Mixed solution with two opposite polarities for separating and purifying waste black ladder explosive components

Abstract

The invention discloses a mixed solution with two opposite polarities for separating and purifying components of waste black ladder explosives, which comprises a polar solvent for dissolving a cyclic trimethylene trinitramine (RDX) component in the waste black ladder explosives and a non-polar solvent for dissolving a trinitrotoluene (TNT) component in the waste black ladder explosives, according to the mixed solution, two opposite-polarity mixed solutions are adopted to separate and purify components of the waste black ladder explosive, so that RDX and TNT in the black ladder explosive are respectively dissolved in two incompatible reverse-polarity solvents, the two solvents are conveniently separated through a liquid separator subsequently, and then RDX, TNT and the corresponding solvents are respectively recovered in a reduced pressure distillation manner; the purity of the obtained RDX and TNT can reach 99.9% or above, and the two reverse polar solvents can be repeatedly used for multiple times.

Description

Technical Field

[0001] The invention belongs to the technical field of resource recycling and utilization, and relates to a two-phase mixed liquid with opposite polarities used for separating and purifying components of waste black ladder explosives. Background Art

[0002] Resource recycling is a strategic emerging industry that benefits the country and the people. The objects of resource recycling cover all equipment and materials with large stocks and high values, including a large number of retired waste explosives. Black ladder explosives, as a type of mixed explosives produced and equipped in large quantities in the early days of my country, have been retired and scrapped as their service life expires. Black ladder explosives are a series of two-component mixed explosives designed by my country in the last century based on the Soviet Union's 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 explosives products include black ladder 50 / 50 (the mass ratio of RDX and TNT is 50:50), black ladder 60 / 40 (the mass ratio of RDX and TNT is 60:40), black ladder 40 / 60 (the mass ratio of RDX and TNT is 40:60), etc. The preparation process of this type of explosive is to first heat TNT to make it completely melt, then add RDX into it, and stir to make it evenly mixed. Then it can be directly loaded into projectiles or made into thin sheets and bagged for standby use.

[0003] For a large number of retired waste black ladder explosives, the traditional disposal method is direct incineration, which not only causes environmental pollution, but also wastes RDX and TNT in black ladder explosives. In order to separate and recover the energetic components in black ladder explosives, Academician Wang Zeshan reported the use of solvents such as benzene and toluene to dissolve TNT in black ladder explosives, and then filter to obtain insoluble RDX. Although this process can extract RDX from black ladder explosives, there is still a solution containing TNT on the surface of the filtered RDX, resulting in the RDX purity not meeting the national military standard requirements. Summary of the invention

[0004] The purpose of the present invention is to overcome the disadvantages of the above-mentioned prior art and provide a two-way mixed liquid with opposite polarity for separating and purifying waste black ladder explosive components. The mixed liquid uses the two-way mixed liquid with opposite polarity to separate and purify the waste black ladder explosive components, so that RDX and TNT in the black ladder explosive are respectively dissolved in two mutually incompatible opposite polarity solvents, so that the two solvents can be separated by a liquid separator, and then RDX, TNT and the corresponding solvent are respectively 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 many times.

[0005] To achieve the above-mentioned purpose, the present invention discloses a two-phase mixed liquid with opposite polarity for separating and purifying the components of waste black explosives, comprising a polar solvent for dissolving the cyclotrimethylene trinitramine (RDX) component in the waste black explosives and a non-polar solvent for dissolving the trinitrotoluene (TNT) component in the waste black explosives.

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

[0007] The polarity of the non-polar solvent is 0 to 0.1.

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

[0009] Furthermore, the polar solvent is acetonitrile.

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

[0011] Furthermore, the non-polar solvent is cyclohexane.

[0012] Furthermore, the non-polar solvent is hexane.

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

[0014] Furthermore, the polarity of the non-polar solvent is 0.

[0015] Furthermore, the polarity of the non-polar solvent is 1.

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

[0017] The two opposite polarity mixed liquids for separation and purification of waste black ladder explosive components described in the present invention include a polar solvent for dissolving the cyclotrimethylene trinitramine (RDX) component in the waste black ladder explosive and a non-polar solvent for dissolving the trinitrotoluene (TNT) component in the waste black ladder explosive during specific operation, and can separate and purify the components of the waste black ladder explosive, and obtain the purity of RDX and TNT after separation and purification ≥ 99.9%, which meets the purity requirements of the national military standard for these two energetic materials. The present invention realizes the directional dissolution of the two components of the black ladder explosive by controlling the polarity of the selected two-phase solvent and its polarity difference, and only dissolves one energetic material component in each solvent system, so that the purity of the recovered energetic material can be guaranteed. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The accompanying drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the accompanying drawings:

[0019] Figure 1 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 the present invention;

[0021] Figure 3 This is the process diagram for separating components of black ladder explosives. DETAILED DESCRIPTION

[0022] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] In the description of the present invention, it should be understood that the terms “include” and “comprises” indicate the presence of described features, wholes, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, wholes, steps, operations, elements, components and / or collections thereof.

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

[0025] It should be further understood that the term "and / or" used in the present specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes these combinations. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in the present invention generally indicates that the associated objects are in an "or" relationship.

[0026] It should be understood that, although the terms first, second, third, etc. may be used to describe preset ranges, etc. in the embodiments of the present invention, these preset ranges should not be limited to these terms. These terms are only used to distinguish preset ranges from each other. 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] The word "if" as used herein may be interpreted as "at the time of" or "when" or "in response to determining" or "in response to detecting", depending on the context. Similarly, the phrases "if it is determined" or "if (stated condition or event) is detected" may be interpreted as "when it is determined" or "in response to determining" or "when detecting (stated condition or event)" or "in response to detecting (stated condition or event)", depending on the context.

[0028] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. The components of the embodiments of the present invention described and shown in the drawings here can usually be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0029] Various structural schematic diagrams of the embodiments disclosed in the present invention are shown in the accompanying drawings. These figures are not drawn to scale, and some details are magnified and some details may be omitted for the purpose of clear expression. The shapes of various regions and layers shown in the figures and the relative sizes and positional relationships therebetween are only exemplary, and may deviate in practice due to manufacturing tolerances or technical limitations, and those skilled in the art may additionally design regions / layers with different shapes, sizes, and relative positions according to actual needs.

[0030] The design principle of the present invention is:

[0031] The methods for separating the components of black ladder explosives reported so far all use solvents to dissolve TNT, and then filter the precipitated RDX. Since there is a solution containing TNT remaining on the surface of RDX, the surface of the RDX obtained after drying is still covered with a layer of TNT. Therefore, the purity of the obtained RDX does not meet the requirements of the national military standard.

[0032] In view of the shortcoming that the existing separation methods cannot obtain high-purity RDX, the present invention aims to separate the two components of black ladder explosive by adopting two opposite polarity mixed liquids, dissolving RDX and TNT respectively using two-phase solvents, and then separating the two-phase solvents to achieve separation and purification of RDX and TNT in black ladder explosive.

[0033] By screening the polarity of two-phase solvents and controlling their polarity difference, a mixed solution of two opposite polarities is obtained. The solution can be directly used to dissolve and separate RDX and TNT in black ladder explosives. After the dissolution is completed, the immiscible two-phase solvents are separated by a liquid separator to obtain solutions for dissolving RDX and dissolving TNT, respectively. Then, the separated energetic materials and corresponding solvents are recovered by vacuum distillation. The purity of RDX and TNT precipitated in their respective solvents is further improved, which can meet the requirements for product purity stipulated in the national military standard.

[0034] Based on the above, the two oppositely polar mixed liquids used for separation and purification of waste black ladder explosive components described in the present invention include a polar solvent for dissolving cyclotrimethylene trinitramine (RDX) components in waste black ladder explosives and a non-polar solvent for dissolving trinitrotoluene (TNT) components in waste black ladder explosives.

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

[0036] Embodiment 1

[0037] The two opposite polar mixed liquids for separation and purification of waste black ladder explosive components of the present 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 object for separation and purification is black ladder 50 / 50 explosive.

[0038] The separation and purification process is as follows: 1) preparing two mixed solutions of opposite polarity: at room temperature, weighing 50 ml of acetonitrile and 50 ml of normal pentane respectively, and adding the two solvents into a flask with stirring; 2) separating the black ladder 50 / 50 explosive: starting stirring at 100 r / min, slowly adding 50 g of the black ladder explosive into the beaker, and continuing stirring for 5 to 10 minutes after the black ladder explosive is added, and stopping stirring after the black ladder explosive is completely dissolved, and separating the two phases of the solution by using a liquid separator after the solution system is static and stratified; 3) purifying and recovering RDX and TNT samples: using a vacuum distillation device to vacuum distill the solvents for dissolving RDX and dissolving TNT respectively, obtaining purified RDX and TNT while realizing the recovery and reuse of acetonitrile and normal pentane solvents.

[0039] Performance Testing:

[0040] a) Purity: tested by high performance liquid chromatography (HPLC);

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

[0042] Embodiment 2

[0043] The two opposite polar mixed liquids for separation and purification of waste black ladder explosive components of the present invention include 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 object for separation and purification is black ladder 60 / 40 explosive.

[0044] Embodiment 3

[0045] The two opposite polar mixed liquids for separation and purification of waste black ladder explosive components of the present invention include acetonitrile and cyclohexane, wherein the polarity of hexane is 0.06, the polarity of acetonitrile is 6.2, the mass ratio of acetonitrile to n-pentane is 40:60, and the object 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 of the present 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 the present invention is as follows Figure 1 shown.

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

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

[0052] It should be understood that the present invention is not limited to the exact construction that has been described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the present invention is limited only by the appended claims.

[0053] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent structural change made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A two-phase mixed liquid with opposite polarity for separating and purifying components of waste black ladder explosives, characterized in that: The invention comprises a polar solvent for dissolving cyclotrimethylene trinitramine (RDX) component in waste black ladder explosive and a non-polar solvent for dissolving trinitrotoluene (TNT) component in waste black ladder explosive.

2. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The polarity of the polar solvent is 5.4 to 6.2; The polarity of the non-polar solvent is 0 to 0.

1.

3. The two opposite polarity mixed liquids for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The mass ratio of the polar solvent to the non-polar solvent is equal to the mass ratio of cyclotrimethylene trinitramine to trinitrotoluene in the waste black ladder explosive.

4. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The polar solvent is acetonitrile.

5. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The non-polar solvent is n-pentane.

6. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The non-polar solvent is cyclohexane.

7. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The non-polar solvent is hexane.

8. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The polarity of the polar solvent is 6.

2.

9. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The polarity of the non-polar solvent is 0.

10. The two opposite polarity mixed liquid for separation and purification of waste black ladder explosive components according to claim 1, characterized in that: The polarity of the non-polar solvent is 1.

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