CN114479272A - Low-odor automobile interior material and preparation method thereof - Google Patents
Low-odor automobile interior material and preparation method thereof Download PDFInfo
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- CN114479272A CN114479272A CN202210098988.4A CN202210098988A CN114479272A CN 114479272 A CN114479272 A CN 114479272A CN 202210098988 A CN202210098988 A CN 202210098988A CN 114479272 A CN114479272 A CN 114479272A
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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
- C08L23/12—Polypropene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60R—VEHICLES, VEHICLE FITTINGS, OR VEHICLE PARTS, NOT OTHERWISE PROVIDED FOR
- B60R13/00—Elements for body-finishing, identifying, or decorating; Arrangements or adaptations for advertising purposes
- B60R13/02—Internal Trim mouldings ; Internal Ledges; Wall liners for passenger compartments; Roof liners
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Abstract
The invention provides a low-odor automotive interior material and a preparation method thereof, relating to the field of automotive interior materials; the method comprises the following components in parts by weight: 60-85 parts of polypropylene, 10-30 parts of filler, 0.5-2 parts of adsorbent, 0.5-1 part of lubricant, 3-10 parts of toughening agent and 0.3-1 part of antioxidant, blending, adding into a double-screw extruder, uniformly mixing, and obtaining a primary product after melt plasticizing, kneading and mixing, extruding, cooling, granulating and drying; and (3) adding the primary product into an autoclave, and purifying the primary product by adopting an autoclave supercritical fluid batch mode to prepare the low-odor automobile interior material. The invention adopts the high-pressure kettle supercritical fluid intermittent mode to prepare the automobile interior material with the odor grade of 3.0 and below, thereby effectively solving the increasingly strict requirements of the current market on the odor of the automobile material; meanwhile, compared with the method of directly drying the material, the supercritical fluid technology is adopted, so that the efficiency is greatly improved, and the tensile property of the material can be kept and the impact property can be improved.
Description
Technical Field
The invention relates to the technical field of automotive interior materials, in particular to a low-odor automotive interior material and a preparation method thereof.
Background
With the increase of the demand of automobiles in the current market, the requirements of passengers on the odor and VOC of automobile interior materials are also improved along with the increase of the demand, China correspondingly develops the (GB/T2730) standard for controlling the air quality in the automobile in consideration of the requirements of the passengers, the automobile interior materials are the main influence factors of large smell and high VOC in the automobile, small molecular organic matters such as benzene and formaldehyde emitted by the automobile interior materials are the main reasons of large smell in the automobile, and the small molecular organic matters have great damage to the health of the passengers. Therefore, in terms of material selection, it is important to select materials with lower odor and lower VOC for the automotive interior.
The traditional method for preparing the low-odor and low-VOC automotive interior material at present comprises the following steps: (1) the method for treating the vacuum drying material can improve the smell of the material and reduce VOC to a certain extent, but the method has limited improvement effect which is far away from the control standard of air in a vehicle, the treatment time is 10 hours or more, the efficiency is low, and the performance of the material is correspondingly reduced due to the high temperature; (2) the method for adding the inorganic porous adsorbent in the material formula can relatively adsorb partial micromolecules, but the requirement is high when the adsorption balance is required to be achieved, the odor and VOC (volatile organic compounds) of the material are difficult to reduce for a long time, the addition proportion is high, the basic performance of the material is obviously reduced, and the performance required by the material in a vehicle is difficult to achieve.
At present, more and more researchers shift the method for preparing the low-odor material to the supercritical fluid purification technology, the supercritical is a state between gas and liquid, the most used of the method in the market at present are supercritical carbon dioxide and supercritical nitrogen, the method is environment-friendly and simple, the solubility of the supercritical gas to the small molecules is high, and the supercritical carbon dioxide and the supercritical nitrogen can be effectively used as a medium for purifying the automobile interior material, for example, the patent CN107090128B prepares the low-odor material by continuously extruding the supercritical fluid technology, the method is efficient and environment-friendly, but the process control is difficult, the solubility of the supercritical gas to the small molecules is reduced along with the temperature increase, the pressure is increased along with the pressure increase, the extrusion equipment is difficult to realize high pressure, and the temperature is too high, the solubility is low, and the odor improvement and VOC reduction are limited due to the melt extrusion temperature.
Disclosure of Invention
The invention aims to provide a low-odor automobile interior material and a preparation method thereof, which are used for purifying the automobile interior material by using a high-pressure kettle supercritical fluid intermittent mode, so that the increasingly strict requirements on the odor of the automobile material on the current market are fully met, and the odor grade of the material is 3.0 grade or below.
In order to achieve the above purpose, the invention provides the following technical scheme: a preparation method of a low-odor automobile interior material comprises the following steps:
(1) weighing the following components in parts by weight: 60-85 parts of polypropylene, 10-30 parts of filler, 0.5-2 parts of adsorbent, 0.5-1 part of lubricant, 3-10 parts of toughening agent and 0.3-1 part of antioxidant, blending, adding into a double-screw extruder, uniformly mixing, and obtaining a primary product after melt plasticizing, kneading and mixing, extruding, cooling, grain cutting and drying;
(2) and (3) adding the primary product into an autoclave, and purifying the primary product by adopting an autoclave supercritical fluid batch mode to prepare the low-odor automobile interior material.
Further, the process for purifying the primary product in the step (2) by the high-pressure kettle supercritical fluid batch mode comprises the following steps: placing the primary product into an autoclave, controlling the temperature in the autoclave to be 80-140 ℃, controlling the pressure of the supercritical fluid in the autoclave to be 6-12 MPa, keeping the temperature and the pressure constant for 10-90 minutes, cooling to 80 ℃, and then releasing the pressure to the normal pressure at the speed of 1-20 MPa/s; wherein the volume of the primary product in the autoclave is 1/3-2/3 of the volume of the autoclave.
Further, the supercritical fluid is carbon dioxide, nitrogen, pentane, butane or heptane.
Further, the polypropylene is homo-polypropylene, co-polypropylene or a compound of the homo-polypropylene and the co-polypropylene, and the dissolved fat of the polypropylene is more than 10g/10 min.
Further, the filler is one or more of calcium carbonate, talcum powder, wollastonite, alkali barium sulfate, hollow glass beads, whiskers and mica.
Further, the adsorbent is one or more of nano alkali metal chloride, alkali metal sulfate, montmorillonite, porous carbon, molecular sieve and attapulgite.
Further, the lubricant is one or more of stearic acid, polyethylene wax, EBS and ammonium monoacid.
Further, the toughening agent is POE, EMA, EBA, EVA or LDPE.
Further, the antioxidant is one or two of antioxidant 1010, antioxidant 168, antioxidant 330, antioxidant 1098 and antioxidant H318.
The invention also discloses a low-odor automobile interior material, which is prepared by the preparation method of the low-odor automobile interior material.
According to the technical scheme, the technical scheme of the invention has the following beneficial effects:
the invention discloses a low-odor automobile interior material and a preparation method thereof, wherein the preparation method comprises the following steps of weighing the following components in parts by weight: 60-85 parts of polypropylene, 10-30 parts of filler, 0.5-2 parts of adsorbent, 0.5-1 part of lubricant, 3-10 parts of toughening agent and 0.3-1 part of antioxidant, blending, adding into a double-screw extruder, uniformly mixing, and obtaining a primary product after melt plasticizing, kneading and mixing, extruding, cooling, grain cutting and drying; adding the primary product into an autoclave, and purifying the primary product by adopting an autoclave supercritical fluid intermittent mode to prepare a low-odor automobile interior material; the invention can prepare the automobile interior material with the odor grade of 3.0 grade or below by adopting the high-pressure kettle supercritical fluid intermittent mode, and effectively meets the increasingly strict requirements of the current market on the odor of the automobile material.
Meanwhile, compared with the direct drying of the material, the efficiency of the supercritical fluid technology is greatly improved, and because the supercritical fluid has a plasticizing effect on the material, the internal stress in the material can be greatly reduced, so that the mechanical property and the impact property of the material are improved; in addition, because the supercritical fluid is adopted to process the primary product, unstable beta crystals in the primary product are converted into stable alpha crystals, so that the tensile property of the material can be relatively improved.
It should be understood that all combinations of the foregoing concepts and additional concepts described in greater detail below can be considered as part of the inventive subject matter of this disclosure unless such concepts are mutually inconsistent.
The foregoing and other features of the present teachings will be more fully understood from the following description taken in conjunction with the accompanying examples. Additional aspects of the present invention, such as features and/or advantages of exemplary embodiments, will be apparent from the description which follows, or may be learned by practice of specific embodiments in accordance with the teachings of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few 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 described embodiments of the invention without any inventive step, are within the scope of protection of the invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
The use of "first," "second," and similar terms in the description and in the claims of the present application does not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. Similarly, the singular forms "a," "an," or "the" do not denote a limitation of quantity, but rather denote the presence of at least one, unless the context clearly dictates otherwise. The terms "comprises," "comprising," or the like, mean that the elements or items listed before "comprises" or "comprising" encompass the features, integers, steps, operations, elements, and/or components listed after "comprising" or "comprising," and do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
With social development, gradual expansion of the market demand of automobiles and safety and health, the requirements of passengers on the odor and VOC of the automobile interior materials are greatly improved; the low-odor and low-VOC automotive interior material prepared by the traditional method is difficult to achieve the required performance of the automotive interior material due to the existence of factors such as limited improvement effect, long treatment time, influence on material performance and the like; in order to solve the problems, the prior art proposes that a supercritical fluid purification technology is applied to the preparation of low-odor materials, but the process is difficult to control, and the odor improvement and VOC reduction of the materials are limited. The invention provides a low-odor automobile interior material and a preparation method thereof, aiming at the problem of great operation difficulty in preparing the low-odor material by a continuous extrusion mode through a supercritical fluid purification technology, the material is intermittently purified by a supercritical fluid of a high-pressure kettle after being extruded by double screws, and the odor of the obtained material can reach the grade of 3.0 or below, so that the market requirement is fully met.
Specifically, the preparation method of the low-odor automobile interior material disclosed by the invention comprises the following steps of:
(1) weighing the following components in parts by weight: 60-85 parts of polypropylene, 10-30 parts of filler, 0.5-2 parts of adsorbent, 0.5-1 part of lubricant, 3-10 parts of toughening agent and 0.3-1 part of antioxidant, blending, adding into a double-screw extruder, uniformly mixing, and obtaining a primary product after melt plasticizing, kneading and mixing, extruding, cooling, grain cutting and drying;
(2) adding the primary product into an autoclave, and purifying the primary product by adopting an autoclave supercritical fluid intermittent mode to prepare a low-odor automobile interior material; putting the primary product into an autoclave, controlling the temperature in the autoclave at 80-140 ℃, controlling the pressure of a supercritical fluid in the autoclave at 6-12 MPa, keeping the temperature and the pressure constant for 10-90 minutes, cooling to 80 ℃, and then releasing the pressure to the normal pressure at the speed of 1-20 MPa/s; wherein the volume of the primary product in the high-pressure kettle accounts for 1/3-2/3 of the volume of the high-pressure kettle, and the supercritical fluid is one of carbon dioxide, nitrogen, pentane, butane and heptane; carbon dioxide, nitrogen, pentane, butane or heptane are all good in terms of environmental protection, energy and solubility with polymers, and supercritical carbon dioxide is the best effect, so in the embodiment, the supercritical fluid is carbon dioxide.
When the preparation method is implemented, in the step (1), the polypropylene fat dissolving is more than 10g/10min, and homo-polypropylene, co-polypropylene or a compound of the homo-polypropylene and the co-polypropylene are selected; the filling agent is one or more of calcium carbonate, talcum powder, wollastonite, alkali barium sulfate, hollow glass beads, crystal whiskers and mica; the adsorbent is selected from one or more of nanometer alkali metal chloride, alkali metal sulfate, montmorillonite, porous carbon, molecular sieve and attapulgite, and the porous carbon is preferred from the aspects of cost and adsorption effect; the lubricant is one or more of stearic acid, polyethylene wax, EBS and ammonium monoacid, and the compound of polyethylene wax and stearic acid is selected in the following embodiment; the toughening agent is POE, EMA, EBA, EVA or LDPE, and POE is selected in the embodiment; the antioxidant is one or two of antioxidant 1010, antioxidant 168, antioxidant 330, antioxidant 1098 and antioxidant H318, and the antioxidant is preferably a compound of antioxidant 1010 and antioxidant 168 from the viewpoint of cost.
The low-odor automobile interior material and the method for producing the same disclosed in the present invention will be further described with reference to the following examples.
Example 1
Weighing the following components in parts by weight: 74 parts of polypropylene, 20 parts of filler, 5 parts of toughener POE, 0.2 part of antioxidant 1010 and antioxidant 168 and 0.3 part of polyethylene wax and stearic acid respectively, blending the raw materials in a low-speed stirrer for 20 minutes, adding the mixture into a double-screw extruder with two vacuumizing devices, uniformly mixing, and carrying out melt plasticizing, kneading and mixing, extruding, cooling, granulating and drying on the mixed material to obtain a primary product A;
weighing the following components in parts by weight: 73 parts of polypropylene, 20 parts of filler, 5 parts of toughener POE, 1 part of adsorbent, 0.2 part of antioxidant 1010 and antioxidant 168 respectively, and 0.3 part of polyethylene wax and stearic acid respectively, blending the raw materials in a low-speed stirrer for 20 minutes, adding the mixture into a double-screw extruder with two vacuumizing devices, uniformly mixing, and carrying out melt plasticization, kneading and mixing, extrusion, cooling, grain cutting and drying on the mixed material to obtain a primary product B;
weighing the following components in parts by weight: 71 parts of polypropylene, 20 parts of filler, 5 parts of toughener POE, 3 parts of adsorbent, 0.2 part of antioxidant 1010 and antioxidant 168 respectively, and 0.3 part of polyethylene wax and stearic acid respectively, blending the raw materials in a low-speed stirrer for 20 minutes, adding the mixture into a double-screw extruder with two vacuumizing devices, uniformly mixing, and carrying out melt plasticization, kneading and mixing, extrusion, cooling, grain cutting and drying on the mixed material to obtain a primary product C.
The material property tests were performed on each of the virgin products A, B and C, and the property results are shown in Table 1 below.
TABLE 1 comparison of Properties of Primary product A, B, C
According to the parameter results of the primary products, the mechanical property, the impact property and the odor grade of the materials are integrated, the primary product B is selected to continuously prepare the automotive interior material meeting the requirements, namely, the primary product B is placed into an autoclave, the automotive interior material with low odor is prepared by adopting the supercritical fluid technology of the autoclave and through a specific process, the automotive interior material products of the following examples 2-5 and comparative example 1 are obtained by different processes, the performance and the odor of each product are respectively carried out, and the results are shown in the following tables 2 and 3.
Example 2
Placing the primary product B into an autoclave, controlling the temperature in the autoclave to be 100 ℃, controlling the pressure of the supercritical fluid in the autoclave to be 8MPa, keeping the temperature and the pressure constant for 40 minutes, cooling to 80 ℃, and then releasing the pressure to the normal pressure at the speed of 10 MPa/s; wherein the addition amount of the primary product in the autoclave accounts for 2/3 of the volume of the autoclave.
TABLE 2 Process treatment parameters for examples and comparative examples
Comparative example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Constant temperature/. degree.C | / | 100 | 120 | 120 | 120 |
Constant temperature and pressure time/min | / | 40 | 40 | 80 | 80 |
Constant pressure/MPa | / | 8 | 8 | 8 | 10 |
Of these, comparative example 1 is a primary product B that was not treated by the autoclave supercritical fluid technique.
TABLE 3 comparison of Material Properties of examples and comparative examples
In the invention, the odor of the automotive interior material treated by the supercritical autoclave treatment process in examples 2-5 is greatly improved compared with the untreated comparative example, the basic mechanical properties of the material are improved to a certain extent, and the impact toughness is improved most obviously. The product obtained by the invention has low odor and better mechanical properties.
Specifically, in the present invention, it is found by comparing the primary product a, the grade product B, and the grade product C in example 1 that the odor of the product is relatively reduced to a certain extent with the increase of the adsorbent, but the mechanical properties of the product are significantly reduced, and it is difficult to achieve a state of balancing the odor and the mechanical properties, so that the present invention uses the supercritical fluid technology to purify the product to obtain examples 2-5, and the process and performance results are shown in table 3 above, and it can be found that the supercritical fluid purification process has a great influence on the odor and the mechanical properties of the product, and it can be seen from comparison between the examples and comparative examples that the odor of the product is significantly improved and the mechanical properties of the product are relatively improved to a certain extent with the supercritical purification technology. The main difference between example 3 and example 4 is the difference between the constant temperature and pressure time, and it was found that the odor improvement and the mechanical property increase more remarkably with the increase of the constant temperature and pressure time, because the supercritical fluid purification requires a certain saturation time for the fluid to dissolve into the product, the saturation time is insufficient, and the odor improvement is relatively poor compared with the dissolution rate; the main difference between example 2 and example 3 is the difference between the constant temperature, and the constant temperature has a certain influence on the odor and mechanical properties of the product, because the higher the temperature (lower than the melting temperature), the more small molecules affecting the odor in the product are emitted, so that the supercritical fluid is easier to dissolve, and the relative dissolution efficiency is improved; the main difference between examples 4 and 5 is the difference between the constant pressure and the constant pressure, and the comparison shows that the mechanical property and the odor of the product are improved to some extent with the increase of the constant pressure, because the solubility of the supercritical fluid is increased due to the increase of the pressure, so that the more small molecules which affect the odor are dissolved, which results in the improvement of the odor. The mechanical properties of examples 2-5 were all improved, wherein the improvement of impact toughness was due to the plasticizing effect of the supercritical fluid on the product, which greatly reduced the internal stress inside the product, and the improvement of tensile strength was due to the supercritical fluid processing of the product, in which unstable β -crystals in the polyolefin were converted to stable α -crystals, and all tensile properties were relatively improved.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, the protection scope of the present invention should be determined by the appended claims.
Claims (10)
1. A preparation method of a low-odor automobile interior material is characterized by comprising the following steps:
(1) weighing the following components in parts by weight: 60-85 parts of polypropylene, 10-30 parts of filler, 0.5-2 parts of adsorbent, 0.5-1 part of lubricant, 3-10 parts of toughening agent and 0.3-1 part of antioxidant, blending, adding into a double-screw extruder, uniformly mixing, and obtaining a primary product after melt plasticizing, kneading and mixing, extruding, cooling, grain cutting and drying;
(2) and (3) adding the primary product into an autoclave, and purifying the primary product by adopting an autoclave supercritical fluid batch mode to prepare the low-odor automobile interior material.
2. The method for preparing a low-odor automobile interior material according to claim 1, wherein the process for purifying the primary product in the batch manner by using the high-pressure supercritical fluid in the step (2) comprises the following steps: placing the primary product into an autoclave, controlling the temperature in the autoclave to be 80-140 ℃, controlling the pressure of the supercritical fluid in the autoclave to be 6-12 MPa, keeping the temperature and the pressure constant for 10-90 minutes, cooling to 80 ℃, and then releasing the pressure to the normal pressure at the speed of 1-20 MPa/s; wherein the volume of the primary product in the autoclave is 1/3-2/3 of the volume of the autoclave.
3. The method for preparing a low-odor automobile interior material according to claim 1, wherein the supercritical fluid is carbon dioxide, nitrogen, pentane, butane or heptane.
4. The method for preparing a low-odor automobile interior material according to claim 1, wherein the polypropylene is homo-polypropylene, co-polypropylene or a compound of the homo-polypropylene and the co-polypropylene, and the polypropylene solvent is greater than 10g/10 min.
5. The method for producing a low-odor automobile interior material according to claim 1, wherein the filler is one or more of calcium carbonate, talc, wollastonite, basic barium sulfate, hollow glass beads, whiskers, and mica.
6. The method for producing a low-odor automobile interior material according to claim 1, wherein the adsorbent is one or more of nano alkali metal chloride, alkali metal sulfate, montmorillonite, porous carbon, molecular sieve, and attapulgite.
7. The method for producing a low-odor automobile interior material according to claim 1, wherein the lubricant is one or more of stearic acid, polyethylene wax, EBS, ammonium mesoamide.
8. The method for producing a low-odor automobile interior material according to claim 1, wherein the toughening agent is POE, EMA, EBA, EVA, or LDPE.
9. The preparation method of the low-odor automobile interior material as claimed in claim 1, wherein the antioxidant is one or two of antioxidant 1010, antioxidant 168, antioxidant 330, antioxidant 1098 and antioxidant H318.
10. A low-odor automotive interior material, characterized in that it is produced by the method for producing a low-odor automotive interior material according to any one of claims 1 to 9.
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CN106243483A (en) * | 2016-08-29 | 2016-12-21 | 合肥会通新材料有限公司 | A kind of zero VOC polypropylene material and preparation technology thereof |
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CN109722013A (en) * | 2018-12-14 | 2019-05-07 | 宁波能之光新材料科技股份有限公司 | A kind of low VOC high-strength and high ductility nylon and preparation method thereof |
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CN103214740A (en) * | 2013-04-28 | 2013-07-24 | 长城汽车股份有限公司 | Polypropylene composite material for automobile internal ornament, preparation method thereof and internal ornament |
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