CN105836865A - Process for preparing poly aluminum chloride - Google Patents
Process for preparing poly aluminum chloride Download PDFInfo
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- CN105836865A CN105836865A CN201610389486.1A CN201610389486A CN105836865A CN 105836865 A CN105836865 A CN 105836865A CN 201610389486 A CN201610389486 A CN 201610389486A CN 105836865 A CN105836865 A CN 105836865A
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- acid mother
- mother liquor
- hydrogen peroxide
- aluminium polychloride
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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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- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a process for preparing poly aluminum chloride. The process includes steps of S1, adding BB acid mother liquid into an enamel reactor, then slowly adding hydrogen peroxide into the BB acid mother liquid, continuously stirring the hydrogen peroxide and the BB acid mother liquid until gas no longer is generated and then stopping adding the hydrogen peroxide into the BB acid mother liquid; S2, weighing a certain mass of calcium powder and adding the calcium powder into the BB acid mother liquid obtained at the step S1; S3, adding an appropriate quantity of water into the BB acid mother liquid obtained at the step S2, enabling the temperature of the enamel reactor to range from 60 DEG C to 70 DEG C under the control and keeping the temperature unchanged for 1-2 h; S4, allowing reaction at the step S3 to be completely carried out, then increasing the temperature of the enamel reactor until the temperature of the enamel reactor reaches 100-110 DEG C and preserving heat of the enamel reactor for 2.5-4 h to obtain light yellow floccules; S5, sequentially carrying out filter pressing, washing and blotting on the light yellow floccules to obtain a finished product. The process has the advantages that the resource utilization rate can be effectively increased, the purity of the finished product can be improved, and secondary pollution on treated water due to substances such as phthalic anhydride and benzene which are mixed with an existing finished product can be prevented; steps for preparing the poly aluminum chloride can be reduced, and accordingly the production efficiency can be improved.
Description
Technical field
The present invention relates to aluminum chloride flocculant production technical field, particularly to the preparation technology of a kind of aluminium polychloride.
Background technology
Aluminium polychloride is a kind of water-purifying material, and inorganic polymer coagulant is called again poly-aluminium for short, and english abbreviation is PAC,
It is inorganic that the molecular weight produced due to the bridging action of hydroxide ion and the polymerization of multivalent anions is relatively big, electric charge is higher
High molecular water treating chemical.Solid and liquid two kinds can be divided into the most again.Solid by color difference be divided into again sepia,
Ecru, golden yellow and white, liquid can be rendered as water white transparency, slightly yellow, light yellow to yellowish-brown.Different colours
Aluminium polychloride also has bigger difference in application and production technology.
The raw material being used for preparing liquid aluminium polychloride in prior art mainly has aluminium bits, aluminium ash and aluminium slag, aluminium hydroxide, chlorine
Change aluminium and aluminum-containing mineral etc..Additionally, in order to improve the utilization rate of resource and implement the theory of Green Chemistry, therefore, existing
Partial oxidation aluminium manufacturing enterprise is used as raw material with mother liquor remaining in BB acid production process, and its main reaction is former
Reason 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 this
Reaction principle need first pass through interpolation ammoniacal liquor to the acidity neutralizing in mother liquor, and backward by one-tenths point taking-up precipitate A l (OH)3Inside adds
Enter and after hydrochloric acid carries out polymerization curing, make aluminium polychloride again, thus cause a large amount of wastes that hydrochloric acid uses, and also can be to ring
Border pollutes, and due in BB acid mother liquor possibly together with the organic substance such as phthalic anhydride, benzene, so final to aluminium polychloride
Purity will also result in certain impact.
Summary of the invention
It is an object of the invention to provide a kind of preparation reducing material waste and the high aluminium polychloride of alumina leaching amount
Technique.
The above-mentioned purpose of the present invention has the technical scheme that the preparation technology of a kind of aluminium polychloride, bag
Include following steps:
S1, BB acid mother liquor is joined in enamel reactor, and backward BB acid mother liquor is slowly added to hydrogen peroxide, and be stirred continuously,
Stop adding after no longer producing gas；
S2, weigh in the BB acid mother liquor that the calcium powder of certain mass joins in S1；
S3, BB acid mother liquor in S2 add appropriate water, control the temperature of enamel reactor at 60 DEG C～70 DEG C, and keep 1h～
2h；
S4, after S3 has reacted, the temperature that enamel reacts is increased to 100 DEG C～110 DEG C, and is incubated 2.5h～4h, it is thus achieved that be shallow
Yellow floccule；
S5, light yellow floccule is carried out press filtration the most again, wash, blot, finally obtain finished product.
Due to the Organic Ingredients that be left behind when being used for prepare BB acid containing phthalic anhydride, benzene etc. in BB acid mother liquor, and typically
Being insoluble in water, the last very difficult water in reaction is washed away, therefore, when producing polymerization chlorine with BB acid mother liquor as raw material
The when of changing aluminium finished product, the surface of finished product will carry phthalic anhydride and benzene, thus is purifying as flocculant with this aluminium polychloride
New noxious material will be brought in water body when of water body, thus will result in the secondary pollution of water body.And hydrogen peroxide is in acid
Having the strongest oxidisability under conditions of property, phthalic anhydride can be become carbon dioxide, carbon monoxide and water by it with benzene oxidatoin, thus has
It is beneficial to improve the purity of aluminium polychloride.
And BB acid mother liquor just contains hydrogen ion originally, therefore, there is no need to individually add acid from the external world to BB acid mother liquor
In, meanwhile, decrease postorder for neutralizing the input amount of alkaline material needed for BB acid mother liquor.
It addition, put into calcium powder i.e. calcium carbonate in BB acid mother liquor, primarily to make the aluminium ion in BB acid mother liquor and carbon
Acid calcium generation Polymeric and aging reactions generates aluminium polychloride, so compares interpolation ammoniacal liquor and precipitates, and then recycling salt solution enters
For the operation of row curing, greatly reduce operating procedure.Further, calcium carbonate also advantageously improves the basicity of aluminium polychloride,
The polymer poly that so aluminium ion hydrolyzes to form is right the highest, and the charge neutrality ability of its active ingredient and bonding bridge formation ability are more
By force, so flocculating property is the best.
As preferably, the mass fraction of the hydrogen peroxide in S1 is 20%～30%.
As preferably, the speed of the addition of the hydrogen peroxide in S1 is 500mL/min～1000mL/min.
Utilize high concentration, low speed to add hydrogen peroxide, primarily to reduce the number of times that hydrogen peroxide adds, and can also keep away
Exempt from the waste that hydrogen peroxide input amount too much causes, thus substantially increase hydrogen peroxide utilization rate.
As preferably, during S1 adds hydrogen peroxide, air exhausting device is utilized outwards to be got rid of by the gas produced in enamel.
Owing to hydrogen peroxide is when aoxidizing phthalic anhydride and benzene etc. and being organic, it can produce carbon dioxide and carbon monoxide, and an oxygen
Change carbon inherently a kind of poisonous gas, therefore by air exhausting device, the carbon dioxide in enamel reactor and carbon monoxide are arranged
On the one hand go out, be conducive to avoiding the pressure in enamel reactor excessive and cause potential safety hazard, on the other hand can also avoid an oxygen
Change carbon production environment is polluted so that staff occurs toxic hazard.
As preferably, after S1 completes, the temperature of enamel is increased to 50 DEG C～60 DEG C, and keeps 15min～30min.
The hydrogen peroxide low due to concentration will be decomposed at normal temperatures, when the temperature of enamel be increased to 50 DEG C～60 DEG C time
Waiting, the decomposition rate of hydrogen peroxide will be accelerated, and in the range of this temperature, continuation insulation 15min～30min, thus only
Have less than 5% hydrogen peroxide undecomposed complete, be so conducive to avoiding hydrogen peroxide concentration too high and ensuing operation being caused shadow
Ring.
As preferably, the BB acid mother liquor in S2 is 1: 0.1～0.2 with the mass ratio of calcium powder.
As preferably, the BB acid mother liquor in S2 is 1: 0.16 with the mass ratio of calcium powder.
When the mass ratio of calcium powder and BB acid mother liquor more than 0.2 when, the basicity of the aluminium polychloride produced is just
Can be more than 90%.Now, owing to basicity is too high, the hydroxyl in polymer can be made to tend to saturated, generate the hydroxide of indissoluble
Thing micelle, product is difficult to stable existence, affects the flocculating property of product simultaneously.And the mass ratio of calcium powder and BB acid mother liquor
The suitableeest scope is 0.16.
As preferably, the water used by S3 is the washings after washing light yellow floccule in S5.
Utilize in S5 and be used as raw material and dose in S3 with washing the washings after light yellow floccule, so not only increase
The utilization ratio of water resource, meanwhile, on light yellow floccule by under washing again can be by for the chlorion being utilized, aluminium ion etc.
Re-use, and then substantially increase the utilization rate of each element in whole system, therefore, be close to this theory of Green Chemistry.
In sum, the method have the advantages that
1. with the phthalic anhydride in hydrogen peroxide oxidation BB acid mother liquor and benzene, so it can be avoided that phthalic anhydride and benzene are attached on product being purified
Water body causes secondary pollution；
2. utilize calcium carbonate that BB mother liquor carries out Polymeric and aging reactions and produce aluminium polychloride, be so greatly saved the step of operation,
Improve the efficiency of operation；
3. utilize the washings washing light yellow floccule to be used as raw material to join in enamel reactor and react, be so greatly improved
The utilization rate of water resource, calcium ion and chlorion etc., thus more it is close to the environmental protection concept of Green Chemistry.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of aluminium polychloride.
Detailed description of the invention
Below in conjunction with accompanying drawing 1, the present invention is described in further detail.
Embodiment 1,
A kind of preparation technology of aluminium polychloride, step one: the BB acid mother liquor of 100kg is joined in enamel reactor, and backward
BB acid mother liquor is slowly added to, with the speed of 500mL/min～1000mL/min, the hydrogen peroxide that mass fraction is 20%, and constantly
Stirring, stops adding hydrogen peroxide after no longer producing gas；Step 2: enamel is warming up to 50 DEG C～60 DEG C, and be incubated 15min～
30min；Step 3: weigh in the BB acid mother liquor that 10kg calcium powder joins in step one, and add appropriate washings, meanwhile,
The temperature of control enamel reactor is at 60 DEG C～70 DEG C, and keeps 1h～2h；Step 4: after step 3 has been reacted, will ward off
The temperature of porcelain reaction is increased to 100 DEG C, and is incubated 2.5h, it is thus achieved that light yellow floccule；Step 5: light yellow floccule is depended on
Secondary carrying out press filtration again, wash, blot, final obtain liquid aluminium polychloride finished product, the content of the aluminum oxide obtained after detection is
15.3%.
Embodiment two,
A kind of preparation technology of aluminium polychloride, step one: the BB acid mother liquor of 100kg is joined in enamel reactor, and backward
BB acid mother liquor is slowly added to, with the speed of 500mL/min～1000mL/min, the hydrogen peroxide that mass fraction is 30%, and constantly
Stirring, stops adding hydrogen peroxide after no longer producing gas；Step 2: enamel is warming up to 50 DEG C～60 DEG C, and be incubated 15min～
30min；Step 3: weigh in the BB acid mother liquor that 20kg calcium powder joins in step one, and add appropriate washings, meanwhile,
The temperature of control enamel reactor is at 60 DEG C～70 DEG C, and keeps 1h～2h；Step 4: after step 3 has been reacted, will ward off
The temperature of porcelain reaction is increased to 110 DEG C, and is incubated 4h, it is thus achieved that light yellow floccule；Step 5: to light yellow floccule successively
Carrying out press filtration again, wash, blot, final obtain liquid aluminium polychloride finished product, the content of the aluminum oxide obtained after detection is
16.4%.
Embodiment three,
A kind of preparation technology of aluminium polychloride, step one: the BB acid mother liquor of 100kg is joined in enamel reactor, and backward
BB acid mother liquor is slowly added to, with the speed of 500mL/min～1000mL/min, the hydrogen peroxide that mass fraction is 25%, and constantly
Stirring, stops adding hydrogen peroxide after no longer producing gas；Step 2: enamel is warming up to 50 DEG C～60 DEG C, and be incubated 15min～
30min；Step 3: weigh in the BB acid mother liquor that 16kg calcium powder joins in step one, and add appropriate washings, meanwhile,
The temperature of control enamel reactor is at 60 DEG C～70 DEG C, and keeps 1h～2h；Step 4: after step 3 has been reacted, will ward off
The temperature of porcelain reaction is increased to 105 DEG C, and is incubated 3.2h, it is thus achieved that light yellow floccule；Step 5: light yellow floccule is depended on
Secondary carrying out press filtration again, wash, blot, final obtain liquid aluminium polychloride finished product, the content of the aluminum oxide obtained after detection is
16.9%.
Embodiment four,
A kind of preparation technology of aluminium polychloride, step one: the BB acid mother liquor of 100kg is joined in enamel reactor, and backward
BB acid mother liquor is slowly added to, with the speed of 500mL/min～1000mL/min, the hydrogen peroxide that mass fraction is 20%, and constantly
Stirring, stops adding hydrogen peroxide after no longer producing gas；Step 2: enamel is warming up to 50 DEG C～60 DEG C, and be incubated 15min～
30min；Step 3: weigh in the BB acid mother liquor that 20kg calcium powder joins in step one, and add appropriate washings, meanwhile,
The temperature of control enamel reactor is at 60 DEG C～70 DEG C, and keeps 1h～2h；Step 4: after step 3 has been reacted, will ward off
The temperature of porcelain reaction is increased to 110 DEG C, and is incubated 2.5h, it is thus achieved that light yellow floccule；Step 5: light yellow floccule is depended on
Secondary carrying out press filtration again, wash, blot, final obtain liquid aluminium polychloride finished product, the content of the aluminum oxide obtained after detection is
17.2%.
Embodiment five,
A kind of preparation technology of aluminium polychloride, step one: the BB acid mother liquor of 100kg is joined in enamel reactor, and backward
BB acid mother liquor is slowly added to, with the speed of 500mL/min～1000mL/min, the hydrogen peroxide that mass fraction is 30%, and constantly
Stirring, stops adding hydrogen peroxide after no longer producing gas；Step 2: enamel is warming up to 50 DEG C～60 DEG C, and be incubated 15min～
30min；Step 3: weigh in the BB acid mother liquor that 10kg calcium powder joins in step one, and add appropriate washings, meanwhile,
The temperature of control enamel reactor is at 60 DEG C～70 DEG C, and keeps 1h～2h；Step 4: after step 3 has been reacted, will ward off
The temperature of porcelain reaction is increased to 110 DEG C, and is incubated 4h, it is thus achieved that light yellow floccule；Step 5: to light yellow floccule successively
Carrying out press filtration again, wash, blot, final obtain liquid aluminium polychloride finished product, the content of the aluminum oxide obtained after detection is
16.5%.
Embodiment six,
A kind of preparation technology of aluminium polychloride, step one: the BB acid mother liquor of 100kg is joined in enamel reactor, and backward
BB acid mother liquor is slowly added to, with the speed of 500mL/min～1000mL/min, the hydrogen peroxide that mass fraction is 25%, and constantly
Stirring, stops adding hydrogen peroxide after no longer producing gas；Step 2: enamel is warming up to 50 DEG C～60 DEG C, and be incubated 15min～
30min；Step 3: weigh in the BB acid mother liquor that 16kg calcium powder joins in step one, and add appropriate washings, meanwhile,
The temperature of control enamel reactor is at 60 DEG C～70 DEG C, and keeps 1h～2h；Step 4: after step 3 has been reacted, will ward off
The temperature of porcelain reaction is increased to 105 DEG C, and is incubated 3.2h, it is thus achieved that light yellow floccule；Step 5: light yellow floccule is depended on
Secondary carrying out press filtration again, wash, blot, final obtain liquid aluminium polychloride finished product, the content of the aluminum oxide obtained after detection is
17.1%.
Comparative example,
Step one: join in enamel reactor by the BB acid mother liquor of 100kg, is configured to ammoniacal liquor 3～5mol/L solution and quantitatively adds
Enter in enamel and in still, open stirring and be slowly added to BB acid mother liquor, with cooling water control reaction temperature≤45 DEG C, neutralize terminal
PH=6.5～7；Step 2: by Al (OH)3Gel mixture press filtration is washed；Step 3: by the Al (OH) after washing and filter pressing3
Gel is transferred in reactor, and is less than 10%～20% with the speed addition mass fraction of 500mL/min～1000mL/min
Dilute hydrochloric acid solution 1kg, the uniform thin liquid pasty material of final acquisition；Step 4: open stirring, with 250mL/min～
500mL/min constant speed adds the dilute hydrochloric acid solution 1.5kg of 10%～20%, control reaction temperature 90～105 DEG C, and pressure is normal pressure,
Reaction time 3～4h, it is thus achieved that light color floccule；Step 5: light color floccule is carried out pressure again, washs and blot and obtain liquid
The aluminium polychloride finished product of state, detects that the content of aluminum oxide is 15.2%～16.9%.
By to the data in can obtaining such as table 1 below to the analysis of aluminium polychloride finished product:
Can be drawn by upper table 1, the aluminium polychloride prepared as raw material by BB acid mother liquor and calcium carbonate, obtained polymerization chlorine
The residue changing the phthalic anhydride in aluminium and benzene will be well below by the polymerization chlorine out prepared by BB acid mother liquor, ammoniacal liquor and hydrochloric acid
Change aluminium.
Further, the basicity of the aluminium polychloride prepared done in embodiment one to embodiment six is basic with the basicity of comparative example
Identical, it is possible to meet the national standard of polyaluminium chlorine.And, in the production process of whole aluminium polychloride, embodiment one
Water consumption between embodiment six will be out and away less than the water consumption of comparative example, so substantially increasing the utilization rate of water resource.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, and those skilled in the art exist
As required the present embodiment can be made after reading this specification and there is no the amendment of creative contribution, but as long as the present invention's
All protected by Patent Law in right.
Claims (8)
1. a preparation technology for aluminium polychloride, comprises the following steps:
S1, BB acid mother liquor is joined in enamel reactor, and backward BB acid mother liquor is slowly added to hydrogen peroxide, and be stirred continuously,
Stop adding after no longer producing gas；
S2, weigh in the BB acid mother liquor that the calcium powder of certain mass joins in S1；
S3, BB acid mother liquor in S2 add appropriate water, control the temperature of enamel reactor at 60 DEG C～70 DEG C, and keep 1h～
2h；
S4, after S3 has reacted, the temperature that enamel reacts is increased to 100 DEG C～110 DEG C, and is incubated 2.5h～4h, it is thus achieved that be shallow
Yellow floccule；
S5, light yellow floccule is carried out press filtration the most again, wash, blot, finally obtain finished product.
The preparation technology of a kind of aluminium polychloride the most according to claim 1, it is characterised in that: the quality of the hydrogen peroxide in S1 is divided
Number is 20%～30%.
The preparation technology of a kind of aluminium polychloride the most according to claim 2, it is characterised in that: the addition of the hydrogen peroxide in S1
Speed is 500mL/min～1000mL/min.
The preparation technology of a kind of aluminium polychloride the most according to claim 3, it is characterised in that: the mistake of hydrogen peroxide is added at S1
Cheng Zhong, utilizes air exhausting device outwards to be got rid of by the gas produced in enamel.
The preparation technology of a kind of aluminium polychloride the most according to claim 4, it is characterised in that: after S1 completes, by enamel
Temperature be increased to 50 DEG C～60 DEG C, and keep 15min～30min.
The preparation technology of a kind of aluminium polychloride the most according to claim 1, it is characterised in that: the BB acid mother liquor in S2 and calcium
The mass ratio of powder is 1: 0.1～0.2.
The preparation technology of a kind of aluminium polychloride the most according to claim 6, it is characterised in that: the BB acid mother liquor in S2 and calcium
The mass ratio of powder is 1: 0.16.
The preparation technology of a kind of aluminium polychloride the most according to claim 1, it is characterised in that: the water used by S3 is to wash in S5
Wash the washings after light yellow floccule.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063468A (en) * | 1991-01-22 | 1992-08-12 | 山西大学 | From the waste water of producing anthraquinone, reclaim the method for aluminum compound |
| FI942338A0 (en) * | 1994-05-20 | 1994-05-20 | Kemira Chemicals Oy | Method for purification of impure alumina by extraction |
| 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 |
| 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 |
-
2016
- 2016-06-04 CN CN201610389486.1A patent/CN105836865B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063468A (en) * | 1991-01-22 | 1992-08-12 | 山西大学 | From the waste water of producing anthraquinone, reclaim the method for aluminum compound |
| FI942338A0 (en) * | 1994-05-20 | 1994-05-20 | Kemira Chemicals Oy | Method for purification of impure alumina by extraction |
| 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 |
| 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 |
Non-Patent Citations (1)
| Title |
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| 孙惠国: ""合成蒽醌BB酸母液生产高纯聚氯化铝及聚硫氯化铝的工艺"", 《上海化工》 * |
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