The preparation method of spherical basic lead picrate and lead azoimide double salt primary explosive
One technical field
The present invention relates to the preparation method of a kind of industrial detonator, the preparation method of particularly a kind of spherical basic lead picrate and lead azoimide double salt primary explosive with basic lead picrate and lead azoimide double salt primary explosive.
Two background technologies
Detonator has multiple with priming explosive, as dextrin lead azide, DDNP, DS co-precipitation, GTG, KD double salt primary explosive or the like, wherein to detonate be the abbreviation of basic lead picrate and lead azoimide double salt primary explosive to KD double salt, it is that the eighties in last century is by the novel priming explosive of Nanjing Science ﹠ Engineering Univ Liu from a kind of excellent property of a small brass gong, Jiang Rongguang invention, once obtained 1988 annual national invention third prizes, this priming explosive has excellent property, stable; Produce safe in utilization; Wastewater flow rate is few, composition is simple, processing easily; Starting material are easily high, low cost and other advantages.Since this priming explosive came out, successively 10 tame factories applied at home, and all kinds of KD industrial detonators of accumulative total production and sales reach about 3,000,000,000, and steady quality is reliable, and economic results in society are remarkable.But because there is defective in existing KD double salt primary explosive preparation method: crystallization is wayward, often the forked crystallization of irregular rod occurs, and the product mechanical sensitivity is higher; The medicament dust is more, causes in actual production, and detonator pressing working procedure " pressing blast " frequency is higher, is unfavorable for capsular assembling safety, thereby brings difficulty for applying of KD double salt primary explosive.For reducing the mechanical sensitivity of priming explosive, U.S. Pat 3238076 has proposed a kind of method that adopts alkylated aromatic sulfonic acid salt, dextrin to prepare spherical four oxygen alkene or dextrin lead azide as tensio-active agent, this method be by adopt dextrin or alkylated aromatic sulfonic acid salt do tensio-active agent add priming explosive synthetic in, production technique is changed, thereby the priming explosive crystallization change over spherical outwardly.And domestic no spherical priming explosive crystallization.
Three summary of the invention
The object of the present invention is to provide a kind of mechanical sensitivity that can reduce product effectively, eliminate the spherical basic lead picrate of " pressing blast " in the detonator assembling and the preparation method of lead azoimide double salt primary explosive.
The technical solution that realizes the object of the invention is: the preparation method of a kind of basic lead picrate and lead azoimide double salt primary explosive, and its technical process and reaction conditions carry out in the following manner: will mix the formation mixed solution with crystal control agent, sodiumazide, the sodium picrate basic solution that alkylbenzene sulfonate, tartrate, carboxymethylcellulose sodium solution mix; Place lead nitrate solution to constitute liquid at the bottom of the chemical combination dextrin solution; Earlier a spot of mixed solution is added at the bottom of the chemical combination in the liquid as shifting to an earlier date liquid, under 65 ℃~80 ℃, in 30~60 minutes, in end liquid, evenly add mixed solution then, regulating the pH value is 4.0~5.0, the mother liquor siphon is handled, in combination apparatus, wash then, discharging, promptly getting does not have dust, spherical KD double salt primary explosive.
The preparation method of basic lead picrate of the present invention and lead azoimide double salt primary explosive can dextrin in aqueous solution be a liquid at the bottom of the chemical combination, and lead nitrate and mixed solution are added drop-wise in the combination apparatus simultaneously.
Among the preparation method of basic lead picrate of the present invention and lead azoimide double salt primary explosive, washing is carried out in combination apparatus, or carries out in suction filtration, and siphon top mother liquor or washing lotion are to eliminate crystallization in small, broken bits.
Among the preparation method of basic lead picrate of the present invention and lead azoimide double salt primary explosive, earlier 5% mixed solution is added at the bottom of the chemical combination in the liquid as shifting to an earlier date liquid.
The spherical KD double salt primary explosive of the present invention preparation has kept that former KD double salt primary explosive detonating capability is big, resistance to pressure good, major advantage such as flame sensitivity height, heat-resistant quality are good, free from environmental pollution, stable and reliable product quality, production are safe in utilization, and eliminated the medicament dust, reduced the mechanical sensitivity of product, improved the intrinsic safety of medicament, free-running property is good, is convenient to the constant volume measurement powder charge, can overcome " pressing blast " drawback in the detonator assembling.
Four description of drawings
Accompanying drawing is the preparation method's of spherical basic lead picrate of the present invention and lead azoimide double salt primary explosive a process flow diagram.
Five embodiments
Below in conjunction with accompanying drawing the present invention is further described.
Embodiment 1: in conjunction with the accompanying drawings, add earlier the lead nitrate of 29L~33L 18% in combination apparatus, add 45L pure water and 5L 5% dextrin solution again, as end liquid, control pH is 4.0~5.0 with this; Will be by 1.08kg picric acid, pure water, 4.1L10% sodium nitride, 500mL 0.5% Xylo-Mucine, the 48L sodium picrate basic solution (adding NaOH solution) that 50g sodium tartrate and 125g Sodium dodecylbenzene sulfonate are made into is formed mixed solution with 11.5L~13.5L 10% sodium azide solution; Under agitation, in combination apparatus, add the 2.6L mixed solution in 60 ℃~80 ℃ as shifting to an earlier date liquid, at the uniform velocity splash into mixed solution behind the 5min again, the reinforced time is 30min~60min, and reinforced finishing continues reaction 5min, reduces to then about 50 ℃, top mother liquor siphon is handled, and in combination apparatus, add pure water, washing secondary, discharging.The product apparent density can reach 2.1g/cm
3
Embodiment 2: add pure water 440mL and 5% dextrin solution 20mL~60mL earlier in combination apparatus, as end liquid, regulating end liquid pH is 4.5~5.0 with this; Be dropping liquid with 18% lead nitrate solution 115mL and mixed solution (composition and blending ratio are with example 1) 230mL again; Before reinforced, elder generation is interior in mixed solution toward combination apparatus: the ratio of lead nitrate solution=4: 2 (mL/min) adds liquid in advance, stops to expect 5min behind the 3min, at the uniform velocity adds in above-mentioned flow velocity ratio again, reacts the Decanter that finishes and separates out material, and all the other are with embodiment 1.