CN113549327A - Composite material, composite material injection molding material, composite material product and preparation method - Google Patents

Composite material, composite material injection molding material, composite material product and preparation method Download PDF

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CN113549327A
CN113549327A CN202110873978.9A CN202110873978A CN113549327A CN 113549327 A CN113549327 A CN 113549327A CN 202110873978 A CN202110873978 A CN 202110873978A CN 113549327 A CN113549327 A CN 113549327A
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powder
composite material
injection molding
modifier
preparing
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CN113549327B (en
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肖升
吴沙鸥
钟丽萍
贺鹏华
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Shenzhen Taotao Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C45/00Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
    • B29C45/0053Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor combined with a final operation, e.g. shaping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02Thermal after-treatment
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/40Glass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium

Abstract

The invention provides a preparation method of a composite material, which comprises the following steps: respectively weighing first powder and second powder, wherein the first powder is inorganic powder, and the second powder is engineering resin powder with a benzene ring structure; carrying out surface modification treatment on the first powder by using a modifier to obtain modified powder slurry, wherein the modifier is a surfactant with a benzene ring structure; drying the modified powder slurry to obtain modified powder; mixing the modified powder and the second powder, and then carrying out banburying and granulation to obtain the composite material injection molding material, wherein the temperature range of the banburying and the granulation is 250-400 ℃. Also provides a composite material injection molding material prepared by the preparation method, a preparation method of a composite material product and the composite material product. The preparation method of the composite material provided by the invention can obviously improve the interface bonding strength of the composite material, so that the bending strength of the composite material and the composite material product is improved.

Description

Composite material, composite material injection molding material, composite material product and preparation method
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a composite material, a composite material injection molding material, a composite material product and a preparation method thereof.
Background
With the continuous progress of science and technology, people have not only a single material but also a demand for a material. As a novel material, the composite material has better comprehensive performance, is more and more concerned by people and causes a large number of researchers to research the composite material. In the field of composite materials, composite materials composed of organic materials and inorganic materials are particularly advocated by people, but the organic materials and the inorganic materials have the problem of difficult combination, the interface combination strength of the composite materials is always the first problem which troubles researchers, and the poor interface combination strength directly causes the overall performance of the composite materials to be reduced, and even causes serious problems of fracture, falling off and the like at the interface.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a composite material, a composite material injection molding material, a composite material product and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of making a composite material comprising the steps of:
respectively weighing first powder and second powder, wherein the first powder is inorganic powder, and the second powder is engineering resin powder with a benzene ring structure;
carrying out surface modification treatment on the first powder by using a modifier to obtain modified powder slurry, wherein the modifier is a surfactant with a benzene ring structure;
drying the modified powder slurry to obtain modified powder;
mixing the obtained modified powder and the second powder, and then carrying out banburying and granulation to obtain the composite material injection molding material, wherein the temperature range of the banburying and the granulation is 250-400 ℃.
The further improvement of the technical scheme is as follows:
the modifier comprises one or more of benzoic acid, sodium benzoate, ammonium benzoate, terephthalic acid, phthalic acid, or sodium phthalate.
The surface modification treatment is specifically as follows:
preparing the first powder, a modifier and deionized water into slurry with the mass fraction of 10-60%, and stirring the slurry in stirring equipment for 2-30h to obtain the surface modified powder slurry.
The mass ratio of the first powder to the second powder is 3-6: 2.
the first powder comprises one or more of ceramic powder, metal powder or silicate glass powder.
The second powder comprises any one of polyphenylene sulfide powder, polyphenylene oxide powder, polyphenylsulfone powder or polystyrene powder.
The mass ratio of the modifier to the first powder is 0.1-10: 100.
the invention also provides a composite material injection molding material prepared by the preparation method of the composite material.
The invention also provides a preparation method of the composite material product, which comprises the following steps:
and (3) performing injection molding on the composite material injection molding material, wherein the injection molding temperature range is 200-380 ℃, and the composite material injection molding material is the composite material injection molding material.
The invention also provides a composite material product prepared from the composite material injection molding material.
According to the technical scheme, the preparation method of the composite material comprises the steps of firstly modifying the inorganic powder to functionalize the surface of the inorganic powder, wherein the modifying agent is a surfactant with a benzene ring structure, and after the inorganic powder is modified, the modifying agent with the benzene ring structure is adsorbed or grafted on the surface of the inorganic powder, so that the interface bonding strength between the inorganic powder and the modifying agent is enhanced. Meanwhile, because the second powder is engineering resin powder with a benzene ring structure, after the modified granulated powder is mixed with the second powder, the second powder also has a benzene ring structure, and based on a similar compatibility principle, the modifier can be firmly combined with the second powder to form a large pi bond between the benzene ring structures, so that the interface bonding strength of the modifier and the second powder is enhanced, and the bonding strength of two interfaces of the composite material is increased to a certain extent, so that the first powder and the second powder are combined more tightly, the interface bonding strength is improved, and the mechanical property of the composite material is better. And the preparation process is simple and the production cost is low. The composite material injection molding material and the composite material product prepared by using the composite material also have excellent bending strength.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a composite material according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a method for preparing a composite product according to an embodiment of the present invention.
FIG. 3 is a surface SEM image of a composite product prepared in example 1 of the present invention.
FIG. 4 is a surface SEM image of a composite product prepared in example 2 of the present invention.
FIG. 5 is a surface SEM image of a composite product prepared in example 3 of the present invention.
FIG. 6 is a surface SEM image of a composite product prepared by comparative example of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In a specific embodiment, as shown in fig. 1, the method for preparing the composite material comprises the following steps:
s1, preparing raw materials: respectively weighing first powder and second powder according to the mass ratio requirement, wherein the first powder is inorganic powder, and the second powder is engineering resin powder with a benzene ring structure. The mass ratio of the first powder to the second powder is 3-6: 2. the first powder comprises one or more of ceramic powder, metal powder or silicate glass powder. For example, the ceramic powder may be alumina powder, zirconia powder, silica powder, or the like. The metal powder can be tungsten steel powder, aluminum powder or iron powder and the like. The second powder comprises any one of polyphenylene sulfide powder (PPS), polyphenylene oxide powder (PPO), Polyphenylsulfone Powder (PPSU) or polystyrene powder (EPS).
S2, modifying the first powder: and carrying out surface modification treatment on the first powder by using a modifier to obtain modified powder slurry, wherein the modifier is a surfactant with a benzene ring structure. The modifier comprises one or more of benzoic acid, sodium benzoate, ammonium benzoate, terephthalic acid, phthalic acid, or sodium phthalate. The mass ratio of the modifier to the first powder is 0.1-10: 100.
the specific process of the surface modification treatment is as follows: preparing the first powder, a modifier and deionized water into slurry with the mass fraction of 10-60%, and placing the slurry into stirring equipment to be fully stirred for 2-30h to obtain the surface modified powder slurry. The stirring device can be any one of a sand mill, a roller mill, a planetary ball mill or a reaction kettle.
S3, drying: and drying the modified powder slurry to obtain modified powder. The drying includes one or more of spray drying, vacuum drying, or supercritical drying. The drying temperature is 100-300 ℃.
S4, banburying and granulating: and mixing the modified powder and the second powder, and then carrying out banburying in a mixer and granulation in a granulator to obtain the composite material injection molding material, wherein the temperature range of the banburying and the granulation is 250-400 ℃.
The internal mixing and granulating temperature range in the method is proper, the interface bonding strength of the composite material can be improved, and if the temperature is too high, the high polymer material can be carbonized, and the interface strength is influenced. If the temperature is too low, the mixture cannot be subjected to banburying granulation, and the effect of improving the interface bonding strength cannot be achieved.
In a specific embodiment, the method of making a composite product further comprises the steps of:
s5, injection molding: and (3) performing injection molding on the composite material to obtain a composite material product, wherein the injection molding temperature is 200-380 ℃.
In particular embodiments, the method of making a composite product may further comprise the steps of:
s6, heat treatment and processing: and carrying out heat treatment and processing treatment on the composite material product. The four-point bending strength requirement of the composite material product is 180-400 MPa.
As shown in fig. 1 and 2, example 1: the embodiment provides a preparation method of a composite material, a preparation method of a composite material product, and a composite material injection molding material and a composite material product prepared by the preparation method, wherein the preparation method specifically comprises the following steps:
s1, preparing raw materials: respectively weighing first powder and second powder according to the mass ratio requirement, wherein the first powder is alumina powder, and the second powder is polyphenylene sulfide powder (PPS). According to the mass parts, the first powder is 50 parts, and the second powder is 17 parts.
S2, modifying the first powder: and carrying out surface modification treatment on the first powder by using a modifier to obtain modified powder slurry, wherein the modifier is sodium benzoate. The addition amount of the modifier is 1 part by mass.
The specific process of the surface modification treatment is as follows: preparing 50 parts by mass of first powder, 1 part by mass of modifier and deionized water into slurry with the mass fraction of 40%, and placing the slurry in a sand mill for full stirring modification for 6 hours to obtain the surface modified powder slurry.
S3, drying: and carrying out spray drying treatment on the modified powder slurry to obtain modified powder. The drying temperature is 100-300 ℃.
S4, banburying and granulating: and (3) blending the modified powder with 17 parts by mass of second powder for 30 hours, and then carrying out banburying and granulation by a granulator to obtain the composite material injection molding material. The banburying temperature is 300 ℃, and the banburying time is 4 hours. The granulator is a screw granulator, and the granulation temperature is 280 ℃.
S5, injection molding: and carrying out injection molding on the composite material injection molding material to obtain a composite material product, wherein the injection molding temperature is 360 ℃.
S6, heat treatment and processing: and carrying out heat treatment and processing treatment on the composite material product.
Example 2: this example provides a method for preparing a composite material, a method for preparing a composite material product, and a composite material injection molding compound and a composite material product prepared by the above preparation methods, the preparation methods are substantially the same as those of example 1, and the same parts are not described herein again, except that:
s1, preparing raw materials: the first powder is tungsten steel powder, and the second powder is polyphenylene sulfide powder (PPS). The powder comprises, by mass, 20 parts of the first powder and 11 parts of the second powder.
S2, modifying the first powder: the modifier is benzoic acid, and the addition amount of the modifier is 2 parts by weight.
The specific process of the surface modification treatment is as follows: preparing 20 parts by mass of first powder, 2 parts by mass of modifier and deionized water into slurry with the mass fraction of 40%, and placing the slurry in a sand mill for full stirring modification for 6 hours to obtain the surface modified powder slurry.
S3, drying: and carrying out spray drying treatment on the modified powder slurry to obtain modified powder.
S4, banburying and granulating: and (3) blending the modified powder and 11 parts by mass of second powder for 30 hours, and then carrying out banburying and granulation by a granulator to obtain the composite material injection molding material.
S5, injection molding: and carrying out injection molding on the composite material injection molding material to obtain a composite material product.
S6, heat treatment and processing: and carrying out heat treatment and processing treatment on the composite material product.
Example 3: this example provides a method for preparing a composite material, a method for preparing a composite material product, and a composite material injection molding compound and a composite material product prepared by the above preparation methods, the preparation methods are substantially the same as those of example 1, and the same parts are not described herein again, except that:
s1, preparing raw materials: the first powder is silicate glass powder, and the second powder is polyphenylene sulfide powder (PPS). The powder comprises, by mass, 30 parts of the first powder and 10 parts of the second powder.
S2, modifying the first powder: the modifier is benzoic acid, and the addition amount of the modifier is 0.03 part by mass.
The specific process of the surface modification treatment is as follows: preparing slurry with the mass fraction of 40% by using 30 parts by mass of the first powder, 10 parts by mass of the modifier and deionized water, and placing the slurry in a sand mill for full stirring modification for 6 hours to obtain the surface modified powder slurry.
S3, drying: and carrying out spray drying treatment on the modified powder slurry to obtain modified powder.
S4, banburying and granulating: and blending the modified powder and 10 parts by mass of second powder for 30 hours, and then carrying out banburying and granulation by a granulator to obtain the composite material injection molding material.
S5, injection molding: and carrying out injection molding on the composite material injection molding material to obtain a composite material product.
S6, heat treatment and processing: and carrying out heat treatment and processing treatment on the composite material product.
Comparative example: the comparative example provides a preparation method of a composite material, a preparation method of a composite material product, and a composite material injection molding material and a composite material product prepared by the preparation method, and the preparation method specifically comprises the following steps:
s1, preparing raw materials: and respectively weighing the first powder and the second powder, and uniformly mixing the first powder and the second powder to obtain mixed powder. Wherein the mixing time is 30 h. The first powder is alumina powder, and the second powder is PPS powder. The powder comprises, by mass, 3 parts of the first powder and 1 part of the second powder.
S2, banburying and granulating: and carrying out banburying and granulation by a granulator on the mixed powder to obtain the composite material injection molding material. The banburying granulation temperature is 300 ℃, and the banburying time is 4 hours. The granulator is a screw granulator, and the granulation temperature is 280 ℃.
S3, injection molding: and carrying out injection molding on the composite material injection molding material to obtain a composite material product blank, wherein the injection molding temperature is 360 ℃.
S4, heat treatment and processing: and carrying out heat treatment and processing treatment on the composite material product.
Four-point bending strength tests were conducted on each of the three examples and the comparative example, and the test results are shown in table 1.
TABLE 1
Figure BDA0003189679480000081
As can be seen from the above table, the four-point bending strength of the examples 1, 2 and 3 all reach the design requirement of 180-400MPa, while the four-point bending strength of the comparative example does not reach the design value requirement and is lower in strength.
Fig. 3, 4 and 5 are surface SEM images of the composite products prepared in examples 1, 2 and 3, respectively, and it can be seen that the composite products in fig. 3, 4 and 5 have good material interface bonding and no obvious cracking and degranulation phenomena. Fig. 6 is a surface SEM image of the composite product prepared in the comparative example, and it can be seen from the image that the composite product of fig. 6 has a significant gap at the interface joint, and the product has a cracking phenomenon and a degranulation phenomenon. It is also apparent from the data results in table 1 that the four-point bending strength of the composite material product prepared by the scheme of the present invention is much greater than that of the composite material product prepared by the comparative example method, indicating that the interface bonding of the composite material prepared by the scheme of the present invention is firmer. The composite material prepared by the scheme of the invention can obviously improve the interface bonding strength, and the composite material prepared by the invention has better bending strength performance index.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only express preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A preparation method of a composite material is characterized by comprising the following steps: the method comprises the following steps:
respectively weighing first powder and second powder, wherein the first powder is inorganic powder, and the second powder is engineering resin powder with a benzene ring structure;
carrying out surface modification treatment on the first powder by using a modifier to obtain modified powder slurry, wherein the modifier is a surfactant with a benzene ring structure;
drying the modified powder slurry to obtain modified powder;
mixing the modified powder and the second powder, and then carrying out banburying and granulation to obtain the composite material injection molding material, wherein the temperature range of the banburying and the granulation is 250-400 ℃.
2. The method for preparing a composite material according to claim 1, characterized in that: the modifier comprises one or more of benzoic acid, sodium benzoate, ammonium benzoate, terephthalic acid, phthalic acid, or sodium phthalate.
3. The method for preparing a composite material according to claim 1, characterized in that: the surface modification treatment is specifically as follows:
preparing the first powder, a modifier and deionized water into slurry with the mass fraction of 10-60%, and stirring the slurry in stirring equipment for 2-30h to obtain the surface modified powder slurry.
4. The method for preparing a composite material according to claim 1, characterized in that: the mass ratio of the first powder to the second powder is 3-6: 2.
5. the method for preparing a composite material according to claim 1, characterized in that: the first powder comprises one or more of ceramic powder, metal powder or silicate glass powder.
6. The method for preparing a composite material according to claim 1, characterized in that: the second powder comprises any one of polyphenylene sulfide powder, polyphenylene oxide powder, polyphenylsulfone powder or polystyrene powder.
7. The method for preparing a composite material according to claim 1, characterized in that: the mass ratio of the modifier to the first powder is 0.1-10: 100.
8. the composite material injection molding material is characterized in that: prepared by the preparation method of any one of claims 1 to 7.
9. A method of making a composite product, comprising: the method comprises the following steps:
and (3) carrying out injection molding on the composite material injection molding material, wherein the injection molding temperature is 200-380 ℃, and the composite material injection molding material is the composite material injection molding material in the claim 8.
10. A composite product characterized by: prepared from the composite injection molding compound of claim 8.
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