Method for recovering fine crystalline agents produced during the nickel hydrazine nitrate complexing process

Abstract

The application discloses a method for recycling fine-crystal medicaments generated in a nickel hydrazine nitrate combination process, and belongs to the field of initiating explosive devices and explosive medicaments, and comprises collection of the fine-crystal medicaments and granulation of the fine-crystal medicaments; under the premise that the combination process and device of the nickel hydrazine nitrate are not changed, the fine-crystal nickel hydrazine nitrate is recycled through the crystallization collection technology and the secondary granulation technology, the yield of the nickel hydrazine nitrate is improved, the waste gas produced in the waste medicament destruction process is eliminated, and the environmental protection is improved; the obtained granulated nickel hydrazine nitrate is detected by using a particle size analyzer, and the particle size distribution of the granulated nickel hydrazine nitrate is as follows: 20 mesh to 40 mesh particles account for about 30% of the product, 40 mesh to 60 mesh particles account for about 35%, and 60 mesh to 100 mesh particles account for about 35%, so that the particle size distribution is relatively uniform.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of initiating explosive, in particular to a method for recycling fine crystalline explosive generated in the process of synthesizing nickel hydrazine nitrate. BACKGROUND

[0002] Nickel hydrazine nitrate is a green and environmentally friendly primary explosive with excellent performance, which is mainly used in industrial detonators. Compared with other primary explosives, it has the characteristics of wide raw material sources, safe preparation, simple process and less wastewater. The current synthesis method of the explosive is the combination reaction of nickel nitrate solution and high-concentration hydrazine hydrate solution. Due to the influence of factors such as stirring method, solution concentration, feeding speed and temperature control, part of the fine crystalline (particle size about 2-100 microns) nickel hydrazine nitrate particles are easily generated in the synthesis process. If not separated out, it will have a great influence on the flowability and initiation performance of nickel hydrazine nitrate primary explosive, mainly showing heavy explosive dust, uneven charging, metering plate jamming and safety risks such as burning and explosion during the charging process.

[0003] Specifically, after the combination reaction, the mother liquor containing fine crystalline nickel hydrazine nitrate separated is usually put into a mother liquor tank. After the mother liquor is left to stand, the fine crystalline nickel hydrazine nitrate will sink to the bottom of the tank. According to statistics, 20-25 g of fine crystalline explosive will be generated per production of 1 kg of nickel hydrazine nitrate. If 100 kg of explosive is produced per day, 2.0-2.5 kg of deposited explosive will be generated per day. If not handled in time, it will form a safety hazard.

[0004] Although the deposited explosive can be reused as a component of the sensitizing agent of the ignition head, the amount of explosive used by the ignition head is particularly limited. Most of the deposited explosive can only be treated by incineration, which not only causes waste but also is not conducive to environmental protection. SUMMARY

[0005] The purpose of the present application is to provide a method for recycling fine crystalline explosive generated in the process of synthesizing nickel hydrazine nitrate, so as to solve the above problems.

[0006] In order to achieve the above purpose, the technical scheme adopted by the present application is as follows: a method for recycling fine crystalline explosive generated in the process of synthesizing nickel hydrazine nitrate, comprising the following steps:

[0007] (1) Collection of fine crystalline explosive

[0008] 1) A mother liquor transfer tank capable of being vacuumized is added in the pharmaceutical process. After the combination of the material liquid in the combination device (combination temperature 72-76℃) is completed and the heat preservation is finished, the temperature is lowered and the material liquid is left to stand. Then the mother liquor transfer tank is vacuumized. The upper layer of the material liquid containing fine crystalline in the combination device is sucked into the mother liquor transfer tank through the suction pipe. The mother liquor in the mother liquor transfer tank is left to stand, and the fine crystalline nickel hydrazine nitrate is deposited at the bottom of the tank. The upper clear mother liquor is pumped into the mother liquor tank.

[0009] 2) The mother liquor in the transfer tank is emptied, the bottom deposited medicament is put into the filter at the lower part of the transfer tank, vacuum filtration is carried out, and the fine crystalline nickel hydrazine nitrate is recovered by cleaning;

[0010] (2) Granulation of the fine crystalline medicament

[0011] Pure water is added to the compounder, and the fine crystalline nickel hydrazine nitrate obtained in step (1) is added to the compounder to obtain a suspension. Granulation of the fine crystalline nickel hydrazine nitrate is realized by stirring, heating, and adding a high molecular binder.

[0012] The fine crystalline nickel hydrazine nitrate mother liquor is drawn into the vacuum transfer tank, discharged after deposition, and the safety risk is reduced. Then, the high molecular binder is used for secondary granulation (polycrystal) to realize the particle size recombination of the fine crystalline nickel hydrazine nitrate, and improve the flowability and uniformity of the medicament.

[0013] The present application optimizes the collection method of fine crystalline nickel hydrazine nitrate, and recycles the fine crystalline nickel hydrazine nitrate. By adding a small amount of high molecular binder, the fine crystalline medicament is recombined, which solves the environmental protection problem, reduces the production cost, and improves the yield of nickel hydrazine nitrate.

[0014] Compared with the existing reported granulation method, the present application does not need to use a dispersant, and does not need to be sieved, and the operation is relatively simple and the cost is lower.

[0015] As a preferred technical solution: in step 1), the temperature of the liquid in the compounder is reduced to 50-60℃, and the liquid is allowed to stand for 1-2 min; the standing time of the mother liquor in the transfer tank is more than 1.5 h.

[0016] As a preferred technical solution: in step (2), the high molecular binder is methyl methacrylate. The present application preferably uses methyl methacrylate (MMA) with the chemical formula C5H8O2. The present application further preferably uses ethyl acetate to dissolve methyl methacrylate to ensure that methyl methacrylate is fully dissolved in ethyl acetate to prepare an adhesive solution.

[0017] As a further preferred technical solution: the mass percentage ratio of the fine crystalline nickel hydrazine nitrate to methyl methacrylate is (98.0%-99.5%):(0.5%-2.0%).

[0018] As a preferred technical solution: in step (2), the specific granulation method is: the mass of the added pure water is 2-3 times that of the fine crystalline medicament, a suspension is obtained, the suspension is heated to 55-60℃ under stirring, then the adhesive solution is slowly added, and after the adhesive solution is added, the temperature is continued to be raised to 65-75℃.

[0019] As a further preferred technical solution: the speed of the adhesive solution added to the suspension is 400-500 ml / min. Since methyl methacrylate in ethyl acetate is continuously precipitated and coated on the surface of fine crystalline nickel hydrazine nitrate, the speed of the adhesive solution added to the suspension is related to the particle size and uniformity of the particle size distribution of the crystalline product. If the addition speed is too fast, the particle size of the crystalline product will be uneven, resulting in more waste products and not meeting the product particle size requirements. Therefore, the addition speed is strictly controlled.

[0020] Compared with the prior art, the advantages of the present application are that the present application realizes the recovery of fine crystalline nickel hydrazine nitrate, improves the yield of nickel hydrazine nitrate, eliminates waste gas produced in the waste drug destruction process, and improves environmental protection without changing the combination process and device of nickel hydrazine nitrate. The particle size analyzer is used for detection, and the particle size distribution of the obtained granulated nickel hydrazine nitrate is that the particles of 20-40 mesh account for about 30% of the product, the particles of 40-60 mesh account for about 35%, and the particles of 60-100 mesh account for about 35%, and the particle size distribution is relatively uniform. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 The processing flowchart of the present application is shown in Figure 2 The collection device diagram of the fine crystalline drug in Example 1 of the present application is shown in

[0022] In the figure: 1, a compounder; 2, a mother liquor transfer tank; 3, a suction filter; 4, a valve; 5, a discharge pipe; 6, a vacuum pipe; 7, a suction pipe; 8, a liquid level pipe. DETAILED DESCRIPTION

[0023] The present application will be further described below with reference to the accompanying drawings. Example 1

[0024] Referring to Figure 1 A fine crystalline drug recovery treatment method produced in the process of combining nickel hydrazine nitrate, comprising the following steps: (1) collecting the crystalline drug

[0025] The device used in this step is shown in Figure 2 The device used in this step is shown in

[0026] The main work is divided into two steps: by adding a mother liquor transfer tank 2 which can be vacuumized to the existing synthesis equipment, when the material liquid in the compounder 1 is completed, the compound temperature is 75°C and the temperature is kept, after the end, the temperature is reduced to 55°C;

[0027] The material liquid is placed for 2 minutes, the mother liquor transfer tank 2 is connected with a vacuum device through a vacuum pipe 6 to be vacuumized, the upper mother liquor containing fine crystals in the compounder 1 is sucked into the mother liquor transfer tank 2 through a suction pipe 7, the mother liquor in the mother liquor transfer tank 2 is placed for 2 hours, the fine crystalline nickel hydrazine nitrate is deposited at the bottom of the tank, and the upper clear mother liquor is pumped into the mother liquor tank of the existing synthesis process;

[0028] Then the mother liquor transfer tank 2 is emptied, the deposited reagent at the bottom is put into the filter 3 at the lower part of the mother liquor transfer tank 2 through the valve 4, vacuumization is carried out for filtration and washing, and the reagent is recovered;

[0029] (2) Granulation of fine crystalline reagent

[0030] Pure water is added to the compounder, fine crystalline nickel hydrazine nitrate is added, the mass of the added water is 2.5 times of the fine reagent, and a suspension is obtained;

[0031] Then methyl methacrylate is taken and fully dissolved in ethyl acetate to prepare an adhesive solution; the mass ratio of methyl methacrylate to ethyl acetate is 1:6;

[0032] In a stirring state, the suspension is heated to 55°C, then the adhesive solution is added at a speed of 500 ml / min, after the addition of the adhesive solution is completed, heating is continued to 65°C. The upper vacuum system of the compounder is opened, the upper part of the suspension in the compounder is vacuumized to discharge ethyl acetate, the solution continues to be heated to 75°C, after the ethyl acetate is completely evaporated, the cold water circulation of the compounder is started, the material liquid in the compounder is cooled to 35°C, the vacuumization is stopped, and then the material liquid is discharged to a tray tank for washing, filtration, tray, drying, and finally the granulated nickel hydrazine nitrate is obtained.

[0033] In this embodiment, the feeding amount of the fine crystalline reagent is 15 kg, the yield of the granulated reagent is about 98%, and there are still 2% of fine crystalline reagents, which are finally sucked into the mother liquor transfer tank for repeated recycling. The particle size distribution of the obtained granulated nickel hydrazine nitrate is that the particles of 20-40 mesh account for about 30% of the product, the particles of 40-60 mesh account for about 35%, and the particles of 60-100 mesh account for about 35%. Example 2

[0034] Compared with Example 1, the adhesive solution adding speed is 380ml / min, and the rest conditions are the same as those in Example 1, the yield is 80%, the obtained granulated nickel hydrazine nitrate has a particle size distribution of 20-40 mesh particles accounting for about 25% of the product, 40-60 mesh particles accounting for about 25%, and 60-100 mesh particles accounting for about 50%. The medicament is relatively fine, and dust phenomenon exists in the use process. Example 3

[0035] Compared with Example 1, the adhesive solution adding speed is 530ml / min, and the rest conditions are the same as those in Example 1, the yield is 98%, the obtained granulated nickel hydrazine nitrate has a particle size distribution of 20-40 mesh particles accounting for about 40% of the product, 40-60 mesh particles accounting for about 45%, and 60-100 mesh particles accounting for about 15%. The medicament is relatively coarse, has good flowability, but half-explosion phenomenon of detonator exists in the use process. Example 4

[0036] Compared with Example 1, in step (1), after the combining and heat preservation are completed, the temperature is reduced to 65℃ for discharging, and the rest conditions are the same as those in Example 1, the yield is about 78%.

[0037] It is illustrated that the temperature has an influence on the solubility of nickel hydrazine nitrate in water, and also has an influence on the combining effect. If the discharging temperature is too high, it is not conducive to the material pipeline and the like when discharging, and also leads to the reduction of the yield of nickel hydrazine nitrate.

[0038] The above only describes the preferred embodiments of the present application and is not used to limit the present application, and any modification, equivalent replacement and improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A method for recovering and processing fine crystalline agents generated in a process for producing nickel hydrazine nitrate, characterized by, It comprises the following steps: (1) collection of fine crystalline medicament 1) A mother liquor transfer tank capable of being vacuumized is added in the pharmaceutical process. After the completion of the combination of the material liquid in the combination device and the end of the heat preservation, the material liquid is cooled and left to stand, then the mother liquor transfer tank is vacuumized, the upper layer mother liquor containing fine crystals in the combination device is sucked into the mother liquor transfer tank through the suction pipeline, the mother liquor in the mother liquor transfer tank is left to stand, the fine crystalline nickel hydrazine nitrate deposits at the bottom of the tank, and the clear mother liquor at the upper part is pumped into the mother liquor tank; 2) The mother liquor transfer tank is emptied, the deposited medicament at the bottom is put into the suction filter at the lower part of the mother liquor transfer tank, vacuumization is carried out for suction filtration and cleaning, and the fine crystalline nickel hydrazine nitrate is recovered; (2) granulation of fine crystalline medicament Pure water is added in the combination device, the fine crystalline nickel hydrazine nitrate obtained in step (1) is added to obtain a suspension, and the granulation of the fine crystalline nickel hydrazine nitrate is realized by stirring, heating and adding a high molecular binder.

2. The method according to claim 1, wherein the fine crystalline agent generated in the process of producing nickel hydrazine nitrate is recovered by, In step 1), the material liquid in the combination device is cooled to 50-60℃, and the material liquid is left to stand for 1-2 min; the mother liquor in the mother liquor transfer tank is left to stand for 1.5 h or more.

3. The method according to claim 1, wherein the fine crystalline agent generated in the process of producing nickel hydrazine nitrate is recovered by the process of, In step (2), the high molecular binder is methyl methacrylate.

4. The method according to claim 3, wherein the fine crystalline agent is recovered by the following steps: The mass percentage ratio of the fine crystalline nickel hydrazine nitrate to methyl methacrylate is (98.0%-99.5%):(0.5%-2.0%). ​ 5. The method of claim 1, wherein the fine crystalline agent is recovered by the process of claim 1. In step (2), the specific granulation method is as follows: under the state of stirring, the suspension is heated to 55-60℃, then the binder solution is slowly added, after the addition of the binder solution is completed, heating is continued to 65-75℃.

6. The method according to claim 5, wherein the fine crystalline agent is recovered by the following steps: The speed of adding the binder solution into the suspension is 400-500 ml / min. ​

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