JPH05155604A - Production of calcium hypochlorite - Google Patents
Production of calcium hypochloriteInfo
- Publication number
- JPH05155604A JPH05155604A JP34844891A JP34844891A JPH05155604A JP H05155604 A JPH05155604 A JP H05155604A JP 34844891 A JP34844891 A JP 34844891A JP 34844891 A JP34844891 A JP 34844891A JP H05155604 A JPH05155604 A JP H05155604A
- Authority
- JP
- Japan
- Prior art keywords
- calcium
- emulsion
- calcium hypochlorite
- mother liquor
- water
- 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.)
- Granted
Links
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000292 calcium oxide Substances 0.000 claims abstract description 16
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 18
- 239000012452 mother liquor Substances 0.000 abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 17
- 239000000839 emulsion Substances 0.000 abstract description 15
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract description 14
- 239000000920 calcium hydroxide Substances 0.000 abstract description 14
- 229910001861 calcium hydroxide Inorganic materials 0.000 abstract description 14
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000460 chlorine Substances 0.000 abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 abstract description 2
- 229910001902 chlorine oxide Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 16
- 238000005660 chlorination reaction Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/04—Hypochlorous acid
- C01B11/06—Hypochlorites
- C01B11/064—Hypochlorites of alkaline-earth metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/04—Hypochlorous acid
- C01B11/06—Hypochlorites
- C01B11/062—Hypochlorites of alkali metals
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は従来から使用されている
水酸化カルシウムの代わりに、酸化カルシウムを直接原
料とする次亜塩素酸カルシウムの製造法に関する。次亜
塩素酸カルシウムは水の消毒剤として利用され、プール
や汚水処理等に多く使用されている。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing calcium hypochlorite by directly using calcium oxide as a raw material instead of the conventionally used calcium hydroxide. Calcium hypochlorite is used as a disinfectant for water and is often used in pools, sewage treatment, etc.
【０００２】[0002]
【従来の技術】 技術的背景 次亜塩素酸カルシウムの製造法は、水酸化カルシウムを
水、又は反応後の濾過液に乳化し、その乳化液に塩素ガ
スを吹き込み次亜塩素酸カルシウムを生成させ濾過回収
後乾燥して製品とする方法が一般的である。また、アル
カリ源として水酸化カルシウムの他に水酸化ナトリウム
と併用して使用する場合もある。製品を回収した後の濾
過液（母液）中には次亜塩素酸カルシウムが溶存してお
り、これを廃棄すると中和処理が必要になる他に、収率
ロスにつながり製造コストが割高になる。このため従来
の製造法に於いては、この濾過液を水酸化カルシウムの
乳化液に利用する方法も採られている。しかしながらこ
れだけでは水バランスが採れず一部の濾過液を廃棄して
いるのが実態であり、このための改善策が望まれてい
た。 類似技術 米国特許３２１６４７号には食塩結晶を大きく成長せし
めて次亜塩素酸カルシウム結晶との分離を容易にするた
めに余剰母液を低温減圧下で蒸発濃縮する方法が示され
ているが、食塩結晶にはまだ多量の次亜塩素酸カルシウ
ム結晶が同伴されており食塩の品位は充分ではなく更に
余剰母液を蒸発するために多量のエネルギーを要する欠
点を有する。2. Description of the Related Art Technical Background A method for producing calcium hypochlorite involves emulsifying calcium hydroxide in water or a filtered liquid after reaction, and blowing chlorine gas into the emulsified liquid to produce calcium hypochlorite. A general method is to obtain a product by drying after filtration and recovery. In addition to calcium hydroxide, it may be used in combination with sodium hydroxide as an alkali source. Calcium hypochlorite is dissolved in the filtrate (mother liquor) after the product is collected, and if this is discarded, neutralization treatment is required and yield loss will result, resulting in a high manufacturing cost. . Therefore, in the conventional manufacturing method, a method of using this filtrate as an emulsion of calcium hydroxide is also adopted. However, the fact is that the water balance cannot be taken with this alone and some of the filtrate is discarded, and improvement measures for this have been desired. Similar Technology US Pat. No. 321,647 discloses a method of evaporating and concentrating excess mother liquor under low temperature and reduced pressure in order to grow a salt crystal to a large extent and facilitate separation from calcium hypochlorite crystal. Since a large amount of calcium hypochlorite crystals are still entrained therein, the quality of the salt is not sufficient, and there is a drawback that a large amount of energy is required to evaporate the excess mother liquor.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、余剰母液を
生成しない効率的な次亜塩素酸カルシウムの製造法を提
供する事を目的とする。SUMMARY OF THE INVENTION It is an object of the present invention to provide an efficient method for producing calcium hypochlorite which does not produce excess mother liquor.
【０００４】[0004]
【課題を解決するための手段】 発明の構成 本発明の次亜塩素酸カルシウムの製造法はつぎの構成か
らなる。塩素化反応の原料として水酸化カルシウムの代
わりに酸化カルシウムを使用する。 詳細な説明 次亜塩素酸カルシウムの製造には、塩素の他に水酸化カ
ルシウムを主原料として使用される。プロセスによって
は苛性ソーダを併用する事もある。従来、水酸化カルシ
ウムの代わりに酸化カルシウムを置換使用することが考
えられなかった理由は、水と酸化カルシウムを直接接触
するとかなりの発熱を生じる事や均一に分散した乳液に
なりにくい事等があったからである。余剰母液を少なく
するために、母液中に水酸化カルシウムを乳化する場合
もあるが、これだけでは通常、水バランスが取りにくく
多少の余剰母液が副生する。またこの代わりに酸化カル
シウムを使用した場合水との接触で急激な発熱を生じ、
母液中の次亜塩素酸カルシウムを分解させる事になり、
収率ロスにつながる。Means for Solving the Problems The method for producing calcium hypochlorite according to the present invention has the following composition. Calcium oxide is used instead of calcium hydroxide as a raw material for the chlorination reaction. Detailed Description In the production of calcium hypochlorite, calcium hydroxide is used as a main raw material in addition to chlorine. Depending on the process, caustic soda may be used together. Conventionally, the reason why it has not been considered to use calcium oxide instead of calcium hydroxide is that direct contact between water and calcium oxide causes considerable heat generation, and it is difficult to form a uniformly dispersed emulsion. This is because the. In order to reduce the excess mother liquor, calcium hydroxide may be emulsified in the mother liquor. However, this alone usually makes it difficult to balance the water, and some excess mother liquor is by-produced. When calcium oxide is used instead of this, a sudden heat generation occurs on contact with water,
It will decompose calcium hypochlorite in the mother liquor,
This leads to yield loss.
【０００５】この改善策として、反応槽にジャケットま
たはコイルを取り付けてブライン冷却する方法が考えら
れるが、発熱は酸化カルシウムと水とが接触した瞬間に
生ずるため、十分な対応ができない。しかしながら母液
中に苛性ソーダを混合した後に酸化カルシウムを乳化す
ると発熱による温度上昇も大幅に減少し、次亜塩素酸カ
ルシウムの分解もなく均一な乳化液を得る事を発見し
た。As a remedy for this, a method in which a jacket or a coil is attached to the reaction tank to cool the brine is conceivable. However, heat is generated at the moment when calcium oxide and water come into contact with each other, so that it cannot be sufficiently dealt with. However, it was discovered that when calcium oxide is emulsified after mixing caustic soda into the mother liquor, the temperature rise due to heat generation is greatly reduced, and a uniform emulsion is obtained without decomposition of calcium hypochlorite.
【０００６】[0006]
【実施例】本発明の実施例を示すが、本発明はこれらに
限定されるものではない。EXAMPLES Examples of the present invention are shown below, but the present invention is not limited thereto.
【０００７】実施例１ 次亜塩素酸カルシウム製造に当たっての塩素化用原料液
（母液のリサイクル液を含む各種の液を適当な処理を施
した液）8,４５５ｇに４９％苛性ソーダ３８０ｇ混合し
た後、攪拌しながら酸化カルシウム粉末を徐々に４７３
ｇを混合し均一な乳液とする。この間、乳化液の温度上
昇は、外部冷却をしなかったにもかかわらず、約２℃程
度でおさまり２５℃を越えることはなかった。この乳液
9,３０８ｇの組成は、次亜塩素酸カルシウム１2.6 ％、
食塩１6.３％、アルカリ7.７、水６2.８％、その他0.６
％であった。この乳液を攪拌しながら、塩素ガスを約３
時間吹き込み塩素化を終了した。塩素化終了後の塩化液
の組成は、次亜塩素酸カルシウム１7.７％、食塩２0.１
％、アルカリ0.９％、水６0.４％、その他0.９％であっ
た。この場合の次亜塩素酸カルシウムの分解は、極めて
わずかだった。この液を通常の処理（次亜塩素酸カルシ
ウムの結晶と溶液を分離し、結晶は乾燥後製品とし、溶
液は塩素化用原料としてリサイクルする。）して、製品
とした時の次亜塩素酸カルシウムの濃度は７６％であ
り、通常の製品と遜色ないものであった。Example 1 In the production of calcium hypochlorite, 455 g of a raw material liquid for chlorination (a liquid obtained by appropriately treating various liquids including a mother liquor recycling liquid) was mixed with 380 g of 49% caustic soda, Gradually 473 calcium oxide powder while stirring
g to form a uniform emulsion. During this period, the temperature rise of the emulsion was suppressed to about 2 ° C. and never exceeded 25 ° C., though the external cooling was not performed. This emulsion
The composition of 9,308 g is 12.6% calcium hypochlorite,
Salt 16.3%, Alkaline 7.7, Water 62.8%, Others 0.6
%Met. While stirring this emulsion, about 3 chlorine gas was added.
The time-blown chlorination was completed. The composition of the chlorinated solution after the completion of chlorination is calcium hypochlorite 17.7%, salt 20.1.
%, Alkali 0.9%, water 60.4%, and other 0.9%. The decomposition of calcium hypochlorite in this case was extremely slight. This solution is subjected to normal treatment (the crystals of calcium hypochlorite are separated from the solution, the crystals are dried and then made into a product, and the solution is recycled as a raw material for chlorination). The calcium concentration was 76%, which was comparable to that of ordinary products.
【０００８】比較例１ 次亜塩素酸カルシウム製造に当たっての塩素化用原料液
（母液のリサイクル液を含む各種の液を適当な処理を施
した液）8,４５５ｇに酸化カルシウム粉末４７３ｇを実
施例と同様な操作で混合を開始したが、酸化カルシウム
が液に接触するとすぐ、激しく発熱し液温度が２１℃か
ら急激に３０℃を越え、ガス発生（次亜塩素酸カルシウ
ムの分解ガスとおもわれる）が、生じたので実験を中断
した。COMPARATIVE EXAMPLE 1 In the production of calcium hypochlorite, 455 g of a raw material liquid for chlorination (a liquid obtained by appropriately treating various liquids including a recycled liquid of a mother liquor) and 473 g of calcium oxide powder were used. Mixing was started by the same operation, but as soon as calcium oxide came into contact with the liquid, it vigorously generated heat and the liquid temperature rapidly exceeded 30 ° C from 21 ° C, generating gas (this is considered to be decomposition gas of calcium hypochlorite). However, the experiment was stopped because it occurred.
【０００9 】比較例２ 次亜塩素酸カルシウム製造に当たっての塩素化用原料液
（母液のリサイクル液を含む各種の液を適当な処理を施
した液）９，５０４ｇに４９％苛性ソーダ４２８ｇ混合
した後、攪拌しながら水酸化カルシウム粉末を徐々に５
１５ｇを混合し均一な乳液とする。この間、乳化液の温
度上昇は、外部冷却をしなかったにもかかわらず、約２
℃程度でおさまり２５℃を越えることはなかった。この
乳液１０，４４７ｇの組成は、次亜塩素酸カルシウム１
2.5 ％、食塩１6.３％、アルカリ7.4 、水６3.2 ％、そ
の他0.６％であった。この乳液を攪拌しながら、塩素ガ
スを約３時間吹き込み塩素化を終了した。塩素化終了後
の塩化液の組成は、次亜塩素酸カルシウム１7.3 ％、食
塩２0.１％、アルカリ0.９％、水６0.9 ％、その他0.8
％であった。この場合の次亜塩素酸カルシウムの分解
は、極めてわずかだった。この液を通常の処理（次亜塩
素酸カルシウムの結晶と溶液を分離し、結晶は乾燥後製
品とし、溶液は塩素化用原料としてリサイクルする。）
して、次亜塩素酸カルシウムの濃度が７６％の製品を得
た。但し、この場合、必要母液をリサイクルしても、31
9gの母液が余った。Comparative Example 2 In the production of calcium hypochlorite, 9,504 g of a raw material liquid for chlorination (a liquid obtained by appropriately treating various liquids including a recycling liquid of a mother liquor) was mixed with 428 g of 49% caustic soda. Gradually add 5 powders of calcium hydroxide while stirring.
Mix 15 g to make a uniform emulsion. During this time, the temperature rise of the emulsion was about 2 even though external cooling was not performed.
The temperature did not exceed 25 ° C at a temperature of about 25 ° C. The composition of 10,447 g of this emulsion is calcium hypochlorite 1
It was 2.5%, salt 16.3%, alkali 7.4, water 63.2%, and other 0.6%. While stirring this emulsion, chlorine gas was blown therein for about 3 hours to complete the chlorination. After completion of chlorination, the composition of the chlorinated solution is as follows: calcium hypochlorite 17.3%, salt 20.1%, alkali 0.9%, water 60.9%, other 0.8.
%Met. The decomposition of calcium hypochlorite in this case was extremely slight. This solution is subjected to normal treatment (calcium hypochlorite crystals are separated from the solution, the crystals are dried and then used as a product, and the solution is recycled as a raw material for chlorination.)
Thus, a product having a calcium hypochlorite concentration of 76% was obtained. However, in this case, even if the necessary mother liquor is recycled, 31
9 g of mother liquor was left over.
【００１０】[0010]
【発明の効果】酸化カルシウムを水酸化カルシウムの代
わりに使用する事によって酸化カルシウムが水と反応し
て水酸化カルシウムを生成するのに要する水の分だけ反
応系全体の水バランスを改善する事ができ、余剰母液の
副生を防止できる。By using calcium oxide in place of calcium hydroxide, the water balance of the entire reaction system can be improved by the amount of water required for calcium oxide to react with water to produce calcium hydroxide. It is possible to prevent by-product of excess mother liquor.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 釜土 良則 新潟県中頸城郡中郷村大字藤沢950 日本 曹達株式会社二本木工場内 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Yoshinori Kadochi 950 Fujisawa, Nakago-mura, Nakakubiki-gun, Niigata Nihongi Plant, Nippon Soda Co., Ltd.
Claims (1)
次亜塩素酸カルシウムの製造法。A method for producing calcium hypochlorite, which comprises using calcium oxide as a raw material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34844891A JP3640677B2 (en) | 1991-12-05 | 1991-12-05 | Production method of calcium hypochlorite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34844891A JP3640677B2 (en) | 1991-12-05 | 1991-12-05 | Production method of calcium hypochlorite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05155604A true JPH05155604A (en) | 1993-06-22 |
| JP3640677B2 JP3640677B2 (en) | 2005-04-20 |
Family
ID=18397076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34844891A Expired - Lifetime JP3640677B2 (en) | 1991-12-05 | 1991-12-05 | Production method of calcium hypochlorite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3640677B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100424006C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
| CN100424005C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
-
1991
- 1991-12-05 JP JP34844891A patent/JP3640677B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100424006C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
| CN100424005C (en) * | 2005-11-21 | 2008-10-08 | 江苏索普（集团）有限公司 | Production of high-efficiency bleaching powder by calcium method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3640677B2 (en) | 2005-04-20 |
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