Two-phase reverse polarity mixed solution for separating and purifying waste black powder components

Abstract

This invention discloses a two-opposite-polarity mixture for the separation and purification of components from waste black tantalum explosives. The mixture comprises a polar solvent for dissolving the cyclotrimethylenetrinitramine (RDX) component in the waste black tantalum explosives and a non-polar solvent for dissolving the trinitrotoluene (TNT) component in the waste black tantalum explosives. This mixture separates and purifies the components of the waste black tantalum explosives, allowing RDX and TNT to dissolve separately in two incompatible opposite-polarity solvents. This facilitates subsequent separation of the two solvents using a separator, followed by vacuum distillation to recover RDX, TNT, and their corresponding solvents. The purity of the obtained RDX and TNT can reach over 99.9%, and the two opposite-polarity solvents can be reused multiple times.

Description

Technical Field

[0001] This invention belongs to the field of resource recycling technology and relates to a mixture of two opposite polarities for the separation and purification of components of waste black ladder explosives. Background Technology

[0002] Resource recycling is a strategic emerging industry that benefits the country and its people. It encompasses all large-scale, high-value equipment and materials, including a large number of decommissioned and discarded explosives. Black ladder-type explosives, a type of mixed explosive that was produced and deployed in large quantities in my country in its early days, are now in a state of decommissioning and scrapping after reaching the end of their service life. Black ladder explosives are a series of two-component mixed explosives designed in my country in the last century by imitating the Soviet TG series explosives. Their formula consists of two energetic materials, RDX and TNT, with the mass ratio of RDX to TNT ranging from 30:70 to 80:20. Representative black ladder explosive products include Black Ladder 50 / 50 (mass ratio of RDX to TNT of 50:50), Black Ladder 60 / 40 (mass ratio of RDX to TNT of 60:40), and Black Ladder 40 / 60 (mass ratio of RDX to TNT of 40:60). The preparation process of this type of explosive is to first heat the TNT until it is completely melted, then add RDX and stir to mix it evenly. It can then be directly filled into projectiles or made into thin sheets and bagged for later use.

[0003] Traditionally, large quantities of decommissioned black dart explosives are disposed of through direct incineration. This not only causes environmental pollution but also wastes RDX and TNT contained in the black dart explosives. To separate and recover the energetic components from black dart explosives, Academician Wang Zeshan reported using solvents such as benzene and toluene to dissolve the TNT, followed by filtration to obtain insoluble RDX. While this process can extract RDX from black dart explosives, the filtered RDX still retains TNT-containing solution on its surface, resulting in RDX purity that does not meet national military standards. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide a two-opposite-polarity mixture for the separation and purification of components of waste black dextrin explosives. This mixture uses two-opposite-polarity mixtures to separate and purify the components of waste black dextrin explosives, so that RDX and TNT in the black dextrin explosives are dissolved in two incompatible opposite-polarity solvents, which facilitates the subsequent separation of the two solvents by a separator, and then the RDX, TNT and corresponding solvents are recovered by vacuum distillation. The purity of the obtained RDX and TNT can reach more than 99.9%, and the two opposite-polarity solvents can also be reused multiple times.

[0005] To achieve the above objectives, the present invention discloses a two-opposite-polarity mixture for the separation and purification of components of waste black tahini explosives, comprising a polar solvent for dissolving the cyclic trimethylenetrinitramine (RDX) component in waste black tahini explosives and a non-polar solvent for dissolving the trinitrotoluene (TNT) component in waste black tahini explosives.

[0006] Furthermore, the polarity of the polar solvent is 5.4 to 6.2;

[0007] The polarity of the nonpolar solvent is 0 to 0.1.

[0008] Furthermore, the mass ratio of polar solvent to non-polar solvent is equal to the mass ratio of cyclotrimethylenetrinitramine to trinitrotoluene in waste black dart explosive.

[0009] Furthermore, the polar solvent is acetonitrile.

[0010] Furthermore, the nonpolar solvent is n-pentane.

[0011] Furthermore, the nonpolar solvent is cyclohexane.

[0012] Furthermore, the nonpolar solvent is hexane.

[0013] Furthermore, the polarity of the polar solvent is 6.2.

[0014] Furthermore, the polarity of the nonpolar solvent is 0.

[0015] Furthermore, the polarity of the nonpolar solvent is 1.

[0016] The present invention has the following beneficial effects:

[0017] The present invention describes a two-phase, oppositely polar mixture for the separation and purification of components from spent black tantalum explosives. In specific operation, it includes a polar solvent for dissolving the cyclic trimethylenetrinitramine (RDX) component in the spent black tantalum explosives and a non-polar solvent for dissolving the trinitrotoluene (TNT) component. This mixture can separate and purify the components of spent black tantalum explosives, obtaining RDX and TNT with a purity ≥99.9%, meeting the purity requirements of the national military standard for these two energetic materials. By controlling the polarity and polarity difference of the selected two-phase solvents, the present invention achieves the directional dissolution of the two components of the black tantalum explosives. In each solvent system, only one energetic material component is dissolved, thus ensuring the purity of the recovered energetic material. Attached Figure Description

[0018] The accompanying drawings, which form part of this specification, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings:

[0019] Figure 1 This refers to the RDX obtained after separation and purification in Example 1 of the present invention;

[0020] Figure 2 The TNT obtained after separation and purification in Example 1 of this invention;

[0021] Figure 3 This is a process diagram for separating components of the black ladder explosive. Detailed Implementation

[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] In the description of this invention, it should be understood that the terms "comprising" and "including" indicate the presence of the described features, integrals, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or collections thereof.

[0024] It should also be understood that the terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. As used in this specification and the appended claims, the singular forms “a,” “an,” and “the” are intended to include the plural forms unless the context clearly indicates otherwise.

[0025] It should also be further understood that the term "and / or" as used in this specification and the appended claims refers to any combination and all possible combinations of one or more of the associated listed items, and includes such combinations. For example, A and / or B can represent three cases: A alone, A and B simultaneously, and B alone. Additionally, the character " / " in this invention generally indicates that the preceding and following objects have an "or" relationship.

[0026] It should be understood that although terms such as first, second, third, etc., may be used in the embodiments of the present invention to describe the preset range, these preset ranges should not be limited to these terms. These terms are only used to distinguish the preset ranges from one another. For example, without departing from the scope of the embodiments of the present invention, the first preset range may also be referred to as the second preset range, and similarly, the second preset range may also be referred to as the first preset range.

[0027] Depending on the context, the word "if" as used here can be interpreted as "when," "when," "in response to determination," or "in response to detection." Similarly, depending on the context, the phrase "if determination" or "if detection (of the stated condition or event)" can be interpreted as "when determination," "in response to determination," "when detection (of the stated condition or event)," or "in response to detection (of the stated condition or event)."

[0028] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. The components of the embodiments of the present invention described and shown in the accompanying drawings can generally be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0029] The accompanying drawings illustrate various structural schematic diagrams according to embodiments disclosed in this invention. These drawings are not to scale, and some details have been enlarged for clarity, and some details may have been omitted. The shapes of the various regions and layers shown in the drawings, as well as their relative sizes and positional relationships, are merely exemplary and may deviate from reality due to manufacturing tolerances or technical limitations. Furthermore, those skilled in the art can design regions / layers with different shapes, sizes, and relative positions as needed.

[0030] The design principle of this invention is as follows:

[0031] Current reports on the separation of TNT components in Black Ladder explosives all involve dissolving TNT in a solvent and then filtering the precipitated RDX. Because the RDX surface retains residual TNT-containing solution, the dried RDX is still coated with a layer of TNT. Therefore, the purity of the obtained RDX does not meet the requirements of the national military standards.

[0032] To address the shortcomings of existing separation methods in obtaining high-purity RDX, this invention aims to separate the two components of Black Ti explosive by using a mixture of two opposite polarities. RDX and TNT are dissolved separately using two phase solvents, and then the two phase solvents are separated to achieve the separation and purification of RDX and TNT in Black Ti explosive.

[0033] By screening the polarity of the two-phase solvents and controlling their polarity difference, a mixed solution with two opposite polarities was obtained. This solution can be directly used to dissolve and separate RDX and TNT in black ladder explosive. After dissolution, a separator was used to separate the two immiscible solvents to obtain solutions of RDX and TNT. Then, vacuum distillation was used to recover the separated energetic materials and corresponding solvents. The purity of RDX and TNT precipitated in their respective solvents was further improved, meeting the requirements for product purity specified in the national military standard.

[0034] Based on the above, the two opposite polarity mixtures for the separation and purification of components of waste black tactic explosives described in this invention include a polar solvent for dissolving the cyclic trimethylenetrinitramine (RDX) component in waste black tactic explosives and a non-polar solvent for dissolving the trinitrotoluene (TNT) component in waste black tactic explosives.

[0035] Specifically, the polarity of the polar solvent is 5.4 to 6.2; the polarity of the non-polar solvent is 0 to 0.1; the mass ratio of the polar solvent to the non-polar solvent is equal to the mass ratio of cyclotrimethylenetrinitramine to trinitrotoluene in the waste black dart explosive.

[0036] Example 1

[0037] The two opposite polarity mixtures for the separation and purification of components of waste black ladder explosives described in this invention include acetonitrile and n-pentane, wherein the polarity of n-pentane is 0, the polarity of acetonitrile is 6.2, the mass ratio of acetonitrile to n-pentane is 1:1, and the target for separation and purification is black ladder 50 / 50 explosive.

[0038] The separation and purification process is as follows: 1) Preparation of two opposite polarity mixtures: Weigh 50 ml of acetonitrile and 50 ml of n-pentane at room temperature, and add the two solvents to a flask equipped with a stirrer; 2) Separation of Black Ti 50 / 50 explosive: Start stirring to 100 r / min, slowly add 50 g of Black Ti 50 explosive to a beaker, and continue stirring for 5 min to 10 min after the Black Ti 50 explosive is added, until the Black Ti 50 explosive is completely dissolved, then stop stirring. After the solution system has settled and separated into layers, use a separator to separate the two phases; 3) Purification and recovery of RDX and TNT samples: Use a vacuum distillation apparatus to perform vacuum distillation on the solvents that dissolved RDX and TNT, respectively, to obtain purified RDX and TNT while recovering and reusing the acetonitrile and n-pentane solvents.

[0039] Performance testing:

[0040] a) Purity: Tested using high performance liquid chromatography (HPLC);

[0041] b) Moisture and volatile matter, mechanical sensitivity: tested using methods 102.1, 601.1 and 602.1 in GJB772A-97, respectively.

[0042] Example 2

[0043] The present invention describes a two-opposite polarity mixture for the separation and purification of components from waste black ladder explosives, comprising acetonitrile and cyclohexane, wherein the polarity of cyclohexane is 0.1, the polarity of acetonitrile is 6.2, the mass ratio of acetonitrile to n-pentane is 60:40, and the target for separation and purification is black ladder 60 / 40 explosive.

[0044] Example 3

[0045] The present invention describes a two-opposite polarity mixture for the separation and purification of components from waste black ladder explosives, comprising acetonitrile and cyclohexane, wherein the polarity of hexane is 0.06, the polarity of acetonitrile is 6.2, and the mass ratio of acetonitrile to n-pentane is 40:60. The target for separation and purification is black ladder 40 / 60 explosive.

[0046] The purity, friction sensitivity, and impact sensitivity test values ​​of RDX and TNT obtained after separation and purification according to this invention are shown in Table 1.

[0047] Table 1 Performance data of the present invention

[0048]

[0049] The RDX obtained after separation and purification in Example 1 of this invention is as follows: Figure 1 As shown.

[0050] The TNT obtained after separation and purification in Example 1 of this invention is as follows: Figure 2 As shown.

[0051] Other embodiments of the invention will readily occur to those skilled in the art upon consideration of the specification and disclosure of the invention. This application is intended to cover any variations, uses, or adaptations of the invention that follow the general principles of the invention and include common knowledge or customary techniques in the art not disclosed herein. The specification and examples are to be considered exemplary only, and the true scope and spirit of the invention are indicated by the following claims.

[0052] It should be understood that the present invention is not limited to the precise structure described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of the invention is limited only by the appended claims.

[0053] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation on the present invention. Any simple modifications, alterations, or equivalent structural changes made to the above embodiments based on the technical essence of the present invention shall still fall within the protection scope of the present invention.

Claims

1. A mixture of two opposite polarities for the separation and purification of components from waste black ladder-type explosives, characterized in that, This includes polar solvents for dissolving the cyclic trimethylenetrinitramine (RDX) component in spent black dynamite explosives and non-polar solvents for dissolving the trinitrotoluene (TNT) component in spent black dynamite explosives; The polarity of the polar solvent is 5.4 to 6.2; The polarity of the nonpolar solvent is 0 to 0.

1.

2. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The mass ratio of polar solvent to nonpolar solvent is equal to the mass ratio of cyclotrimethylenetrinitramine to trinitrotoluene in waste black dart explosive.

3. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The polar solvent is acetonitrile.

4. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The nonpolar solvent is n-pentane.

5. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The nonpolar solvent is cyclohexane.

6. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The nonpolar solvent is hexane.

7. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The polarity of the polar solvent is 6.

2.

8. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The polarity of the nonpolar solvent is 0.

9. The two opposite polarity mixture for the separation and purification of components from waste black ladder explosives according to claim 1, characterized in that, The polarity of the nonpolar solvent is 0.1.

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