CN85100236A - The preparation method of the lead-iron bi-metal complex that one class is novel - Google Patents
The preparation method of the lead-iron bi-metal complex that one class is novel Download PDFInfo
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- CN85100236A CN85100236A CN85100236.6A CN85100236A CN85100236A CN 85100236 A CN85100236 A CN 85100236A CN 85100236 A CN85100236 A CN 85100236A CN 85100236 A CN85100236 A CN 85100236A
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- lead
- iron
- water
- metal complex
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Abstract
The present invention relates to the preparation method of the novel lead-iron bi-metal complex of a class.The chemical formula of its complex compound is (PbIn)
3(Fe (CN)
6)
2, when L is bitooth ligand (as 2,2 '-dipyridyl etc.), n=2; When L is unidentate ligand (as pyridine oxide etc.), n=4.The preparation main points are: drip the methyl alcohol or the water-methanol solution of part ℃ in the mixed aqueous solution of lead salt and metallic iron prussiate in room temperature to 90, promptly generate high yield, highly purified crystalline powder product.This type of complex compound adds in the double-base solid propellant component, and its stability and consistency are good, and the combustion speed of double-base solid propellant is had significant catalytic effect.
Description
The present invention relates to the preparation method of the novel lead-iron bi-metal complex of a class.The chemical formula of prepared lead-iron bi-metal complex is (PbLn)
3(Fe(CN)
6)
2, L represents part in the formula.When L be bitooth ligand (as 2,2 '-dipyridyl, 1,10-phenanthroline or neighbour-diaminobenzene etc.) time, n=2; When L is unidentate ligand (as pyridine oxide etc.), n=4.
Chemical formula is (PbLn)
3(Fe(CN)
6)
2Lead-iron bi-metal complex, be for developing the class novel cpd that well behaved solid propellant combustion rate catalyzer designs.According to reported in literature, the current burningrate catalyst that uses in solid propellant has inorganic metal oxygen-containing compound and organo-transition metal compound two big classes, and the former is representative with ferric oxide, copper chromite, and the latter is representative with ferrocene and derivative thereof.But the metal oxygen-containing compound usually can not satisfy the requirement of higher burning rate, and ferrocene and derivative thereof often run into problems such as distillation and partial crystallization in solid propellant.The lead-iron bi-metal complex of the present invention's preparation adds in the double-base solid propellant component, and not only its stability and consistency are good, and the combustion speed of double-base solid propellant is had significant catalytic effect.
The purpose of this invention is to provide a preparation chemical formula and be (Pb(dipy)
2)
3(Fe(CN)
6)
2The method of the lead-iron bi-metal complex of (dipy represents 2,2 ' one dipyridyl in the formula).Another object of the present invention is to disclose to use some relevant character with this complex compound in solid propellant, and adds catalysis in the double-base solid propellant to as burningrate catalyst
The effect of speed.
Preparation chemical formula provided by the invention is (Pb(dipy)
2)
3(Fe(CN)
6)
2The operation steps of method be: prepare certain density lead salt solution and metallic iron cyanide solution respectively, then under stirring and room temperature to 90 ℃ condition, these two kinds of solution are mixed mutually, in this mixed solution, slowly splash into a certain amount of 2 again, 2 '-water-methanol, water-ethanol, methyl alcohol or the ethanolic soln of dipyridyl, promptly separate out throw out.After continuing to stir certain hour, filtering precipitate.Water, ethanol, ether be washing precipitate respectively, drains, and promptly gets solid product.Solid product is identified through ultimate analysis and infrared spectra, confirms that its chemical formula is (Pb(dipy)
2)
3(Fe(CN)
6)
2
Lead salt related in operation steps can be used lead nitrate, lead acetate, lead chlorate or lead perchlorate etc., preferably can use the Tripotassium iron hexacyanide, the Trisodium hexacyanoferrate, iron lithium cyanide or ammonium-cu hexacyanoferrate with lead nitrate metallic iron prussiate, preferably uses the Tripotassium iron hexacyanide; The solvent of lead salt and metallic iron prussiate can water, water-methanol or water-ethanol, preferably water.2,2 '-the used solvent of dipyridyl preferably methanol-water or methyl alcohol.
Chemical formula with method preparation provided by the invention is (Pb(dipy)
2)
3(Fe(CN)
6)
2Lead-iron bi-metal complex be flaxen finely powdered crystallisate.Complex compound is stable in air at room temperature, and does not have obvious weightlessness and phenomenon of deflation in two days through 70 ℃ of bakings.Differential thermal analysis shows that the temperature that complex compound begins to occur exothermic decomposition is 172 ℃.Complex compound is water insoluble, pure, ether, benzene, haloalkane equal solvent, is dissolved in methyl-sulphoxide.
Chemical formula with method preparation provided by the invention is (Pb(dipy)
2)
3(Fe(CN)
6)
2Lead-iron bi-metal complex, good to the consistency of each component of the double-base solid propellant of nitro-cotton one nitroglycerine system.In the double-base solid propellant component, add the solid propellant that the 0.01-1% complex compound makes, in 20 ℃ and 100 kilograms per centimeter
2Recording its combustionvelocity under the pressure is～35 mm/second.
The preparation chemical formula is (Pb(dipy)
2)
3(Fe(CN)
6)
2The concrete operations step of method of lead-iron bi-metal complex, available the following example statement.
Embodiment 1
With 5.30 gram (0.016 mole) Pb(NO
3)
2Under room temperature, be dissolved in the 30ml water, get solution I; In addition with 3.52 gram (0.0107 mole) K
3(Fe(CH)
6) under room temperature, be dissolved in the 30ml water, get the solution II; Under agitation I is mixed mutually with II then, and be dissolved in the gram of 5.00 in 40ml methyl alcohol one aqueous solution (volumetric ratio of methyl alcohol and water is 1: 1) (0.032 mole) 2,2 ' one dipyridyl to slow dropping of this mixing solutions in room temperature with under stirring.Promptly separate out solid sediment in the dropping process.Dropping is finished, and continues to stir this reaction mixture 30 minutes, filters solid sediment, difference water, ethanol, each secondary of ether filter wash cake, and each washing lotion consumption is 10ml.Get solid product 9.50 grams (0.0048 mole) after draining, productive rate is that 90.6%(is in lead).Ultimate analysis (%): Pb31.36(actual measurement), 31.37(calculates); The Fe5.58(actual measurement), 5.64(calculates).The ir data that records with the KBr compressing tablet (centimetre
-1): 3050(W), 2100(W), 2050(S), 1593(m), 1578(sh, m), 1560(w), 1492(w), 1475(w), 1454(w), 1440(m), 1416(m), 1385(s), 1356(m), 1338(w), 1318(w), 1245(w), 1215(w), 1174(w), 1160(w), 1090(w), 1062(w), 1041(w), 1013(m), 908(w), 835(w), 814(w), 788(s), 761(m), 736(w), 650(w), 630(w), 592(w), 458(w), 410(w).(annotate: S-is strong, among the m-, and a little less than the w-, the sh-shoulder).
Embodiment 2
With 20.2 gram (0.061 mole) Pb(NO
3)
2Under room temperature, be dissolved in the 100ml water, get solution I; In addition with 13.4 gram (0.041 mole) K
3(Fe(CN)
6) be dissolved in the 100ml water, get the solution II; Under agitation I is mixed mutually with II then, and be dissolved in the gram of 19.0 in the 100ml methyl alcohol (0.122 mole) 2,2 ' one dipyridyl to slow dropping of this mixing solutions in room temperature with under stirring.Promptly separate out solid sediment in the dropping process.Drip and finish, continue to stir this reaction mixture 30 minutes, filter solid sediment, difference water, ethanol, each secondary of ether filter wash cake, each washing lotion consumption is 30ml, gets solid product 37.6 grams (0.019 mole) after draining, and productive rate is that 95.0%(is in lead).Ultimate analysis (%): Pb31.03(actual measurement), 31.37(calculates); The Fe5.38(actual measurement), 5.64(calculates).Ir data is with embodiment 1.
Claims (5)
1, a kind of short-cut method for preparing lead-iron bi-metal complex is characterized in that adding ligand solution in the solution that contains lead salt and metallic iron prussiate, reacts under appropriate condition.
2,, it is characterized in that the chemical formula of the lead-iron bi-metal complex for preparing is (PbLn), (Fe(CN) according to the said method of claim 1
6)
2, L represents part in the formula, when L is bitooth ligand, and n=2, when L is unidentate ligand, n=4.
3, according to the said method of claim 1, it is characterized in that lead salt is lead nitrate, lead acetate, lead chlorate or lead perchlorate, the metallic iron prussiate is the Tripotassium iron hexacyanide, the Trisodium hexacyanoferrate, iron lithium cyanide or ammonium-cu hexacyanoferrate, part is 2,2 '-dipyridyl, 1, (unidentate ligands) such as 10-phenanthroline, ortho-diaminobenzene (above is bitooth ligand) or pyridine oxides.
4, according to the said method of claim 1, the solvent that it is characterized in that lead salt and metallic iron prussiate is water, water-methanol or water-ethanol, and the solvent of part is water-methanol, water-ethanol, methyl alcohol or ethanol.
5,, it is characterized in that being reflected at room temperature to 90 and ℃ carry out according to the said method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100236.6A CN1004810B (en) | 1985-04-01 | 1985-04-01 | Method for preparing bimetallic complex of pb and fe |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85100236.6A CN1004810B (en) | 1985-04-01 | 1985-04-01 | Method for preparing bimetallic complex of pb and fe |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85100236A true CN85100236A (en) | 1986-07-16 |
| CN1004810B CN1004810B (en) | 1989-07-19 |
Family
ID=4790996
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85100236.6A Expired CN1004810B (en) | 1985-04-01 | 1985-04-01 | Method for preparing bimetallic complex of pb and fe |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1004810B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1886536B (en) * | 2003-11-24 | 2010-12-08 | 巴斯福股份公司 | Method for electrochemical production of a crystalline porous metal organic skeleton material |
| CN101531587B (en) * | 2009-03-04 | 2012-06-13 | 西安近代化学研究所 | Zirconium lead tartrate double metal salt, preparation method and application thereof |
-
1985
- 1985-04-01 CN CN85100236.6A patent/CN1004810B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1886536B (en) * | 2003-11-24 | 2010-12-08 | 巴斯福股份公司 | Method for electrochemical production of a crystalline porous metal organic skeleton material |
| CN101531587B (en) * | 2009-03-04 | 2012-06-13 | 西安近代化学研究所 | Zirconium lead tartrate double metal salt, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1004810B (en) | 1989-07-19 |
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