CN106517463B - High-purity high basicity nanoscale PACS flocculant and preparation method thereof - Google Patents
High-purity high basicity nanoscale PACS flocculant and preparation method thereof Download PDFInfo
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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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- 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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Abstract
The present invention relates to the preparation methods of high-purity high basicity nanoscale PACS flocculant, comprising the following steps: (1), generates one section of PAC material;(2), two sections of high-purity PAC materials are generated;(3), material level-one separates;(4), the second-order separation.PACS flocculant made from the preparation method has nanoscale crystalline structure form, significantly improves hydroxyl polymeric degree and basicity, to increase inorganic polymer amount, has extraordinary purifying water effect.
Description
Technical field
The invention belongs to water environmental protection technical field, it is related to a kind of water purification PACS flocculant, more particularly to a kind of high-purity high
Basicity nanoscale PACS flocculant and preparation method thereof.
Background technique
PACS product is the high efficiency composition product that High-purity Polyaluminum Chloride introduces sulfate ion.Its existing production method is
Temperature-pressure in a kettle will contain Al2O364% or so gel aluminum hydroxide in a kettle be lower than the equivalent thickness of aluminium salt
Acid dissolves out molten aluminum under conditions of temperature-pressure, and one-step synthesis obtains limpid bright aluminium polychloride liquid after separation.Its
Reaction are as follows:
Al(OH)3+HCl→Al(OH)2Cl+H2O
2Al(OH)2Cl+HCl→Al2(OH)3Cl3+H2O
Al2(OH)3Cl3→〔Al2(OH)nCl6-n〕M
The aluminium polychloride general formula of M < 10.
The various compound states of hydroxyl polymeric aluminum belong to aluminium ion hydrolyze, be complexed in the solution, peptization, precipitating, crystallization
Reaction intermediate, it is also to be classified according to the molecular weight of the degree of polymerization.In earliest PAC solution be added sulfate radical from
Son is that Japanese studies, and charge density is slightly lower, and zero point is in PH7.5, and traditional PAC and aluminum sulfate, charge density
Lower, in pH value up to switching to negative electrical charge after neutral, it is many that the charge neutrality of flocculant and net catch function reduction, for this purpose, domestic
PAC product be also initially added into some sulfate radicals, form later PACS product.
As the domestic Chinese Academy of Sciences is in the modal developmental research of hydroxy Al, from the exploration of theory and practice, chemically product
By Al in the mechanism of purification13Research extraction risen to from the point of view of nanometer technology material, with Al13It is combined and detached from extraction
During, a part for being applied to nanometer technology synthesis of sulfate ion, and examine sulfate radical and hydroxy Al raw
The form composition of solution is detected at sediment, it may be assumed that Al13O4(OH)24(H2O)+7 12(general molecular formula), shows sulfate radical and hydroxyl
Aluminum solutions existing chemical dynamics process, fundamental reaction under different shape are as follows:
Ala+n SO2- 4→Al- a(SO4)nTransient response generates dissolution complex compound
Alb+n SO2- 4→Al- b(SO4)nSlow reaction generates crystal precipitation
Alc+n SO2- 4→Al- c(SO4)nFast reaction generates amorphous sediment object
Add BaProduct salt and calcium displace Alb material.
The crystalline structure formed are as follows:
Na〔Al13O4(OH)24(H2O)12(SO4)4〕
Al- b(SO4)n+nBa(NO3)2n→Al- b(NO3)2n+nBaSO4
Isolate BaSO4Precipitating obtains: Al- b(NO3)2n→Alb→Al13
In addition, the process of existing preparation method due to producing usually as shown in Figure 1, still, during the preparation process, synthesize
Condition and mode it is different, as soon as especially compounded in the production of step material, controlled in production basicity condition have it is very big
Difference.From the point of view of the production technology of Japan, it is to generate sodium aluminate by aluminium hydroxide alkali soluble, then by CO2Gas acidification generates hydrogen
Aluminium oxide, then one section of material with dissolving with hydrochloric acid polymerization as aluminium polychloride, add sulfate radical SO2 -4, fundamental reaction formula are as follows:
Al(OH)3+Na OH→NaAl(OH)4
2NaAl(OH)4+CO2→Al(OH)3↓+Na2CO3+H2O
2Al(OH)3+(6-n)HCl→〔Al2(OH)n Cl6-n〕+(6-n)H2O
So this technique produces the basicity adjustability of a step material with regard to larger.And China directly uses gel aluminum hydroxide
It is reacted with hydrochloric acid, liquid material basicity can not be done up, and the excessive hydrolytic polymerization degree for causing formation mechanism of acidity is inadequate, condensate
Molecular weight do not increase yet, then be added SO4Root improves AL13The content of nanotechnology is just highly difficult in actual production.Japan
It is also to have any problem that basicity, which reaches 60% or more, when same One-step production polymeric aluminum.Therefore, day originally provides basicity
Between 45%-60%, and containing sulfate radicals are no more than 3.5%, and the degree of polymerization of product is improved with sulfate radical.It is in fact, sulfur-bearing
Acid group AL/SO4Theoretical value basicity the most suitable degree of polymerization should be had in 70%-75%.For this purpose, every country is in reality
In water treatment applications, all make every effort to be improved the PACS product basicity that a step produces.
1 Japan of table is compared with China's PACS technical standard
Compare from the technical standard of Japan and China, in high-purity PACS product, gap is very big for we.It alkalizes first
Degree is since production technology is different, and actual variance has 15%, and the difference of sulfate radical is just bigger, because the molten aluminium hydroxide of acid is done
Method, the sulfate of addition is not only without improving basicity, instead due to SO4Hydrogen ion concentration, which increases, in root makes high-purity PAC liquid
The decline of body basicity, so that basicity be made to can not improve, the simple polymeric molecular weight and molecular weight of hydroxy Al is used in water process
Middle available hydroxyl degree aluminium polymerization degree of hydrolysis is inadequate, affects the charge neutrality in colloid chemistry, the function such as catches, builds bridge, adsorbs in net
It can be not so good as the products such as the PACV of high basicity in body.For this purpose, domestic many factories are in SO-4Addition in Japanese technology, all
SO-4Radical content has been increased between 2.0%-3.0%, and PACS product has apparent improvement, but the raising of basicity is still
The project of one tackling key problem.Because it is equally known that Al/SO4Synthesis be condition that PACV aluminium salt cannot have nanometer technology,
So capturing Al/SO4Changing basicity is a very big technical problem.Therefore, for current PACS product both domestic and external
Nanoscale crystalline structure form, improve hydroxyl polymeric degree and change basicity and increase inorganic polymer amount, here it is current
The very difficult break-through point of water purification agent PACS product.
In view of the above-mentioned technological deficiency of the prior art, there is an urgent need to develop a kind of novel preparation method of PACS flocculant.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies of existing technologies, a kind of high-purity high basicity nanoscale PACS flocculant is provided
And preparation method thereof, PACS flocculant has nanoscale crystalline structure form, hydroxyl polymeric degree and basicity are significantly improved, from
And inorganic polymer amount is increased, there is extraordinary purifying water effect.
To achieve the goals above, the invention provides the following technical scheme: high-purity high basicity nanoscale PACS flocculant
Preparation method, which comprises the following steps:
(1), it generates one section of PAC material: the hydrochloric acid that aluminium hydroxide, water and acidity are 31% being added in reaction kettle and is carried out
Reaction, wherein the dosage of aluminium hydroxide is Al in control total reactant2O3Content is 13.5%-14.5%, and concentration is 31%
The dosage of hydrochloric acid is so that the acidity of total reactant is 16%, also, reaction pressure is made to be 0.2- during the reaction
0.25Mpa, reaction temperature are 125 DEG C -135 DEG C, the reaction time is 4 hours, and reaction terminates that one section of PAC material can be obtained;
(2), two sections of high-purity PAC materials are generated: one section of PAC material is placed in synthesis reactor, are 31% with acidity
Its acidity is adjusted to 8%-12% by hydrochloric acid, and calcium aluminate powder is added, and carries out synthesis under normal pressure, wherein the addition of the calcium aluminate powder
Amount is so that Al in total reactant2O3Content is 14.5%-15.5%, also, makes during synthesis under normal pressure the reaction temperature to be
105 DEG C -115 DEG C, reaction time 2-3h, are added Al after synthesis under normal pressure2(SO4)3·18H2O, the Al2(SO4)3·
18H2The additional amount of O is control SO-4Discharging standard be 2.5%-3.5%, two sections of high-purity PAC materials can be obtained;
(3), material level-one separates: being carried out instead with the high purity aluminum powder that purity is 99.9% to described two sections high-purity PAC materials
Should replace makes its deviate from micro ferro element, wherein and the reaction temperature for reacting displacement is 75 DEG C -90 DEG C, reaction time 1-2h, and
And vegetable active charcoal is added after reaction displacement and carries out physical absorption, wherein after physical absorption 15 minutes, to fluid temperature 75
Non ionic polymer auxiliary agent is added when between DEG C -90 DEG C and removes impurity, and is pumped into filter press filtering, obtains Al2O3Content is
15.5%-16.5%, basicity 65%-75%, SO-4For the high-purity Nano-class PAC material of 2.5%-3.5%;
(4), the second-order separation: the high-purity Nano-class PAC material after level-one filters pressing is subjected to curing precipitating 36h, is filled into later
Vegetable active charcoal carries out adsorption bleaching, and the adsorption bleaching time is 15 minutes, later, the material after adsorption bleaching is pumped into filter press
It is middle to carry out secondary filters pressing, obtain limpid bright high-purity high basicity nanoscale PACS flocculant.
Further, wherein the aluminium hydroxide in the step (1) is Al2O3The technical grade hydroxide that content is 65%
Aluminium.
Further, wherein the calcium aluminate powder in the step (2) adds calcium oxide to fire by aluminium oxide or aluminium hydroxide
It forms, and Al in the calcium aluminate powder2O3Content be 65-75%, the content of CaO is 25-35%.
Still further, wherein, the vegetable active charcoal is the high-purity vegetable active charcoal of coconut husk of 200 mesh.
Again further, wherein the dosage of the non ionic polymer auxiliary agent is 1.5 ‰, and its molecular weight is 1200
Ten thousand.
Furthermore, wherein the dosage for the high purity aluminum powder that the purity is 99.9% is the 1- of described two sections high-purity PAC materials
3%.
Further, wherein the dosage of the vegetable active charcoal in the step (3) is described two sections high-purity PAC materials
30-60%.
Further, wherein the dosage of the vegetable active charcoal in the step (4) is the high-purity Nano-class PAC object
The 20-50% of material.
In addition, the present invention also provides a kind of high-purity high basicity nanoscale PACS flocculants, characterized in that this is high-purity with high salt
Base degree nanoscale PACS flocculant is made with any of the above-described kind of preparation method.
Compared with existing preparation method, the side of high-purity high basicity nanoscale PACS flocculant of the invention and its preparation
Method has following advantageous effects: 1, which solve the hydroxyl polymeric degree of PACS product and the Upgrade Problems of basicity;2,
The high-quality PACS product that the degree of polymerization is good, basicity is high is arrived, to improve the application prospect of high-purity Nano-class PACS product.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of existing PACS flocculant of the invention.
Fig. 2 is the flow chart of the preparation method of high-purity high basicity nanoscale PACS flocculant of the invention.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples, and the content of embodiment is not as to guarantor of the invention
Protect the limitation of range.
Fig. 2 shows the flow charts of the preparation method of high-purity high basicity nanoscale PACS flocculant of the invention.Such as Fig. 1
It is shown, the preparation method of high-purity high basicity nanoscale PACS flocculant of the invention the following steps are included:
First, one section of PAC material is generated.
In the present invention, the hydrochloric acid that aluminium hydroxide, water and acidity are 31% is added in reaction kettle and is reacted.Its
In, the dosage of aluminium hydroxide is Al in control total reactant2O3Mass percentage is 13.5%-14.5%.Meanwhile concentration is
The dosage of 31% hydrochloric acid is so that the acidity of total reactant is 16%.Also, in the present invention, make during the reaction anti-
Answering pressure is 0.2-0.25Mpa, reaction temperature is 125 DEG C -135 DEG C, the reaction time is 4 hours.Reaction terminates to can be obtained one
Section PAC material.
In addition, in the present invention, hydrochloric acid must use the height that the acidity of pollution-free (heavy metal free, without organic matter) is 31%
Pure industrial synthesis hydrochloric acid.Also, the aluminium hydroxide is Al2O3The technical grade aluminium hydroxide that content is 65%.
Secondly, generating two sections of high-purity PAC materials.
In the present invention, one section of PAC material is placed in synthesis reactor, the hydrochloric acid for being 31% with acidity is by its acidity tune
To 8%-12%, and calcium aluminate powder is added, carries out synthesis under normal pressure.Wherein, the additional amount of the calcium aluminate powder is so that overall reaction
Al in object2O3Content is 14.5%-15.5%.Also, in the present invention, making reaction temperature during synthesis under normal pressure is 105
DEG C -115 DEG C, reaction time 2-3h.
In addition, in the present invention, Al is added after synthesis under normal pressure2(SO4)3·18H2O.The Al2(SO4)3·
18H2The additional amount of O is control SO-4Discharging standard be 2.5%-3.5%.Two sections of high-purity PAC materials can be obtained later.And
And the Al2(SO4)3·18H2O meets drinking water grade national standard.
It should be noted that in the present invention, the calcium aluminate powder by aluminium oxide or aluminium hydroxide add calcium oxide fire and
At, that is,
And Al in the calcium aluminate powder2O3Content be 65-75%, the content of CaO is 25-35%.Under normal conditions, institute
The ingredient for stating calcium aluminate powder is as shown in table 2 below:
The ingredient of 2 calcium aluminate powder of table
Composition | Al2O3 | CaO | SiO2 | F2O3 | TiO2 | MgO |
Content % | 65-75 | 25-35 | 0.02-0.05 | 0.001-0.0005 | 0.002-0.0005 | 0.002-0.0005 |
In the present invention, by the way that the liquor alumini chloridi of sulfate radical and the calcium aluminate powder progress acid of this sintering synthesis will be added
Change, catalysis, hydrolytic-polymeric reaction, improves the hydroxyl polymeric degree and basicity of PACS product.
Again, material level-one separates.
In the present invention, after generating two sections of high-purity PAC materials, need the high purity aluminum powder for being 99.9% with purity to described
Two sections of high-purity PAC materials, which carry out reaction displacement, makes it deviate from micro ferro element.Wherein, react displacement reaction temperature be 75 DEG C-
90 DEG C, reaction time 1-2h.Also, the dosage for the high purity aluminum powder that the purity is 99.9% is described two sections high-purity PAC objects
The 1-3% of material.
In addition, vegetable active charcoal, which is added, after reaction displacement carries out physical absorption.Wherein, after physical absorption 15 minutes, to
Non ionic polymer auxiliary agent is added when fluid temperature is between 75 DEG C -90 DEG C and removes impurity, and is pumped into filter press filtering, obtains
Al2O3Content is 15.5%-16.5%, basicity 65%-75%, SO-4For the high-purity Nano-class PAC object of 2.5%-3.5%
Material.
In the present invention, it is preferred to which the vegetable active charcoal is the high-purity vegetable active charcoal of coconut husk of 200 mesh.It is highly preferred that
The dosage of the vegetable active charcoal is the 30-60% of described two sections high-purity PAC materials.Moreover it is preferred that the nonionic high score
The dosage of sub- auxiliary agent is 1.5 ‰, and its molecular weight is 12,000,000.
Finally, carrying out the second-order separation.
The material that by-pass filtration is separated has the process of a slaking reaction, and it is heavy that the material of usual level-one filters pressing will cure
Shallow lake 36h, ultra-fine calcium sulphate crystal becomes larger precipitation in room temperature, normal pressure in liquid.Therefore, it is necessary to will be high-purity after level-one filters pressing
Nanoscale PAC material carries out curing precipitating 36h, fills into vegetable active charcoal later and carries out adsorption bleaching.Wherein, the adsorption bleaching
Time is 15 minutes.Later, the material after adsorption bleaching is pumped into filter press and carries out secondary filters pressing, obtain limpid bright height
Pure high basicity nanoscale PACS flocculant.
In the present invention, it is preferred to which the dosage of the vegetable active charcoal is the 20- of the high-purity Nano-class PAC material
50%.
Drink of high-purity high basicity PACS flocculant in different regions [acid soil] made from preparation method of the invention
With all having the characteristics that under the conditions of water, food, paper-making sizing, white water recycle, oil field waste etc., it is than high-purity PAC, PACS
Application range is wider, and it is the nanoscale high-end product on an advanced edge that treatment effect is more preferable, with high purity, dosage is few.
We have carried out comparative test with current domestic several representational products, it may be assumed that
The test medicine correlation data that table 3 is selected
Serial number | Name of product | Al2O3% | Basicity % | SO2‐ 4 % |
1 | PACV | 30.18 | 84 | ‐ |
2 | PAC (high-purity) | 29.41 | 43.2 | ‐ |
3 | PACS | 29.12 | 41.6 | 2.45 |
4 | Nanoscale PACS of the invention | 34 | 67 | 4.5 |
Experimental technique condition
Calculated in weight percent, 1ml contains 10mg/L, i.e. 10ppm.
[experiment one]
It takes Youjiang River river water to test, obtains the result such as the following table 4.
4 test data of table compares
[experiment two]
It is tested using raw water with mud, obtains the result such as the following table 5.
5 test data of table compares
Compared by test and market it is corresponding the result shows that, nanoscale PACS flocculant of the invention is in countries such as Southeast Asia
Using effect is very good in drinking water treatment.
In order to improve hydroxyl polymeric degree and the change of basicity of PACS product, aluminium chloride of the present invention addition sulfate radical
Solution and the novel calcium aluminate powder of special aluminium hydroxide sintering synthesis be acidified, be catalyzed, hydrolytic-polymeric reaction, then passes through one
Vegetalitas activity powdered carbon adsorbing separation is added after grade separation, and pluronic polymer is added, ultra-fine crystal of calcium sulfate body is complete
Separation removal, to obtain high-purity high basicity nanoscale PACS flocculant.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.Here all embodiments can not be exhaustive.It is all to belong to skill of the invention
The obvious changes or variations that art scheme is extended out are still in the scope of protection of the present invention.
Claims (7)
1. a kind of preparation method of high-purity high basicity nanoscale PACS flocculant, which comprises the following steps:
(1), it generates one section of PAC material: the hydrochloric acid that aluminium hydroxide, water and concentration are 31% being added in reaction kettle and is carried out instead
It answers, wherein the dosage of aluminium hydroxide is Al in control total reactant2O3Content is 13.5%-14.5%, the salt that concentration is 31%
The dosage of acid is so that the acidity of total reactant is 16%, also, reaction pressure is made to be 0.2- during the reaction
0.25Mpa, reaction temperature are 125 DEG C -135 DEG C, the reaction time is 4 hours, and reaction terminates that one section of PAC material can be obtained;
(2), two sections of high-purity PAC materials are generated: one section of PAC material is placed in synthesis reactor, the hydrochloric acid for being 31% with concentration
Its concentration is adjusted to 8%-12%, and calcium aluminate powder is added, carries out synthesis under normal pressure, wherein the additional amount of the calcium aluminate powder is
So that Al in total reactant2O3Content is 14.5%-15.5%, also, makes reaction temperature be 105 during synthesis under normal pressure
DEG C -115 DEG C, reaction time 2-3h, are added Al after synthesis under normal pressure2(SO4)3·18H2O, the Al2(SO4)3·
18H2The additional amount of O is control SO4 -2Discharging standard be 2.5%-3.5%, two sections of high-purity PAC materials can be obtained;
(3), material level-one separates: the high purity aluminum powder for being 99.9% with purity carries out reaction to described two sections high-purity PAC materials and sets
Changing makes its deviate from micro ferro element, wherein and the reaction temperature for reacting displacement is 75 DEG C -90 DEG C, reaction time 1-2h, and
Reaction displacement after be added vegetable active charcoal carry out physical absorption, wherein after physical absorption 15 minutes, to fluid temperature 75 DEG C-
Non ionic polymer auxiliary agent is added when between 90 DEG C and removes impurity, and is pumped into filter press filtering, obtains Al2O3Content is 15.5%-
16.5%, basicity 65%-75%, SO4 -2For the high-purity Nano-class PAC material of 2.5%-3.5%;
(4), the second-order separation: the high-purity Nano-class PAC material after level-one filters pressing is subjected to curing precipitating 36h, fills into plant later
Active carbon carry out adsorption bleaching, the adsorption bleaching time be 15 minutes, later, by after adsorption bleaching material be pumped into filter press in into
The secondary filters pressing of row, obtains limpid bright high-purity high basicity nanoscale PACS flocculant.
2. the preparation method of high-purity high basicity nanoscale PACS flocculant according to claim 1, characterized in that described
Aluminium hydroxide in step (1) is Al2O3The technical grade aluminium hydroxide that content is 65%.
3. the preparation method of high-purity high basicity nanoscale PACS flocculant according to claim 2, characterized in that described
Calcium aluminate powder in step (2) adds calcium oxide to fire by aluminium oxide or aluminium hydroxide, and Al in the calcium aluminate powder2O3's
Content is 65-75%, and the content of CaO is 25-35%.
4. the preparation method of high-purity high basicity nanoscale PACS flocculant according to claim 3, characterized in that described
Vegetable active charcoal is the high-purity vegetable active charcoal of coconut husk of 200 mesh.
5. the preparation method of high-purity high basicity nanoscale PACS flocculant according to claim 4, characterized in that described
The dosage for the high purity aluminum powder that purity is 99.9% is the 1-3% of described two sections high-purity PAC materials.
6. the preparation method of high-purity high basicity nanoscale PACS flocculant according to claim 5, characterized in that described
The dosage of vegetable active charcoal in step (3) is the 30-60% of described two sections high-purity PAC materials.
7. the preparation method of high-purity high basicity nanoscale PACS flocculant according to claim 6, characterized in that described
The dosage of vegetable active charcoal in step (4) is the 20-50% of the high-purity Nano-class PAC material.
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CN107628631B (en) * | 2017-08-31 | 2019-09-13 | 四川齐力绿源水处理科技有限公司 | A kind of aluminium polychloride preparation method |
CN107487826B (en) * | 2017-09-20 | 2020-10-20 | 北京美斯顿科技开发有限公司 | Composite coagulant for treating flue gas desulfurization waste liquid and preparation method and application thereof |
CN111115781A (en) * | 2020-01-05 | 2020-05-08 | 广东佰国环保科技有限公司 | Production method of high-salinity high-sulfate polyaluminium chloride sulfate |
CN111747435B (en) * | 2020-07-08 | 2022-10-25 | 宁夏蓝田农业开发有限公司 | Method for preparing flocculant by oxadiargyl byproduct |
CN114195176B (en) * | 2021-10-28 | 2024-02-06 | 广州市芦苇环保科技有限责任公司 | Preparation process of polyaluminum chloride water purifying agent |
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