CN109534467A - A kind of high-performance aluminium polychloride and preparation method thereof - Google Patents
A kind of high-performance aluminium polychloride and preparation method thereof Download PDFInfo
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- CN109534467A CN109534467A CN201811542137.4A CN201811542137A CN109534467A CN 109534467 A CN109534467 A CN 109534467A CN 201811542137 A CN201811542137 A CN 201811542137A CN 109534467 A CN109534467 A CN 109534467A
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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
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Abstract
The invention discloses a kind of high-performance aluminium polychlorides, are made of the primary raw material of following parts by weight: 40-50 parts of modified polyaluminium chloride, 15-20 parts of sodium chlorate, 10-16 parts of Nacl, 6-9 parts of zinc chloride, 20-30 parts of 36% technical hydrochloric acid, 10-15 parts of sodium metasilicate, without 80-100 parts of ammonia distilled water, NaHCO318-25 parts of solution;The invention also discloses the preparation methods of the high-performance aluminium polychloride.The present invention is based on modified polyaluminium chloride, it is copolymerized during preparation with zinc chloride, polysilicon acid, obtain a kind of polymer for having both aluminium salt, magnesium salts and zinc salt, pass through addition sodium chlorate and Nacl again, obtain the high performance aluminium polychloride, the high performance aluminium polychloride is in wastewater treatment process, the sinking speed of waste is faster, except algae effect is good, wadding body is big, wadding body is closely knit, sinking speed is fast, dosage is low, it can be effectively reduced cost, have great importance to water supply quality is guaranteed with water producing cost is reduced.
Description
Technical field
The invention belongs to inorganic polymer technical fields, and in particular, to a kind of high-performance aluminium polychloride and its preparation
Method.
Background technique
In inorganic polymer flocculant, AlSnSi alloy kind is more, and process of preparing is more mature.Wherein it polymerize
Aluminium chloride (Polyaluminium Chloride), abbreviation PAC, commonly referred to as aluminium chloride, poly- hydroxy Al etc., are current
Industrial production technology is most mature, efficiency highest, the kind being most widely used.It is not a certain kind representated by aluminium polychloride
Specific inorganic compound, but a series of general name of inorganic polymers.
Polyaluminum ferric chloride is that aluminium chloride, magnesium chloride are built bridge a kind of inorganic high score formed by hydroxyl in aqueous solution
Sub- flocculant, the molecule have a variety of polymeric forms, the bending of molecule long-chain, twisting cyclization, in chain chain using long-chain as basic structure
Between, between the face of face be key connection, chain link repeats ordered arrangement into macromolecule, constitutes complicated orderly molecular structure, it was both
There are the excellent flocculating property and powerful charge effect of aluminium polychloride, and has the strong adsorption of magnesium chloride, settling velocity fast
Characteristic, flocculant can be made, be used for purifying drinking water and water treatment, it may also be used for sanitary sewage, Industrial Wastewater Treatment, use are red
The waste liquid preparation polyaluminum ferric chloride that mud extracts scandium has highly important application value.
It is existing to prepare aluminium polychloride method there is higher costs, product effective constituents A l13Content is lower, total Al is dense
Degree is not high, is also easy to produce the deficiencies of pollution place.
Summary of the invention
The purpose of the present invention is to provide a kind of high-performance aluminium polychlorides and preparation method thereof, with modified polyaluminium chloride
Based on, it is copolymerized during preparation with zinc chloride, polysilicon acid, obtains a kind of polymer for having both aluminium salt, magnesium salts and zinc salt,
Again by addition sodium chlorate and Nacl, a kind of high performance aluminium polychloride, high performance polymerization chlorine obtained is prepared
Change aluminium in wastewater treatment process, the sinking speed of waste faster, except algae effect is good, wadding body is big, wadding body is closely knit, sinking speed
Fastly, dosage is low, can be effectively reduced cost, high performance aluminium polychloride is to guarantee water supply quality and reduces water producing cost tool
There is important meaning.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of high-performance aluminium polychloride, is made of the primary raw material of following parts by weight: 40-50 parts of modified polyaluminium chloride, chlorine
Sour sodium 15-20 parts, 10-16 parts of Nacl, 6-9 parts of zinc chloride, 20-30 parts of 36% technical hydrochloric acid, 10-15 parts of sodium metasilicate, without ammonia steam
80-100 parts of distilled water, NaHCO318-25 parts of solution;
The high-performance aluminium polychloride is made of following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 30-40min is stirred in 45-55 DEG C of thermostat water bath, chlorination is made
Zinc solution;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3-4,60
In DEG C thermostat water bath, 30r/min magnetic agitation 60-70min, polysilicon acid solution is made;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 60-70min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure
30h obtains thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
Further, the NaHCO3The mass concentration of solution is 22g/L.
Further, the modified polyaluminium chloride is prepared by the following method:
1) hydrochloric acid solution that mass fraction is 25.3% is prepared, it is spare;
2) waste alumina mud is added in above-mentioned hydrochloric acid solution according to mass ratio 1:0.6-0.7, is 60 DEG C, mixing speed in reaction temperature
Under conditions of 250r/min, 90-100min is reacted, filtering obtains aluminum trichloride solution;
3) aluminum trichloride solution is placed in a beaker, under conditions of 26 DEG C of reaction temperature, mixing speed are 250r/min, is pressed
Al/Mg molar ratio is 1:9 addition magnesium chloride solution, then into solution with P/(Al3++Mg2+) molar ratio be 0.1 be added stabilizer
Sodium phosphate cures 2h, and modified polyaluminium chloride is made.
A kind of preparation method of high-performance aluminium polychloride, includes the following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 30-40min is stirred in 45-55 DEG C of thermostat water bath, chlorination is made
Zinc solution;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3-4,60
In DEG C thermostat water bath, 30r/min magnetic agitation 60-70min, polysilicon acid solution is made;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 60-70min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure
30h obtains thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
Beneficial effects of the present invention:
The present invention first leaches liquor alumini chloridi with waste alumina mud using modified polyaluminium chloride as main body, then by molten in aluminium chloride
Liquid is added polychloride magnesium and modified polyaluminium chloride, liquor alumini chloridi and magnesium chloride solution is prepared through abundant during polymerizeing
Mixing, curing modified polyaluminium chloride obtained are a kind of polyaluminium magnalium coagulant, and polyaluminium magnalium is a kind of novel
Inorganic macromolecular composite coagulant, the advantages of combining two kinds of coagulant of magnesium salts and aluminium salt, overcome the remaining coloration of magnesium salts
Greatly, the alumen ustum of stability difference and aluminium salt generates the disadvantage that slow, alumen ustum is light, sedimentation is slow, has more excellent than single magnesium salts or aluminium salt
Good coagulation performance;Efficient modified polyaluminium chloride can not only be made by waste alumina mud, additionally it is possible to turn waste into wealth, Neng Goubao
Ecological environment is protected, good economic benefit is created;
The present invention is copolymerized during preparation with zinc chloride, polysilicon acid based on modified polyaluminium chloride, is obtained a kind of simultaneous
Have the polymer of aluminium salt, magnesium salts and zinc salt, then by addition sodium chlorate and Nacl, a kind of high performance polymerization chlorine is prepared
Change aluminium, high performance aluminium polychloride obtained in wastewater treatment process, the sinking speed of waste faster, except algae effect it is good,
Wadding body is big, wadding body is closely knit, sinking speed is fast, and dosage is low, can be effectively reduced cost, high performance aluminium polychloride is to guarantee
Water supply quality and reduction water producing cost have great importance.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiment obtained without creative efforts belongs to what the present invention protected
Range.
A kind of high-performance aluminium polychloride, is made of the primary raw material of following parts by weight: modified polyaluminium chloride 40-50
Part, 15-20 parts of sodium chlorate, 10-16 parts of Nacl, 6-9 parts of zinc chloride, 20-30 parts of 36% technical hydrochloric acid, 10-15 parts of sodium metasilicate,
Without 80-100 parts of ammonia distilled water, NaHCO318-25 parts of solution;
The NaHCO3The mass concentration of solution is 22g/L;
The modified polyaluminium chloride is prepared by the following method:
1) hydrochloric acid solution that mass fraction is 25.3% is prepared, it is spare;
2) waste alumina mud is added in above-mentioned hydrochloric acid solution according to mass ratio 1:0.6-0.7, is 60 DEG C, mixing speed in reaction temperature
Under conditions of 250r/min, 90-100min is reacted, filtering obtains aluminum trichloride solution;
The step is the leaching to waste alumina mud, can obtain aluminium content (with Al2O3Meter) it is that 6.72%, free acid (in terms of HCl) is
0.85% aluminum trichloride solution, wherein aluminium leaching rate reaches 99.08%;
3) aluminum trichloride solution is placed in a beaker, under conditions of 26 DEG C of reaction temperature, mixing speed are 250r/min, is pressed
Al/Mg(molar ratio)=1:9 addition magnesium chloride solution, then into solution with P/(Al3++Mg2+)=0.1(molar ratio) it is added and stablizes
Agent sodium phosphate cures 2h, and modified polyaluminium chloride is made;
Liquor alumini chloridi first is leached with waste alumina mud, then is prepared by the way that polychloride magnesium is added during liquor alumini chloridi polymerize
To modified polyaluminium chloride, liquor alumini chloridi, which is adequately mixed with magnesium chloride solution, cures modified polyaluminium chloride obtained, is
A kind of polyaluminium magnalium coagulant, polyaluminium magnalium are a kind of novel inorganic macromolecular composite coagulant, combine magnesium
The advantages of two kinds of coagulant of salt and aluminium salt, the remaining coloration for overcoming magnesium salts is big, stability is poor and the alumen ustum of aluminium salt generates slow, alum
Disadvantage light, that sedimentation is slow is spent, there is the coagulation performance more excellent than single magnesium salts or aluminium salt;
Efficient modified polyaluminium chloride can not only be made by waste alumina mud, additionally it is possible to turn waste into wealth, it being capable of protecting ecology ring
Good economic benefit is created in border;
The preparation method of the high-performance aluminium polychloride, includes the following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 30-40min is stirred in 45-55 DEG C of thermostat water bath, chlorination is made
Zinc solution;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3-4,60
In DEG C thermostat water bath, 30r/min magnetic agitation 60-70min, polysilicon acid solution is made;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 60-70min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure
30h obtains thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
Embodiment 1
A kind of high-performance aluminium polychloride, is made of the primary raw material of following parts by weight: 40 parts of modified polyaluminium chloride, sodium chlorate
15 parts, 10 parts of Nacl, 6 parts of zinc chloride, 20 parts of 36% technical hydrochloric acid, 10 parts of sodium metasilicate, without 80 parts of ammonia distilled water, NaHCO3It is molten
18 parts of liquid;
The high-performance aluminium polychloride is made of following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 40min is stirred in 45 DEG C of thermostat water baths, it is molten that zinc chloride is made
Liquid;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3, at 60 DEG C
In thermostat water bath, 30r/min magnetic agitation 60min, be made polysilicon acid solution;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 60min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure 30h,
Obtain thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
Embodiment 2
A kind of high-performance aluminium polychloride, is made of the primary raw material of following parts by weight: 45 parts of modified polyaluminium chloride, sodium chlorate
18 parts, 13 parts of Nacl, 7.5 parts of zinc chloride, 25 parts of 36% technical hydrochloric acid, 13 parts of sodium metasilicate, without 90 parts of ammonia distilled water, NaHCO3
21 parts of solution;
The high-performance aluminium polychloride is made of following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 35min is stirred in 50 DEG C of thermostat water baths, it is molten that zinc chloride is made
Liquid;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3.5,60
In DEG C thermostat water bath, 30r/min magnetic agitation 65min, polysilicon acid solution is made;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 650min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure
30h obtains thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
Embodiment 3
A kind of high-performance aluminium polychloride, is made of the primary raw material of following parts by weight: 50 parts of modified polyaluminium chloride, sodium chlorate
20 parts, 16 parts of Nacl, 9 parts of zinc chloride, 30 parts of 36% technical hydrochloric acid, 15 parts of sodium metasilicate, without 100 parts of ammonia distilled water, NaHCO3It is molten
25 parts of liquid;
The high-performance aluminium polychloride is made of following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 30min is stirred in 55 DEG C of thermostat water baths, it is molten that zinc chloride is made
Liquid;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 4, at 60 DEG C
In thermostat water bath, 30r/min magnetic agitation 70min, be made polysilicon acid solution;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 70min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure 30h,
Obtain thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
Following performance test, commercially available flocculant of polymeric aluminium chloride are done to the embodiment 1-3 aluminium polychloride being prepared
It compares:
It takes 200mL waste water water sample in beaker, 15g flocculant is added, first quickly (about 200r/min) stirs 2min, then at a slow speed
(60r/min) stirs 10min, stands 60min and takes supernatant liquor with pipette after settling of floccus is complete, tests its absorbance
And COD value, the practical flocculating effect of flocculant, test knot are judged as evaluation index using coloration removal efficiency and COD removal efficiency
Fruit is as follows:
It is found that the aluminium polychloride that the present invention is prepared reaches 87.4-87.9% to the coloration removal efficiency of waste water, to COD removal efficiency
Up to 68.7-68.8%, compared to commercially available flocculant, the flocculating effect for the aluminium polychloride that the present invention is prepared is good, flocculation efficiency
It is high.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (4)
1. a kind of high-performance aluminium polychloride, which is characterized in that be made of the primary raw material of following parts by weight: modified poly chlorination
40-50 parts of aluminium, 15-20 parts of sodium chlorate, 10-16 parts of Nacl, 6-9 parts of zinc chloride, 20-30 parts of 36% technical hydrochloric acid, sodium metasilicate
10-15 parts, without 80-100 parts of ammonia distilled water, NaHCO318-25 parts of solution;
The high-performance aluminium polychloride is made of following steps:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 30-40min is stirred in 45-55 DEG C of thermostat water bath, chlorination is made
Zinc solution;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3-4,60
In DEG C thermostat water bath, 30r/min magnetic agitation 60-70min, polysilicon acid solution is made;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 60-70min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure
30h obtains thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
2. a kind of high-performance aluminium polychloride according to claim 1, which is characterized in that the NaHCO3The quality of solution
Concentration is 22g/L.
3. a kind of high-performance aluminium polychloride according to claim 1, which is characterized in that the modified polyaluminium chloride by
Following method preparation:
1) hydrochloric acid solution that mass fraction is 25.3% is prepared, it is spare;
2) waste alumina mud is added in above-mentioned hydrochloric acid solution according to mass ratio 1:0.6-0.7, is 60 DEG C, mixing speed in reaction temperature
Under conditions of 250r/min, 90-100min is reacted, filtering obtains aluminum trichloride solution;
3) aluminum trichloride solution is placed in a beaker, under conditions of 26 DEG C of reaction temperature, mixing speed are 250r/min, is pressed
Al/Mg molar ratio is 1:9 addition magnesium chloride solution, then into solution with P/(Al3++Mg2+) molar ratio be 0.1 be added stabilizer
Sodium phosphate cures 2h, and modified polyaluminium chloride is made.
4. a kind of preparation method of high-performance aluminium polychloride, which comprises the steps of:
Step 1: zinc chloride is added in 36% technical hydrochloric acid, 30-40min is stirred in 45-55 DEG C of thermostat water bath, chlorination is made
Zinc solution;
Step 2: by sodium metasilicate be added without in ammonia distilled water, add mass fraction be 37% sulphur acid for adjusting pH to 3-4,60
In DEG C thermostat water bath, 30r/min magnetic agitation 60-70min, polysilicon acid solution is made;
Step 3: the liquor zinci chloridi of above-mentioned preparation and polysilicon acid solution are slowly added into modified polyaluminium chloride, it is added
NaHCO3Solution, 30r/min stirring and dissolving and the polymerization reaction 60-70min at 55 DEG C, then be placed in 108 DEG C of drying boxes and cure
30h obtains thick liquid;
Step 4: powder is made through dilution, filtering and spray drying in above-mentioned thick liquid;
Step 5: powder, sodium chlorate and Nacl are uniformly mixed, high-performance aluminium polychloride is made.
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