Process for producing antimicrobial compounds

{
  "publication_number": "US5441717A",
  "country": "US",
  "kind": "A",
  "title": "Process for producing antimicrobial compounds",
  "abstract": "A process for producing an antimicrobial compound represented by the following formula [1]: M.sup.1.sub.a H.sub.b A.sup.1.sub.c M.sup.2.sub.2 (PO.sub.4).sub.3.nH.sub.2 O [1] wherein M 1 is at least one metal ion selected from silver, copper, zinc, tin, mercury, lead, iron, cobalt, nickel, manganese, arsenic, antimony, bismuth, barium, cadmium and chromium, A 1 is at least one ion selected from alkali metal ion and alkaline earth metal ion, M 2 is a tetravalent metal, n is a number which satisfies 0≦n≦6, a and b are positive numbers and c is 0 or a positive number, and a, b and c satisfy ka+b+mc=1 where k is a valence of M 1 and m is a valence of A 1, by supporting at least one metal ion selected from silver, copper, zinc, tin, mercury, lead, iron, cobalt, nickel, manganese, arsenic, antimony, bismuth, barium, cadmium and chromium on a phosphate represented by the following formula [2]: A.sup.2.sub.d M.sup.2.sub.2 (PO.sub.4).sub.3.nH.sub.2 O [2] wherein A 2 is at least one ion selected from alkali metal ion, alkaline earth metal ion and ammonium ion, M 2 and n are as defined above and d is 1/m' where m' is a valence of A 2, characterized in that said phosphate is synthesized by a wet process and furthermore characterized in that a step of supporting hydrogen ion and a step of firing at 500° to 1300° C. are employed.",
  "claims": [
    "1. In a process for producing an antimicrobial compound represented by the following formula [1]: M.sup.1.sub.a H.sub.b A.sup.1.sub.c M.sup.2 (PO.sub.4).sub.3.nH.sub.2 O[1] wherein M 1 is at least one metal ion selected from the group consisting of silver, copper, zinc, tin, mercury, lead, iron, cobalt, nickel, manganese, arsenic, antimony, bismuth, barium, cadmium and chromium, A 1 is at least one ion selected from the group consisting of alkali metal ion and alkaline earth metal ion, M 2 is a tetravalent metal, n is a number which satisfies 0≦n≦6, a and b are positive numbers and c is 0 or a positive number, and a, b and c satisfy ka+b+mc=1 where k is a valence of M 1 and m is a valence of A 1, by adding at least one metal ion selected from the group consisting of silver, copper, zinc, tin, mercury, lead, iron, cobalt, nickel, manganese, arsenic, antimony, bismuth, barium, cadmium and chromium to a phosphate represented by the following formula [2]: A.sup.2.sub.d M.sup.2.sub.2 (PO.sub.4).sub.3.nH.sub.2 O [2] wherein A 2 is at least one ion selected from the group consisting of alkali metal ion, alkaline earth metal ion and ammonium ion, M 2 and n are as defined above and d is 1/m' where m' is a valence of A 2, the improvement comprising synthesizing said phosphate of formula 2 by a wet process, adding hydrogen ion to said phosphate, adding said at least one metal ion M 1 to said phosphate to produce an antimicrobial phosphate and, firing the antimicrobial phosphate at 500° to 1300° C.",
    "2. A process according to claim 1, wherein the phosphate is a crystalline compound having a three-dimensional network structure and represented by the formula [2] in which A 2 is sodium ion and M 2 is zirconium or titanium.",
    "3. A process according to claim 1, wherein the antimicrobial compound is a crystalline compound having a three-dimensional network structure and represented by the formula [1] in which M 1 is silver ion, a is 0.01 to 0.5, A 1 is sodium ion, and M 2 is zirconium or titanium.",
    "4. A process according to claim 1 wherein when the phosphate represented by formula 2 contains ammonium ion, the step of adding hydrogen ion is carried out by thermally decomposing the ammonium ion in the phosphate represented by formula 2 in the firing step to leave hydrogen ion in the compound formed in the firing step.",
    "5. A process according to claim 1 wherein when the phosphate represented by formula 2 does not contain ammonium ion, the step of adding hydrogen ion is carried out by immersing the phosphate represented by formula 2 in an acid solution.",
    "6. In a process for producing an antimicrobial compound represented by the following formula: M.sup.1.sub.a H.sub.b A.sup.1.sub.c M.sup.2.sub.2 (PO.sub.4).sub.3.nH.sub.2 O [1] wherein M 1 is at least one metal ion selected from the group consisting of silver, copper, zinc, tin, mercury, lead, iron, cobalt, nickel, manganese, arsenic, antimony, bismuth, barium, cadmium and chromium, A 1 is at least one ion selected from the group consisting of alkali metal ion and alkaline earth metal ion, M 2 is a tetravalent metal, n is a number which satisfies 0≦n≦6, a and b are positive numbers and c is 0 or a positive number, and a, b, and c satisfy ka+b+mc=1 wherein k is the valence of M 1 and m is the valence of A 1, by adding at least one metal ion selected from the group consisting of sliver, copper, zinc, tin, mercury, lead, iron, cobalt, nickel, manganese, arsenic, antimony, bismuth, barium, cadmium and chromium to a phosphate represented by the following formula: A.sup.2.sub.d M.sup.2.sub.2 (PO.sub.4).sub.3.nH.sub.2 O [2] wherein A 2 is at least one ion selected from the group consisting of alkali metal ion, alkaline earth metal ion and ammonium ion, M 2 and n are as defined above and d is 1/m', where m' is the valence of A 2, the improvement comprising synthesizing the phosphate of formula [2] by a wet process, adding said at least one metal ion M1 and hydrogen ion simultaneously to said phosphate to produce an antimicrobial phosphate, then firing said antimicrobial phosphate at a temperature of from 500° to 1300° C.",
    "7. A process according to claim 6 wherein the phosphate is a crystalline compound having a three-dimensional network structure and represented by the formula [2] in which A 2 is sodium ion and M 2 is zirconium or titanium.",
    "8. A process according to claim 6 wherein the antimicrobial compound is a crystalline compound having a three-dimensional network structure and represented by the formula [1] in which M 1 is silver ion, a is 0.01 to 0.5, A 1 is sodium ion, and M 2 is zirconium or titanium.",
    "9. A process according to claim 6 wherein the phosphate represented by formula 2 contains ammonium ion, the step of adding hydrogen ion is carried out by thermally decomposing the ammonium ion in the phosphate represented by formula 2 in the firing step to leave hydrogen ion in the compound formed in the firing step.",
    "10. A process according to claim 6 wherein when the phosphate represented by formula 2 does not contain ammonium ion, the step of adding hydrogen ion is carried out by immersing the phosphate represented by formula 2 in an acid solution."
  ],
  "cpc": [
    "C01B 25/45",
    "A01N 55/02",
    "A01N 57/10",
    "A01N 59/26"
  ],
  "assignees": [
    "TOA GOSEI CHEM IND"
  ],
  "filing_date": "1993-05-20",
  "publication_date": "1995-08-15",
  "grant_date": "1995-08-15",
  "priority_date": "1992-05-21",
  "application_number": "US-6370493-A",
  "family_id": "26482663",
  "citations": [
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    "GB2224727A",
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    "JPH03275627A",
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    "JPH04142340A",
    "JPS5877805A",
    "JPS6283309A",
    "JPS63265809A",
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  ]
}