JP2000226213A - Production of aluminum polysulfate - Google Patents
Production of aluminum polysulfateInfo
- Publication number
- JP2000226213A JP2000226213A JP11026287A JP2628799A JP2000226213A JP 2000226213 A JP2000226213 A JP 2000226213A JP 11026287 A JP11026287 A JP 11026287A JP 2628799 A JP2628799 A JP 2628799A JP 2000226213 A JP2000226213 A JP 2000226213A
- Authority
- JP
- Japan
- Prior art keywords
- aluminum
- aluminum hydroxide
- reaction
- polysulfate
- sulfate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 229910001679 gibbsite Inorganic materials 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 230000003311 flocculating effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 10
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 230000015271 coagulation Effects 0.000 description 4
- 238000005345 coagulation Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 102100033007 Carbonic anhydrase 14 Human genes 0.000 description 3
- 101000867862 Homo sapiens Carbonic anhydrase 14 Proteins 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は凝集剤として有用な
ポリ塩化アルミニウムに添加して、その凝集性能を向上
させるポリ硫酸アルミニウムの製造方法に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing polyaluminum sulfate which is added to polyaluminum chloride useful as a coagulant to improve the coagulation performance.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】ポリ塩
化アルミニウムは浄水用、汚水用等の凝集剤として多量
に使用されている。ポリ塩化アルミニウムに硫酸根を含
有させると凝集性能が向上することはよく知られてお
り、ＪＩＳ：Ｋ−１４７５（水道用ポリ塩化アルミニウ
ム）では硫酸根を3.5 ％以下と規定している。硫酸根源
としては硫酸ナトリウム、硫酸カリウム、硫酸アルミニ
ウム、硫酸マグネシウム、硫酸第一鉄、硫酸第二鉄、硫
酸亜鉛等のいろいろな硫酸塩が提案されている。またポ
リ硫酸アルミニウム（ＰＡＳ）をポリ塩化アルミニウム
（ＰＡＣ）に添加、混合すると凝集性能が向上するとい
う報告がある（特公昭４７−１９２４２号公報）。ポリ
硫酸アルミニウムは一般式[Al2(OH)n(SO4)3-2/n] で表
され、その製造方法については、例えば特公昭４５−４
９号公報に記載されている。この方法は炭酸ガスまたは
亜硫酸ガスの加圧ガス気流中にアルミン酸アルカリ液を
循環噴霧し、微細な水酸化アルミニウムを析出させ（こ
のとき、反応系を水冷し温度を30℃以下に保つ）、析出
した水酸化アルミニウムを濾過、水洗し、回収した後、
硫酸または硫酸アルミニウムに50〜80℃で加熱攪拌反応
せしめてポリ硫酸アルミニウムを製造するものである。
しかし、この方法は工程が長く操作が煩雑であり、また
冷却したり加熱したりするため熱エネルギーを多量に使
用し、さらには原料に使用するアルミン酸アルカリは比
較的高価であり、製品が高価になるという問題がある。
一方、水酸化アルミニウムの結晶は、その結晶系の違い
により、ダイヤスポア、ベーマイト、ハイドラジライト
（ギブサイト）、バイヤーライト等があり、工業的に安
価に入手できるのはハイドラジライト系（ギブサイト）
であるが、ハイドラジライト系の水酸化アルミニウムは
酸には溶け難く、僅かに熱濃硫酸に正塩の化学当量まで
溶解するが塩基性にはならないとされていた。2. Description of the Related Art Polyaluminum chloride is used in large quantities as a coagulant for water purification and sewage. It is well known that the addition of sulfate to polyaluminum chloride improves coagulation performance, and JIS: K-1475 (polyaluminum chloride for water supply) specifies that the sulfate is 3.5% or less. Various sulfates such as sodium sulfate, potassium sulfate, aluminum sulfate, magnesium sulfate, ferrous sulfate, ferric sulfate, and zinc sulfate have been proposed as sulfate sources. There is also a report that adding and mixing aluminum polysulfate (PAS) to aluminum polychloride (PAC) improves the coagulation performance (Japanese Patent Publication No. 47-19242). Aluminum polysulfate is represented by the general formula [Al 2 (OH) n (SO 4 ) 3 -2 / n ].
No. 9 is described. In this method, an alkali aluminate solution is circulated and sprayed into a pressurized gas stream of carbon dioxide gas or sulfurous acid gas to precipitate fine aluminum hydroxide (at this time, the reaction system is cooled with water and the temperature is kept at 30 ° C. or less). The precipitated aluminum hydroxide was filtered, washed with water and collected,
It reacts with sulfuric acid or aluminum sulfate under heating and stirring at 50 to 80 ° C to produce polyaluminum sulfate.
However, this method requires a long process and complicated operation, uses a large amount of heat energy for cooling and heating, and furthermore, the alkali aluminate used for the raw material is relatively expensive, and the product is expensive. Problem.
On the other hand, crystals of aluminum hydroxide include diamond spores, boehmite, hydrazirite (gibbsite), and bayerite, etc., depending on the crystal system.
However, hydrazirite-based aluminum hydroxide is hardly soluble in acids, and slightly soluble in hot concentrated sulfuric acid up to the chemical equivalent of a normal salt, but is not considered basic.
【０００３】[0003]
【課題を解決するための手段】本発明者らは、ハイドラ
ジライト系の水酸化アルミニウムと硫酸を反応させて硫
酸アルミニウム溶液を得る方法を鋭意検討した結果、反
応条件によっては、硫酸アルミニウムが塩基性になるこ
とを認め、工業製品として安価に使用できるハイドラジ
ライト系結晶性水酸化アルミニウムと硫酸とを原料にし
て、ポリ硫酸アルミニウムを製造し得ることを見出し
た。即ち、本発明は水酸化アルミニウムと硫酸を反応さ
せてポリ硫酸アルミニウムを製造する方法において、水
酸化アルミニウムとしてハイドラジライト系結晶性水酸
化アルミニウムを使用し、且つ反応温度100 〜140 ℃の
範囲で反応を行うことを特徴とするポリ硫酸アルミニウ
ムの製造方法である。Means for Solving the Problems The present inventors have conducted intensive studies on a method of reacting hydrazirite-based aluminum hydroxide with sulfuric acid to obtain an aluminum sulfate solution. It has been found that polyhydric aluminum sulfate can be produced using hydrazilite-based crystalline aluminum hydroxide and sulfuric acid, which can be used at low cost as industrial products, as raw materials. That is, the present invention relates to a method for producing aluminum polysulfate by reacting aluminum hydroxide and sulfuric acid, wherein a hydrazirite-type crystalline aluminum hydroxide is used as the aluminum hydroxide and the reaction temperature is in the range of 100 to 140 ° C. A method for producing aluminum polysulfate, comprising performing a reaction.
【０００４】[0004]
【発明の実施の形態】以下、本発明を詳細に説明する。
本発明では、反応温度100 〜140 ℃で反応を行うことを
特徴とする。100 ℃未満では水酸化アルミニウムと硫酸
の反応は正塩までしか生成せず塩基性にはならないた
め、本発明の目的とするポリ硫酸アルミニウムは得られ
ない。また、140℃を越えると、一旦生成したポリ硫酸
アルミニウムが加水分解を起こし、微細な水酸化アルミ
ニウムが生成する。この微細な水酸化アルミニウムは濾
過回収し硫酸に溶解するとポリ硫酸アルミニウムとなる
が、生成した水酸化アルミニウムが微細なことにより、
濾過作業に多大の労力を要する。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
The present invention is characterized in that the reaction is carried out at a reaction temperature of 100 to 140 ° C. If the temperature is lower than 100 ° C., the reaction between aluminum hydroxide and sulfuric acid forms only a normal salt and does not become basic, so that the polyaluminum sulfate intended in the present invention cannot be obtained. On the other hand, when the temperature exceeds 140 ° C., the once produced aluminum polysulfate is hydrolyzed to produce fine aluminum hydroxide. When this fine aluminum hydroxide is collected by filtration and dissolved in sulfuric acid, it becomes polyaluminum sulfate, but due to the fine aluminum hydroxide produced,
A great deal of labor is required for the filtering operation.
【０００５】本発明では、反応圧力0.05〜1.0MPaの範囲
で反応を行うことが好ましい。この場合、本発明に使用
する反応器は耐酸耐圧製であるのがよく、また反応は密
閉状態で行うのがよい。水酸化アルミニウムと硫酸を反
応器に入れ、密閉状態にし、100 ℃に加熱すると圧力は
0.05MPa 以上になる。この状態で反応を行うと本発明の
ポリ硫酸アルミニウムが得られる。反応器を密閉状態に
しないで、大気圧下で反応を行うと、硫酸アルミニウム
は正塩までにしかならず、本発明のポリ硫酸アルミニウ
ムは得られない。反応圧力は1.0MPa以下で行うのが望ま
しい。現在、工業的に使用可能な耐酸耐圧製の反応器の
材質はグラスライニングであり、このものの耐圧力はあ
まり高くない。従って、現実的には1.0MPa以下で反応を
行うのが好ましい。In the present invention, it is preferable to carry out the reaction at a reaction pressure of 0.05 to 1.0 MPa. In this case, the reactor used in the present invention is preferably made of acid and pressure resistant, and the reaction is preferably carried out in a closed state. When aluminum hydroxide and sulfuric acid are put into a reactor, sealed, and heated to 100 ° C, the pressure becomes
It becomes 0.05MPa or more. When the reaction is performed in this state, the polyaluminum sulfate of the present invention is obtained. If the reaction is carried out at atmospheric pressure without keeping the reactor closed, aluminum sulfate can only be converted to a normal salt, and the polyaluminum sulfate of the present invention cannot be obtained. The reaction pressure is desirably 1.0 MPa or less. At present, the material of the acid-proof and pressure-resistant reactor that can be used industrially is glass lining, which is not very high in pressure resistance. Therefore, it is practically preferable to carry out the reaction at 1.0 MPa or less.
【０００６】上記反応の反応時間は、反応温度、使用す
る水酸化アルミニウムの含水率、平均粒子径、粒度分布
あるいは硫酸濃度によりかわるが、概ね１〜８時間の範
囲で行うのが望ましい。また、硫酸と水酸化アルミニウ
ムの割合は、所望する塩基度に必要な水酸化アルミニウ
ムの理論量に対して０〜10％過剰にするのがよい。水酸
化アルミニウムが少ないと所望する塩基度が得られにく
く、多すぎると濾過設備が大きなものとなる。[0006] The reaction time of the above reaction varies depending on the reaction temperature, the water content of the aluminum hydroxide used, the average particle size, the particle size distribution and the sulfuric acid concentration. Further, the ratio of sulfuric acid to aluminum hydroxide is preferably set to be 0 to 10% excess with respect to the theoretical amount of aluminum hydroxide required for a desired basicity. If the amount of aluminum hydroxide is small, it is difficult to obtain a desired basicity, and if it is too large, the filtration equipment becomes large.
【０００７】本発明のポリ硫酸アルミニウムの塩基度は
10〜50％である。ポリ硫酸アルミニウムの塩基度が10％
以下であると、塩基度を上げるのに多量のアルカリ剤が
必要となり、あまり経済的ではない。また、本発明によ
る反応は塩基度が50％以上になると、一旦、反応中に生
成したポリ硫酸アルミニウムが加水分解を起こし、粒子
径１μ以下の微細な水酸化アルミニウムとなる。本発明
で得られる塩基度は実質50％までである。ただしアルカ
リ剤を加えることにより、塩基度を30〜70％まで上げる
ことが出来るが、塩基度70％以上のポリ硫酸アルミニウ
ムは保存性がよくなく、実用的ではない。アルカリ剤と
しては、水酸化ナトリウム、水酸化カリウム、水酸化カ
ルシウム、炭酸ナトリウム、炭酸水素ナトリウム、炭酸
カルシウム等が使用できる。The basicity of the polyaluminum sulfate of the present invention is
10 to 50%. 10% basicity of aluminum polysulphate
Below, a large amount of alkali agent is required to increase the basicity, which is not very economical. In addition, in the reaction according to the present invention, when the basicity becomes 50% or more, the aluminum polysulfate generated during the reaction once undergoes hydrolysis to form fine aluminum hydroxide having a particle diameter of 1 μm or less. The basicity obtained in the present invention is substantially up to 50%. However, by adding an alkali agent, the basicity can be increased to 30 to 70%. However, aluminum sulfate having a basicity of 70% or more has poor storage stability and is not practical. As the alkaline agent, sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, sodium hydrogen carbonate, calcium carbonate and the like can be used.
【０００８】ポリ塩化アルミニウム（ＰＡＣ）の硫酸根
として、本発明のポリ硫酸アルミニウムを使用する場
合、ＰＡＣに添加するポリ硫酸アルミニウムの量は、Ｐ
ＡＣ中の硫酸根が1.5 〜3.5 ％の範囲になるようにする
のがよい。1.5 ％以下では凝集剤としての性能が劣り、
3.5 ％以上では保存安定性が悪くなる。When the aluminum sulfate of the present invention is used as a sulfate group of aluminum polychloride (PAC), the amount of aluminum sulfate added to the PAC is P
It is preferred that the sulfate content in the AC be in the range of 1.5 to 3.5%. Below 1.5%, the performance as a flocculant is inferior,
If it is more than 3.5%, the storage stability will be poor.
【０００９】[0009]
【実施例】以下、実施例により、本発明をより具体的に
説明するが、本発明はこれらに限定されるものではな
い。 実施例１ 工業用ハイドラジライト系結晶性水酸化アルミニウム
（平均粒子径50μ):100ｇ（含水率：10％）と50％硫酸
200ｇ、水 740ｇを１Ｌガラス製オートクレーブ反応器
に入れ加熱した。反応系の温度を 130℃、圧力0.15〜0.
2MPaに２時間保持したのち、加熱を止めた。冷却した
後、反応液を取り出したところ、わずかに未反応の水酸
化アルミニウムが含まれていた。濾過を行ったところ、
簡単に分離でき、ほとんど透明なポリ硫酸アルミニウム
溶液1020ｇを得た。未反応の水酸化アルミニウムの平均
粒子径は25μであり、微細な水酸化アルミニウムではな
かった。この溶液の組成は次の通りであった。 Al2O3 5.0％、塩基度 35％、SO4 9.4％ 実施例２ 工業用ハイドラジライト系結晶性乾燥水酸化アルミニウ
ム（平均粒子径60μ）：80ｇ、95％硫酸 135ｇ、水 400
ｇを１Ｌガラス製オートクレーブ反応器に入れ、反応系
の温度を 100℃、圧力を0.05〜0.1MPaに５時間保持した
のち、加熱を止めた。冷却した後、反応液を取り出し、
ほとんど透明なポリ硫酸アルミニウム溶液 610ｇを得
た。この溶液の組成は次の通りであった。 Al2O3 8.5％、塩基度 17％、SO4 19.8％ 実施例３ 工業用ハイドラジライト系結晶性乾燥水酸化アルミニウ
ム（平均粒子径60μ）：100 ｇ、95％硫酸 100ｇ、水 7
00ｇを１Ｌガラス製オートクレーブ反応器に入れ、反応
系の温度を 140℃、圧力を0.3 〜0.5MPaに２時間保持し
たのち、加熱を止めた。冷却した後、反応液を取り出
し、ほとんど透明なポリ硫酸アルミニウム溶液 880ｇを
得た。この溶液の組成は次の通りであった。 Al2O3 7.4％、塩基度 50％、SO4 10.8％ 比較例１ 反応系の温度を 150℃、圧力を0.5 〜0.6MPaにした他は
実施例３と同じ条件で反応を行った。冷却後反応液を取
り出したところ、微細な粒子が多量に生成していた。通
常の方法で濾過を行ったが、終了するまで非常に時間を
要した。微細な粒子の組成を調べたところ、粒子径が１
μ以下の水酸化アルミニウムであった。EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the present invention is limited thereto. Example 1 Industrial-use hydrazirite-based crystalline aluminum hydroxide (average particle size: 50μ): 100 g (water content: 10%) and 50% sulfuric acid
200 g and 740 g of water were placed in a 1 L glass autoclave reactor and heated. The temperature of the reaction system is 130 ° C and the pressure is 0.15 ~ 0.
After holding at 2 MPa for 2 hours, heating was stopped. After cooling, the reaction solution was taken out and found to contain slightly unreacted aluminum hydroxide. After filtering,
1020 g of an aluminum polysulfate solution which was easily separated and was almost transparent was obtained. The average particle size of the unreacted aluminum hydroxide was 25 μ, and it was not a fine aluminum hydroxide. The composition of this solution was as follows: Al 2 O 3 5.0%, basicity 35%, SO 4 9.4% Example 2 Industrial-use hydrazirite crystalline dry aluminum hydroxide (average particle size 60μ): 80 g, 95% sulfuric acid 135 g, water 400
g was placed in a 1 L glass autoclave reactor, the temperature of the reaction system was maintained at 100 ° C., the pressure was maintained at 0.05 to 0.1 MPa for 5 hours, and then the heating was stopped. After cooling, take out the reaction solution,
610 g of an almost transparent aluminum polysulfate solution was obtained. The composition of this solution was as follows: Al 2 O 3 8.5%, basicity 17%, SO 4 19.8% Example 3 Hydrazilite crystalline dry aluminum hydroxide for industrial use (average particle diameter 60 μ): 100 g, 95% sulfuric acid 100 g, water 7
00 g was placed in a 1 L glass autoclave reactor, the temperature of the reaction system was kept at 140 ° C. and the pressure was kept at 0.3 to 0.5 MPa for 2 hours, and then the heating was stopped. After cooling, the reaction solution was taken out to obtain 880 g of an almost transparent aluminum polysulfate solution. The composition of this solution was as follows: Al 2 O 3 7.4%, basicity 50%, SO 4 10.8% Comparative Example 1 The reaction was carried out under the same conditions as in Example 3 except that the temperature of the reaction system was 150 ° C. and the pressure was 0.5 to 0.6 MPa. When the reaction solution was taken out after cooling, a large amount of fine particles were generated. Filtration was performed in the usual manner, but it took a very long time to finish. Examination of the composition of the fine particles revealed that the particle diameter was 1
It was aluminum hydroxide of μ or less.
【００１０】比較例２ 反応系の温度を90℃、圧力を0.03〜0.05MPa にした他は
実施例２と同じ条件で反応を行った。冷却後反応液を取
り出したところ、未反応の水酸化アルミニウムを含んだ
反応液が得られた。ろ過を行ったところ、簡単に分離で
き、ほとんど透明な溶液 590ｇを得た。この溶液を調べ
たところ、アルミナ分 7.5％の硫酸アルミニウム溶液で
あった。塩基度は０％で、この溶液は本発明の目的とす
るポリ硫酸アルミニウムではなかった。Comparative Example 2 A reaction was performed under the same conditions as in Example 2 except that the temperature of the reaction system was 90 ° C. and the pressure was 0.03 to 0.05 MPa. After cooling, the reaction solution was taken out, and a reaction solution containing unreacted aluminum hydroxide was obtained. Filtration yielded 590 g of an almost transparent solution that was easily separated. When this solution was examined, it was an aluminum sulfate solution having an alumina content of 7.5%. The basicity was 0%, and this solution was not the target aluminum sulfate of the present invention.
【００１１】（参考例）Al2O3 13.0％、塩基度62％のポ
リ塩化アルミニウム 500ｇに、実施例１で得たポリ硫酸
アルミニウム250 ｇを添加したところ、Al2O3 10.3％、
塩基度60％、SO43.1％の硫酸根含有ポリ塩化アルミニウ
ム 750ｇが得られた。この試作品と市販の硫酸根含有ポ
リ塩化アルミニウム（Al2O3 10.2％、塩基度62％、 SO4
3.0％）を使用して、水温17℃、濁度27°、ｐＨ 7.2の
利根川河川水の凝集試験を行った。凝集試験はジャーテ
スターで行い、河川水にＰＡＣを５、10、15、20ppm 添
加し、上澄液濁度を測定した。ジャーテストの試験条
件、上澄液濁度測定結果は、表１、表２の通りであっ
た。[0011] (Reference Example) Al 2 O 3 13.0%, the basicity of 62% polyaluminum chloride 500 g, was added poly aluminum sulphate 250 g obtained in Example 1, Al 2 O 3 10.3% ,
As a result, 750 g of a sulfated-containing polyaluminum chloride having a basicity of 60% and SO 4 of 3.1% was obtained. This prototype and commercially available sulfate-containing polyaluminum chloride (Al 2 O 3 10.2%, basicity 62%, SO 4
(3.0%) was used to conduct a cohesion test of Tonegawa river water at a water temperature of 17 ° C, a turbidity of 27 °, and a pH of 7.2. The coagulation test was performed using a jar tester, PAC was added to river water at 5, 10, 15, and 20 ppm, and the supernatant turbidity was measured. The test conditions of the jar test and the measurement results of the supernatant turbidity were as shown in Tables 1 and 2.
【００１２】[0012]
【表１】 [Table 1]
【００１３】[0013]
【表２】 [Table 2]
【００１４】本発明により得たポリ硫酸アルミニウムを
添加して試作した硫酸根含有ポリ塩化アルミニウムは、
市販のポリ塩化アルミニウムと同等以上の凝集性能を持
つことがわかった。本発明により得られるポリ硫酸アル
ミニウムは、ポリ塩化アルミニウムの硫酸根として有用
であることがわかった。The sulfate-containing polyaluminum chloride produced by adding the aluminum polysulfate obtained according to the present invention is as follows:
It was found that it had a cohesion performance equal to or higher than that of commercially available polyaluminum chloride. The aluminum polysulfate obtained by the present invention was found to be useful as a sulfate group of polyaluminum chloride.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4D015 BA03 BA10 CA02 CA14 DA04 DC02 EA02 EA32 4D062 BA03 BA10 CA02 CA14 DA04 DC02 EA02 EA32 4G076 AA14 AA19 AB06 BA12 BC07 BD02 BD04 CA14 DA28 ──────────────────────────────────────────────────続 き Continued on front page F term (reference) 4D015 BA03 BA10 CA02 CA14 DA04 DC02 EA02 EA32 4D062 BA03 BA10 CA02 CA14 DA04 DC02 EA02 EA32 4G076 AA14 AA19 AB06 BA12 BC07 BD02 BD04 CA14 DA28
Claims (3)
ポリ硫酸アルミニウムを製造する方法において、水酸化
アルミニウムとしてハイドラジライト系結晶性水酸化ア
ルミニウムを使用し、且つ反応温度100 〜140 ℃の範囲
で反応を行うことを特徴とするポリ硫酸アルミニウムの
製造方法。1. A method for producing aluminum polysulfate by reacting aluminum hydroxide with sulfuric acid, wherein a hydrazirite-type crystalline aluminum hydroxide is used as the aluminum hydroxide and the reaction temperature is in the range of 100 to 140 ° C. A method for producing aluminum polysulfate, which comprises conducting a reaction.
うことを特徴とする請求項１記載のポリ硫酸アルミニウ
ムの製造方法。2. The method according to claim 1, wherein the reaction is carried out at a reaction pressure of 0.05 to 1.0 MPa.
H)n(SO4)3-2/n] で表した時の塩基度（ｎ／６×100
％）が10〜50％であることを特徴とする請求項１又は２
記載のポリ硫酸アルミニウムの製造方法。3. An aluminum polysulfate having the general formula [Al 2 (O
H) n (SO 4 ) 3-2 / n ] basicity (n / 6 × 100
%) Is 10 to 50%.
The method for producing aluminum polysulfate according to the above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11026287A JP2000226213A (en) | 1999-02-03 | 1999-02-03 | Production of aluminum polysulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11026287A JP2000226213A (en) | 1999-02-03 | 1999-02-03 | Production of aluminum polysulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000226213A true JP2000226213A (en) | 2000-08-15 |
Family
ID=12189094
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11026287A Pending JP2000226213A (en) | 1999-02-03 | 1999-02-03 | Production of aluminum polysulfate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000226213A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005013863A (en) * | 2003-06-25 | 2005-01-20 | Sony Corp | Waste water treating agent and waste water treatment method |
| CN103172149A (en) * | 2012-12-14 | 2013-06-26 | 新疆德蓝股份有限公司 | Flocculating agent for processing low-temperature and low-turbidity water |
| WO2015092004A3 (en) * | 2013-12-20 | 2015-09-11 | Sika Technology Ag | Method for producing a gunned-concrete accelerator using new raw materials |
| KR101973986B1 (en) * | 2018-06-01 | 2019-08-23 | 염선화 | Method of preparation for coagulant and treating method of water/wastewater using the same |
-
1999
- 1999-02-03 JP JP11026287A patent/JP2000226213A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005013863A (en) * | 2003-06-25 | 2005-01-20 | Sony Corp | Waste water treating agent and waste water treatment method |
| CN103172149A (en) * | 2012-12-14 | 2013-06-26 | 新疆德蓝股份有限公司 | Flocculating agent for processing low-temperature and low-turbidity water |
| WO2015092004A3 (en) * | 2013-12-20 | 2015-09-11 | Sika Technology Ag | Method for producing a gunned-concrete accelerator using new raw materials |
| AU2018260805B2 (en) * | 2013-12-20 | 2020-03-19 | Sika Technology Ag | Method for Producing a Gunned-Concrete Accelerator Using New Raw Materials |
| KR101973986B1 (en) * | 2018-06-01 | 2019-08-23 | 염선화 | Method of preparation for coagulant and treating method of water/wastewater using the same |
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