DE2335251B2 - PENTAERYTHRITRANITRATE AND METHOD FOR ITS MANUFACTURING AND ITS USE FOR MANUFACTURING ROPE ROPES, FREE OF BINDERS - Google Patents

Description

The present invention relates to a composition: it is free-flowing, but does not bake under

drive to the production of a pentaerythritol tetranitride- the action of pressure or when together-

tes that are both free-flowing and also after being pressed together.

Compaction firmly adhered to one another and pure trickle. Surprisingly, it has been shown that one after

ability largely loses. 40 pen manufactured by the method according to the invention

Pentaerythritol granitrate is pourable in increasingly stronger taerythritol granitrate and is also free-flowing

Measures used in such detonating cords, whose in a compaction, as they are in the manufacture of

Explosives fill weight is well over 10 g / m. This detonating cord is common so stuck together that

Detonating cords have a detonating cord made with them in the same meter range.

Fill weights which can be up to 100 g, in some cases even 45, without the pentaerythritol granitrate coming off

can even be up to 150 g. Simultaneously with the filling the detonating cord trickles.

men ^ e, however, also takes the diameter of the penta-

Detonating cords too, so that the said reinforced erythrittetranitrat differs in its shape

Spiengschnürc explosive core diameter is not at all of the previously known

zen, which can be up to 10.9 mm, during 50 drive produced pentaerythritol tetranitrate. Even

the standard detonating cords with a filling weight his analysis resulted in values that - due to the

of approx. 12.5 g / m a diameter of the explosive results of a thin layer chromatography - itself

have a core of about 3.6 mm. only slightly different from what has been known so far

In the case of these reinforced detonating cords, Pcntnervthvittetranitmt has an effect in the inter "= rheidet. These pnten

disadvantageous from the fact that when severing the explosive properties of the Pcntaerythritol tetranitrate are

strings of explosives trickling out of them. The larger it is, although no binding agents have been added

The greater the diameter of the cords, the more sinuous.

more explosives trickle out of the cords. The present process can be divided into the same Of course, trickling out means carrying out some equipment in which the usual strong Danger to working with. Detonating cords 60 produced a pure pentaerythritol granitrate spot where there is going to be a slicing of. Also other common procedural measures, Detonating cords for the production of pieces of cord which are desired in the known production of pure penta-shaped cords Length cannot be avoided. erythritol granitrate can be used at

The depth to which the explosive from the method according to the invention is used. If the detonating cord can trickle out, the ratio of nonsolvent to solution depends, of course, on the type of treatment of the agent, as is the case with the previously customary process end piece of the cut detonating cord. So ren, at 1: 2.5,
is the trickle depth for a detonating cord with The nitriding added during the dissolution process

by-products are those products that Nitrieriuw of pentaerythritol with nitrating acid together with pentaerythritol tetranitrate arise and during the separation of the crude pentaerythritol tetranitrate obtained from this solution after separation of the solvent. This mixture - hereinafter referred to as the nitration by-product - contains the main component Also contains pentaerythritol tetranitrate and, as the most important by-product, dipentaerythritol hexanitrate this nitration by-product, in addition to small amounts of pentaerythritol trinitrate, also tripentaerythritol octonitrate and other, more highly nitrated secondary products of pentaerythritol, which cannot be determined in more detail. The composition has the following average values:

Pentaerythritol tetranitrate 71.2 ° / o

fenlaerythritol trinitrate 0.5%

Dipentaerythritol hexanitrate 7.5%

Tripentaerythritoctonitrate 3.0%

Nitrous bodies not specified in more detail, 3.0 per cent

H ₂ O 14.8%

The amount of nitrate by-products to be added to the solution of pentaerythritol tetranitrate can be between 7 and 12% by weight, based on the pentaerythritol tetranitrate. Preferably about 10% by weight used. These products must be in the pentaerythritol tetranitrate solution is present in dissolved form before the addition of the nonsolvent.

If acetone is used as the solvent - this is used as the preferred solvent -, it is advisable to increase the temperature to 50-56 "C before adding the non-solvent, to ensure that both the pentaerythritol granitrate and the nitrate by-products be in solution.

Water is preferably used as the nonsolvent. According to the invention, the amount of nonsolvent must be greater than that of the previously known Process for the pure preparation of pentaerythritol tetranitrate. The ratio of nonsolvent to solvent should be between 1: 2 and 1: 1.2. A ratio of 1: 1.7 is preferably used.

Those produced according to the method according to the specification Crystals of pentaerythritol tetranitrate are made up of a wafer-thin layer of nitrate by-products surround. This layer can only be seen as crystal opacity, even at high magnification. Analyzes show that there is no accumulation of nitrate by-products or impurities in the Pentaerythritol tetranitrate can be determined by this. Chromatographic analysis revealed the following Results:

Table 2 Table 1

Nitropenta, outlined without additives sn-miter by-product, with the relationship Fäü water too Solution of

Nitropenta, uiiicrystallized with the addition from approx. 12 »/« Nitration by-product, with the ratio Fall water to Solution of 1: 1.7

Nitropenta 99.4 ° / e

Pentaerythritol trinitrate -

Dipentaerythritol -
hexanitrate

Tripentaerythritol -
octonitrate

Further nitriding -
byproducts

H ₂ O 0.6 ⁰ zo
example

99.4%

0.1 ^β / β

0.5 »Ό

200 kg of crude pentaerythritol tetranitrate are placed in a stirred kettle dissolved in 700 kg of acetone with heating. After the solution has taken place, 20 kg of nitration by-products are obtained added and also brought into solution. The final temperature of the solution is about 52 ° C. After this solution in a precipitation kettle has been admitted, 400 liters of water are added with stirring. There's one in the water the amount of sodium carbonate (about 100 g) dissolved to neutralize the crystals in the crude pentaerythritol tetranitrate enclosed nitric acid is sufficient.

The pentaerythritol tetranitrate which has precipitated in the precipitation kettle is filtered off, washed with water and dried. It is then processed into detonating cords in a known manner. The detonating cords have a filling weight of pentaerythritol tetranitrate of 40g'm and 80g'm. Then the trickle depth was determined in the above manner. The values are given in Table 2 below.

For comparison, detonating cords with a pentaerythritol tetranitrate were made in the same way, whose purification was carried out in a completely analogous manner as described above, with the difference that the solution of the crude pentaerythril tetranitrate no nitration by-products were added and that in the precipitation kettle for precipitation only 2801 water were admitted. The determined discharge depths of these detonating cords go also shown in Table 2.

Discharge depth (cm) Detonating cord

with a filling weight of 40 g / m

comparison of the invention

Detonating cord

with a filling weight of 80 g / m

comparison of the invention

according to

Cut the detonating cord with a sharp 0 1–2 0 1–2.5 Knife on a wooden base

Free pounding back and forth of a 50 cm long 0-1 5-25 0-1 10-40 End piece (10 X)

Milling an end piece by hand 3–6 30–70 6–12 50–120

Claims (1)

a fill weight of 40 g / m pentaerythritol tetrani- patent claims occurred when the detonating cord was cut with a sharp knife on a wooden base 1. Process for the production of pourable I -2 cm. If, on the other hand, the end piece is on a length and binder-free pentaerythritol tetranitrate, beaten back and forth 5 of 50 cm 10 times, increased that when compacted, adheres to each other, thereby spreading the outlets to 5 - 25 cm; she still cherishes characterized in that you get a solution of higher (between 30 and 70 cm) when the end piece Crude pentaerythritol granitrate in a solution was hand drummed. medium 7 to 12 wt .-% based on the raw It was now em binder-free pentaerythritol pentaerythritol granitrate, Nitriei by-products, the io tranitrate found, which is neselfqual and is used for Use in the manufacture of pentaerythritol granitrate manufacture of such detonating cords accrue, clogs and brings into solution, this I, ö- leaves an explosive soul with a slight inclination have a nonsolvent for pentaerythration to trickle out. This penfierythritol granitrate in such a quantity that tranitrate is made by one of a Lödas The weight ratio of nonsolvent to solution of crude pentaerythritol tetrautrate in a solvent is between 1: 1.2 and 1: 2, and the solvent is 7-12 wt occurred in a manner known per se. in the production of pentaerythane tetranitrate 2. The method according to claim 1, thereby falling, adding and solving this solution indicates that the solvent used is acetone * o a non-solvent for pentaerythritol tetranitrate in and the dissolving of the nitrate byproducts adds such an amount that the weight products Performs at temperatures between the ratio of non-solvent to solvent between 50 and 56 ° C. see 1: 1,2 and 1: 2 cherishes, and then that 3. Free-flowing and binder-free penta-precipitated pentaerythritol granitrate on per se beerythritol granitrate, that adheres to compression, 25 separates in a known manner. produced according to claim 1. It is already known, pentaerythritol tetranitrate 4. Using one according to the method of together with dipentaerythritol hexanitrate and higher Claims 1 and 2 produced pentaerythritol nitride by-products that are used in the production of tranitrats for the manufacture of detonating cords. Pentaerythritol granitrate accumulate, together with 30 cases. In these known processes, the amount of nitration by-products does not matter, and it does the pentaerythritol granitrate becomes significantly with a larger amount of water precipitated. This precipitation process gives a pentaerythritol tetranitrate, the 35 detectable amounts of dipentaerythritol hexanitrate