CN111253664B - Preparation method of aerogel foamed polyethylene cotton composite material - Google Patents
Preparation method of aerogel foamed polyethylene cotton composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of an aerogel foaming polyethylene cotton composite material, and belongs to the technical field of heat preservation and insulation chemical materials. The preparation method comprises the following steps: (1) mixing a silicon source precursor, a solvent, water and a catalyst, preparing a silicon dioxide sol with a space three-dimensional network structure by a sol-gel method, adding a surface modifier, and uniformly mixing to prepare a modified nano porous silicon dioxide sol; (2) mixing low-density polyethylene powder with the modified sol obtained in the step one (1), adding a surface modifier, an initiator and an organic auxiliary agent, and mixing, granulating and drying to obtain polyethylene-aerogel composite master batches; (3) adding the polyethylene-aerogel composite master batch, the antistatic agent, the foaming agent and the talcum powder into a high-pressure reaction kettle, foaming, extruding and molding, cooling, re-expanding and finally rolling to obtain the foamed polyethylene cotton composite material.
Description
Technical Field
The invention belongs to the technical field of heat preservation and insulation chemical materials, and relates to a preparation method of an aerogel foaming polyethylene cotton composite material.
Background
Foamed polyethylene, abbreviated as EPE, is a polymer foam, generally composed of Low Density Polyethylene (LDPE) which is physically foamed to generate numerous independent cells. The polyethylene foam has the advantages of light weight, environmental protection, heat insulation, heat preservation, sound insulation, shock resistance, water insulation, moisture resistance, strong toughness, good plasticity, strong impact resistance and the like, and is widely applied to the fields of sound insulation, heat preservation materials, high-grade furniture, household appliances, instruments and meters, craft gifts, wooden products, glass ceramics, building water resistance, carpet interlayers, travel bags, precision parts and the like. The adhesive products of polyethylene foam and various fabrics are good interior materials for various vehicles and living rooms. The composite product of the polyethylene foam cotton and the aluminum foil or the aluminum-plated film has excellent anti-infrared ray and ultraviolet ray capabilities and heat preservation performance, and is a necessary product for shading the sun of chemical equipment refrigerators, cold chain container liners, heat preservation boxes in the refrigeration and transportation process of foods and medicines, and camping equipment and automobiles. In addition, the polyethylene foam has the advantage of repeated recycling, does not pollute the environment, and has the effect of environmental protection. With the progress of science and technology, polyethylene foam is showing its superiority more and more, and the production application is expanding and innovated continuously.
Aerogel, known as Aerogel, is an inorganic nanoporous material, which is a solid material having a three-dimensional network structure formed by crosslinking nanoscale silica particles with each other and filled with gaseous dispersion media in pores. The aerogel has rich nano-scale holes, typical pore size is 2-50 nm, and the aerogel has the characteristics of low density (0.003-0.5 g/cm 3), high porosity (80-99.8%), high specific surface area (1000 m 2/g), good heat insulation performance (the heat conductivity is as low as 0.015W/m.K at normal temperature) and the like. The average pore size of the aerogel is smaller than the average free path of air molecules, and the aerogel has a fine nanometer solid framework. The unique nanostructure effectively inhibits heat conduction and convection heat transfer, and therefore has thermal conductivity far lower than that of the traditional thermal insulation material, even lower than that of static air, and is considered as a 'super insulation material'. In addition, the components of the silica aerogel are inorganic silica nanoparticles, so the silica aerogel has the characteristics of non-combustibility, long service life, no pollution, transparency, hydrophobicity and the like. At present, silica aerogel products are applied to heat insulation in the fields of steam pipelines, petrochemical industry, ships, vehicles, deep cooling heat insulation, lighting and heat insulation systems of building roofs and curtain walls, building external walls and internal walls and the like.
However, the application of the traditional polyethylene foam in the field of heat insulation still has some problems. On one hand, the bubble structure obtained by physically foaming the low-density polyethylene is a non-crosslinked closed pore structure, the size is in the micrometer level and is larger than the mean free path of air molecules, and therefore, the heat transfer inhibition effect on gas molecules is not ideal. Therefore, the polyethylene foam has unsatisfactory heat insulation effect and high thermal conductivity (the thermal conductivity at room temperature is about 0.041W/m.K). On the other hand, the polyethylene foam cotton is made of organic polyethylene, and is used as a heat insulation material, so that the polyethylene foam cotton is poor in flame retardant property, and is easy to burn when meeting a fire source, and toxic smoke is generated to cause huge threat and damage to life safety of people. If the aerogel material with excellent heat insulation and flame retardant properties can be compounded in situ, the polyethylene foam cotton/aerogel composite heat insulation material with extremely low heat conductivity, good heat insulation effect, good mechanical properties, certain flame retardancy, economy and durability is formed, and the problems are solved to a great extent.
Disclosure of Invention
The invention aims to provide a preparation method of an aerogel foaming polyethylene cotton composite material. Aims to provide a foaming polyethylene cotton composite material which has extremely low heat conductivity, good heat preservation effect, good mechanical property, certain flame retardance, economy and durability.
In order to solve the technical problems, the preparation method of the aerogel foaming polyethylene cotton composite material comprises the following steps:
(1) mixing a silicon source precursor, a solvent, water and a catalyst, preparing nano porous silica sol by a sol-gel reaction synthesis method, adding a surface modifier, and mixing uniformly to prepare modified nano porous silica sol;
(2) mixing low-density polyethylene powder with the modified nano-porous silica sol obtained in the step one (1), adding a surface modifier, an initiator and an organic assistant, and mixing, granulating and drying to obtain polyethylene-aerogel composite master batches;
(3) adding the polyethylene-aerogel composite master batch obtained in the step two (2), the antistatic agent, the foaming agent and the talcum powder into a high-pressure reaction kettle, foaming, extruding and molding, cooling, re-extending and finally rolling to obtain a foamed polyethylene cotton composite material;
the solvent in the step (1) is one or more of ethanol, methanol, acetone and isopropanol, the organic auxiliary agent in the step (2) is polyethylene wax, and the molecular weight range is 1000-4000.
In one embodiment of the present invention, in step (1), the silicon source precursor, the solvent, the water, and the catalyst are mixed, and a volume ratio of the silicon source precursor, the solvent, the water, and the catalyst is 1: (1-5): (0.1-0.5): (0.01-0.1);
and (2) adding a surface modifier in the step (1) and uniformly mixing, wherein the addition amount of the surface modifier is 5-10 parts of the surface modifier per 100 parts of the silica sol.
In one embodiment of the present invention, the silicon source precursor in step (1) is one or more of tetraethyl orthosilicate, tetramethyl orthosilicate, industrial water glass, silica sol and poly-silicon.
In one embodiment of the present invention, the catalyst in step (1) is an acidic catalyst or a basic catalyst, the acidic catalyst is one or more of hydrochloric acid, nitric acid, acetic acid and oxalic acid, and the basic catalyst is one or more of ammonia, sodium carbonate and sodium hydroxide.
In one embodiment of the present invention, the preparation of the nanoporous silica sol in step (1) by the sol-gel reaction synthesis method is to mix and stir the precursor of the silicon source, the solvent, the water and the catalyst at room temperature, wherein the stirring speed is 300-500 rpm, and the stirring time is 30-60 min.
In one embodiment of the invention, the low-density polyethylene powder, the nano-porous silica sol, the surface modifier, the initiator and the organic auxiliary agent in the step (2) are prepared from the following components in parts by weight: 100: (3-35): (0.05-0.15): 2.4: (0.5-2).
In one embodiment of the invention, the SiO in the nanoporous silica sol is modified 2 The mass ratio of the content to the polyethylene is 0.9-10.5%.
In one embodiment of the present invention, the surface modifier in step (2) is any one or more of vinyltriethoxysilane or aminopropyltriethoxysilane or mercaptopropyltrimethoxysilane.
The silane coupling agent can graft the silica aerogel nanoparticles with polyethylene chains, and plays a role in surface modification and dispersion of the nanoporous silica sol nanoparticles.
In one embodiment of the present invention, the initiator in step (2) is dicumyl peroxide, and the initiation reaction temperature is 120-150 ℃.
In one embodiment of the present invention, the mixing and granulating in step (2) is to put the reactants into a mixer, mix them at 120-150 ℃ for 30-50 minutes, and then put them into a twin-screw granulator for granulation.
In one embodiment of the present invention, the drying in the step (2) is performed at 45-60 ℃ for 2-4 hours.
In one embodiment of the present invention, the polyethylene/aerogel composite masterbatch obtained in step (2) is plastic particles with uniform size, and the diameter is about 3-5 mm.
In one embodiment of the present invention, in step (3), the polyethylene/aerogel master batch, the antistatic agent, the foaming agent, and the talc powder are added into the high-pressure reactor together, and the mass fraction ratio of the polyethylene/aerogel master batch, the antistatic agent, the foaming agent, and the talc powder is: 100: (1-5): (5-10): (0.1-5).
In one embodiment of the present invention, the antistatic agent in step (3) is ethylene oxide and polyethylene oxide, and 0.3 to 2 parts by mass of the antistatic agent is added to 100 parts of the polyethylene/aerogel master batch.
In one embodiment of the present invention, the talc powder in step (3) is added in an amount of: 0.2-1 part by mass of talcum powder is added into every 100 parts of polyethylene/aerogel master batch.
In one embodiment of the present invention, the blowing agent in step (3) is one or more of butane, carbon dioxide, supercritical nitrogen and supercritical carbon dioxide.
In one embodiment of the present invention, the foaming in step three (3) is foaming at a temperature of 100 ℃ and 140 ℃ and a pressure of 10-12 MPa.
In one embodiment of the invention, the foamed polyethylene cotton composite material is prepared by using SiO 2 The mass ratio of the aerogel is 0.9-9.5%.
The beneficial technical effects are as follows:
(1) the invention provides a foamed polyethylene cotton composite material which has low thermal conductivity (the thermal conductivity is less than 0.035W/m.K), good heat preservation effect, good mechanical property, certain flame retardance, economy and durability;
(2) according to the preparation method of the foamed polyethylene cotton composite material, provided by the invention, the nano porous silica sol obtained by hydrolysis and polycondensation of the silicon source precursor is subjected to in-situ compounding with the polyethylene powder, so that the uniform micro compounding of the pearl cotton and the aerogel can be realized, and the heat preservation and insulation effects of the pearl cotton are improved. The material disclosed by the invention is simple in preparation method, low in cost, low in density, low in heat conductivity, certain in flame retardance, good in stability, green, environment-friendly, overall hydrophobic and long in service life, can be widely applied to the fields of chemical equipment refrigerators, cold chain container liners, insulation boxes in the processes of food and medicine refrigerated transportation and the like, ensures the temperature stability in the cold chain transportation process, and avoids the product quality from being endangered by temperature change.
Drawings
FIG. 1 is an SEM image of a prior art foamed polyethylene wool;
FIG. 2 is an SEM image of a foamed polyethylene wool composite according to one embodiment of the invention;
fig. 3 is an SEM image of silica aerogel in the foamed polyethylene wool composite according to one embodiment of the present invention.
Detailed Description
Example 1: the preparation method of the aerogel foamed polyethylene cotton composite material comprises the following steps:
step one, tetraethyl orthosilicate, ethanol, water and 0.01mol/L hydrochloric acid serving as a catalyst are mixed according to a volume ratio of 1: 2: 0.2: 0.02, and stirring for 30 minutes at room temperature through a sol-gel process to obtain the nano porous silica sol. Then, hexamethyldisiloxane is added as a surface modifier, 8 parts of the surface modifier are added to each 100 parts of the sol, and the mixture is stirred for 30 minutes at room temperature to obtain the modified nano-porous silica sol. Then, the modified nano-porous silica sol is diluted to SiO by ethanol 2 The solid content is 30wt% for later use.
Step two, mixing the low-density polyethylene powder and the modified nano-porous silica sol obtained in the step one (1) according to the mass ratio of 100: 10 are mixed. Then sequentially adding vinyl triethoxysilane as a dispersing agent and a surface modifier, dicumyl peroxide as an initiator and polyethylene wax with molecular weight of 3000 as an organic auxiliary agent, mixing for 30 minutes at 130 ℃, putting into a double-screw granulator for granulation, and drying for 3 hours at 50 ℃ to obtain the polyethylene/aerogel composite master batch. Wherein the low-density polyethylene powder, the silica sol, the silane coupling agent, the dicumyl peroxide and the polyethylene wax are prepared from the following components in parts by mass: 100: 10: 0.1: 2.4: 1, the mass fraction of the silicon dioxide aerogel in the polyethylene/aerogel composite master batch obtained by granulation is about 2.9 wt%.
And step three, adding the polyethylene/aerogel master batch obtained by granulation in the step two (2), the antistatic agent, the foaming agent and the talcum powder into a high-pressure reaction kettle, and performing foaming, extrusion molding, cooling, re-extension and final winding to obtain the polyethylene cotton/aerogel composite type heat insulation material. Wherein, 5 parts of antistatic agent foaming agent, 8 parts of butane foaming agent and 2 parts of talcum powder are added into each 100 parts of polyethylene/aerogel master batch, the foaming temperature is 120 ℃, and the pressure is 11 MPa.
The mass fraction of the aerogel in the finally obtained foamed polyethylene cotton composite material is about 2.9wt%, and the room temperature thermal conductivity of the foamed polyethylene cotton composite material is measured by a steady-state heat flow method (the instrument model is relaxation-resistant HFM 446 Lambda), so that the result is 0.030W/m.K.
Example 2
The present embodiment is basically the same as embodiment 1, except that the silicon source precursor in the present embodiment is a silica sol. The preparation method comprises the following steps:
step one, mixing silica sol, water and 0.01mol/L hydrochloric acid serving as a catalyst according to a volume ratio of 1: 1: 0.02, and stirring for 30 minutes at room temperature through a sol-gel process to obtain the nano porous silica sol. Then, hexamethyldisiloxane was added as a surface modifier, 10 parts of the surface modifier was added to 100 parts of the sol, and the mixture was stirred at room temperature for 30 minutes to obtain a modified silica sol. Then, the modified silica sol is diluted to SiO by deionized water 2 The solid content is 30wt% for later use.
Step two, mixing the low-density polyethylene powder and the modified silica sol obtained in the step one (1) according to the mass ratio of 100: 10 are mixed. Then sequentially adding vinyl triethoxysilane as a dispersing agent and a surface modifier, dicumyl peroxide as an initiator and polyethylene wax with molecular weight of 3000 as an organic auxiliary agent, mixing for 30 minutes at 130 ℃, putting into a double-screw granulator for granulation, and drying for 3 hours at 50 ℃ to obtain the polyethylene/aerogel composite master batch. Wherein the low-density polyethylene powder, the silica sol, the silane coupling agent, the dicumyl peroxide and the polyethylene wax are prepared from the following components in parts by mass: 100: 10: 0.1: 2.4: 1, the mass fraction of the silicon dioxide aerogel in the polyethylene/aerogel composite master batch obtained by granulation is about 2.9 wt%.
And step three, adding the polyethylene/aerogel master batch obtained by granulation in the step two (2), the antistatic agent, the foaming agent and the talcum powder into a high-pressure reaction kettle, and performing foaming, extrusion molding, cooling, re-extension and final winding to obtain the foamed polyethylene cotton composite material. Wherein, 5 parts of antistatic agent foaming agent, 8 parts of butane foaming agent and 2 parts of talcum powder are added into each 100 parts of polyethylene/aerogel master batch, the foaming temperature is 120 ℃, and the pressure is 11 MPa.
Example 3
The present example is basically the same as example 2, except that the amount of silica sol in step two (2) in the present example is different, and the mass ratio of the low-density polyethylene powder to the silica sol is 100: and 20, the mass fraction of the silicon dioxide aerogel in the polyethylene/aerogel composite master batch obtained by granulation is 5.6 wt%. The mass fraction of aerogel in the prepared foamed polyethylene cotton composite material is about 5.6 wt%.
Example 4
The present example is basically the same as example 2, except that the amount of silica sol in step two (2) in the present example is different, and the mass ratio of the low-density polyethylene powder to the silica sol is 100: 30, the mass fraction of the silicon dioxide aerogel in the polyethylene/aerogel composite master batch obtained by granulation is about 8.3 wt%. The mass fraction of aerogel in the prepared foamed polyethylene cotton composite material is about 8.3 wt%.
Example 5
This example is substantially the same as example 1, except that in step one (1) of this example, 10M ammonia water was used as a catalyst, and tetraethyl orthosilicate, ethanol, water, and catalyst ammonia water were mixed in a volume ratio of 1: 2: 0.2: 0.05.
example 6
This example is substantially the same as example 1 except that in this example, the amount of ethanol as a solvent in the first step (1) is different, and tetraethyl orthosilicate, ethanol, water, and catalyst hydrochloric acid are mixed in a volume ratio of 1: 5: 0.2: 0.02.
example 7
The present embodiment is substantially the same as embodiment 1, except that, in the present embodiment, the silane coupling agent in step two (2) is different, aminopropyltriethoxysilane is selected as the silane coupling agent, and the mass part ratios of the low-density polyethylene powder, the silica sol, the aminopropyltriethoxysilane, the dicumyl peroxide and the polyethylene wax are as follows: 100: 10: 0.1: 2.4: 1.
example 8
The embodiment is basically the same as the embodiment 1, except that the silane coupling agent in the step two (2) is different, mercaptopropyl trimethoxysilane is selected as the silane coupling agent, and the mass part ratio of the low-density polyethylene powder, the silica sol, the mercaptopropyl trimethoxysilane, the dicumyl peroxide and the polyethylene wax is as follows: 100: 10: 0.1: 2.4: 1.
in the comparative example, the preparation method of the non-compounded pearl wool thermal insulation material is as follows:
(1) step one, compared to example 1, there is no step one.
(2) And step two, mixing low-density polyethylene powder, dicumyl peroxide and polyethylene wax with the molecular weight of 3000 at 130 ℃ for 30 minutes, putting the mixture into a double-screw granulator for granulation, and drying the mixture for 3 hours at 50 ℃ to obtain the polyethylene master batch. Wherein the low-density polyethylene powder dicumyl peroxide and the polyethylene wax comprise the following components in parts by weight: 100: 2.4: 1.
(3) and step three, adding the polyethylene master batch obtained by granulation in the step two (2), the antistatic agent, the foaming agent and the talcum powder into a high-pressure reaction kettle, and performing foaming, extrusion molding, cooling, re-extension and final winding to obtain the non-composite pearl cotton heat-insulating material. Wherein, every 100 parts of polyethylene master batch is added with 5 parts of antistatic agent foaming agent, 8 parts of butane foaming agent and 2 parts of talcum powder, the foaming temperature is 120 ℃, and the pressure is 11 MPa.
The room temperature thermal conductivity of the finally obtained non-compounded pearl cotton is tested by a steady-state heat flow method (the instrument model is relaxation-resistant HFM 446 Lambda), and the result is 0.041W/m.K.
Claims (15)
1. The preparation method of the aerogel foaming polyethylene cotton composite material is characterized by comprising the following steps:
(1) mixing a silicon source precursor, a solvent, water and a catalyst, preparing nano porous silica sol by a sol-gel reaction synthesis method, adding a surface modifier, and uniformly mixing to prepare modified nano porous silica sol;
(2) mixing low-density polyethylene powder with the modified nano-porous silica sol obtained in the step (1), adding a surface modifier, an initiator and an organic auxiliary agent, and mixing, granulating and drying to obtain polyethylene-aerogel composite master batches;
(3) adding the polyethylene-aerogel composite master batch obtained in the step (2), an antistatic agent, a foaming agent and talcum powder into a high-pressure reaction kettle, and performing foaming, extrusion molding, cooling, re-extension and final winding to obtain a foamed polyethylene cotton composite material;
the solvent in the step (1) is one or more of ethanol, methanol, acetone and isopropanol, the organic auxiliary agent in the step (2) is polyethylene wax, and the molecular weight range is 1000-4000.
2. The preparation method of the aerogel-foamed polyethylene cotton composite material according to claim 1, wherein in the step (1), the silicon source precursor, the solvent, water and the catalyst are mixed, and the volume ratio of the silicon source precursor, the solvent, the water and the catalyst is 1: (1-5): (0.1-0.5): (0.01-0.1);
and (2) adding a surface modifier in the step (1) and uniformly mixing, wherein the addition amount of the surface modifier is 5-10 parts of the surface modifier per 100 parts of the silica sol.
3. The preparation method of the aerogel foamed polyethylene wool composite material according to claim 1, wherein the silicon source precursor in the step (1) is one or more of tetraethyl orthosilicate, tetramethyl orthosilicate, industrial water glass, silica sol and poly-silicon.
4. The method for preparing the aerogel expanded polyethylene cotton composite material according to claim 1, wherein the catalyst in step (1) is an acidic catalyst or a basic catalyst, the acidic catalyst is one or more of hydrochloric acid, nitric acid, acetic acid and oxalic acid, and the basic catalyst is one or more of ammonia water, sodium carbonate and sodium hydroxide.
5. The preparation method of the aerogel foamed polyethylene cotton composite material according to claim 1, wherein the nano-porous silica sol prepared by the sol-gel reaction synthesis method in the step (1) is prepared by mixing and stirring a silicon source precursor, a solvent, water and a catalyst at room temperature, wherein the stirring speed is 300-.
6. The preparation method of the aerogel foamed polyethylene cotton composite material according to claim 1, wherein the mass part ratio of the low-density polyethylene powder, the nano-porous silica sol, the surface modifier, the initiator and the organic auxiliary agent in the step (2) is as follows: 100: (3-35): (0.05-0.15): 2.4: (0.5-2).
7. The method for preparing the aerogel foamed polyethylene wool composite according to claim 1, wherein SiO in the modified nanoporous silica sol 2 The mass ratio of the content to the polyethylene is 0.9-10.5%.
8. The method for preparing the aerogel foamed polyethylene wool composite according to claim 1, wherein the surface modifier in step (2) is any one or more of vinyltriethoxysilane or aminopropyltriethoxysilane or mercaptopropyltrimethoxysilane.
9. The method for preparing the aerogel foamed polyethylene wool composite material as claimed in claim 1, wherein the initiator in step (2) is dicumyl peroxide, and the initiation reaction temperature is 120-150 ℃.
10. The method for preparing the aerogel expanded polyethylene cotton composite material according to claim 1, wherein the mixing and granulating in the step (2) are carried out by putting the reactants into a mixing mill, mixing at 120-150 ℃ for 30-50 minutes, and then putting into a twin-screw granulator for granulation.
11. The preparation method of the aerogel foamed polyethylene cotton composite material according to claim 1, wherein the polyethylene-aerogel master batch, the antistatic agent, the foaming agent and the talcum powder are added into the high-pressure reaction kettle together in the step (3), and the mass fraction ratio of the polyethylene-aerogel master batch to the antistatic agent to the foaming agent to the talcum powder is as follows: 100: (1-5): (5-10): (0.1-5).
12. The method for preparing the aerogel foamed polyethylene wool composite according to claim 1, wherein the foaming agent in the step (3) is one or more of butane, carbon dioxide, supercritical nitrogen and supercritical carbon dioxide.
13. The preparation method of the aerogel foamed polyethylene wool composite material as claimed in claim 1, wherein the foaming in step (3) is carried out at the temperature of 100-140 ℃ and the pressure of 10-12 MPa.
14. The method for preparing the aerogel-foamed polyethylene wool composite material according to any one of claims 1 to 13, wherein the mass ratio of aerogel in the prepared foamed polyethylene wool composite material is 0.9 to 10.5%.
15. The application of the foamed polyethylene cotton composite prepared by the preparation method of the aerogel foamed polyethylene cotton composite according to claim 14 is characterized in that the foamed polyethylene cotton composite is applied to heat-insulation distribution boxes and greenhouse heat-insulation films.
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| CN110294867B (en) * | 2019-07-05 | 2021-11-19 | 四川农业大学 | Novel nano-silicon aerogel packaging composite film and preparation method thereof |
| CN110791004B (en) * | 2019-11-18 | 2022-03-22 | 界首市天路包装材料有限公司 | Environment-friendly degradable heat-insulation food packaging bag |
| CN111533990B (en) * | 2020-04-07 | 2022-08-23 | 北京弘暖纤科技有限公司 | Heat insulation master batch and preparation method thereof |
| CN111532589A (en) * | 2020-06-04 | 2020-08-14 | 罗瑞尔纳米合成材料(江苏)有限公司 | Recyclable functional heat preservation box made of nano synthetic material |
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