JP3576160B2 - Method for producing calcium hydroxide - Google Patents
Method for producing calcium hydroxide Download PDFInfo
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- JP3576160B2 JP3576160B2 JP2003376202A JP2003376202A JP3576160B2 JP 3576160 B2 JP3576160 B2 JP 3576160B2 JP 2003376202 A JP2003376202 A JP 2003376202A JP 2003376202 A JP2003376202 A JP 2003376202A JP 3576160 B2 JP3576160 B2 JP 3576160B2
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- calcium hydroxide
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- digestion
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- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 title claims description 41
- 239000000920 calcium hydroxide Substances 0.000 title claims description 41
- 229910001861 calcium hydroxide Inorganic materials 0.000 title claims description 41
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 30
- 239000000292 calcium oxide Substances 0.000 claims description 26
- 230000029087 digestion Effects 0.000 claims description 23
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 22
- 239000013078 crystal Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 235000012255 calcium oxide Nutrition 0.000 description 25
- 239000002245 particle Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229930006000 Sucrose Natural products 0.000 description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
本発明は水酸化カルシウムの製造方法に関するもので、大きな比表面積を持ち、しかもサイロやタンクでの貯蔵時や配管等での輸送時に棚つりや付着、固結が起こりにくい流動性が良好な粉末水酸化カルシウムの製造方法に関する。 The present invention relates to a method for producing calcium hydroxide, a powder having a large specific surface area, and having good fluidity that does not easily cause shelf hanging, adhesion, and consolidation during storage in silos or tanks or transportation through pipes or the like. The present invention relates to a method for producing calcium hydroxide.
工業的に水酸化カルシウムを製造する方法として、原料となる酸化カルシウムを消化機に装入しここで酸化カルシウムが水酸化カルシウムに水和するのに必要な理論量の１．３〜２倍の水を加え、酸化カルシウムと水を強力に撹拌して消化させ、さらに熟成機で撹拌しながら消化ムラを無くし過剰の水分を蒸発させて排出後必要に応じて粉砕、分級するいわゆる乾式消化法が知られている。この方法で得られた水酸化カルシウムは一般に付着水分０．５％以下、粒度−１５０μｍ以下の不定形の粉末で比表面積が小さく流動性も悪い。従ってサイロやタンクでの貯蔵時や配管等での輸送時に棚つりや付着、固結が起こりやすい。またこれらの問題を解決するために、水、アルコール、界面活性剤を消化水として用いる方法が提唱されているが、アルコール処理のための設備が必要となるためコスト的に高くなる。 As a method for industrially producing calcium hydroxide, calcium oxide as a raw material is charged into a digester, and the theoretical amount of calcium oxide required for hydration of the calcium oxide into calcium hydroxide is 1: 1 . Add 3 to 2 times the water, and vigorously stir the calcium oxide and water to digest it. Eliminate the unevenness of the digestion while stirring with an aging machine, evaporate excess water, discharge and pulverize and classify as necessary. A so-called dry digestion method is known. The calcium hydroxide obtained by this method is generally an amorphous powder having an attached water content of 0.5% or less and a particle size of -150 μm or less, and has a small specific surface area and poor fluidity. Accordingly, shelf storage, adhesion, and consolidation are likely to occur during storage in silos or tanks or during transportation through pipes or the like. In order to solve these problems, a method using water, alcohol, and a surfactant as digestion water has been proposed. However, since equipment for alcohol treatment is required, the cost becomes high.
本発明は乾式消化装置において特別な装置を付加することなく、比表面積が大きく流動性の良好な水酸化カルシウム粉末を安価に得ることを目的とする。 An object of the present invention is to obtain a calcium hydroxide powder having a large specific surface area and good fluidity at low cost without adding a special device in a dry digester.
本発明の水酸化カルシウムの製造方法は、酸化カルシウムに消化遅延剤を溶解した水を必要水量より過剰に添加、混合して得られた含水状態の水酸化カルシウムを乾燥させることを特徴とする。 The method for producing calcium hydroxide of the present invention is characterized in that water obtained by dissolving a digestion retardant in calcium oxide is added in excess of the required amount of water, and the resulting water-containing calcium hydroxide is dried.
本発明の水酸化カルシウムの製造方法によれば安価に比表面積が大きく流動性の良好な水酸化カルシウムが得られる。 According to the method for producing calcium hydroxide of the present invention, calcium hydroxide having a large specific surface area and good fluidity can be obtained at low cost.
本発明は乾式消化装置において消化遅延剤を原料酸化カルシウム１００重量部に対して０．０５〜３重量部添加した水を必要水量より過剰に消化開始時に一度に添加することが望ましい。この時に使用される消化遅延剤としてはセメントの硬化消化遅延剤として知られるクエン酸、酒石酸、リグニンスルホン酸およびこれらの塩あるいはしょ糖などが例示される。添加される水の量は、生成した水酸化カルシウム１００重量部に対し水が１５〜３５重量部になるように調整する。上記のようにして得られた水酸化カルシウム含水物は熟成機で撹拌しながら熟成した後乾燥し、必要に応じて粉砕、分級する。 In the present invention, it is desirable that in a dry digester, water obtained by adding 0.05 to 3 parts by weight of a digestion retarder to 100 parts by weight of the raw material calcium oxide is added at a time at the start of digestion in excess of the required amount of water. Examples of the digestion retardant used at this time include citric acid, tartaric acid, ligninsulfonic acid, salts thereof and sucrose which are known as hardening digestion retarders for cement. The amount of water to be added is adjusted so that water is 15 to 35 parts by weight based on 100 parts by weight of the generated calcium hydroxide. The hydrated calcium hydroxide obtained as described above is aged while stirring with an aging machine, dried, and, if necessary, ground and classified.
一般に乾式消化装置で製造される水酸化カルシウムは、原料である酸化カルシウムと水が反応する際に短時間で大きな発熱反応を伴うために結晶面が発達せず不定形粒子になりやすい。この消化反応中あるいは消化反応終了後に過剰の水を加えて撹拌するとその水分により水酸化カルシウムの団粒化が起きる。団粒化した粒子の大きさは水分量を調節することにより容易に調整できる。しかしこの場合団粒化した粒子を構成する水酸化カルシウムは不定形であるため、団粒化した粒子は気孔率が小さく見かけの表面積が低くなり水酸化カルシウムの反応性の低下が懸念される。 Generally, calcium hydroxide produced by a dry digester is accompanied by a large exothermic reaction in a short period of time when the raw material calcium oxide and water react with each other, so that crystal faces do not develop and tend to be irregular shaped particles. If excess water is added during or after the digestion reaction and the mixture is stirred, the water causes aggregation of calcium hydroxide. The size of the aggregated particles can be easily adjusted by adjusting the water content. However, in this case, since the calcium hydroxide constituting the aggregated particles is amorphous, the aggregated particles have a small porosity and a small apparent surface area, and there is a concern that the reactivity of the calcium hydroxide may be reduced.
一方前述したような消化遅延剤を添加した水を用いて消化反応を行うと結晶化が促進され板状の水酸化カルシウムが生成しやすいことが知られている。この水酸化カルシウム粒子の比表面積は大きいが板状のため不定形粒子よりもかえって流動性が悪化することがある。従って酸化カルシウムに消化遅延剤を添加した水を必要水量より過剰に添加、混合して消化反応を行い、団粒化を行うことで流動性が改善できる。またこのようにして得られた団粒化した粒子は板状結晶がカードハウス状に凝集しているため見かけの表面積も低下せず反応性を低下しない。 On the other hand, it is known that when a digestion reaction is performed using water to which the above-mentioned digestion retardant is added, crystallization is promoted and plate-like calcium hydroxide is easily generated. Although the specific surface area of the calcium hydroxide particles is large, the fluidity may be worse than the irregular particles due to the plate shape. Therefore, the flowability can be improved by adding and mixing the water obtained by adding the digestion retardant to the calcium oxide in excess of the required water amount, performing a digestion reaction, and performing agglomeration to perform the aggregation. The aggregated particles thus obtained do not decrease the apparent surface area and the reactivity because the plate-like crystals are aggregated in a card house shape.
本発明における消化遅延剤の添加量は原料となる酸化カルシウムと水との反応性、いわゆる活性や粒度との兼ね合いで決定される。消化遅延剤が少ないと消化が速く水酸化カルシウムの結晶が十分に成長しないし多すぎると消化反応が終了するまでの時間が長くなりすぎるため装置全体の効率の低下を招くため、原料酸化カルシウム１００重量部に対し消化遅延剤０．０５〜３重量部用いるのが良い。さらに原料の酸化カルシウムは均一な遅延効果を得るために３ｍｍ以下の粉粒物が好ましい。添加する水の量は生成する水酸化カルシウムの飽和含水量との兼ね合いで決定される。少なすぎると団粒化が不十分になり、得られた水酸化カルシウムの流動性が悪化する。多すぎると大きな塊あるいは粘土状になってしまうため、生成した水酸化カルシウム１００重量部に対して水１５〜３５重量部になるように調整することが望ましい。 The amount of the digestion retardant added in the present invention is determined in consideration of the reactivity between the raw material calcium oxide and water, that is, the activity and the particle size. When the amount of the digestion delaying agent is small, the digestion is fast, and the crystals of calcium hydroxide do not grow sufficiently. It is preferable to use 0.05 to 3 parts by weight of the digestion retarder based on parts by weight. Further, the powdered calcium oxide is preferably 3 mm or less in order to obtain a uniform delay effect. The amount of water to be added is determined in consideration of the saturated water content of the generated calcium hydroxide. If the amount is too small, agglomeration becomes insufficient, and the fluidity of the obtained calcium hydroxide deteriorates. If the amount is too large, a large mass or clay is formed. Therefore, it is preferable to adjust the amount of water to 15 to 35 parts by weight with respect to 100 parts by weight of the generated calcium hydroxide.
また消化開始時に添加、混合される水は、生成した水酸化カルシウム１００重量部に対して水１５〜３５重量部になるように調製する。乾燥は一般的に用いられる方法で行えば良いが、約５５０℃で水酸化カルシウムが脱水して酸化カルシウムに変化するためこの温度以下で行う必要がある。また燃料ガス等酸性ガスを多く含むもので直接加熱することは水酸化カルシウムと酸性ガスが反応してカルシウム塩を生成してしまうため避けなければならない。 The water to be added and mixed at the start of digestion is adjusted to be 15 to 35 parts by weight of water based on 100 parts by weight of the generated calcium hydroxide . Drying may be carried out by commonly used that way, but it is necessary to carry out at this temperature or less for calcium hydroxide at about 550 ° C. is changed into calcium oxide by dehydration. Further, direct heating with a gas containing a large amount of an acidic gas such as a fuel gas must be avoided because calcium hydroxide and the acidic gas react with each other to generate a calcium salt.
そのほかに乾燥を補助する目的で、生成した含水水酸化カルシウムに酸化カルシウムを添加すれば酸化カルシウムの水和のために必要な水分と水和熱による水分の蒸発により含水量を低下させることは可能であるが、あまり多くの酸化カルシウムを添加すると乾燥のために添加した酸化カルシウムは通常の乾式消化と同じため比表面積の低下や流動性の悪化を招く恐れがある。 In addition, if calcium oxide is added to the generated hydrous calcium hydroxide to assist drying, the water content can be reduced by evaporating the water necessary for hydration of calcium oxide and the heat of hydration. However, if too much calcium oxide is added, the calcium oxide added for drying is the same as in ordinary dry digestion, which may cause a decrease in specific surface area or deterioration of fluidity.
（実施例）
自社製生石灰（ＪＩＳ工業用石灰 生石灰特号）を−１ｍｍに粉砕して酸化カルシウム原料とした。この時のＤＩＮ１０６０による反応性はｔｕ＝２．３分であった。消化遅延剤として食品として市販されている白砂糖を酸化カルシウム１００重量部に対して１．５重量部になるように調整した消化水を酸化カルシウムが水酸化カルシウムに消化するに必要な理論水量の２．９倍になるように原料酸化カルシウムと撹拌、混合した。その後加水せずに生成した含水水酸化カルシウムの水分を測定すると水酸化カルシウム１００重量部に対し水２７．６重量部であった。このようにして得られた含水水酸化カルシウムを熟成、乾燥後−１５０μｍに粉砕分級して得られた水酸化カルシウム粉末の見かけ比重、安息角、比表面積の測定結果を表１に示す。なお見かけ比重、安息角の測定にはホソカワミクロン製パウダーテスターを用い、比表面積の測定には窒素吸着法によるＢＥＴ比表面積計を用いた。
(Example)
In-house manufactured lime (JIS industrial lime quick lime special number) was pulverized to -1 mm to obtain a calcium oxide raw material. The reactivity according to DIN 1060 at this time was tu = 2.3 minutes. Digestion water obtained by adjusting white sugar, which is commercially available as a food as a digestion retardant, to 1.5 parts by weight with respect to 100 parts by weight of calcium oxide, has a theoretical water amount required for calcium oxide to be digested into calcium hydroxide. The mixture was stirred and mixed with the raw material calcium oxide so as to be 2.9 times. Thereafter, the water content of the hydrous calcium hydroxide formed without water was measured, and it was 27.6 parts by weight of water with respect to 100 parts by weight of the calcium hydroxide. The hydrated calcium hydroxide thus obtained was aged, dried and pulverized and classified to -150 μm. The measurement results of the apparent specific gravity, angle of repose, and specific surface area of the calcium hydroxide powder obtained are shown in Table 1. The apparent specific gravity and angle of repose were measured using a powder tester made by Hosokawa Micron, and the specific surface area was measured using a BET specific surface area meter by a nitrogen adsorption method.
（比較例）
自社製生石灰（ＪＩＳ工業用石灰 生石灰特号）を−１ｍｍの生石灰粉を酸化カルシウム原料として消化遅延剤を用いず酸化カルシウムが水酸化カルシウムに消化するのに必要な理論水量の１．３倍の水とを撹拌、混合した。その後加水せずに得られた水酸化カルシウムの水分を測定すると水酸化カルシウム１００重量部に対し水０．２重量部であった。このようにして得られた含水水酸化カルシウムを熟成、乾燥後−１５０μｍに粉砕分級して得られた水酸化カルシウム粉末の見かけ比重、安息角、比表面積の測定結果を表１に示す。表１からも判るとおり本発明による得られた水酸化カルシウムは比表面積が大きく流動性も良好である。
(Comparative example)
In-house quicklime (JIS industrial lime, quicklime special number) is -1 mm of quicklime powder, which is 1.3 times the theoretical amount of water required for calcium oxide to be digested into calcium hydroxide without using a digestion delaying agent as a calcium oxide raw material. The mixture was stirred and mixed with water. Thereafter, the water content of the calcium hydroxide obtained without adding water was measured and found to be 0.2 parts by weight of water with respect to 100 parts by weight of calcium hydroxide. The hydrated calcium hydroxide thus obtained was aged, dried and pulverized and classified to -150 μm. The measurement results of the apparent specific gravity, angle of repose, and specific surface area of the calcium hydroxide powder obtained are shown in Table 1. As can be seen from Table 1, the calcium hydroxide obtained according to the present invention has a large specific surface area and good fluidity.
Claims (1)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003376202A JP3576160B2 (en) | 2003-11-05 | 2003-11-05 | Method for producing calcium hydroxide |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2003376202A JP3576160B2 (en) | 2003-11-05 | 2003-11-05 | Method for producing calcium hydroxide |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP08577296A Division JP3575911B2 (en) | 1996-03-14 | 1996-03-14 | Method for producing calcium hydroxide |
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| JP2004043303A JP2004043303A (en) | 2004-02-12 |
| JP3576160B2 true JP3576160B2 (en) | 2004-10-13 |
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