JPH0986903A - Production of calcium hypochlorite composition tablet whose solubility is controlled - Google Patents
Production of calcium hypochlorite composition tablet whose solubility is controlledInfo
- Publication number
- JPH0986903A JPH0986903A JP7271806A JP27180695A JPH0986903A JP H0986903 A JPH0986903 A JP H0986903A JP 7271806 A JP7271806 A JP 7271806A JP 27180695 A JP27180695 A JP 27180695A JP H0986903 A JPH0986903 A JP H0986903A
- Authority
- JP
- Japan
- Prior art keywords
- alkali
- chlorination
- weight
- calcium hypochlorite
- calcium
- 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
- 239000000203 mixture Substances 0.000 title claims abstract description 47
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000003513 alkali Substances 0.000 claims abstract description 44
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000000460 chlorine Substances 0.000 claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000008267 milk Substances 0.000 claims description 13
- 210000004080 milk Anatomy 0.000 claims description 13
- 235000013336 milk Nutrition 0.000 claims description 13
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 12
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 12
- 239000004571 lime Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 6
- YALMXYPQBUJUME-UHFFFAOYSA-L calcium chlorate Chemical compound [Ca+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O YALMXYPQBUJUME-UHFFFAOYSA-L 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 claims 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 18
- 235000002639 sodium chloride Nutrition 0.000 abstract description 13
- 239000000920 calcium hydroxide Substances 0.000 abstract description 11
- 235000011116 calcium hydroxide Nutrition 0.000 abstract description 11
- 239000011780 sodium chloride Substances 0.000 abstract description 10
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000011575 calcium Substances 0.000 abstract description 4
- 239000012467 final product Substances 0.000 abstract description 4
- 239000005708 Sodium hypochlorite Substances 0.000 abstract description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract 2
- 229910052791 calcium Inorganic materials 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 14
- 238000004090 dissolution Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 6
- 239000001110 calcium chloride Substances 0.000 description 6
- 229910001628 calcium chloride Inorganic materials 0.000 description 6
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 6
- 230000001954 sterilising effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000004061 bleaching Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 238000007908 dry granulation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000007922 dissolution test Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、次亜塩素酸カルシ
ウム組成物錠剤の製造工程において、塩素化工程終末管
理を工夫することにより、新たな手間をかけずなおかつ
再現性良く、溶解性を制御した次亜塩素酸カルシウム組
成物錠剤の製造を可能とするものである。TECHNICAL FIELD The present invention relates to a method for controlling the solubility of a calcium hypochlorite composition tablet by devising control of the terminal chlorination step in the manufacturing process of the tablet, which is highly reproducible and has good reproducibility. The present invention enables the production of tablets of the calcium hypochlorite composition.
【０００２】[0002]
【従来の技術】次亜塩素酸カルシウム組成物は、苛性ソ
ーダ水溶液を塩素化し次亜塩素酸ナトリウムと食塩を生
成させ、このうち食塩を分離し、石灰を加え次亜石灰乳
とし再度塩素化することによって得られる。通常、次亜
塩素酸カルシウムを７０重量％以上含有し、その他アル
カリ，食塩，塩化カルシウムなどを含む。2. Description of the Related Art A calcium hypochlorite composition is prepared by chlorinating an aqueous solution of caustic soda to produce sodium hypochlorite and sodium chloride, of which sodium chloride is separated and lime is added to form hypolimestone milk and chlorinated again. Obtained by Usually, it contains 70% by weight or more of calcium hypochlorite, and also contains alkali, salt, calcium chloride and the like.
【０００３】次亜塩素酸カルシウム組成物は強力な酸化
剤であり、その殺菌漂白効果により、プール，上下水
道，排水の殺菌消毒や、食品・パルプ・繊維の漂白に用
いられている。この次亜塩素酸カルシウム組成物は、慣
用名“高度晒粉”と呼ばれており、流通している形状と
しては顆粒剤と錠剤の２種類がある。このうち顆粒剤は
速効性を求められる場合に用いられ、錠剤は滅菌器，殺
菌筒などに充填され、継続的に使用される。そのため、
顆粒剤では速溶性が、錠剤では遅溶性が求められる。次
亜塩素酸カルシウム組成物錠剤は、上記用途からも遅溶
性であることが望ましく、溶解速度が速いと滅菌器，殺
菌筒への供給回数が増加し、利便性が低下する。この次
亜塩素酸カルシウム組成物錠剤の遅溶化をはかる方法と
して、最終製品中のアルカリ量を増加させるとよいこと
が経験的に知られている。Calcium hypochlorite composition is a strong oxidizer and is used for sterilizing and sterilizing pools, water and sewage and drainage, and bleaching food, pulp and fiber due to its sterilizing and bleaching effect. This calcium hypochlorite composition is commonly called "highly bleached powder", and there are two types of commercially available forms, a granule and a tablet. Of these, granules are used when fast-acting is required, and tablets are filled in a sterilizer, a sterilizing cylinder or the like and continuously used. for that reason,
Granules require fast solubility and tablets require slow solubility. It is desirable that the calcium hypochlorite composition tablet has a slow solubility in view of the above-mentioned applications, and if the dissolution rate is high, the number of times of supply to the sterilizer and the sterilization cylinder increases and the convenience decreases. It has been empirically known that as a method for slowing the dissolution of the calcium hypochlorite composition tablet, it is preferable to increase the amount of alkali in the final product.
【０００４】特公昭４４−１０１９７号には、乾燥造粒
された次亜塩素酸カルシウム組成物に、消石灰または塩
基性塩法で得られたＣａ（ＣｌＯ）2 ６３．８重量％，
Ｃａ（ＯＨ）2 ２１．２重量％，ＣａＣｌ2 ７．３重量
％その他からなる水酸化カルシウムを多量に含む塩基性
次亜塩素酸カルシウムを混合打錠する方法が開示されて
いる。また、特開昭５５−９０４０４号には次亜塩素酸
カルシウム組成物に塩化カルシウムと消石灰を混合打錠
することによる遅溶化方法が示されている。しかし、こ
れらの方法では、固体と固体の混合操作であるため不均
一になりやすく、石灰分のみが溶け残り、残渣となりや
すい欠点があった。Japanese Patent Publication No. 44-10197 discloses a dry granulated calcium hypochlorite composition containing 63.8% by weight of Ca (ClO) 2 obtained by a slaked lime or basic salt method.
Disclosed is a method for tableting a mixture of basic calcium hypochlorite containing a large amount of calcium hydroxide composed of 21.2% by weight of Ca (OH) 2 and 7.3% by weight of CaCl 2 . Further, JP-A-55-90404 discloses a delayed dissolution method by mixing and compressing calcium chloride and slaked lime into a calcium hypochlorite composition. However, these methods have a drawback that they are likely to be non-uniform because they are solid-solid mixing operations, and only lime remains undissolved, leaving residues.
【０００５】また、必要量のアルカリをあらかじめ残し
て終末とする方法もあり、自動管理する方法が特開平５
−３０７０１９に記載されている。特開平５−３０７０
１９はＯＲＰ電位の変化率を用いて塩素化工程の終末自
動管理を行うものであるが、この方法では終末スラリー
での残アルカリ濃度が約１．０重量％以下でなくてはな
らない。つまり特開平５−３０７０１９では、ＯＲＰ電
位は同じ残アルカリ濃度であっても数１０ｍＶのシフト
は避けられず、ＯＲＰ電位の絶対値によって終点管理を
行おうとすると困難を伴う。しかし、ＯＲＰ電位の変化
率は、塩素化終末に近づくと急激に大きくなる。そこ
で、事前に変化率とアルカリ量との関係を求めておけ
ば、反応完了スラリーの残アルカリ量はコントロールで
きることが示されている。だがこの方法でコントロール
が出来るのはスラリーで１．０重量％程度であり、製品
を遅溶化するのに必要な最終製品中のアルカリを５重量
％以上にする場合はＯＲＰ電位変化率による自動管理は
行えず、終末近くになるとアルカリ量を手分析しながら
終末点を決定せねばならず、省力化・自動化が難しい。
さらに、溶解速度の差異により銘柄に差別化をはかろう
とする場合、これに対応したアルカリ分を残すために
は、残アルカリ量を分析しながら塩素化終点を管理せね
ばならず、別途要員を必要とし、省力化の妨げとなる。There is also a method of leaving a necessary amount of alkali in advance and terminating it, and a method of automatic management is disclosed in Japanese Patent Laid-Open No.
-307019. JP-A-5-3070
No. 19 is for automatically controlling the end of the chlorination step using the rate of change of the ORP potential, but in this method, the residual alkali concentration in the end slurry must be about 1.0% by weight or less. In other words, according to Japanese Patent Laid-Open No. 5-307019, a shift of several tens of mV is inevitable even if the ORP potential is the same residual alkali concentration, and it is difficult to manage the end point by the absolute value of the ORP potential. However, the rate of change of the ORP potential rapidly increases near the end of chlorination. Therefore, it has been shown that the amount of residual alkali in the reaction-completed slurry can be controlled by previously obtaining the relationship between the rate of change and the amount of alkali. However, this method can control about 1.0% by weight of the slurry, and when the alkali in the final product required to slow the product is 5% by weight or more, it is automatically controlled by the ORP potential change rate. However, when the end point is reached, the end point must be determined by manually analyzing the amount of alkali, which makes labor saving and automation difficult.
Furthermore, when trying to differentiate the brand due to the difference in the dissolution rate, in order to keep the alkali content corresponding to this, it is necessary to manage the chlorination end point while analyzing the residual alkali amount, and a separate person is required. It is necessary and hinders labor saving.
【０００６】さらに、最近では次亜塩素酸カルシウム組
成物錠剤製品の安全性が求められるため、高含水品（水
分を１０重量％以上含有する）が流通するようになった
が、高温下など保管条件が悪い場合、経時変化を引き起
こし溶解性が変化するなどの問題があった。Furthermore, recently, since the safety of the calcium hypochlorite composition tablet product is required, a high water content product (containing 10% by weight or more of water) has come into circulation, but it is stored at a high temperature or the like. When the conditions are not good, there is a problem that it causes a change over time and the solubility changes.
【０００７】[0007]
【発明が解決しようとする課題】水に溶かした時、残渣
が生じにくく、溶解性の経時変化が少なく、遅溶化され
た次亜塩素酸カルシウム組成物錠剤を得ること、さらに
はその錠剤を製造するにあたり塩素化工程の終末を煩雑
化することなく自動管理できる方法を得ることを目的と
する。[Problems to be Solved by the Invention] To obtain a calcium hypochlorite composition tablet in which a residue hardly occurs when dissolved in water, the solubility is little changed with time, and the solution is delayed, and further the tablet is produced. In doing so, it is an object of the present invention to provide a method capable of automatically controlling the end of the chlorination process without complicating it.
【０００８】[0008]
【問題点を解決するための手段】本発明は、乾燥造粒後
アルカリを添加するのではなく、乾燥工程までにスラリ
ーの状態でアルカリ濃度を高くするものであり、さらに
詳しくは、（次亜石灰乳の）塩素化工程をＯＲＰ電位の
変化率による自動管理にて終末とし、乾燥造粒後アルカ
リを添加するのではなく、乾燥工程までにスラリーの状
態でアルカリ濃度を高くすることにより必要とされるア
ルカリ源を定量自動供給することにより最終製品である
次亜塩素酸カルシウム組成物錠剤の遅溶化をはかる製法
である。According to the present invention, the alkali concentration is increased in the slurry state before the drying step, instead of adding the alkali after dry granulation. The chlorination process (of lime milk) is terminated by automatic control according to the rate of change of the ORP potential, and it is necessary to increase the alkali concentration in the slurry state before the drying process, rather than adding alkali after dry granulation. In this method, the final product, calcium hypochlorite composition tablets, is slow-dissolved by quantitatively and automatically supplying an alkali source.
【０００９】即ち本発明は、 石灰乳と苛性ソーダ水溶
液を塩素化して次亜塩素酸カルシウム組成物を製造する
方法において、塩素化が終了した後、乾燥工程の前にア
ルカリを一定量加えることを特徴とする、組成物中のア
ルカリ濃度が高められた次亜塩素酸カルシウム組成物錠
剤の製造法であり、特には塩素化の終了をＯＲＰ電位の
変化率による自動管理で行うことを特徴とする製造法で
ある。That is, the present invention is a method for producing a calcium hypochlorite composition by chlorinating lime milk and an aqueous solution of caustic soda, wherein a certain amount of alkali is added after chlorination and before the drying step. And a method for producing a calcium hypochlorite composition tablet having an increased alkali concentration in the composition, which is characterized in that the chlorination is completed by automatic control according to the change rate of the ORP potential. Is the law.
【００１０】[0010]
【発明の実施の形態】次亜塩素酸カルシウム組成物は、
苛性ソーダ水溶液を塩素化し次亜塩素酸ナトリウムと食
塩を生成させ、このうち食塩を分離し、石灰を加え次亜
石灰乳とし、再度これを塩素化することによって得られ
る。BEST MODE FOR CARRYING OUT THE INVENTION The calcium hypochlorite composition comprises
It is obtained by chlorinating a caustic soda aqueous solution to form sodium hypochlorite and sodium chloride, separating sodium chloride from this solution, adding lime to form hypocalcinite milk, and chlorinating this again.
【００１１】本発明は、次亜石灰乳の塩素化において、
ＯＲＰ電位変化率による管理により一旦終末とし、不足
する分のアルカリを後から加える。ＯＲＰ電位変化率に
よる終点自動管理では、スラリー中の残アルカリ量は既
知であるから、添加すべきアルカリ量は容易に計算され
るので、必要な分のアルカリを流量積算計等を用いて自
動的に供給すればよい。この際、アルカリの複塩形成に
よる偏析を防ぐため、攪拌機付き貯槽，アジター，ライ
ンミキサーなどで混合するとよい。また、塩素化終了後
のスラリーを遠心分離器にて振りきる際、適当な脱水時
間をとってケーキにアルカリ源をスプレーして加えても
よい。The present invention relates to the chlorination of hypolimite milk,
The end is once determined by the control based on the ORP potential change rate, and the insufficient alkali is added later. In the automatic end point management based on the ORP potential change rate, the amount of residual alkali in the slurry is already known, so the amount of alkali to be added can be easily calculated. Can be supplied to. At this time, in order to prevent segregation due to formation of double salt of alkali, it is advisable to mix in a storage tank with a stirrer, an agitator, a line mixer or the like. Further, when the slurry after chlorination is shaken off with a centrifuge, a suitable dehydration time may be taken and an alkali source may be sprayed and added to the cake.
【００１２】供給するアルカリ源として、塩素化する前
の次亜石灰乳液もしくは濃厚な石灰乳等が考えられる。
このうち塩素化する前の次亜石灰乳液は、有効塩素１０
〜１３重量％，アルカリとして６〜１５重量％を含んで
いる。また、石灰乳を用いる場合は有効塩素濃度低下を
防ぐため濃厚な方がよく１０〜５０％、取り扱いの容易
さから２６〜４０重量％乳を用いると良い。As an alkali source to be supplied, hypochlorite emulsion before chlorination or concentrated lime milk can be considered.
Of these, hypochlorite emulsion before chlorination is available chlorine 10
.About.13% by weight and 6 to 15% by weight as alkali. Further, when lime milk is used, it is preferable that it is concentrated in order to prevent a decrease in effective chlorine concentration, and 10 to 50% milk is used. From the viewpoint of easy handling, it is preferable to use 26 to 40% by weight milk.
【００１３】得られる次亜塩素酸カルシウム組成物を常
法によって打錠すれば錠剤が得られる。A tablet can be obtained by tableting the obtained calcium hypochlorite composition by a conventional method.
【００１４】本発明によって得られる次亜塩素酸カルシ
ウム組成物錠剤の組成は、有効塩素６５重量％から７５
重量％であり、かつ水分が８重量％から１５重量％、全
アルカリが５重量％から１０重量％であるものが好まし
い。The composition of the calcium hypochlorite composition tablet obtained by the present invention has an effective chlorine content of 65% by weight to 75%.
It is preferable that the water content is 8% by weight, the water content is 8% by weight to 15% by weight, and the total alkali is 5% by weight to 10% by weight.
【００１５】本発明の錠剤の溶解速度は３．５〜６．０
ｇ／Ｈｒであり、通常のアルカリ４．５％含有錠剤の溶
解速度８±２ｇ／Ｈｒに比べ遅溶性である。The dissolution rate of the tablet of the present invention is 3.5 to 6.0.
It is g / Hr, which is slower than the dissolution rate of a normal tablet containing 4.5% of alkali of 8 ± 2 g / Hr.
【００１６】また、アルカリ源をスラリー状態で混合す
ることにより、特公昭４４−１０１９７号，および特開
昭５５−９０４０４号の如く固体で混合する場合と異な
り、溶解残渣を生成しにくいといった特徴も有してい
る。さらに、製品の高温下で保管しても溶解性の変化が
少ないといった特長も有す。In addition, by mixing the alkali source in a slurry state, unlike the case of mixing in a solid state as in JP-B-44-10197 and JP-A-55-90404, it is difficult to form a dissolution residue. Have Furthermore, it has the advantage that the solubility of the product does not change even when stored at high temperatures.
【００１７】[0017]
【実施例】以下、本発明の実施例及び比較例を示すが、
本発明はこれらに限定されるものではない。EXAMPLES Examples and comparative examples of the present invention will be shown below.
The present invention is not limited to these.
【００１８】実施例１ 反応：１８７５ｋｇの母液と４９重量％の苛性ソーダ水
溶液１２５ｋｇに、２５℃に保ちながら塩素ガスおよそ
５５ｋｇを導入して塩素化を行う。析出した食塩を分級
によりのぞき、消石灰１３０ｋｇ及び水５ｋｇを加えミ
キサーで乳化し、次亜石灰乳液とする。この次亜石灰乳
液のアルカリ濃度は、７．５重量％であった。これを２
５℃で保ちながら、およそ２００ｋｇの塩素を通じ再度
塩素化を行う。塩素化終点管理は、ＯＲＰ電極電位変化
率による自動管理で行った。こうして得られた次亜塩素
酸カルシウム組成物スラリーの組成は、次亜塩素酸カル
シウム１７．９重量％，塩化ナトリウム１８．３重量
％，塩化カルシウム０．９重量％，水酸化カルシウム
０．８重量％を含んでいた。これにアルカリ源として、
別に上記次亜石灰乳液４９０ｋｇをアジター中で加え、
よく混合した。そのときのスラリー組成は、次亜塩素酸
カルシウム１７．２重量％，水酸化ナトリウム２．０重
量％であった。Example 1 Reaction: Chlorination was carried out by introducing approximately 55 kg of chlorine gas into 125 kg of mother liquor and 125 kg of 49 wt% caustic soda aqueous solution while maintaining the temperature at 25 ° C. The precipitated salt is removed by classification, 130 kg of slaked lime and 5 kg of water are added, and the mixture is emulsified with a mixer to obtain a hypocalcinus emulsion. The alkali concentration of this hypolime emulsion was 7.5% by weight. This is 2
Chlorination is performed again by passing about 200 kg of chlorine while maintaining the temperature at 5 ° C. The chlorination end point control was performed automatically by the ORP electrode potential change rate. The composition of the calcium hypochlorite composition slurry thus obtained was as follows: calcium hypochlorite 17.9% by weight, sodium chloride 18.3% by weight, calcium chloride 0.9% by weight, calcium hydroxide 0.8% by weight. % Was included. As an alkali source for this,
Separately, add 490 kg of the above hypolime emulsion in an agitator,
Mixed well. The slurry composition at that time was 17.2% by weight of calcium hypochlorite and 2.0% by weight of sodium hydroxide.
【００１９】濾過・乾燥・造粒・打錠：この次亜塩素酸
カルシウム組成物スラリーを、遠心分離器にて濾過し、
母液と次亜塩素酸カルシウム組成物ケーキとに分離し
た。このケーキを乾燥・造粒・打錠して次亜塩素酸カル
シウム組成物２０ｇ錠剤製品を得た。この製品の組成
は、次亜塩素酸カルシウム７２．０重量％，塩化ナトリ
ウム７．８重量％，塩化カルシウム１．５重量％、水酸
化カルシウム６．５重量％，水分その他１２重量％であ
った。Filtration / Drying / Granulation / Tabletting: This calcium hypochlorite composition slurry is filtered by a centrifuge,
Separated into mother liquor and calcium hypochlorite composition cake. The cake was dried, granulated and tabletted to obtain a 20 g tablet product of the calcium hypochlorite composition. The composition of this product was as follows: calcium hypochlorite 72.0% by weight, sodium chloride 7.8% by weight, calcium chloride 1.5% by weight, calcium hydroxide 6.5% by weight, water and other 12% by weight. .
【００２０】実施例２ 実施例１において、次亜石灰乳液塩素化終了後のスラリ
ーに加えるアルカリ源を、４０重量％石灰乳７０ｋｇに
替えた以外は同様に処理して次亜塩素酸カルシウム組成
物（２０ｇ錠剤）を得た。この製品の組成は、次亜塩素
酸カルシウム７２．７重量％，塩化ナトリウム７．７重
量％，塩化カルシウム１．２重量％，水酸化カルシウム
６．５重量％，水分その他１１．９重量％であった。Example 2 A calcium hypochlorite composition was prepared in the same manner as in Example 1, except that the alkali source added to the slurry after completion of chlorination of hypochlorite emulsion chlorination was changed to 70 kg of 40% by weight lime milk. (20 g tablet) was obtained. The composition of this product is 72.7% by weight calcium hypochlorite, 7.7% by weight sodium chloride, 1.2% by weight calcium chloride, 6.5% by weight calcium hydroxide, 11.9% by weight water and others. there were.
【００２１】比較例 実施例１において、次亜石灰乳液の塩素化終了後のスラ
リーにアルカリ源を加えることなく、同様に処置して次
亜塩素酸カルシウム組成物（２０ｇ錠剤）を得た。この
製品の組成は、次亜塩素酸カルシウム７２．９重量％，
塩化ナトリウム８．３重量％，塩化カルシウム２．０重
量％，水酸化カルシウム４．５重量％，水分その他１
２．３重量％であった。Comparative Example The calcium hypochlorite composition (20 g tablet) was obtained in the same manner as in Example 1 except that the slurry after the chlorination of the hypocalcite emulsion was not added with an alkali source. The composition of this product is 72.9% by weight of calcium hypochlorite,
Sodium chloride 8.3% by weight, calcium chloride 2.0% by weight, calcium hydroxide 4.5% by weight, water and others 1
It was 2.3% by weight.
【００２２】試験例 （保管試験）製品の保管形態（ポリエチレンの０．２ｍ
ｍチューブに充填され、２０ｋｇずつ段ボールに梱包さ
れる）のまま、恒温倉庫で３０，４０℃で１カ月間保管
した。 （溶解速度の測定）３Ｌの蒸留水を入れた５Ｌの広口ビ
ーカーを、３０℃の恒温槽に入れ、あらかじめ正確に重
量を測定した試料（２０ｇ錠剤）４個をビーカー内の決
められた場所に置き、羽根付き攪拌機で攪拌した。攪拌
速度は１００ｒｐｍに調整した。１時間溶解後、攪拌を
止め錠剤を取り出し、実験用ワイパー紙で軽く水分をふ
き取った。溶解試験前後の重量差から、溶解量を求め、
これを溶解速度とした。これを５回繰り返し、計２０個
の錠剤について平均溶解速度を求めた。実施例１，２お
よび比較例で得られた製品（２０ｇ錠剤）につき、保管
試験前，３０℃保管試験後，４０℃保管試験後で溶解速
度を比較した。 試験結果 結果は以下の通りであった。Test Example (Storage Test) Product storage form (0.2 m of polyethylene)
m tube was packed and 20 kg each was packed in a corrugated board), and stored in a constant temperature warehouse at 30, 40 ° C. for 1 month. (Measurement of dissolution rate) A 5 L wide-mouth beaker containing 3 L of distilled water was placed in a constant temperature bath at 30 ° C., and four accurately weighed samples (20 g tablets) were placed in a predetermined place in the beaker. Place and stir with a stirrer with blades. The stirring speed was adjusted to 100 rpm. After dissolving for 1 hour, stirring was stopped, the tablet was taken out, and the moisture was wiped off lightly with a test wiper paper. From the weight difference before and after the dissolution test, determine the dissolution amount,
This was taken as the dissolution rate. This was repeated 5 times, and the average dissolution rate was calculated for 20 tablets in total. The dissolution rates of the products (20 g tablets) obtained in Examples 1 and 2 and Comparative Example were compared before the storage test, after the 30 ° C. storage test, and after the 40 ° C. storage test. Test results The results were as follows.
【００２３】[0023]
【表１】 [Table 1]
【００２４】[0024]
【発明の効果】次亜石灰乳の塩素化工程終了後、必要と
されるアルカリ源を乾燥工程の前に添加し、次亜塩素酸
カルシウム組成物錠剤を製造することにより、 （１）錠剤を遅溶化することができる。 （２）塩素化工程の終末管理を自動のまま行え、溶解性
の差異により銘柄が増加しても、人的負担を増加する必
要がない。 （３）錠剤の溶解性の保管による経時変化を抑えること
が出来る。[Effects of the Invention] After the chlorination step of hypolysine milk is finished, the required alkali source is added before the drying step to produce a calcium hypochlorite composition tablet. It can be slow-solubilized. (2) The terminal management of the chlorination process can be automatically performed, and it is not necessary to increase the human burden even if the brands increase due to the difference in solubility. (3) It is possible to suppress the change over time in the solubility of tablets due to storage.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 丸山 昭司 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 (72)発明者 尾島 信昭 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 the front page (72) Inventor Shoji Maruyama 950 Fujisawa Nakago-mura, Nakakubiki-gun, Niigata Nihongi Plant, Nippon Soda Co., Ltd. Nihongi Factory Co., Ltd.
Claims (7)
次亜塩素酸カルシウム組成物を製造する方法において、
塩素化が終了した後、乾燥工程の前にアルカリを一定量
加えることを特徴とする、組成物中のアルカリ濃度が高
められた次亜塩素酸カルシウム組成物錠剤の製造法。1. A method for producing a calcium hypochlorite composition by chlorinating lime milk and an aqueous solution of caustic soda,
A method for producing a calcium hypochlorite composition tablet having an increased alkali concentration in a composition, which comprises adding a certain amount of alkali after the chlorination and before the drying step.
る自動管理で行うことを特徴とする請求項１記載の製造
法。2. The production method according to claim 1, wherein the chlorination is completed by automatic control based on the rate of change of the ORP potential.
が、有効塩素６５重量％から７５重量％であり、かつ水
分が８重量％から１５重量％、全アルカリが５重量％か
ら１０重量％である、請求項１または２記載の次亜塩素
酸カルシウム組成物錠剤の製造法。3. The composition of the calcium hypochlorite composition tablet has an effective chlorine content of 65% by weight to 75% by weight, a water content of 8% by weight to 15% by weight, and a total alkali content of 5% by weight to 10% by weight. The method for producing a calcium hypochlorite composition tablet according to claim 1 or 2.
カリ源が、塩素化する前の石灰乳化液である、請求項１
〜３記載の次亜塩素酸カルシウム組成物錠剤の製造法。4. The alkali source of alkali added after completion of chlorination is a lime emulsion before chlorination.
[3] A method for producing a calcium hypochlorite composition tablet according to [3].
１０〜５０重量％石灰乳である、請求項４記載の次亜塩
素酸カルシウム組成物錠剤の製造法。5. The lime emulsion added after the completion of chlorination comprises:
The method for producing a calcium hypochlorite composition tablet according to claim 4, which comprises 10 to 50% by weight of lime milk.
を、攪拌機付き貯槽、アジター、ラインミキサーのうち
１種もしくは２種以上を組み合わせで行うことを特徴と
する請求項１〜５記載の次亜塩素酸カルシウム組成物錠
剤の製造法。6. The hypothiae according to claim 1, wherein the mixing of the alkali added after the completion of the chlorination is carried out by one kind or a combination of two or more kinds among a storage tank with a stirrer, an agitator and a line mixer. A method for producing a tablet of a calcium chlorate composition.
を、塩素化スラリー遠心分離中に行うことを特徴とする
請求項１〜５記載の次亜塩素酸カルシウム組成物錠剤の
製造法。7. The method for producing a calcium hypochlorite composition tablet according to claim 1, wherein the mixing of the alkali added after the completion of chlorination is performed during chlorinated slurry centrifugation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27180695A JP3769740B2 (en) | 1995-09-26 | 1995-09-26 | Method for producing calcium hypochlorite composition tablets with controlled solubility |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27180695A JP3769740B2 (en) | 1995-09-26 | 1995-09-26 | Method for producing calcium hypochlorite composition tablets with controlled solubility |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0986903A true JPH0986903A (en) | 1997-03-31 |
| JP3769740B2 JP3769740B2 (en) | 2006-04-26 |
Family
ID=17505115
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27180695A Expired - Lifetime JP3769740B2 (en) | 1995-09-26 | 1995-09-26 | Method for producing calcium hypochlorite composition tablets with controlled solubility |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017052656A (en) * | 2015-09-07 | 2017-03-16 | 東ソー株式会社 | Method for producing calcium hypochlorite composition |
| CN110523319A (en) * | 2019-08-27 | 2019-12-03 | 广州泰道安医疗科技有限公司 | A kind of disinfectant production technology |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5614402A (en) * | 1979-07-17 | 1981-02-12 | Toyo Soda Mfg Co Ltd | Manufacture of stable potassium hypochlorite composition |
| JPS5756304A (en) * | 1980-08-07 | 1982-04-03 | Olin Mathieson | Manufacture of calcium hypochlorite |
| JPS605005A (en) * | 1983-06-15 | 1985-01-11 | オリン・コ−ポレイシヨン | Manufacture of calcium hypochlorite |
| JPS63162505A (en) * | 1986-12-26 | 1988-07-06 | Tosoh Corp | Production of granular calcium hypochlorite composition |
| JPH05307019A (en) * | 1992-04-28 | 1993-11-19 | Nippon Soda Co Ltd | Reaction terminating point managing method by use of orp electrode |
-
1995
- 1995-09-26 JP JP27180695A patent/JP3769740B2/en not_active Expired - Lifetime
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5614402A (en) * | 1979-07-17 | 1981-02-12 | Toyo Soda Mfg Co Ltd | Manufacture of stable potassium hypochlorite composition |
| JPS5756304A (en) * | 1980-08-07 | 1982-04-03 | Olin Mathieson | Manufacture of calcium hypochlorite |
| JPS605005A (en) * | 1983-06-15 | 1985-01-11 | オリン・コ−ポレイシヨン | Manufacture of calcium hypochlorite |
| JPS63162505A (en) * | 1986-12-26 | 1988-07-06 | Tosoh Corp | Production of granular calcium hypochlorite composition |
| JPH05307019A (en) * | 1992-04-28 | 1993-11-19 | Nippon Soda Co Ltd | Reaction terminating point managing method by use of orp electrode |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017052656A (en) * | 2015-09-07 | 2017-03-16 | 東ソー株式会社 | Method for producing calcium hypochlorite composition |
| CN110523319A (en) * | 2019-08-27 | 2019-12-03 | 广州泰道安医疗科技有限公司 | A kind of disinfectant production technology |
| CN110523319B (en) * | 2019-08-27 | 2021-12-10 | 广州泰道安医疗科技有限公司 | Disinfectant fluid production process |
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|---|---|
| JP3769740B2 (en) | 2006-04-26 |
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