JPH1087307A - Production of calcium phosphate-containing composition having antimicrobial property - Google Patents

Production of calcium phosphate-containing composition having antimicrobial property

Info

Publication number
JPH1087307A
JPH1087307A JP24335896A JP24335896A JPH1087307A JP H1087307 A JPH1087307 A JP H1087307A JP 24335896 A JP24335896 A JP 24335896A JP 24335896 A JP24335896 A JP 24335896A JP H1087307 A JPH1087307 A JP H1087307A
Authority
JP
Japan
Prior art keywords
phosphoric acid
calcium phosphate
shells
calcium
antimicrobial property
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.)
Withdrawn
Application number
JP24335896A
Other languages
Japanese (ja)
Inventor
Joji Yamahara
條二 山原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Research Institute for Production Development
Original Assignee
Research Institute for Production Development
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Research Institute for Production Development filed Critical Research Institute for Production Development
Priority to JP24335896A priority Critical patent/JPH1087307A/en
Publication of JPH1087307A publication Critical patent/JPH1087307A/en
Withdrawn legal-status Critical Current

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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain a calcium phosphate-contg. compsn. having antimicrobial property by allowing shells of animals to react with phosphoric acid compds., especially by effectively using sea shells which are usually treated as an industrial waste. SOLUTION: Shells of animals are made to react with phosphoric acid compds. to obtain calcium phosphate having antimicrobial property. As for sells of animals, especially seashells or fresh water shells (e.g. oyster and scallop) are preferably used. As for the phosphoric acid compds., phosphoric acid or phosphates such as calcium phophate, bruncite and monetite can be used. To produce the calcium phosphate having antimicrobial property, animal shells are pulverized to prepare a water suspension having 2 to 15wt.% concn., and then phosphoric acid compds. are added by 0.3 to 0.33 equiv. calculated as P2 O5 to calcium (CaO) in the reaction liquid at 50 to 150 deg.C for 1 to 5 hours.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、従来、その大部分
が廃棄されていた動物の殻、特に貝殻を有効利用して、
抗菌性を有するリン酸カルシウムを製造する方法に関す
る。
BACKGROUND OF THE INVENTION The present invention relates to the use of animal shells, particularly shells, which have been largely discarded.
The present invention relates to a method for producing calcium phosphate having antibacterial properties.

【0002】[0002]

【従来の技術】従来、リン酸カルシウムは石灰とリン酸
化合物で製造されているが、この方法では、石灰石の採
掘とそれに伴う自然破壊の問題があり、また、原料価格
も上昇している。ところで、天然の貝殻類は、炭酸カル
シウムを多量に含有しているにもかかわらず、その一部
が土壌改良材、中和剤、漢方薬原料等として使用されて
いる程度で、大部分は、産業廃棄物として処理されてい
る。
2. Description of the Related Art Conventionally, calcium phosphate has been produced from lime and a phosphate compound. However, this method has a problem of mining limestone and accompanying natural destruction, and the cost of raw materials has been rising. By the way, despite the fact that natural shells contain large amounts of calcium carbonate, some of them are used as soil conditioners, neutralizers, raw materials for herbal medicines, etc. Treated as waste.

【0003】[0003]

【発明が解決しようとする課題】本発明者らは、産業廃
棄物として処分されている貝殻類の有効利用を図るべく
鋭意研究を重ねた結果、貝殻類に限らず、それらを含
め、炭酸カルシウムを含有する動物の殻から、安価に抗
菌作用を有し且つリン酸カルシウムを含む成分が得られ
ることを見いだし、本発明を完成するに至った。
SUMMARY OF THE INVENTION The present inventors have conducted intensive studies to effectively use shells disposed of as industrial waste, and as a result, not only shells but also calcium carbonate including them. The present inventors have found that a component having an antibacterial effect and containing calcium phosphate can be obtained at low cost from animal shells containing the compound, and have completed the present invention.

【0004】[0004]

【課題を解決するための手段】すなわち本発明は、動物
の殻と、リン酸化合物を反応させることを特徴とする、
抗菌性を有するリン酸カルシウムの製造方法
That is, the present invention is characterized in that an animal shell is reacted with a phosphate compound.
Method for producing calcium phosphate having antibacterial properties

【0005】[0005]

【発明の実施の態様】本発明において、リン酸化合物と
の反応に供する動物の殻としては、炭酸カルシウムを含
有するものいずれでもよく、例えば、腔腸動物(例、カ
ンザシゴカイ等)、棘皮動物(例、ウニ等)、軟体動物
(例、甲イカ、貝類、蝸牛類等)、節足動物(例、甲殻
類等)および脊椎動物(例、鳥類)の殻、甲および卵殻
が挙げられる。これらは、単独でも、また、二種以上を
混合して用いてもよく、入手し易さや、量的な観点か
ら、特に、海水産、淡水産の貝類(例、カキ、ホタテ
等)が好ましい。
BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, the shell of an animal to be subjected to a reaction with a phosphate compound may be any one containing calcium carbonate, for example, a coelenterate animal (eg, Kansashigokai, etc.), an echinoderm animal ( Eg, sea urchins), molluscs (eg, squid, shellfish, cochleas, etc.), arthropods (eg, crustaceans, etc.) and vertebrate (eg, birds) shells, shells and eggshells. These may be used alone or as a mixture of two or more. From the viewpoints of availability and quantity, particularly preferred are seawater and freshwater shellfish (eg, oysters, scallops, etc.). .

【0006】これらの動物の殻は、要すれば、清浄化し
た後、炭酸カルシウム(CaCO3)原料として、そのま
ままたは好ましくは平均粒度1〜10μm程度に粉砕し
て、リン酸化合物との反応に供することができる。
[0006] If necessary, these animal husks are cleaned and then ground as a raw material for calcium carbonate (CaCO 3 ) or, preferably, to an average particle size of about 1 to 10 µm to react with the phosphoric acid compound. Can be offered.

【0007】動物の殻との反応に使用するリン酸化合物
としては、リン酸、リン酸一カルシウム、ブルシャイ
ト、モネタイトのようなリン酸塩が挙げられる。動物の
殻と、リン酸化合物との反応は、反応に供する動物の殻
中の炭酸カルシウムや、生石灰の量により異なるが、通
常、動物の殻を2〜15重量%の水懸濁液とし、これ
に、反応液中のカルシウム(CaO)に対してリン酸
(P25)として0.3〜0.33当量のリン酸化合物を
用い、50〜150℃で、1〜5時間反応させる。得ら
れた反応混合物は、要すれば、中和し、そのまま、ある
いは反応生成物を、濾過、遠心分離等の常法により、分
離し、150℃〜500℃で乾燥して使用する。これら
反応生成物の組成は、X線回析や、IPC発光分析法に
より同定、分析でき、通常、反応生成物の固形分あたり
15重量%以上のリン酸カルシウムを含む反応生成物が
得られる。
[0007] Phosphoric acid compounds used for the reaction with animal hulls include phosphates such as phosphoric acid, monocalcium phosphate, brushite and monetite. The reaction between the animal hull and the phosphate compound varies depending on the amount of calcium carbonate and quick lime in the animal husk to be subjected to the reaction. The reaction is carried out at 50 to 150 ° C. for 1 to 5 hours using a phosphoric acid compound of 0.3 to 0.33 equivalent as phosphoric acid (P 2 O 5 ) with respect to calcium (CaO) in the reaction solution. . If necessary, the obtained reaction mixture is neutralized and used as it is, or the reaction product is separated by a conventional method such as filtration or centrifugation, and dried at 150 to 500 ° C. for use. The composition of these reaction products can be identified and analyzed by X-ray diffraction or IPC emission spectrometry, and usually a reaction product containing 15% by weight or more of calcium phosphate per solid content of the reaction product is obtained.

【0008】得られたリン酸カルシウム含有組成物は、
公知のリン酸カルシウムと同様に、医薬原料、食品添加
物、歯磨きの基材などの分野で使用することができる。
[0008] The resulting calcium phosphate-containing composition comprises:
Like the known calcium phosphate, it can be used in the fields of pharmaceutical raw materials, food additives, toothpastes, and the like.

【0009】[0009]

【実施例】以下に実施例を挙げて本発明をさらに詳しく
説明するが、これらに限定されるものではない。実施例
中、「%」とあるは、特に断らない限り、重量%を意味
する。 実施例1 カキ殻粉末(炭酸カルシウム含量96%;平均粒度6μ
m)1000gに水9000gを加えて、よく撹拌して
懸濁させ、90℃以上に保持しながら、撹拌下に、43
%リン酸1285gを1時間かけて滴下し、反応させ
た。反応終了後、反応混合液を濾過し、残った固形分を
温水で洗浄した。ついで、250℃にて5時間乾燥し、
反応生成物1150gを得た。これをサンプルミルで平
均粒度9μmに粉砕した。この反応生成物をX線回析、
ICP発光分析により分析したところ、リン酸カルシウ
ム15%とヒドロキシアパタイト85%を含有すること
が判明した。
The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the invention is limited thereto. In Examples, “%” means “% by weight” unless otherwise specified. Example 1 Oyster husk powder (calcium carbonate content 96%; average particle size 6μ)
m) 1000 g of water and 9000 g of water were added, and the mixture was stirred well and suspended.
1285 g of phosphoric acid was added dropwise over 1 hour to cause a reaction. After completion of the reaction, the reaction mixture was filtered, and the remaining solid content was washed with warm water. Then, dried at 250 ° C. for 5 hours,
1150 g of a reaction product was obtained. This was ground with a sample mill to an average particle size of 9 μm. X-ray diffraction of this reaction product,
Analysis by ICP emission analysis revealed that it contained 15% calcium phosphate and 85% hydroxyapatite.

【0010】実施例2 実施例1と同様にして、ただし、ホタテ粉末(炭酸カル
シウム含量95%;平均粒度3μm)およびその焼成物
(1200℃にて2時間焼成)を用い、リン酸との反応
温度150℃として、反応生成物を得た。得られた反応
生成物のX線回析、ICP発光分析による成分分析結果
を次に示す。
Example 2 In the same manner as in Example 1, except that scallop powder (calcium carbonate content: 95%; average particle size: 3 μm) and its calcined product (calcined at 1200 ° C. for 2 hours) were reacted with phosphoric acid. The reaction product was obtained at a temperature of 150 ° C. The results of component analysis by X-ray diffraction and ICP emission analysis of the obtained reaction product are shown below.

【0011】CaO:55.04% P25:38.02% CaO/P25モル比:3.66 灼熱減量:3.18%CaO: 55.04% P 2 O 5 : 38.02% CaO / P 2 O 5 molar ratio: 3.66 Loss on burning: 3.18%

【0012】実施例3 実施例2で得た組成物の抗菌試験 実施例2で得たリン酸カルシウム組成分をまず高圧蒸気
減菌器で121℃、15分間減菌した。ニュートリエン
ト寒天平板培地に、500μg/mlまたは5000μ
g/mlとなる様に十分懸濁させ、シャーレの蓋を取
り、3時間放置後37℃で48時間培養することによ
り、空気中の落下細菌に対する抗菌性を評価した。表1
に示した様に、実施例2で得たリン酸カルシウム組成物
は顕著な抗菌力を示し、全く菌の成育は認められなかっ
た。
Example 3 Antibacterial test of the composition obtained in Example 2 The calcium phosphate composition obtained in Example 2 was sterilized in a high-pressure steam sterilizer at 121 ° C. for 15 minutes. 500 μg / ml or 5000 μl on a nutrient agar plate
g / ml, suspended in a petri dish, allowed to stand for 3 hours, and cultured at 37 ° C. for 48 hours to evaluate the antibacterial activity against falling bacteria in the air. Table 1
As shown in the above, the calcium phosphate composition obtained in Example 2 exhibited remarkable antibacterial activity, and no growth of bacteria was observed.

【0013】[0013]

【表1】 [Table 1]

【0014】[0014]

【発明の効果】以上記載したごとく、本発明によれば、
従来、廃棄されていた動物の殻、特に貝殻を用いて、抗
菌作用を有するリン酸カルシウム組成物を安価に提供で
きる。
As described above, according to the present invention,
A conventionally used calcium phosphate composition having an antibacterial effect can be provided at low cost by using animal shells, particularly shells, which have been discarded.

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 動物の殻と、リン酸化合物を反応させる
ことを特徴とする抗菌性を有するリン酸カルシウムの製
造方法。
1. A method for producing antibacterial calcium phosphate, comprising reacting an animal shell with a phosphate compound.
【請求項2】 動物の殻が、貝殻である請求項1に記載
の製造方法。
2. The method according to claim 1, wherein the animal shell is a shell.
【請求項3】 リン酸化合物が、リン酸またはその塩で
ある請求項1に記載の製造方法。
3. The method according to claim 1, wherein the phosphate compound is phosphoric acid or a salt thereof.
【請求項4】 動物の殻を粉砕して2〜15重量%の水
懸濁液とし、これに、反応液中のカルシウム(CaO)
に対してリン酸(P25)換算で0.3〜0.33当量の
リン酸化合物を用いて、50〜150℃で、1〜5時間
反応させることを特徴とする抗菌性を有するリン酸カル
シウムの製造方法。
4. An animal hull is crushed into a 2 to 15% by weight aqueous suspension, to which calcium (CaO) in the reaction solution is added.
A phosphoric acid compound in an amount of 0.3 to 0.33 equivalent in terms of phosphoric acid (P 2 O 5 ), and reacted at 50 to 150 ° C. for 1 to 5 hours. A method for producing calcium phosphate.
JP24335896A 1996-09-13 1996-09-13 Production of calcium phosphate-containing composition having antimicrobial property Withdrawn JPH1087307A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP24335896A JPH1087307A (en) 1996-09-13 1996-09-13 Production of calcium phosphate-containing composition having antimicrobial property

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24335896A JPH1087307A (en) 1996-09-13 1996-09-13 Production of calcium phosphate-containing composition having antimicrobial property

Publications (1)

Publication Number Publication Date
JPH1087307A true JPH1087307A (en) 1998-04-07

Family

ID=17102657

Family Applications (1)

Application Number Title Priority Date Filing Date
JP24335896A Withdrawn JPH1087307A (en) 1996-09-13 1996-09-13 Production of calcium phosphate-containing composition having antimicrobial property

Country Status (1)

Country Link
JP (1) JPH1087307A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000042853A1 (en) * 1999-01-20 2000-07-27 Firma Darinphos Ag Phytosanitary product for crop plants
JP2009120449A (en) * 2007-11-16 2009-06-04 Amino Up Chemical Co Ltd Method for producing bioapatite, and method for separating substance having biological activity

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000042853A1 (en) * 1999-01-20 2000-07-27 Firma Darinphos Ag Phytosanitary product for crop plants
JP2009120449A (en) * 2007-11-16 2009-06-04 Amino Up Chemical Co Ltd Method for producing bioapatite, and method for separating substance having biological activity

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Effective date: 20031202