TW200848374A - Process for preparing ferrous-silica water treating agent - Google Patents

Process for preparing ferrous-silica water treating agent Download PDF

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Publication number
TW200848374A
TW200848374A TW097116956A TW97116956A TW200848374A TW 200848374 A TW200848374 A TW 200848374A TW 097116956 A TW097116956 A TW 097116956A TW 97116956 A TW97116956 A TW 97116956A TW 200848374 A TW200848374 A TW 200848374A
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Taiwan
Prior art keywords
iron
aqueous solution
water
concentration
agent
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TW097116956A
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Chinese (zh)
Inventor
Masahiro Takesue
Yoshiaki Koga
Takao Hasegawa
Yasushi Masuda
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Tokuyama Corp
Suido Kiko Kk
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Application filed by Tokuyama Corp, Suido Kiko Kk filed Critical Tokuyama Corp
Publication of TW200848374A publication Critical patent/TW200848374A/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D21/00Separation of suspended solid particles from liquids by sedimentation
    • B01D21/01Separation of suspended solid particles from liquids by sedimentation using flocculating agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/126Preparation of silica of undetermined type
    • C01B33/128Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20Jet mixers, i.e. mixers using high-speed fluid streams
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/23Mixing by intersecting jets
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention relates to a process for preparing ferrous-silica water treating agent which process can produce excellent aggregative ferrous-silica water treating agent effectively in short time by using a simple device, and relates to a process for preparing ferrous-silica water treating agent exhibiting excellent stability. The process for preparing ferrous-silica water treating agent of the present invention is characterized by conflict mixing an aqueous solution of ferric chloride or an aqueous solution containing ferric salt and mineral acid with an aqueous silicic acid solution so that the ferrous-silica water treating agent has a pH of from 0.3 to 1, a Fe concentration of from 30g/L to 120g/L, and a SiO2 concentration of from 10g/L to 50g/L.

Description

200848374 九、發明說明: 【發明所屬之技術領域】 本發明有關一種鐵-氧化矽水處理凝集劑之新穎方 ,。更詳言之,有關-種即使於高的鐵濃度亦可簡便地 存安定性優異之鐵-氧化矽水處理凝集劑之方法。 、 【先前技術】 ηΐϋί削水或排水中移除懸浮物質或其他雜質而進 二$二進二有$該用水或排水中注入凝集劑使該等雜 ί的水處理方法,作為此目的時的凝集劑,使 用有硫酸鋁、聚氣化鋁、氯化鐵等。 上述凝集劑中,尤其廣泛使用硫酸鋁或聚氯化鋁。 ^此魏_時,水溫祕,因树 ===不增加凝集劑之添加量,由_為兩== 合性鋁,故有殘留於處理水中之問題點。又,由於鋁系 次木於低水溫下凝集性低,故有需增大使用量之缺點、。…、 添加的問題,近來,於聚合石夕酸(氧化石夕溶膠)令 乳切水歧凝_由於其高峡集性能及ΐ 生之减集物可於土壤帽原輯賴目。w此姑 之化f水處理凝集劑係於容器中於鹽酸、硫酸等 =it氧化石夕溶谬,接著一面·‘酸 ί ^ 中添加鐵鹽而獲得(參考專利文獻1、2)。 能之中記载之方法為了得到具有良好性 右,攪拌數小時同化石夕溶膠)加熱至啊左 又,由於製為用於加熱之裝置成為必要, 另二時間’有工業實施方面的問題。 水處理凝集劑之U案/f以工f上簡便之方法製造鐵-氧化矽 添加矽酸鹽水溶液〔二,如,提案有:於氯化鐵水溶液中直接 ',猎此f丨起鐵與氧化矽反應之同時,亦進行 IP080246/SF-1907f 6 200848374 水溶水鎌情加魏鹽 本i 靳=賴強力授拌或長時間反應的必要。 需要以-小時以上應中之氧化石夕溶膠谬凝化而 加矽酸鹽水溶液,藉由^狀\, °又’即使缓緩地添 ^文獻1 ·日本特公平4_75796號公報 ί利文獻2 ··日本特許第2732076號公報 日本特許第37_92號公報 [發明欲解決之課題] 高凝=能提供—種簡易地赌時間製造顯示 ΐ他= 水凝集處理劑之方法。又,本發明之 度製造伴存安〗^如上述之製造方法,其細高的鐵濃 優^鐵·祕财處顧細之方法。 银於本狀等為解決上述課題而進行刻意研究。盆社果,發 之操作時,亦益乂二猎由翻^5專而進而混合鐵鹽水溶液 定ί也^乳化石夕之膠凝化困擾,而可以短時間、安 成本ίίτ持兩旋集性能之鐵-氧化石夕水處理凝集劑,因而完 IP080246/SF-1907f 200848374 f即二本發明係一種鐵氧化石夕水處理凝集劑之製造方 特徵為在藉由使石夕酸鹽水溶液與鐵鹽水溶液反應而製造 匕石夕水處理劑時,包含使製造上述鐵-氧化石夕水處理凝集 I中所使用之錢鹽水溶液全量與紐水溶液之至少-部;分 進行衝突混合之衝突混合步驟。 鹽水i液衝突混合之鐵 制、本發明,提供上述之鐵_氧切水處理凝集劑之 旦其中上述衝突混合步驟中,經衝突混合之鐵鹽水溶 ί — 71里為,相對於鐵-氧化矽水處理凝集劑之製造中所使 倍莫ίίίΐί液之全量中之矽元綱,鐵元素(Fe)成為。.5 仅六if ’對使用上述方法所得之鐵·氧辦水處理凝集劑之 ΐί ίϊίί高條件下進行檢討之結果,發現卿(氧$ /辰度、鐵浪度及ΡΗ在下述範圍内為有效。 之!發明’提供上述之鐵_氧切水處理凝集劑 製:法中該鐵_氧化梦水處理凝集劑之阳為〇3〜 .,鐵7〇素(Fe)濃度為2〇2几〜12〇砂,s l〇g/L〜50g/L,且_莫耳比為i以下。设 2 /辰度為 又進而,本發明之上述終氧化石夕水處理凝集劑之 H’U所得之鐵·氧化财處理凝 $ 之樣態,包含以下樣態。 來1千 趟水朗狀树躲驗全量與鐵 藉由任意“ 鐵氧财水處理賴^減破縣為目的物之 (2)於衝突混合步驟中,使所用之石夕酸鹽水溶液全 鹽水溶液全量衝突混合,而灌握士、& α 里/、鐵 理凝集劑之職。喊㈣為目缝·•氧切水處 IP080246/SF-1907f 8 200848374 也擔(!)於上述⑴、(2)樣態中’於衝突混合步驟申,藉由添加 ΐίί調整PH而獲得成為目的物之鐵-氧化矽水處理凝集劑 娜(4i於上Jl(1)、(2)樣態中,於衝突混合後藉由添加無機酸 果 1又付成為目的物之鐵氧化石夕水處理凝集劑之樣態。 依巧本㈣’藉㈣述触辣,細_氧切 二ϊϋ造中ί用之石夕酸鹽水溶液全量與鐵鹽水溶液之至少 伤進彳了衝突混合,可以辦間安定 -氧化矽水溶液凝集劑。 疋罘注此间之鐵 叫之pH較所狀鐵氧切水處理凝集 j之pH鐵及矽兀素浪度、以及該鐵與矽之莫 製造’可獲得長期保存软性優異之聲氧化石夕水處ί 【實施方式】 於本發明中,作為原料之魏鹽為通常之 口 要為鐵-氧化财處理難針所 限^ ^ =夕酸驗金屬鹽,具體而言,為魏鈉、中 ^慮原才^成本等’較好使用石夕酸納。使用石夕酸納時,&盥 並無特別限制,但較好莫耳比為2.5〜4.〇。2 ” 柄月中’包含上述石夕酸鹽之水溶液濃度 =之鐵·氧切水處理凝集劑之阳、鐵ί t亦即’藉由滿足此範圍,可容易地以ir夸t巧二3= &不會發生瞬間膠凝化物反而凝集性優里之 =製 凝集劑安定性優異之鐵氧切水處ϊϊίϊί 又’依據本發明,如後述,以—邊娜鐵鹽“添加 IP080246/SF-1907f 9 200848374 矽酸鹽水溶液之過去的製造方法 濃度為76孤以上之雜鹽水溶難^如能夠使用Si〇2 有困難。為此,本發明可以短時間過去的製造方法 處理凝集#!。,高濃度之鐵^聲氧化石夕水 製造的效率化之同時,於儲存 7 ^凝集劑在實現 用時’可料轉為鮮濃如===、$又,於使 能亦成為-,其讀上調製凝集 鐵-氧化二之:::要是可使用於通常之 鐵、硫酸鐵^酸鐵/。者即可’而無特別限制’可使用氯化 财溶财之氣化職ί較= 原料魏财驗及峨水溶液作為 ίϊΐΐ述f 夕水處理凝集劑之製造方法,其包含相對 处理旋集劑之製造中使用之石夕酸鹽水溶液全量,使至少 一部份顧水溶液進行衝纽合之賊混合步ί使至" :石=水溶液與鐵鹽水溶液之反應中,衝突 ίΐΐί if月所採用者。藉此,亦不會發生在反應器内J 二口此$讀之触製造方法膽生之氧切麟化困擾,而 K糾間安定地獲得維持高凝集性能之鐵_氧化石夕水處理凝 、H入本文中,上述石夕酸鹽水溶液其全量與鐵鹽水溶液進行衝突 具有重要性:亦即,推測係藉由使石夕酸鹽*溶液與鐵鹽水 ^液衝突混合,藉由與鐵鹽水溶液之反應,魏鹽水溶液中之 ,化石夕成伤殳化成難以膠凝化之形態,藉由衝突混合時或其後 鐵鹽水>谷液之反應而防止凝膠發生者。 因此’於本發明中,藉衝突混合與矽酸鹽水溶液全量反應 IP080246/SF-1907f 200848374 <1^^之1可為其—部份亦可為其全量。 衝突混合鐵鹽水雜之一部份與矽酸鹽水溶液 _»几2^ 、、工衝大洗合之鐵鹽水溶液之混合量為,相掛於科 矽元素凝製造時所使用之石夕酸鹽水溶液之全量中 溶液itii水t係f由使含上述原料之鐵鹽水 Λ個原料供給管合流,在該原料供給管 字iii應器等),器(γ字管型、Τ 該等管型反應封,若===1上4合f卩衝突混合。 ^ 本制_2= 】1 本發明之¥字管型反應11之一例。 所字管型反應器,於各原料供給管之中間 ;二=口=節自泵供給的原 :,字:好 使用如此裝置時,於成為上述合 ί兩水溶液分別為5娜以上,較好以7轉iir更好 上必、、、、口速度上限並無特別限制 20_少左右以上,有其《已成物_= 又’較好反應物以lm/秒以上,較 以1.5m/秒以上之速度自排出管6 則 度可能變快,另一方面,若變粗則排出速度^則排出速 明 使用上述γ字管型反應器之較佳樣態於圖!加以說 IP080246/SF-1907f 11 200848374 八首先,鐵鹽水溶液之儲存槽〗、矽酸鹽水溶液之儲存槽2, L別儲存在儲存槽1及儲存槽2之鐵鹽水溶液(或包含鐵^及 …、機酸之水溶液)及矽酸鹽水溶液,供給至γ字管型反應哭 或原料供給管4,),在反應部5使兩水H衝 物rSif j此,藉由自反應部5通過翻管6取出反應 物了裊造鐵·氧化石夕水處理凝集劑。 本發明中,鐵_氧化矽水處理凝集劑之製造中使用之 水雜之比継無__,可鎌制地採用 發明綠#,較_對_元素的比例 孕乂大的組成,亦可無問題地製造。 y i又’ Ϊ上述’以上述比例使用之矽酸鹽水溶液與鐵鹽水溶 鹽水溶液較好其至少—部份藉由衝突混合而 則,由通常的混合例如使贿有授 “ 同别述’鐵鹽水溶液僅一部份與矽 液亦較好使用議莫耳比成為。.5以上之量 因此,本發明如前述可包含以下樣態者。 (1) 於衝突混合步驟巾,使姻之 =溶^之-部份衝突混合,獲得部份混 絲合麵賴水魏_得_目的物之 鐵·氧化矽水處理凝集劑之樣態。 1 (2) 於衝突混合步驟中,使所用、曰 鹽水溶液全量衝突混合,而嬅俨i /文皿水/合液全1與鐵 理凝集劑之樣態。 侍成為目的物之鐵-氧化石夕水處 之至少?由使矽酸鹽水溶液與鐵鹽水溶液 時間製造凝紐能《之餐氧切水故可以短 又,如離,/L之高的Si〇2濃度、且^性能優異之 IP080246/SF-1907f 12 200848374200848374 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a novel aspect of an iron-cerium oxide water treatment aggregating agent. More specifically, a method of treating an iron-nitric acid water treatment aggregating agent excellent in stability even in a high iron concentration can be easily obtained. [Prior Art] η ΐϋ 削 削 削 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或 或 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削 削As the aggregating agent, aluminum sulfate, polyaluminized aluminum, ferric chloride or the like is used. Among the above aggregating agents, aluminum sulfate or polyaluminum chloride is particularly widely used. ^When this is _, the water temperature is secret, because the tree === does not increase the addition amount of the aggregating agent, and the _ is two == compliant aluminum, so there is a problem remaining in the treated water. Further, since the aluminum-based secondary wood has low aggregability at a low water temperature, there is a disadvantage that the amount of use is required to be increased. ..., the problem of addition, recently, in the polymerization of sulphuric acid (Oxidized Oxide sol) to make the water cut off the water _ due to its high-gorge performance and the reduction of the epidemic can be in the soil cap original. w 此 化 f f 水 水 水 水 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 In order to obtain goodness in the method described in the right, the mixture is heated to the left after stirring for several hours, and it is necessary to manufacture the device for heating, and the other two times have problems in industrial implementation. The U case/f of the water treatment aggregating agent is made by the simple method of manufacturing iron-yttria added yttrium acid solution [2, if, the proposal is: directly in the aqueous solution of ferric chloride], hunting this f丨 iron and At the same time as the cerium oxide reaction, it is also necessary to carry out IP080246/SF-1907f 6 200848374 water-soluble water sensation plus Wei salt. It is necessary to add an aqueous solution of bismuth oxide in the oxidized sol-gel solution of -hours or more, and to add a sulphate aqueous solution by ^^, °, and even if it is slowly added to the literature 1 · Japanese special fair 4_75796 bulletin 2 Japanese Patent No. 2732076 (Japanese Patent No. 37-92) [Problems to be Solved by the Invention] High coagulation = a method for producing a water agglutination treatment agent by providing a simple gambling time. Further, the manufacturing method of the present invention is accompanied by the above-described manufacturing method, and the method of the fine iron-rich iron and iron. Silver is deliberately studied in order to solve the above problems. Potted fruit, when the operation is carried out, it is also beneficial to the second hunting by turning the ^5 special and then mixing the iron salt aqueous solution to determine the emulsification of the emulsified stone eve, but can be short-term, the cost of the ίίτ holding two sets Performance of iron-oxidized stone water treatment agglutinating agent, thus completing IP080246/SF-1907f 200848374 f, that is, the invention is characterized in that the iron oxide oxide aqueous agglomerating agent is manufactured by using an aqueous solution of When the iron salt aqueous solution is reacted to produce a waste water treatment agent, it comprises a conflict mixing of the total amount of the money salt aqueous solution used in the production of the iron-oxide oxide treatment agglutination I and the at least one portion of the new aqueous solution; step. The present invention provides the above-mentioned iron-oxygen water-cutting aggregating agent. In the above conflict mixing step, the conflict-mixed iron salt water dissolves in the water, and is relative to the iron-oxidation. In the manufacture of the water-repellent aggregating agent, the elemental element of the total amount of the liquid is obtained, and the iron element (Fe) is obtained. .5 only six if's the results of a review under the high conditions of the iron/oxygen water treatment agglutinating agent obtained by the above method, it was found that the oxygen (oxygen / / degree, iron wave and ΡΗ in the following range is Effective! The invention provides the above-mentioned iron_oxygen water treatment agglutinating agent system: in the method, the iron _ oxidized dream water treatment agglutinating agent has a yang of 3 ., and the iron 7 〇 (Fe) concentration is 2 〇 2 a few ~ 12 〇 sand, sl 〇 g / L ~ 50g / L, and _ molar ratio is below i. Set 2 / Chen degrees to further, the above-mentioned final oxidized stone treatment of the present invention H'U The form of the obtained iron and oxidation treatment is as follows: The 1 趟 趟 状 树 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 躲 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2) In the conflict mixing step, the total amount of the aqueous solution of the aqueous solution of the aqueous solution of the solution is mixed and mixed, and the position of the occluder, & α, / iron agglutination agent. Shout (four) for the eye seam • oxygen cut The water supply IP080246/SF-1907f 8 200848374 also bears (!) in the above (1), (2) form, in the conflict mixing step, by adding ΐίί to adjust the PH The iron-oxidized strontium water treatment agglutinating agent Na (4i in the upper Jl (1), (2) state, after the conflict is mixed, by adding the inorganic acid fruit 1 and paying the target iron oxide stone Xishui treatment of the form of agglutination agent. According to Qiao Ben (four) 'borrow (four) said spicy, fine _ oxygen cut two ϊϋ ϊϋ ί 用 用 ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί ί It can be used to stabilize the cerium oxide aqueous solution agglutinating agent. Note that the pH of the iron in this case is higher than that of the ferrite-treated water, the pH of the iron and the alizarin wave, and the iron and yttrium. Acoustic Oxidized Stones with Excellent Long-Term Preservation Softness ί 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施 实施The salt, in particular, is a good use of the sodium sulphate, the middle of the original, the cost, etc. 'When using the sodium sulphate, the & 盥 is not particularly limited, but the molar ratio is 2.5. ~4.〇.2 "In the middle of the handle", the concentration of the aqueous solution containing the above-mentioned oxalate is determined by the iron/oxygen-cut water treatment agglutinating agent. , Tie Tie, that is, by satisfying this range, it is easy to use ir boast t 2 2 & no instant gelation instead of agglutination yuli = agglomerate excellent stability of ferrite cut water依据 ϊ ϊ 又 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 依据 IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP IP 〇2 has difficulty. For this reason, the present invention can process agglomeration in a short-time manufacturing method. The efficiency of the high-concentration iron-oxygen oxide oxidized water is simultaneously reduced, and the storage of the 7 ^ aggregating agent is realized. 'It can be converted to fresh as ===, $, and also becomes -, which reads the modulated agglomerated iron-oxidized two::: If it can be used for ordinary iron, iron sulfate / iron. It can be 'without special restrictions'. It can be used in the chlorination of the liquefied acid. The raw material Weicai and the hydrazine aqueous solution are used as the manufacturing method of the shui water treatment agglutinating agent, which contains the relative processing rotator. The total amount of the aqueous solution of the sulphuric acid salt used in the manufacture, so that at least a part of the aqueous solution of the squid is mixed with the thief, and the reaction to the " : stone solution and the aqueous solution of the iron salt is conflicted. By. Therefore, it does not occur in the reactor, the two-portion of the method of manufacturing the bile oxygenation, and the K-correction to obtain the iron that maintains the high agglutination performance. In this paper, it is important that the above-mentioned aqueous solution of the aqueous solution of the cerevisiae collides with the aqueous solution of the iron salt: that is, it is presumed that by mixing the solution of the oxalate salt with the solution of the iron salt solution, with iron In the reaction of the saline solution, in the aqueous solution of the Wei salt, the fossilized into a scar is formed into a form which is difficult to gel, and the gel is prevented by the reaction of the conflict or the subsequent reaction of the iron salt and the valley liquid. Therefore, in the present invention, the total amount of the reaction mixture can be mixed with the aqueous solution of the citrate IP080246/SF-1907f 200848374 <1^^1. The mixing amount of the mixed mixed iron salt water and the aqueous solution of bismuth sulphate _»2 2, and the large amount of the iron salt aqueous solution of the industrial washing is the same as that used in the manufacture of the scorpion element. In the total amount of the aqueous solution, the solution iii water t is f, and the iron salt containing the above-mentioned raw materials is mixed with a raw material supply pipe, and the raw material is supplied to the pipe iii, etc.), and the tubular type reaction is carried out. Seal, if ===1, 4合f卩 conflicts mixed. ^Production_2= 】1 An example of the ¥-tube type reaction 11 of the present invention. The tubular type reactor is in the middle of each raw material supply pipe; Two = mouth = section from the original supply of the pump:, word: When using such a device, it is more than 5 nanometers for the above two aqueous solutions, preferably 7 turns iir better, the upper limit of the mouth speed There is no particular restriction on 20_s or more, and there is a better reactant in lm/sec or more, which may be faster than the discharge tube 6 at a speed of 1.5 m/sec or more. On the one hand, if it is thicker, the discharge speed is then discharged. The preferred mode of using the above-mentioned γ-tube type reactor is shown in the figure! It is said that IP080246/SF- 1907f 11 200848374 VIII First, the storage tank of the aqueous solution of iron salt, the storage tank 2 of the aqueous solution of citrate, L, the aqueous solution of iron salt stored in the storage tank 1 and the storage tank 2 (or the aqueous solution containing iron and... And the aqueous solution of citrate is supplied to the gamma tube type reaction crying or raw material supply pipe 4, and the two water H is flushed in the reaction unit 5, and the reactant is taken out from the reaction portion 5 through the turn tube 6. The iron-oxidized stone is used to treat the agglutinating agent. In the present invention, the ratio of water miscellaneous used in the manufacture of the iron-cerium oxide water treatment aggregating agent is not __, and the invention green # can be used in a tanning manner, and the composition of the invention is larger than that of the _ element. Manufactured without problems. Yi ' ' Ϊ Ϊ ' 以 ' 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以 以Only a part of the saline solution is preferably used in combination with the sputum. The amount of 5 or more is therefore the following aspect of the present invention as described above. (1) In the conflict mixing step, the marriage = The mixture-partial conflict is mixed, and a part of the mixed silk surface is obtained, and the iron and yttrium oxide water treatment agglutinating agent is used. 1 (2) In the conflict mixing step, the used The total amount of strontium salt solution is mixed in conflict, and the 嬅俨i / water/liquid mixture is the same as the iron agglutinating agent. The iron-oxidized stone is at least the target of the target. It is possible to make a condensate with the iron salt solution time. The food can be cut into oxygen, so it can be short, and the concentration of Si 〇 2 is high, and the performance is excellent. IP080246/SF-1907f 12 200848374

200848374 述之過本;理難劑亦可在1分勒製造2L。目此,與前 睡水、、二、y夕=之使聚合石夕酸(氧化石夕轉)進行聚合後,添加鐵 _水、/if於反應容器中於氯化鐵水溶液中添加石夕酸 極辦間製造,料發揮與過錢術_以上之L 處理驚ϊί是’相較於先前技術所製造之鐵-氧化石夕水 理减集劑具有更長期之保存安定性。 卜处 维持法所得之鐵·氧化财處理凝集劑為了仍舊 麟更細蚊性,_使所得之 於Γβ且A L木别之pH較好成為0·3〜h5,更好成為小 20^100^ ; ^ ^Tii\2〇^12〇g/L ? l〇g/L〜50gT之方式^广成為1〇g/L〜零’更好成為 了疋,藉由凋整為上述條件所得氧、 ,後述實施例所述般,在3(rc、^ j 日古3二不-產生膠凝化物地保存亦成為可能。:且,由於^ 口^二= 處,疑集劑,可降低運輸費而在經濟i 以使所制气^水液係呈酸性,故亦可使用作為用 今w t處理凝集劑的ρΗ降低之阳調節劑,作 顧集劑之pH,在鐵濃度不變化下 ^無機酸。此種無機酸並無特別限制,而可適^使用硫^或】. ^即,本發明中,包含如下述般之樣態。 (3)於上述(1)、(2)樣態中,於衝 人 * :;調整pH而獲得成為目的物之鐵:夕:處 IP080246/SF-1907f 13 200848374 調整(P4ii^A(2目中’於衝突混合後藉由添加^ 加均的樣1Γ於衝突混合步驟中, 1二======’再將此與心鹽 合步驟中及織麵添加在衝突混 用』ί 得之鐵_氧_水處理凝集劑可直接使 實=釋為適㈣度而有效地使用作為各種排水之水處理劑吏 定於ίίΐ=刊實施例更具體加以說明,但本發明不限 ⑴衝突混合裝,(鐵-氧化石夕水處理凝集劑之製造裝置) 泸1所γ子官型反應1^ ’係以自節流部的管徑(内 1Gmm之原料供給管4供給御_水溶液, =樣疋^L部管徑(内徑)為Ummx長度10醜之原料供給 給,鐵水溶液,於反應部5進行衝突混合,自排出'管 徑(内徑)為6mmx長度30mm)取出混合液之方式使用。γ ϋΐ反ί裝置之兩個原料供給管4及4,所成的角度為90度。 (Λ)黏度测定 定。使用A&D股份有限公司之音叉型振動式黏度計在抓測 ⑶凝集性能之評估 於自來水t添加高駐(和統㈣水質試 調整為濁度2〇之物作為試驗水進行瓶杯^^ est)。於l〇〇〇ml δ式驗水中,使對水1L相當於巧為5啤之方 式添加凝集劑,以擾拌速度150rpm攪拌5分鐘,接著以攪拌 速度50rpm攪拌1〇分鐘,進而,靜置1〇分鐘後,採取上澄液 5〇ml。藉由狀_之綠,檢驗縣發騎得之鐵-氧化 鐵水處理凝集劑之水處理性能。 IP080246/SF-1907f 14 200848374 (4)保存安定性之評估 將鐵-氧化矽水處理凝集劑放置在3(rc,以目視判定 度’則丨起職鱗凝料止之日數_安定性,。 m /Γ售的矽酸鈉(矽酸鹽水溶液·· Si〇2濃度28質量〇/〇, 』2 asO莫耳比丄⑸以水稀釋,成為別〇2濃度%机之水溶 = 二使市f 39質量%之氯化鐵溶液(鐵鹽水溶液) ‘Ϊΐ成J =鐵濃Ϊ 19〇g/L之水溶液。該等水溶液分別 π :自原?供給官4以流量L〇L/min供給石夕酸納水溶 料供給管4’以流量〇.9L/min供給氯化鐵水溶液,在 riHi打=突混合,自排出管6取出。以約2分40秒獲 仵鐵-虱化矽水處理凝集劑5L。 發酸納水溶液及氯化鐵水溶液流 向分別為ia8m/s、13減。又該水處 理嫂集劑自排出管排出之流速為Um/s。 卜处 箄,處理凝細並無氧化歡賴化物 鐵濃度為3lg/L,Si/Fe莫耳比為U1,^為^度為37机 下的保存安定性。此等結果示於表1。 、於實施例1所得之鐵-氧化石夕水處理凝 使凝集劑之pH成為1.05。添加硫酸直至成為鐵產化^ 處理凝鋪為止之關,自 處理凝集劑之凝集性能及保存安定性示於表b、、刀、’ [實施例3] 實施例1所得之鐵_氧化梦水處理凝集 入 氯化鐵水溶液以及硫酸,使水I 稀釋 離,鐵嶋離,f叫濃度成為 旲斗比為0·25,PH為〇·85。以 IP080246/SF-1907f 15 200848374 氯化鐵水溶液以及硫酸直至成為最終鐵_氧化石夕 ίίίϊί縣止之_,自賊混合_賴為5分鐘。此 i處理破_之凝雜缺健蚊鮮於表卜 [實施例4] 文鈉水溶液為市售的矽酸鈉(別〇2濃度%質量%, 1 2入,〇莫耳比3·2)以水稀釋,成為邮濃度^峡之水溶 鐵及無機酸之水溶液,係使市f 38 f量%之氣化 ^稀釋、’進而添加48質量%硫酸,成為含硫酸濃度 ,a /sfl化鐵漠度258g/L之氯化鐵水溶液。使用該等水溶 給f ^赠量H/d11供給魏财溶液,自 iy, 2 Z1以流10.9L/mm供給含有硫酸之氣化鐵水溶 5’丨在反應部5進行衝突混合,自排出管6取出。以約2分 π 氧化财處理凝製猶所個之魏鹽水溶 =王鐵鹽水溶液之一部份的反應液(此亦稱為「部份混合 時向反應部5供給之石夕酸納水溶液與含有硫酸之 虱化鐵必5水溶液之流速分別為10.8m/s、13.3m/s。 人旦ΐ ’ t述衝突混合步驟中,經衝突混合之鐵鹽水溶液之混 =ί ^目對於聲氧切水處理難㈣造時所制之石夕酸 二水洛液全量中的石夕元素⑼’鐵元素㈣成為㈣倍莫耳之 置0 所得之部份混合液並無氧化石夕之膠凝化物 4im部份混合液之⑽2濃料離, 42g/L ’ Si/Fe 莫耳比為 ΐ·28,pH 為 1·〇8。 ,此500ml置於容器中,授拌下於其中添加水 m 質量%氣化鐵水溶液460ml,獲得si〇2灑声盔 1,/L ’鐵濃度為60g/L ’ Si/Fe莫耳比為〇 25,pH為〇 82 :氧化矽水處概細⑻細。魏此鐵_氧切水處理凝集劑 =====分鐘’又,此水處理凝集劑之凝集 IP080246/SF-1907f 16 200848374 [實施例5] 除了矽酸鈉水溶液之Si0:2濃度成為9〇g/L、含有硫酸之氯 化鐵水溶,之氯化鐵濃度成為264g/L及硫酸濃度成為2〇_ .以外’進行與實施例4同樣反應,以約2分40秒獲得盔稾化 矽凝膠之黃褐色透明之部份混合液5L。 此部份混合液之Si〇2濃度為47g/L,鐵濃度為 ,8胸 莫耳比為1·02,pH為1.58。 、曰^、’上述衝突混合步驟中,經衝突混合之氯化鐵水溶液之 混合量為,相對於鐵_氧化矽水處理凝集劑製造時所使用之 酸,水溶液全量中_元素⑼,鐵元素㈣成為。%倍 之吾。 、 仰ft部ίΞ合液500ml置於容器中,擾拌下於其中添加水 俾曲貝痒里^風化鐵水溶液35_、50質量%硫酸4遍, 獲仲s】〇2》辰度為20g/L,鐵濃度為75g/L,Si/pe莫耳 pH為0.73之鐵-氧化石夕水處理凝集劑118偏。製造此鐵-氧 石夕水處理凝_係自触混合開始進躺 、’ 理凝集劑讀雜缺絲鍵㈣域丨。X此水處 [實施例6] 於實施例5藉衝突混合製造之如2濃 為43砂·莫耳比為l.G2,PH為i.58之部份混8^液^^ 中’添g 31_ ' 4G f量%氯化鐵水溶液^ : 匕Γο,2ΓηΤ^度為¥,鐵濃度為獅 理凝以=1分 取於實施例5藉触混合製造之Si〇2濃 度為43g/L,Si/Fe莫耳比為丨〇2,pH為丨^份、 ⑽^ 置於容器中,於其中添加水—質* IP080246/SF-1907f 17 200848374 110ml、50質量%硫酸6.5ml,獲得Si〇2濃度為25g/L,鐵濃度 為47g/L,Si/Fe莫耳比為〇·5,pH為0.98之鐵_氧化石夕水處$ 减集劑946ml。製造此鐵_氧化秒水處理凝集劑係自衝突混合開 始進行約5分鐘,又,此水處理凝集劑之凝集性能及保存^定 性示於表1。 [參考例1] 市售矽酸鈉(Si〇2濃度28重量%,Si〇2/Na20莫耳比3 以水稀釋,攪拌下於i小時内將s们:sn汀、二 =液化導入猶漠度=將之===之::酸 /if 40g/L、ΡΗ2·0之氧化石夕溶膠溶液2L。於此氧化$ 2 液中添加驗,調整至_,在室溫熟成3小時。/膠令 取此氧化石夕溶膠200ml,加入水5〇ml及% ^谷液15Gml,獲得Si〇2濃度為2 ^K /^匕 莫耳比為G.25,pH為〇 42⑽i f75抓’ Si/Fe 製造此鐵·氧切7]^^切水處理凝細40_。 止需要4小時==频納至製造為 存安定性示於表丨。 此水處理,縣劑之難性能及保 IP080246/SF-1907f 18 200848374 【I¾ 參考例l / 水 FeCl3 h2so4 025 0.42 寸 ο 00 實施例7 FeCl3 h2so4 0.98 水 FeCl3 h2so4 0.98 寸· 實施例6 FeCl3 h2so4 0.98 水 FeCl3 h2so4 0.25 0.18 in d ο 實施例5 FeCl3 h2so4 0.98 水 FeCl3 h2so4 0.25 0.73 rn ο 實施例4 FeCl3 h2so4 0.78 水 FeCl3 VO 0.25 0.82 cn g 實施例3 FeCl3 0.90 水 FeCl3 h2so4 νο 0.25 0.85 CN 實施例2 FeCl3 0.90 h2so4 r-H r-H 1.05 Ό 〇 o 實施例I FeCl3 0.90 I cn p; r—H 1.54 in c3 Fe/Si 衝突後之添加 成分 鐵元素(Fe)濃度 (g^) 氧化矽(Si02)濃 度(於) Si/Fe(莫耳比) 濁度 保存安定性(天) 衝突混合條 件 最終調整條 件 凝集劑性狀 凝集劑性能 ροε : 你寒 餾1^:(58¾ ^SNS5 - 61 JI>06I 丨fes/9 寸 sooodl 200848374 [實施例8、q 為,^中’於衝突混合中之氯化鐵水溶液之混合量 溶液全量之;^ 1氧1 化矽水處理凝集劑製造中所使用之矽酸鹽水 數,剩餘部鐵元素(Fe)變化為表2所示之莫耳倍 獲得鐵,77之氣化鐵水溶液添加量與實施例5同樣地調整, ^保存I定凝集劑。所得水處理凝集劑之凝集性能 [表 2] ^ ^ ° 實施例 8 實施例 9 實施例 10 參考比 較例1 參考比 衡哭混 合條件 與石夕酸納衝 突混合之原 料成分 FeCl3 H2S04 FeCl3 H2SO4 FeCl3 H2S〇4 Τ-Λ. \7ι\ Δί 整條件 加成分 JA3 0.5 1.00 — 水 FeCl3 水 FeCl3 水 FeCl3 H2SO4 H2SO4 H2SO4 凝集劑 性狀 鐵元素(Fe) 濃度(g/L) -----^ 75 75 37 (3.45) (3.45) (3.45) 氧化石夕 (Si02)濃度 (g/L) 20 20 20 (1.82) (1.5) (2.0) Si/Fe(莫耳 比) 0.25 0.25 0.5 0.4 0.53 pH 0.73 0.73 1.01 1 1 凝集劑 濁度 ----- --------- ^03 0.4 0.4 性能 保存安定性 (天_ 40 39 50 45 33200848374 is described as the original; the hard agent can also be used to make 2L in 1 minute. In this way, after the polymerization of the polymerized rock acid (oxidized stone), the water is added to the aqueous solution of the ferric chloride in the reaction vessel. The acid is extremely manufactured, and it is expected to have a longer-term preservation stability than the iron-oxidized stone shui water-reducing agent manufactured by the prior art. The iron and oxidation treatment agglutination agent obtained by the maintenance method is more finely mosquito-like, and the pH obtained from the Γβ and AL wood is preferably 0·3~h5, and more preferably becomes 20^100^. ^ ^Tii\2〇^12〇g/L ? l〇g/L~50gT method ^ Widely becomes 1〇g/L~zero' is better, by neglecting the oxygen obtained under the above conditions, As described in the following examples, it is also possible to store gelatinized material at 3 (rc, ^j, and 3). Moreover, due to the ^^^^, the suspected agent can reduce the transportation cost. In the economy i, the gas system is made acidic, so it can also be used as a pH adjusting agent for the pH of the agglomerating agent, and the pH of the collector is not changed under the iron concentration. The inorganic acid is not particularly limited, and sulfur (or) can be suitably used. That is, in the present invention, it includes the following forms. (3) In the above (1), (2)中,于冲人* :; Adjusting the pH to obtain the iron of the target: Xi: IP080246/SF-1907f 13 200848374 Adjustment (P4ii^A (in the case of 2 items in the case of conflict mixing by adding ^ plus 1Γ in the conflict mixing step In the middle, 1 2 ======', and this is added to the heart salt mixing step and the weave surface is added to the conflict. The iron_oxy_water treatment agglutinating agent can directly make the real = release to the appropriate (four) degrees. The use of the water treatment agent as various drainages is exemplified in more detail. However, the present invention is not limited to (1) conflict mixing equipment, (iron-oxidized stone water treatment aggregating agent manufacturing apparatus) 泸1 The γ submandatory reaction 1^ ' is based on the pipe diameter of the self-throttle portion (the inner 1Gmm raw material supply pipe 4 supplies the _ aqueous solution, the 疋 疋 ^ L pipe diameter (inner diameter) is Ummx length 10 ugly raw material supply The iron aqueous solution was mixed and mixed in the reaction unit 5, and the mixed liquid was taken out from the discharge 'pipe diameter (inner diameter) of 6 mm x length 30 mm). The two raw material supply pipes 4 and 4 of the γ ϋΐ ϋΐ ί device were used. The angle of the formation is 90 degrees. (Λ) Viscosity determination. Using the tuning fork vibrating viscometer of A&D Co., Ltd. in the capture test (3) Evaluation of agglutination performance in the tap water t addition high station (and system (four) water quality test adjustment The turbidity 2 〇 is used as the test water for the bottle cup ^^ est). In the l〇〇〇ml δ type test water, the water is equivalent to 1L Add a coagulant to the method of 5 beer, stir at a stirring speed of 150 rpm for 5 minutes, then stir at a stirring speed of 50 rpm for 1 minute, and then, after standing for 1 minute, take 5 〇ml of the supernatant. _ Green, the water treatment performance of the iron-iron oxide water treatment aggregating agent in the county. IP080246/SF-1907f 14 200848374 (4) Evaluation of preservation stability The iron-phosphorus oxide water treatment agglutinating agent is placed in 3 (rc, the degree of visual judgment is 'the number of days that the scaly conglomerate is _ stability. m / sale of sodium citrate (aqueous solution of citrate · · Si 〇 2 concentration 28 mass 〇 / 〇, 』 2 asO Mobi 丄 (5) diluted with water, become a water soluble solution of 2% concentration machine f 39% by mass of ferric chloride solution (iron salt aqueous solution) 'Ϊΐ成J = iron concentrated Ϊ 19〇g/L of aqueous solution. These aqueous solutions are respectively π: supplied from the original supply to the official 4 at a flow rate L〇L/min The iron sulphate soda supply pipe 4' is supplied with an aqueous solution of ferric chloride at a flow rate of 99 L/min, and is mixed with riHi, and taken out from the discharge pipe 6. The ferroniobium-deuterated hydrazine is obtained in about 2 minutes and 40 seconds. The agglutinating agent is treated with 5 L. The flow rate of the aqueous sodium acid solution and the aqueous solution of ferric chloride is ia8 m/s and 13 respectively, and the flow rate of the water treatment agent is discharged from the discharge pipe is Um/s. The iron oxide concentration of the oxidized caribene is 3 lg/L, the Si/Fe molar ratio is U1, and the ^ is the storage stability under the machine of 37. The results are shown in Table 1. The iron obtained in Example 1 - The pH of the agglutinating agent is adjusted to 1.05 by the oxidation of the oxidized stone, and the sulfuric acid is added until the iron is produced, and the agglutination performance and preservation stability of the self-treated aggregating agent are achieved. Table b, Knife, 'Example 3> The iron-oxidized dream water obtained in Example 1 was agglomerated into an aqueous solution of ferric chloride and sulfuric acid to dilute the water I, and the iron was separated, and the concentration of f became a bucket. The ratio is 0·25, and the pH is 〇·85. With IP080246/SF-1907f 15 200848374 aqueous solution of ferric chloride and sulfuric acid until it becomes the final iron _ oxidized stone ί ί ί ί ί ί, _ _ _ _ _ _ _ _ _ _ _ _ i treatment of broken _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ Diluted with water, it becomes the aqueous solution of water-soluble iron and inorganic acid in the concentration of the gorge, and the gasification of the city f 38 f% is diluted, and then 48% by mass of sulfuric acid is added to become a sulfuric acid concentration, a /sfl iron desert 258g / L of aqueous solution of ferric chloride. Use these water soluble to supply the F ^ gift quantity H / d11 to the Wei Cai solution, from iy, 2 Z1 to the flow of 10.9L / mm of sulfurized steel containing sulfuric acid to dissolve 5' The reaction unit 5 performs collision mixing and is taken out from the discharge pipe 6. The argon oxidation treatment is used to condense the Wei salt solution of the sulphate A part of the reaction liquid (this is also referred to as "the partial flow rate of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of the aqueous solution of In the mixed step of the conflict, the mixed mixture of the iron salt solution in conflicts is ί 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 对于 夕 夕 夕 夕 夕 夕 夕 夕 夕 夕 夕 夕Element (9) 'Iron element (4) becomes part of the mixture obtained from (4) times Moules 0. There is no oxidized stone gelatin compound 4im partial mixture of (10) 2 concentrated material, 42g/L ' Si/Fe Mo Erbi It is ΐ·28, and the pH is 1·〇8. 500ml was placed in a container, and 460 ml of water m% by weight of an aqueous solution of iron oxide was added thereto, and a si〇2 sprinkling helmet was obtained, and the iron concentration was 60 g/L. The Si/Fe molar ratio was 〇25, pH is 〇82: The oxidized mash is fine (8). Wei this iron_oxygen water treatment agglutinating agent=====minutes', this water treatment agglutinating agent agglutination IP080246/SF-1907f 16 200848374 [Example 5] In addition to the sodium citrate aqueous solution, the Si0:2 concentration becomes 9 〇g/L, ferric chloride containing sulfuric acid was dissolved in water, the concentration of ferric chloride was 264 g/L, and the concentration of sulfuric acid was 2 〇. Other than that, the same reaction as in Example 4 was carried out, and the helmet was obtained in about 2 minutes and 40 seconds.黄 Gel yellowish brown transparent part of the mixture 5L. The concentration of Si〇2 in this partial mixture was 47 g/L, the iron concentration was 8, the molar ratio of the chest was 1.02, and the pH was 1.58.曰^, 'In the above conflict mixing step, the mixing amount of the conflict-mixed ferric chloride aqueous solution is the acid used in the manufacture of the agglomerating agent for the iron-cerium oxide water treatment, the total amount of the aqueous solution _ element (9), iron element (4) Become. %倍之吾.仰 ft Ξ Ξ 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft ft L, iron concentration of 75g / L, Si / pe molar pH of 0.73 of iron - oxidized stone evening water treatment agglutination agent 118 bias. The production of the iron-oxygen stone water treatment coagulation _ is self-touch mixing and begins to lie, and the agglutination agent reads the missing silk bond (four) domain 丨. X This water [Example 6] In Example 5, the mixture was made by conflict mixing, such as 2 concentrated to 43 sand · Mo Er ratio is l.G2, PH is part of i.58 mixed 8^ liquid ^^ g 31_ ' 4G f amount % ferric chloride aqueous solution ^ : 匕Γο,2ΓηΤ^ degree is ¥, iron concentration is lion condensed by =1, and the concentration of Si 〇 2 produced by the mixture of Example 5 is 43 g/L. The Si/Fe molar ratio is 丨〇2, the pH is 丨^, and (10)^ is placed in a container, and water-quality* IP080246/SF-1907f 17 200848374 110 ml, 50% by mass sulfuric acid 6.5 ml, and Si are obtained. The concentration of 〇2 is 25g/L, the iron concentration is 47g/L, the Si/Fe molar ratio is 〇·5, and the pH is 0.98 iron _ oxidized stone at the night water at $ 946ml. The production of this iron-oxidized second water treatment aggregating agent was started from the conflict mixing for about 5 minutes, and the agglutination performance and storage stability of the water treatment aggregating agent are shown in Table 1. [Reference Example 1] Commercially available sodium citrate (Si〇2 concentration: 28% by weight, Si〇2/Na20 molar ratio 3 is diluted with water, and s: tintin, s = liquefaction is introduced into the y in stirring within one hour. Moisture = ====:: Acid/if 40g/L, ΡΗ2·0 Oxide sol solution 2L. Add this test to the oxidized $ 2 solution, adjust to _, and mature at room temperature for 3 hours. / Glue to take this oxidized stone sol sol 200ml, add water 5 〇 ml and % ^ gluten 15Gml, get Si 〇 2 concentration of 2 ^ K / ^ 匕 Mo Er ratio is G.25, pH is 〇 42 (10) i f75 catch ' Si/Fe manufactures this iron and oxygen cut 7]^^ cut water treatment condensation 40_. It takes 4 hours == frequency to manufacture and the stability is shown in the table. This water treatment, the difficult performance and protection of the county agent IP080246/SF-1907f 18 200848374 [I3⁄4 Reference Example 1 / Water FeCl3 h2so4 025 0.42 inch ο 00 Example 7 FeCl3 h2so4 0.98 Water FeCl3 h2so4 0.98 inch · Example 6 FeCl3 h2so4 0.98 Water FeCl3 h2so4 0.25 0.18 in d ο Example 5 FeCl3 h2so4 0.98 Water FeCl3 h2so4 0.25 0.73 rn ο Example 4 FeCl3 h2so4 0.78 Water FeCl3 VO 0.25 0.82 cn g Example 3 FeCl3 0.90 Water FeCl3 h2so4 νο 0. 25 0.85 CN Example 2 FeCl3 0.90 h2so4 rH rH 1.05 Ό 〇o Example I FeCl3 0.90 I cn p; r-H 1.54 in c3 Fe/Si Post-conflict additive iron element (Fe) concentration (g^) yttrium oxide (Si02) Concentration (in) Si/Fe (Morby ratio) Turbidity Preservation stability (days) Conflict mixing conditions Final adjustment conditions Aggregant properties Aggregator performance ροε : You cold distill 1^: (583⁄4 ^SNS5 - 61 JI&gt ;06I 丨fes/9 inch sooodl 200848374 [Example 8, q is, ^中' the total amount of the mixed solution of the ferric chloride aqueous solution in the conflict mixing; ^ 1 Oxygen 1 used in the treatment of agglomerated water The number of citrate water was changed to the remaining iron element (Fe) to obtain iron in the molar amount shown in Table 2, and the amount of the aqueous solution of the vaporized iron in 77 was adjusted in the same manner as in Example 5, and the I set aggregating agent was stored. Aggregation performance of the obtained water treatment aggregating agent [Table 2] ^ ^ ° Example 8 Example 9 Example 10 Reference Comparative Example 1 Reference raw material crying mixing condition and the composition of the mixture of the metal salt of the mixture of FeCl3 H2S04 FeCl3 H2SO4 FeCl3 H2S 〇4 Τ-Λ. \7ι\ Δί Entire condition plus composition JA3 0 .5 1.00 — Water FeCl3 Water FeCl3 Water FeCl3 H2SO4 H2SO4 H2SO4 Aggregator Properties Iron (Fe) Concentration (g/L) -----^ 75 75 37 (3.45) (3.45) (3.45) Oxide Oxide (Si02) Concentration (g/L) 20 20 20 (1.82) (1.5) (2.0) Si/Fe (Morby ratio) 0.25 0.25 0.5 0.4 0.53 pH 0.73 0.73 1.01 1 1 Aggregate turbidity --------- ------ ^03 0.4 0.4 Performance preservation stability (day _ 40 39 50 45 33

FeCl3 :氯化鐵水溶液 H2S04:硫酸 參考比較例1、2 :日本特許3700892號所揭示之水處理凝集劑 鐵原素濃度:實細^、參考比較例1及2之括肋标重量%加%) IP080246/SF-1907f 20 200848374 保存安定性··參考比較例1及2在室溫,其餘在30°C [實施例10] 除了矽酸鋼水溶液之Si〇2濃度為90g/L、含有硫酸之氯化 鐵水溶液之氯化鐵濃度為270g/L以及硫酸濃度為31g/L以 =卜,與實施例4同樣進行反應,以約2分40秒獲得無氧化矽 凝膠=凝膠的黃褐色透明中間混合液5L。此部份混合液之 Si〇2濃度為47g/L、鐵濃度為44g/L、Si/Fe莫耳比為丨00, 為U7。 … Ρ π 士 ’上述衝突混合步驟中,經衝突混合之氯化鐵水溶液之 ; 混合量為,相對於鐵-氧化矽水處理凝集劑製造時所使用之矽 酸f水溶液全量中的矽元素(Si),鐵元素(Fe)成為丨.00倍莫耳 之量。 、 产外凡部物屁合液5〇〇ml,於其中添加水563ml、39質量% 2^鐵!fm卜5G f量%硫酸4.4ml,獲得Si〇2濃度為 i〇g/L ’ =度為37g/L,職莫耳比為〇 5,pH為ι 〇ι之鐵_ ίίΤί處職細1184ml。製造此鐵氧切核理凝隼劑 集劑之綾集性能及保存安定性示於表2。 [參考比較例1、2] 辦ίΐ所tit考比較例1、2係專利文獻3(特許第3700892 ΐ隹、魏鈉之方法所製造之鐵·氧化石夕水處理凝ΐ劑之 集角彳之氧化砍;辰度略低濃度者及略$濃 實施例K)所得之水處理凝集^目略^辰度者。鐵浪度及阳與 以實水ff疑集劑之性能比較, 度者、高濃度者相比,均得到j好乳化矽濃度稍低濃 進而一之保;===, IP080246/SF-1907f 200848374 比在比較參考例中之保存 嚴苛的齡。師麵溫為更 預測以本發明製造方法所得 保存文定性,可 之可使用之反應器概略圖 圖1為適用於本發明製造方法 (Υ字管型反應器部份為剖面圖)。 【主要元件符號說明】 1 2 3 鐵鹽水溶液(或包含_及錢酸之水練)之儲存槽 石夕酸鹽水溶液儲存槽 γ字型反應器 4 原料供給管 4’ 原料供給管 5 反應部 6 排出管 IP080246/SF-1907f 22FeCl3: aqueous solution of ferric chloride H2S04: sulfuric acid reference comparative example 1, 2: concentration of iron-treated agglutinating agent disclosed in Japanese Patent No. 3700892: actual fine ^, reference to comparative examples 1 and 2, rib weight % plus % IP080246/SF-1907f 20 200848374 Preservation stability · Refer to Comparative Examples 1 and 2 at room temperature, and the rest at 30 ° C [Example 10] In addition to the concentration of Si〇2 in a citric acid steel aqueous solution of 90 g/L, containing sulfuric acid The ferric chloride aqueous solution had a ferric chloride concentration of 270 g/L and a sulfuric acid concentration of 31 g/L to be in the same manner as in Example 4, and a non-cerium oxide gel = gel yellow was obtained in about 2 minutes and 40 seconds. Brown transparent intermediate mixture 5L. The mixed solution had a Si〇2 concentration of 47 g/L, an iron concentration of 44 g/L, and a Si/Fe molar ratio of 丨00, which was U7. ... Ρ π 士 'The above-mentioned conflict mixing step, the conflict-mixed aqueous solution of ferric chloride; the amount of hydrazine in the total amount of citric acid f aqueous solution used in the manufacture of the agglomerating agent for iron-yttria water treatment ( Si), the iron element (Fe) becomes 00.00 times the molar amount. 5,ml of water, add 563ml of water, 39% by mass of 2^ iron! fm Bu 5G f amount of 4.4ml of sulfuric acid, and obtain the concentration of Si〇2 as i〇g/L ' = The degree is 37g/L, the occupational molar ratio is 〇5, the pH is ι 〇ι iron _ ίίΤί, the job is fine 1184ml. The collection performance and storage stability of the ferrite-cutting gelling agent collector are shown in Table 2. [Reference Comparative Example 1 and 2] The 集 ΐ t 比较 比较 比较 1、 1、 1、 1、 1、 1、 1、 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较 比较The oxidative chopping; the slightly lower concentration of the Chen and the slightly more concentrated Example K) obtained by the water treatment agglutination. Compared with the performance of iron wave and yang and real water ff suspect agent, compared with those of high concentration and high concentration, the concentration of emulsified cesium is slightly lower and stronger, and then one is guaranteed; ===, IP080246/SF-1907f 200848374 is more stringent than the preservation in the comparative reference example. The surface temperature of the teacher is predicted to be obtained by the manufacturing method of the present invention. The outline of the reactor which can be used is shown in Fig. 1 which is suitable for the production method of the present invention (the cross-sectional view of the reactor portion of the 管-tube type). [Explanation of main component symbols] 1 2 3 Storage solution of iron salt aqueous solution (or water containing _ and hydroxy acid) Storage tank aqueous solution storage tank γ-type reactor 4 Raw material supply pipe 4' Raw material supply pipe 5 Reaction part 6 Discharge pipe IP080246/SF-1907f 22

Claims (1)

200848374 •、申請專利範園: ,麵絲在藉由使 睹,句冬蚀制、Γ,鐵现欠/谷液反應而製造鐵_氧化矽水處理劑 法,1中上、1項之鐵·氧化石夕水處理凝集劑之製造方 沒入混合㈣中,經触混合之麵水溶液之 二2、、=對於^_氧切水處理賴狀製造巾所使用之 耳以二t液之全量中石夕元素(si),鐵元素㈣成為0.5倍莫 .,利範圍第1或2項之鐵_氧化矽水處理凝集劑之製造 ί、1其中該鐵-氧化矽水處理凝集劑之ί>Η為0.3〜1.5,鐵 、辰度為 20g/L〜.120g/L,Si〇2 濃度為 i〇g/L〜50g/L,且 Si/Fe 冥耳比為1以下。 4·=申1專利範圍第1至3項中任一項之鐵_氧化矽水處理凝集 j之製造方法,其包含於衝突混合後所得之混合物中添加剩 餘部份之鐵鹽水溶液之步驟。 5·如申凊專利範圍第1至3項中任一項之鐵-氧化石夕水處理凝集 劑之製造方法,其包含於衝突混合後所得之混合物中添加^ 餘部份之鐵鹽水溶液以及無機酸之步驟。 IP080246/SF,i907f 23200848374 • Applying for the patent garden: The surface silk is made by the method of making 睹, sentence winter etching, Γ, iron owe/cold reaction, iron 矽 矽 矽 water treatment agent method, 1 middle and upper iron ·The manufacturer of the oxidized stone water treatment agglomerating agent is not mixed into the mixture (4), and the surface of the mixed aqueous solution is 2nd, 2, and the total amount of the two liquids used for the treatment of the water is treated. The medium-stone element (si), the iron element (four) becomes 0.5 times Mo., the iron of the range 1 or 2 is produced _ 矽 矽 处理 处理 ί 制造 1 1 1 1 1 1 1 1 1 该 该 该 该 该 该 该 该 该 该 该 该 该 该 该 该 该The enthalpy is 0.3 to 1.5, the iron and the elongation are 20 g/L to 1.120 g/L, the Si 〇 2 concentration is i 〇 g/L 〜 50 g/L, and the Si/Fe phantom ratio is 1 or less. The method for producing an iron-hydrazine oxide water treatment agglomerate according to any one of claims 1 to 3, which comprises the step of adding the remaining portion of the aqueous iron salt solution to the mixture obtained after the conflict mixing. The method for producing an iron-stone oxide water treatment aggregating agent according to any one of claims 1 to 3, which comprises adding the remaining portion of the iron salt aqueous solution to the mixture obtained after the conflict mixing and The step of mineral acid. IP080246/SF, i907f 23
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