CN116283458B - A kind of single substance purple smoke agent and preparation method thereof - Google Patents

Abstract

The invention discloses a single-substance purple smoke agent and a preparation method thereof. The smoke agent is a single-substance organic amine iodate salt, and the steps are: using an organic amine as a reducing agent and iodic acid as an oxidizing agent, dripping an aqueous solution of the organic amine into an iodic acid solution, and keeping the temperature at a certain temperature for a period of time to react, so as to obtain an organic amine iodate salt. The invention can utilize the characteristics of iodic acid easily forming a halogen bond and nitrogen in the organic amine providing a lone pair of electrons to form compounds with different iodic acid contents in the molecule, and can completely eliminate the problems of danger and uneven mixing of the composite component colored smoke agent in the mixing process. The obtained smoke agent can be detonated under external stimulation, has a certain output power, and can generate a large amount of purple smoke in the process of explosion and combustion, so it can be used as a purple smoke agent.

Description

A kind of single substance purple smoke agent and preparation method thereof

Technical Field

The invention belongs to energetic compounds, and in particular relates to a single substance purple smoke agent and a preparation method thereof.

Background Art

Smoke agents are a type of pyrotechnic agent that uses aerosol effects to produce special effects. They are widely used in military and civilian applications. In the military, smoke agents can be used to transmit signals and indicate tools during the day, and the smoke produced can also be used for photoelectric interference; in civilian applications, they can be used for film and television effects and entertainment.

Existing smoke agents are mostly composite components, mainly composed of oxidants, reducing agents and color dyes. However, during the mixing and preparation process of multi-component composite agents, they are prone to accidental ignition due to friction, which is dangerous, and the finished products are also uneven. Therefore, preparing pyrotechnic agents with uniform and simple components can not only reduce the preparation cost, but also reduce or eliminate the dangers brought about by the preparation process.

In addition, the oxidants in traditional colored smoke agents are mainly potassium nitrate, potassium chlorate, and potassium perchlorate with low decomposition temperatures, especially potassium chlorate, but the presence of chlorine brings certain harm to the environment. Reducing agents are mainly organic substances such as lactose, sucrose, and starch. The dyes widely used at present are mostly organic compounds such as azo and anthraquinone that are harmful to human health and carcinogenic, and have potential harm to the human body. Therefore, the research and development of simple preparation and green and environmentally friendly smoke agents are of great significance to the formulation of colored smoke agents in military and civilian use.

Summary of the invention

The purpose of the present invention is to provide a single substance purple smoke agent and a preparation method thereof, so as to reduce or eliminate the safety and uniformity problems existing in the preparation process of the composite color smoke agent under the condition that the contained components do not pollute the environment.

The technical solution of the present invention is: a single substance purple smoke agent, wherein the smoke agent is a single substance of organic ammonium iodate.

The preparation method of the above-mentioned single substance purple smoke agent comprises: using organic amine as a reducing agent and iodic acid as an oxidizing agent, dropping an aqueous solution of the organic amine into an iodic acid solution, and reacting at a certain temperature for a period of time to obtain an organic amine iodate.

Preferably, the organic amine is soluble in water, and the organic amine is preferably a primary amine or a tertiary amine with nitrogen exposed externally.

Specifically, the organic amine is any one of anhydrous ethylenediamine or triethylenediamine.

Preferably, the reaction is carried out in a solution state, that is, the organic amine is prepared into a solution and then added dropwise to the iodic acid solution.

Preferably, when the organic amine is ethylenediamine, the molar ratio of ethylenediamine to iodic acid is 1:2; when the organic amine is triethylenediamine, the molar ratio of triethylenediamine to iodic acid is 1:4.

Preferably, the aqueous solution of the organic amine is added dropwise to the iodic acid solution for 5 to 10 minutes.

Preferably, the reaction is kept at 50°C-75°C for more than 10 minutes.

Preferably, after the reaction is completed, the organic amine iodide is obtained by cooling and crystallizing by natural cooling, water cooling or refrigeration equipment.

Compared with the prior art, the present invention has the following significant advantages: (1) Simple preparation. The target product can be obtained by combining two raw materials in an aqueous solution without the need for mixing procedures. (2) Good safety. The obtained organic ammonium iodate can be realized by a one-step reaction in an aqueous solution, and the preparation process is safe. (3) Simple components. Multiple components such as oxidants, combustibles, and colored fuels are no longer required. The combustion of a single organic ammonium iodate can produce a strong purple smoke. (4) Compared with the existing colored smoke-generating agents, the organic ammonium iodate can not only produce purple smoke, but also play a large-scale sterilization role because the main component of the purple smoke is iodine vapor. (5) With the difference in the iodic acid content inside the molecule and the density of the formed charge, it exhibits the characteristics of smoke generation, gas generation, and explosives. Therefore, it can be used in the fields of ignition, gas generation, explosion work, fireworks, etc.

BRIEF DESCRIPTION OF THE DRAWINGS

Figure 1 is a comparison of the XRD patterns of ethylenediamine diiodate and raw material iodic acid.

FIG. 2 is a comparison diagram of XRD of triethylenediamine tetraiodate and raw material iodic acid.

Figure 3 is a photo of ethylenediamine diiodate burning and emitting smoke.

Figure 4 is a photo of triethylenediamine tetraiodate burning and fuming.

DETAILED DESCRIPTION

The following examples illustrate the present invention in more detail but are not intended to further limit the present invention.

The invention utilizes the characteristics of iodic acid easily forming halogen bonds and nitrogen in organic amine providing lone pair electrons to form compounds with different iodic acid contents in the molecule, and can completely eliminate the problems of danger and uneven mixing in the mixing process of the composite component colored smoke agent.

The inventors tried to use organic amines and iodic acid to prepare single energetic compounds, hoping to be able to be used in iodine-containing anti-biological warfare agents, thereby developing energetic compounds with simple preparation, high iodine content and high energy level. However, in the present application, the inventors unexpectedly found that the prepared organic amine iodide salts do not have the characteristics of detonating explosives, but can release a large amount of purple smoke during combustion and explosion, and can be used as purple smoke agents.

Embodiment 1:

Weigh 0.6g of anhydrous ethylenediamine, dissolve it in deionized water and dilute it to a 5% solution by mass. Weigh 53.7g of 6.5% iodic acid solution and place it in a jacketed reaction cup to form a bottom liquid. Turn on the stirring and heat the temperature to 70°C. Use a peristaltic pump to add the ethylenediamine solution to the combiner. The feeding is completed in 5 minutes and the reaction is kept warm for 10 minutes. Then cool to room temperature, filter, wash with anhydrous ethanol 2-3 times, and dry and weigh the obtained ethylenediamine diiodate. The combustion and smoke experiment is as follows

Weigh 1 g of ethylenediamine diiodate and place it in an iron shell with a diameter of 1.3 cm. Use a nitrocellulose strip to ignite it, and it can produce strong purple smoke. The specific smoke generation is shown in Figure 3.

Embodiment 2:

Weigh 1.12g of triethylenediamine, dissolve it in deionized water and dilute it to a solution with a mass fraction of 10%. Weigh 60g of iodic acid solution with a mass fraction of 12% and place it in a jacketed reaction cup to form a bottom liquid. At the same time, start stirring and heat the temperature to 70°C. Use a peristaltic pump to add the triethylenediamine solution to the combiner. The feeding is completed in 5 minutes and the reaction is kept warm for 10 minutes. Then evaporate the reaction liquid to 60ml at the combination temperature, cool it to room temperature, filter it, wash it with anhydrous ethanol 2-3 times, and dry and weigh the obtained triethylenediamine tetraiodate. The combustion and smoke experiment is as follows: weigh 1g of ethylenediamine diiodate and place it in an iron shell with a diameter of 1.3cm. Use a nitrocellulose strip to ignite it, which can produce strong purple smoke. The specific smoke situation is shown in Figure 4.

Embodiment 3:

In order to verify whether other oxygen-containing acids of ethylenediamine and triethylenediamine have smoke-generating properties, ethylenediamine nitrate, ethylenediamine perchlorate, ethylenediamine periodate, triethylenediamine nitrate, triethylenediamine perchlorate, and triethylenediamine periodate were prepared and ignition combustion experiments were carried out. The smoke generation conditions are shown in Table 1 below, wherein ethylenediamine diperiodate and triethylenediamine diperiodate are prepared by the same method as in the example, except that iodic acid is replaced by periodic acid.

Table 1

As shown in the table above, among the several organic amine oxyacid salts in the examples, only the organic amine iodate salt has the characteristic of purple smoke.

Embodiment 4:

Since ethylenediamine is a strong alkaline solution at room temperature, triethylenediamine and iodic acid were selected to be physically mixed for ignition experiment. The specific process is as follows: 0.28g of triethylenediamine and 1.76g of iodic acid were weighed, mixed evenly on weighing paper, and then the mixture was placed in an iron shell with a diameter of 1.3cm. Nitrocellulose strips were used for ignition. The results showed that the mixture of the two could not burn continuously and did not produce purple smoke.

From the above results, it can be seen that the elemental organic ammine iodate has a unique smoke-generating property. It can not only omit the physical mixing process of the oxidant, combustible agent and color dye in the traditional smoke-generating agent, but also can evenly mix the oxidant and the reductant at the molecular level to form the elemental organic ammine iodate.

Claims (8)

1. The use of an organic amine iodate simple substance as a purple smoke agent is characterized in that the organic amine iodate simple substance is ethylenediamine diiodinate or triethylenediamine tetraiodate.

2. The use according to claim 1, wherein the simple substance of organoamiodarone is prepared by the steps of: and (3) dropwise adding an aqueous solution of the organic amine into the iodic acid solution by taking the organic amine as a reducing agent and iodic acid as an oxidizing agent, and reacting for a period of time at a certain temperature in a heat preservation way to obtain the organic amine iodate.

3. The use according to claim 2, wherein the organic amine is soluble in water and is selected from primary amines and tertiary amines with nitrogen exposed to the outside.

4. The use according to claim 2, wherein the organic amine is any one of anhydrous ethylenediamine or triethylenediamine.

5. Use according to claim 2, wherein when the organic amine is ethylenediamine, the molar ratio of ethylenediamine to iodic acid is 1:2, and when the organic amine is triethylenediamine, the molar ratio of triethylenediamine to iodic acid is 1:4.

6. The use according to claim 2, wherein the aqueous solution of the organic amine is added dropwise to the iodic acid solution for a period of 5 to 10 minutes.

7. The use according to claim 2, wherein the reaction is carried out at a temperature of 50 ℃ to 75 ℃ for more than 10 minutes.

8. The method according to claim 4, wherein after the reaction is completed, the organic amine iodate is obtained by cooling crystallization by natural cooling, water cooling or refrigeration equipment.