Powder explosion inhibitor and preparation method thereof

Abstract

The application discloses a kind of powder explosion inhibitor and preparation method thereof, belong to the technical field of explosion inhibitor. Including the following steps: bivalent metal cation solution and trivalent metal cation solution are added to deionized water, heated and stirred, to obtain solution A;NaOH solution and NaH2PO4 solution are added to deionized water, heated and stirred, to obtain solution B;In nitrogen atmosphere, the solution B is added dropwise to solution A, keep pH value as 8-10 during the process of dropwise addition, after dropwise addition, reaction 12h;After reaction, washed with anhydrous ethanol, centrifuged, suction filtration, drying, can obtain powder explosion inhibitor.The explosion inhibitor has good explosion suppression effect, environment-friendly, economic and other characteristics, its preparation method is simple, little pollution, easy to realize magnitude production.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of explosion suppressants, and particularly relates to a powder explosion suppressant and a preparation method thereof. BACKGROUND

[0002] Metal dusts such as aluminum, magnesium and their alloys are widely used in the industries of metallurgy, aerospace, 3D printing, etc., and the risk of explosion exists in the links of dust production, dust collection and disposal. The metal dusts have the characteristics of easy spontaneous combustion, low ignition energy, large explosion power and various disaster factors. In recent years, accidents of fire and explosive have occurred frequently. In addition to the above characteristics, the self-oxygen system of fire and explosive makes it more dangerous. Once an accident occurs, it will cause serious personnel casualties, economic losses and adverse social impacts.

[0003] Dust explosion has become an important supervision field for preventing and controlling major production safety accidents, and metal dust explosion has become the top priority of various dust explosion accident prevention. The importance of explosive safety production is also increasing. At present, the development of explosion suppression technology is insufficient, and there is still a significant gap in the overall technical level of metal dust explosion accident and fire and explosive production accident prevention compared with developed countries, which seriously restricts the healthy development of safety production.

[0004] Today's powder explosion suppressants are single in form and low in efficiency, and there is a lack of efficient, environmentally friendly and economical explosion suppressants. At the same time, the existing new powder explosion suppressants also need to be improved. SUMMARY

[0005] In view of the above technical problems, the application provides a powder explosion suppressant and a preparation method thereof. The explosion suppressant has the characteristics of good explosion suppression effect, environmental friendliness and economy, and the preparation method is simple in operation, small in pollution and easy to realize mass production.

[0006] To achieve the above purpose, the application provides the following technical solutions.

[0007] A preparation method of a powder explosion suppressant comprises the following steps:

[0008] A divalent metal cation solution and a trivalent metal cation solution are added to deionized water, heated and stirred to obtain solution A;

[0009] NaOH solution and NaH2PO4 solution are added to deionized water, heated and stirred to obtain solution B;

[0010] In a nitrogen atmosphere, the solution B is added dropwise to the solution A, the pH value is maintained at 8-10 during the dropwise addition, and the reaction is carried out for 8-12 hours after the dropwise addition is completed;

[0011] After the reaction is completed, the powder explosion suppressant is obtained by washing with anhydrous ethanol, centrifugation, suction filtration and drying.

[0012] Further, the volume ratio of the divalent metal cation solution and the trivalent metal cation solution is (3-5) : 1.

[0013] Further, the divalent metal cation is Mg 2+ , Co 2+ , Fe 2+ or Ni 2+ ; and the trivalent metal cation is Al 3+ or Fe 3+ .

[0014] Further, the temperature of the heating and stirring is 70℃.

[0015] Further, the volume ratio of the NaOH solution and the NaH2PO4 solution is 4:1.

[0016] The application further provides a powder explosion inhibitor prepared by the preparation method.

[0017] The application further provides an application of the powder explosion inhibitor as an explosion suppression material.

[0018] Further, the use concentration of the powder explosion inhibitor is 300-600g / m 3 .

[0019] Further, the use concentration of the powder explosion inhibitor is 600g / m 3 .

[0020] Compared with the prior art, the application has the following advantages and technical effects:

[0021] (1) The powder explosion inhibitor prepared by the application has better effect than the traditional explosion inhibitor, has physical and chemical synergistic explosion suppression effect, and has superior explosion suppression performance;

[0022] (2) The application has the characteristics of environmental friendliness and economic efficiency.

[0023] (3) The preparation method is simple, the raw materials are cheap and easy to obtain, and the mass production can be easily realized. BRIEF DESCRIPTION OF DRAWINGS

[0024] The accompanying drawings, which form a part of this application, are included to provide a further understanding of the application and are incorporated in and constitute a part of this application. The embodiments illustrated in the drawings are provided to explain the present application and are not intended to limit the present application. In the drawings:

[0025] Figure 1 SEM image of the powder explosion inhibitor prepared in Example 1;

[0026] Figure 2 XRD image of the powder explosion inhibitor prepared in Example 1;

[0027] Figure 3 Figure for the relationship between the concentration of aluminum powder and the explosion pressure;

[0028] Figure 4 Figure for the relationship between the concentration of the powder explosion inhibitor prepared in Example 1 and the explosion pressure;

[0029] Figure 5 Figure for the relationship between the different injection time of the new powder explosion inhibitor prepared in Example 1 and the explosion pressure;

[0030] Figure 6 Figure for the relationship between the concentration of different explosion inhibitors and the explosion pressure;

[0031] Figure 7 Figure for the relationship between different concentrations of Mg(OH)2 and the explosion pressure. DETAILED DESCRIPTION

[0032] Various exemplary embodiments of the present application will now be described in detail, which should be considered to be illustrative of certain aspects, features and embodiments of the present application, but not a limitation thereof.

[0033] It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the present application. Additionally, the use of the term "about" in relation to a value or a range of values is intended to include each individual intermediate value and each smaller range that falls within the range of values. The upper and lower limits of these smaller ranges can be included or excluded from the range.

[0034] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application, preferred methods and materials are described. All publications mentioned in this specification are herein incorporated by reference to disclose and describe the methods and / or materials in connection with which the publications are cited. The citation of any reference in this specification is not intended as an admission that the reference is prior art, but rather that the reference is part of the technical literature that is relevant to A person of ordinary skill in the art.

[0035] Many modifications and variations of this application specification can be made in the light of the above teachings without departing from the spirit or ambit of the application. Other implementations of the application will be apparent to those skilled in the art from consideration of the specification and practice of the application. The specification and examples are illustrative only.

[0036] The embodiment of the present application discloses a preparation method of a powder explosion inhibitor, comprising the following steps:

[0037] The divalent metal cation solution and the trivalent metal cation solution are added into deionized water, heated and stirred to obtain solution A;

[0038] The NaOH solution and the NaH2PO4 solution are added into deionized water, heated and stirred to obtain solution B;

[0039] The solution B is added dropwise into the solution A under a nitrogen atmosphere, the pH value is kept at 8-10 during the dropwise addition, and the reaction is carried out for 8-12 hours after the dropwise addition is completed.

[0040] After the reaction is completed, the powder explosion inhibitor is obtained by washing with anhydrous ethanol, centrifugation, suction filtration and drying.

[0041] In some preferred embodiments, the volume ratio of the divalent metal cation solution to the trivalent metal cation solution is (3-5) : 1, such as 3:1, 4:1 or 5:1.

[0042] In some preferred embodiments, the divalent metal cation is Mg 2+ , Co 2+ , Fe 2+ or Ni 2+ ; preferably Mg 2 + ; the trivalent metal cation is Al 3+ or Fe 3+ , preferably Al 3+ . The salt for providing the divalent metal cation can be a magnesium-containing salt such as Mg(NO3)2, MgCl2, etc.; the salt for providing the trivalent metal cation can be an aluminum-containing salt such as Al(NO3)3, AlCl3, etc.

[0043] In some preferred embodiments, the temperature of the heating and stirring is 70°C.

[0044] In some preferred embodiments, the volume ratio of the NaOH solution to the NaH2PO4 solution is 4:1.

[0045] The powder explosion inhibitor prepared by the above preparation method can be used as an explosion suppression material, has physical and chemical synergistic explosion suppression effect, and has superior explosion suppression performance. When the use concentration of the powder explosion inhibitor is 300-600 g / m 3 , the explosion suppression effect is superior to that of a conventional explosion inhibitor, and therefore in some preferred embodiments, the use concentration of the powder explosion inhibitor is 300-600 g / m 3 ; in more preferred embodiments, the use concentration of the powder explosion inhibitor is 600 g / m 3 .

[0046] Among the numerous explosion prevention and control technologies, explosion suppression technology is considered as the most potential means to reduce or even eliminate the explosion hazards, which can detect and prevent the combustion from turning into explosion in the early stage of combustion. The metal layer plates of the powder explosion suppressant of the present application carry a large number of hydroxyl groups. When the metal layer plates are in the explosion field, the ordered layered structure is destroyed and the hydroxyl groups of the metal layer plates have excellent physical heat absorption and cooling effect through evaporation. At the same time, the metal layer plates are composed of metal ions of M 2+ and M 3+ . The metal ions can generate metal oxides by reacting with oxygen radicals in the explosion field, interrupt the explosion chain reaction and further reduce the explosion hazards. Sodium bicarbonate and ammonium dihydrogen phosphate in the traditional dry powder inhibitor have excellent chemical inhibition effect. Therefore, the bicarbonate and dihydrogen phosphate are inserted into the metal layer plates to form a stable layered structure. The combination of the hydroxyl group evaporation heat absorption of the layered structure, the heat absorption of the collapsed metal layer plates, the oxygen deprivation of the layered structure and the neutralization of the free radicals by the anions between the layers can achieve fast physical heat absorption and cooling, strong chemical inhibition and multi-dimensional explosion suppression.

[0047] The powder explosion suppressant of the present application enters the core area of the explosion reaction in the form of powder. With the occurrence of the collapse of the layered structure, the separation of the components, the evaporation of the liquid phase, the thermal decomposition of the multiple phases and the interaction with the flame radicals, the physical heat absorption explosion suppression of the collapsed layered structure, the chemical free radical explosion suppression of the anions between the layers and the explosion suppression of the metal ions of the layered structure are involved. The explosion suppression material has the synergistic effect of multi-dimensional explosion suppression of physical heat absorption and chemical radical inhibition.

[0048] As to the terms such as “comprising”, “including”, “having”, “containing” and the like used in the present application, they are all open terms, i.e. meaning containing but not limited to.

[0049] The “room temperature” described in the present application means 20-30℃ unless otherwise specified.

[0050] The raw materials used in the present application are all purchased from the market.

[0051] The technical solutions of the present application are further illustrated by the following examples.

[0052] Example 1

[0053] 1) Mg(NO3)2·6H2O was dissolved in water to prepare a Mg(NO3)2 solution, Al(NO3)3·9H2O was dissolved in water to prepare an Al(NO3)3 solution, and the two were mixed in a volume ratio of 3:1 and dissolved in deionized water, so that the concentration of Mg 2+ was 0.3M and the concentration of Al 3+ was 0.1M. The solution was stirred uniformly at 70℃ to obtain solution A;

[0054] 2) NaOH solution and NaH2PO4 solution are added into deionized water in a volume ratio of 4:1, so that the concentration of NaOH solution in the solution is 0.8M and the concentration of NaH2PO4 solution is 0.1M, and the solution is stirred uniformly at 70°C to obtain solution B;

[0055] 3) Solution B is added dropwise into solution A under a nitrogen atmosphere, and the pH value is kept at 10 during the dropwise addition, and the reaction is continuously carried out for 12h after the dropwise addition is completed; after the reaction is completed, the powder is washed with 200mL of anhydrous ethanol, centrifuged, and suction filtered, and the three steps of washing, centrifuging and suction filtering are repeated three times, and then the powder is dried for 12h to obtain the powder explosion inhibitor (LDHs, hydrotalcite).

[0056] Figure 1 The SEM image of the powder explosion inhibitor prepared in Example 1 is shown in Fig. 1. Figure 1 As can be seen from Fig. 1, the powder explosion inhibitor prepared by the method of Example 1 has a layered structure, and H2PO4 - ions have successfully entered the interlayer.

[0057] Figure 2 The XRD image of the powder explosion inhibitor prepared in Example 1 is shown in Fig. 2. Figure 2 As can be seen from Fig. 2, the material shows typical LDHs diffraction peaks, and the (003), (006) and (009) crystal face diffraction peaks appear at 11.69°, 23° and 35° respectively, and correspondingly, d(003) is 7.56, which is different from the 0.76-0.78(CO3 2- intercalation) recorded in the prior art, indicating that the H2PO4 - ions with a larger size and a tetrahedral structure have entered the LDH interlayer to form Mg-Al-H2PO4. - The intensity of the (009) crystal face diffraction peak is significantly enhanced, indicating that H2PO4 - ions have successfully intercalated into the interlayer. - The above, the present application has prepared H2PO4 2+ intercalated layered structure, i.e. Mg-Al-H2PO4.

[0058] Example 2

[0059] 1) Co(NO3)2·6H2O is dissolved in water to prepare a Co(NO3)2 solution, Fe(NO3)3·9H2O is dissolved in water to prepare a Fe(NO3)3 solution, and the two are mixed in a volume ratio of 3:1 and dissolved in deionized water, so that the concentration of Co 2+ is 0.3M and the concentration of Fe3+ The concentration is 0.1M, and the solution A is obtained by stirring uniformly at 70°C;

[0060] 2) NaOH solution and NaH2PO4 solution are added into deionized water at a volume ratio of 4:1, so that the concentration of NaOH solution in the solution is 0.8M, and the concentration of NaH2PO4 solution is 0.1M, and the solution B is obtained by stirring uniformly at 70°C;

[0061] 3) Solution B is added dropwise into solution A under a nitrogen atmosphere, and the pH value is kept at 10 during the dropwise addition, and the reaction is continuously reacted for 12h after the dropwise addition is completed; after the reaction is completed, 200mL of anhydrous ethanol is used for washing, centrifugation, and suction filtration, and the three steps of washing, centrifugation, and suction filtration are repeated three times, and then the powder explosion inhibitor is obtained after drying for 12h.

[0062] Application example

[0063] 1. Pure aluminum powder explosion

[0064] The 20L spherical explosion device is used to test the explosion pressure generated by aluminum powder with different concentrations, and the specific experimental method is as follows: 200g / m 3 , 300g / m 3 , 400g / m 3 , 500g / m 3 , 600g / m 3 , 700g / m 3 , and 800g / m 3 of aluminum powder are respectively put into a 20L sphere for testing, and the average value obtained by repeating the experiment three times is recorded as the explosion pressure of the aluminum powder.

[0065] Figure 3 is the relationship between the aluminum powder concentration and the explosion pressure. It can be found that the explosion pressure is the largest when the aluminum powder concentration is 700g / m 3 , there is obvious aluminum powder residue in the experimental container when the aluminum powder concentration is 800g / m 3 , and a small peak of pressure is reached when the aluminum powder concentration is 400g / m 3 . When the aluminum powder concentration is 700g / m 3 , the explosion pressure is large, the temperature is high, and there is aluminum powder residue, and the experimental risk is relatively large. Therefore, the aluminum powder concentration of 400g / m 3 is selected as the research object to study the explosion suppression effect of the explosion suppressant prepared in Example 1.

[0066] 2. Powder explosion inhibitor inhibiting aluminum powder explosion

[0067] The 20L spherical explosion device is used to test the influence of different concentrations of powder explosion inhibitor as explosion inhibitor on aluminum powder explosion, and the specific experimental method is as follows: the aluminum powder concentration is set to 400g / m 3, respectively, using the powder explosion inhibitor with the concentration of 0 (i.e. without adding the explosion inhibitor), 150, 300, 450, 600 g / m 3 . Other modes are the same as above.

[0068] Figure 4 The relationship diagram between the concentration of the powder explosion inhibitor prepared in Example 1 and the explosion pressure can be seen that the powder explosion inhibitor prepared in Example 1 has the inhibition effect on the aluminum powder explosion, and the best explosion inhibition effect is obtained when the concentration is 600 g / m 3 , and the maximum explosion pressure of the aluminum powder explosion is reduced from 0.955 MPa to 0.676 MPa.

[0069] 3. Inhibition of the explosion of the aluminum-containing explosive by the powder explosion inhibitor

[0070] The influence of the spraying time of the new powder explosion inhibitor on the explosion of the aluminum-containing explosive is tested by using the 20L spherical explosion device, and the specific test method is as follows: the concentration of the explosive is set to 300 g / m 3 , the concentration of the explosion inhibitor is set to 300 g / m 3 , and the explosion inhibitor is sprayed at 10 ms, 20 ms, and 30 ms after the explosion of the explosive, respectively, and the average value obtained by repeating the experiment three times is recorded as the relationship between the different spraying times of the new explosion inhibitor and the explosion pressure.

[0071] Figure 5 The relationship diagram between the different spraying times of the new powder explosion inhibitor prepared in Example 1 and the explosion pressure can be seen that the new powder explosion inhibitor prepared in Example 1 has the inhibition effect on the aluminum powder explosion, and the best explosion inhibition effect is obtained when the explosion inhibitor is sprayed at 10 ms after the explosion of the aluminum powder, and the explosive is basically completely inhibited.

[0072] 4. Comparison of the inhibition of the aluminum powder explosion by the powder explosion inhibitor and the traditional explosion inhibitor

[0073] The influence of different kinds of explosion inhibitors on the aluminum powder explosion is tested by using the 20L spherical explosion device to verify the effect of the powder explosion inhibitor prepared in Example 1. The specific test method is as follows: the concentration of the aluminum powder is set to 400 g / m 3 , and the concentration of the explosion inhibitor is set to 0 (i.e. without adding the explosion inhibitor), 150, 300, 450, 600 g / m 3 . Other modes are the same as 2.

[0074] The traditional explosion inhibitors are as follows:

[0075] 1) NaHCO3, from Guangzhou Keqi Chemical Technology Co., Ltd.;

[0076] 2) NaH2PO4, from Guangzhou Keqi Chemical Technology Co., Ltd.

[0077] Figure 6The concentration of different explosion suppressants and the relationship diagram of explosion pressure can be seen from the figure, under the same working condition, the explosion suppression effect of the explosion suppressant prepared in example 1 is better than that of the traditional explosion suppressant, and the effect is more obvious with the increase of the concentration of the explosion suppressant.

[0078] Comparative example 1

[0079] The difference from example 1 is that the Mg (NO3) 2 solution is replaced by the Mg (OH) 2 solution. The Mg (OH) 2 has metal cation oxygen, and water is also easy to form in the reaction by heat absorption to suppress explosion, but there is no layered structure.

[0080] The 20L spherical explosion device is used to test the influence of different kinds of explosion suppressants on the explosion of aluminum powder, and the effect of the powder explosion suppressant prepared in example 1 is verified. The specific test method is as follows: the concentration of aluminum powder is set to 400g / m 3 , the concentration of explosion suppressant is set to 0 (i.e. no explosion suppressant is added), 150, 300, 450, 600g / m 3 . Other modes are the same as 2.

[0081] Figure 7 The concentration of different explosion suppressants and the relationship diagram of explosion pressure can be seen from the figure, under the same working condition, the explosion suppression effect of the explosion suppressant prepared in example 1 is better than that of the traditional explosion suppressant, and the effect is more obvious with the increase of the concentration of the explosion suppressant.

[0082] It is found that the new powder explosion suppressant prepared in the application has a layered structure, and the explosion suppression effect is better than that of other chemical explosion suppressants without a layered structure, because the layered structure will collapse in the explosion field, and this phenomenon will compete with the explosion object for oxygen in the explosion field, so as to inhibit the explosion reaction.

[0083] The above is only a preferred specific embodiment of the present application, but the protection scope of the present application is not limited thereto, any skilled person in the art can easily think of changes or replacements within the technical range disclosed in the present application, which should be covered in the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A method for preparing a powder explosion suppressant, characterized by, The method comprises the following steps: adding a divalent metal cation solution and a trivalent metal cation solution into deionized water, heating and stirring to obtain solution A; adding a NaOH solution and a NaH2PO4 solution into deionized water, heating and stirring to obtain solution B; adding the solution B into the solution A drop by drop under a nitrogen atmosphere, keeping the pH value at 8-10 during the dropwise addition, and reacting for 8-12 hours after the dropwise addition is completed; after the reaction is completed, washing with anhydrous ethanol, centrifuging, suction filtering and drying to obtain the powder explosion inhibitor; the divalent metal cation solution is a Mg(NO3)2, MgCl2 or Co(NO3)2 solution; and the trivalent metal cation solution is an Al(NO3)3, AlCl3 or Fe(NO3)3 solution.

2. The method of claim 1, wherein the powder explosion suppression agent is prepared by the steps of: the volume ratio of the divalent metal cation solution and the trivalent metal cation solution is (3-5):

1.

3. The method of claim 1, wherein the powder explosion suppression agent is prepared by the steps of: the temperature of the heating and stirring is 70℃.

4. The method of claim 1, wherein the powder explosion suppression agent is prepared by the steps of: the volume ratio of the NaOH solution and the NaH2PO4 solution is 4:

1.

5. A powder explosion inhibitor prepared by the preparation method of any one of claims 1-4.

6. Application of the powder explosion inhibitor of claim 5 as an explosion suppression material.

7. Use according to claim 6, characterized in that, The using concentration of the powder explosion inhibitor is 300-600 g / m 3 .

8. Use according to claim 7, characterized in that, The using concentration of the powder explosion inhibitor is 600g / m 3 .

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