JP2008113661A - Method for producing calcium powder of ozone egg shell - Google Patents

Method for producing calcium powder of ozone egg shell Download PDF

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JP2008113661A
JP2008113661A JP2007287151A JP2007287151A JP2008113661A JP 2008113661 A JP2008113661 A JP 2008113661A JP 2007287151 A JP2007287151 A JP 2007287151A JP 2007287151 A JP2007287151 A JP 2007287151A JP 2008113661 A JP2008113661 A JP 2008113661A
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powder
eggshell
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calcium
ozone
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Hatsuyu Ryu
劉發勇
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a calcium powder of ozone egg shell. <P>SOLUTION: The calcined egg shell powder produced by the method has an excellent effect for suppressing harmful pathogenic microbes such as Escherichia coli (E. coli) and an effect for removing harmful additives remaining in foods such as sulfur dioxide and a bleaching agent. Microbes and residual pesticides sticking to the surface of vegetables and fruits are effectively removed by the method to a level meeting the national standards and international criteria. Waste egg shells are regenerated to a resource to decrease the environmental destruction caused by pollutants and the calcined product is applicable as a food material having sterilizing antiseptic effects to enable the suppression of bacteria and the maintenance of the freshness of the food material. It is also effective for reducing residual toxicity of pesticides and harmful additives. Calcium is supplemented by directly taking the egg shell. The egg shell is also usable for the soil amelioration by mixing the soil with the calcium powder of ozone egg shell to improve oxidized soil and improve the pH value. It increases the fertility of the soil and reduces the wash-out of minerals. The egg shell powder lowers the activity of putrefactive bacteria, increases bacteria good for health and decreases the damages caused by diseases and insects. It reduces the quantity of wastes and enables valuable recovery applications. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明はオゾン卵殻カルシウム粉の製造方法に関するものであって、高温焼成下で成型する卵殻粉で、まず、卵殻粉の化学特性、アルカリ度、pH値、及び、酸化カルシウム含量を測定し、更に、オゾン卵殻カルシウム粉を分析し、卵殻粉の微生物に対する殺菌、菌の抑制、及び、卵殻粉の食材上の二酸化硫、及び、有害添加物残留量に対する効果的除去、野菜や果物表面の残留農薬に対し、効果的に除去できるかを分析し、以上の応用により、製品の食材として利用でき、資源回収、再利用の目的を達成するオゾン卵殻カルシウム粉の製造方法に関する。   The present invention relates to a method for producing ozone eggshell calcium powder, which is an eggshell powder molded under high-temperature firing, and firstly measures the chemical properties, alkalinity, pH value, and calcium oxide content of eggshell powder, Analyzing ozone eggshell calcium powder, sterilization of eggshell powder against microorganisms, suppression of bacteria, sulfur dioxide on eggshell powder ingredients and effective removal of residual harmful additives, pesticide residues on vegetable and fruit surfaces In contrast, the present invention relates to a method for producing ozone eggshell calcium powder that can be effectively removed and can be used as a food ingredient for products by the above application and achieves the purpose of resource recovery and reuse.

一般に、鶏卵の組成は、卵殻が卵全体の10〜11%の重量で、厚さは約0.2〜0.4mmであり、中華民国養鶏協会の統計によると、国民は国産鶏卵の平均年消費が275個で、中華民国93年度の鶏卵産量は31248380箱(一箱12キログラム)であり、卵殻の占める比例で推算すると、全年の廃棄卵殻は約37.5万トンである。卵加工においては、国内の液状卵加工工場は、毎日、約93.6トンの卵を処理し、液状卵工場から、毎日、9.36トンの廃棄卵殻があり、もし、これらの卵殻が適当に処理されなければ、環境汚染になる可能性がある。 In general, the composition of chicken eggs is that the eggshell is 10 to 11% of the total weight of the eggs and the thickness is about 0.2 to 0.4 mm. According to the statistics of the China Poultry Association, the population is the average year of domestic eggs. Consumption is 275, and the egg production in 1993 in China is 31248380 boxes (12 kilograms per box). If estimated by the proportion occupied by eggshell, the waste eggshell of all years is about 375,000 tons. In egg processing, domestic liquid egg processing factories process about 93.6 tons of eggs every day, and there are 9.36 tons of discarded eggshells every day from liquid egg factories. If it is not treated properly, there is a possibility of environmental pollution.

日本の学者(澤井氏)は、貝殻を高温下で加熱処理し、貝殻中の炭酸カルシウムと酸化カルシウムの成分を利用した微生物生長に対する研究で、高温処理後の貝殻粉は細菌の繁殖に対し、明らかな抑制効果があることが示されている。また、貝殻粉懸濁液で野菜を洗浄後、細菌数の減少に対しても明らかな作用がある。しかし、貝殻の過度な採取は貝殻の消失を招き、生態平衡が破壊され、よって、本発明は、卵殻を回収し、高温で粉末に焼成し、卵殻粉の基本特性を理解し、資源の再利用の用途を模索する。 A Japanese scholar (Mr. Sawai) studied the growth of microorganisms using heat-treated shells at high temperatures and the components of calcium carbonate and calcium oxide in shells. It is shown that there is a clear inhibitory effect. In addition, after washing vegetables with shellfish powder suspension, there is a clear effect on the reduction of the number of bacteria. However, excessive collection of shells leads to the loss of shells and disrupts ecological equilibrium, so the present invention collects eggshells, fires them into powder at high temperatures, understands the basic characteristics of eggshell powder, and restores resources. Search for usages.

公知の二酸化硫は、漂白、消毒の作用があり、アルコール飲料、果汁、乾燥食品の酸化で褐色になるのを防止し、酵母、黴菌、細菌の生長を抑制し、果物、野菜、酒類、及び、肉品の殺菌、防腐に応用されるが、二酸化硫残留物は、人体に吸収された後、身体の各部位に沈積して排除できず、よって、喘息や呼吸器疾病の原因となる。   Known sulfur dioxide has a bleaching and disinfecting action, prevents browning due to oxidation of alcoholic beverages, fruit juices, and dried foods, suppresses the growth of yeast, bacilli, and bacteria, fruits, vegetables, liquor, and Although it is applied to the sterilization and antiseptic of meat products, the sulfur dioxide residue is absorbed by the human body and cannot be removed by being deposited on each part of the body, thus causing asthma and respiratory diseases.

よって、オゾン卵殻カルシウム粉の製造方法を提供し、高温焼成下で成型される卵殻粉は、卵殻粉の化学特性、アルカリ度、pH値、及び、酸化カルシウム含量により、食材として利用できるようにし、卵殻粉の微生物生長に対する制御、及び、卵殻粉の二酸化硫に対し、抗菌、鮮度維持の効果を有し、野菜や果物の表面に残留した農薬の排除率に効果比較分析を実行して、資源回収、再利用の目的を達成することが必要である。   Therefore, a method for producing ozone eggshell calcium powder is provided, and eggshell powder molded under high-temperature firing can be used as a food, depending on the chemical properties, alkalinity, pH value, and calcium oxide content of eggshell powder, Control the effect on the growth of microorganisms in eggshell powder and the effect of antibacterial and freshness maintenance on sulfur dioxide in eggshell powder, and perform comparative analysis of the effect on the removal rate of pesticides remaining on the surface of vegetables and fruits. It is necessary to achieve the purpose of collection and reuse.

本発明の目的は、オゾン卵殻カルシウム粉の製造方法を提供することにある。 An object of the present invention is to provide a method for producing ozone eggshell calcium powder.

本発明のオゾン卵殻カルシウム粉の製造方法は、廃棄卵殻を収集し、卵殻を洗浄後、オーブンに入れて乾燥させ、卵殻内外表面を乾燥させる材料準備工程と、準備工程を経た卵殻を分けて焼却炉に送り、焼成後に得られる異なる白色度の卵殻灰粉末を得る工程と、焼成工程後、ナノ機により細粒粉状物に圧砕し、分析する工程と、からなる。   The method for producing ozone eggshell calcium powder according to the present invention collects waste eggshells, cleans eggshells, puts them in an oven and dries them, and separates and incinerates the eggshells that have undergone the preparation steps from the material preparation step for drying the eggshell inner and outer surfaces It consists of a step of obtaining eggshell ash powder of different whiteness obtained after firing and firing, and a step of crushing into a fine-grained powder by a nano machine and analyzing after the firing step.

1.
大腸菌(E.col)等の人体の健康に有害な微生物に対する抑制効果に優れ、食品中に残留した二酸化硫は農薬除去に応用できる。
2.
本発明の焼成後の産物は、殺菌、防腐効果を有し、食材の菌の抑制、鮮度維持が可能で、農薬、有害添加物の毒性残留を減少させる。直接食用すると、カルシウムの補充ができる。土壌改良において、オゾン卵殻カルシウム粉と土壌混合後、酸化土質を改善でき、pH値を向上させることができる。土地肥沃力を増加し、ミネラルの流失を減少させる。腐敗菌の活性を低下させ、体によいバクテリアを増加させ、病虫害を減少させる。廃棄物を減少させ、付加価値のある回収応用が可能である。
3.
汚染物の環境破壊を低下させるだけでなく、資源再生利用が可能である。
1.
It has an excellent inhibitory effect on microorganisms harmful to human health such as E. coli, and sulfur dioxide remaining in food can be applied to remove agricultural chemicals.
2.
The product after baking of the present invention has a bactericidal and antiseptic effect, can suppress the fungus of the food material, maintain the freshness, and reduce the toxic residue of agricultural chemicals and harmful additives. If eaten directly, calcium supplementation is possible. In soil improvement, after mixing with ozone eggshell calcium powder and soil, the oxidized soil quality can be improved and the pH value can be improved. Increase land fertility and reduce mineral loss. Decrease the activity of spoilage bacteria, increase healthy bacteria and reduce pest damage. Waste reduction and value-added collection applications are possible.
3.
In addition to reducing the environmental destruction of pollutants, resource recycling is possible.

図1は、本発明のオゾン卵殻カルシウム粉の製造方法を示す図で、以下の工程からなる。
材料準備工程10:廃棄された卵殻を収集し、卵殻は水道水で洗浄後、オーブンで定温110℃で20分焼き、卵殻内外表面を乾燥状態にする。
焼成工程20:材料準備工程10後の卵殻は、分けて焼却炉に送られ、それぞれ、定温800℃で60分焼成、定温1000℃で60分焼成、定温1200℃で60分焼成し、焼成後に得られる異なる白色度の卵殻灰粉末を得て、また、卵殻灰粉末は酸化カルシウム(CaO)を含む固形の結晶体で、室温冷却後、表1で示されるように、異なる温度で焼成後の卵殻形成物の実体外観図であり、卵殻はナノ機により細粒粉状物に圧砕され、異なる保存瓶中に保存されて封され、焼成余剰率(回収率)は:回収率=焼成後の卵殻重量/乾燥後の卵殻重量×100%;
FIG. 1 is a diagram showing a method for producing ozone eggshell calcium powder according to the present invention, which comprises the following steps.
Material preparation step 10: Collect the discarded eggshells, wash the eggshells with tap water, and bake them in an oven at a constant temperature of 110 ° C. for 20 minutes to dry the eggshell inner and outer surfaces.
Firing step 20: The eggshells after the material preparation step 10 are separately sent to an incinerator, and baked at a constant temperature of 800 ° C. for 60 minutes, at a constant temperature of 1000 ° C. for 60 minutes, and at a constant temperature of 1200 ° C. for 60 minutes. Obtained eggshell ash powder with different whiteness is obtained, and eggshell ash powder is a solid crystal containing calcium oxide (CaO), and after cooling at room temperature, as shown in Table 1, after firing at different temperatures It is the substance appearance figure of eggshell formation, eggshell is crushed into fine powder by nano machine, stored in different storage bottles and sealed, and baking surplus rate (recovery rate) is: recovery rate = after baking Eggshell weight / dry eggshell weight × 100%;

検査工程30:焼成工程20後、ナノ機により細粒粉状物に圧砕し、以下の分析を行い、その工程は、化学特性分析301を含み、化学特性分析301は、主に、卵殻粉アルカリ度測定3011、卵殻粉水溶液pH値測定3012、及び、卵殻粉中の酸化カルシウム含量の測定3013、を含み、卵殻粉アルカリ度測定3011は、標準の酸調法と標定法により測定し、まず、0.001グラムの卵殻粉を正確に計り、100mlの水を加えて溶解し、ブンゼンバーナー中に入れて加熱し、二酸化炭素を除去し、メチルオレンジ指示薬を2〜3滴加入した後、標定した0.01Nの塩酸を滴定し(ピンク色に変色)、塩酸滴定量を記録し、アルカリ度を計算する。アルカリ度=0.01N塩酸ミリリットル(ml)/卵殻粉の重量(g)であり、表2を参照すると、異なる焼成温度の卵殻粉溶液サル仮度に対する影響を示し、その結果は、800℃のアルカリ度が36.42meq/gで、温度が1200℃になると、アルカリ度は72.80meq/gに増加し、焼成温度が高いと、灰化率も高くなり、アルカリ度も高くなる。
Inspection process 30: After the baking process 20, the powder is crushed by a nano-machine and the following analysis is performed. The process includes a chemical characteristic analysis 301. The chemical characteristic analysis 301 mainly includes an egg shell powder alkali. Degree measurement 3011, eggshell powder aqueous solution pH value measurement 3012, and measurement 3013 of calcium oxide content in eggshell powder, eggshell powder alkalinity measurement 3011 is measured by a standard acid method and standardization method, Accurately measure 0.001 gram eggshell powder, add 100 ml of water to dissolve, heat in Bunsen burner, remove carbon dioxide, add 2-3 drops of methyl orange indicator, and then standardize. Titrate 0.01N hydrochloric acid (change color to pink), record hydrochloric acid titration, and calculate alkalinity. Alkalinity = 0.01N hydrochloric acid milliliter (ml) / weight of eggshell powder (g), and referring to Table 2, the effect of different baking temperatures on the egg shell powder solution monkey provision is shown, the result is When the alkalinity is 36.42 meq / g and the temperature is 1200 ° C., the alkalinity increases to 72.80 meq / g, and when the baking temperature is high, the ashing rate increases and the alkalinity also increases.

卵殻粉水溶液pH値測定3012は、異なる濃度に調合された卵殻粉溶液により、純水と卵殻粉の比例サンプリング(純水/卵殻粉)は、(
~
)で、リトマス紙により水溶液のアルカリ値を測定し、表3で示されるように、濃度が800℃の卵殻粉で量測されるpH値が11.5で、濃度の増加に伴って、pH値も緩慢になり、濃度が1200℃の時、pH値は13.2に達し、同濃度下、異なる温度焼成の卵殻粉溶液を比較すると、焼成温度が高いほど、pH値も高くなる。
Eggshell powder aqueous solution pH value measurement 3012 is based on eggshell powder solutions prepared at different concentrations, and proportional sampling of pure water and eggshell powder (pure water / eggshell powder) is (
~
), The alkaline value of the aqueous solution was measured with litmus paper, and as shown in Table 3, the pH value measured with eggshell powder having a concentration of 800 ° C. was 11.5, and as the concentration increased, the pH The value also becomes slow, and when the concentration is 1200 ° C., the pH value reaches 13.2. When comparing the eggshell powder solutions of different temperature baking under the same concentration, the higher the baking temperature, the higher the pH value.

また、卵殻粉中の酸化カルシウム含量の測定3013は、過マンガン酸カリウム滴定法により定量の炭酸カルシウムサンプル中の酸化カルシウムの測定法で、測定法は、以下の工程からなる。
1.
卵殻粉を計り、250mlのビーカーに入れ、1ml、36%の塩化水素(HCL)、及び、純水20mlを加入し、加熱溶解する。
2.ろ過液をビーカーに入れ、5%の(NH4)2C2O4溶液を50ml加え、沈殿が現れたら、再度、塩化水素を入れて溶解する。
3.70〜80℃まで持続して加熱し、2〜3滴のメチルオレンジを加え、溶液が赤色反応を呈し、10%のNH4OHを加え、溶液が黄色になり、シュウ酸カルシウム(CaC2O4)が沈殿し、アンモニアの匂いがでるまで攪拌を停止する。
4.
ろ過後、シュウ酸カルシウム(CaC2O4)沈殿物を純水で2〜3回洗浄した後、沈殿物を取り出して、希硫酸により三角錐瓶中で溶解し、純水により1〜2回洗浄する。
5.
溶液を70〜80℃まで加熱し、0.1N KmnO4標準溶液を滴定し、微赤色反応を呈し、且つ、30秒色褪せしないよう保持し、終了である。
The measurement 3013 of the calcium oxide content in the eggshell powder is a method for measuring calcium oxide in a calcium carbonate sample quantified by the potassium permanganate titration method, and the measurement method includes the following steps.
1.
Weigh eggshell powder, put it in a 250 ml beaker, add 1 ml, 36% hydrogen chloride (HCL) and 20 ml of pure water and dissolve by heating.
2. The filtrate is put into a beaker, 50 ml of 5% (NH 4 ) 2 C 2 O 4 solution is added, and when precipitation appears, hydrogen chloride is added again to dissolve.
3. Heat continuously to 70-80 ° C., add 2-3 drops of methyl orange, the solution exhibits a red reaction, 10% NH 4 OH is added, the solution turns yellow, calcium oxalate (CaC Stop stirring until 2 O 4 ) precipitates and smells of ammonia.
4).
After filtration, the calcium oxalate (CaC 2 O 4 ) precipitate is washed 2-3 times with pure water, then the precipitate is taken out, dissolved in a triangular pyramid bottle with dilute sulfuric acid, and once or twice with pure water. Wash.
5.
The solution is heated to 70-80 ° C., a 0.1N KmnO 4 standard solution is titrated, exhibits a slight red reaction, and keeps it from fading for 30 seconds.

表4で示されるように、表中の結果により、焼成温度の酸化カルシウム(CaO)含量に対する影響を表示し、温度が高いほど、酸化カルシウム(CaO)含量が増加する。
As shown in Table 4, the results in the table show the influence of the firing temperature on the calcium oxide (CaO) content, and the higher the temperature, the higher the calcium oxide (CaO) content.

二酸化硫は、漂白、消毒作用を有し、アルコール飲料、果汁、乾燥フルーツ、野菜の酸化で褐色になるのを防止し、効果的に、酵母、黴菌、細菌の生長を抑制するので、食品の漂白功能以外に、果物、野菜、酒類、肉類の殺菌、防腐効果を有する。しかし、中華民国消費者文教基金会が中華民国87年9月に出版した「消費者報道」によると、ディリリー乾燥品の二酸化硫残留問題を報告し、消費者基金会は、14件の市販のディリリー乾燥品が、皆、500ppm基準を超過し(大部分の検査サンプルが10000〜20000ppmで、最高残留量は30000ppm以上であった)、ニュースで報道後、多くのメディアにも取り上げられたので、消費者は、喘息や呼吸器系の疾病を恐れ、ディリリー製品、及び、その他の二酸化硫が残留しやすい製品を排斥するようになった。二酸化硫とディリリー花は、花蓮県のディリリー危機処理部門の努力により、行政院衛生署が、ディリリー乾燥品の二酸化硫残留量基準を4000ppm(4.0g/kg)に修正し、88年5月14日、衛生署食字第88027729号公告が出された。二酸化硫はディリリー等の食材の色を保護し、殺菌、防腐効果があり、付加価値を増加するが、消費者にとっては隠滅された重大な危機である。   Sulfur dioxide has a bleaching and disinfecting effect, prevents browning due to oxidation of alcoholic beverages, fruit juices, dried fruits and vegetables, and effectively suppresses the growth of yeast, gonorrhea and bacteria. In addition to bleaching, it has the effect of sterilizing and preserving fruits, vegetables, liquors and meats. However, according to the "Consumer Report" published in September 1987 by the Consumer Education Foundation of the Republic of China, it reported a sulfur dioxide residue problem in Dilily dried products. Dilily dried products all exceeded the 500ppm standard (most of the test samples were 10,000 to 20000ppm, the maximum residual was over 30000ppm), and after being reported in the news, it was taken up by many media, Consumers are afraid of asthma and respiratory illnesses and are now banned from Dilili products and other products that are prone to residual sulfur dioxide. As for sulfur dioxide and dilily flowers, due to the efforts of the Dilili crisis management department in Hualien County, the administrative office's health department revised the sulfur dioxide residue standard for dried lily products to 4000 ppm (4.0 g / kg). On the 14th, an announcement of Sanitary Department food letter No. 88027729 was issued. Sulfur dioxide protects the color of foods such as dilily, has a bactericidal and antiseptic effect, increases added value, but is a serious crisis for consumers.

よって、本発明は、後遺症のない予防方法に採用を改め、オゾン卵殻カルシウム粉の二酸化硫残留物に対する比較実験302では、市販のディリリー花の表面の二酸化硫残留物に対し測定を実行する。   Therefore, the present invention is re-applied to a preventive method without sequelae, and in the comparative experiment 302 for the sulfur dioxide residue of ozone eggshell calcium powder, the measurement is performed on the sulfur dioxide residue on the surface of the commercially available Dilily flower.

まず、食品中の亜硫酸塩の測定法により測定し、その工程は以下のようである。
1.
市販のディリリー1グラムを計り、異なる焼成温度、及び、異なる濃度の卵殻粉溶液に15分間浸し、浸した後、ディリリーを取り出し、浸した液を残し、ディリリーと液中の二酸化硫含量を測定する。
2.
ディリリーを砕いて、丸底フラスコ内に放置する。
3.
20mlの純水、及び、2mlの純度が95%のアルコールを加入する。
4.
シリンダ内に0.3%のH2O2溶液10mlを加入して吸収液とし、混合指示液1〜2滴加入し、この時、淡い紫色の反応を呈し、更に、0.01NのNaOH溶液を1〜2滴加え、溶液がオリーブ色になるよう反応させる。
5.
10mlの25%の燐酸を丸底フラスコに加入し、蒸留が開始する。
6.
15分加熱後、加熱器をオフにする。
7.
シリンダを取り、煮沸冷却した蒸留水でガラス管前端を洗浄し、シリンダ内を洗い、オリーブ色を15秒呈するまで、0.01NのNaOHにより滴定する。
First, it measures by the measuring method of the sulfite in a foodstuff, The process is as follows.
1.
Weigh 1 gram of commercially available dillilly, soak for 15 minutes in different baking temperatures and eggshell powder solutions of different concentrations, and after soaking, take out the dillilly, leave the soaked liquid, and measure the dillilly and sulfur dioxide content in the liquid. .
2.
Crush the dilily and leave in a round bottom flask.
3.
Add 20 ml of pure water and 2 ml of 95% pure alcohol.
4).
Add 10 ml of 0.3% H 2 O 2 solution into the cylinder to make an absorbing solution, add 1 to 2 drops of mixing indicator solution, and at this time, a pale purple reaction is exhibited, and a 0.01 N NaOH solution is added. 1 to 2 drops is added and the solution is allowed to react until it is olive.
5.
10 ml of 25% phosphoric acid is added to the round bottom flask and distillation begins.
6).
After heating for 15 minutes, turn off the heater.
7).
Remove the cylinder, wash the front end of the glass tube with boiling cooled water, wash the inside of the cylinder and titrate with 0.01 N NaOH until it gives an olive color for 15 seconds.

表5で示されるように、異なる温度処理、及び、濃度の卵殻粉溶液のディリリー二酸化硫残留量の固体に対する影響を示し、卵殻粉の固体のディリリー、及び、ディリリーを浸した液の優れた残留量除去効果を表示し、焼成後の卵殻粉は、温度が高いほど効果が優れている。
表5 異なる濃度、及び、異なる温度段階下の卵殻粉対ディリリーの二酸化残留量(ppm)
Table 5 shows the effect of different temperature treatments and concentrations of residual Dilily sulfur dioxide in eggshell powder solutions on solids, and excellent residuals of Dilily in eggshell powder and liquids dipped in Dilily The amount removal effect is displayed, and the fired eggshell powder is more effective at higher temperatures.
Table 5 Residues in ppm of eggshell powder vs. Diliri under different concentrations and different temperature steps (ppm)

更に、卵殻粉溶液を浸す回数対ディリリーの二酸化硫残留量の測定について、表6を参照すると、表中、卵殻粉溶液に浸す回数が多いほど、二酸化硫残留量は倍数で下降する。
表6 1/1000 濃度の卵殻粉のディリリーの二酸化硫残留量(ppm)
Furthermore, referring to Table 6 for the measurement of the number of times the eggshell powder solution is soaked versus the amount of residual sulfur dioxide in Dililey, as the number of times of soaking in the eggshell powder solution increases in the table, the sulfur dioxide residue decreases in multiples.
Table 6 Residual amount of sulfur dioxide (ppm) in Dilily of eggshell powder at 1/1000 concentration

上述のように、卵殻粉は、その強い酸化性とカルシウム自身のキレート力により、食品中の添加物を酸化させるか、或いは、大分子にキレート結合し、その残留量を減少させる。二酸化硫(SO2)残留量において、実験で証明されているのは、同一の濃度下で、1200℃の1/1000濃度の卵殻粉溶液は、ディリリーが含む二酸化硫(SO2)残留量を99.4%以上下降させることができる。 As described above, eggshell powder oxidizes additives in food due to its strong oxidizability and the chelating power of calcium itself, or chelate-bonds to large molecules to reduce the residual amount. In the residual amount of sulfur dioxide (SO 2 ), it has been proved by experiments that, under the same concentration, an egg shell powder solution at a concentration of 1200 ° C. has a residual sulfur dioxide (SO 2 ) content of Dilily. It can be lowered by 99.4% or more.

微生物殺菌の実験分析303は、焼成温度1200℃の卵殻粉を1/1000濃度の水溶液に配合し、培養基上に塗布すると非常に効果的な殺菌効果がある。実施例によると、主に、NA(nutrient agar)培養基を製作し、凝固後、大腸菌液50μlを均一に塗布し、24時間培養後、菌落数を対照組とする。   The experimental analysis 303 of microbial sterilization has a very effective sterilization effect when eggshell powder having a baking temperature of 1200 ° C. is blended in an aqueous solution having a 1/1000 concentration and applied onto a culture medium. According to the examples, mainly an NA (nutrient agar) culture medium is prepared, after coagulation, 50 μl of E. coli solution is uniformly applied, cultured for 24 hours, and the number of bacteria is used as a control group.

大腸菌E.coliにより純菌活性後、活性菌の懸濁液に、異なる温度焼成後(800℃)の卵殻粉を添加し、卵殻粉は、洗浄液の比率が1/1000で、10、20、30分後の浸し液を50μl取り出し、NA培養基上に塗布し、37℃下で、24時間培養後、菌落数を計算して実験組とし、実験結果は、対照組の菌落数は4538/CFUであることを証明し、結果は、1200℃で焼成処理した者は、10分浸した後、菌落数が16/CFUまで減少し、浸す時間が30分まで増加すると、菌落数は、約0/CFU、更には、完全に大腸菌E.Coliを殺すことが示され、同時に、焼成温度が高いと、浸す時間も長くなり、微生物の繁殖能力に対する抑制効果が更に強くなることが推論でき、また、1200℃、30分、生菌数が0の浸し効果が一番よく、その実施例のデータは、以下の表で示される。
After pure bacterial activity by E. coli E. coli, eggshell powder after baking at different temperatures (800 ° C.) is added to the suspension of active bacteria, and the eggshell powder has a washing liquid ratio of 1/1000, 10, 20, After 30 minutes, 50 μl of the soaking solution was taken out, applied on the NA culture medium, cultured at 37 ° C. for 24 hours, and the number of bacteria was calculated to obtain an experimental group. The experimental result shows that the number of bacteria in the control group is 4538 / CFU. As a result, the result of the calcination treatment at 1200 ° C. is that the number of bacteria is reduced to 16 / CFU after being immersed for 10 minutes, and the number of bacteria is about 0 when the immersion time is increased to 30 minutes. / CFU, and even E. coli completely killed, and at the same time, it can be inferred that the higher the baking temperature, the longer the immersion time, and the stronger the inhibitory effect on the ability of microorganisms to propagate. 1200 ° C, 30 minutes, the best soaking effect with 0 viable count is the best Example data is shown in the table below.

本発明は、更に、農薬除去に応用でき、簡単には、農薬は農林作物を害虫やその他の生物による危害から保護する化学品で、現在、世界中で市販される農薬は約600種類あり、主に、殺虫剤、殺菌剤、除草剤、殺ダニ剤、殺線虫剤、殺鼠剤、植物生長調節剤、がある。   The present invention can also be applied to pesticide removal. Briefly, pesticides are chemicals that protect agricultural and forestry crops from harm by pests and other organisms. Currently, there are about 600 types of pesticides marketed worldwide. There are mainly insecticides, fungicides, herbicides, acaricides, nematicides, rodenticides, plant growth regulators.

農薬の発展は、早期から、無機物と天然物を利用し、その後、有機化学合成品が迅速に発展し、その理化性質、毒性、防治効果、及び、人類と環境に対する影響は皆異なり、農薬の毒性が低く、残留が少なくても、環境生態や人体に影響がある。農民は苦労して栽培した農作物を害虫に侵蝕されるのを恐れ、農薬を噴射するが、現在、台湾では、毎年300万トンの野菜や果物の内、約3%(即ち、9万トン)が不合格で、残りの「合格」野菜は、農薬がないことを保証するものではなく、農薬の残量が許容範囲内であるだけであり、つまり、購入した野菜には、農薬が含有されている可能性があり、農業委員会薬物毒物試験所も、金門島で中国の農産品に対し農薬残留検査を行ったところ、中華民国90年の検査結果では、野菜の不合格率が33%に達し、果物は11%、91年度に再度検査を行ったところ、野菜の不合格率は50%、果物の不合格率は20%にも達し、稲も農薬が残留することが普遍的である。   The development of agricultural chemicals uses inorganic and natural products from an early stage, and then organic chemical synthesis products develop rapidly, and their rationalization properties, toxicity, preventive effects, and effects on humans and the environment are all different. Even if it is low in toxicity and low in residue, it has an impact on environmental ecology and the human body. Farmers are afraid of pests eroding their hard-grown crops and spray pesticides. Currently, in Taiwan, about 3% (ie 90,000 tons) of the 3 million tons of vegetables and fruits every year Failing and the remaining “passed” vegetables are not guaranteed to be free of pesticides, and the remaining amount of pesticides is only acceptable, that is, the purchased vegetables contain pesticides. Agricultural Commission's Drug Toxicology Laboratory also conducted a pesticide residue test on Chinese agricultural products on Kinmen Island. According to the results of the inspection in 1990, the rejection rate of vegetables was 33%. The fruit was 11%, and when it was inspected again in fiscal 1991, the rejection rate of vegetables reached 50%, the rejection rate of fruits reached 20%, and it was universal that rice also contained pesticides. is there.

本発明の新規性と実用性を更に明らかなものにするため、公知技術との比較分析は以下のようである。
公知技術:
1.
二酸化硫残留物は、人体に吸収されて身体の各部位に堆積して排除できず、喘息や呼吸器系疾病の原因となる。
2.
廃棄卵殻を適切に処理しなければ、環境汚染につながる。
本発明の長所:
2.
大腸菌(E.col)等の人体の健康に有害な微生物に対する抑制効果に優れ、食品中に残留した二酸化硫は農薬除去に応用できる。
3.
本発明の焼成後の産物は、殺菌、防腐効果を有し、食材の菌の抑制、鮮度維持が可能で、農薬、有害添加物の毒性残留を減少させる。直接食用すると、カルシウムの補充ができる。土壌改良において、オゾン卵殻カルシウム粉と土壌混合後、酸化土質を改善でき、pH値を向上させることができる。土地肥沃力を増加し、ミネラルの流失を減少させる。腐敗菌の活性を低下させ、体によいバクテリアを増加させ、病虫害を減少させる。廃棄物を減少させ、付加価値のある回収応用が可能である。
4.
汚染物の環境破壊を低下させるだけでなく、資源再生利用が可能である。{ひよく}
In order to further clarify the novelty and practicality of the present invention, a comparative analysis with known techniques is as follows.
Known technology:
1.
Sulfur dioxide residues are absorbed by the human body and cannot be eliminated by depositing on various parts of the body, causing asthma and respiratory diseases.
2.
If waste eggshells are not treated properly, it can lead to environmental pollution.
Advantages of the present invention:
2.
It has an excellent inhibitory effect on microorganisms harmful to human health such as E. coli, and sulfur dioxide remaining in food can be applied to remove agricultural chemicals.
3.
The product after baking of the present invention has a bactericidal and antiseptic effect, can suppress the fungus of the food material, maintain the freshness, and reduce the toxic residue of agricultural chemicals and harmful additives. If eaten directly, calcium supplementation is possible. In soil improvement, after mixing with ozone eggshell calcium powder and soil, the oxidized soil quality can be improved and the pH value can be improved. Increase land fertility and reduce mineral loss. Decrease the activity of spoilage bacteria, increase healthy bacteria and reduce pest damage. Waste reduction and value-added collection applications are possible.
4).
In addition to reducing the environmental destruction of pollutants, resource recycling is possible. {Frequently}

本発明では好ましい実施例を前述の通り開示したが、これらは決して本発明に限定するものではなく、当該技術を熟知する者なら誰でも、本発明の精神と領域を脱しない範囲内で各種の変動や潤色を加えることができ、従って本発明の保護範囲は、特許請求の範囲で指定した内容を基準とする。 In the present invention, preferred embodiments have been disclosed as described above. However, the present invention is not limited to the present invention, and any person who is familiar with the technology can use various methods within the spirit and scope of the present invention. Variations and moist colors can be added, so the protection scope of the present invention is based on what is specified in the claims.

本発明の製造工程図である。It is a manufacturing-process figure of this invention. 本発明の卵殻形成物の実体外観図である。It is a substance external view of the eggshell formation thing of the present invention.

符号の説明Explanation of symbols

10 材料準備工程
20 焼成工程
30 検査工程
301 化学特性分析
3011 卵殻粉アルカリ度測定
3012 卵殻粉水溶液pH値測定
3013 卵殻粉中の酸化カルシウム含量の測定
302 二酸化硫残留物の比較分析
303 微生物殺菌の実験分析
DESCRIPTION OF SYMBOLS 10 Material preparation process 20 Baking process 30 Inspection process 301 Chemical characteristic analysis 3011 Eggshell powder alkalinity measurement 3012 Eggshell powder aqueous solution pH value measurement 3013 Measurement of calcium oxide content in eggshell powder 302 Comparative analysis of sulfur dioxide residue 303 Experiment of microorganism sterilization analysis

Claims (8)

オゾン卵殻カルシウム粉の製造方法であって、
廃棄卵殻を収集し、前記卵殻を洗浄後、オーブンに入れて乾燥させ、前記卵殻内外表面を乾燥させる材料準備工程と、
前記準備工程を経た卵殻を分けて焼却炉に送り、焼成後に得られる異なる白色度の卵殻灰粉末を得る工程と、
からなり、前記卵殻灰粉末は酸化カルシウム(CaO)を含む固形の結晶体で、これにより、廃棄卵殻を資源生成し、汚染物の環境破壊を減少させ、焼成後の産物は殺菌、防腐効果を有し、食材の細菌抑制や鮮度の維持に応用できると共に、農薬、有害添加物の毒性残留を減少させる。直接食用すると、カルシウムの補充ができ、土壌改良において、オゾン卵殻カルシウム粉と土壌混合後、酸化土質を改善でき、pH値を向上させることができ、土地肥沃力を増加し、ミネラルの流失を減少させ、腐敗菌の活性を低下させ、体によいバクテリアを増加させ、病虫害を減少させ、廃棄物を減少させ、付加価値のある回収応用が可能であることを特徴とするオゾン卵殻カルシウム粉の製造方法。
A method for producing ozone eggshell calcium powder,
A material preparation step of collecting waste eggshells, washing the eggshells, drying them in an oven, and drying the inner and outer surfaces of the eggshells;
Dividing the eggshell that has undergone the preparation step and sending it to an incinerator to obtain eggshell ash powders of different whiteness obtained after firing; and
The eggshell ash powder is a solid crystal containing calcium oxide (CaO), which generates waste eggshell as resources, reduces the environmental destruction of pollutants, and the baked product has a sterilizing and antiseptic effect. It can be applied to control the bacteria of foodstuffs and maintain freshness, and reduce the residual toxicity of pesticides and harmful additives. When directly edible, calcium can be replenished, and in soil improvement, after mixing with ozone eggshell calcium powder and soil, oxidized soil quality can be improved, pH value can be increased, land fertility is increased, and mineral loss is reduced Production of ozone eggshell calcium powder, which can reduce the activity of spoilage bacteria, increase healthy bacteria, reduce pest damage, reduce waste, and enable value-added recovery applications Method.
前記焼成工程後、更に、機器により細粒粉状物に圧砕され、検査工程中の化学特性分析の卵殻粉アルカリ度測定は、標準の酸調法と標定法により測定されることを特徴とする請求項1に記載のオゾン卵殻カルシウム粉の製造方法。 After the firing step, the powder is further crushed into fine powder by an apparatus, and the eggshell powder alkalinity measurement in chemical property analysis during the inspection step is measured by a standard acid method and a standard method. The manufacturing method of the ozone eggshell calcium powder of Claim 1. 前記焼成工程は、更に、ナノ機により細粒粉状物に圧砕され、検査工程中の化学特性分析の卵殻粉中の酸化カルシウム含量の測定は、過マンガン酸カリウム滴定法により定量の炭酸カルシウムサンプル中の酸化カルシウムの測定法であることを特徴とする請求項1に記載のオゾン卵殻カルシウム粉の製造方法。 The calcining step is further crushed into fine powder by a nano machine, and the calcium oxide content in eggshell powder for chemical property analysis during the inspection step is measured by a potassium permanganate titration method. 2. The method for producing ozone eggshell calcium powder according to claim 1, wherein the method is a method for measuring calcium oxide in the solution. 前記卵殻粉中の酸化カルシウム含量の測定法は、主に、
1.
卵殻粉を計り、250mlのビーカーに入れ、1ml、36%の塩化水素(HCL)、及び、純水20mlを加入し、加熱溶解する工程と、
2.
ろ過液をビーカーに入れ、5%の(NH4)2C2O4溶液を50ml加え、沈殿が現れたら、再度、塩化水素を入れて溶解する工程と、
3.
70〜80℃まで持続して加熱し、2〜3滴のメチルオレンジを加え、溶液が赤色反応を呈し、10%のNH4OHを加え、溶液が黄色になり、シュウ酸カルシウム(CaC2O4)が沈殿し、アンモニアの匂いがでるまで攪拌を停止する工程と、
4.
ろ過後、シュウ酸カルシウム(CaC2O4)沈殿物を純水で2〜3回洗浄した後、沈殿物を取り出して、希硫酸により三角錐瓶中で溶解し、純水により1〜2回洗浄する工程と、
5.
溶液を70〜80℃まで加熱し、0.1N KmnO4標準溶液を滴定し、微赤色反応を呈し、且つ、30秒色褪せしないよう保持する工程と、
からなることを特徴とする請求項3に記載のオゾン卵殻カルシウム粉の製造方法。
The method for measuring the calcium oxide content in the eggshell powder is mainly:
1.
Measuring eggshell powder, putting it in a 250 ml beaker, adding 1 ml, 36% hydrogen chloride (HCL), and 20 ml of pure water, heating and dissolving;
2.
Put the filtrate in a beaker, add 50 ml of 5% (NH 4 ) 2 C 2 O 4 solution, and when precipitation appears, add hydrogen chloride again to dissolve,
3.
Heat continuously to 70-80 ° C., add 2-3 drops of methyl orange, the solution reacts red, 10% NH 4 OH is added, the solution turns yellow, calcium oxalate (CaC 2 O 4 ) precipitating and stopping stirring until ammonia smells;
4).
After filtration, the calcium oxalate (CaC 2 O 4 ) precipitate is washed 2-3 times with pure water, then the precipitate is taken out, dissolved in a triangular pyramid bottle with dilute sulfuric acid, and once or twice with pure water. A cleaning step;
5.
Heating the solution to 70-80 ° C., titrating a 0.1N KmnO 4 standard solution to exhibit a faint red reaction and hold for 30 seconds without fading;
The method for producing ozone eggshell calcium powder according to claim 3, comprising:
前記検査工程中の微生物殺菌の実験分析は、NA培養基を製作し、凝固後、大腸菌液50μlを均一に塗布し、24時間培養後、菌落数を対照組とすることを特徴とする請求項1に記載のオゾン卵殻カルシウム粉の製造方法。 The experimental analysis of sterilization of microorganisms during the inspection process is characterized in that NA culture medium is produced, coagulated, 50 μl of E. coli solution is uniformly applied, cultured for 24 hours, and the number of bacteria is used as a control group. The manufacturing method of ozone eggshell calcium powder as described in 2. 大腸菌E.coliにより純菌活性後、活性菌の懸濁液に、異なる温度焼成後(800℃)の卵殻粉を添加し、前記卵殻粉は、洗浄液の比率が1/1000で、10、20、30分後の浸し液を50μl取り出し、NA培養基上に塗布し、37℃下で、24時間培養後、菌落数を計算して実験組とすることを特徴とする請求項5に記載のオゾン卵殻カルシウム粉の製造方法。 After pure bacterial activity by E. coli, eggshell powder after baking at different temperatures (800 ° C.) is added to the suspension of active bacteria, and the eggshell powder has a washing liquid ratio of 1/1000 and 10, 20 6. The ozone according to claim 5, wherein 50 μl of the immersion solution after 30 minutes is taken out, applied onto an NA culture medium, cultured at 37 ° C. for 24 hours, and the number of bacteria is calculated to form an experimental group. A method for producing eggshell calcium powder. 前記検査工程中の二酸化流残留物の比較実験は、市販のディリリー花の表面の二酸化硫残留物に対し測定を実行し、食品中の亜硫酸塩の測定法により測定することを特徴とする請求項1に記載のオゾン卵殻カルシウム粉の製造方法。 The comparison experiment of the dioxide residue during the inspection step is performed by measuring a sulfur dioxide residue on the surface of a commercially available dilily flower and measuring by a method of measuring sulfite in food. 2. The method for producing ozone eggshell calcium powder according to 1. 前記二酸化硫残留物の比較実験は、
1.
市販のディリリー1グラムを計り、異なる焼成温度、及び、異なる濃度の卵殻粉溶液に15分間浸し、浸した後、ディリリーを取り出し、浸した液を残し、ディリリーと液中の二酸化硫含量を測定する工程と、
2.
ディリリーを砕いて、丸底フラスコ内に放置する工程と、
3.
20mlの純水、及び、2mlの純度が95%のアルコールを加入する工程と、
4.
シリンダ内に0.3%のH2O2溶液10mlを加入して吸収液とし、混合指示液1〜2滴加入し、この時、淡い紫色の反応を呈し、更に、0.01NのNaOH溶液を1〜2滴加え、溶液がオリーブ色になるよう反応させる工程と、
5.
10mlの25%の燐酸を丸底フラスコに加入し、蒸留が開始する工程と、
6.
15分加熱後、加熱器をオフにする工程と、
7.
シリンダを取り、煮沸冷却した蒸留水でガラス管前端を洗浄し、シリンダ内を洗い、オリーブ色を15秒呈するまで、0.01NのNaOHにより滴定する工程と、
からなることを特徴とする請求項7に記載のオゾン卵殻カルシウム粉の製造方法。
Comparative experiment of the sulfur dioxide residue
1.
Weigh 1 gram of commercially available dillilly, soak for 15 minutes in different baking temperatures and eggshell powder solutions of different concentrations, and after soaking, take out the dillilly, leave the soaked liquid, and measure the dillilly and sulfur dioxide content in the liquid. Process,
2.
Crushing the Dilily and leaving it in a round bottom flask;
3.
Adding 20 ml of pure water and 2 ml of 95% pure alcohol;
4).
Add 10 ml of 0.3% H 2 O 2 solution into the cylinder to make an absorbing solution, add 1 to 2 drops of mixing indicator solution, and at this time, a pale purple reaction is exhibited, and a 0.01 N NaOH solution is added. Adding 1 to 2 drops and reacting the solution so that it becomes olive color;
5.
Adding 10 ml of 25% phosphoric acid to the round bottom flask and starting distillation;
6).
After heating for 15 minutes, turning off the heater;
7).
Removing the cylinder, washing the front end of the glass tube with boiled and cooled distilled water, washing the inside of the cylinder, and titrating with 0.01 N NaOH until an olive color is exhibited for 15 seconds;
The method for producing ozone eggshell calcium powder according to claim 7, comprising:
JP2007287151A 2006-11-06 2007-11-05 Method for producing calcium powder of ozone egg shell Pending JP2008113661A (en)

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CN103302081A (en) * 2013-06-27 2013-09-18 北京二商健力食品科技有限公司 Preparation method of eggshell powder and processing device
CN103341481A (en) * 2013-06-27 2013-10-09 北京二商健力食品科技有限公司 Method and equipment for processing egg shell powder
JP2014171402A (en) * 2013-03-06 2014-09-22 Q P Corp Agent for reducing concentration of radioactive cesium in crops, and method for reducing concentration of radioactive cesium in crops
CN104297318A (en) * 2014-09-09 2015-01-21 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of network-structure nano-material for gas sensor

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TWI715980B (en) * 2019-05-15 2021-01-11 鄧有偉 Biological calcium filter material and manufacturing method thereof

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JPH0576313A (en) * 1991-09-19 1993-03-30 Nakajima Nouchikusan Kenkyusho:Kk Production of healthy food using eggshell as raw material
JPH073263A (en) * 1993-06-14 1995-01-06 Nippon Suisan Kaisha Ltd Soil improver of pulverized eggshell with good affinity to soil and production thereof
JPH0717711A (en) * 1993-02-24 1995-01-20 G & G:Kk Highly active calcium oxide and powdering agent
JP2002255597A (en) * 2001-02-23 2002-09-11 Ube Material Industries Ltd Highly reactive slaked lime and manufacturing method for the same
JP2002265311A (en) * 2001-03-14 2002-09-18 Mtc:Kk Fungicidal/antimicrobial agent and fungicidal/ antimicrobial method
JP2006246706A (en) * 2005-03-08 2006-09-21 Masataka Sato Egg-shell ion powder and method for producing the same

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JPH0576313A (en) * 1991-09-19 1993-03-30 Nakajima Nouchikusan Kenkyusho:Kk Production of healthy food using eggshell as raw material
JPH0717711A (en) * 1993-02-24 1995-01-20 G & G:Kk Highly active calcium oxide and powdering agent
JPH073263A (en) * 1993-06-14 1995-01-06 Nippon Suisan Kaisha Ltd Soil improver of pulverized eggshell with good affinity to soil and production thereof
JP2002255597A (en) * 2001-02-23 2002-09-11 Ube Material Industries Ltd Highly reactive slaked lime and manufacturing method for the same
JP2002265311A (en) * 2001-03-14 2002-09-18 Mtc:Kk Fungicidal/antimicrobial agent and fungicidal/ antimicrobial method
JP2006246706A (en) * 2005-03-08 2006-09-21 Masataka Sato Egg-shell ion powder and method for producing the same

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014171402A (en) * 2013-03-06 2014-09-22 Q P Corp Agent for reducing concentration of radioactive cesium in crops, and method for reducing concentration of radioactive cesium in crops
CN103302081A (en) * 2013-06-27 2013-09-18 北京二商健力食品科技有限公司 Preparation method of eggshell powder and processing device
CN103341481A (en) * 2013-06-27 2013-10-09 北京二商健力食品科技有限公司 Method and equipment for processing egg shell powder
CN103302081B (en) * 2013-06-27 2016-01-27 北京二商健力食品科技有限公司 A kind of preparation method of egg-shell meal and process equipment
CN104297318A (en) * 2014-09-09 2015-01-21 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of network-structure nano-material for gas sensor

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