JPH02225308A - Production of calcium nitride powder - Google Patents
Production of calcium nitride powderInfo
- Publication number
- JPH02225308A JPH02225308A JP4624689A JP4624689A JPH02225308A JP H02225308 A JPH02225308 A JP H02225308A JP 4624689 A JP4624689 A JP 4624689A JP 4624689 A JP4624689 A JP 4624689A JP H02225308 A JPH02225308 A JP H02225308A
- Authority
- JP
- Japan
- Prior art keywords
- calcium nitrite
- powder
- aqueous solution
- stirring
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- -1 calcium nitride Chemical class 0.000 title description 3
- 229910052791 calcium Inorganic materials 0.000 title 1
- 239000011575 calcium Substances 0.000 title 1
- RAFRTSDUWORDLA-UHFFFAOYSA-N phenyl 3-chloropropanoate Chemical compound ClCCC(=O)OC1=CC=CC=C1 RAFRTSDUWORDLA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 239000004568 cement Substances 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 2
- 238000007711 solidification Methods 0.000 abstract 2
- 230000008023 solidification Effects 0.000 abstract 2
- 239000002994 raw material Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 9
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 150000004682 monohydrates Chemical class 0.000 description 2
- 230000003449 preventive effect Effects 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- SQJJEJSKPDGMNG-UHFFFAOYSA-L O.O.O.O.[Ca++].[O-]N=O.[O-]N=O Chemical compound O.O.O.O.[Ca++].[O-]N=O.[O-]N=O SQJJEJSKPDGMNG-UHFFFAOYSA-L 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 239000007798 antifreeze agent Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011150 reinforced concrete Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/085—Acids or salts thereof containing nitrogen in the anion, e.g. nitrites
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、亜硝酸カルシウムの製造方法に関する。本発
明で得られた粉末は、コンクリ−１・に有害な塩化物お
よびアルカリ金属塩を含まずかつ鋼材に対し防錆作用を
もつので、鉄筋コンクリートの塩害用防錆剤として、ま
たモルタルやコンクリートの凝結促進剤、硬化促進剤お
よび防凍剤として利用できる。また、亜硝酸ナトリウム
の代替の用途もある。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing calcium nitrite. The powder obtained in the present invention does not contain chlorides or alkali metal salts that are harmful to concrete, and has a rust preventive effect on steel materials, so it can be used as a rust preventive agent for salt damage in reinforced concrete, and for mortar and concrete. It can be used as a setting accelerator, curing accelerator and antifreeze agent. There are also alternative uses for sodium nitrite.
（従来の技術）
亜硝酸カルシウムは、一般には３０〜３５重量％水溶液
として利用されている。(Prior Art) Calcium nitrite is generally used as a 30-35% by weight aqueous solution.
亜硝酸カルシウムの固体を得る場合には、亜硝酸カルシ
ウム水溶液を亜硝酸カルシウムの４水塩および／または
１水塩として晶析させ、これを遠心分離機などにより固
液分離を行ない。When solid calcium nitrite is obtained, an aqueous calcium nitrite solution is crystallized as calcium nitrite tetrahydrate and/or monohydrate, and solid-liquid separation is performed using a centrifuge or the like.
付着水を乾燥・除去して固体の亜硝酸カルシウムを得る
か、または、亜硝酸カルシウム水溶液を４水塩および／
または１水塩となるまで、濃縮し、ドラムフレーカにて
固体の亜硝酸カルシウムを得ている。後者の方法が簡便
に適用される。Either dry and remove the adhering water to obtain solid calcium nitrite, or convert the calcium nitrite aqueous solution to tetrahydrate and/or
Alternatively, it is concentrated until it becomes monohydrate, and solid calcium nitrite is obtained using a drum flaker. The latter method is conveniently applied.
（発明が解決しようとする課題）
しかし、上記の方法では、亜硝酸カルシウムの粉末を得
ることは、困難である０本質的に結晶水を持った固体で
あるので、亜硝酸カルシウムとしての有効成分は少なく
経済的に不利であり、しかも、外部からの水分を遮断し
た密閉の容器に入れておいても、亜硝酸カルシウム固体
の強い固結は避けられないという重大な問題があった。(Problem to be Solved by the Invention) However, with the above method, it is difficult to obtain powder of calcium nitrite.0 Since it is essentially a solid with water of crystallization, it is difficult to obtain powder of calcium nitrite. It is economically disadvantageous because the amount of calcium nitrite is small, and there is also a serious problem in that strong caking of calcium nitrite solids cannot be avoided even if the calcium nitrite is kept in a sealed container that blocks moisture from entering.
（課題を解決するための手段）
従って、本発明の目的は、上記の諸問題を解決するため
、実質的に無水物の亜硝酸カルシウム粉末の製造方法を
提供するにある。(Means for Solving the Problems) Therefore, an object of the present invention is to provide a method for producing a substantially anhydrous calcium nitrite powder in order to solve the above-mentioned problems.
本発明は、亜硝酸カルシウムを主成分とする水溶液を、
撹拌および／または分散させながら、材料温度が１２０
〜２００℃の間、望ましくは、 １３０〜１７０℃の間
にて、乾量基準の含水率が５重量％以下、望ましくは２
重量％以下となるように乾燥させることを特徴とする、
亜硝酸カルシウム粉末を得る方法である。The present invention provides an aqueous solution containing calcium nitrite as a main component.
While stirring and/or dispersing, the material temperature is 120°C.
~200°C, preferably 130~170°C, the moisture content on a dry basis is 5% by weight or less, preferably 2%.
% by weight or less,
This is a method of obtaining calcium nitrite powder.
材料温度が１２０℃以下では、乾燥度のよい粉末が得ら
れず、材料温度が２００℃以上とするには加熱源が不利
となる他、亜硝酸カルシウムが徐々に分解するおそれが
ある。If the material temperature is 120° C. or lower, powder with good dryness cannot be obtained, and if the material temperature is 200° C. or higher, the heating source will be disadvantageous, and there is a risk that calcium nitrite will gradually decompose.
材料を撹拌および／または分散させながら乾燥させるた
めの乾燥装置としては、溝型撹拌乾燥機、噴霧乾燥器、
特殊可動羽根付撹拌型薄膜蒸発機が例示される。これら
の乾燥装置は、いづれも−工程で粉末が得られしかも連
続操作が容易であり、さらに製品粉末の含水率を５重量
％以下の低水準で任意に制御できるので好都合である。Drying equipment for drying materials while stirring and/or dispersing them includes groove type stirring dryers, spray dryers,
An example is a stirring type thin film evaporator with special movable blades. All of these drying apparatuses are advantageous because powder can be obtained in one step and continuous operation is easy, and furthermore, the moisture content of the product powder can be arbitrarily controlled at a low level of 5% by weight or less.
原料の亜硝酸カルシウムを主成分とする水溶液は、亜硝
酸カルシウムが２５重量％以上、硝酸カルシウムが亜硝
酸カルシウムの１０重量％以下、望ましくは３４重量％
以上の亜硝酸カルシウム、４重量％以下の硝酸カルシウ
ムを含むが、場合によっては予め濃縮してから所定の乾
燥機に供給することも可能である。また、他の物質を原
料液に添加して、同時に乾燥することも可能である。The aqueous solution containing calcium nitrite as a main component contains 25% by weight or more of calcium nitrite and 10% by weight or less of calcium nitrite, preferably 34% by weight of calcium nitrite.
The above calcium nitrite contains 4% by weight or less of calcium nitrate, but in some cases it is also possible to concentrate it in advance and then supply it to a predetermined dryer. It is also possible to add other substances to the raw material liquid and dry it at the same time.
（作 用）
亜硝酸カルシウムを主成分とする原料水溶液が、濃縮さ
れるに従い粘ちょう物となりさらに粘着性が強くなり、
全体が団塊化を起こし取り扱いが困難となるので、本発
明の方法では、この団塊化過程をいかにうまく経過させ
て、流動する無水塩粉末にまで乾燥させるかということ
にある。すなわち、該原料を攪拌および／または分散さ
せながら乾燥させることが本発明において本質的に重要
である。また、無水塩ないし無水塩に近い粉末を得なけ
れば、製品粉末が固結するという重大な問題があるので
、無水塩となる温度以上で、かつ亜硝酸カルシウムの分
解温度以下で乾燥しなければならない。(Function) As the raw material aqueous solution containing calcium nitrite as its main component becomes concentrated, it becomes viscous and becomes more sticky.
Since the whole product becomes agglomerated and becomes difficult to handle, the method of the present invention focuses on how to successfully carry out this agglomeration process and dry it to a fluid anhydrous salt powder. That is, it is essentially important in the present invention to dry the raw materials while stirring and/or dispersing them. In addition, unless an anhydrous salt or a powder close to an anhydrous salt is obtained, there is a serious problem that the product powder will solidify, so it must be dried at a temperature above the temperature at which it becomes an anhydrous salt and below the decomposition temperature of calcium nitrite. It won't happen.
以下、比較例および実施例を示して本発明の詳細な説明
する。Hereinafter, the present invention will be explained in detail by showing comparative examples and examples.
（実施例）
比較例１
２６０ ｘ ３６５ Ｘ ９０ｍｍ寸法のステンレス
製ヴアットに、亜硝酸カルシウム３４．８重量％および
硝酸カルシウム３．８重量％含む原料水溶液４Ｋｇを入
れ、 １５０℃の熱風式箱型乾燥器にて２４時間蒸発乾
燥した。得られた固体は、頑丈な板状体であった。これ
を取り出しハンマーにて粗粉砕した後、更に微粉砕し、
１５０℃で再乾燥して無水塩粉末１．５Ｋｇ （含水
率０．２％ＤＢ）を得た。(Example) Comparative Example 1 4 kg of a raw material aqueous solution containing 34.8% by weight of calcium nitrite and 3.8% by weight of calcium nitrate was placed in a stainless steel vat measuring 260 x 365 x 90 mm, and dried in a hot air box at 150°C. The mixture was evaporated and dried in a container for 24 hours. The obtained solid was a sturdy plate-like body. After taking this out and coarsely crushing it with a hammer, it is further finely crushed,
It was re-dried at 150°C to obtain 1.5 kg of anhydrous salt powder (moisture content 0.2% DB).
比較例２および実施例Ｉ
Ｋ社製回分式伝導加熱溝型撹拌乾燥機（幅２２０ｍｍ、
トラフ長８００ｎｕｏ、実効内容積２５℃）に、比較例
１と同じ原料液を２５Ｋｇ入れ、加熱ジャケットおよび
回転シャフトに５ Ｋｇ／ｃｍ”Ｇの飽和スチームを通
して回転数２２〜３７ｒｐｍで撹拌しながら蒸発させた
。液面が低下した途中で該原料液１２Ｋｇを逐次追加し
た。濃縮につれ粘ちょう物となり、シャフトと羽根に団
塊状に一体化して乾燥は容易に進行しないので、攪拌を
時々中断し、シャフトおよび羽根に粘着している粘ちょ
う物を剥しながら乾燥を続けて流動性の良い亜硝酸カル
シウム粉末を得た１次に、撹拌状態にある亜硝酸カルシ
ウムの粉面に団塊化を起こさないように、該原料液をス
プレィにて連続的に一様に噴霧しながら蒸発乾燥を続け
た。スプレィによる該原料の供給全量は２９Ｋｇであっ
た。スプレィ噴霧による該原料液の供給方法は、連続式
溝型撹拌乾燥機に応用できる。Comparative Example 2 and Example I Batch conduction heating groove type stirring dryer manufactured by K Company (width 220 mm,
25 kg of the same raw material liquid as in Comparative Example 1 was put into a trough length of 800 nuo and an effective internal volume of 25° C., and saturated steam of 5 kg/cm"G was passed through the heating jacket and rotating shaft to evaporate it while stirring at a rotation speed of 22 to 37 rpm. While the liquid level was decreasing, 12 kg of the raw material liquid was added successively.As it concentrated, it became viscous and was integrated into the shaft and blades in the form of nodules, making drying difficult. Then, drying was continued while removing the sticky substance sticking to the blades to obtain calcium nitrite powder with good fluidity. 1st step was to prevent agglomeration from occurring on the surface of the calcium nitrite powder while stirring. The raw material liquid was continuously and uniformly sprayed and evaporated to dryness.The total amount of the raw material supplied by spraying was 29 kg.The method of supplying the raw material liquid by spraying was a continuous groove. Can be applied to type stirring dryers.
約４時間にて亜硝酸カルシウム８８．３重量％、硝酸カ
ルシウム９．６重量％および水分２．０重量％含む粉末
２６Ｋｇを得た。分析値より亜硝酸カルシウムは、全く
分解していないことがわかる。In about 4 hours, 26 kg of powder containing 88.3% by weight of calcium nitrite, 9.6% by weight of calcium nitrate and 2.0% by weight of water was obtained. The analytical values show that calcium nitrite is not decomposed at all.
乾燥時の粉末温度は、 １２５〜１３０℃であった。The powder temperature during drying was 125-130°C.
なお、得られた粉末は、密閉したポリエチレン袋に入れ
ておいたとき強い固結は認められなかった。Note that no strong caking was observed in the obtained powder when it was placed in a sealed polyethylene bag.
実施例２
実施例１と同じ原料液を用いて、Ａ社製試験用ディスク
型噴霧乾燥器（チャンバ径２．５ｍ、直胴部２．０ｍ、
コーン部２．５ｍ、ディスク径１．２０ｍｍ）による乾
燥試験を行なった。ディスク回転数１ ｘ １０’ｒｐ
ｍ、入口温度１８０℃、出口温度１２３°Ｃ１供給量１
３Ｋｇ／ｈの条件にて良好な亜硝酸カルシウム粉末（５
Ｋｇ／ｈ、含水率２．２％ＤＢ）を得た。Example 2 Using the same raw material liquid as in Example 1, a test disk-type spray dryer manufactured by Company A (chamber diameter 2.5 m, straight body part 2.0 m,
A drying test was conducted using a cone section of 2.5 m and a disk diameter of 1.20 mm. Disc rotation speed 1 x 10'rp
m, inlet temperature 180°C, outlet temperature 123°C1 supply amount 1
Good calcium nitrite powder (5 kg/h condition)
Kg/h, moisture content 2.2% DB).
実施例３
実施例１と同じ原料液を用いて、Ｓ社製特殊可動羽根付
撹拌型薄膜蒸発機（竪型落下式、伝熱面積０．５７ｍ”
、羽根回転数７１Ｏｒｐｍ、羽根と加熱面の間隙０．
５ｍｍ）により濃縮・粉末化試験を行なった。装置本体
の上部からの蒸発水は、コンデンサにて冷却凝縮させた
。加熱用ジャケットに８ Ｋｇ／ｃｍ”Ｇの飽和スチー
ムを通し、原料液の供給量４１Ｋｇ／ｈの条件にて、実
質上無水塩の亜硝酸カルシウム粉末（含水率０．２％Ｄ
Ｂ）が１６Ｋｇ／ｈで得られた。なお、７ Ｋｇ／ｃｍ
”Ｇのスチームの場合にも、同じ供給量にて、含水率０
．８％ＤＢの亜硝酸カルシウム粉末が得られた。Example 3 Using the same raw material liquid as in Example 1, a stirring type thin film evaporator with special movable blades manufactured by S company (vertical falling type, heat transfer area 0.57 m) was used.
, blade rotation speed 71Orpm, gap between blade and heating surface 0.
A concentration/powderization test was conducted using 5 mm). Evaporated water from the upper part of the apparatus body was cooled and condensed in a condenser. Substantially anhydrous calcium nitrite powder (moisture content: 0.2% D
B) was obtained at 16 kg/h. In addition, 7 kg/cm
``In the case of G steam, the moisture content is 0 at the same supply amount.
．． A calcium nitrite powder of 8% DB was obtained.
（発明の効果）
本発明によれば、亜硝酸カルシウム水溶液から直接ワン
パスにて、乾量基準で５重量％以下の実質的に無水塩粉
末が得られる。該粉末は、有効成分が多くしかも、密閉
下の保存中に固結を起こすことがなく、安定な製品とし
てセメント混和剤、その他の用途に利用できる。(Effects of the Invention) According to the present invention, a substantially anhydrous salt powder containing 5% by weight or less on a dry weight basis can be obtained directly from an aqueous calcium nitrite solution in one pass. Although the powder contains a large amount of active ingredients, it does not cause caking during storage under closed conditions, and can be used as a stable product for cement admixtures and other uses.
特許出願人 日産化学工業株式会社
代理人 弁理士 萼 優 美 ・□、”・くほか
２名Patent applicant: Nissan Chemical Industries, Ltd. Agent: Patent attorney: Yumi Sae, ``□,'', and 2 others
Claims (2)
および／または分散させながら、材料温度が１２０〜２
００℃の間にて乾燥することを特徴とする、乾量基準の
含水率が５重量％以下である亜硝酸カルシウム粉末の製
造方 法。(1) While stirring and/or dispersing an aqueous solution containing calcium nitrite as a main component, the material temperature
A method for producing calcium nitrite powder having a moisture content of 5% by weight or less on a dry weight basis, the method comprising drying at a temperature between 00°C and 00°C.
重量％以上の亜硝酸カルシウムを含有することを特徴と
する請求項第（１）項記載の亜硝酸カルシウム粉末の製
造方法。(2) An aqueous solution containing calcium nitrite as a main component is 25
The method for producing calcium nitrite powder according to claim 1, characterized in that the powder contains at least % by weight of calcium nitrite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4624689A JPH02225308A (en) | 1989-02-27 | 1989-02-27 | Production of calcium nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4624689A JPH02225308A (en) | 1989-02-27 | 1989-02-27 | Production of calcium nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02225308A true JPH02225308A (en) | 1990-09-07 |
Family
ID=12741794
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4624689A Pending JPH02225308A (en) | 1989-02-27 | 1989-02-27 | Production of calcium nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02225308A (en) |
-
1989
- 1989-02-27 JP JP4624689A patent/JPH02225308A/en active Pending
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