Preparation process and preparation system of wet glass fiber aerogel product

Abstract

The invention provides a preparation process and a preparation system of a wet glass fiber aerogel product, and relates to the technical field of new energy automobiles, the preparation process of the wet glass fiber aerogel product comprises the following steps: preparing a glue solution; the prepared glue solution enters a glue dipping tank, the sheet-shaped wet glass fiber felt is fully dipped in the glue solution in the tank, and then the sheet-shaped wet glass fiber felt is placed on a belt and enters a microwave section for gel forming; putting the prepared product into a product basket, and then putting the product basket into an aging tank for aging-modification; and after aging-modification is completed, directly taking out the product basket in the aging tank, putting the product basket into a supercritical drying tank, and carrying out supercritical drying on the product. Through a continuous microwave forming production mode, the product gelation time is greatly shortened, the production efficiency is improved, due to the fact that product gelation is accelerated through microwave heating, it can be guaranteed that the product gel surface is uniform, the product gelation time is greatly shortened, the production efficiency is improved, and the product quality is guaranteed.

Description

Technical Field

[0001] The present invention relates to the technical field of new energy vehicles, and in particular to a preparation process and a preparation system for a wet-process glass fiber aerogel product. Background Art

[0002] With the development of new energy vehicles, the safety of new energy batteries has become the focus of public attention. How to effectively extend the escape time during battery failure has become the focus of most car companies. Wet-processed glass fiber aerogel insulation sheets have become the preferred products of car companies due to their low thermal conductivity, small space occupation, and Class A flame retardancy. However, due to the late start of wet-processed glass fiber aerogel insulation sheets, which have only appeared in the past two or three years, the production process is immature and there are few manufacturers, resulting in market demand exceeding supply.

[0003] Wet-laid fiberglass is a textile made of a mixture of glass fibers and special resins. It is made through a fiber wet papermaking process, where the glass fibers are first mixed with water, and then the mixture is evenly spread on a grid-like mold. Subsequently, the fibers and resin are solidified together through pressurization and drying to form a tough and durable fiber material. Wet-laid fiberglass has the characteristics of light weight, corrosion resistance, high temperature resistance, low thermal conductivity, high strength, as well as good durability and stability.

[0004] The thickness of traditional aerogel products is generally 6-20mm, and its national standard only requires thermal insulation performance, mechanical properties, fire resistance and other requirements; but the thickness of wet-process glass fiber aerogel products is generally 1.0-4.0mm, and the quality requirements must not only meet the national standards of traditional aerogel products, but also meet the requirements of uniform thickness of the products, uniform aerogel content, smooth and flat surface, etc.

[0005] Due to the thin thickness of wet-process glass fiber, the aerogel content is difficult to control, which affects its gel state and gel uniformity. Poor gel state and uniformity will cause the thermal conductivity of the product to increase significantly; and wet-process glass fiber aerogel felts mostly adopt a sheet production mode, resulting in low mass production efficiency. Summary of the invention

[0006] In view of this, one of the objects of the present invention is to provide a preparation process for a wet-process glass fiber aerogel product, so as to solve the technical problems that the gel state and gel uniformity of the wet-process glass fiber aerogel product prepared in the prior art are difficult to control, resulting in a significant increase in the thermal conductivity of the product, and the wet-process glass fiber aerogel felt mostly adopts a sheet production mode, resulting in low mass production efficiency.

[0007] A second object of the present invention is to provide a system for preparing a wet-process glass fiber aerogel product.

[0008] In order to achieve one of the above purposes, an embodiment of the present invention provides a preparation process of a wet-laid glass fiber aerogel product, comprising the following steps:

[0009] Step S1: preparing glue solution;

[0010] Step S2: the prepared glue solution enters the glue dipping tank, the sheet-shaped wet-process glass fiber felt is soaked with the glue solution in the tank, and then placed on the belt and enters the microwave section for gel forming;

[0011] Step S3: placing the product prepared in step S2 into a product basket, and then placing the product basket into an aging tank for aging-modification;

[0012] Step S4: After the aging-modification is completed, the product basket in the aging tank is directly taken out and placed in a supercritical drying tank to perform supercritical drying on the product.

[0013] Optionally, the preparation of the glue solution in step S1 is to directly feed the raw materials in the raw material storage tank into the stirring reactor through a metering pump to complete the glue making.

[0014] Optionally, the belt speed in step S2 is adjusted by a belt speed control system, and the adjustment range is 0.5-3.0 m / min.

[0015] Optionally, the microwave section in step S2 is divided into a main section and a secondary section of microwaves, and the rates of the two sections of microwaves are both adjusted by a microwave power control system, and the microwave power control range is: 100w-2000w.

[0016] Optionally, the gel-formed products in step S2 are detected by a product gel state detection system, and the products with qualified gel will enter the product basket, and the unqualified products will be scrapped, and the microwave power and belt rotation speed are adjusted according to the gel state of the unqualified products.

[0017] Optionally, the modifier in step S3 is one of methyltriethoxysilane, dimethyldiethoxysilane, trimethylchlorosilane and hexamethyldisilazane.

[0018] In order to achieve the second of the above-mentioned purposes, an embodiment of the present invention provides a preparation system for the preparation process of any of the above-mentioned wet-process glass fiber aerogel products, characterized in that it includes a stirring reactor, a dipping tank, a microwave forming device, a product basket, a heating aging tank and a supercritical drying reactor that are connected and communicated in sequence.

[0019] Optionally, the microwave forming device includes a belt transmission mechanism and a microwave generating mechanism, the belt transmission mechanism is arranged adjacent to the glue dipping tank, and the microwave generating mechanism is arranged above the belt transmission mechanism.

[0020] Optionally, the microwave generating mechanism comprises a main microwave generator and a sub-microwave generator, and the main microwave generator and the sub-microwave generator are arranged one after the other.

[0021] Optionally, the microwave forming device further includes a microwave control module, a belt control module and a product gel state detection module. The microwave control module is control-connected to the main microwave generator and / or the auxiliary microwave generator at the same time, and is used to control the microwave intensity of the main microwave generator and / or the auxiliary microwave generator. The belt control module is control-connected to the belt transmission mechanism, and is used to control the belt transmission speed of the belt transmission mechanism. The product gel state detection module is arranged at the end of the belt transmission mechanism, and is used to detect whether the product after gel forming is qualified.

[0022] The preparation process of the wet-process glass fiber aerogel product provided by the present invention has the following technical effects:

[0023] The preparation process of this kind of wet-process glass fiber aerogel product includes preparing glue liquid; conveying the prepared glue liquid into a glue dipping tank, soaking the sheet-shaped wet-process glass fiber felt in the tank with glue liquid, and then placing it on a belt and entering the microwave section for gel forming; placing the prepared product into a product basket, and then placing the product basket into an aging tank for aging-modification; after the aging-modification is completed, directly taking out the product basket from the aging tank and placing it into a supercritical drying tank to perform supercritical drying on the product. The present invention greatly shortens the gel time of the product and improves production efficiency through a continuous microwave forming production method. Since microwave heating accelerates the gelation of the product, it can ensure that the surface of the product gel is uniform, greatly shortens the gel time of the product, improves production efficiency, and ensures product quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0025] Figure 1 It is a structural schematic diagram of the preparation system of wet-process glass fiber aerogel products.

[0026] in, Figure 1 :

[0027] 1. Stirring reactor; 11. Silicon source storage tank; 12. Ethanol storage tank; 13. Deionized water storage tank; 14. Catalyst storage tank;

[0028] 21. Glue dipping tank; 22. Glue dipping liquid recovery tank;

[0029] 31. Main microwave generator; 32. Auxiliary microwave generator; 33. Belt; 34. Roller; 35. Microwave control module; 36. Belt control module; 37. Product gel state detection module;

[0030] 4. Product basket; 5. Heating aging tank; 6. Supercritical drying kettle. DETAILED DESCRIPTION

[0031] To make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be described in detail below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other implementation methods obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.

[0032] Below in conjunction with specific embodiments 1-3 and attached Figure 1 The preparation process and preparation system of a wet-process glass fiber aerogel product of the present invention are described in detail.

[0033] The present invention provides a preparation system for a wet-process glass fiber aerogel product preparation process, such as Figure 1 As shown, it includes a stirring reactor 1, a glue dipping tank 21, a microwave forming device, a product basket 4, a heating aging tank 5 and a supercritical drying reactor 6 which are connected and communicated in sequence.

[0034] The stirred reactor 1 is connected and communicated with the silicon source storage tank 11, the ethanol storage tank 12, the deionized water storage tank 13 and the catalyst storage tank 14 at the same time, that is, the silicon source storage tank 11, the ethanol storage tank 12, the deionized water storage tank 13 and the catalyst storage tank 14 are all connected in parallel with the stirred reactor 1, and a metering pump is provided on the pipeline between the silicon source storage tank 11, the ethanol storage tank 12, the deionized water storage tank 13 and the catalyst storage tank 14 and the stirred reactor 1, and the amount of liquid entering the stirred reactor 1 is determined by the metering pump.

[0035] The liquid outlet of the stirring reactor 1 is communicated with the dipping tank 21 , and a dipping liquid recovery tank 22 is provided below the dipping tank 21 , that is, the dipping liquid recovery tank 22 can recover the residual dipping liquid.

[0036] Continue to see Figure 1 As shown, the microwave forming device of this embodiment includes a belt transmission mechanism and a microwave generating mechanism. The belt transmission mechanism is arranged adjacent to the resin dipping tank 21, and the microwave generating mechanism is arranged above the belt transmission mechanism.

[0037] The belt transmission mechanism includes a belt 33 , a roller 34 and a driving motor. The driving motor is drivingly connected to the roller 34 . The belt 33 is wound around the roller 34 , and the belt 33 is driven by the rotation of the roller 34 .

[0038] The microwave generating mechanism includes a main microwave generator 31 and a sub-microwave generator 32. The main microwave generator 31 and the sub-microwave generator 32 are arranged one after the other. The main microwave generator 31 generates the main microwave, and the sub-microwave generator 32 generates the sub-microwave.

[0039] In addition, see Figure 1 As shown, the microwave forming device further includes a microwave control module 35 , a belt control module 36 and a product gel state detection module 37 .

[0040] The microwave control module 35 is simultaneously connected to the main microwave generator 31 and / or the auxiliary microwave generator 32 for controlling the microwave intensity of the main microwave generator 31 and / or the auxiliary microwave generator 32. The microwave power control range is 100w-2000w.

[0041] The belt regulating module 36 is connected to the belt transmission mechanism for controlling the transmission speed of the belt 33, and the adjustment range is 0.5-3.0 m / min.

[0042] The product gel state detection module 37 is arranged at the end of the belt transmission mechanism, and is used to detect whether the gel-formed product is qualified. The qualified gel products will enter the product basket 4, and the unqualified products will be scrapped. The microwave power and the rotation speed of the belt 33 are adjusted according to the gel state of the unqualified products, that is, the unqualified signal is transmitted to the microwave control module 35 and the belt control module 36, and the microwave intensity of the main microwave generator 31 and / or the auxiliary microwave generator 32 is controlled by the microwave control module 35, and the transmission speed of the belt 33 is controlled by the belt control module 36.

[0043] Embodiment 1:

[0044] A preparation process of a wet-process glass fiber aerogel product, the specific steps comprising:

[0045] (1) Place 1.0 mm thick wet-process glass fiber felt into the dipping tank.

[0046] (2) Open the feed valve of the reactor and add ethyl orthosilicate, ethanol and deionized water into the reactor in a molar ratio of 1:12:4 in sequence. Turn on the stirring device of the reactor and stir for 15 minutes, then add concentrated ammonia water, adjust the pH value to 9 and continue stirring for 10 minutes.

[0047] (3) After stirring evenly, open the discharge valve at the bottom of the reactor and transfer the prepared glue solution into the dipping tank to soak the 1.0 mm thick wet-process glass fiber felt.

[0048] (4) Rotate the belt and set the belt speed to 2m / min, turn on the main microwave generator and the auxiliary microwave generator, set the main microwave power to 600W, and set the auxiliary microwave power to 500W. Place the wet glass fiber felt soaked with glue on the belt, and transfer it through the microwave area of ​​the main microwave generator and the auxiliary microwave generator to heat the gel. After 30 minutes, the wet glass fiber composite aerogel felt is output from the tail of the molding machine through the product gel state detection module.

[0049] (5) Place the gelled wet-process glass fiber composite aerogel felt into a product basket, hoist the product basket into an aging tank, turn on the aging tank heating device, and set the equipment temperature to 25° C. Pass ethanol into the aging tank to cover the product basket, and add 10% by mass of dimethyldiethoxysilane into the tank to age-modify the wet-process glass fiber composite aerogel felt for 48 hours.

[0050] (6) After aging-modification for 48 hours, the product basket was taken out and hoisted into a drying kettle for supercritical drying. After drying for 7 hours, the density was 0.13 g / cm 3 The thermal conductivity coefficient at room temperature is 0.025W / (m·K), the hot surface is heated at 550℃ for 2min and the temperature difference between the hot and cold surfaces is 162℃ under 0.7MPa.

[0051] Embodiment 2:

[0052] A preparation process of a wet-process glass fiber aerogel product, the specific steps comprising:

[0053] (1) Place 1.2 mm thick wet-process glass fiber felt into the dipping tank.

[0054] (2) Open the feed valve of the reactor and add ethyl orthosilicate, ethanol and deionized water into the reactor in a molar ratio of 1:12:4 in sequence. Turn on the stirring device of the reactor and stir for 15 minutes, then add concentrated ammonia water, adjust the pH value to 9 and continue stirring for 10 minutes.

[0055] (3) After stirring evenly, open the discharge valve at the bottom of the reactor and transfer the prepared glue solution into the dipping tank to soak the 1.2 mm thick wet-process glass fiber felt.

[0056] (4) Rotate the belt and set the belt speed to 1.5 m / min, turn on the main microwave generator and the auxiliary microwave generator, set the main microwave power to 500 W, and set the auxiliary microwave power to 450 W. Place the wet glass fiber felt soaked with glue on the belt, and transfer it through the microwave area of ​​the main microwave generator and the auxiliary microwave generator to heat the gel. After 40 minutes, the gel is completed, and the wet glass fiber composite aerogel felt is output from the tail of the molding machine through the product gel state detection module.

[0057] (5) Place the gelled wet-process glass fiber composite aerogel felt into a product basket, hoist the product basket into an aging tank, turn on the aging tank heating device, and set the equipment temperature to 30° C. Pass ethanol into the aging tank to cover the product basket, and add 10% by mass of dimethyldiethoxysilane into the tank to age-modify the wet-process glass fiber composite aerogel felt for 48 hours.

[0058] (6) After aging-modification for 48 hours, the product basket was taken out and hoisted into a drying kettle for supercritical drying. After drying for 7 hours, a wet-process glass fiber composite aerogel product with a density of 0.15 g / cm3, a thermal conductivity of 0.030 W / (m·K) at room temperature, a hot surface heated at 550°C for 2 minutes and a hot and cold surface temperature difference of 156°C under 0.7 MPa was obtained.

[0059] Embodiment 3:

[0060] A preparation process of a wet-process glass fiber aerogel product, the specific steps comprising:

[0061] (1) Place 1.5 mm thick wet-process glass fiber felt into the dipping tank.

[0062] (2) Open the feed valve of the reactor and add ethyl orthosilicate, ethanol and deionized water into the reactor in a molar ratio of 1:12:4 in sequence. Turn on the stirring device of the reactor and stir for 15 minutes, then add concentrated ammonia water, adjust the pH value to 9 and continue stirring for 10 minutes.

[0063] (3) After stirring evenly, open the discharge valve at the bottom of the reactor and transfer the prepared glue solution into the dipping tank to soak the 1.5 mm thick wet-process glass fiber felt.

[0064] (4) Rotate the belt and set the belt speed to 1.0 m / min, turn on the main microwave generator and the auxiliary microwave generator, set the main microwave power to 450 W, and set the auxiliary microwave power to 300 W. Place the wet-process glass fiber felt soaked with glue on the belt, and transfer it through the microwave areas of the main microwave generator and the auxiliary microwave generator to heat the gel. After 60 minutes of gelation, the wet-process glass fiber composite aerogel felt is output from the tail of the molding machine through the product gel state detection module.

[0065] (5) Place the gelled wet-process glass fiber composite aerogel felt into a product basket, hoist the product basket into an aging tank, turn on the aging tank heating device, and set the equipment temperature to 40° C. Pass ethanol into the aging tank to cover the product basket, and add 10% by mass of dimethyldiethoxysilane into the tank to age-modify the wet-process glass fiber composite aerogel felt for 48 hours.

[0066] (6) After aging-modification for 48 hours, the product basket was taken out and hoisted into a drying kettle for supercritical drying. After drying for 7 hours, the density was 0.18 g / cm 3The thermal conductivity coefficient at room temperature is 0.032W / (m·K), the hot surface is heated at 550℃ for 2min and the temperature difference between the hot and cold surfaces is 159℃ under 0.7MPa.

[0067] The following table shows the wet-process glass fiber composite aerogel products prepared in different embodiments:

[0068]

[0069] It can be seen from the above table that the continuous microwave molding production method not only meets the requirements of uniform thickness, uniform aerogel content, smooth and flat surface of wet-process glass fiber composite aerogel products, but also has good mechanical properties, thermal insulation properties and fire resistance.

[0070] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A preparation process of a wet-laid glass fiber aerogel product, characterized in that: The following steps are involved: Step S1: preparing glue solution; Step S2: The prepared glue solution is transported into a glue dipping tank, and the sheet-shaped wet-process glass fiber felt is soaked with the glue solution in the tank, and then placed on a belt and enters a microwave section for gel forming; Step S3: placing the product prepared in step S2 into a product basket, and then placing the product basket into an aging tank for aging-modification; Step S4: After the aging-modification is completed, the product basket in the aging tank is directly taken out and placed in a supercritical drying tank to perform supercritical drying on the product.

2. The preparation process of the wet-process glass fiber aerogel product according to claim 1, characterized in that: The preparation of the glue solution in step S1 is to directly feed the raw materials in the raw material storage tank into the stirring reactor through a metering pump to complete the glue making.

3. The preparation process of the wet-process glass fiber aerogel product according to claim 1, characterized in that: The belt speed in step S2 is adjusted by a belt speed control system, and the adjustment range is 0.5-3.0 m / min.

4. The preparation process of the wet-process glass fiber aerogel product according to claim 3, characterized in that: The microwave section in step S2 is divided into a main section and a secondary section. The microwave rates of the two sections are both adjusted by a microwave power control system. The microwave power control range is 100w-2000w.

5. The preparation process of the wet-process glass fiber aerogel product according to claim 4, characterized in that: In step S2, the gel-formed products are detected by a product gel state detection system. Products with qualified gel will be put into a product basket, and unqualified products will be scrapped. The microwave power and belt rotation speed are adjusted according to the gel state of the unqualified products.

6. The preparation process of the wet-process glass fiber aerogel product according to claim 1, characterized in that: The modifier in step S3 is one of methyltriethoxysilane, dimethyldiethoxysilane, trimethylchlorosilane and hexamethyldisilazane.

7. A preparation system for the preparation process of the wet-process glass fiber aerogel product according to any one of claims 1 to 6, characterized in that: The invention comprises a stirring reaction kettle, a glue dipping tank, a microwave forming device, a product basket, a heating aging tank and a supercritical drying kettle which are connected and communicated in sequence.

8. The preparation system according to claim 7, characterized in that: The microwave forming device comprises a belt transmission mechanism and a microwave generating mechanism. The belt transmission mechanism is arranged adjacent to the glue dipping tank, and the microwave generating mechanism is arranged above the belt transmission mechanism.

9. The preparation system according to claim 8, characterized in that: The microwave generating mechanism comprises a main microwave generator and a sub-microwave generator, and the main microwave generator and the sub-microwave generator are arranged one after the other.

10. The preparation system according to claim 9, characterized in that: The microwave forming device also includes a microwave control module, a belt control module and a product gel state detection module. The microwave control module is control-connected with the main microwave generator and / or the auxiliary microwave generator at the same time, and is used to control the microwave intensity of the main microwave generator and / or the auxiliary microwave generator. The belt control module is control-connected with the belt transmission mechanism, and is used to control the belt transmission speed of the belt transmission mechanism. The product gel state detection module is arranged at the end of the belt transmission mechanism, and is used to detect whether the product after gel forming is qualified.

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