CN110776697A - Environment-friendly foaming master batch and preparation method thereof - Google Patents
Environment-friendly foaming master batch and preparation method thereof Download PDFInfo
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- CN110776697A CN110776697A CN201911012644.1A CN201911012644A CN110776697A CN 110776697 A CN110776697 A CN 110776697A CN 201911012644 A CN201911012644 A CN 201911012644A CN 110776697 A CN110776697 A CN 110776697A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J2423/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J2423/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
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Abstract
The invention discloses an environment-friendly foaming master batch which comprises the following raw materials in percentage by mass: 30-50% of end group functionalized polyethylene, 40-60% of cellulose modified polyethylene and 2-10% of foaming agent. The environment-friendly foaming master batch provided by the invention has higher melt strength in the foaming process, simultaneously cellulose has very high mechanical strength, excellent mechanical properties are provided for a foaming material, and the existence of the cellulose is also beneficial to supporting foam pores, so that the generated foam pores are not easy to collapse. The final foamed polypropylene material prepared by the invention is green, environment-friendly and recyclable plastic; according to the micro-foaming method provided by the invention, the environment-friendly foaming master batch and the base material are mixed and then can be subjected to injection molding foaming by a common injection molding machine, so that the equipment investment is low, and the micro-foaming method is suitable for large-scale popularization.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to an environment-friendly foaming master batch and a preparation method thereof.
Background
The master batch is composed of excessive chemical additives, carrier resin and dispersing agent, the master batch is an aggregate obtained by uniformly loading excessive chemical additives in resin, and the commonly used master batch is divided into cooling master batch, brightening master batch, moisture absorption defoaming master batch, flame retardant master batch and foaming master batch.
The foaming agent is widely applied to the injection molding industry, can reduce the weight of plastic products, reduce the usage amount of raw materials and reduce the production cost, and has positive social significance. The polypropylene foaming material has the characteristics of excellent mechanical property, good chemical resistance stability, excellent price and the like, and is widely applied to the fields of automobiles, buildings and electric appliances. Particularly in the field of automobiles, along with the development of the trend of weight reduction of automobiles, the development demand of high-performance foamed polypropylene is more urgent.
However, the melt strength of polypropylene is low, the viscosity is low, and the foaming effect is poor, so that the industrialization realization time of the foamed polypropylene is much later than that of other materials. In the traditional physical foaming or supercritical foaming, the process is complex, the equipment investment is large, the product quality control is difficult, and special polypropylene with high melt strength is needed as a foaming base material. In addition, the existing micro-foamed polypropylene has the defects of poor performance, unobvious weight reduction effect and the like due to the characteristics of the material, poor foaming multiplying power, poor foam pore distribution and the like, and has few practical mass production applications for a while.
Therefore, how to provide an environment-friendly foaming master batch to overcome the technical defects is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides an environment-friendly foaming master batch, which has high melt strength and very high mechanical strength of cellulose in a foaming process, so as to provide excellent mechanical properties for a foaming material, and the existence of the cellulose is also helpful for supporting foam pores, so that the generated foam pores are not easy to collapse. According to the micro-foaming method provided by the invention, the environment-friendly foaming master batch and the base material are mixed and then can be subjected to injection molding foaming by a common injection molding machine, the equipment investment is low, and the method is suitable for large-scale popularization.
In order to achieve the purpose, the invention adopts the following technical scheme:
the environment-friendly foaming master batch comprises the following raw materials in percentage by mass:
30-50% of end group functionalized polyethylene
40-60% of cellulose modified polyethylene
2 to 10 percent of foaming agent.
By adopting the technical scheme, the invention has the technical effects that: the functional polyethylene is end group modified trimethyl siloxane, wherein the siloxane can react with hydroxyl on the surface of cellulose in self-made cellulose modified polyethylene to generate a stable silicon hydroxyl chemical bond, so that the environment-friendly foaming master batch material provided by the invention provides higher melt strength in the foaming process, and simultaneously the cellulose has very high mechanical strength up to 130-145GPa, so that excellent mechanical properties are provided for the foaming material, the existence of the cellulose is also beneficial to supporting foam holes, and the generated foam holes are not easy to collapse.
Preferably, the end group functionalized polyethylene is prepared by the following steps:
s1, under the protection of nitrogen, reacting polyethylene, gamma-mercaptopropyltrimethoxysilane and 1, 1' -azo (cyanocyclohexane) in a solvent toluene at the temperature of 85-95 ℃ for 3-8 hours to obtain a reaction product;
and S2, collecting the reaction product obtained after the operation of the step S1, washing the reaction product with a solvent, and drying the reaction product to obtain the end group functionalized polyethylene.
In the technical scheme, the protection of nitrogen is to prevent reactants from being oxidized, and the reaction temperature is set to be the activation energy to open the bond reaction.
Preferably, the mass ratio of the polyethylene, the gamma-mercaptopropyltrimethoxysilane and the 1, 1' -azo (cyanocyclohexane) in the step S1 is 1 (2-4) to (0.2-0.8), and the mass-volume ratio of the polyethylene to the toluene is 1 g: (2-5) mL.
Preferably, the solvent in the step S2 is selected from any one of ethanol, methanol, acetone, chloroform, and diethyl ether.
Preferably, the drying process in the step S2 is as follows: and putting the mixture into a 65 ℃ oven to be dried for 2 hours.
Preferably, the cellulose modified polyethylene comprises the following raw materials in percentage by mass: 60-40% of polyethylene and 40-60% of cellulose.
By adopting the preferable technical scheme, the invention has the technical effects that: the cellulose has very high mechanical strength, and can provide excellent mechanical properties for polyethylene, and further provide excellent mechanical properties for the foaming material; in addition, the adopted cellulose is an environment-friendly renewable resource, and the prepared final foamed polypropylene material is green, environment-friendly and recyclable plastic.
Preferably, the cellulose modified polyethylene is prepared by the following steps:
s1, mixing polyethylene and cellulose at the temperature of 20-30 ℃ at the mixing speed of: mixing for 3-10 minutes under the conditions of 200-500rpm to obtain a mixture for later use;
s2, melting, extruding and granulating the mixture obtained in S1 at the temperature of 170-220 ℃ and the rotating speed of 300-450rpm to obtain the cellulose modified polyethylene.
By adopting the preferable technical scheme, the invention has the technical effects that: the foaming master batch is modified by cellulose, the cellulose has very high mechanical strength, and the siloxane in the functional polyethylene modified trimethyl siloxane prepared by the method can react with the hydroxyl on the surface of the cellulose in the self-made cellulose modified polyethylene to provide high melt strength for the foaming master batch.
Preferably, the foaming agent is an olefinic microsphere foaming agent.
By adopting the technical scheme, the invention has the technical effects that: the environment-friendly foaming master batch can be directly injection-molded after being mixed with polypropylene, and the obtained foaming material with uniform, dense and complete foam pores is obtained.
The invention also provides the environment-friendly foaming master batch which is prepared by the following steps:
1) end group functionalized polyethylene, cellulose modified polyethylene and a foaming agent are mixed at the temperature of 20-30 ℃ at the mixing rate of: mixing for 3-10 minutes under the conditions of 200-500rpm to obtain a mixture for later use;
2) and melting, extruding and granulating the mixture obtained in the step 1) under the conditions that the temperature is 170-220 ℃ and the rotating speed is 300-450rpm to obtain the environment-friendly foaming master batch.
The invention further provides application of the environment-friendly foaming master batch in a micro-foaming polypropylene material.
Preferably, the preparation method of the micro-foaming polypropylene material comprises the following steps: and mixing the environment-friendly foaming master batch with polypropylene, and carrying out micro-foaming injection molding to obtain the micro-foaming polypropylene material.
Preferably, the weight ratio of the environment-friendly foaming master batch to the polypropylene is as follows: (5-8):100.
According to the technical scheme, compared with the prior art, the environment-friendly foaming master batch and the preparation method thereof provided by the invention have the following beneficial effects:
(1) in the environment-friendly foaming master batch provided by the invention, functional polyethylene is end group modified trimethyl siloxane, wherein the siloxane can react with hydroxyl on the surface of cellulose in self-made cellulose modified polyethylene to generate stable silicon hydroxyl chemical bonds, so that the environment-friendly foaming master batch material provided by the invention provides higher melt strength in the foaming process, and simultaneously cellulose has very high mechanical strength which is up to 130-145GPa, so that excellent mechanical properties are provided for the foaming material, and the existence of the cellulose is also beneficial to supporting foam holes, so that the generated foam holes are not easy to collapse.
(2) Compared with the traditional foaming modification method, the cellulose material used in the master batch is an environment-friendly renewable resource, and the prepared final foamed polypropylene material is green, environment-friendly and recyclable plastic.
(3) According to the micro-foaming method provided by the invention, the environment-friendly foaming master batch and the base material are mixed and then can be subjected to injection molding foaming by a common injection molding machine, so that the equipment investment is low, and the micro-foaming method is suitable for large-scale popularization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment 1-5 discloses an environment-friendly foaming master batch, which comprises the following components: end group functionalized polyethylene, cellulose modified polyethylene and foaming agent, wherein the specific raw material dosage is shown in table 1;
wherein the end group functionalized polyethylene is self-made, polyethylene, gamma-mercaptopropyltrimethoxysilane and 1, 1' -azo (cyanocyclohexane) are used as reaction raw materials, toluene is used as a reaction solvent, and the raw material dosage and reaction condition parameters in the specific preparation process are shown in table 2;
the cellulose modified polyethylene is self-made, polyethylene and cellulose are used as raw materials, and the raw material dosage and reaction condition parameters in the specific preparation process are shown in table 3.
Embodiments 1 to 5 of the present invention further provide a micro-bubble polypropylene material, wherein the environment-friendly foaming master batch and the polypropylene obtained in embodiments 1 to 5 are used as raw materials, and the specific raw material amounts are shown in table 4.
TABLE 1 raw material proportioning table (weight) of environmental protection foaming master batch
TABLE 2 table of raw material amounts and reaction condition parameters for preparing end group functionalized polyethylene
TABLE 3 table of raw material amounts and reaction condition parameters for preparing cellulose-modified polyethylene
TABLE 4 raw material ratio table (mass percent) of micro-foaming polypropylene material
The preparation method of the environment-friendly foaming master batch provided by the embodiment 1-5 of the invention specifically comprises the following steps:
(1) the preparation of end group functionalized polyethylene comprises the following steps:
s1, weighing polyethylene, gamma-mercaptopropyl trimethoxysilane and 1,1 '-azo (cyanocyclohexane), dissolving the polyethylene in toluene, adding the gamma-mercaptopropyl trimethoxysilane and the 1, 1' -azo (cyanocyclohexane), heating the reaction solution to 85-95 ℃ under the protection of nitrogen, and reacting for 3-8 hours to obtain a reaction product;
and S2, collecting the reaction product obtained after the operation of the step S1, washing the reaction product with ethanol, and putting the reaction product into a 65 ℃ oven to be dried for 2 hours to obtain the end group functionalized polyethylene.
(2) The preparation of the cellulose modified polyethylene comprises the following steps:
s1, weighing polyethylene and cellulose, and placing the polyethylene and the cellulose in a high-speed mixer at the temperature of 170 ℃ and 220 ℃ at the mixing speed of: mixing for 3-10min under the conditions of 200-500rpm to obtain a mixture for later use;
s2, placing the mixture obtained in S1 in a double-screw extruder, wherein the temperature is 170-.
(3) The preparation method of the environment-friendly foaming master batch comprises the following steps:
1) weighing end group functionalized polyethylene, cellulose modified polyethylene and a foaming agent, and placing the end group functionalized polyethylene, the cellulose modified polyethylene and the foaming agent in a high-speed mixer, wherein the temperature is 20-30 ℃, and the mixing speed is as follows: mixing for 3-10min under the conditions of 200-500rpm to obtain a mixture for later use;
2) and placing the mixture obtained in the step 1) in a double-screw extruder, wherein the temperature of the double-screw extruder is 170-.
The preparation method of the micro-foaming polypropylene material provided by the embodiments 1-5 of the invention comprises the following specific processes: and mixing the environment-friendly foaming master batch with polypropylene, and carrying out micro-foaming injection molding to obtain the micro-foaming polypropylene material.
Comparative example 1
And mixing the foaming agent with polypropylene according to the addition ratio of 8%, and carrying out foaming injection molding to obtain the common foamed polypropylene material.
To better illustrate that the environmental-friendly foaming master batches prepared in examples 1 to 5 can obviously improve mechanical properties when applied to the micro-foaming polypropylene material, the performance test of the micro-foaming polypropylene material obtained in examples 1 to 5 is carried out, and the test results are shown in table 5, and the specific processes are as follows:
TABLE 5 Performance test results of microcellular foamed polypropylene materials
As is apparent from the test results in Table 5, the microcellular foamed polypropylene materials prepared in examples 1 to 5 had densities of 0.33 to 0.48 (g/cm)
3) Comparative example 1(0.85 (g/cm)
3) About half of the total weight of the polypropylene materials), the average cell diameter of the micro-foamed polypropylene materials prepared in the examples 1 to 5 is also obviously smaller than that of the comparative example 1, and the properties of the micro-foamed polypropylene materials prepared in the examples 1 to 5, such as tensile strength, notched izod impact strength, flexural modulus, etc., are obviously better than those of the comparative example 1.
The above results show that: compared with the prior art, the invention has lower density and cell diameter, excellent tensile strength and cantilever beam notch impact strength, and obvious technical effect. The reason for this is that siloxane in the self-made functionalized polyethylene provided by the invention can react with hydroxyl on the surface of cellulose in the self-made cellulose modified polyethylene to generate stable silicon hydroxyl chemical bonds, so that the environment-friendly foaming master batch material provided by the invention provides higher melt strength in the foaming process; meanwhile, the cellulose has very high mechanical strength which is as high as 130-145GPa, so that excellent mechanical properties are provided for the foaming material, and the existence of the cellulose is also helpful for supporting the foam holes, so that the generated foam holes are not easy to collapse.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The environment-friendly foaming master batch is characterized by comprising the following raw materials in percentage by mass:
30-50% of end group functionalized polyethylene
40-60% of cellulose modified polyethylene
2 to 10 percent of foaming agent.
2. The environment-friendly foaming masterbatch according to claim 1, wherein the end-functionalized polyethylene is prepared by the following steps:
s1, under the protection of nitrogen, reacting polyethylene, gamma-mercaptopropyltrimethoxysilane and 1, 1' -azo (cyanocyclohexane) in a solvent toluene at the temperature of 85-95 ℃ for 3-8 hours to obtain a reaction product;
and S2, collecting the reaction product obtained after the operation of the step S1, washing the reaction product with a solvent, and drying the reaction product to obtain the end group functionalized polyethylene.
3. The environment-friendly foaming masterbatch according to claim 2, wherein the mass ratio of the polyethylene, the gamma-mercaptopropyltrimethoxysilane and the 1, 1' -azo (cyanocyclohexane) in the step S1 is 1 (2-4) to (0.2-0.8), and the mass/volume ratio of the polyethylene to the toluene is 1 g: (2-5) mL.
4. The environmental friendly foaming concentrate as claimed in claim 2, wherein the solvent in step S2 is selected from any one of ethanol, methanol, acetone, chloroform and diethyl ether.
5. The environment-friendly foaming masterbatch according to claim 1, wherein the cellulose-modified polyethylene comprises the following raw materials by mass: 60-40% of polyethylene and 40-60% of cellulose.
6. The environment-friendly foaming masterbatch according to claim 5, wherein the cellulose-modified polyethylene is prepared by the following steps:
s1, mixing the polyethylene and the cellulose for 3-10 minutes under the conditions that the temperature is 20-30 ℃, the mixing speed is 200-500rpm, and obtaining a mixture for later use;
s2, melting, extruding and granulating the mixture obtained in S1 at the temperature of 170-220 ℃ and the rotating speed of 300-450rpm to obtain the cellulose modified polyethylene.
7. The environmental-friendly foaming masterbatch according to claim 1, wherein the foaming agent is an olefinic microsphere foaming agent.
8. The method for preparing the environment-friendly foaming masterbatch according to any one of claims 1 to 7, comprising the following steps:
1) mixing the end group functionalized polyethylene, the cellulose modified polyethylene and the foaming agent for 3-10 minutes at the temperature of 20-30 ℃ and the mixing speed of 200-500rpm to obtain a mixture for later use;
2) and melting, extruding and granulating the mixture obtained in the step 1) under the conditions that the temperature is 170-220 ℃ and the rotating speed is 300-450rpm to obtain the environment-friendly foaming master batch.
9. The use of the environmentally friendly foaming concentrate as claimed in any one of claims 1 to 6 in a micro-foamed polypropylene material.
10. The use of the environment-friendly foaming masterbatch according to claim 9, wherein the weight ratio of the environment-friendly foaming masterbatch to the polypropylene is: (5-8):100.
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