Magnesium styphnate

Lead styphnate monohydrate is precipitated as the basic salt from a mixture of solutions of magnesium styphnate and lead acetate followed by conversion to the normal form by acidification using dilute nitric acid (97—99). 

Magnesium Chlorate. See under Chlorates Magnesium Styphnate or Magnesium Trinitro-... 

Normal lead styphnate (LS) [Structure (2.10)] was first reported by Von Herze in 1914, although its basic salt, that is, basic LS was prepared by Griess [7] way back in 1874, by the reaction of acidified magnesium styphnate with lead nitrate/acetate in hot aqueous solution. It is precipitated as mono hydrate and consists of reddish-brown rhombic crystals. It is filtered off, washed with water, sieved through a stainless steel sieve and dried. Like other initiatory explosives, it is kept in wet conditions until used. 

It is usually prepared by adding a solution of lead nitrate to one of magnesium styphnate. The latter is an easily soluble and weakly basic salt of trinitroresorcinate. The use of suitable salts and conditions (pH, temperature, rate and sequence in adding the raw materials) is of great importance, since unsuitable salts and condi-... 

The basic salt is formed by the reaction of lead acetate with sodium or magnesium styphnate. The chemical composition of the basic salts formed depends upon the reaction conditions. The basic salt is usually credited with the structural formula (II), corresponding to the dibasic salt ... 

In the method employed at Wolfratshausen [31] a solution of magnesium styphnate was first prepared, adding to 20 kg of magnesium oxide a suspension (partly solution) of 120 kg of trinitroresorcinol in 350 1. of water. The temperature rose... 

From the magnesium styphnate solution so prepared, 86.4 1. of liquid was decanted, leaving the lower layer in which the sediment was collected. This solution was heated to 60°C, while stirring, and 22.71. of 34% solution of lead nitrate, s.g. 1.274 (31°Be) was then poured into it during a period of 20-30 min, while stirring continued and the temperature was maintained at 60°C. When the solutions were mixed, the contents of the reactor were cooled as quickly as possible to 25°C when this temperature has been reached the stirrer was stopped and the precipitated sediment of lead styphnate was allowed to settle. The liquid from above the sediment Was then decanted, and the latter was first washed out of the reactor by a stream of water, and transferred onto a cloth filter, where it was washed again as is the custom with other primary explosives. From the above mentioned amounts of raw material about 8 kg of lead azide was obtained. 

For this production, the starting materials are needed trinitroresorcinol and magnesium oxide to form magnesium styphnate and lead nitrate, all disssolved in distilled water. 

Lead styphnate is commonly prepared by adding a solution of magnesium styphnate 52 at 70° to a well-stirred solution of lead acetate at 70°. A voluminous precipitate of the basic salt separates. The mixture is stirred for 10 or 15 minutes then dilute... 

MAF-40 - X = mixed amine fuels (Hydine) (USA) magazine 44 138 209 299 magnesium carbonate 328 magnesium trinitroresorcinate magnesium styphnate 202 MAN = methylamine nitrate 328 mannitol hexanitrate 209 328 Manoverpulver > porous powder 261 Mantelsprengstoffe = sheathed explosives 284... 

Summary Lead styphnate is easily prepared by reacting a lead nitrate solution with a solution of magnesium styphnate. When the two solutions are mixed, the lead styphnate precipitates. Vacuum filtration is then used for isolating the lead styphnate. Commercial Industrial note Part or parts of this laboratory process may be protected by international, and/or commercial/industrial processes. Before using this process to legally manufacture the mentioned explosive, with intent to sell, consult any protected commercial or industrial processes related to, similar to, or additional to, the process discussed in this... 

Place 132 milliliters of the magnesium styphnate solution (prepared in step 1) into a flask and heat to 80 Celsius while stirring. Then slowly add 114 milliliters of the lead nitrate solution (prepared in step 2) over a period of 40 minutes while maintaining the temperature of the magnesium styphnate solution at 80 Celsius and stirring. After addition of the lead nitrate solution, continue heating the mixture at 80 Celsius for 10 minutes and then remove the heat source, and allow the mixture to cool to room temperature. Afterwards, filter-off the lead styphnate precipitate, and then wash with 1000 milliliters of water. Then vacuum dry or air-dry the product (no heat). 

Magnesium Styphnate or Magnesium Trinitro-resorcinate. See under Styphnic Acid and Styphnates... 

Derivation Prepared by adding a solution of magnesium styphnate (from magnesium oxide and styph-nic acid) to a lead salt solution. 

Allow this diluted solution to stand for 12 hours. This liquid is now a diluted magnesium styphnate solution. 

Place 3.1 u.b.w. of the diluted magnesium styphnate solution into the heat/acid-resistant container. Save the remainder of this solution so that on the next batch you can start right from this step instead of having to manufacture more of the magnesium styphnate solution. 

Place the heaty acid-resistant container of magnesium styphnate solution into the pan of water. 

Slowly heat the magnesium styphnate solution to 55°C (131 °F), then turn off the heat source. 

Very SLOWLY (one drop at a time) stir 1 u.b.w. of lead nitrate solution into the magnesium styphnate solution. Watch the temperature of this new mixture if it begins to approach 60°C (140°F), then stop adding the lead nitrate solution and continue stirring until the temperature drops to 55°C (131 °F). 

TLY stir the mixture of lead nitratc/magnesium styphnate until it cools to 25°C (77°F). WARNING This mixture now contains a primary explosive. 

Lead styphnate (lead salt of 2,4,6-trinitrobenzene-1,3-diol, LS, LTNR, tricinate) was, according to the well-established reference [8], first prepared by Edmund von Herz in 1914 by reaction of magnesium styphnate with lead acetate in presence of nitric acid. However, in reality, preparation of LS was published more than 40 years earlier by Stenhouse [28]. This discrepancy in historical data is probably caused by the fact that Herz patented the substance as a component of a detonator primary charge and was therefore the first one who found some real application [29,30]. The preparation route used by Stenhouse is based on the reaction of lead acetate with an aqueous solution of styphnic acid [28]. 

The usual way of LS preparation is based on adding a solution of a soluble styphnate salt (Na, K, Mg, most conunonly magnesium styphnate, to a well-... 

Magnesium styphnate is prepared by addition of magnesium oxide to trinitror-esorcine water suspension [8, 10, 12, 53-55]. Precipitation of pure LS requires a... 

An unusual dihydrate of LS can be prepared via magnesium styphnate in a similar way to that for normal LS. However, the solutions used for preparation of the dihydrate must be diluted, reaction temperature must be low (about 9 °C), and the reaction mixture must not be stirred. The dihydrate forms within several hours (about 18 h) as red needles [33]. 

Preparation of barium styphnate monohydrate for practical applications is similar to preparation of LS. Magnesium styphnate is used as a starting material which reacts with barium nitrate, chloride, or acetate resulting in precipitation of barium styphnate. A reaction temperature of 60-85 °C is recommended. Product precipitates in form of the trihydrate, which dehydrates to the monohydrate by the slow addition of sufficiently dilute lutric acid [75]. It is difficult to re-crystallize in a suitable form and it is therefore recommended to use a crystal-modifying agent (e.g., carboxymethyl cellulose) [2, 26, 27]. 

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