CN109825091B - Silica gel product and preparation process thereof - Google Patents
Silica gel product and preparation process thereof Download PDFInfo
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- CN109825091B CN109825091B CN201910127477.9A CN201910127477A CN109825091B CN 109825091 B CN109825091 B CN 109825091B CN 201910127477 A CN201910127477 A CN 201910127477A CN 109825091 B CN109825091 B CN 109825091B
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Abstract
The invention provides a silica gel product, wherein silica gel is distributed on a fiber product with a three-dimensional structure, and the filling density of the silica gel is 0.010g/cm3‑0.150g/cm3. The raw material of the silicone gel can be vinyl silicone oil and hydrogen-containing silicone oil which are used as raw materials and are solidified into the silicone gel in a gel state through crosslinking. The distribution form of the silica gel in the fiber product with the three-dimensional structure is one or the mixture of several forms of silica gel particles, continuous silica gel layers and silica gel groups. The silica gel product disclosed by the invention is mainly applied to a slow rebound buffering scene, has good energy absorption, sound absorption and shock absorption functions, and can be applied to the fields of furniture, automobile accessories, sports equipment, medical equipment, clothes and the like.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a silica gel product and a preparation process thereof.
Background
Silicone gels are a class of low cross-link density silicone rubbers without added fillers. Unlike common silicone elastomers, silicone gels are transparent or translucent gels in appearance, have very low mechanical strength, are difficult to measure for hardness, and are generally characterized by their physical strength in terms of penetration. The silicone gel has the advantages of high and low temperature resistance, safety, no toxicity, good biocompatibility, good electrical insulating property and the like of common silicone materials, and also has the performances of gel-state substances such as vibration absorption, adhesion, sealing property and the like. The silica gel has the advantages of good buffer performance, no color, transparency, easy performance adjustment, convenient processing and forming, good fluidity, easy filling of fine structures and the like, and is widely applied to the fields of medical prosthesis, medical dressing, electronic and electrical encapsulation and the like.
The application of the silica gel in the field of daily necessities is also developed rapidly, and the non-toxic and non-irritant properties and the vibration absorption buffering performance of the silica gel are mainly utilized. Silicone gel has been used in the market as a sole cushion, a cushion, an underwear pad, and the like. However, the direct use of the current silicone gel products in daily necessities has the following main disadvantages: firstly, the silica gel product has higher density, and does not meet the light requirement of daily necessities, for example, underwear has certain load after using silica gel as buffer sediment; secondly, the mechanical strength of the silicone gel is very low, and a layer of high-strength material is required to be coated outside the silicone gel for sealing when the silicone gel is used in the field of daily necessities, but the risks of breakage of the coating material, breakage, leakage and failure of the silicone gel still exist; thirdly, the silicon gel has poorer air permeability, and the air permeability is poorer after the outer coating material is sealed, so that the use comfort level is reduced.
The silicone rubber/three-dimensional fiber product is already publicly used, and Chinese patent CN 105696352B discloses a silicon silk cotton product, wherein chemical fiber cotton is soaked by addition type liquid silicone rubber with the Shore hardness of 15-70 degrees, and a two-layer completely synchronous net-shaped elastic structure is formed after curing, so that the defect that the chemical fiber product is easy to deform after being compressed for a long time, used for a long time and washed by water is overcome, and the product has excellent resilience and compression deformation. Chinese patent 201810441654.6 discloses a silicone rubber elastomer/fiber composite material, in particular, a silicone rubber elastomer in the form of particles distributed in a fiber product, the hardness range of the silicone rubber elastomer used is shore hardness (type a) of 1-70 degrees, preferably 5-50 degrees, and the obtained composite material has excellent quick rebound performance and rebound durability. However, the products of the above two inventions are not suitable for applications in scenes requiring high buffering and slow rebound.
Chinese patent 201710315996.9 discloses a silicone gel composite three-dimensional cotton mold cup, which comprises a middle three-dimensional cotton layer, an inner flat cotton layer compounded on the inner side surface of the middle upright cotton layer and an outer flat cotton layer compounded on the outer side surface of the middle upright cotton layer, wherein the inner side surface of the middle upright cotton layer and the inner flat cotton layer, and the outer side surface of the middle upright cotton layer and the outer flat cotton layer are compounded together through silicone gel layers. The invention utilizes the advantages of stability of various physical properties after the silicone gel is thermoset-molded to solve the defect of vertical continuous washing. However, the product can only play a supporting role because the silica gel layer is thin, the cushioning performance mainly depends on the three-dimensional cotton, and the product has poor air permeability and poor comfortable feeling after being worn for a long time.
Disclosure of Invention
The invention aims to provide a silica gel product which has the advantages of good buffering, good air permeability and low density.
Another object of the present invention is to provide a process for preparing the above silicone gel product.
The invention is realized by the following technical scheme:
a silica gel product is prepared by distributing silica gel on fiber product with three-dimensional structure, wherein the packing density of silica gel is 0.010g/cm3-0.150g/cm3。
Compared with a pure silica gel block-shaped or sheet-shaped product, the silica gel product has the advantages that the silica gel is distributed in the three-dimensional structure, and under the filling density, the silica gel product has good buffering performance, good air permeability and low density.
The silicone gel is formed by crosslinking and solidifying vinyl silicone oil and hydrogen-containing silicone oil which are used as raw materials into a gel state. The catalyst mainly comprises platinum group metal catalyst.
Vinyl silicone oil refers to a linear polysiloxane containing a vinyl group directly bonded to a silicon atom in the molecule. The silicone gel is generally a silicone having a dimethylsilyloxy group at both ends of the molecular chain and containing no vinyl group in the chain. Hydrogen-containing silicone oil refers to a linear polysiloxane containing hydrogen atoms directly bonded to silicon atoms in the molecule. In order to reduce the crosslinking density of the cured silicone gel, the silicone gel uses hydrogen-containing silicone oil with low hydrogen content. The platinum group metal catalyst is a metal or metal compound of ruthenium, rhodium, palladium, osmium, iridium, platinum capable of catalyzing hydrosilylation, such as platinum black, chloroplatinic acid, a complex of chloroplatinic acid and divinyltetramethyldisiloxane, and a complex of chloroplatinic acid and divinyltetramethyldisiloxane is more commonly used. The inhibitor is a compound which can inhibit the activity of a hydrosilylation catalyst at a certain temperature, so that after the silica gel raw materials are uniformly mixed, the curing and crosslinking cannot be realized in an operation period, and the curing and crosslinking cannot be influenced under the curing condition. The inhibitor can be selected from vinyl siloxane, alkynol, alkynone, organic amine, organic oxime, phosphine, phosphite, unsaturated amide, maleate, etc., preferably vinyl siloxane and alkynol.
In addition, the formula of the silicone gel can enrich the color of the product, add pigment, enhance the mildew-proof and bacteriostatic effects of the product, add other components such as bacteriostatic agent and the like, enhance the adhesion, add tackifier and the like. These components are added according to specific requirements, and are not necessary.
The raw materials in the formula proportion are uniformly mixed and cured under certain conditions to obtain the silica gel. The curing conditions can be normal temperature curing, heating curing or ultraviolet curing and the like according to different formula designs. The silicone gel is a transparent or translucent soft gel-like substance after curing.
Commercially available silicone gel materials are generally sold in the form of A, B bi-components. A. The component B can be stored for a long time when being placed independently. In use, the A, B components are mixed uniformly in the formula design ratio and the process steps are completed within the formula design operating period.
The microscopic distribution of the silicone gel in the three-dimensional structured fibrous product is: the silica gel is distributed on the surfaces of the fiber filaments of the fiber product and is filled in partial pores among the fiber filaments.
The fiber yarns are of a basic framework structure attached by the organic silicon gel and provide good air permeability; the silica gel is distributed in the internal structure of the fiber product, and provides good slow rebound performance of the product.
The microstructure is as follows: the form of the silica gel is one or a mixture of several forms of silica gel particles, continuous silica gel layers and silica gel groups.
The silica gel particles are distributed as independent small particles under the observation of a microscope, and the volume of the silica gel particles is obviously smaller than that of a cube formed by a plurality of nearest fiber filaments; the continuous silica gel layer can be a silica gel layer coated on the fiber yarns, and can also be a layer of three-dimensional silica gel layer of a surface formed by a plurality of fiber yarns; the silica gel mass is a large silica gel particle having a volume larger than that of a cube formed by the closest plurality of filaments.
The penetration degree of the silicone gel is more than or equal to 10;
preferably, the penetration of the silicone gel is 50 to 250.
The penetration degree of the silicon gel after the silicon gel material is cured is measured according to the method of national standard GB/T4509-2010 (load 100g, temperature 25 ℃ and time 5 s), and the range is more than or equal to 10, preferably 50-250. When the penetration of the selected silicone gel is less than 10, the slow rebound time of the prepared elastic silicone gel product is too short, the energy absorption and shock absorption effects are poor, the comfort level of human body use is poor, and the use effect is poor. The selection of the penetration degree of the silicone gel needs to be adjusted according to the requirements of an application scene, when the penetration degree is too large, the slow rebound time of the prepared slow rebound silicone gel product is too long, the original shape is not easy to recover, and the prepared product is inconvenient to use. The penetration preferably ranges from 50 to 250, which provides a good balance between comfort and convenience of the product.
Preferably, the silicone gel has a packing density of 0.024g/cm3-0.100g/cm3。
The filling density of the silica gel in the fiber product is more than 0.150g/cm3When the filling amount of the silicone gel is too much, the silicone gel blocks the gaps of the product, so that the product has too high density and loses the advantages of light weight and air permeability; the filling density of the silica gel in the fiber product is less than 0.010g/cm3During the process, the filling amount of the silica gel is not enough to provide good slow resilience performance, the slow resilience recovery time is too short, the energy absorption and shock absorption effects are poor, and the use comfort of a human body is not good. The silica gel in the fiber product preferably has a packing density of 0.024 to 0.100g/cm3When the gel product is used, a better balance between comfort and breathability of the finally obtained gel product is achieved.
The density of the fiber product is less than or equal to 0.025g/cm3；
Preferably, the density of the fiber product is 0.012g/cm3-0.020g/cm3。
The density of the fiber product is more than or equal to 0.025g/cm3During the process, the fiber product has high hardness and high fiber density, so that the obtained silicone gel product has short slow rebound time, poor energy absorption and shock absorption effects and poor use comfort of human bodies, and the air permeability of the final product is influenced. The density of the fibrous product is preferably in the range of 0.012-0.020 g/cm3When the hardness of the fiber product is within a proper range, the fiber density of the fiber product is within a proper range, and a better balance is obtained on the comfort and convenience of the finally obtained silicone gel product.
The fiber product is made of chemical fiber and/or natural fiber; the thickest part of the fiber product with the three-dimensional structure is more than or equal to 5 mm;
preferably, the thickest part of the three-dimensional structure fiber product is more than or equal to 10 mm.
The shape of the selected fiber product can be regular geometric shape or irregular shape, and the thickness of the thickest part in the three-dimensional structure is more than or equal to 5 mm. When the thickness of the fiber product is less than 5mm, the prepared silica gel product has small supporting force and is easy to compress to the limit thickness under the action of external force, and the characteristic of slow rebound of the product is difficult to be realized. The maximum thickness of the fiber product is limited by the state of the art of the preparation of fiber products and the subsequent state of the art of the preparation of silicone gel products.
The preparation process of the silica gel product comprises the following steps: soaking the silica gel raw material into the fiber product, separating out more silica gel raw material according to the final filling density established by the silica gel product, and crosslinking and solidifying the silica gel raw material into silica gel under certain conditions to obtain the silica gel product.
In the preparation process, how to control the filling density of the silica gel and the microstructure and distribution of the silica gel is the key of the good comfort performance of the final product. Is mainly adjusted by controlling the viscosity of the solvent-free silicone gel raw material, the amount of the raw material remaining in the fiber product before curing and the curing conditions.
Wherein the curing conditions of the silica gel raw material comprise normal temperature curing, heating curing, ultraviolet curing and the like; separating the more than one silica gel raw material by at least one of centrifugation, air blowing, extrusion and the like.
The silicone gel raw material used in the invention is a solvent-free silicone gel raw material. The solvent-free silica gel raw material is used, so that the retention amount of the silica gel raw material in the fiber product can be better controlled, and the process has an environmental protection value.
More preferably, the viscosity of the solvent-free silica gel raw material is less than or equal to 5000 mPas. If the viscosity is higher than 5000, the silica gel raw material is not easy to permeate into the fiber product and is not easy to extrude to control the packing density, and meanwhile, too high viscosity of the silica gel raw material can cause the silica gel to gather into large particles in the fiber product, thereby affecting the air permeability and the slow rebound performance.
The silicon gel product has good balance of the buffering performance and the air permeability when the air permeability and the slow rebound recovery time are reached.
The invention has the following beneficial effects:
according to the invention, the silica gel is distributed in the three-dimensional fiber product, and the conditions such as the micro-light form of the silica gel, the filling density of the silica gel, the density of the fiber product and the like are controlled, so that the silica gel product is obtained, has good air permeability, good buffering performance, good sound absorption performance, good slow resilience performance and proper density, and is suitable for being applied to the fields of furniture, automobile accessories, sports equipment, medical equipment, clothes and the like.
Detailed Description
The present invention will be further illustrated by the following specific embodiments, and the following examples are illustrative of the present invention and are not intended to limit the present invention.
The raw materials used in the examples and comparative experiments are, but not limited to, the following:
silicon gel: JH-6500 series of organosilicon gel produced by Guangdong polymerization science and technology corporation, with penetration degree adjustable within 5-250, AB dual-component formula, before use, AB component is mixed uniformly at a ratio of 1:1 and then used in an operation period, curing condition is 150 deg.C, 3min, and silicon gel is obtained after curing.
Fiber products: the commercially available polyester fiber upright cotton has different density specifications, and the density can be increased by a hot pressing method.
Examples and comparative examples the preparation of silicone gel articles was as follows: soaking the silica gel raw material into the fiber product, separating out more silica gel raw material according to the final filling density established by the silica gel product, and crosslinking and solidifying the silica gel raw material into silica gel under certain conditions to obtain the silica gel product.
The performance test method comprises the following steps:
(1) penetration degree: according to the method of the national standard GB T4509-2010 asphalt penetration measuring method, 200g of silica gel raw material is placed in a 250mL beaker (the diameter of the cup body is 71mm, and the height is 97 mm), and after the silica gel is directly and completely cured under the curing condition, the silica gel raw material is detected on a penetration detector meeting the standard. The test conditions were 25 ℃, load 100g, time 5s, three times at different positions, and the average was taken.
(2) Density of the fiber product: weighing a sample mass m of a raw fiber material0Measuring the length, width and thickness of the composite material, and calculating the volume V of the composite material, wherein the density = m of the fiber product0/V。
(3) Packing density of silicone gel: weighing a sample mass m of a raw fiber material0And the mass m of the composite material sample obtained1Measuring the length, width and thickness of the composite material, and calculating the volume V and the filling density = (m) of the composite material1-m0)/V。
(4) Slow rebound recovery time: referring to the method of national standard GBT26392-2011 determination of recovery time of slow-rebound foam, the size of a prepared elastic silicon gel product sample is 400mm multiplied by 100mm, and after the preparation is finished and the sample is placed at room temperature for 7 days, the sample is determined by using a slow-rebound foam recovery time tester (YMHT-01, produced by Nanjing Anyang measurement and control technology Co., Ltd.).
(5) And (3) testing air permeability: the test was carried out by using a fully automatic fabric air permeability tester (YG 461E-II, manufactured by Wenzhou Limited company for high test) according to the method of GB-T5453-1997 determination of textile fabric air permeability, which is the national standard, and the experimental area is 20cm2The pressure drop was 200 Pa.
Table 1: examples and comparative examples silicone gel articles parameters and performance test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| Density of fiber product, g/cm3 | 0.010 | 0.012 | 0.015 | 0.020 | 0.025 | 0.015 | 0.015 |
| Penetration of silica gel | 150 | 150 | 150 | 150 | 150 | 150 | 150 |
| Silica gel packing Density, g/cm3 | 0.059 | 0.061 | 0.060 | 0.058 | 0.059 | 0.010 | 0.024 |
| Slow rebound recovery time, second | 5.5 | 5.1 | 4.6 | 3.9 | 3.1 | 2.1 | 3.4 |
| Air permeability, mm/s | 495 | 453 | 427 | 401 | 368 | 585 | 522 |
TABLE 1
| Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Comparative example 1 | Comparative example 2 | |
| Density of fiber product, g/cm3 | 0.015 | 0.015 | 0.020 | 0.020 | 0.020 | 0.010 | 0.020 |
| Penetration of silica gel | 150 | 150 | 10 | 50 | 200 | 150 | 150 |
| Silica gel packing Density, g/cm3 | 0.098 | 0.143 | 0.060 | 0.060 | 0.062 | 0.008 | 0.167 |
| Slow rebound recovery time, second | 6.5 | 7.8 | 6.9 | 5.6 | 3.5 | <2.0 | 8.1 |
| Air permeability, mm/s | 378 | 315 | 406 | 403 | 397 | 613 | 251 |
Examples 1 to 5, controlling the density of the fiber product as a variable during the test, found that the greater the density of the fiber product, the lower the air permeability and the higher the rebound speed, and in order to obtain a good slow rebound time, the density of the fiber product is preferably 0.012g/cm3-0.020g/cm3。
In examples 4/10-12, the penetration of silicone gel was controlled as a variable, and it was found that the penetration of silicone gel was high and the rebound rate was high, and that the rebound rate was suitable when the penetration of silicone gel was 50-250.
Examples 3/6-9, wherein the packing density of the silicone gel was controlled as a variable, it was found that the larger the packing density of the silicone gel, the smaller the air permeability and the slower the rebound velocity, and in order to obtain the balance between air permeability and slow rebound velocity, it is preferable that the packing density of the silicone gel be 0.024g/cm3-0.100g/cm3。
Claims (7)
1. A silica gel product is characterized in that silica gel is distributed on a fiber product with a three-dimensional structure, and the silica gel is distributed on the surface of fiber yarns of the fiber product and filled in partial pores among the fiber yarns in a form of one or a mixture of silica gel particles, continuous silica gel layers and silica gel clusters; the silicone gel is vinylSilicone oil and hydrogen-containing silicone oil are used as raw materials and are solidified into silicone gel in a gel state through crosslinking; the packing density of the silica gel was 0.010g/cm3-0.150g/cm3(ii) a The penetration degree of the silicone gel is 10-250; the density of the fiber product is 0.012g/cm3-0.020g/cm3。
2. The silicone gel article of claim 1, wherein the silicone gel has a penetration of 50-250.
3. The silicone gel article of claim 1, wherein the silicone gel has a packing density of 0.024g/cm3-0.100g/cm3。
4. The silicone gel article of claim 1, wherein said fiber article is made of chemical fibers and/or natural fibers; the three-dimensional structure of the fiber product is a regular three-dimensional shape or an irregular three-dimensional shape.
5. Silicone gel product according to claim 4, characterised in that the fibre product of the three-dimensional structure has a maximum thickness of ≥ 5 mm.
6. Silicone gel product according to claim 5, characterised in that the fibre product of the three-dimensional structure has a maximum thickness of 10mm or more.
7. A process for preparing a silicone gel article according to any of claims 1 to 6, comprising the steps of: soaking a solvent-free silica gel raw material into a fiber product, separating redundant silica gel raw materials according to the final filling density established by the silica gel product, and crosslinking and curing the silica gel raw materials into silica gel under certain conditions to obtain a silica gel product; the curing condition of the silica gel raw material is at least one of normal temperature curing, heating curing and ultraviolet curing; separating out redundant silica gel raw materials by at least one of the modes of centrifugation, air blowing and extrusion; the viscosity of the solvent-free silica gel raw material is less than or equal to 5000mPa & s.
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Effective date of registration: 20230413 Address after: Room 207, 2nd Floor, Building 1, Dinghu Shuangchuangyuan, No. 15 Guanyan Avenue, 30 Guicheng New City, Dinghu District, Zhaoqing City, Guangdong Province, 526070 Patentee after: Guangdong kangbain Technology Co.,Ltd. Address before: 528400 906, building 13, Jiankang Huacheng, Torch Development Zone, Zhongshan City, Guangdong Province Patentee before: Sun Fei |