CN113651917A - Method for improving grafting rate of low-odor maleic anhydride grafted polyolefin for automobile - Google Patents
Method for improving grafting rate of low-odor maleic anhydride grafted polyolefin for automobile Download PDFInfo
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- CN113651917A CN113651917A CN202111213167.2A CN202111213167A CN113651917A CN 113651917 A CN113651917 A CN 113651917A CN 202111213167 A CN202111213167 A CN 202111213167A CN 113651917 A CN113651917 A CN 113651917A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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Abstract
A method for improving the grafting rate of maleic anhydride grafted polyolefin compatilizer master batch is characterized in that polyolefin is pretreated by vacuum heating, organic oil prepared from organic solvent and other additives is mixed with the pretreated polyolefin by vacuum suction, and the mixed material is prepared into the maleic anhydride grafted polyolefin compatilizer master batch.
Description
Technical Field
The invention belongs to the technical field of plastic processing. The low-odor maleic anhydride grafted polyolefin compatilizer master batch prepared by the method is suitable for production and processing of plastic materials for vehicles.
Background
The maleic anhydride grafted polyolefin is a common compatilizer for producing modified polyolefin products, and can be independently prepared into compatilizer master batches for producing downstream modified polyolefin plastic materials.
The conventional production method of maleic anhydride grafted polyolefin master batches is a melt grafting process. The reaction principle is that polyolefin resin, maleic anhydride, a free radical initiator, an antioxidant and the like are added into a double-screw extruder, and the resin is melted and plasticized and all auxiliary agents are dispersed through the rotating shearing action of a front-section double screw and the heating action of a heating device; and (3) completely melting and homogenizing the materials in the middle and rear half sections of the screw, grafting, and finally extruding and granulating to obtain the maleic anhydride grafted polyolefin master batch product.
The traditional production method of maleic anhydride grafted polyolefin master batch is to put all raw materials into a double-screw extruder simultaneously and directly, and the method has the problems of uneven dispersion of various auxiliaries in polyolefin, low production efficiency and low grafting rate. If the addition proportion of the additives is simply increased in order to increase the grafting ratio, the problems of pre-crosslinking and the like occur, which are represented by the generation of a large number of gel points and black points in the master batch and the increase of the residue of various additives, which causes the defects of increased product odor, poor appearance, reduced performance and the like.
The polyolefin material is widely applied to automobile interiors such as instrument boards, central channels, door panels and the like, and has higher requirements on odor control. The maleic anhydride grafted polyolefin compatilizer master batch prepared by the traditional process generally has the problem of residual smell.
Disclosure of Invention
The invention aims to provide a method for improving the grafting rate of maleic anhydride grafted polyolefin compatilizer master batch aiming at the defects in the prior art. The method comprises the steps of pretreating polyolefin by vacuum heating, mixing organic oil prepared from a solvent and other auxiliaries with the pretreated polyolefin in a vacuum suction mode, and preparing maleic anhydride grafted polyolefin compatilizer master batch from the mixed material through a double-screw extrusion device. The maleic anhydride grafted polyolefin compatilizer master batch prepared by the method not only improves the grafting rate of the product and reduces the odor residue of the product, but also improves the comprehensive performance of the product while not affecting the yield and the product appearance, and is suitable for producing and processing downstream polyolefin vehicle plastic materials or parts.
In some embodiments, the present invention provides a method for increasing the grafting rate of a maleic anhydride grafted polyolefin compatibilizer masterbatch comprising the steps of:
step 1: putting polyolefin into a rotating container provided with a baffle plate, heating, vacuumizing and rotating;
step 2: adding a free radical initiator, maleic anhydride and other auxiliaries into a proper organic solvent, and uniformly stirring to prepare mixed organic oil;
and step 3: stopping rotating, sucking the mixed organic oil liquid prepared in the step (2) into a rotating container by using the negative pressure formed by the vacuum in the step (1), and continuing rotating, heating and vacuumizing;
and 4, step 4: and (4) putting the material treated in the step (3) into a double-screw extruder production line for extrusion granulation to obtain the maleic anhydride grafted polyolefin master batch.
In some embodiments, the heating temperature of the rotating vessel in step 1 or step 3 is from 40 to 80 ℃. The temperature of step 1 and step 3 may be the same or different and is independently selected from 45, 50, 52, 52.8, 53, 54, 55, 56, 57, 58, 59, 60, 65, 75, 80 ℃.
In some embodiments, the vacuum of the rotary vessel in step 1 or step 3 is from-0.01 to-0.08 MPa. The vacuum degrees of the step 1 and the step 3 can be the same or different and are respectively and independently selected from-0.01, -0.02, -0.03, -0.04, -0.05, -0.06, -0.07 or-0.08 MPa.
In some embodiments, the rotating vessel of step 1 or step 3 is rotated at a speed of 10 to 200 revolutions per minute. The rotating speed of the rotating container in the step 1 and the step 3 can be the same or different and is respectively and independently selected from 10, 20, 30, 40, 50, 60, 70, 80, 90, 100, 150 and 200 revolutions per minute.
In some embodiments, the heating temperature of the rotary container in step 1 or step 3 is 50-70 ℃, the vacuum degree is-0.01 to-0.05 MPa, and the rotation speed is 20-50 r/min.
In some embodiments, the heating temperature of the rotary container in step 1 or step 3 is 52.8-60 ℃, the vacuum degree is-0.03 to-0.05 MPa, and the rotation speed is 20-40 r/min.
In some embodiments, the polyolefin is one or a combination of high density polyethylene, medium density polyethylene, low density polyethylene, linear low density polyethylene, metallocene polyethylene, ultra low density polyethylene, homo polypropylene, co polypropylene, ethylene vinyl acetate, ethylene butyl acrylate, ethylene methyl acrylate, ethylene ethyl acrylate, ethylene acrylic acid copolymer, polyolefin elastomer.
In some embodiments, the polyolefin is a polyolefin elastomer. Polyolefin elastomers (polyofin elastomers) (POE) are ethylene-alpha olefin copolymers synthesized by DOW chemical company in the united states using metallocenes as catalysts, thermoplastic elastomers having a narrow relative molecular mass distribution and a uniform short chain branch distribution. The polymer has the characteristics of extremely low crystallinity, very low density, narrow molecular weight distribution, low glass transition temperature and the like. The POE elastomer is selected from DuPont Dow series: POE8999, 8150, 8842, 8200, 7467, 7447, 7256, eckson company series: 5061. 5371, 5181, 5101, 5361, KN140, mitrer: DF610, DF710, DF740, DF810, DF840, or LG chemical series: LC170, LC670, LC175, LC 565.
In some embodiments, the suitable organic solvent in step 2 is selected from one or a combination of acetone, butanone and styrene.
In some embodiments, the suitable organic solvent is used in the amount of 3 to 10 parts by weight, relative to 100 parts by weight of the polyolefin in step 2. Specifically, it may be selected from 3, 4, 5, 6, 7, 8, 9, and 10 parts by weight.
In some embodiments, the maleic anhydride is used in an amount of 1 to 5 parts by weight, relative to 100 parts by weight of the polyolefin in step 1. Specifically, it may be selected from 1.0, 1.5, 2, 2.5, 3.0, 3.5, 4, 4.5, 5 parts by weight.
In some embodiments, the other auxiliary agents are selected from one or a combination of several of free radical initiators, lubricants, antioxidants.
In some embodiments, the free radical initiator is selected from one or a combination of DCP, BPO, BIPB, DTBH, DTBP.
In some embodiments, the free radical initiator is used in an amount of 0.01 to 0.5 parts by weight, relative to 100 parts by weight of the polyolefin. Specifically, it may be selected from 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.2, 0.3, 0.4, 0.5 parts by weight.
In some embodiments, the lubricant is selected from one or a combination of stearic acid, stearic acid amide, oleic acid amide, erucic acid amide, paraffin, silicone oil, white oil.
In some embodiments, the lubricant is used in an amount of 0.1 to 1 parts by weight, relative to 100 parts by weight of the polyolefin. Specifically, it may be selected from 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0 parts by weight.
In some embodiments, the antioxidant is one or a combination of 3114, 300, 1010, 1076, 1098, 168, 626, DLTP, DSTDP.
In some embodiments, the antioxidant is used in an amount of 0.01 to 1 part by weight, relative to 100 parts by weight of the polyolefin. Specifically, it may be selected from 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0 parts by weight.
On the other hand, the invention provides a maleic anhydride grafted polyolefin compatilizer master batch, and the master batch is prepared by the method.
In another aspect, the invention provides a use of the maleic anhydride grafted polyolefin compatibilizer masterbatch in the preparation of vehicle plastic materials or parts. The addition amount of the compatilizer master batch in the vehicle plastic material or the part is 2-5% of the total weight. Specifically, it may be selected from 2%, 3%, 4%, 5%.
Advantageous effects
(1) The preparation method provided by the invention improves the particle grafting rate of the maleic anhydride grafted polyolefin compatilizer mother material and reduces the odor grade.
(2) The preparation method provided by the invention can use less auxiliary agents on the basis of good grafting rate, and particularly reduces the dosage of solvent, maleic anhydride and free radical initiator.
(3) The preparation method provided by the invention reduces the occurrence of pre-crosslinking and reduces the number of black spots in the maleic anhydride grafted polyolefin compatilizer master batch.
Drawings
FIG. 1 is a schematic diagram of the conventional preparation of a maleic anhydride grafted polyolefin compatibilizer masterbatch.
FIG. 2 is a schematic diagram of the preparation of a maleic anhydride grafted polyolefin compatibilizer masterbatch 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 in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiment is a module embodiment of the present invention, not a whole embodiment. Elements and features described in one embodiment of the invention may be combined with elements and features shown in one or more other embodiments. It should be noted that the illustration omits illustration and description of components and processes not relevant to the present invention that are known to those of ordinary skill in the art for clarity purposes. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
TABLE 1 Components and abbreviations
Example 1
Weighing the following components in parts by weight: 100 kg of POE, 0.05 kg of DCP, 2 kg of MAH, 10100.1 kg of antioxidant and 0.5 kg of silicone oil.
According to the flow chart shown in the attached figure 1, the components are blended in a low-speed stirrer for 5 minutes, and are directly added into a double-screw extruder through a feeding device, and the temperatures of zones 1 to 12 of the extruder are set as follows: 100, 140, 190, 200, 190, 170, 160, 150 ℃ and 180 ℃ at the head temperature. The mixture is subjected to the steps of melting plasticization, kneading and mixing, extruding by a machine head, granulating, cooling, and granulating and packaging.
Example 2
Weighing the following components in parts by weight: POE 100 kg; the organic oil liquid is prepared from the following components in percentage by weight: butanone 5 kg, DCP 0.05 kg, MAH 2 kg, antioxidant 10100.1 kg, and silicone oil 0.5 kg.
Step 1: according to the flow chart shown in the attached FIG. 2, POE was charged into a rotary vessel equipped with baffles, and vacuum-dried at 50 ℃ under a vacuum degree of-0.05 for 15 minutes.
Step 2: adding DCP, MAH, antioxidant 1010 and silicone oil into butanone, and mixing to obtain organic oil.
And step 3: and (3) sucking the organic oil prepared in the step (2) into a rotary container by utilizing the vacuum negative pressure in the step (1), rotating for 30 minutes at the temperature of 50 ℃, the vacuum degree of-0.05 and the rotating speed of 30 revolutions per minute, and cooling to room temperature.
And 4, step 4: and (3) preparing the mixture obtained in the step (3) into master batches by using a double-screw extruder according to the same process parameters as those in the example 1, and completing the steps of granulation and packaging.
Example 3
Weighing the following components in parts by weight: POE 100 kg; the organic oil liquid is prepared from the following components in percentage by weight: 4 kg of butanone, 0.03 kg of DCP, 1.5 kg of MAH, 10100.1 kg of antioxidant and 0.5 kg of silicone oil.
Step 1: according to the flow chart shown in the attached FIG. 2, POE was charged into a rotary vessel equipped with baffles, and vacuum-dried at 60 ℃ under a vacuum degree of-0.05 for 15 minutes.
Step 2: adding DCP, MAH, antioxidant 1010 and silicone oil into butanone, and mixing to obtain organic oil.
And step 3: and (3) sucking the organic oil prepared in the step (2) into a rotary container by utilizing the vacuum negative pressure in the step (1), rotating for 60 minutes at the temperature of 60 ℃, the vacuum degree of-0.05 and the rotating speed of 50 revolutions per minute, and cooling to room temperature.
And 4, step 4: and (3) preparing the mixture obtained in the step (3) into master batches by using a double-screw extruder according to the same process parameters as those in the example 1, and completing the steps of granulation and packaging.
Example 4
The master batch products prepared in examples 1-3 were randomly sampled and tested for grafting, odor rating and black dot number.
The method for measuring the grafting ratio comprises the following steps:
and (3) measuring the sample by using an infrared spectrometer, and reading a characteristic peak in a spectrogram and automatically acquired spectrogram characteristic peak intensity data.
The grafting ratio is calculated according to the following formula:
G=a×A/A1
in the formula: g-grafting rate, MAH and other grafting monomer mass fractions;
a, obtaining experience coefficients, wherein different products correspond to different experience coefficients and are obtained by comparing and summarizing infrared spectrometry and chemical titration measurement methods in a large quantity;
a-peak intensity of infrared characteristic absorption peak of graft monomer, MAH1779-1795 cm-1；
A1-characteristic absorption peak intensity of matrix resin, and the PP matrix resin is 1165-1169 cm-1The PE and POE matrix resin is 715-sand 725 cm-1。
Method for measuring odor and grade evaluation standard
1) 10g of sample is weighed by an electronic balance and placed in a 1000ml wide-mouth bottle with a cover, and the bottle body is marked with a serial number.
2) The jar was placed in an oven at 80 ℃ for 2 h.
3) After storage for 2h, five testing personnel performed the tests in the evaluation room (one testing personnel smelled no more than eight samples at a time).
4) Odor test was performed in a test vessel cooled to (60 + -5) ° c at room temperature. When the container cools to about 60 c, the first tester opens the cap a little bit, smells it, recloses the cap and passes the container to the second tester. The second inspector passes the container to a third inspector after inspection, and thus to a fifth inspector. Finally, each inspector gives a score, and the recorder records the score.
5) During smelling of the samples, one sample must be 1 min apart from the next in order for the tester to neutralize the perception of smell. After smelling a sample with heavy or bad smell, the user should go out to breathe fresh air.
TABLE 2 rating evaluation criteria
Black point number measuring method
The standard light source box D65 light source is used as the illumination condition, the dirty point gauge is used as the inspection scale, the sample particles are flatly paved on white paper, whether different color points exist on each particle is observed, and the number of the actual different color points of the observed 100g sample is counted.
The results of the tests for substantivity, odor grade, black dot number for examples 1-3 are summarized in Table 3.
Table 3 test results for the products of examples 1-3
Example 1 the product was obtained without pre-dispersion by rotating the rotating vessel and directly fed into the twin-screw extruder line. The product produced in example 1 had a low grafting yield and a large residue, resulting in a high odor level, and was easy to produce black spots with a high number of black spots.
Example 2 the same formulation as example 1, the method pretreats the polyolefin by vacuum heating, and mixes the organic oil prepared from solvent and other auxiliary agents with the pretreated polyolefin by vacuum suction. The method of example 2 can improve the grafting rate of the compatilizer master batch, reduce the odor level and reduce the number of black spots.
Example 3 the process parameters were adjusted on the basis of example 2, and the high performance maleic anhydride grafted polyolefin product with higher grafting ratio, lower odor, and lower black spots was obtained while reducing the amount of each adjuvant, especially the amount of organic solvent, maleic anhydride, and radical initiator. The compatilizer masterbatch prepared in the embodiments 2-3 can meet the requirements of high performance and low odor of vehicle plastic materials.
Claims (19)
1. A method for improving the grafting rate of maleic anhydride grafted polyolefin compatilizer master batch is characterized by comprising the following steps:
step 1: putting polyolefin into a rotating container provided with a baffle plate, heating, vacuumizing and rotating;
step 2: adding a free radical initiator, maleic anhydride and other auxiliaries into a proper organic solvent, and uniformly stirring to prepare mixed organic oil;
and step 3: sucking the mixed organic oil liquid prepared in the step (2) into a rotary container by using the negative pressure formed by the vacuum in the step (1), and continuously rotating, heating and vacuumizing;
and 4, step 4: and (4) putting the material prepared in the step (3) into a double-screw extruder production line for extrusion granulation to obtain the maleic anhydride grafted polyolefin master batch.
2. The method of claim 1, wherein the heating temperature of the rotating vessel in step 1 or step 3 is 40-80 ℃.
3. The method of claim 2, wherein the rotary container in step 1 or step 3 has a vacuum of-0.01 to-0.08 MPa.
4. The method of claim 3, wherein the rotating vessel of step 1 or step 3 is rotated at a speed of 10 to 200 rpm.
5. The method according to claim 1, wherein the heating temperature of the rotary container in step 1 or step 3 is 50-70 ℃, the vacuum degree is-0.01 to-0.05 MPa, and the rotation speed is 20-50 r/min.
6. The method of claim 5, wherein the polyolefin is one or a combination of high density polyethylene, medium density polyethylene, low density polyethylene, linear low density polyethylene, metallocene polyethylene, ultra low density polyethylene, homo polypropylene, co-polypropylene, ethylene vinyl acetate, ethylene butyl acrylate, ethylene methyl acrylate, ethylene ethyl acrylate, ethylene acrylic acid copolymer, polyolefin elastomer.
7. The process according to any one of claims 1 to 6, wherein the suitable organic solvent in step 2 is selected from one or more of acetone, butanone and styrene.
8. The process of claim 7, wherein the suitable organic solvent is used in the amount of 3 to 10 parts by weight, relative to 100 parts by weight of the polyolefin in step 2.
9. The method of claim 8, wherein the maleic anhydride is used in an amount of 1 to 5 parts by weight with respect to 100 parts by weight of the polyolefin in step 1.
10. The method of claim 9, wherein the other auxiliary agents are selected from one or more of radical initiator, lubricant and antioxidant.
11. The method of claim 10, wherein the radical initiator is selected from one or more of DCP, BPO, BIPB, DTBH, DTBP.
12. The method of claim 10, wherein the radical initiator is used in an amount of 0.01 to 0.5 parts by weight, relative to 100 parts by weight of the polyolefin.
13. The method of claim 10, wherein the lubricant is selected from the group consisting of stearic acid, stearic acid amide, oleic acid amide, erucic acid amide, paraffin, silicone oil, and white oil.
14. The method of claim 13, wherein the lubricant is used in an amount of 0.1 to 1 part by weight relative to 100 parts by weight of the polyolefin.
15. The method of claim 10, wherein the antioxidant is one or a combination of 3114, 300, 1010, 1076, 1098, 168, 626, DLTP, DSTDP.
16. The method of claim 15, wherein the antioxidant is used in an amount of 0.01 to 1 part by weight, relative to 100 parts by weight of the polyolefin.
17. A maleic anhydride grafted polyolefin compatibilizer masterbatch characterized by being prepared using the method of any one of claims 1-16.
18. Use of a masterbatch of maleic anhydride grafted polyolefin compatibiliser prepared by the process of any of claims 1-16 for the preparation of a vehicle plastics material or component.
19. The use of claim 18, wherein the maleic anhydride grafted polyolefin compatibilizer masterbatch is added in an amount of 2 to 5% by weight of the total weight in the vehicle plastic material or component.
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