CN112341716A - Polypropylene composite material for laser welding and preparation method thereof - Google Patents
Polypropylene composite material for laser welding and preparation method thereof Download PDFInfo
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- CN112341716A CN112341716A CN202011327893.2A CN202011327893A CN112341716A CN 112341716 A CN112341716 A CN 112341716A CN 202011327893 A CN202011327893 A CN 202011327893A CN 112341716 A CN112341716 A CN 112341716A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention relates to a polypropylene composite material for laser welding and a preparation method thereof. The composite material comprises the following components in parts by weight: 39-80 parts of polypropylene, 10-30 parts of inorganic filler, 5-25 parts of toughening agent, 5-15 parts of laser welding modifier, 0.2-0.5 part of antioxidant, 0.2-0.5 part of weather resistant agent, 0.1-0.3 part of lubricant and 0.5-1.0 part of black master batch. The composite material and nylon have better welding strength.
Description
Technical Field
The invention belongs to the field of laser welding materials and preparation methods thereof, and particularly relates to a polypropylene composite material for laser welding and a preparation method thereof.
Background
With the development of welding technology, laser welding is gradually accepted and is used more and more. The welding mode has no VOC (volatile organic compounds) emission of glue, is not easy to generate welding marks, and has the advantages of no contact, strong flexibility, short period, high welding precision, high automation degree and the like. The laser welding process is also considered more and more for the connection between plastic parts in the automobile industry, for example, the welding of a radar bracket, a wind guide bracket and a bumper is applied, and the laser welding of an inner plate and an outer plate of an all-plastic tail door is also under development. However, the parts are all made of polypropylene materials, the welding strength of the polypropylene parts can be higher as long as the light transmittance is higher in laser welding, and the automobile parts are also partially made of nylon materials, so that the high welding strength cannot be generally obtained when the nylon materials and the polypropylene materials are welded, because the compatibility of the nylon materials and the polypropylene materials is poor. Therefore, it is necessary to develop a polypropylene material capable of performing laser welding with nylon material, and the use of laser welding is widened.
In the study of laser transmission welding process of modified polypropylene and nylon 66, Jianghai Rong et al, it is mentioned that maleic anhydride grafted polypropylene is obtained by grafting maleic anhydride on the side chain of polypropylene, thereby achieving good welding between maleic anhydride grafted polypropylene and nylon 6. However, as is well known, the modified polypropylene for automobiles usually relates to filling, toughening and modified polypropylene, and the maleic anhydride grafted polypropylene is usually added only in a small amount as an auxiliary raw material due to factors such as poor fluidity, poor compatibility with a toughening agent POE, poor heat aging resistance and weather resistance, and is not suitable for replacing polypropylene as a main raw material of filling, toughening and modified polypropylene, so the application field of the polypropylene is greatly limited. Chinese patent CN1839031A discloses the addition of modified polyolefins (such as maleic anhydride grafted polypropylene) to polyolefins to prepare laser welded articles. However, the compatibility of the modified polyolefin with polypropylene is not particularly good, and the mechanical properties of the material are greatly lost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a polypropylene composite material for laser welding and a preparation method thereof, so as to overcome the defect that maleic anhydride grafted polypropylene in the prior art is not suitable for filling a main raw material of a toughened and modified polypropylene material and causes great loss on mechanical properties when being used as an auxiliary raw material.
The invention provides a polypropylene composite material for laser welding, which comprises the following components in parts by weight: 39-80 parts of polypropylene, 10-30 parts of inorganic filler, 5-25 parts of toughening agent, 5-15 parts of laser welding modifier, 0.2-0.5 part of antioxidant, 0.2-0.5 part of weather resistant agent, 0.1-0.3 part of lubricant and 0.5-1.0 part of black master batch, wherein the laser welding modifier is a block copolymer of polypropylene and polyamide.
The polypropylene is at least one of homo-polypropylene and co-polypropylene, and the melt index of the polypropylene is 1-100g/10min (the test condition is 230 ℃ and 2.16 kg).
The inorganic filler is at least one of talcum powder, calcium carbonate, wollastonite, mica, barium sulfate and magnesium sulfate whisker; the particle size of the inorganic filler is 1-10 μm.
The toughening agent is a copolymer of ethylene and an alpha-olefin containing 3 to 10 carbon atoms, and the toughening agent has a melt index of 0.5 to 30g/10min (test conditions of 190 ℃ C., 2.16 kg).
The antioxidant is at least one of phenol antioxidant, amine antioxidant, phosphite antioxidant and hindered phenol antioxidant.
The weather resisting agent is at least one of hindered amine light stabilizer, benzotriazole light stabilizer, benzophenone light stabilizer and triazine benzylidene malonate light stabilizer.
The lubricant is at least one of an amide lubricant, a stearic acid lubricant, a fatty acid lubricant and an ester lubricant.
The invention also provides a preparation method of the polypropylene composite material for laser welding, which comprises the following steps:
mixing polypropylene, inorganic filler, toughening agent, laser welding modifier, antioxidant, weather resistant agent, lubricant and black master batch, adding the mixed raw materials into a double-screw extruder for melt blending, extruding and granulating to obtain the polypropylene composite material for laser welding.
The block copolymer of polypropylene and polyamide is prepared by reacting carboxyl-terminated polypropylene with polyamide under the action of a catalyst.
The preparation method of the block copolymer of polypropylene and polyamide comprises the following steps: adding polyamide, double-end carboxyl polypropylene and a catalyst into a toluene solution, carrying out reflux reaction for 24-30h under the protection of nitrogen, cooling, precipitating in methanol, washing and drying to obtain the catalyst, wherein the weight ratio of amino in the polyamide to carboxyl in the double-end carboxyl polypropylene is 2-2.5:1, the mass ratio of the catalyst to the polyamide is 92-97:3-8, the viscosity of the polyamide is 5000-70000mpa.s/40 ℃, and preferably 10000-50000mpa.s/40 ℃.
The washing is sequentially washing with methanol and acetone.
The preparation method of the double-end carboxyl polypropylene comprises the following steps: mixing polypropylene and concentrated nitric acid at a ratio of 100g:450-550ml, heating to 120-140 ℃, stirring for 12-20h, washing, and drying to obtain the polypropylene with a molecular weight of 1000-6000g/mol, preferably 3000-5000 g/mol.
The washing is water and acetone in sequence.
The mixing time is 1-2min, and the mixing speed is 600-1000 rpm.
The melt blending temperature is 180-230 ℃.
The invention also provides application of the polypropylene composite material for laser welding in laser welding.
Advantageous effects
The block copolymer of polypropylene and polyamide added in the invention not only can make the filling modified polypropylene material have good compatibility with nylon 6, but also has good compatibility with polypropylene, thereby making the filling modified polypropylene material have good fusion with the nylon 6 in the melting process of laser welding, improving the welding strength, and having little influence on the mechanical properties of the polypropylene material. And the block copolymer of polypropylene and polyamide is added into the traditional modified polypropylene material, so that the multi-dimensional design of filling, toughening and the like of the material is not influenced, and the application range of the modified polypropylene material covers all types of modified polypropylene materials.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The raw materials in the examples and comparative examples of the present invention are, but not limited to, the following:
PP BX 3920: copolymerized polypropylene, SK corporation, korea;
PP K9017: copolypropylene, taiwan Taiwan;
AH-3000N 9: pulvis Talci, 3000 mesh, and folium Artemisiae Argyi;
POE 8137: ethylene octene copolymers, dow chemical;
antioxidant 1010: primary antioxidant, basf;
antioxidant 168: secondary antioxidants, basf;
UV-3808PP 5: weather resistance agents, cyanogen specialty chemicals;
TR 451: lubricants, Sruktol corporation, usa;
PE 2772: black masterbatch, cabot;
maleic anhydride graft-modified polypropylene wax: of Clariant
AR504。
The preparation method of the block copolymer of polypropylene and polyamide comprises the following steps: polyamide (Changzhou mountain chemical industry, SF-650-200, viscosity 20000mpa.s/40 ℃) and carboxyl-terminated polypropylene are weighed according to the ratio of amino to carboxyl being 2.2:1, the sum of the weights of the polyamide and the carboxyl-terminated polypropylene is 50g, catalyst p-toluenesulfonic acid is weighed according to the mass ratio of 95:5 to the polyamide, the mixture is placed in 500mL of toluene solution, heated and refluxed under the protection of nitrogen for reaction for 24 hours, then a reaction product is cooled and precipitated in methanol, washed by methanol and acetone in sequence, and then placed in a vacuum oven for drying, and the block copolymer is obtained.
The preparation method of the double-end carboxyl polypropylene comprises the following steps: 100g of polypropylene (COSCHEM, Korea, CS-53NC, molecular weight 3500g/mol) and 500mL of 70% strength concentrated nitric acid were placed in a vessel, heated to 130 ℃ and stirred for 16h, and the reaction product was washed with water and then acetone and then dried in a vacuum oven.
Example 1
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392028.6 parts, K901735 parts, AH-3000N 912 parts, POE 813718 parts, 5 parts of a polypropylene and polyamide block copolymer, an antioxidant 10100.15 parts, an antioxidant 1680.15 parts, UV-3808PP 50.2 parts, TR 4510.2 parts and PE 27720.7 parts.
The preparation method of the composite material comprises the following steps: mixing all the components at the mixing speed of 600 revolutions per minute for 2min, adding the mixed raw materials into a main feeding port of a double-screw extruder, carrying out melt blending at the temperatures of 180 ℃, 200 ℃, 220 ℃, 230 ℃, 220 ℃ and 210 ℃ in each section, and carrying out extrusion granulation to obtain the polypropylene composite material for laser welding.
Example 2
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392023.6 parts, K901735 parts, AH-3000N 912 parts, POE 813718 parts, polypropylene and polyamide block copolymer 10 parts, antioxidant 10100.15 parts, antioxidant 1680.15 parts, UV-3808PP 50.2 parts, TR 4510.2 parts and PE 27720.7 parts.
The preparation method of the composite material comprises the following steps: mixing all the components at the mixing speed of 1000 revolutions per minute for 1min, adding the mixed raw materials into a main feeding port of a double-screw extruder, carrying out melt blending at the temperatures of 180 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃ and 220 ℃ in each section, and carrying out extrusion granulation to obtain the polypropylene composite material for laser welding.
Example 3
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392023.6 parts, K901730 parts, AH-3000N 912 parts, POE 813718 parts, polypropylene and polyamide block copolymer 15 parts, antioxidant 10100.15 parts, antioxidant 1680.15 parts, UV-3808PP 50.2 parts, TR 4510.2 parts and PE 27720.7 parts.
The preparation method of the composite material comprises the following steps: mixing all the components at the mixing speed of 1000 revolutions per minute for 1min, adding the mixed raw materials into a main feeding port of a double-screw extruder, carrying out melt blending at the temperatures of 180 ℃, 190 ℃, 210 ℃, 220 ℃, 210 ℃ and 210 ℃ in each section, and carrying out extrusion granulation to obtain the polypropylene composite material for laser welding.
Example 4
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392029.4 parts, K901720 parts, AH-3000N 921 parts, POE 813723 parts, 5 parts of a polypropylene and polyamide block copolymer, 10100.2 parts of an antioxidant, 1680.2 parts of an antioxidant, UV-3808PP 50.3 parts, TR 4510.2 parts and PE 27720.7 parts.
The preparation method of the composite material comprises the following steps: mixing all the components at the mixing speed of 800 revolutions per minute for 1min, adding the mixed raw materials into a main feeding port of a double-screw extruder, carrying out melt blending at the temperatures of 180 ℃, 200 ℃, 220 ℃, 230 ℃, 220 ℃ and 210 ℃ in each section, and carrying out extrusion granulation to obtain the polypropylene composite material for laser welding.
Example 5
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392024.4 parts, K901720 parts, AH-3000N 921 parts, POE 813723 parts, polypropylene and polyamide block copolymer 10 parts, antioxidant 10100.2 parts, antioxidant 1680.2 parts, UV-3808PP 50.3 parts, TR 4510.2 parts and PE 27720.7 parts.
The above composite material was prepared in the same manner as in example 4.
Example 6
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392024.4 parts, K901715 parts, AH-3000N 921 parts, POE 813723 parts, polypropylene and polyamide block copolymer 15 parts, antioxidant 10100.2 parts, antioxidant 1680.2 parts, UV-3808PP 50.3 parts, TR 4510.2 parts and PE 27720.7 parts.
The above composite material was prepared in the same manner as in example 4.
Example 7
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392021.1 parts, K901732 parts, AH-3000N 930 parts, POE 813710 parts, 5 parts of a polypropylene and polyamide block copolymer, an antioxidant 10100.2 parts, an antioxidant 1680.3 parts, UV-3808PP 50.5 parts, TR 4510.2 parts and PE 27720.7 parts.
The preparation method of the composite material comprises the following steps: mixing all the components at the mixing speed of 700 revolutions per minute for 1.5min, adding the mixed raw materials into a main feeding port of a double-screw extruder, carrying out melt blending at the temperatures of 180 ℃, 210 ℃, 230 ℃, 230 ℃, 230 ℃ and 220 ℃ in each section, and carrying out extrusion granulation to obtain the polypropylene composite material for laser welding.
Example 8
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392018.1 parts, K901730 parts, AH-3000N 930 parts, POE 813710 parts, polypropylene and polyamide block copolymer 10 parts, antioxidant 10100.2 parts, antioxidant 1680.3 parts, UV-3808PP 50.5 parts, TR 4510.2 parts and PE 27720.7 parts.
The above composite material was prepared in the same manner as in example 7.
Example 9
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392015.1 parts, K901728 parts, AH-3000N 930 parts, POE 813710 parts, 15 parts of a polypropylene and polyamide block copolymer, antioxidant 10100.2 parts, antioxidant 1680.3 parts, UV-3808PP 50.5 parts, TR 4510.2 parts and PE 27720.7 parts.
The above composite material was prepared in the same manner as in example 7.
Example 10
The polypropylene composite material for laser welding comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392038.6 parts, K901738 parts, AH-3000N 912 parts, POE 81375 parts, 5 parts of a polypropylene and polyamide block copolymer, 10100.15 parts of an antioxidant, 1680.15 parts, UV-3808PP 50.2 parts, TR 4510.2 parts and PE 27720.7 parts.
The above composite material was prepared in the same manner as in example 1.
Comparative example 1
This comparative example provides a polypropylene composite and a process for its preparation, according to example 1, 33.6 parts by weight of BX3920 in the composite was changed, without adding a block copolymer of polypropylene and polyamide, the remainder being the same as in example 1.
Comparative example 2
This comparative example provides a polypropylene composite and a process for its preparation, according to example 4, the BX3920 parts by weight of the composite was changed to 35.4 parts, no block copolymer of polypropylene and polyamide was added, AH-3000N9 parts by weight was changed to 20 parts, and the remainder was the same as in example 4.
Comparative example 3
This comparative example provides a polypropylene composite and a process for its preparation, according to example 7, the BX3920 parts by weight of the composite was changed to 26.1 parts, without adding a block copolymer of polypropylene and polyamide, the remainder being the same as in example 7.
Comparative example 4
According to the chinese patent CN1839031A, the present comparative example provides a polypropylene composite material, which comprises the following components in parts by weight: the anti-oxidation coating comprises, by weight, BX 392028.6 parts, K901735 parts, AH-3000N 912 parts, POE 813718 parts, maleic anhydride graft modified polypropylene wax 5 parts, antioxidant 10100.15 parts, antioxidant 1680.15 parts, UV-3808PP 50.2 parts, TR 4510.2 parts and PE 27720.7 parts. The composite material was prepared in the same manner as in example 1.
The composite materials in examples 1-10 and comparative examples 1-4 were injection molded into standard ISO mechanical splines for mechanical property testing (according to ISO standard method) under the same injection molding process (which is a conventional injection molding process in the field); and was injection molded with a selected nylon 6 material (Xinhui Meida PA 6M 2800) into a specimen having a size of 150mm x 15mm x 2mm, laser welded by a large-scale laser welder (WFD 120W-PCTS 333 SP) (welding process: laser wavelength 915nm, power 20W, welding speed 20mm/s, wherein nylon 6 is a light transmitting layer, and the polypropylene composite material of the present invention is a light absorbing layer) and then tested for welding force on a tensile machine (tensile speed 50 mm/min). The test results are shown in table 1.
TABLE 1
As can be seen from Table 1, the composite material of comparative example 1, in which no block copolymer of polypropylene and polyamide was added, had a significantly lower weld strength than that of example 1, a slightly lower tensile strength and flexural modulus than that of example 1, and a slightly higher notched impact strength than that of example 1. The composite material in comparative example 2, which does not contain the block copolymer of polypropylene and polyamide, has a significantly lower weld strength than example 4, a lower tensile strength and flexural modulus than example 4, and a slightly higher notched impact strength than example 4. The composite material of comparative example 3, in which no block copolymer of polypropylene and polyamide was added, had a significantly lower weld strength than example 7, a slightly lower tensile strength and flexural modulus than example 7, and a slightly higher notched impact strength than example 7. Therefore, whether the talcum powder is low or high, the welding force can be obviously improved by adding the block copolymer of the polypropylene and the polyamide into the composite material, the tensile strength and the flexural modulus are improved to a certain degree, and the impact strength is reduced to a small extent. The composite material in comparative example 4 added with maleic anhydride graft-modified polypropylene wax had a lower welding force than the polypropylene and polyamide block copolymer of the present invention, and the addition thereof caused a significant decrease in the tensile strength, flexural modulus and impact strength of the material at the notch of a simple beam. The amount of the block copolymer of polypropylene and polyamide added to the composite material was 10 parts, and the laser welding force was improved to 2 times or more as compared with the case where the block copolymer of polypropylene and polyamide was not added, while the amount of the block copolymer added was 15 parts, and the laser welding force was improved to 3 times or more.
Claims (10)
1. The polypropylene composite material for laser welding is characterized by comprising the following components in parts by weight: 39-80 parts of polypropylene, 10-30 parts of inorganic filler, 5-25 parts of toughening agent, 5-15 parts of laser welding modifier, 0.2-0.5 part of antioxidant, 0.2-0.5 part of weather resistant agent, 0.1-0.3 part of lubricant and 0.5-1.0 part of black master batch, wherein the laser welding modifier is a block copolymer of polypropylene and polyamide.
2. The composite material according to claim 1, wherein the polypropylene is at least one of homo-polypropylene and co-polypropylene, and the polypropylene melt index is 1-100g/10 min; the inorganic filler is at least one of talcum powder, calcium carbonate, wollastonite, mica, barium sulfate and magnesium sulfate whisker; the particle size of the inorganic filler is 1-10 μm.
3. The composite of claim 1, wherein the toughening agent is a copolymer of ethylene and an alpha olefin containing 3 to 10 carbon atoms, the toughening agent melt index is 0.5 to 30g/10 min; the antioxidant is at least one of phenol antioxidant, amine antioxidant, phosphite antioxidant and hindered phenol antioxidant.
4. The composite material according to claim 1, wherein the weather-resistant agent is at least one of a hindered amine light stabilizer, a benzotriazole light stabilizer, a benzophenone light stabilizer, and a triazine benzylidene malonate light stabilizer.
5. The composite material of claim 1, wherein the lubricant is at least one of an amide lubricant, a stearic lubricant, a fatty acid lubricant, and an ester lubricant.
6. A method of making the composite material of claim 1, comprising:
mixing polypropylene, inorganic filler, toughening agent, laser welding modifier, antioxidant, weather resistant agent, lubricant and black master batch, adding the mixed raw materials into a double-screw extruder for melt blending, extruding and granulating to obtain the polypropylene composite material for laser welding.
7. The method according to claim 6, wherein the block copolymer of polypropylene and polyamide is prepared by: adding polyamide and double-end carboxyl polypropylene into a toluene solution, carrying out reflux reaction for 24-30h under the protection of nitrogen, cooling, precipitating in methanol, washing and drying to obtain the polyamide, wherein the weight ratio of amino in the polyamide to carboxyl in the double-end carboxyl polypropylene is 2-2.5:1, and the viscosity of the polyamide is 5000-70000mpa.s/40 ℃.
8. The method of claim 7, wherein the carboxyl-terminated polypropylene is prepared by the following steps: mixing polypropylene and concentrated nitric acid at a ratio of 100g:450-550ml, heating to 120-140 ℃, stirring for 12-20h, washing, and drying to obtain the polypropylene with a molecular weight of 1000-6000 g/mol.
9. The method of claim 6, wherein the mixing time is 1-2 min; the melt blending temperature is 180-230 ℃.
10. Use of the composite material of claim 1 in laser welding.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114685905A (en) * | 2022-03-23 | 2022-07-01 | 上海金发科技发展有限公司 | Polypropylene composite material and preparation method and application thereof |
| CN115368701A (en) * | 2022-07-26 | 2022-11-22 | 武汉金发科技有限公司 | Weather-resistant laser-weldable polypropylene composite material and preparation method and application thereof |
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