Inert hydroxyl-terminated polybutadiene composite solid propellant and preparation method thereof

Abstract

The invention discloses an inert hydroxyl-terminated polybutadiene composite solid propellant and a preparation method thereof, and relates to the field of solid propellants, the inert hydroxyl-terminated polybutadiene composite solid propellant comprises the following raw materials by weight: 40-60 parts of an inert filler, 10-25 parts of metal powder, 15-30 parts of an adhesive, 2-4 parts of a plasticizer, 1-3 parts of a curing agent, 0.2-0.5 part of a bonding agent and 0.2-1 part of an anti-aging agent; wherein the preparation method of the inert filler is as follows; the preparation method comprises the following steps: ultrasonically dispersing nanofiber particles in a mixed solution of ethanol and ammonia water, continuously dropwise adding tetraethyl orthosilicate and 3-glycidyl ether oxypropyl triethoxy silane for reaction, then performing centrifugal drying to obtain rod-point particles, and then mixing the rod-point particles with fine sand to obtain the composite material. According to the invention, the fine particles with rod-point structures are added into the fine sand, so that the surface of the fine sand has a micro-nano concave-convex structure, the fine sand has excellent hydrophobic performance, and the moisture absorption performance of the slurry is reduced; and the density of the propellant can be adjusted by changing the content of the fine sand, so that the requirements of inert propellants with different density requirements are met.

Description

Technical Field

[0001] The invention relates to the field of solid propellants, and in particular to an inert butyl hydroxyl composite solid propellant and a preparation method thereof. Background Art

[0002] During the development of solid rocket engines, in order to reduce the danger of the test, non-combustible inert propellants are needed instead of real propellants. Inert propellants are widely used in the full nitrogen docking and debugging measurements of solid engines, environmental experiments of engines, such as shock, vibration, overload and other tests, as well as training, parades, exhibitions and other occasions.

[0003] At present, most inorganic substances added to inert propellants are metal chlorides (such as NaCl salt). During use, there are mainly the following problems: (1) Metal chlorides are easy to absorb moisture, and the HTPB / TDI curing system in the propellant components is sensitive to moisture. Improper handling of metal chloride moisture during the propellant manufacturing process can easily cause the propellant slurry process performance to deteriorate, affect the pouring of the propellant slurry, and cause pores to form inside the propellant grain. (2) During the storage process of inert propellants using metal chlorides, if they are exposed to air or the engine seal is not in place, the metal chlorides in the inert medicine are easy to absorb moisture, causing "water seepage" on the surface of the grain, affecting the mechanical properties of the grain. Summary of the invention

[0004] The purpose of the present invention is to solve at least one of the technical problems existing in the prior art and to provide an inert butyl hydroxyl composite solid propellant and a preparation method thereof.

[0005] The technical solution of the present invention is as follows:

[0006] An inert hydroxybutyrate composite solid propellant comprises the following raw materials in parts by weight: 40-60 parts of an inert filler, 10-25 parts of a metal powder, 15-30 parts of an adhesive, 2-4 parts of a plasticizer, 1-3 parts of a curing agent, 0.2-0.5 parts of a bonding agent, and 0.2-1 parts of an antioxidant;

[0007] The preparation method of the inert filler is as follows:

[0008] The nanofiber particles are ultrasonically dispersed in a mixed solution of ethanol and ammonia water, tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are continuously added dropwise for reaction, and then centrifugally dried to obtain rod-point particles, which are then mixed with fine sand to obtain the product.

[0009] As a preferred embodiment of the present invention, the nanofiber particles are nano-attapulgite fibers or calcium carbonate whiskers.

[0010] As a preferred embodiment of the present invention, the volume ratio of ethanol to aqueous ammonia is 3-8:1.

[0011] As a preferred embodiment of the present invention, the concentration of the nanofiber particles is 10-50 g / L.

[0012] As a preferred embodiment of the present invention, the addition amounts of tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are 30-80 ml / L and 5-8 ml / L respectively.

[0013] As a preferred embodiment of the present invention, the mass ratio of the rod point particles to the fine sand is 1-5:20.

[0014] As a preferred embodiment of the present invention, the metal powder is aluminum powder;

[0015] The binder is hydroxyl-terminated polybutadiene;

[0016] The plasticizer is diisooctyl sebacate;

[0017] The curing agent is toluene diisocyanate;

[0018] The bonding agent is tris-(2-methylaziridinyl)phosphine oxide;

[0019] The antioxidant is N,N-diphenyl-p-phenylenediamine.

[0020] As a preferred embodiment of the present invention, the particle size of the fine sand is 10-20 meshes.

[0021] A method for preparing an inert hydroxybutyric acid composite solid propellant comprises the following steps:

[0022] S1: premixing metal powder, adhesive, plasticizer, bonding agent and antioxidant to obtain slurry;

[0023] S2: adding an inert filler to the slurry, mixing well, then adding a curing agent, injecting into an engine housing for curing, and demoulding to obtain the product.

[0024] As a preferred embodiment of the present invention, the premixing temperature is 40-60° C., and the premixing time is 20-40 min.

[0025] The beneficial effects of the present invention are:

[0026] The inert butyl hydroxyl composite solid propellant of the present invention has excellent hydrophobicity by adding tiny particles of a rod-point structure into fine sand, so that the surface of the fine sand has a micro-nano concave-convex structure, thereby reducing the hygroscopicity of the drug slurry and solving the problem of "water seepage" of the traditional drug column; and the rod-point structure can improve the mechanical strength of the drug column and reduce the generation of pores and cracks; in addition, in specific applications, the density of the propellant can be adjusted by changing the fine sand content to meet the needs of inert propellants with different density requirements. DETAILED DESCRIPTION

[0027] The embodiments of the present invention are described in detail below. The embodiments described below are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention. If no specific techniques or conditions are specified in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. The reagents or instruments used that do not specify the manufacturer are all conventional products that can be obtained commercially.

[0028] Example 1

[0029] An inert hydroxybutyrate composite solid propellant comprises the following raw materials in parts by weight: 40 parts of inert filler, 15 parts of metal powder, 20 parts of adhesive, 3 parts of plasticizer, 2 parts of curing agent, 0.3 parts of bonding agent and 0.5 parts of antioxidant;

[0030] The preparation method of the inert filler is as follows:

[0031] The nanofiber particles are ultrasonically dispersed in a mixed solution of ethanol and ammonia water, tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are continuously added dropwise for reaction, and then centrifugally dried to obtain rod-point particles, which are then mixed with fine sand to obtain the product.

[0032] The nanofiber particles are nano attapulgite fibers or calcium carbonate whiskers.

[0033] The volume ratio of the ethanol to the ammonia water is 5:1.

[0034] The concentration of the nanofiber particles is 30 g / L.

[0035] The added amounts of tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are 50 ml / L and 6 ml / L respectively.

[0036] The added mass ratio of the rod point particles to the fine sand is 1:20.

[0037] The metal powder is aluminum powder;

[0038] The binder is hydroxyl-terminated polybutadiene;

[0039] The plasticizer is diisooctyl sebacate;

[0040] The curing agent is toluene diisocyanate;

[0041] The bonding agent is tris-(2-methylaziridinyl)phosphine oxide;

[0042] The antioxidant is N,N-diphenyl-p-phenylenediamine.

[0043] The particle size of the fine sand is 10-20 meshes.

[0044] The preparation method thereof comprises the following steps:

[0045] S1: Premix metal powder, adhesive, plasticizer, bonding agent and antioxidant to obtain slurry; pre-bake the metal powder at 60-70°C for 4 days.

[0046] S2: Add inert filler to the slurry, mix well, then add curing agent, inject into the engine housing and cure for 5 days, demould, and obtain. Premixing environmental conditions: 20℃±5℃, relative humidity ≤60%;

[0047] The premixing temperature is 50° C. and the premixing time is 30 min.

[0048] Example 2

[0049] An inert hydroxybutyrate composite solid propellant comprises the following raw materials in parts by weight: 40 parts of inert filler, 15 parts of metal powder, 15 parts of adhesive, 2 parts of plasticizer, 3 parts of curing agent, 0.2 parts of bonding agent and 0.2 parts of antioxidant;

[0050] The preparation method of the inert filler is as follows:

[0051] The nanofiber particles are ultrasonically dispersed in a mixed solution of ethanol and ammonia water, tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are continuously added dropwise for reaction, and then centrifugally dried to obtain rod-point particles, which are then mixed with fine sand to obtain the product.

[0052] The nanofiber particles are nano attapulgite fibers or calcium carbonate whiskers.

[0053] The volume ratio of the ethanol to the ammonia water is 3:1.

[0054] The concentration of the nanofiber particles is 10 g / L.

[0055] The added amounts of tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are 50 ml / L and 7 ml / L respectively.

[0056] The added mass ratio of the rod point particles to the fine sand is 3:20.

[0057] The metal powder is aluminum powder;

[0058] The binder is hydroxyl-terminated polybutadiene;

[0059] The plasticizer is diisooctyl sebacate;

[0060] The curing agent is toluene diisocyanate;

[0061] The bonding agent is tris-(2-methylaziridinyl)phosphine oxide;

[0062] The antioxidant is N,N-diphenyl-p-phenylenediamine.

[0063] The particle size of the fine sand is 10-20 meshes.

[0064] The preparation method thereof comprises the following steps:

[0065] S1: Premix metal powder, adhesive, plasticizer, bonding agent and antioxidant to obtain slurry; pre-bake the metal powder at 60-70°C for 4 days.

[0066] S2: Add inert filler to the slurry, mix well, then add curing agent, inject into the engine housing and cure for 5 days, demould, and obtain. Premixing environmental conditions: 20℃±5℃, relative humidity ≤60%;

[0067] The premixing temperature is 50° C. and the premixing time is 30 min.

[0068] Example 3

[0069] An inert hydroxybutyrate composite solid propellant comprises the following raw materials in parts by weight: 50 parts of inert filler, 10 parts of metal powder, 20 parts of adhesive, 3 parts of plasticizer, 2 parts of curing agent, 0.3 parts of bonding agent and 0.2 parts of antioxidant;

[0070] The preparation method of the inert filler is as follows:

[0071] The nanofiber particles are ultrasonically dispersed in a mixed solution of ethanol and ammonia water, tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are continuously added dropwise for reaction, and then centrifugally dried to obtain rod-point particles, which are then mixed with fine sand to obtain the product.

[0072] The nanofiber particles are nano attapulgite fibers or calcium carbonate whiskers.

[0073] The volume ratio of the ethanol to the ammonia water is 6:1.

[0074] The concentration of the nanofiber particles is 40 g / L.

[0075] The added amounts of tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are 50 ml / L and 7 ml / L respectively.

[0076] The added mass ratio of the rod point particles to the fine sand is 1:5.

[0077] The metal powder is aluminum powder;

[0078] The binder is hydroxyl-terminated polybutadiene;

[0079] The plasticizer is diisooctyl sebacate;

[0080] The curing agent is toluene diisocyanate;

[0081] The bonding agent is tris-(2-methylaziridinyl)phosphine oxide;

[0082] The antioxidant is N,N-diphenyl-p-phenylenediamine.

[0083] The particle size of the fine sand is 10-20 meshes.

[0084] The preparation method thereof comprises the following steps:

[0085] S1: Premix metal powder, adhesive, plasticizer, bonding agent and antioxidant to obtain slurry; pre-bake the metal powder at 60-70°C for 4 days.

[0086] S2: Add inert filler to the slurry, mix well, then add curing agent, inject into the engine housing and cure for 5 days, demould, and obtain. Premixing environmental conditions: 20℃±5℃, relative humidity ≤60%;

[0087] The premixing temperature is 50° C. and the premixing time is 30 min.

[0088] Example 4

[0089] An inert hydroxybutyrate composite solid propellant comprises the following raw materials in parts by weight: 60 parts of inert filler, 25 parts of metal powder, 18 parts of adhesive, 3 parts of plasticizer, 2 parts of curing agent, 0.3 parts of bonding agent and 0.8 parts of antioxidant;

[0090] The preparation method of the inert filler is as follows:

[0091] The nanofiber particles are ultrasonically dispersed in a mixed solution of ethanol and ammonia water, tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are continuously added dropwise for reaction, and then centrifugally dried to obtain rod-point particles, which are then mixed with fine sand to obtain the product.

[0092] The nanofiber particles are nano attapulgite fibers or calcium carbonate whiskers.

[0093] The volume ratio of the ethanol to the ammonia water is 8:1.

[0094] The concentration of the nanofiber particles is 40 g / L.

[0095] The added amounts of tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are 50 ml / L and 7 ml / L respectively.

[0096] The added mass ratio of the rod point particles to the fine sand is 1:4.

[0097] The metal powder is aluminum powder;

[0098] The binder is hydroxyl-terminated polybutadiene;

[0099] The plasticizer is diisooctyl sebacate;

[0100] The curing agent is toluene diisocyanate;

[0101] The bonding agent is tris-(2-methylaziridinyl)phosphine oxide;

[0102] The antioxidant is N,N-diphenyl-p-phenylenediamine.

[0103] The particle size of the fine sand is 10-20 meshes.

[0104] The preparation method thereof comprises the following steps:

[0105] S1: Premix metal powder, adhesive, plasticizer, bonding agent and antioxidant to obtain slurry; pre-bake the metal powder at 60-70°C for 4 days.

[0106] S2: Add inert filler to the slurry, mix well, then add curing agent, inject into the engine housing and cure for 5 days, demould, and obtain. Premixing environmental conditions: 20℃±5℃, relative humidity ≤60%;

[0107] The premixing temperature is 50° C. and the premixing time is 30 min.

[0108] Comparative Example 1

[0109] Different from Example 2, the inert filler is fine sand.

[0110] Comparative Example 2

[0111] Different from Example 2, the inert filler is a mixture of nanofiber particles and fine sand in a mass ratio of 1:20.

[0112] The performance of the above embodiments and comparative examples were tested, and the test results are shown in Table 1.

[0113] Table 1 Performance test results of embodiments and comparative examples

[0114]

[0115] It can be seen from Table 1 that the performance of the embodiment is better than that of the comparative example. The main reasons may be: from the analysis of the comparative example, it can be seen that the embodiment adds tiny particles of a rod-point structure into the fine sand, so that the surface of the fine sand has a micro-nano concave-convex structure, thereby having excellent hydrophobic properties, reducing the hygroscopic properties of the slurry, and solving the problem of "water seepage" of the traditional medicine column; from the analysis of comparative example 2, it can be seen that the rod-point structure in the embodiment can improve the mechanical strength of the medicine column and reduce the generation of pores and cracks.

[0116] The above-mentioned embodiments only express the preferred implementation modes of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the present invention. It should be pointed out that, for ordinary technicians in this field, various other corresponding changes and deformations can be made according to the technical solutions and concepts described above, and all these changes and deformations should fall within the scope of protection of the claims of the present invention.

Claims

1. An inert hydroxybutyric acid composite solid propellant, characterized in that: The material comprises the following raw materials in parts by weight: 40-60 parts of inert filler, 10-25 parts of metal powder, 15-30 parts of adhesive, 2-4 parts of plasticizer, 1-3 parts of curing agent, 0.2-0.5 parts of bonding agent and 0.2-1 parts of antioxidant; The preparation method of the inert filler is as follows: The nanofiber particles are ultrasonically dispersed in a mixed solution of ethanol and ammonia water, tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are continuously added dropwise for reaction, and then centrifugally dried to obtain rod-point particles, which are then mixed with fine sand to obtain the product.

2. An inert HTPB composite solid propellant according to claim 1, characterized in that: The nanofiber particles are nano attapulgite fibers or calcium carbonate whiskers.

3. The inert HTPB composite solid propellant according to claim 1, characterized in that: The volume ratio of the ethanol to the ammonia water is 3-8:

1.

4. The inert HTPB composite solid propellant according to claim 1, characterized in that: The concentration of the nanofiber particles is 10-50 g / L.

5. The inert HTPB composite solid propellant according to claim 1, characterized in that: The addition amounts of tetraethyl orthosilicate and 3-glycidyloxypropyltriethoxysilane are 30-80 ml / L and 5-8 ml / L respectively.

6. The inert HTPB composite solid propellant according to claim 1, characterized in that: The added mass ratio of the rod point particles to the fine sand is 1-5:

20.

7. The inert HTPB composite solid propellant according to claim 1, characterized in that: The metal powder is aluminum powder; The binder is hydroxyl-terminated polybutadiene; The plasticizer is diisooctyl sebacate; The curing agent is toluene diisocyanate; The bonding agent is tris-(2-methylaziridinyl)phosphine oxide; The antioxidant is N,N-diphenyl-p-phenylenediamine.

8. The inert HTPB composite solid propellant according to claim 1, characterized in that: The particle size of the fine sand is 10-20 meshes.

9. A method for preparing an inert hydroxybutyl composite solid propellant, characterized in that: The following steps are involved: S1: premixing metal powder, adhesive, plasticizer, bonding agent and antioxidant to obtain slurry; S2: adding an inert filler to the slurry, mixing well, then adding a curing agent, injecting into an engine housing for curing, and demoulding to obtain the product.

10. The method for preparing an inert HTPB composite solid propellant according to claim 9, characterized in that: The premixing temperature is 40-60° C., and the premixing time is 20-40 minutes.

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