CN107987375B - Polypropylene composite material and preparation method thereof - Google Patents
Polypropylene composite material and preparation method thereof Download PDFInfo
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- CN107987375B CN107987375B CN201711075842.3A CN201711075842A CN107987375B CN 107987375 B CN107987375 B CN 107987375B CN 201711075842 A CN201711075842 A CN 201711075842A CN 107987375 B CN107987375 B CN 107987375B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K11/00—Use of ingredients of unknown constitution, e.g. undefined reaction products
- C08K11/005—Waste materials, e.g. treated or untreated sewage sludge
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Treatment Of Sludge (AREA)
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Abstract
The invention discloses a polypropylene composite material and a preparation method thereof, wherein the polypropylene composite material comprises the following components: 70-90 parts of polypropylene resin and 5-30 parts of boron mud carbonization residue. According to the invention, the boron mud carbonization residue is applied to the polypropylene composite material, the compatibility between the boron mud carbonization residue and polypropylene can be obviously improved through the optimization of each component in the formula and the optimization of the process, the prepared composite polypropylene material has better tensile strength, bending strength and impact property, can replace inorganic reinforcing fillers such as talcum powder and calcium carbonate, can reduce the production cost of polypropylene products, has the characteristics of energy conservation and environmental protection, and greatly improves the comprehensive utilization value of the boron mud.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of solid wastes, and particularly relates to a polypropylene composite material and a preparation method thereof.
Background
The boron mud is alkaline solid waste generated in the borax production process by taking ascharite as a raw material, 4 tons of boron mud waste is generated along with the production of 1 ton of borax, the emission of the boron mud is large, a large amount of accumulated boron mud occupies land, and soda is added in the borax production process, so that the boron mud is strong in alkalinity and pollutes rivers.
At present, the treatment means of boron mud in China mainly utilizes boron mud waste to produce basic magnesium carbonate, boron-magnesium-phosphorus compound fertilizer, building bricks and the like. The process for preparing basic magnesium carbonate by using boron mud as a raw material through a carbonization method is the most mature, and the boron mud is used in the largest amount, but a large amount of calcium oxide is added in the process of producing the basic magnesium carbonate by using the method, so that almost equal amount of secondary solid waste (namely boron mud carbonization residue) can be generated. The main components of the material are 26.98 percent of magnesium oxide, 18.35 percent of calcium oxide, 4.09 percent of aluminum oxide, 2.53 percent of ferric oxide, 0.31 percent of potassium oxide, 0.14 percent of titanium oxide, 0.12 percent of manganese oxide and the like. The method is not favorable for comprehensive utilization of the boric sludge, and also does not accord with the national treatment principle of reduction, reutilization and resource utilization of waste resources. Therefore, the solid waste (namely the boron sludge carbonization residue) generated by the boron sludge for producing basic magnesium carbonate by the carbonization method must be further developed and utilized.
Through the analysis of the boron mud carbonization residue, the main chemical composition is as follows: magnesium oxide, silicon oxide, aluminum oxide, calcium oxide, iron oxide, sodium oxide, potassium oxide, and the like. The phase composition mainly comprises forsterite, calcite, quartz, pyrite, albite, potash feldspar and the like. At present, researches on the use of boron mud treated as polypropylene reinforcing filler have been reported, such as CN1044479, but the patent discloses a simple treatment mode of boron mud, and does not fully utilize effective components in boron mud.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the polypropylene composite material, and the composite material adopts boric sludge carbonization residues as raw materials to replace fillers such as talcum powder, calcium carbonate and the like, so that the comprehensive utilization value of the boric sludge is greatly improved.
The invention also aims to provide a preparation method of the polypropylene composite material.
The invention is realized by the following technical scheme:
the polypropylene composite material comprises the following components in parts by weight:
70-90 parts of polypropylene resin
5-30 parts of boron mud carbonization residues.
The boron mud carbonization residue provided by the invention is solid waste generated in the process of producing basic magnesium carbonate by using boron mud as a raw material and adopting a carbonization method. The X-ray diffractometer D8-FOCUS model of German Bruker company is adopted, and the test conditions are as follows: the scanning range is 5-70 degrees, the scanning speed is 2 degrees/min, the Cu and Ka radiation has the wavelength of 1.54A, and the main components are analyzed as follows: 25-27% of magnesium oxide, 17-20% of calcium oxide, 3-5% of aluminum oxide, 2-3% of ferric oxide, 0-0.5% of potassium oxide, 0-0.2% of titanium oxide, 0-0.2% of manganese oxide and the like, and the average grain diameter is less than 3 mu m by testing with a laser particle size analyzer.
Preferably, the boron mud carbonization residue is boron mud carbonization residue pretreated by a coupling agent, the addition amount of the coupling agent is 0-2 parts based on 100 parts of the boron mud carbonization residue, the coupling agent is one or a mixture of silane coupling agent, aluminate or stearic acid, and Si69 or KH560 is preferable. The boron mud carbonization residue adopted by the invention belongs to secondary waste residue, is alkaline, and has a pH value of 9.5-10, and the surface pretreatment of the boron mud carbonization residue is carried out by reasonably selecting a coupling agent according to the alkaline physical characteristics of the boron mud carbonization residue, so that the compatibility of the boron mud carbonization residue with a polypropylene matrix can be improved, the filling amount is increased, and the mechanical property of the composite material is improved.
According to actual performance requirements, the polypropylene composite material also comprises 0-2 parts of other additives by weight, wherein the other additives are one or a mixture of several of an antioxidant, a lubricant or a light stabilizer.
Wherein the antioxidant is 2, 6-di-tert-butyl-4-methylphenol (antioxidant 264), 3- (3 ', 5' -di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010) and the like.
The lubricant is polyethylene wax, N' -ethyl bis stearamide EBS and the like;
the light stabilizer is 4-benzoyloxy-2, 2, 6, 6-tetramethylpiperidine (light stabilizer 744), 2' -thiobis (4-tert-octylphenoloxy) nickel (light stabilizer AM-101) and the like.
The invention also provides a preparation method of the polypropylene composite material, which comprises the following steps:
(1) according to the mass ratio of the raw materials, placing the boron mud carbonization residue in a high-speed ball-milling mixer for pretreatment to obtain pretreated boron mud carbonization residue for later use;
(2) and (3) mixing the polypropylene resin, the pretreated boron mud carbonization residue and other auxiliaries in a high-speed mixer to obtain a premix, performing melt extrusion on the premix by a screw extruder, and granulating to obtain the polypropylene composite material.
Preferably, in step (1), the pretreatment conditions are as follows: the rotating speed is 800 r/min-1000 r/min, the time is 10-30 min, and the temperature is 80-100 ℃.
Preferably, in the step (2), the extrusion conditions of the extruder are as follows: the temperature of a first area is controlled to be 140-160 ℃, the temperature of a first area is controlled to be 150-170 ℃, the temperature of a third area is controlled to be 180-190 ℃, the temperature of a fourth area is controlled to be 180-190 ℃, the temperature of a fifth area is controlled to be 180-190 ℃, and the temperature of a machine head is controlled to be 190-210 ℃; the rotation speed is 200 and 500 r/min.
As a preferable technical scheme of the invention, before the step (1), the boron mud carbonization residue is calcined at high temperature, and the method comprises the following specific steps: putting the boron mud carbonization residue into a high-temperature-resistant open mold, calcining in a high-temperature box-type resistance furnace with set temperature and time, cooling to room temperature along with the furnace, and taking out to obtain the boron mud carbonization residue after high-temperature calcination, wherein the high-temperature calcination conditions are as follows: heating at a speed of 5 ℃/min before 600 ℃ in the high-temperature box type resistance furnace, heating at a speed of 3 ℃/min after 600 ℃, then preserving heat at 800 ℃ for 4h, and then naturally cooling. According to the invention, the boron mud carbonization residue is calcined at high temperature in advance, so that the types and the number of surface active points of the boron mud carbonization residue are increased, the particle size is increased, the specific surface area is reduced, the surface energy is reduced, the dispersity of the boron mud carbonization residue is improved, and the structure becomes loose due to high-temperature calcination and amorphization, so that the dispersity is further improved.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention applies the boron mud carbonization residue to the polypropylene composite material, and optimizes the components in the formula and
the compatibility between the boron mud carbonization residue and the polypropylene can be obviously improved by optimizing the process, the prepared composite polypropylene material has better tensile strength, bending strength and impact property, can replace inorganic reinforcing fillers such as talcum powder, calcium carbonate and the like, can greatly reduce the use of the reinforcing fillers such as high-energy-consumption and high-pollution talcum powder, calcium carbonate and the like, not only can reduce the production cost of polypropylene products, but also has the characteristics of energy conservation and environmental protection, and greatly improves the comprehensive utilization value of the boron mud.
(2) The production method is simple, can effectively treat a large amount of waste materials generated in the process of producing basic magnesium carbonate from boron sludge, and accords with the national treatment principle of reduction, reutilization and resource utilization of waste resources.
Detailed Description
The following examples are given to specifically describe the present invention, but are not limited thereto.
B, boron mud carbonization residue: the method comprises the steps of using boron mud as a main raw material, adding calcium oxide to carry out digestion reaction, cooling a mixed solution, placing the cooled mixed solution in a high-pressure reaction kettle, pressurizing and introducing carbon dioxide to carry out carbonization reaction, stopping introducing the carbon dioxide when the pH of the mixed solution reaches 7, drying and grinding solid waste filtered by the mixed solution to obtain boron mud carbonization residues, and testing the average particle size of the boron mud carbonization residues to be 2.54 mu m by using a laser particle size analyzer.
Other raw materials used in the examples and comparative examples of the present invention were all commercially available.
Examples 1 and 6-7, comparative examples 1-2:
(1) placing the boron mud carbonization residues in a high-speed ball milling mixer according to the table 1, and pretreating to obtain pretreated boron mud carbonization residues for later use; the pretreatment conditions are as follows: the rotating speed is 800 r/min-1000 r/min, the time is 10-30 min, and the temperature is 80-100 ℃;
(2) mixing polypropylene resin, pretreated boron mud carbonization residues and other auxiliaries in a high-speed mixer to obtain a premix, performing melt extrusion on the premix by a screw extruder, and granulating to obtain a polypropylene composite material; the extrusion conditions were: the temperature of a first area is controlled to be 140-160 ℃, the temperature of a first area is controlled to be 150-170 ℃, the temperature of a third area is controlled to be 180-190 ℃, the temperature of a fourth area is controlled to be 180-190 ℃, the temperature of a fifth area is controlled to be 180-190 ℃, and the temperature of a machine head is controlled to be 190-210 ℃; the rotating speed is 200 r/min.
Examples 2 to 5:
as shown in Table 1, the boron sludge carbonization residue and the coupling agent were put in a high-speed ball mill mixer for pretreatment to obtain a pretreatment
The treated boron mud carbonization residue is reserved; the pretreatment conditions are as follows: the rotating speed is 800 r/min-1000 r/min, the time is 10-30 min, and the temperature is 80-100 ℃;
the rest is the same as example 1.
Example 8:
before the pretreatment in the step (1), carrying out high-temperature calcination on the boron mud carbonization residue, and specifically comprising the following steps: putting the boron mud carbonization residue into a high-temperature-resistant open mold, calcining in a high-temperature box-type resistance furnace with the set temperature and time, cooling to room temperature along with the furnace, and taking out to obtain the boron mud carbonization residue after high-temperature calcination, wherein the high-temperature calcination conditions are as follows: heating at a speed of 5 ℃/min before 600 ℃ in the high-temperature box type resistance furnace, heating at a speed of 3 ℃/min after 600 ℃, then preserving heat at 800 ℃ for 4h, and then naturally cooling;
the rest of the procedure was the same as in example 1.
Drying the obtained polypropylene composite material under the following conditions: the temperature is 105 ℃, and the time is 2 hours; then, the corresponding sample strips are molded according to the standard, and the injection molding conditions are as follows: the temperature of the front section is 160-; the performance test was carried out as follows, and the test results are shown in Table 2.
The performance test method comprises the following steps:
tensile strength: testing according to GB/T1040-2006, wherein the stretching speed is 10 mm/min;
bending strength: testing according to GB/T9341-2000, wherein the bending speed is 2 mm/min;
flexural modulus: testing according to GB/T9341-2000, wherein the bending speed is 2 mm/min;
cantilever beam impact strength: testing according to GB/T1843-2008, type A notch;
elongation at break: testing according to GB/T1040-2006, wherein the stretching speed is 10 mm/min;
average particle size: a laser particle size analyzer is adopted, water is used as a medium, a certain amount of boron mud carbonization residue sample is added into a sample pool, sample particles are dispersed in the water through physical mechanical stirring, ultrasonic waves are started to disperse agglomerated particles, a circulating pump is started to uniformly distribute the particles in the system, the shading ratio is controlled to be 1-2 in the whole process, and the test is carried out.
TABLE 1 concrete compounding ratio (parts by weight) of each component in each example and comparative example
TABLE 2 Performance test data for each of the examples and comparative examples
As can be seen from the comparison between example 1 and comparative examples 1-2 in Table 2, the polypropylene composite material prepared from the boron sludge carbonization residue as a raw material has better performance than the comparative example using talc powder and calcium carbonate as raw materials, so that the boron sludge carbonization residue can be completely used for preparing the polypropylene composite material instead of the talc powder and the calcium carbonate.
Claims (10)
1. The polypropylene composite material is characterized by comprising the following components in parts by weight:
70-90 parts of polypropylene resin
5-30 parts of boron mud carbonization residue
The boron mud carbonization residue is solid waste generated in the process of producing basic magnesium carbonate by using boron mud as a raw material through a carbonization method, and the average particle size of the boron mud carbonization residue is less than 3 mu m by using a laser particle size analyzer.
2. The polypropylene composite according to claim 1, wherein the boron sludge carbonization residue is a boron sludge carbonization residue pretreated with a coupling agent.
3. The polypropylene composite material according to claim 2, wherein the coupling agent is added in an amount of 0-2 parts based on 100 parts of the boron mud carbonization residue, and the coupling agent is one or a mixture of silane coupling agent, aluminate or stearic acid.
4. The polypropylene composite according to claim 3, wherein the coupling agent is Si69 or KH 560.
5. The polypropylene composite material as claimed in claim 1, further comprising 0-2 parts by weight of other additives.
6. The polypropylene composite material according to claim 5, wherein the other auxiliary agent is one or a mixture of several of an antioxidant, a lubricant, or a light stabilizer.
7. Process for the preparation of a polypropylene composite according to any one of claims 1 to 6, characterized in that it comprises the following steps:
(1) according to the mass ratio of the raw materials, placing the boron mud carbonization residue in a high-speed ball-milling mixer for pretreatment to obtain pretreated boron mud carbonization residue for later use;
(2) and (3) mixing the polypropylene resin, the pretreated boron mud carbonization residue and other auxiliaries in a high-speed mixer to obtain a premix, performing melt extrusion on the premix by a screw extruder, and granulating to obtain the polypropylene composite material.
8. The method for preparing a polypropylene composite material according to claim 7, wherein the pretreatment conditions in step (1) are as follows: the rotating speed is 800 r/min-1000 r/min, the time is 10-30 min, and the temperature is 80-100 ℃.
9. The method for preparing a polypropylene composite material according to claim 7, wherein in the step (2), the extrusion conditions of the extruder are as follows: the temperature of a first area is controlled to be 140-160 ℃, the temperature of a first area is controlled to be 150-170 ℃, the temperature of a third area is controlled to be 180-190 ℃, the temperature of a fourth area is controlled to be 180-190 ℃, the temperature of a fifth area is controlled to be 180-190 ℃, and the temperature of a machine head is controlled to be 190-210 ℃; the rotation speed is 200 and 500 r/min.
10. The preparation method of the polypropylene composite material according to claim 7, wherein before the step (1), the boron mud carbonization residue is calcined at high temperature, and the method comprises the following specific steps: putting the boron mud carbonization residue into a high-temperature-resistant open mold, calcining in a high-temperature box-type resistance furnace with set temperature and time, cooling to room temperature along with the furnace, and taking out to obtain the boron mud carbonization residue after high-temperature calcination, wherein the high-temperature calcination conditions are as follows: heating at a speed of 5 ℃/min before 600 ℃ in the high-temperature box type resistance furnace, heating at a speed of 3 ℃/min after 600 ℃, then preserving heat at 800 ℃ for 4h, and then naturally cooling.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109111599A (en) * | 2018-07-07 | 2019-01-01 | 大连地拓环境科技有限公司 | A kind of PVC fillers activated boron preparation method |
| CN109279833A (en) * | 2018-08-28 | 2019-01-29 | 武汉金发科技有限公司 | A kind of boron mud carbonized residue/foamed polystyrene insulation board and a kind of preparation method of foaming insulation board |
| CN109370044A (en) * | 2018-09-11 | 2019-02-22 | 上海宝田新型建材有限公司 | A kind of slag micropowder modified polypropylene composite material and preparation method thereof |
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|---|---|---|---|---|
| EP0051230A1 (en) * | 1980-10-31 | 1982-05-12 | Deutsche ITT Industries GmbH | Suspensions containing microfibrillated cullulose, and process for their preparation |
| CN101962458A (en) * | 2010-10-11 | 2011-02-02 | 北京立高科技股份有限公司 | PVC waterproof coiled material and preparation process thereof |
| CN103979584A (en) * | 2014-06-03 | 2014-08-13 | 李广凡 | Process for preparing light magnesium carbonate from boron mud |
| CN105566773A (en) * | 2014-10-13 | 2016-05-11 | 夏安娜 | Environment-friendly flame retardant rubber and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044479A (en) * | 1989-11-11 | 1990-08-08 | 姜国刚 | Application in boron mud powder production technique and the rubber item |
| CN103923379B (en) * | 2013-01-14 | 2016-08-10 | 中国地质大学（北京） | A kind of utilize boric sludge for the method for flame-retardant high-molecular composite |
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- 2017-11-06 CN CN201711075842.3A patent/CN107987375B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0051230A1 (en) * | 1980-10-31 | 1982-05-12 | Deutsche ITT Industries GmbH | Suspensions containing microfibrillated cullulose, and process for their preparation |
| CN101962458A (en) * | 2010-10-11 | 2011-02-02 | 北京立高科技股份有限公司 | PVC waterproof coiled material and preparation process thereof |
| CN103979584A (en) * | 2014-06-03 | 2014-08-13 | 李广凡 | Process for preparing light magnesium carbonate from boron mud |
| CN105566773A (en) * | 2014-10-13 | 2016-05-11 | 夏安娜 | Environment-friendly flame retardant rubber and preparation method thereof |
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