 DEG C, and keeps 15min~30min.
A kind of 6. preparation process of aluminium polychloride according to claim 1, it is characterised in that：BB acid mother liquors in S2 with
The mass ratio of calcium powder is 1: 0.1~0.2.
A kind of 7. preparation process of aluminium polychloride according to claim 6, it is characterised in that：BB acid mother liquors in S2 with
The mass ratio of calcium powder is 1: 0.16.
A kind of 8. preparation process of aluminium polychloride according to claim 1, it is characterised in that：Water used in S3 is in S5
Wash the washings after light yellow floccule.
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| CN1031501C (en) * | 1991-01-22 | 1996-04-10 | 山西大学 | Process for recovery of aluminium compound from waste water during production of anthraquinone |
| FI98508C (en) * | 1994-05-20 | 1997-07-10 | Kemira Chemicals Oy | Method for purification of impure alumina by extraction |
| CN104671273A (en) * | 2013-11-28 | 2015-06-03 | 常州校果信息服务有限公司 | Method for producing drinking water treatment agent polyaluminum chloride from hydrogen chloride waste gas and aluminum salt water waste liquid generated from anthraquinone synthesizing production |
| CN104671269A (en) * | 2013-11-28 | 2015-06-03 | 常州校果信息服务有限公司 | Method for producing polyaluminum chloride from hydrogen chloride waste gas and aluminum salt water waste liquid generated from anthraquinone synthesizing production |
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Effective date of registration: 20220712 Address after: 132000 No. 361 Lijiang Road, Longtan District, Jilin City, Jilin Province Patentee after: Jilin Zirui New Material Co.,Ltd. Address before: 214442 No. 308, Binjiang West Road, Jiangyin City, Wuxi City, Jiangsu Province Patentee before: JIANGYIN CHANGJIANG CHEMICAL Co.,Ltd. |