US2418753A - Explosive purification - Google Patents
Explosive purification Download PDFInfo
- Publication number
- US2418753A US2418753A US556909A US55690944A US2418753A US 2418753 A US2418753 A US 2418753A US 556909 A US556909 A US 556909A US 55690944 A US55690944 A US 55690944A US 2418753 A US2418753 A US 2418753A
- Authority
- US
- United States
- Prior art keywords
- cyclonite
- perborate
- bath
- purification
- poaching
- 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
- 238000000746 purification Methods 0.000 title description 6
- 239000002360 explosive Substances 0.000 title description 4
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 29
- 238000000034 method Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 7
- 229910052783 alkali metal Inorganic materials 0.000 description 6
- 150000001340 alkali metals Chemical class 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 229960001922 sodium perborate Drugs 0.000 description 4
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0091—Elimination of undesirable or temporary components of an intermediate or finished product, e.g. making porous or low density products, purifying, stabilising, drying; Deactivating; Reclaiming
Definitions
- This invention relates to explosives and their production and more particularly to their refinement.
- This invention has utility when employed in the manufacture of purified cyclotrimethylenetrinitramine, which is commonly known as cyclonite and will be referred to herein as such as well as in the appended claims.
- a primary object of the present invention is to produce purified cyclonite from impure or crude cyclonite by an inexpensive process requiring the use of comparatively low cost materials.
- Another object is to produce a cyclonite with a lower acid content than the normal or crude cyclonite formed by the usual reactions.
- Still another object is to produce a cyclonite with a higher melting point and having improved stability.
- Cyclonite can be prepared in several ways, as, for example, the nitration of hexamethylenetetramine (CeI-I12N4) which is an intermediate formed by the evaporation of an aqueous solution of formaldehyde and ammonia.
- CeI-I12N4 hexamethylenetetramine
- the production of cyclonite and its properties are described in Chemistry of Powder and Explosives by Davis, vol. II, page 396 (published 1943 by John Wiley & Sons).
- Alkali metal and alkaline earth metal perborates are preferred in the treatment or poach, since these appear to be most effective in purification and improving the stability.
- any suitable alkaline perborate may be employed to advantage, perborates of such metals as sodium or potassium, are preferred.
- the concentration of perborate in the poaching bath may be varied appreciably without losing the beneficial action and from the standpoint of economy, the bath preferably contains only an amount sufficient to effect the desired purification and stabilization.
- a bath containing sodium perborate in amounts in the neighborhood of 0.3% to 1% solution is ordinarily entirely satisfactory.
- the treating bath is heated to above atmospheric temperature, but at a temperature less than boiling and preferably at 60 to 80 C.
- the time of treatment may be varied from about two hours to as long .as 12 hours, or longer, depending on the char- 2 acter of the material being amount of purification desired.
- the crude cyclonite having a melting point of about 195 C. to 200 C. is taken directly from the nitration reaction and without previous purification other than water washing.
- the cyclonite is heated under a reflux condenser in an aqueous solution containing 1% sodium perborate for about six hours at a temperature in the range of 73 C. to 76 C. and preferably not over about 80 C. with the pH of the bath being maintained at about 7.5 to 8.0.
- the constituents of the bath are subjected to vigorous agitation to suspend the cyclonite and provide for uniformity of treatment.
- the cyclonite is separated from the bath in any suitable manner, for instance by filtering, and the cyclonite is thoroughly water washed to remove any residual constituents of the bath and then dried.
- Purified cyclonite in a high yield of 97% or more is thus obtained with a low acidity, good stability, melting point and other characteristics satisfactorily meeting the specifications ordinarily required for such material.
- a product may be obtained having a 10W acidity, a melting point of about 20l.2 C., and a stability of about 3.2, the stability being given in cubic centimeters of gas evolved by five grams of cyclonite held at C., in vacuo, for twenty-four hours.
- reagents may be added to the perborate solution.
- favorable results were obtained by poaching 80 grams of cyclonite in a solution of 350 grams of water, 1 gram of sodium perborate, 2500 grams of ammonia and 16 grams of ethyl methyl ketone.
- Treating oyclonite by subjecting the same to an alkali-metal perborate bath of a character whereby the stability of the cyclonite is improved, washing the treated cyclonite and drying the same.
- the method of purifying cyclonite comprising heating said cyclonite in an aqueous a1- kaline perborate solution.
- the method of purifying cyolonite comprising heating said cycionite in an aqueous alkaline inorganic perborate solution.
- the method of purifying oyclonite comprising suspending said oyclonite in an aqueous alkali metal perborate solution at elevated temperature.
- the method of purifyin cyclonite comprising suspending said cyolonite in an aqueous alkaline earth metal perborate solution at elevated temperature.
Description
Patented Apr. 8, 1947 EXPLOSIVE PURIFICATION Jerome G. Burtle, Alton, Ill;-, assignor to Olin Industries, Inc., a corporation of Delaware No Drawing. Application October 2, 1944,
Serial No. 555,909
14 Glaims.
This invention relates to explosives and their production and more particularly to their refinement.
This invention has utility when employed in the manufacture of purified cyclotrimethylenetrinitramine, which is commonly known as cyclonite and will be referred to herein as such as well as in the appended claims.
A primary object of the present invention is to produce purified cyclonite from impure or crude cyclonite by an inexpensive process requiring the use of comparatively low cost materials.
Another object is to produce a cyclonite with a lower acid content than the normal or crude cyclonite formed by the usual reactions.
Still another object is to produce a cyclonite with a higher melting point and having improved stability.
Other objects will be apparent in the following specification and claims.
Cyclonite can be prepared in several ways, as, for example, the nitration of hexamethylenetetramine (CeI-I12N4) which is an intermediate formed by the evaporation of an aqueous solution of formaldehyde and ammonia. The production of cyclonite and its properties are described in Chemistry of Powder and Explosives by Davis, vol. II, page 396 (published 1943 by John Wiley & Sons).
It has been discovered that the physical properties of cyclonite are vastly improved by the invention disclosed herein which comprises subjecting crude or unstable cyclonite to a treatment in an aqueous solution of a perborate.
Alkali metal and alkaline earth metal perborates are preferred in the treatment or poach, since these appear to be most effective in purification and improving the stability. For instance, although any suitable alkaline perborate may be employed to advantage, perborates of such metals as sodium or potassium, are preferred. The concentration of perborate in the poaching bath may be varied appreciably without losing the beneficial action and from the standpoint of economy, the bath preferably contains only an amount sufficient to effect the desired purification and stabilization. For instance, a bath containing sodium perborate in amounts in the neighborhood of 0.3% to 1% solution is ordinarily entirely satisfactory. The treating bath is heated to above atmospheric temperature, but at a temperature less than boiling and preferably at 60 to 80 C. The time of treatment may be varied from about two hours to as long .as 12 hours, or longer, depending on the char- 2 acter of the material being amount of purification desired.
By way of example, following is a preferred embodiment of the invention, in which the crude cyclonite having a melting point of about 195 C. to 200 C. is taken directly from the nitration reaction and without previous purification other than water washing. The cyclonite is heated under a reflux condenser in an aqueous solution containing 1% sodium perborate for about six hours at a temperature in the range of 73 C. to 76 C. and preferably not over about 80 C. with the pH of the bath being maintained at about 7.5 to 8.0. During this poaching treatment, the constituents of the bath are subjected to vigorous agitation to suspend the cyclonite and provide for uniformity of treatment. After the six hour period, the cyclonite is separated from the bath in any suitable manner, for instance by filtering, and the cyclonite is thoroughly water washed to remove any residual constituents of the bath and then dried.
Purified cyclonite in a high yield of 97% or more is thus obtained with a low acidity, good stability, melting point and other characteristics satisfactorily meeting the specifications ordinarily required for such material. For instance a product may be obtained having a 10W acidity, a melting point of about 20l.2 C., and a stability of about 3.2, the stability being given in cubic centimeters of gas evolved by five grams of cyclonite held at C., in vacuo, for twenty-four hours.
If desired other reagents may be added to the perborate solution. For instance, in one embodiment favorable results were obtained by poaching 80 grams of cyclonite in a solution of 350 grams of water, 1 gram of sodium perborate, 2500 grams of ammonia and 16 grams of ethyl methyl ketone.
It should be understood that the concentrations, times, temperatures, and other conditions set forth in the above detail embodiments are only by way of illustration and that variations therefrom may be made without departin from the spirit and scope of the invention as define in the appended claims.
Having thus described the invention, what is claimed and desired to secure by Letters Patent 1. The method of purifying cyclonite by subjecting crude cyclonite to a bath containing a perborate.
2. The method of purifying cyclonite by poaching in a bath containing an alkaline perborate.
treated and the 3. The method of purifying cyclomte by poaching in an aqueous bath of an alkali-metal perborate.
4. The method of claim 3 where the perborate content is in the neighborhood 0.3% to 1%- 5. The method of claim 3 where the bath has a temperature in the range of approximately 60 to 80 C. I
6. The method of claim 3 'where the length of poaching time is in the range of about two to twelve hours.
7. The method of treating crude oyclonite including poaching in a bath of sodium perborate.
8. The method of treating crude cyclonite by subjecting the same to a poaching in an aqueous bath of approximately 0.3% to 1% of an alkali metal perborate content for about two to twelve hours at a temperature in the: range of to 80 C.
9. Treating cyclonite by poaching in a bath containing an alkali-metal perborate, washing the treated product and drying the same.
10. Treating oyclonite by subjecting the same to an alkali-metal perborate bath of a character whereby the stability of the cyclonite is improved, washing the treated cyclonite and drying the same.
11. The method of purifying cyclonite comprising heating said cyclonite in an aqueous a1- kaline perborate solution.
12. The method of purifying cyolonite comprising heating said cycionite in an aqueous alkaline inorganic perborate solution.
about 60 13. The method of purifying oyclonite comprising suspending said oyclonite in an aqueous alkali metal perborate solution at elevated temperature.
14. The method of purifyin cyclonite comprising suspending said cyolonite in an aqueous alkaline earth metal perborate solution at elevated temperature.
JEROME G. BURTLE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US556909A US2418753A (en) | 1944-10-02 | 1944-10-02 | Explosive purification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US556909A US2418753A (en) | 1944-10-02 | 1944-10-02 | Explosive purification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2418753A true US2418753A (en) | 1947-04-08 |
Family
ID=24223319
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US556909A Expired - Lifetime US2418753A (en) | 1944-10-02 | 1944-10-02 | Explosive purification |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2418753A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2525252A (en) * | 1948-02-25 | 1950-10-10 | Willson Francis George | Cyclo-trimethylenetrinitramine |
| US2535350A (en) * | 1950-12-26 | Eecoveky of cyclotrimethylene |
-
1944
- 1944-10-02 US US556909A patent/US2418753A/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| None * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2535350A (en) * | 1950-12-26 | Eecoveky of cyclotrimethylene | ||
| US2525252A (en) * | 1948-02-25 | 1950-10-10 | Willson Francis George | Cyclo-trimethylenetrinitramine |
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