US2230629A - Manufacture of semipyrophoric compounds - Google Patents
Manufacture of semipyrophoric compounds Download PDFInfo
- Publication number
- US2230629A US2230629A US158594A US15859437A US2230629A US 2230629 A US2230629 A US 2230629A US 158594 A US158594 A US 158594A US 15859437 A US15859437 A US 15859437A US 2230629 A US2230629 A US 2230629A
- Authority
- US
- United States
- Prior art keywords
- semipyrophoric
- compounds
- pyrophoric
- manufacture
- condition
- 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.)
- Expired - Lifetime
Links
- 150000001875 compounds Chemical class 0.000 title description 11
- 238000004519 manufacturing process Methods 0.000 title description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 23
- 239000000126 substance Substances 0.000 description 16
- 150000002736 metal compounds Chemical class 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 150000002739 metals Chemical class 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 229940062993 ferrous oxalate Drugs 0.000 description 4
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
- C06C15/00—Pyrophoric compositions; Flints
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06F—MATCHES; MANUFACTURE OF MATCHES
- C06F3/00—Chemical features in the manufacture of matches
Definitions
- This invention relates to a process for the manufacture of semipyrophoric compounds and -to compositions containing these compounds.
- the semipyrophoric condition of metals is well- 5 known as are also processes for obtaining metals in this condition.
- the present invention is concerned essentially with the production of metal compounds, for example lower oxides, in a semipyrophoric condition. It is possible by means of the invention to obtain the compounds in any intermediate stage, 'as desired, between the ordinary condition and the pyrophoric condition, all of which intermediate conditions are comprised under the term semipyrophoric. It is also possible to produce metal compounds which ignite at a desired temperature.
- the semipyrophoric condition of metal compounds may be defined as being similar to the semipyrophoric condition of metals, that is to say it includes those forms of the compounds of which the ignition temperature lies between that of the normal substance and that of the pyrophoric substance.
- This temperature difierence may be from about 50 to 300 C.
- the causes of the pyrophoric condition are not exactly known and can not be ascertained from the literature on the subject. .
- the causes of the semipyrophoric condition of a metals and'metal compounds cannot be exactly explained, although it may be assumed that the semipyrophoric condition dependsin part upon the size of the particles of, the substance in question and is also a consequence of adsorption phenomena .which result in chemical changes taking place at least at the surface.
- the semipyrophoric compounds which are manufactured in accordance with the invention are, for example, semipyrophoric metallic sub-oxidies, such as FeO.
- the semipyrophoric compounds can be manufactured, in accordance with the invention, by
- the decomposition for example by means of hea of metal compounds, for example by decomposi- 'tion'of ferrous oxalate into ferrous oxide. Since these metal compounds can also be obtained in a pyrophoric form as well as in a semipyrophoric form, the conditions under which the reaction is carried out in accordance with the invention must be such, as regards pressure, temperature etc., that neither the normal nor the pyrophoric form is produced. In this case, according to the conditions of the reaction a part of the starting material can be simultaneously obtained in the 5 form of semipyrophoric metal, so that mixtures of semipyrophoric metal compounds" in a low stage of oxidation together with semipyrophoric metals can be produced.
- the low heat tone when semipyrophorlc metal compounds are burned as compared with semipyrophoric metals'isa decided advantage, since this property can be em- 20 ployed for retarding the combustion process and for regulating the heat produced.
- the two stages can also be conducted in such a way that a continuous process results.
- the conversion from the pyrophoric to the semipyrophoric state is eflected either by treating the pyrophoric substance with a gas free from oxygen at an elevated temperature and maintaining such conditions during the reaction that the substance loses the p'yrophoric condition but does not attain the normal condition, or by storing the pyrophoric body for a considerable time in an atmosphere which is free from oxygen but to which very diluted oxygen has slow access.
- a further possibility is to introduce the pyrophoric substance in a hot or cold state into a suitable liquid, for example methyl alcohol, acetone, esters, ketones, aldehydes, ether, etc., which is then evaporated or the suspension itself is subjected to further treatment.
- Example 1 For the manufacture of a'semipyrophoric ferrous oxide which-consists mainly of FeO, 1.50 grams of ferrous oxalate are heated at a temperature of 390-410 C. in a glass tube -at the other end, The decomposition of the ferrous oxalate which can be recognised by the change of color from light yellow to greenish black and then to deep blue-black, is complete afterabout five minutes. The heating: is then continued for about 5 to 6 minutes andthe material is allowed to cool down to room temperature. About 0.61 gram of senilpyrophoric ferrous oxide are obtained.
- the gases formed during the reaction consist mainly of steam, which originates from the water of crystallisation and ,carbon monoxide.
- Example 3 Into a vessel which contains pyrophoric iron oxide in an atmosphere of hydrogen, air is allowed to enter slowly during'the course of several; days untilthe hydrogen has been driven out. The residual powder is semipyro phoric. v
- Example 4 A current of nitrogen is allowed to flow for some minutes over freshly prepared pyrophoric iron oxide while it is cooling down, that is to say at a temperature of about 100 to 300 C. when room temperature is reached the 9,230,629 semipyrophoric final product directly from the pyrophoric-iron oxide has become semipyrophoric.
- Example 5 Freshly prepared pyrophoric iron is allowed to fall while still hot, ,into acetone, the access of air being excluded. The supernatant acetone is decanted and the remainder of the acetone is allowed to evaporate in the air. Semipyrophoric iron remains behind.
- Example 6 Freshly prepared pyrophoric iron oxide is allowed to fall in a cold condition into acetone, access of air being excluded; the supernatant acetone is decanted and the remainder of the acetone is allowed to evaporate in the air.
- A. Semipyrophoric metal compounds are used for the manufacture of combustible bodies which contain substances which are easily vaporised.
- the following combustible composition can be used for the development of iodine vapor.
- 10 parts of semipyrophoric ferrous oxide are mixed with 1 part of adsorption charcoal in which about 10% of elemental iodine has been adsorbed.
- the powdery mixture is stirred into a paste with a suitable binding agent, for example collodion solution, and may or may not be applied to a suitable carrier.
- the dry mass can be ignited by means of a flame.
- compound with corresponding development of Oxidation of the metalheat then begins at the place at which it was ignited.
- the reaction proceeds slowly from the point at which ignition was effected and-spreads through the mass, while at the same time, owing to the rise in temperature, the adsorbed iodine is driven 05 from the charcoal.
- 1..A' safety igniting composition which comprises a mixture of a binding agent, a. frictionproducing agent and a semipyrophoric iron oxide.
- a safety igniting composition which'comprises a mixture of a binding agent, a frictionproducing agent,' and semipyrophoricflerroua oxide.
- A' safety igniting composition which com prises a binding agent, a friction producing agent,
- semipyrophoric iron and a semipyrophoric iron consisting of a mixture of a semipyrophoric iron oxide and semipyrophoric iron.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
Description
Patented Feb. 4, 1941 MANUFACTURE OF SEMIPYROPHORIC COMPOUNDS Alfred Schmid, Berlin-Dahlem, Germany, asignor to Oswald Fidel Wyss, Berlin, Germany No Drawing. Application August 11, 1937, Serial No. 158,594. In Germany August 25, 1936 Claims.
This invention relates to a process for the manufacture of semipyrophoric compounds and -to compositions containing these compounds.
The semipyrophoric condition of metals is well- 5 known as are also processes for obtaining metals in this condition. As distinguished therefrom, the present invention is concerned essentially with the production of metal compounds, for example lower oxides, in a semipyrophoric condition. It is possible by means of the invention to obtain the compounds in any intermediate stage, 'as desired, between the ordinary condition and the pyrophoric condition, all of which intermediate conditions are comprised under the term semipyrophoric. It is also possible to produce metal compounds which ignite at a desired temperature.
The semipyrophoric condition of metal compounds may be defined as being similar to the semipyrophoric condition of metals, that is to say it includes those forms of the compounds of which the ignition temperature lies between that of the normal substance and that of the pyrophoric substance. This temperature difierence may be from about 50 to 300 C.
The causes of the pyrophoric condition are not exactly known and can not be ascertained from the literature on the subject. .Similarly the causes of the semipyrophoric condition of a metals and'metal compounds cannot be exactly explained, although it may be assumed that the semipyrophoric condition dependsin part upon the size of the particles of, the substance in question and is also a consequence of adsorption phenomena .which result in chemical changes taking place at least at the surface. The semipyrophoric compounds which are manufactured in accordance with the invention are, for example, semipyrophoric metallic sub-oxidies, such as FeO. In view of what is known about semipyrophoric metals it is surprising that it is also 1 possible to manufacture semipyrophoric metal compounds and that these may'even be oxides. In view of the low heat tone of oxides such a i ready oxidation would not be expected at low temperatures.
The semipyrophoric compounds can be manufactured, in accordance with the invention, by
the decomposition, for example by means of hea of metal compounds, for example by decomposi- 'tion'of ferrous oxalate into ferrous oxide. Since these metal compounds can also be obtained in a pyrophoric form as well as in a semipyrophoric form, the conditions under which the reaction is carried out in accordance with the invention must be such, as regards pressure, temperature etc., that neither the normal nor the pyrophoric form is produced. In this case, according to the conditions of the reaction a part of the starting material can be simultaneously obtained in the 5 form of semipyrophoric metal, so that mixtures of semipyrophoric metal compounds" in a low stage of oxidation together with semipyrophoric metals can be produced. .The properties of both substances are however so similar that separa- 10 tion is only possible with difficulty. This resemblance between the properties of semipyrophoric metals and those of semipyrophoric metal compounds enables the latter metal compounds to be used for the same purposes as the semipyrol6 phoric metals and also for other-purposes. For
, many purposes however, the low heat tone when semipyrophorlc metal compounds are burned as compared with semipyrophoric metals'isa decided advantage, since this property can be em- 20 ployed for retarding the combustion process and for regulating the heat produced.
In the investigation of semipyrophoric substances and in the development of processes for their manufacture considerable difliculties were as encountered in connection with the apparatus to be used. The reproduction of the same substance v with exactly the same properties depends not only on the canditions of the reaction, such as pressure, temperature, and time, under which neither the pyrophoric nor the normal form is produced, being kept constant, but also on the quantities which are being worked with and on the form of the apparatus as a whole. A numberof contradictory statements which are to be 35 found in the literature rega;dlng the semipyrophoric state can be entirely explained as being due to the use of diflerenttypes of apparatus to which insuflicient attention was paid by the authors of the statements in question. 40
The great advantage of using semipyrophoric compounds as initial igniting substances, or as combustible materials instead of the known substances such as carbon, sulphur, phosphorus which have previously been used for similar purposes is that the semipyrophoric compounds burn without giving off noxious, poisonous or nauseating gases. In the various processes by which metal compounds are decomposed, it may be assumed, in general, that the pyrophoric condition has to be passed through before the semipyrophoric condition is arrived at. Owing to this it is possible to develop a number of variants of the same process. One process in accordance with the invention consists in obtaining the a metal compound to be decomposed by maintaining definite conditions during the course of the reaction without interrupting the process of manufacture. Another: possible process is to isolate the pyrophoric body and to subject it sep-' arately to further treatment. In this case the reaction proceeds in two stages, namely:
1. The decomposition of the metal compound to form'a pyrophoric substance, and I v 2. The conversion of the pyrophoric substance into the semipyrophoric condition.
The two stages can also be conducted in such a way that a continuous process results.
The conversion from the pyrophoric to the semipyrophoric state is eflected either by treating the pyrophoric substance with a gas free from oxygen at an elevated temperature and maintaining such conditions during the reaction that the substance loses the p'yrophoric condition but does not attain the normal condition, or by storing the pyrophoric body for a considerable time in an atmosphere which is free from oxygen but to which very diluted oxygen has slow access. A further possibility is to introduce the pyrophoric substance in a hot or cold state into a suitable liquid, for example methyl alcohol, acetone, esters, ketones, aldehydes, ether, etc., which is then evaporated or the suspension itself is subjected to further treatment.
In accordance also with the invention these various possibilities can also be employed for the manufacture of semipyrophoric metals.
The invention will now be explained with the aid of the following examples which explain both the process of manufacture and the manner in which the semipyroph'oric material can be used.
Example 1.For the manufacture of a'semipyrophoric ferrous oxide which-consists mainly of FeO, 1.50 grams of ferrous oxalate are heated at a temperature of 390-410 C. in a glass tube -at the other end, The decomposition of the ferrous oxalate which can be recognised by the change of color from light yellow to greenish black and then to deep blue-black, is complete afterabout five minutes. The heating: is then continued for about 5 to 6 minutes andthe material is allowed to cool down to room temperature. About 0.61 gram of senilpyrophoric ferrous oxide are obtained.
The gases formed during the reaction consist mainly of steam, which originates from the water of crystallisation and ,carbon monoxide.
Example 2.-Pyrophoric iron manufactured by thermal'decomposition. of ferrous oxalate becomes semipyrophoric after being stored for 58V? eral days in an atmosphere of nitrogen.
Example 3.Into a vessel which contains pyrophoric iron oxide in an atmosphere of hydrogen, air is allowed to enter slowly during'the course of several; days untilthe hydrogen has been driven out. The residual powder is semipyro phoric. v
Example 4.A current of nitrogen is allowed to flow for some minutes over freshly prepared pyrophoric iron oxide while it is cooling down, that is to say at a temperature of about 100 to 300 C. when room temperature is reached the 9,230,629 semipyrophoric final product directly from the pyrophoric-iron oxide has become semipyrophoric.
Example 5.Freshly prepared pyrophoric iron is allowed to fall while still hot, ,into acetone, the access of air being excluded. The supernatant acetone is decanted and the remainder of the acetone is allowed to evaporate in the air. Semipyrophoric iron remains behind.
Example 6.--Freshly prepared pyrophoric iron oxide is allowed to fall in a cold condition into acetone, access of air being excluded; the supernatant acetone is decanted and the remainder of the acetone is allowed to evaporate in the air.
Examples of the applications to which. the semipyrophoric substances can bev put the carrier. I
B. Semipyrophoric metal compounds are used for the manufacture of combustible bodies which contain substances which are easily vaporised. Thus, the following combustible composition can be used for the development of iodine vapor. 10 parts of semipyrophoric ferrous oxide are mixed with 1 part of adsorption charcoal in which about 10% of elemental iodine has been adsorbed. The powdery mixture is stirred into a paste with a suitable binding agent, for example collodion solution, and may or may not be applied to a suitable carrier. The dry mass can be ignited by means of a flame. compound with corresponding development of Oxidation of the metalheat then begins at the place at which it was ignited. The reaction proceeds slowly from the point at which ignition was effected and-spreads through the mass, while at the same time, owing to the rise in temperature, the adsorbed iodine is driven 05 from the charcoal.
These examples illustrate only two of a large number of possibilities, and the invention is not restricted to these two examples.
I claim:
1..A' safety igniting composition which comprises a mixture of a binding agent, a. frictionproducing agent and a semipyrophoric iron oxide.
2. A safety igniting composition which'comprises a mixture of a binding agent, a frictionproducing agent,' and semipyrophoricflerroua oxide.
3. A' safety igniting composition which com prises a binding agent, a friction producing agent,
semipyrophoric iron and a semipyrophoric iron consisting of a mixture of a semipyrophoric iron oxide and semipyrophoric iron.
ALFRED SCHMID.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2230629X | 1936-08-25 |
Publications (1)
Publication Number | Publication Date |
---|---|
US2230629A true US2230629A (en) | 1941-02-04 |
Family
ID=7991376
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US158594A Expired - Lifetime US2230629A (en) | 1936-08-25 | 1937-08-11 | Manufacture of semipyrophoric compounds |
Country Status (1)
Country | Link |
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US (1) | US2230629A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007057676A2 (en) * | 2005-11-18 | 2007-05-24 | Pains-Wessex Limited | Decoy countermeasures |
-
1937
- 1937-08-11 US US158594A patent/US2230629A/en not_active Expired - Lifetime
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007057676A2 (en) * | 2005-11-18 | 2007-05-24 | Pains-Wessex Limited | Decoy countermeasures |
WO2007057676A3 (en) * | 2005-11-18 | 2007-11-15 | Pains Wessex Ltd | Decoy countermeasures |
US20090050245A1 (en) * | 2005-11-18 | 2009-02-26 | Chemring Countermeasures Limited | Decoy countermeasures |
US9067844B2 (en) | 2005-11-18 | 2015-06-30 | Chemring Countermeasures Limited | Decoy countermeasures |
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