In a further patent (Eng. Pat. 3,020, 1903) the authors propose with the object of preventing the formation and separation of nitro-glycerine in the waste acids, after the nitro-glycerine initially formed in the nitrating vessel has been separated and removed, to add a small quantity of water to the waste acids; this is carried out as follows. A relatively small quantity of water is added, and this prevents all further separation of nitro-glycerine, and at the same time the strength of the waste acids is so slightly reduced that their separation and re-concentration are not affected. "After-separation" is thus done away with, and the nitro- glycerine plant simplified and its output increased. After nitration separation is commenced at a temperature such that when all the displacing acid has been added, and the separation of the nitro-glycerine is complete, the temperature of the contents of the nitrating vessel shall not be lower than 15° C. A sufficient quantity of the displacing acid is then run off through the waste-acid cock to allow of the remaining acids being air-stirred without splashing over the top. A small quantity of water, from 2 to 3 per cent. according to strength of acid; if waste consists of sulphuric acid (monohydrate), 62 per cent.; nitric acid (anhydrous), 33 per cent. and water 5 per cent.; temperature 15° C., then 2 per cent. of water is added; if waste acids contain less than 4 per cent. of water of temperature lower than 15° C., from 3 to 5 per cent. of water may have to be added. The water is added slowly through the separator cylinder, and the contents of the nitrator air-stirred, but not cooled, the temperature being allowed to rise slowly and regularly as the water is added—usually about 3° C. for each per cent. of water added. When air-agitation has been stopped, the acids are kept at rest for a short time, in order to allow of any small quantity of initially formed nitro-glycerine adhering to the coils and sides of the vessel rising to the top. When this has been separated by displacement, the acids are ready for denitration, or can be safely stored without further precaution.
~Separation.~—The nitro-glycerine, together with the mixed acids, flows from the nitrating house to the separating house, which must be on a lower level than the former. The separating house contains a large lead-lined tank, closed in at the top with a wooden lid, into which a lead pipe of large bore is fixed, and which is carried up through the roof of the building, and acts as a chimney to carry off any fumes. A little glass window should be fixed in this pipe in order that the colour of the escaping fumes may be seen. The conduit conveying the nitro-glycerine enters the building close under the roof, and discharges its contents into the tank through the pipe G (Fig. 8). The tank is only about two-thirds filled by the charge. There is in the side of the tank a small window of thick plate glass, which enables the workman to see the level of the charge, and also to observe the progress of the separation, which will take from thirty minutes to one hour.
The tank should be in connection with a drowning tank, as the charge sometimes gets very dangerous in this building. It must also be connected by a conduit with the filter house, and also to the secondary separator by another conduit. The tank should also be fitted with a compressed air pipe, bent in the form of a loop. It should lie upon the bottom of the vat. The object of this is to mix up the charge in case it should get too hot through decomposition. A thermometer should of course be fixed in the lid of the tank, and its bulb should reach down to the middle of the nitro-glycerine (which rests upon the surface of the mixed acids, the specific gravity of the nitro-glycerine being 1.6, and that of the waste acids 1.7; the composition of the acids is now 11 per cent. HNO_{3}, 67 per cent. H_{2}SO_{4}, and 22 per cent. water), and the temperature carefully watched.
[Illustration: FIG. 8.—SEPARATOR. A, Compressed Air Pipes; G, Nitro-
glycerine enters from Nitrator; N, Nitro-glycerine to P; L, Lantern
Window; W, Window in Side; S, Waste Acids to Secondary Separator; T,
Tap to remove last traces of Nitro-glycerine; P, Lead Washing Tank; A,
Compressed Air; W, Water Pipe; N, Nitro-glycerine from Separator.]
If nothing unusual occurs, and it has not been necessary to bring the compressed air into use, and so disturb the process of separation, the waste acids may be run away from beneath the nitro-glycerine, and allowed to flow away to the secondary separator, where any further quantity of nitro-glycerine that they contain separates out after resting for some days. The nitro-glycerine itself is run into a smaller tank in the same house, where it is washed three or four times with its own bulk of water, containing about 3 lbs. of carbonate of soda to neutralise the remaining acid. This smaller tank should contain a lead pipe, pierced and coiled upon the bottom, through which compressed air may be passed, in order to stir up the charge with the water and soda. After this preliminary washing, the nitro-glycerine is drawn off into indiarubber buckets, and poured down the conduit to the filter house. The wash waters may be sent down a conduit to another building, in order to allow the small quantity of nitro-glycerine that has been retained in the water as minute globules to settle, if thought worth the trouble of saving. This, of course, will depend upon the usual out-turn of nitro-glycerine in a day, and the general scale of operations.
[Illustration: FIG. 9.—FILTERING AND WASHING PLANT. W, Lead Washing
Tank; WP, Water Pipe; L, Lid; S, Nitro-glycerine from Separator; A,
B, C, Filtering Tanks; B2, Indiarubber Bucket.]
~Filtering and Washing.~—The filter house (Fig. 9), which must of course be again on a somewhat lower level than the separating house, must be a considerably larger building than either the nitrating or separating houses, as it is always necessary to be washing some five or six charges at the same time. Upon the arrival of the nitro-glycerine at this house, it first flows into a lead-lined wooden tank (W), containing a compressed air pipe, just like the one in the small tank in the separating house. This tank is half filled with water, and the compressed air is turned on from half to a quarter of an hour after the introduction of the charge. The water is then drawn off, and fresh water added. Four or five washings are generally necessary. The nitro-glycerine is then run into the next tank (A), the top of which is on a level with the bottom of the first one. Across the top of this tank is stretched a frame of flannel, through which the nitroglycerine has to filter. This removes any solid matters, such as dirt or scum. Upon leaving this tank, it passes through a similar flannel frame across another tank (B), and is finally drawn off by a tap in the bottom of the tank into rubber buckets. The taps in these tanks are best made of vulcanite.
At this stage, a sample should be taken to the laboratory and tested. If the sample will not pass the tests, which is often the case, the charge must be rewashed for one hour, or some other time, according to the judgment of the chemist in charge. In the case of an obstinate charge, it is of much more avail to wash a large number of times with small quantities of water, and for a short time, than to use a lot of water and wash for half an hour. Plenty of compressed air should be used, as the compound nitric ethers which are formed are thus got rid of. As five or six charges are often in this house at one time, it is necessary to have as many tanks arranged in tiers, otherwise one or two refractory charges would stop the nitrating house and the rest of the nitro-glycerine plant. The chief causes of the washed material not passing the heat test are, either that the acids were not clean, or they contained objectionable impurities, or more frequently, the quality of the glycerine used. The glycerine used for making nitro-glycerine should conform to the following tests, some of which, however, are of greater importance than others. The glycerine should—
1. Have minimum specific gravity at 15° C. of 1.261.
2. Should nitrify well.