CN107698876B - VOC (volatile organic compound) extracting agent for modified polypropylene as well as preparation method and application of VOC extracting agent - Google Patents
VOC (volatile organic compound) extracting agent for modified polypropylene as well as preparation method and application of VOC extracting agent Download PDFInfo
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Abstract
The invention discloses a VOC extractant for modified polypropylene and a preparation method and application thereof. The VOC extracting agent for modified polypropylene comprises, by weight, 11-50wt% of a polypropylene carrier and 50-89wt% of a non-fluorine non-ionic surfactant solution; the non-fluorine non-ionic surfactant solution comprises 0.1 to 2.5 weight percent of non-fluorine non-ionic surfactant and 97.5 to 99.9 weight percent of solvent. The VOC extracting agent for modified polypropylene has the characteristics of safety, environmental protection, low price and the like, and has extremely high removal efficiency on VOC in the modified polypropylene material; in the preparation process of the environment-friendly modified polypropylene material, the VOC extractant for modified polypropylene is mixed with polypropylene and an auxiliary agent, and then the mixture is stirred and mixed uniformly by a high-efficiency mixer and then extruded and granulated by a double screw to obtain the environment-friendly modified polypropylene composite material.
Description
Technical Field
The invention relates to a composite high polymer material and the processing technical field thereof, in particular to a VOC extracting agent for modified polypropylene and a preparation method and application thereof.
Background
Polypropylene is a thermoplastic resin obtained by polymerizing propylene, has the advantages of heat resistance and corrosion resistance, and is the lightest general-purpose plastic. The modified polypropylene has the characteristics of high crystallinity, excellent mechanical property, easy processing and forming, excellent appearance and low price, is widely applied to automotive interior parts, such as instrument panels, auxiliary instrument panels, door panels, map bags, glove boxes, stand columns and the like, and the dosage of the modified polypropylene accounts for about 50 percent of the polymer material of the whole automobile.
During the extrusion, granulation and molding processes of the polypropylene resin, due to the melt shearing and thermo-oxidative degradation, Volatile Organic Compounds (VOC) such as amine, phenol, thiol, peroxide, benzene, aldehyde, ketone, some plasticizers and flame retardants are released, and TVOC is the total amount of Volatile organic compounds to be detected. Volatile organic compounds contain benzene series and aldehyde ketone compounds with different concentrations and cause harm to human health, and alkane compounds of C6-C16 are main sources of peculiar smell and bring discomfort to drivers and passengers. In 2012, the first national standard for the air quality in the vehicle, namely 'guidance for evaluating the air quality in the vehicle for passenger' GB/T27630-. The 2016 department of environmental protection reissues the latest "guidance for evaluating air quality in passenger vehicles", which is a standard that is updated from recommendation to mandatory and is enforced from 1/2017. Each automotive host plant modifies the relevant standards and enhances material VOC and odor management. Therefore, how to further reduce the VOC of the modified polypropylene material for automobiles and improve the odor grade is a problem to be solved.
The reduction of volatile organic compounds and odor can be done mainly from two aspects, one is the removal of volatile organic compounds during the extrusion process and the other is the reduction and containment of sources. US5109056 reports high vacuum devolatilization during extrusion, with a high temperature bake process to further reduce VOC. The method can remove VOC generated in the extrusion process to a certain extent, but the residual part is left after the forming processing and even the assembly of a workpiece, so the devolatilization method in the extrusion process can only be used as a general compensation method and is not suitable for large-scale blending modification.
The addition of the adsorbent can produce physisorption and/or chemisorption of the volatile. The Chinese patent CN 1727389A adds an odor remover in the basic formula of the polypropylene material, and the odor remover can effectively reduce the odor of the polypropylene material and reduce the volatile gas in the material. The odor remover added in the invention is a fine-pore silica gel material with the pore diameter of 20-30 angstroms and the fineness of 800-6000 meshes. The odor of the polypropylene material can be effectively reduced through micropores with specific pore size and uniform distribution of the fine-pore silica gel. However, the porous silica gel has poor compatibility with polypropylene plastics, and other properties of the plastics are affected. Patent CN 105504507 a controls VOC release by adsorption of volatile organic compounds by water-soluble fluorocarbon surfactant, and the fluorine-containing surfactant remains in the material and can cause potential health damage.
Disclosure of Invention
The invention aims to provide the VOC extractant for the modified polypropylene, which has the advantages of low cost, simple process, environmental protection and good VOC removing effect. The invention also aims to provide a preparation method of the VOC extracting agent and application of the VOC extracting agent in preparation of environment-friendly modified polypropylene.
The invention is realized by the following technical scheme:
the VOC extracting agent for the modified polypropylene comprises the following components in percentage by weight:
11-50wt% of polypropylene carrier;
50-89wt% of non-fluorine non-ionic surfactant solution.
The polypropylene carrier comprises 60-90wt% of high melt strength polypropylene and 10-40wt% of porous adsorbent according to weight percentage; the high melt strength polypropylene is selected from polypropylene with melt strength more than or equal to 30 cN.
The melt strength test method comprises the following steps: measured using a rheometer at 230 ℃ with an acceleration of 30m/s2The melt strand was drawn off and the tensile hardness value and draw-off rate were recorded.
The melt strength of the polypropylene carrier is more than or equal to 30cN, the pore diameter of the cells is 20-60 microns,the distribution density of the foam holes is more than or equal to 105/cm3. The method for testing the pore diameter and the distribution density of the cells comprises the following steps: observing the section by using a scanning electron microscope, and calculating the average pore diameter and the distribution density in a statistical mode: the average pore size is obtained by analyzing with nano measurer software, and the distribution density is calculated by the following formula: n is a radical off=(nM2/A)3/2(ii) a Wherein Nf is distribution density, and A is area cm of scanning electron microscope field2N is the number of cells in the field of view and M is the magnification.
The porous adsorbent is selected from at least one of silicate and aluminosilicate.
Wherein the silicate can be at least one of diatomite, expanded perlite, expanded vermiculite and attapulgite; the aluminosilicate can be selected from zeolite, 3A molecular sieve, 4A molecular sieve, 5A molecular sieve, 10X molecular sieve, 13X molecular sieve, etc.
Preferably, the porous adsorbent has a water vapor adsorption capacity of more than or equal to 30mg/g at 10% RH and more than or equal to 300mg/g at 50% RH, and the test standard is GB/T6287-.
The non-fluorine non-ionic surfactant solution comprises 97.5 to 99.9 weight percent of one or more of water or alcohols with the boiling point lower than 120 ℃ and 0.1 to 2.5 weight percent of non-fluorine non-ionic surfactant; the alcohol with the boiling point lower than 120 ℃ is selected from at least one of methanol, ethanol, propanol and butanol.
The non-fluorine non-ionic surfactant is at least one selected from polysorbates, Triton non-ionic surfactants, polyoxyethylene ether non-ionic surfactants, fluorine-free low-foam quick-acting scouring and bleaching agents and 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol (TMDD).
The polysorbate is selected from at least one of Tween 20 (Tween 20), Tween 60 (Tween 60) and Tween 80 (Tween 80).
The Triton nonionic surfactant is selected from Triton X-100.
The polyoxyethylene ether nonionic surfactant can be one or more of laurylamine polyoxyethylene ether and stearylamine polyoxyethylene ether.
The fluorine-free low-foam quick-acting scouring and bleaching agent is selected from JL-906-F.
The preparation method of the VOC extractant for the modified polypropylene comprises the following steps:
and (3) stirring the polypropylene carrier and the non-fluorine non-ionic surfactant solution for 3-5 minutes at the speed of 1000 revolutions per minute by a high-speed stirrer according to the proportion so that the non-fluorine non-ionic surfactant solution is fully adsorbed on the polypropylene carrier to obtain the VOC extracting agent for modified polypropylene.
The preparation method of the polypropylene carrier comprises the following steps:
a. fully and uniformly mixing the high-melt-strength polypropylene and the porous adsorbent in a high-speed stirrer, and performing melt blending extrusion granulation in an extruder to obtain a foamed polypropylene precursor;
b. foaming the foamed polypropylene precursor by adopting a physical foaming agent to prepare a polypropylene carrier;
the physical foaming agent is one or two of nitrogen or supercritical carbon dioxide.
The VOC extractant for the modified polypropylene is used for preparing an environment-friendly modified polypropylene material, and the process flow is as follows: and adding talcum powder into the extruder from a side feeding port, uniformly mixing the polypropylene and the VOC extractant in a high-speed mixer, and adding the mixture into the double-screw extruder from a main feeding port for melt blending. Controlling the vacuum degree, extruding and granulating to obtain the environment-friendly modified polypropylene composite material. The addition amount of the VOC extractant for the modified polypropylene is 0.1-15 parts by weight of the total weight of the environment-friendly modified polypropylene, and the specific amount is set according to the concentration of the non-fluorine nonionic surfactant solution, the total mass percentage of the VOC extractant for the modified polypropylene and the odor performance and mechanical performance required by the prepared environment-friendly modified polypropylene material.
The mechanism of the invention is as follows: the non-fluorine non-ionic surfactant solution is adsorbed in the foam pores of the foamed polypropylene, and the porous adsorption material with physical adsorption effect is dispersed in the foamed polypropylene carrier at the same time. During the extrusion process of polypropylene, the porous adsorption material in the foamed polypropylene adsorbs a large amount of VOC. The non-fluorine non-ionic surfactant has the function of increasing VOC capacity, VOC in the porous adsorption material is extracted and adsorbed in a non-fluorine non-ionic surfactant solution, the non-fluorine non-ionic surfactant solution is heated to form tiny fog beads, and the non-fluorine non-ionic surfactant solution containing VOC is extracted and separated under the action of vacuum negative pressure, so that the process of porous adsorption-extraction-devolatilization is realized. The extraction-devolatilization process which does not pass through the porous adsorption material exists in the extrusion process at the same time. The two processes supplement each other, and the VOC removing efficiency is obviously improved.
The invention has the following beneficial effects for the prior art:
1. the VOC extractant for modified polypropylene prepared by the invention is mainly alcohols or water with the boiling point lower than 120 ℃ in the total mass of the VOC extractant, and the non-fluorine non-ionic surfactant solution absorbs a large amount of VOC in the extrusion process of polypropylene and is extracted in vacuum, so that secondary pollution is avoided. Therefore, the extractant has the characteristics of safety, environmental protection and the like.
2. The VOC extracting agent for modified polypropylene has extremely high efficiency of removing VOC in polypropylene: a small amount of non-fluorine non-ionic surfactant plays a role in increasing the adsorption effect of the solvent on VOC, and the VOC removing efficiency is remarkably improved through the process of porous adsorption, extraction and devolatilization without the extraction and devolatilization of a porous adsorption material in the polypropylene extrusion process. The VOC content of the modified polypropylene material is greatly reduced, and the odor is also obviously reduced.
3. According to the VOC extracting agent for the modified polypropylene, the processed environment-friendly modified polypropylene has the advantages that the VOC content is greatly reduced, the odor is remarkably reduced, and a small amount of porous adsorbent remained in the environment-friendly modified polypropylene hardly influences the mechanical property of the polypropylene.
4. The non-fluorine nonionic surfactant and the porous adsorbent used in the VOC extracting agent for modified polypropylene are cheap and easily available, and the processing procedure is simple, so that the VOC extracting agent is suitable for large-scale production.
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, not intended to limit the scope of the invention.
The raw materials used in the examples and comparative experiments are, but not limited to, the following:
polypropylene: PP M2600R, a co-polypropylene, melt flow rate 25g/10min (230 ℃, 2.16 kg), commercially available from Shanghai petrochemicals;
high melt strength polypropylene: PP WB140HMS available from northern european chemical with a melt strength of 35 cN;
ordinary polypropylene: EP300M, kadsura, melt strength 8cN;
talc powder: TYT-777A, 3000 mesh, purchased from Aihai, Liaoning;
diatomite: purchased from CELITE, water vapor adsorption capacity 90 mg/g (10% RH) and 460mg/g (50% RH);
concave-convex rod: xuyi Xin Yuan technology Co., Ltd, water vapor adsorption amounts of 76 mg/g (10% RH) and 387mg/g (50% RH);
expanded perlite: purchased from Wuhanyounike, water vapor adsorption amounts of 55 mg/g (10% RH) and 365mg/g (50% RH);
zeolite: purchased from Jiahe and New materials, water vapor adsorption 85 mg/g (10% RH) and 438mg/g (50% RH);
3A molecular sieve: purchased from Shanghai Hengshi molecular sieves, Inc., having water vapor adsorption amounts of 98 mg/g (10% RH) and 465mg/g (50% RH);
5A molecular sieve: purchased from Shanghai Hengshi molecular sieves, Inc., having water vapor adsorption amounts of 110 mg/g (10% RH) and 480mg/g (50% RH);
3000 mesh talc powder: AH51205, quality of Talc from Aihai, Liaoning, with water vapor adsorption of 5mg/g (10% RH) and 600mg/g (50% RH);
water: self-made deionized water;
ethanol: absolute ethanol, purchased from Guangzhou chemical industries;
triton X-100: purchased from Sigma-Aldrich;
tween 20: purchased from Haian petrochemical;
tween 60: purchased from Haian petrochemical;
tween 80: purchased from Haian petrochemical;
laurylamine polyoxyethylene ether: wedomine E1202, available from Wedu chemical industries;
stearylamine polyoxyethylene ether: wedomine E1802, available from Wedu chemical;
examples 1-20 and comparative examples 1-2:
preparation of polypropylene carrier:
according to the mixture ratio of tables 1 and 2, polypropylene and the porous adsorbent are fully and uniformly mixed in a high-speed stirrer, and are melted, blended, extruded and granulated in an extruder to obtain a foaming polypropylene precursor; foaming the foamed polypropylene precursor by adopting a physical foaming agent to prepare a polypropylene carrier; the polypropylene support performance test results are shown in table 4.
Preparing a VOC extractant for modified polypropylene:
according to the mixture ratio of the table 1 and the table 2, the prepared polypropylene carrier and the non-fluorine non-ionic surfactant solution are stirred for 3-5 minutes at the speed of 1000 revolutions per minute by a high-speed stirrer according to the mixture ratio to obtain the VOC extracting agent for the modified polypropylene.
Examples 21 to 40 and comparative examples 3 to 4:
preparation of the environment-friendly modified polypropylene composite material:
the VOC extractants for modified polypropylene prepared according to the sequence in the tables 1 and 2 are used for further preparing environment-friendly modified polypropylene composite materials in sequence (examples 1-20 correspond to examples 21-40 in sequence, and comparative examples 1-2 correspond to comparative examples 3-4 in sequence): 20 parts by weight of talcum powder is put into an extruder from a side feeding port, 78 parts by weight of polypropylene and 2 parts by weight of VOC (volatile organic compound) extractant are uniformly mixed in a high-speed mixer and then are put into a double-screw extruder from a main feeding port for melt blending. Controlling the vacuum degree, extruding and granulating to obtain the environment-friendly modified polypropylene composite material. The odor performance test results of the environment-friendly modified polypropylene composite material are shown in Table 3, and the mechanical performance test results are shown in Table 5.
The performance test method comprises the following steps:
VOC was measured as SJ-NW-39, SJ-NW-42 and SJ-NW-43;
odor was measured according to popular PV 3900: sampling: 20 plus or minus 2g of plastic particles; the test conditions are as follows: putting the sample into a 1L popular smell bottle, drying for 2h +/-10 min at the temperature of 80 +/-2 ℃, taking out and cooling to 60 +/-5 ℃; evaluation: at least 3 odor panelists rating; the determination requirements are as follows,
the tensile strength is according to ISO 527-2, the test condition is 50mm/min, 23 ℃;
the bending strength and the bending modulus are according to ISO 178, the testing conditions are 2mm/min and 23 ℃;
the impact strength of the cantilever beam notch is according to ISO 180, the test condition is 23 ℃, and the pendulum energy is 4J;
melt strength test method: measured using a rheometer at 230 ℃ at 30m/s2The melt wire was drawn off with acceleration and the tensile hardness value and draw off rate were recorded.
The method for testing the pore diameter and the distribution density of the cells comprises the following steps: and observing the section by using a scanning electron microscope, and calculating the average pore diameter and the distribution density in a statistical manner. The average pore size is obtained by analyzing with nano measurer software, and the distribution density is calculated by the following formula: n is a radical off=(nM2/A)3/2Wherein Nf is distribution density, and A is area cm of scanning electron microscope field2N is the number of cells in the field of view and M is the magnification.
Table 1: examples 1-20 VOC extraction agents for Polypropylene were prepared in the proportions (wt%)
TABLE 1
Table 2: comparative examples 1-2 VOC extraction agents for Polypropylene in respective component ratios (wt%)
Table 3: odor performance test result of environment-friendly modified polypropylene composite material
TABLE 3
TABLE 3
Table 4: test results on Polypropylene Carrier
Table 5: mechanical property test result of environment-friendly modified polypropylene composite material
As can be seen from the examples and comparative examples, the use of the VOC extractants for modified polypropylene effectively removes VOCs from the modified polypropylene and reduces odor levels. In general, the addition of the non-fluorine type non-ionic surfactant has a great promoting effect on the removal of VOC, and the VOC removal efficiency is increased along with the increase of the dosage of the non-fluorine type non-ionic surfactant. According to the test results of the melt strength, the cell diameter and the cell distribution density of the polypropylene carrier, the invention has the advantages that the polypropylene with high melt strength is used, the porous adsorbent can be uniformly distributed in the foamed polypropylene carrier in a large amount, the cell sizes are uniformly distributed, and the VOC removing effect is higher.
Claims (6)
1. The VOC extractant for the modified polypropylene is characterized by comprising the following components in percentage by weight:
11-50wt% of polypropylene carrier;
50-89wt% of non-fluorine type non-ionic surfactant solution, wherein the non-fluorine type non-ionic surfactant solution comprises 97.5-99.9 wt% of one or more of water or alcohols with the boiling point lower than 120 ℃ and 0.1-2.5wt% of non-fluorine type non-ionic surfactant, and the non-fluorine type non-ionic surfactant is selected from at least one of Triton type non-ionic surfactant and polyoxyethylene ether type non-ionic surfactant;
the polypropylene carrier comprises 60-90wt% of high melt strength polypropylene and 10-40wt% of porous adsorbent by weight percentage, wherein the porous adsorbent is selected from at least one of silicate and aluminosilicate; the high melt strength polypropylene is selected from polypropylene with melt strength more than or equal to 30 cN; the water vapor adsorption capacity of the porous adsorbent under 10% RH is more than or equal to 30mg/g, the water vapor adsorption capacity under 50% RH is more than or equal to 300mg/g, and the test standard refers to GB/T6287-; the melt strength of the polypropylene carrier is more than or equal to 30cN, the pore diameter of the cells is 20-60 microns, and the distribution density of the cells is more than or equal to 105/cm3(ii) a The melt strength test method comprises the following steps: measured using a rheometer at 230 ℃ with an acceleration of 30m/s2The melt strand was drawn off and the tensile hardness value and draw-off rate were recorded.
2. The VOC extractant of claim 1, wherein the silicate is at least one selected from diatomaceous earth, expanded perlite, expanded vermiculite, and attapulgite; the aluminosilicate is at least one selected from zeolite, 3A molecular sieve, 4A molecular sieve, 5A molecular sieve, 10X molecular sieve and 13X molecular sieve.
3. The VOC extractant as claimed in claim 1, wherein the alcohol having a boiling point lower than 120 ℃ is at least one selected from methanol, ethanol, propanol and butanol.
4. The VOC extractant of claim 1, wherein said nonionic surfactant of Triton class is selected from the group consisting of Triton X-100; the polyoxyethylene ether nonionic surfactant is at least one selected from laurylamine polyoxyethylene ether and stearylamine polyoxyethylene ether.
5. The method for preparing a VOC extractant for modified polypropylene as claimed in any one of claims 1 to 4, which comprises the steps of:
and (3) stirring the polypropylene carrier and the non-fluorine non-ionic surfactant solution for 3-5 minutes at the speed of 1000 revolutions per minute by a high-speed stirrer according to the proportion so that the non-fluorine non-ionic surfactant solution is fully adsorbed on the polypropylene carrier to obtain the VOC extracting agent for modified polypropylene.
6. The method for preparing VOC extractants for modified polypropylene as claimed in claim 5, wherein said method for preparing polypropylene carrier comprises the following steps:
a. fully and uniformly mixing the high-melt-strength polypropylene and the porous adsorbent in a high-speed stirrer, and performing melt blending extrusion granulation in an extruder to obtain a foamed polypropylene precursor;
b. foaming the foamed polypropylene precursor by adopting a physical foaming agent to prepare a polypropylene carrier;
the physical foaming agent is one or two of nitrogen or supercritical carbon dioxide.
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| CN109161172A (en) * | 2018-08-28 | 2019-01-08 | 安徽江淮汽车集团股份有限公司 | A kind of low VOC antibacterial PBT composite and preparation method thereof |
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| CN111500076B (en) * | 2020-05-14 | 2022-04-05 | 南京京锦元科技实业有限公司 | Low-odor thermoplastic elastomer material for automotive interior and preparation method thereof |
| CN112574440A (en) * | 2020-12-17 | 2021-03-30 | 武汉金发科技有限公司 | Adsorption type low-odor master batch for polypropylene and preparation method thereof |
| CN113980397A (en) * | 2021-10-12 | 2022-01-28 | 中广核三角洲（江苏）塑化有限公司 | Low-odor and low-VOC (volatile organic compound) TPV (thermoplastic vulcanizate) material for automobiles and preparation method thereof |
| CN116333465B (en) * | 2023-05-23 | 2023-08-08 | 北京助天科技集团有限公司 | Organic-inorganic composite material, preparation method and application thereof |
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