NAVY MIL-P-231 A-1955 PROPELLANT PYROCELLULOSE《高氮硝化纤维素推进剂》.pdf

1、MIL-P-23LA I3 = 7777706 0270863 8 I!-, MILP=23lA (Nord) 1 September 1955 Superseding 13 April 19h9 JAN-P-231 MILITARY SPECIFICATION 1. SCOPE 1.1 Scope. - This specification covers smokeless propellant intended for use 1.2 Classification. - Propellant powder covered by this specification shall as a p

2、rooelling charge for cannon. be furnished in the following types, as specified: Type I - Cylindrical mitiple-perforated grains Type II - Cylindrical single-perforated grains . 2. APPLICABLE WCUWNTS 2.1 The following specifications, standards, publications and drawings of the issue in effect on date

3、of invitation for bids, form a part ofthis specification: SPECIFIC ATIONS JAN-D-98 - Diphenylamine JAN-G155 - Graphite (For Use in Ammunition) JAN-P-193 - Potassi- Sulfate (For Ordnance Use) JAN-E-199 - Ether, Diethyl JAN-N-244 - Nitrocellulose (For Use in Explosives) JAN-P-270 - Ponder, Propellant,

4、 Cannon JAN-A-463 - Alcohol, Ethyl (For Ordnance Use) MILLi861f3 - Lead Carbonate, Bash, Dry (For Ordnance Use) STANDARDS dIKrrm?ierce CmmAssien regulations are new Q part of the Ceda endent of Documents, Chvernmenk Printing. Office, Washington 25, D.C. of Federal Regulatirum (1947 Fdikiem-Revised 1

5、950) avaiable fram the Ordera for the abeve pubicahien should cite f49 CFR 0.15 pats* - * Total Volatiles shall not exceed the maximum as shown by the curve of total volatiles on Fig. 1, * Mandatory for Uavy; optional for Army. 3.2.1 Graphite. - If a graphite coating is required, the contant shall b

6、e as specified in the contract or order. 3.2.2 Potassium Sulfate. - If incorporation of potassium sulfate in the propellant is required in the contract or order, the content shall be within 0.30 parts of the amount specified. 3.2.3 Total luoisture. - The total moisture when determined by the procedu

7、re in 403.6 shall be 0.60 f. 0.40 per cent, 3.3 Heat Test at 131.5OC. - When subjected to the.tcst in 4.3.3, the propellant shall not change the color of nrmeilmethylviolet test paper to the standard salmon pink color in less than 1 hour, and shall not emlode in less than 5 hours. 3 Provided by IHSN

8、ot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-P-23LA 23 = 9777706 027Ohh 3 W biIbI- 23lA (NOrd) 3.h millance Test . request of the Bureau Q$? Qrdg The compressibility test shall only be made on special g, oy at qptiag o. insgecting laboratory. 3.7 ProceSsiq it

9、 shall. be not less than 64 per cent of the total momt of solvent use in mixing, Di-inenylamine of approved purity, in the amount required, shall be dissolved in ether and added to the charge. The responsibility is upon the contractor to use the proportion of solvent which with his other processes,

10、will result in practically perfect colloiding, as shown by the strand as it issues from the graining press being of unifrirrri texture, free Xrom spots and blemishes. the solvent is uniformly distributed throughout the mass. reworked separately or by addition to fresh materials in the iilixers. work

11、ing of dirty scrap is not perniissible. or other component required to be added to prod.iice ssecified percentayes in the finished propellant, shall be incorporated in each mixing charge. The necessary amdmt o9 ether to be added is determined by climatic The mixing shall be continued until Cletan sc

12、rap may be The re- The necessary mount of diphenylamine, 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-P-231A 13 W 9999906 0290867 5 W fl i.IIL-P-23l.A (NOrd) 3.7.4 Pressine;. - The material coming from the mixers-shall be blocked and straine

13、d for the removal of lumps and any foreign naterial before goin3 throwh, or in, the graining press. vith such uniformity as will produce the standard grain required. the screen holes of the die must be at least 1% times the area of the cross section of the die. The colioid shall be pressed tnrough d

14、ies and cat The area of 3.7.5 Dryinq. - The specif icat ion contemplates as standard practice that the propellant shall be subjected to a suitable solvent recovery process, followed by a period of drying in air-dry houses. Ifhen the invitation for bids is so worded as to all-ow it, proposals or alte

15、rnative proposals may be submitted for the propellant dried by different processes, sufficiently described to permit their effect upon the propellant, and therefore their permissibility, to be judged. A11 snch processes, as for instance, %iater drying,“ must conform to the general principles of the

16、standard process; that is,-such initially mild treatment afia gently progressive increase of tehiperatvre (with rigid maximm limits) as may be adjudged sufficiently favor- able to the production of a. first-class finished propellant. Propellant manufactured under my such allowed alternative of dryin

17、g must, in the absence of special exceptions in the contract, meet all the tests herein described in order to be acceptable. wise specified. in the contract or order, shall be as follows: The propellant, after graining,may be placed at once in the solvent recovery apparatus, but the temperature and

18、other conditions of treatment therein must be so mild at first and so gently progressive that no harmful effects shall be produced in the propellant,and in no case shall tne temperature in solvent recovery exceed 55OC. The propellant shall thenbe finally dried. iil air in dry houses at a temperature

19、 not exceeding 55OC. A recording thermometer shall be suitably located in each dry house. At least two maximum and minimum thermometers shall be placed in the propellant, one in the hottest and the other in the coolest part,and daily temperature records shall be kept. Upon completion of the drying,

20、the heat shall be turned. off and the propellant allowed to cool to a temperature below 35 o C. 3.7.6 Handling. - The propellant and its standard ingredients shall at all times be protected from the action of direct sunlight and acid fumes. 3.7.7 Sortine. - The propellant shall be sorted thoroughly

21、so as to remove cracked, distorted, short and long grains and any otherwise deformed grains. This provision applies only to 8 inch grains and larger. acceptance, the contractor shall furnish, on official blanks, eight copies of a description sheet giving a complete history of its manufacture togethe

22、r with chemical and physical analyses. The standard drying practice, required unless other- 3.8 Description Sheets. - With every lot of propellant submitted for 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-P-23LA 13 7977706 0290868 7 M MIL-

23、P- 23U (Nord) 4te QUALIm MURANCE FROVISXmS AND TEST REQuXBEN?3 4.1 kt Size. - The Qt size shall bs 8 maximum of 165, pound6 pinless otherwise specified the contrct, or order, When cross-blends of sections are requested, a dum of 630,000 pounds will be pernttd. Specification iTWP-270. samples shall i

24、nc1ud.e zt least one samoliiag from each section. 4.2 SamplinS an4 Inspection, - This shall be done in accordance with If the lot is nade up of Fiore than one section, the 4.3 Test Procedures. - For Navy purchases, the tests shall be conducted at 4,S.i Ballistic Tests, - Ballistic tests sna91 be con

25、diicted as specified by 4.3.2 Compressibility Tests.- - The grocedure described in Specification JA = weigdt of propellant. 4.3.7.2 IliDhenylamine - Reworked Pmder. r Transfer 5 gus, of the ground sample (20 mesh) to a 1 litre Udenburg flask and add 200 al. of 15s NaOH solu- tion. funnel. Pass a cur

26、rent of stem thrau.h the NaOH soliltion and distill at a rate of approximately 7 nl. per minute, see fi,gure No. 3. Naintain the volume in the sair;ple flask at approximately 200 mi. Tne temperature of the distillate should. not exceed 3OoC. After approximately 800 ml. of distillate have been collec

27、ted in a 1000 al. separatory funnel (time will require about 90 min.) disconnect the condenser and steam senerator. throu.$h the condenser. Remove the condenser. Add 10 gus. of laCl to the dis- tillate. Sto-per the fuianel and shake vigorously for one minute. Allow the liquids to separate os appsoxi

28、mately 15 minutes and transfer the methylene chloride layer to a 500 ml, iodiqs flask. Repeat the extraction two additional times with a ml. portions of methylene chloride. in the 500 al. iodine %ask. Evaporate the solvent in a well-ventilated nood with a stram of dry air, Dissolve the residue in 75

29、 ml. of 70,; acetic acid and eo01 %o ljoC, Ada, bgP pipett?, 25 ml. of 0,2 N bromide-bromate solution. Add l m%, of 1:l 861 ana stopper the Pa stopper the flask and allow to stand for 5 minutes, Titrate with the Na2S203 solution to a starch end point. Normality of Xa2S203 = W 0049035 v where W = wei

30、ght of KzCr207 V = ml, of NazS203 consumed 4.3.7.2.3 Apparatus Required. - (a) Ladenburg disti1.ing flask, Capacity 1000 mi. (b) Separatory Funnel, capacity lo00 ml. (c) Spiral Water Condenser, Electric Heater, Central Scientific Co. No, 16530, 250 watts, (a) Electric Heater, Central Scientific Co.

31、 No, i6j95, 750 watts. 4.3.7.3 Gra hite. - Place the crucible used for the determination of diphenylamine + see par. 4.3,7,1) in a muffle furnace or in an incline position over a LS burner and heat strongly until all carbonaceous material has disappeared, Cool the crucible in a desiccator and weigh

32、 in weight as percentage of graphite in the. sample as received. Calculate the loss 4,3.7,4 Total VoPatiles, - 4.3.7,4.1 Preparation for test, - 4.3.7.4.1.1 Dibutylphthalate remnt, - Prepare a large quantity of dibutyl- phthalate reagent containing approxhately 9 . of diphenylamine per liter as fol

33、lows: Dissolve the desired quantity of diphenylamine in a small quantity of hot dibutylphthalate. Pour this solution into a large volume of dibutyl- phthalate and shake this solution VigoFously. When tested separately in the solution-evacuation appratus it should lose less than 10 mg. necessary to p

34、retreat the dibutylphthalate as follows to meet this requirement, Heat the dibutylphthalate for 2 hours at 145O to l5OoC while bubBling dry air It may be through it, Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-PIGF 23U (NOrd) . - Place 10 clean d

35、ry steel balls, 9/16 incb in Iplithalate reageht into each of n series of clean dry solution tube9 (see fig. 3). The dibutylphthalate reagent may be added through a small funnel either by means of a graduated cylinder or from an automatic 5O-al. delivery device provided with a larger-normal outlet.

36、Clean the inlet of each so3.ution tube with absorbent cotton held by steel forceps Using the forceps, insert a wad of pyrex glass wool, or equivalent, (about 0.2 gei.) in the inlet of each tube at such a point that it will not be in danger of falling into the tube and at tne sane time will not be in

37、 too close contact with the cork stoppe that is to be subsequently inserted, By means of 5-cmr pieces of rubber tubingf attach each solution tube to the manifold of a rocking device i oven2 maintained at 8CjC. Attach to the manifold a vacuum line assembl Fig. 4) and a vacuum pimp which is capable of

38、 consistenly maintaining a pressure !Rubber pressure tubing should have a j/l6-inch bore, 3/16-inch wall. Use 5-cm pieces foi? cohnecting the glass tubes to the copper manifold. Cut off a number of pieces, boil these in 5-percent sodium hydroxide solution for 10 to i5 rainutes, wash thoroughly, atid

39、 dry at 100C. after each total volatile determination and replaced when necessary. 2The oven should be fitted with a rocking device and electric motor. By means of the rocking device the tubes are ti.ted back and forth through an angle of approximately 90 at the rate of 12 complete cycles per minu.t

40、e. The oven desig- nated as Catalog No* 95105-A by the Central Scieatific Co. has been found satis- factory and should be pkovided with a safety latch to replace the regul.ar latch. A steam oven, if available, may be used in ylace of an electric oven, The air ad vapors from the solution tubes are pa

41、ssed through a T-tube leading to a McLsod gage, a T- tubing leading through an aspirator bottle I, filled with drierite, to a needle valve E, a three-way stopcock P. a 5OQ-ml. absorption bottle II containing silica gel, a trap D, 8 T-tube leading to a stopcock G, and a pressure regulator C. The boct

42、le of drierite I serves to dry the air which is admitted to the tubes in the oven. The needle valve E pkrmits a much closer control of the pressure during the .initial stage of the eVacu.ation than can be obtained by stopcock B. The three-way stopcock F serves to admit nitrogen to the tubes in the o

43、ven. The ab- sorption bottle of silica gel i is included to absorb the volatiles from the powder and thus make it unnecessary to change the oil in the vacuum pump frequent- ly. The silica gel may become ineffective as shown by the inability of the vacum paq to exhaust the sytem to 1 mm. or less. If

44、this haypens, the silica gel should be replaced with fresh material, The trap D serves to-keep dibutylphtha- late reagent, in the pressure regulator, away from absorption bottle H in case stopcock A is accidently closed when the vacum pump is stopped. The stopcock G serves to admit air into the vacu

45、um pump and pressiire regulator after the tubes hatre been filled With nitrogen. reasent serves to iaaintain the desired interior pressure. 4.3.7.4.1.2 The rubber tubing s1ioul.d be examined 3Vacuum line assembly should be as shown on figure 4. The replator G, containing dibutylphthalate ?% - - Prov

46、ided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-P-231A 13 m 7977906 0270873 O m of 1 mm. or less. Close stopcock G. With stopcock A open and stopcock B and needle valve E closed, turn on the rocking motor and vacuxm pmp, and evacuate the tukes to a p

47、ressure of 1 mm. or less as indicated by the XcLeod zage. Tnis pretreatment procedure is accomplished very easily because the evacuation is started when the dibutylphthalate reagent is still at approxi- mately room temgerature. 1 mm. presswe as the temperature rises. At t5e end of lz hours, stop the

48、 vacum pump and rocking motor, open stopcock Il cautiously, and admit dry air sl.owly by gradually oyening the needle valve E. If air is admitted too rapidly, the wads of Pyrex wool, or equivalent, may be drawn into tne solution tubes. Wearing a pair of gloves, reciove the solution tubes from the ov

49、en, 1.eaving the 5-CU. rubber connecting tubes attached, and place the solution tubes in a vire- screen tray (see Fig. 5). Immediately insert small protective dryins tubed (see Fig. 6) and allow the tubes arid contents to cool to room temperature. This will recgire from 30 to 45 minutes. the admission of atmospheric moisture during the cooling period. mination of the loss in weight of a solution tube involves the measurement of a decre