KR101612513B1 - Method for preparing polyaliminium chloride-based inorganic coagulants having high basicity - Google Patents
Method for preparing polyaliminium chloride-based inorganic coagulants having high basicity Download PDFInfo
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- KR101612513B1 KR101612513B1 KR1020150085868A KR20150085868A KR101612513B1 KR 101612513 B1 KR101612513 B1 KR 101612513B1 KR 1020150085868 A KR1020150085868 A KR 1020150085868A KR 20150085868 A KR20150085868 A KR 20150085868A KR 101612513 B1 KR101612513 B1 KR 101612513B1
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/01—Separation of suspended solid particles from liquids by sedimentation using flocculating 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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- Engineering & Computer Science (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
The present invention relates to a method for producing a high salt-free polychlorinated aluminum-based inorganic coagulant using a rare earth metal.
The aluminum-based coagulant for water treatment includes aluminum sulfate (Alum), poly aluminum chloride (PAC), polyaluminum chloride silicate (PACS), polyaluminum sulphate Silicate: PASS) have been mainly used.
Aluminum sulfate is advantageous in that it is inexpensive as a mono-molecular coagulant, but has a disadvantage in that the coagulation effect is lower than that of the polymer flocculant and the alkalinity and pH of the treated water are significantly lowered after the treatment.
In order to overcome such disadvantages, there has been developed an inorganic polymer flocculant such as PAC, PACS and PASS which is a polymer type. In the case of the inorganic flocculant, there is an advantage that the cohesive force is significantly larger than that of a single molecule of aluminum sulfate, which has a charge amount of positive ions of +7 to +3. In addition, they usually have a basicity of at least 40%.
Among them, poly (aluminum chloride) (PAC) has conventionally been used mainly as a coagulant for water treatment. Especially, it has been mainly used as a flocculant for flocculating huge molecules in water treatment, and thus various techniques for securing a basicity of 45% or more have been proposed.
The basicity is expressed by the following formula 1 as a ratio of the number of OH to the number of Al metal present in the flocculant unit molecule.
[Formula 1]
Basicity (%) = [(number of [OH]) / (number of 3 × [Al])] × 100
In general, as the basicity increases, the molecular weight of the coagulated component increases, so the precipitation performance improves and the amount of calcium hydroxide and caustic soda after the water treatment is reduced. On the other hand, the increase of the basicity There was a limit.
Korean Patent Publication No. 1999-0049511 and Korean Patent No. 0858633 disclose a method of reacting aluminum hydroxide with hydrochloric acid to produce an intermediate compound and to increase the basicity lowered by hydrochloric acid, sodium carbonate, sodium bicarbonate, calcium bicarbonate And a technique of increasing the basicity by using an alkali salt is proposed.
In this technology, a technology capable of increasing the basicity to 80% is proposed, but carbon dioxide gas (CO 2 ) is generated and the structure of the polychlorinated aluminum becomes weak, and the structure of the poly Aluminum (Al (OH) 3 ) precipitates are produced, and the stability of the product is low, and the use of an excessive amount of an alkali salt causes a problem of increased manufacturing cost.
Korean Patent No. 0733286 discloses a method for securing a long-term storage stability for 6 months or longer by using sodium aluminate prepared by reacting aluminum hydroxide with caustic soda to a low-salt airway PAC compound prepared by reacting aluminum hydroxide with hydrochloric acid NaAl (OH) 4 ) is used as an inorganic coagulant.
This technique prevents the precipitation of Al (OH) 3 by reacting in a homogenization reactor by diluting the sodium aluminate concentration to increase the reactivity of the coagulant and sodium aluminate in the low-salt airway. To stabilize the polymer coagulant, It has been disclosed that an inorganic coagulant having 60% or more of high salt resistance without formation of precipitation can be produced even if it is stored for 6 months or more by stabilizing reaction at a constant stirring rate for a certain period of time. However, the sodium aluminate used in the method has poor self-storage stability, and thus has a problem that it is hard to cure or decompose when stored for 6 months or longer.
Korean Patent No. 10-1374191 discloses a method of using sodium aluminum silicate as a high-baseifying agent. However, in the above method, sodium aluminum silicate is mixed at 20 to 80 ° C for 1 to 10 hours and stabilized at 40 to 100 ° C for 1 to 15 hours during the process, so that the manufacturing process takes too long.
Therefore, it is necessary to develop an inorganic coagulant for water treatment, which has a high salt resistance and excellent storage stability and which is excellent in the stability of materials used in the production of coagulant.
The present invention has been developed in consideration of the circumstances of the prior art as described above, and it is possible to obtain a highly salt-free air by using a relatively small amount of a high basicity agent in the production of a highly chlorinated aluminum chloride (PAC) inorganic coagulant It is a highly salt-resistant, polychlorinated aluminum type inorganic flocculant obtained from natural rare earths. It has good flocculation efficiency and does not precipitate even at long-term storage under normal temperature and normal pressure conditions. It has excellent storage stability and does not harden or decompose even during long- The present invention provides a method for producing a highly salt-resistant polychlorinated aluminum-based inorganic coagulant.
The present invention relates to a process for the production of a sulfide ion (SO 4 2- ) in which the concentration of sulfate ion (SO 4 2- ) is from 50 to 80% by weight, based on 100 parts by weight of low salt polychlorinated aluminum having a basicity of 10 to 45% and an Al 2 O 3 concentration of 5 to 25 % Phosphorus sulfate at a ratio of 1 to 20 parts by weight; And
A second step of reacting 100 weight parts of the reaction product of the first step with 0.1 to 10 weight parts of rare earth at a concentration of 50 to 90% to prepare aged poly (aluminum chloride) having a basicity of 50 to 70%;
Based inorganic coagulant. ≪ RTI ID = 0.0 > A < / RTI >
The rare earth metal may be a compound represented by the following general formula (1).
[Chemical Formula 1]
Re (OH) 3
(Re in the above formula (1) is La, Ce, Nd or Sm)
In addition, the rare earths may have a size of 0.1 to 10 탆 in size.
The first step is preferably performed at 20 to 60 ° C for 1 to 5 hours. The second step is preferably performed at a temperature of 20 to 60 ° C for 0.5 to 7 hours.
In addition, the low-salt polychlorinated aluminum is prepared by the reaction of aluminum hydroxide with hydrochloric acid.
In the second step, aging may be carried out at 30 to 60 ° C for 1 to 5 hours.
The sulfate CaSO 4, MgSO 4, FeSO 4 , ZnSO 4 And K 2 SO 4 may be used.
The characteristics and advantages of the method for producing a highly salt-resistant polychlorinated aluminum flocculant for water treatment according to the present invention will be described below.
First, the present invention can effectively produce a polychlorinated aluminum (PAC) -based inorganic flocculant of high salt resistance even if only a relatively small amount of rare earth, which is a natural mineral used as a high base stabilizing agent, can be effectively produced, Stability is also excellent.
Further, the polychlorinated aluminum-based inorganic flocculant of the present invention can easily increase the basicity because the sulfate is used before using the rare earth.
The terminology used herein is for the purpose of describing exemplary embodiments only and is not intended to be limiting of the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, the terms "comprises, " or" having ", and the like, are intended to specify the presence of stated features, integers, Components, or combinations thereof, as a matter of convenience, without departing from the spirit and scope of the invention.
In addition, the present invention can be variously modified and can take various forms, so that specific embodiments are exemplified and will be described in detail below. It should be understood, however, that the invention is not intended to be limited to the particular forms disclosed, but includes all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Hereinafter, the present invention will be described in detail.
According to one embodiment of the present invention, sulfate ion (SO 4 2 -) is added based on 100 parts by weight of low salt polychlorinated aluminum having a basicity of 10 to 45% and an Al 2 O 3 concentration of 5 to 25 (W / V% ) In a ratio of 1 to 20 parts by weight of a sulfate having a concentration of 50 to 80%; And a second step of reacting 100 parts by weight of the reaction product of the first step with 0.1 to 10 parts by weight of rare earth at a concentration of 50 to 90% to prepare aged poly (aluminum chloride) having a basicity of 50 to 70% There is provided a method for producing a high salt-free polychlorinated aluminum-based inorganic coagulant.
More particularly, the present invention relates to a method for producing a high salt-free polychlorinated aluminum-based inorganic coagulant which has excellent storage stability and exhibits a high salt resistance and exhibits high flocculation efficiency and low manufacturing cost during water treatment.
The coagulant of high salt air permeability can not be made of aluminum salt in polymer state, it has a large amount of Al (OH) 2 + ions in the product and easily forms a precipitate in the form of Al (OH) 3 and becomes unstable. This precipitation phenomenon is a fundamental problem of the highly salt-resistant polychlorinated aluminum-based inorganic coagulant. Most of the products developed or marketed so far have a short life span of the product since precipitation occurs after about 3 to 4 months.
In addition, even if stability is maintained, it has disadvantages such as storage stability of raw materials and complicated manufacturing process.
Accordingly, in order to solve such a problem, the present invention provides a polychlorinated aluminum-based inorganic coagulant which is highly salt-resistant by using a novel high-baseifying agent, thereby maintaining high coagulation efficiency and ensuring long-term storage stability for 6 months or longer, Manufacturing time can be reduced and manufacturing costs can be reduced.
The present inventors have found that poly (aluminum chloride) having a high salt resistance of 50% or more and more than 60% can be effectively obtained by reacting a poly (aluminum chloride) with a low salt and a novel high basicity agent, It has been found that highly salt-resistant polyaluminum chloride (PAC) is excellent in flocculation efficiency and stability, and thus the present invention has been completed.
Hereinafter, the method for producing the polychlorinated aluminum-based inorganic coagulant according to the present invention will be described in detail for each step.
The polychlorinated aluminum-based inorganic flocculant of the present invention comprises the first step and the second step. Further, the first step proceeds according to Reaction Scheme 1, and the second step proceeds according to Reaction Scheme 2.
[Reaction Scheme 1]
2Al (OH) 3 + HCl + MSO 4 → [Al 2 (OH) n Cl 6-n and M] + m + SO 4 2 -
[Reaction Scheme 2]
[Al 2 (OH) nCl 6 -n and M] + m + Re (OH ) 3 → [Al 2 (OH) n Cl 6- n ReOH] + (MOH) +
(Wherein M is Ca, Mg, Fe, Zn, or K, Re is La, Ce, Nd or Sm as a rare earth metal, m is 1? M? 10, n is 1? N ≪ / RTI >
Specifically, in the present invention, the amount of sulfate ion (SO 4 2- ) (based on 100 parts by weight of low salt polychlorinated aluminum having a basicity of 10 to 45% and an Al 2 O 3 concentration of 5 to 25 (W / V% And 1 to 20 parts by weight of a sulfate having a concentration of 50 to 80%.
According to Scheme 1 set forth a bar, the first step using the sulfate low salt airway poly aluminum chloride ([Al 2 (OH) n Cl 6-n] m) to increase the basicity of which is used in the second step to be described later rare earth The cohesion and the stability can be easily increased.
The method for producing the low-salt polychlorinated aluminum is not limited to a specific method, and can be carried out according to a method well known in the art. According to one preferred embodiment, the low-salt polychlorinated aluminum may be prepared by the reaction of aluminum hydroxide (Al (OH) 3 ) with hydrochloric acid. The hydrochloric acid may be 15-35% hydrochloric acid (HCl).
Further, in the present invention, it is more preferable that the low-salt poly-aluminum chloride has an Al 2 O 3 concentration of 5 to 25 (W / V%).
The sulfate may be selected from the group consisting of CaSO 4 , MgSO 4 , FeSO 4 , ZnSO 4 and K 2 SO 4 , which may be in powder form. If the amount of the sulfate powder is less than 1 part by weight, there is a problem in increasing the basicity. If the amount is more than 20 parts by weight, the stability is lowered and precipitation occurs.
In the first step, the reaction between the low-salt polychloride aluminum salt and the sulfate salt is preferably performed at 20 to 60 ° C for 1 to 5 hours. In the above reaction, if the temperature is 20 ° C or lower, dissolution is difficult, and at 60 ° C or higher, the energy cost increases and the economical efficiency deteriorates.
At this time, since the reaction in the first step is a reaction between strong acid and strong alkali, it is preferable to use a homogenization reactor having a high-speed stirring blade to prevent precipitation from being generated rapidly by acid-alkali reaction. Specifically, it is preferable to carry out the homogenization reactor maintained at a stirring speed of 200 to 5,000 rpm.
In addition, in the first step, the reaction product produced by the reaction of the low-salt aluminum chloride with the sulfate may represent an aqueous phase.
Next, in the present invention, 0.1 to 10 parts by weight of rare earths at a concentration of 50 to 90% is reacted with 100 parts by weight of the reaction product of the first step to produce aged polychlorinated aluminum having a basicity of 50 to 70% .
Specifically, as shown in Scheme 2, the second step is a step of improving the storage stability of the highly-salt-resistant polychlorinated aluminum compound prepared in the first step by using a specific high-baseifying agent.
That is, in the present invention, a predetermined amount of rare earth, which is a natural mineral, which is a highly basicizing agent, is added to the reaction product (aqueous liquid phase) of the first step.
At this time, rare earths, which are natural minerals used as high base stabilizers, are chemically very stable, they are resistant to dry air and have good heat conduction characteristics and have a feature of precipitating and treating fluorine. In addition, the rare earths can be easily prepared and stored when used as a highly basic agent.
Preferably, the rare earth metal according to the present invention may be a compound represented by the following formula (1), which is easy to purchase and low in cost.
[Chemical Formula 1]
Re (OH) 3
(Re in the above formula (1) is La, Ce, Nd or Sm)
Preferably, the rare earths used in the process for producing high salt resistance polychlorinated aluminum are powders, and those having a size in the range of 0.1 to 10.0 μm are preferably used.
In addition, the rare earths used in the highly salt-resistant polychlorinated aluminum serve as a good coagulation assistant, and thus, a large effect can be obtained even with a small amount of the filler.
Preferably, the above-mentioned rare earth having a concentration of 50 to 90% is used in an amount of 0.1 to 10 parts by weight based on 100 parts by weight of the reaction product (that is, highly salt-resistant polychlorinated aluminum) in the aqueous phase of the first step as described above, 1 to 5 parts by weight. If the amount is less than 0.1 parts by weight, the coagulation efficiency is lowered. If the amount is more than 10 parts by weight, the stability may be lowered and precipitation may occur.
Also, in the present invention, it is preferable that the rare earth and the reaction product of the first stage are reacted at a temperature of 20 to 60 ° C for 0.5 to 7 hours. In the above reaction, dissolution is difficult at a temperature of 20 ° C or lower, and energy cost increases at 60 ° C or higher, resulting in poor economics.
According to the present invention, in order to ensure the stability of the highly salt-resistant polychlorinated aluminum to be produced, it is preferable to include a step of adding a dilute solution in the second step and then aging at 30 to 60 ° C for 1 to 5 hours . At this time, if the above-mentioned condition is not aged, the storage stability at a low temperature such as a winter season may be lowered.
The polychlorinated aluminum flocculant of the present invention obtained by such a method is a highly salt-resistant polychlorinated aluminum (PAC) flocculant having a Al 2 O 3 concentration of 5 to 20 (W / V%) and a basicity of 50 to 80% And the long-term storage stability is also excellent.
That is, the present invention provides a method for efficiently obtaining a highly salt-resistant polychlorinated aluminum-based flocculant having a basicity of 50% or more, more preferably 60% or more, even when a relatively small amount of a high-baseifying agent is used.
In particular, according to the present invention, a coagulant can be chemically and stably produced using rare earths, which are natural minerals, as a highly basic agent for reacting with a low-salt PAC to improve storage stability.
Therefore, the highly salt-resistant polychlorinated aluminum-based inorganic coagulant of the present invention produced by the method of the present invention can secure coagulation efficiency, coagulation stability and long-term storage stability at the same time.
Best Mode for Carrying Out the Invention Hereinafter, the function and effect of the present invention will be described in more detail through a specific embodiment of the present invention. It is to be understood, however, that these embodiments are merely illustrative of the invention and are not intended to limit the scope of the invention.
< Example 1>
258 g of aluminum hydroxide (Al (OH) 3 ) and 714 ml of 35% hydrochloric acid were mixed and stirred for 6 hours at a temperature of 160 캜 and a pressure of 3 kgf / cm 2 to prepare low-salt polyaluminum chloride. The basicity of the low-salt polychlorinated aluminum prepared above was 40%, and the Al 2 O 3 concentration was 17 (W / V%).
Then, 10 g of CaSO 4 having a sulfuric acid ion (SO 4 2- ) concentration of 65% was added to 100 g of the low-salt polychlorinated aluminum salt which had been naturally cooled and reacted at 25 ° C. and 1 atm pressure for 1 hour. Then, 6 g of La (OH) 3 (powder size: 5 탆) having a concentration of 60% was added to 110 g of the reaction product, and the mixture was reacted at 25 캜 for 1 hour.
As a result, it was confirmed that the basicity after aging was 60%, and the production of polychlorinated aluminum having an Al 2 O 3 concentration of 14.6 (W / V%) was confirmed.
< Example 2>
High salt-resistance polychlorinated aluminum was prepared in the same manner as in Example 1 except that Ce (OH) 3 having a concentration of 60% was used instead of La (OH) 3 as a rare earth.
< Example 3>
High salt resistance polychlorinated aluminum was prepared in the same manner as in Example 1 except that Nd (OH) 3 having a concentration of 60% was used instead of La (OH) 3 as a rare earth.
<Example 4>
High salt resistance poly (aluminum chloride) was prepared in the same manner as in Example 1 except that Sm (OH) 3 having a concentration of 60% was used instead of La (OH) 3 as a rare earth.
< Comparative Example 1>
Highly salt-resistant polyaluminum chloride was prepared in the same manner as in Example 1 except that NaOH was used instead of rare earth.
< Comparative Example 2>
High salt-resistance polyaluminum chloride was prepared in the same manner as in Example 1, except that sodium aluminate (NaAl (OH) 4 ) was used instead of rare earth.
< Experimental Example >
Physical property test
For Examples 1 to 4 and Comparative Examples 1 and 2, the performance as a coagulant for wastewater treatment was evaluated, and the results are shown in Table 1.
At this time, the raw water used in the experiment was a desulfurization wastewater of thermal power plant.
Further, after using the examples and the comparative examples as flocculants, the supernatant of the treated water was taken and the turbidity was measured by a pH meter and a turbidimeter (HACH-DR / 890) by a conventional method.
The alkalinity was also measured by the KS I ISO9963-2 method.
(mg / L)
From Table 1, it can be seen that Examples 1 to 4 of the present invention have higher alkalinity of the treated water and particularly improved turbidity, compared with Comparative Examples 1 and 2.
While the present invention has been particularly shown and described with reference to specific embodiments thereof, those skilled in the art will appreciate that such specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereby. something to do. It is therefore intended that the scope of the invention be defined by the claims appended hereto and their equivalents.
Claims (8)
And a second step of reacting 100 parts by weight of the reaction product of the first step with 0.1 to 10 parts by weight of rare earth at a concentration of 50 to 90% to prepare aged poly (aluminum chloride) having a basicity of 50 to 70% In addition,
Wherein the rare earth metal is a compound represented by the following general formula (1).
[Chemical Formula 1]
Re (OH) 3
(Re in the above formula (1) is La, Ce, Nd or Sm)
Wherein the low-salt polychlorinated aluminum is produced by the reaction of aluminum hydroxide with hydrochloric acid.
The sulfate CaSO 4, MgSO 4, FeSO 4 , ZnSO 4 And K 2 SO 4 is used as the inorganic coagulant.
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Cited By (4)
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KR101752276B1 (en) | 2017-03-31 | 2017-06-29 | 주식회사 홍원산업 | Preparing method of poly aluminum chloride inorganic coagulant with low basicity for waste water treatment and purification method of waste water using the inorganic coagulant prepared by the same |
KR20200038054A (en) * | 2018-10-02 | 2020-04-10 | 주식회사 유니테크 | Method for preparing poly aluminium chloride-based coagulants |
KR102291774B1 (en) * | 2021-04-14 | 2021-08-24 | 미주엔비켐 주식회사 | Manufacturing method of polyaluminum chloride coagulant with a concentration of 17% aluminum oxide |
CN117699934A (en) * | 2024-02-06 | 2024-03-15 | 克拉玛依市弘智油田技术服务有限公司 | Water purifying agent and preparation method thereof |
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JP2546818B2 (en) | 1993-06-23 | 1996-10-23 | 東信化学工業株式会社 | Water treatment coagulant for cold water and method for purifying cold water using the same |
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KR101752276B1 (en) | 2017-03-31 | 2017-06-29 | 주식회사 홍원산업 | Preparing method of poly aluminum chloride inorganic coagulant with low basicity for waste water treatment and purification method of waste water using the inorganic coagulant prepared by the same |
KR20200038054A (en) * | 2018-10-02 | 2020-04-10 | 주식회사 유니테크 | Method for preparing poly aluminium chloride-based coagulants |
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KR102291774B1 (en) * | 2021-04-14 | 2021-08-24 | 미주엔비켐 주식회사 | Manufacturing method of polyaluminum chloride coagulant with a concentration of 17% aluminum oxide |
CN117699934A (en) * | 2024-02-06 | 2024-03-15 | 克拉玛依市弘智油田技术服务有限公司 | Water purifying agent and preparation method thereof |
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