A solution-type FIAM flexible intelligent impact-resistant material and preparation method thereof

Abstract

The invention discloses a solution-type FIAM flexible intelligent impact-resistant material, including 100 parts of hydroxy silicone oil and 3-8 parts of boric acid; and also includes a method for preparing the material, including the following steps: weighing hydroxy silicone oil and boric acid for standby; preheating the hydroxy silicone oil; condensation reaction of boric acid and the hydroxy silicone oil; cross-linking reaction of boric acid and the hydroxy silicone oil to obtain a solution-type FIAM flexible intelligent impact-resistant material. The invention realizes the improvement of the transparency of shear thickening gel, reduces the influence on the light transmittance of optical composite materials, and greatly improves its application range; and has low viscosity performance, reduces the inhibition of foaming; and overcomes the problem of uneven mixing of composite materials at room temperature, so that it can be compounded with other substrates at room temperature, reduces the composite reaction temperature, and thus reduces the production cost of composite materials.

Description

Technical Field

[0001] The present invention relates to the technical field of flexible protective materials, and in particular to a solution-type FIAM flexible intelligent impact-resistant material and a preparation method thereof. Background Art

[0002] Personal protective equipment has always pursued the protection goals of lightness, comfort and efficiency. Due to its excellent flexibility, energy absorption and impact resistance, shear thickening materials (STM) represented by shear thickening fluid (STF) and shear thickening gel (STG) have been widely used in various impact protection and vibration suppression fields. More importantly, STM can have a broad spectrum of reinforcing and enabling effects on various protective materials in the form of composite materials, which can greatly improve the impact protection performance of existing materials.

[0003] However, when empowering composites with other materials, STM always faces the following three technical problems: (1) STM and the substrate need to be heated to a predetermined temperature or dissolved in a solvent to achieve uniform mixing, which increases the manufacturing cost of the composite material; (2) For foam composite materials, the high viscosity of STM will lead to phase separation and local clustering behavior between various materials, thereby inhibiting the foaming behavior of the foam composite material; (3) In optical materials with high light transmittance requirements, opaque STM will lead to a significant reduction in the light transmittance of the optical material.

[0004] Therefore, in the preparation and application of impact protection materials, an STM is needed that can be composited with other substrates at room temperature and has physical properties such as good foaming effect and high transparency. Summary of the invention

[0005] The purpose of the present invention is to provide a solution-type FIAM flexible intelligent impact-resistant material and a preparation method thereof, so as to solve the technical problems in the prior art that the shear thickening material has low transparency, is not easy to foam, and requires high temperature when compounded with other materials.

[0006] In order to solve the above technical problems, the present invention specifically provides the following technical solutions:

[0007] The invention provides a solution-type FIAM flexible intelligent impact-resistant material, which comprises 100 parts of hydroxy silicone oil and 3-8 parts of boric acid in terms of parts.

[0008] As a preferred embodiment of the present invention, the viscosity of the solution-type FIAM flexible intelligent impact-resistant material is lower than 100 Pa·s;

[0009] The solution-based FIAM flexible intelligent impact-resistant material has a light transmittance higher than 92%, a haze lower than 1%, and a volatility lower than 1%.

[0010] The present invention provides a method for preparing a solution-type FIAM flexible intelligent impact-resistant material, comprising the following steps:

[0011] Weigh hydroxy silicone oil and boric acid separately for later use;

[0012] preheating the hydroxy silicone oil;

[0013] The boric acid and the hydroxy silicone oil undergo a condensation reaction;

[0014] The boric acid and the hydroxy silicone oil undergo a cross-linking reaction to prepare a solution-type FIAM flexible intelligent impact-resistant material.

[0015] As a preferred embodiment of the present invention, the preheating step comprises:

[0016] The hydroxy silicone oil is brought into the reaction kettle and heated for the first time under stirring;

[0017] After the heating is completed, the hydroxy silicone oil is kept warm for 30 to 50 minutes to obtain a preheated solution.

[0018] As a preferred embodiment of the present invention, the condensation reaction comprises:

[0019] Pour the boric acid into the reactor and mix it evenly with the preheated solution;

[0020] The reaction kettle is subjected to vacuum treatment to obtain a reaction solution.

[0021] As a preferred embodiment of the present invention, the cross-linking reaction comprises:

[0022] The reaction solution is heated for a second time and kept warm for 1 to 2 hours;

[0023] performing the vacuuming treatment on the reactor;

[0024] The solution was cooled to room temperature to obtain the solution-based FIAM flexible intelligent impact-resistant material.

[0025] As a preferred embodiment of the present invention, the vacuum treatment comprises the following steps:

[0026] The reactor is evacuated until the vacuum degree reaches 0.5-0.7 MPa, and the evacuation is stopped;

[0027] When the vacuum degree is lower than 0.2MPa, start vacuuming until the vacuum degree reaches 0.5-0.7MPa;

[0028] The vacuuming operation is repeated for 1 to 2 hours.

[0029] As a preferred embodiment of the present invention, the heating temperature of the first heating satisfies: 110-120°C.

[0030] As a preferred embodiment of the present invention, the heating temperature of the second heating satisfies: 160-180°C.

[0031] As a preferred solution of the present invention, the performance of the solution-based FIAM flexible intelligent impact-resistant material is characterized:

[0032] The solution-type FIAM flexible intelligent impact-resistant material has significant shear thickening properties and buffering energy absorption properties, and both the storage modulus and the loss modulus thereof increase sharply with the increase of the shear frequency.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] 1. Solution-based FIAM flexible intelligent impact-resistant materials show high transparency and have broader development prospects in the application of optical materials;

[0035] 2. The solution-based FIAM flexible intelligent impact-resistant material exhibits a lower viscosity, which reduces the inhibition of the foaming behavior of the foam composite material, and can make the foam composite material have more foam and improve its performance;

[0036] 3. In the process of compounding the shear thickening material prepared by the present invention with various materials, it is reflected that the material overcomes the problem of uneven mixing of composite materials at room temperature, can be compounded with other substrates under solvent-free and room temperature conditions, and reduces the required temperature during the compounding reaction, thereby reducing the production cost of the composite material;

[0037] 4. Compared with the STF of particle suspension system, solution-based FIAM flexible intelligent impact-resistant material exhibits better physical stability, reducing the problems of particle sedimentation and solvent volatilization in the system;

[0038] 5. The invention prepares solution-type FIAM flexible intelligent impact-resistant material by heating, mixing and vacuuming raw materials. The preparation method is simple and easy to reproduce. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] In order to more clearly illustrate the implementation methods of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for the implementation methods or the description of the prior art. Obviously, the drawings in the following description are only exemplary, and for ordinary technicians in this field, other implementation drawings can be derived from the provided drawings without creative work.

[0040] Figure 1Provides a high-transparency sample of a solution-type FIAM flexible intelligent impact-resistant material for the present invention;

[0041] Figure 2 A schematic flow chart of a method for preparing a solution-type FIAM flexible intelligent impact-resistant material is provided for the present invention;

[0042] Figure 3 The present invention provides a graph of rheological properties (relationship between modulus and shear frequency) of a solution-type FIAM flexible intelligent impact-resistant material. DETAILED DESCRIPTION

[0043] 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 only 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.

[0044] The present invention provides a solution-type FIAM flexible intelligent impact-resistant material, which includes 100 parts of hydroxy silicone oil and 3-8 parts of boric acid in terms of weight. The novel solution-type FIAM flexible intelligent impact-resistant material is made of hydroxy silicone oil and boric acid in a mass ratio of 100:3 to 100:8.

[0045] Figure 1 This is a solution sample of FIAM flexible intelligent impact-resistant material. Compared with STM, this solution-type FIAM flexible intelligent impact-resistant material has high permeability and low viscosity. In optical materials with high light transmittance requirements, the solution-type FIAM flexible intelligent impact-resistant material with high transparency will not affect the light transmittance of optical composite materials, greatly improving its application range. The solution-type FIAM flexible intelligent impact-resistant material has a low viscosity and will not inhibit the foaming behavior of the foam composite material, so that the foam composite material has more foam inside, improving its performance.

[0046] In order to obtain the above-mentioned highly transparent solution type, Figure 2 As shown, the present invention provides a method for preparing a solution-type FIAM flexible intelligent impact-resistant material, comprising the following steps:

[0047] 1. Preparation of raw materials and experimental instruments

[0048] Raw materials: hydroxy silicone oil (solution), boric acid (powder);

[0049] Experimental instruments: vacuum high temperature kneading machine, electronic scale, hardness tester, measuring cylinder.

[0050] 2. Weighing of raw materials

[0051] According to the mass ratio of the raw materials (hydroxy silicone oil: boric acid = 100:3 to 100:8), weigh hydroxy silicone oil and boric acid respectively for use.

[0052] 3. Preheat the hydroxy silicone oil

[0053] Pour the hydroxy silicone oil into the reaction kettle, then close the kettle cover and start stirring, and adjust the heating temperature to 110-120°C; when the reaction kettle reaches the predetermined temperature, keep the hydroxy silicone oil warm for 30-50 minutes to obtain a preheated solution.

[0054] 4. Boric acid and the hydroxy silicone oil undergo condensation reaction

[0055] Open the lid of the reactor, pour the boric acid into the preheated solution in the reactor, close the lid and stir evenly to fully mix the boric acid and the preheated solution of the hydroxy silicone oil;

[0056] The reactor was evacuated, and when the vacuum degree reached 0.5-0.7 MPa, the vacuum was turned off; when the vacuum degree was lower than 0.2 MPa, the vacuum was turned on again, and the boric acid and the hydroxy silicone oil were allowed to react for 1-2 hours in this environment to obtain a reaction solution.

[0057] 5. Boric acid and the hydroxy silicone oil undergo cross-linking reaction

[0058] The temperature of the reactor is raised to 160-180°C, and the temperature is maintained for 1-2 hours after reaching the temperature, and the vacuum extraction operation in step 4 is repeated during the reaction. When the chemical reaction between boric acid and hydroxy silicone oil is completed, the heating and stirring are stopped, the lid of the reactor is opened, and the reactor is naturally cooled to room temperature to obtain a solution-type FIAM material, which is a solution-type FIAM flexible intelligent impact-resistant material.

[0059] 6. Characterization of rheological properties of FIAM solution

[0060] Based on the rotational rheometer in shear mode, the rheological properties of FIAM solution were characterized by a frequency of 0.01-100 Hz and an ambient temperature of 25°C. As the shear frequency increased from 0.1 Hz to 100 Hz, the storage modulus of FIAM solution increased from 1.49E-6 kPa to 1.64 kPa, and the loss modulus increased from 1.83E-4 kPa to 2.08 kPa, and its dynamic mechanical properties showed a sensitive strain rate effect. Therefore, FIAM solution has obvious FIAM flexible intelligent impact resistance characteristics.

[0061] Figure 3 The graph is a graph of the rheological properties (relationship between modulus and shear frequency) of FIAM solution.

[0062] The present invention adopts the above method to prepare a solution-type FIAM flexible intelligent impact-resistant material. Characterization proves that the material has good applicability, namely: low viscosity, can be mixed at room temperature, more uniform mixing, and can be used for optical materials.

[0063] Several specific embodiments are provided below. The embodiments are as follows:

[0064] Example 1

[0065] Step 1. Material preparation: Use an electronic scale to take 100 parts of hydroxy silicone oil solution and 3 parts of boric acid powder, with the unit of each material being g, and set aside;

[0066] Step 2, pour the hydroxy silicone oil solution into the reaction kettle according to the formula amount, then close the kettle cover and start stirring, and adjust the heating temperature to 110-120° C.; when the reaction kettle reaches the predetermined temperature, the hydroxy silicone oil is kept warm for 30-50 minutes to obtain a preheated solution;

[0067] Step 3, open the kettle cover of the reactor, pour the boric acid into the preheated solution in the reactor, close the kettle cover and stir evenly to fully mix the boric acid and the preheated solution of the hydroxy silicone oil;

[0068] Step 4: evacuate the reactor using a vacuum high-temperature kneader, and turn off the vacuum when the vacuum degree reaches 0.5-0.7 MPa; turn on the vacuum again when the vacuum degree is lower than 0.2 MPa, and allow the boric acid and hydroxy silicone oil to react in this environment for 1-2 hours to obtain a reaction solution.

[0069] Step 5: Raise the temperature of the reactor to 160-180°C, keep the temperature for 1-2 hours, and repeat the vacuum extraction operation in step 4 during the reaction.

[0070] Step 6: After the chemical reaction between boric acid and hydroxy silicone oil is completed, stop heating and stirring, open the lid of the reactor, and naturally cool to room temperature to obtain a solution-type FIAM material, which is Example 1.

[0071] The solution-type FIAM material prepared in Example 1 was taken to determine whether it could undergo a composite reaction with various substrates at room temperature for a certain period of time, that is, whether it could undergo a composite reaction.

[0072]

[0073] By analyzing Table 1, the following conclusions are drawn: How long can the solution-based FIAM material of the present invention be physically compounded with solution-based substrates such as TPU, PSA and PMMA at room temperature, thereby reducing the reaction temperature required for compounding and greatly reducing the reaction cost of the composite material.

[0074] Embodiment 2:

[0075] Step 1, material preparation: use an electronic scale to take 100 parts of hydroxy silicone oil solution and 5 parts of boric acid powder, the unit of each material is g, and set aside;

[0076] Steps 2, 3, 4, 5, and 6 are all produced according to the formula amount, and the production steps are the same as steps 2, 3, 4, 5, and 6 in Example 1;

[0077] 6. After mixing evenly, put into tube to obtain Example 2.

[0078] Embodiment 3:

[0079] Step 1, material preparation: use an electronic scale to take 100 parts of hydroxy silicone oil solution and 8 parts of boric acid powder, the unit of each material is g, and set aside;

[0080] Steps 2, 3, 4, 5, and 6 are all produced according to the formula amount, and the production steps are the same as steps 2, 3, 4, 5, and 6 in Example 1;

[0081] 6. After mixing evenly, put into tube to obtain Example 3.

[0082] The specific data is as follows:

[0083] Table 2 Comparison of performance parameters of Examples 1, 2, 3 and Comparative Examples

[0084]

[0085] As shown in Table 2, by comparing different embodiments, it can be seen that in this formula, compared with ordinary shear thickening gel (STF, STG), the solution-type FIAM flexible intelligent impact-resistant material prepared by the present invention has lower system viscosity, higher transparency and lower composite reaction temperature with the substrate.

[0086] Through the solution-type FIAM flexible intelligent impact-resistant material and preparation method of this embodiment, the transparency of the shear thickening gel can be improved, the influence on the light transmittance of the optical composite material can be reduced, and its application range can be greatly improved; and it has low viscosity performance, reducing the inhibition of foaming; at the same time, it overcomes the problem of uneven mixing of the composite material at room temperature, so that it can be compounded with other substrates at room temperature, reducing the composite reaction temperature, thereby reducing the production cost of the composite material.

[0087] The above embodiments are only exemplary embodiments of the present application and are not intended to limit the present application. The protection scope of the present application is defined by the claims. Those skilled in the art may make various modifications or equivalent substitutions to the present application within the essence and protection scope of the present application, and such modifications or equivalent substitutions shall also be deemed to fall within the protection scope of the present application.

Claims

1. A method for preparing a solution-based FIAM flexible intelligent impact-resistant material. It is characterized in that The steps include: Weigh hydroxy silicone oil and boric acid separately for use, including 100 parts of hydroxy silicone oil and 3-8 parts of boric acid according to the number of parts; Preheating the hydroxy silicone oil, the preheating step comprising: bringing the hydroxy silicone oil into a reaction kettle, and performing a first heating under stirring, wherein the heating temperature of the first heating satisfies: 110-120° C.; after the heating is completed, keeping the hydroxy silicone oil warm for 30-50 minutes to obtain a preheated solution; The boric acid and the hydroxy silicone oil undergo a condensation reaction, the boric acid is poured into the reactor, and mixed evenly with the preheated solution; the reactor is subjected to a vacuum treatment to obtain a reaction solution; the vacuum treatment comprises the following steps: the reactor is subjected to a vacuum treatment until the vacuum degree reaches 0.5-0.7 MPa, and the vacuum treatment is stopped; when the vacuum degree is lower than 0.2 MPa, the vacuum treatment is started until the vacuum degree reaches 0.5-0.7 MPa; wherein the vacuum treatment is repeated for 1-2 hours; The boric acid and the hydroxy silicone oil undergo a cross-linking reaction, and the cross-linking reaction comprises: heating the reaction solution for a second time, wherein the heating temperature of the second heating satisfies: 160-180° C., and the temperature is kept for 1-2 h; vacuuming the reactor; and cooling to room temperature to obtain a solution-type FIAM flexible intelligent impact-resistant material.

2. A solution-type FIAM flexible intelligent impact-resistant material prepared according to the preparation method of claim 1, It is characterized in that The viscosity of the solution-type FIAM flexible intelligent impact-resistant material is lower than 100 Pa·s; Among them, the solution-based FIAM flexible intelligent impact-resistant material has a light transmittance higher than 92%, a haze lower than 1%, and a volatility lower than 1%.

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