CN111040279A - Preparation method of polyolefin microporous breathable film - Google Patents
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- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2323/08—Copolymers of ethene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention relates to a preparation method of a polyolefin microporous breathable film; the method of the invention is improved on the basis of the prior art, changes the casting process into the film blowing process, and unexpectedly finds that when the polyolefin base material with a specific formula is adopted and the film blowing process adopts specific parameters, the microporous breathable film with lower basis weight and excellent high moisture permeability can be obtained; moreover, the polyolefin microporous breathable film disclosed by the invention has the advantages that the hydrostatic pressure resistance is further improved, the anti-seepage performance is better, and the safety of the sanitary product in use can be more effectively ensured.
Description
Technical Field
The invention relates to a preparation method of a polyolefin microporous breathable film, belonging to the technical field of organic polymer films.
Background
In recent years, various personal hygiene products are increasingly popularized; the use of a base film with humidity regulation function, namely a polyolefin microporous breathable film, in sanitary articles is becoming more and more popular; the main purpose is to improve the damp stuffiness feeling of the sanitary article during use.
Chinese patent CN106397918B discloses a polyolefin microporous breathable film with high moisture permeability, which realizes the basis weight range of 18-25 gsm, and the water vapor transmission rate in GB/T1037 test can reach more than 8000g/m 2.24 h, and the first hour water vapor transmission rate of the film can reach 1000g/m 2.h. The polyolefin microporous breathable film with high moisture permeability effectively improves the humidity adjusting capacity of the hygienic product and improves the use experience of users aiming at the use environment of the hygienic product.
However, under the current environment of 'plastic limitation' and 'plastic reduction', the demand of reducing the usage amount of plastic products is more and more prominent, and sanitary products are no exception. Therefore, on the premise of not reducing material performance, whether the gram weight (also called basis weight) of the polyolefin microporous breathable film can be reduced or not and the usage amount of plastics can be reduced is an urgent demand of hygienic product enterprises.
In summary, it is an urgent technical problem in the art to solve how to reduce the basis weight and the usage amount of plastic while maintaining the high moisture permeability of the microporous polyolefin breathable film.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides, in one aspect, a method for preparing a polyolefin microporous breathable film, wherein,
the preparation method comprises the following steps:
step 1), blending and extruding: mixing a polyolefin base material and an inorganic filler according to a weight ratio of 9: 11-1: 1, preparing a composite material through a blending extrusion process, and obtaining composite material particles through a re-granulation process;
the polyolefin base material is a mixture of metallocene polyethylene and linear low-density polyethylene according to the weight ratio of 1: 1; the metallocene polyethylene has a melt index of 0.25-1.5 g/10min and a density of 0.918-0.927 g/cm3(ii) a The linear low density polyethylene has a melt index of 0.8 to 1g/10min and a density of 0.917 to 0.935g/cm3；
The inorganic filler is one or a mixture of more of calcium carbonate, calcium oxide, calcium hydroxide or titanium dioxide; more than 98% of the particles of the inorganic filler are distributed in the particle size of 1-8 mu m;
step 2), film blowing and extrusion: preparing the composite material particles obtained in the step 1) into a film by a film blowing extrusion process; wherein the melt temperature of the melting stage of the blown film extrusion process is 200-230 ℃;
step 3), stretching: stretching the film obtained in the step 2) by a uniaxial one-step method, wherein the stretching ratio is 3.1-5.5;
step 4), high-temperature heat setting treatment: and (3) carrying out high-temperature thermal setting treatment on the stretched film obtained in the step 3), and controlling the treatment temperature to be 100-120 ℃ to obtain the polyolefin microporous breathable film.
Preferably, the inorganic filler is calcium carbonate and titanium dioxide in a weight ratio of 50: 1.
The invention also provides the application of the polyolefin microporous breathable film obtained by the preparation method in disposable sanitary products.
Preferably, the polyolefin microporous breathable film is applied to disposable sanitary products as an anti-leakage bottom film or an anti-leakage functional layer.
Preferably, the disposable sanitary article comprises a sanitary napkin, panty liner, panty diaper, pull-up diaper, adult panty diaper, disposable bed pad, incontinence pad, nursing pad or spill-proof pad.
The preparation method of the polyolefin microporous breathable film is improved on the basis of the prior art, changes the casting process into the film blowing process, and unexpectedly finds that when the polyolefin base material with a specific formula is adopted and the film blowing process adopts specific parameters, the microporous breathable film with lower basis weight and excellent high moisture permeability can be obtained; moreover, the polyolefin microporous breathable film disclosed by the invention has the advantages that the hydrostatic pressure resistance is further improved, the anti-seepage performance is better, and the safety of the sanitary product in use can be more effectively ensured.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these specific embodiments.
Examples 1 to 3
The preparation process of the polyolefin microporous breathable film of the embodiment is as follows:
step 1), blending and extruding: mixing a polyolefin base material and an inorganic filler according to the weight ratio of 1:1, preparing a composite material through a blending extrusion process, and obtaining composite material particles through a re-granulation process;
the polyolefin substrates used in examples 1-3 were a mixture of metallocene polyethylene and linear low density polyethylene in a weight ratio of 1: 1; wherein the metallocene polyethylene has a melt index of 1.3g/10min and a density of 0.927g/cm3The product is an approved series product from Exxon company; the linear low density polyethylene has a melt index of 1.0g/10min and a density of 0.930g/cm3DOWLEX series products available from DOW corporation;
the inorganic fillers used in examples 1-3 were calcium carbonate and titanium dioxide in a weight ratio of 50: 1, and more than 98% of the particles of the inorganic filler have a particle size distribution of 1 to 8 μm, and are Filmlink series products available from Imerys corporation.
Step 2), film blowing and extrusion: preparing the composite material particles obtained in the step 1) into a film by a film blowing extrusion process; wherein the melt temperature of the melting stage of the blown film extrusion process is 200-230 ℃; specifically, composite material particles are sent into a film blowing extruder for extrusion and melting, and a melt is continuously extruded into a thin film through a die lip gap of an annular die head of the film blowing machine;
step 3), stretching: stretching the film obtained in the step 2) by a single axial one-step method;
step 4), high-temperature heat setting treatment: carrying out high-temperature thermal setting treatment on the stretched film obtained in the step 3), and controlling the treatment temperature to be about 100-120 ℃, thus obtaining the polyolefin microporous breathable film;
example 1, step 3) above, at a stretch ratio of about 5.5, a microporous breathable film was produced having a basis weight of 10 gsm;
example 2, step 3) above, with a stretch ratio of about 4.5, a microporous breathable film was produced with a basis weight of 12 gsm;
example 3, step 3) above, with a stretch ratio of about 3.5, a microporous breathable film was produced having a basis weight of 15 gsm;
the microporous breathable films obtained from examples 1-3 above were each subjected to relevant performance tests.
Examples 4 to 6
The preparation process of the polyolefin microporous breathable film of the embodiment is as follows:
step 1), blending and extruding: mixing a polyolefin base material and an inorganic filler according to a weight ratio of 9:11, preparing a composite material through a blending extrusion process, and obtaining composite material particles through a re-granulation process;
the polyolefin substrates used in examples 4-6 were a mixture of metallocene polyethylene and linear low density polyethylene in a weight ratio of 1: 1; wherein the metallocene polyethylene has a melt index of 0.5g/10min and a density of 0.920g/cm3The product is an approved series product from Exxon company; the linear low density polyethylene has a melt index of 0.85g/10min and a density of 0.926g/cm3ELITE series products from DOW;
examples 4-6 used inorganic fillers of calcium carbonate and titanium dioxide in a weight ratio of 50: 1, and more than 98% of the particles of the inorganic filler have a particle size distribution of 1 to 8 μm, and are Filmlink series products available from Imerys corporation.
Step 2), film blowing and extrusion: preparing the composite material particles obtained in the step 1) into a film by a film blowing extrusion process; wherein the melt temperature of the melting stage of the blown film extrusion process is about 200-230 ℃; specifically, composite material particles are sent into a film blowing extruder for extrusion and melting, and a melt is continuously extruded into a thin film through a die lip gap of an annular die head of the film blowing machine;
step 3), stretching: stretching the film obtained in the step 2) by a single axial one-step method;
step 4), high-temperature heat setting treatment: carrying out high-temperature thermal setting treatment on the stretched film obtained in the step 3), and controlling the treatment temperature to be about 100-120 ℃, thus obtaining the polyolefin microporous breathable film.
Example 4, step 3) above, with a stretch ratio of about 5.0, a microporous breathable film was produced with a basis weight of 10 gsm;
example 5, step 3) above, at a stretch ratio of about 4.1, a microporous breathable film was produced having a basis weight of 12 gsm;
example 6, step 3) above, at a stretch ratio of about 3.5, a microporous breathable film was produced having a basis weight of 15 gsm;
the microporous breathable films obtained from examples 4-6 above were each subjected to relevant performance tests.
Comparative example 1
The polyolefin microporous breathable film (basis weight of 18gsm) obtained by the preparation of example 1 in the chinese patent CN106397918B publication.
Comparative example 2
Microporous breathable films with a basis weight of 15gsm were prepared by adjusting the stretch ratio using the preparation method of example 1 in the publication of Chinese patent CN 106397918B.
Note also that: by adjusting the stretch ratio using the method of example 1 in the chinese patent CN106397918B publication, attempts were made to produce microporous breathable films with basis weights of 10 and 12gsm, but the film broke due to excessive stretching; thus, the trial failed and no acceptable product could be prepared.
Comparative example 3
Microporous breathable film having a basis weight of 15gsm was prepared according to the preparation method of example 1 above, using conventional starting materials (polyolefin substrate type Touch343BF01, manufactured by cantonese chemical limited, guangzhou) and a draw ratio of about 4.5.
The water vapor transmission rate test (test according to GB 1037), the penetration test one (single-pass penetration test), the penetration test two (multiple-pass penetration test) and the hydrostatic pressure resistance test (test according to GB/T4744) were carried out for the above examples 1 to 6 and comparative examples 1 to 3.
The specific operations of the single extrusion penetration test method and the multiple extrusion penetration test method can be found in the publication of chinese patent CN106397918B, and are not described in detail.
The results of the measurements are shown in Table 1 below.
TABLE 1
As can be seen from the results in Table 1 above, first, both comparative example 1 and comparative example 2 employed the method of preparation of example 1 in the publication of Chinese patent CN106397918B, wherein comparative example 2 produced microporous breathable films having a lower basis weight by adjusting the stretch ratio (from 18gsm in comparative example 1 to 15gsm in comparative example 2), but the film was thinner due to the lower basis weight and the leak resistance was affected (the results of the first and second leak tests for the microporous breathable film of comparative example 2 were very poor compared to comparative example 1).
Furthermore, if microporous breathable films with basis weights of 10 and 12gsm were prepared based on the methods of comparative examples 1 and 2, the films broke due to excessive stretching and no acceptable product could be prepared.
This therefore shows that it is difficult to reduce the basis weight by redrawing based on the solution disclosed in chinese patent CN106397918B, and if the basis weight is reduced, the leakage resistance is reduced and even the film is broken.
The inventors of the present application have also tried to change the casting process of the solution disclosed in chinese patent CN106397918B to the blown film process, but found that it is not feasible (the quality and performance of the obtained microporous breathable film product is worse than that of comparative examples 1 and 2); the inventors of the present application have made various adjustments and attempts at raw materials, processes, and process parameters and have surprisingly found that microporous breathable films having lower basis weights and still maintaining excellent high moisture permeability can be obtained when using a polyolefin substrate of a specific formulation and a blown film process using specific parameters.
Referring to Table 1, the microporous breathable films of examples 1-6 of the present invention, obtained by a modified process, had a reduced basis weight as compared to the microporous breathable film of comparative example 1 (18gsm), but the high moisture permeability was not reduced (the water vapor transmission rate of the microporous breathable films of examples 1-6 was up to 8000 g/m)2·24Over h, the water vapor transmission rate in the first hour can reach 1000g/m2H, reach a level equal to that of comparative example 1).
When comparing the microporous breathable films of inventive examples 3 and 6 with comparative examples 2 and 3, inventive examples 3 and 6 have better high moisture permeability properties, although both have a basis weight of 15 gsm.
In addition, the microporous breathable films of examples 1-6 of the present invention were thinner (reduced in basis weight) than the microporous breathable film of comparative example 1 (18 gsm); as is common and well known in the art, the film becomes thinner, hydrostatic pressure resistance generally decreases, and the film is more susceptible to permeation.
However, the inventors of the present application have unexpectedly found that the hydrostatic pressure resistance of the microporous breathable films of examples 1-6 of the present invention is still further improved; referring to Table 1, the microporous breathable films of examples 1-6 of the present invention have hydrostatic pressure resistance of 80-100 cm/H2O, 50-70cm/H higher than that of comparative examples 1-3 of the prior art2O。
In summary, compared with the microporous breathable films in the prior art, the microporous breathable films of embodiments 1 to 6 of the present invention have the advantages of low basis weight, further improved hydrostatic pressure resistance, and better leakage prevention performance while maintaining high moisture permeability, and can more effectively ensure the safety of the sanitary products in use.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (5)
1. A preparation method of polyolefin microporous breathable film is characterized by comprising the following steps:
the preparation method comprises the following steps:
step 1), blending and extruding: mixing a polyolefin base material and an inorganic filler according to a weight ratio of 9: 11-1: 1, preparing a composite material through a blending extrusion process, and obtaining composite material particles through a re-granulation process;
the polyolefin base material is a mixture of metallocene polyethylene and linear low-density polyethylene according to the weight ratio of 1: 1; the metallocene polyethylene has a melt index of 0.25-1.5 g/10min and a density of 0.918-0.927 g/cm3(ii) a The linear low density polyethylene has a melt index of 0.8 to 1g/10min and a density of 0.917 to 0.935g/cm3；
The inorganic filler is one or a mixture of more of calcium carbonate, calcium oxide, calcium hydroxide or titanium dioxide; more than 98% of the particles of the inorganic filler are distributed in the particle size of 1-8 mu m;
step 2), film blowing and extrusion: preparing the composite material particles obtained in the step 1) into a film by a film blowing extrusion process; wherein the melt temperature of the melting stage of the blown film extrusion process is 200-230 ℃;
step 3), stretching: stretching the film obtained in the step 2) by a uniaxial one-step method, wherein the stretching ratio is 3.1-5.5;
step 4), high-temperature heat setting treatment: and (3) carrying out high-temperature thermal setting treatment on the stretched film obtained in the step 3), and controlling the treatment temperature to be 100-120 ℃ to obtain the polyolefin microporous breathable film.
2. The method of claim 1, wherein:
the inorganic filler is calcium carbonate and titanium dioxide according to a weight ratio of 50: 1.
3. Use of the polyolefin microporous breathable film prepared by the preparation method according to claim 1 or 2 in disposable hygienic products.
4. Use according to claim 3, characterized in that: the polyolefin microporous breathable film is applied to disposable hygienic products as an anti-leakage bottom film or an anti-leakage functional layer.
5. Use according to claim 3 or 4, characterized in that:
the disposable sanitary product comprises a sanitary towel, a sanitary pad, a baby diaper, a pull-up diaper, a diaper, an adult diaper, a disposable mattress, an incontinence pad, a nursing pad or an anti-galactorrhea pad.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111533933A (en) * | 2020-05-11 | 2020-08-14 | 上海暖友实业有限公司 | Preparation method of microporous composite membrane with uniform air permeability |
| CN115920114A (en) * | 2022-12-07 | 2023-04-07 | 杭州瑞宇医疗用品有限公司 | Protective pad for female privacy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533933A (en) * | 2020-05-11 | 2020-08-14 | 上海暖友实业有限公司 | Preparation method of microporous composite membrane with uniform air permeability |
| CN111533933B (en) * | 2020-05-11 | 2022-12-02 | 上海暖友实业有限公司 | Preparation method of microporous composite membrane with uniform air permeability |
| CN115920114A (en) * | 2022-12-07 | 2023-04-07 | 杭州瑞宇医疗用品有限公司 | Protective pad for female privacy and preparation method thereof |
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