CN103665723A - Method for preparing high-toughness high-strength polypropylene material through in-situ compatibilization - Google Patents
Method for preparing high-toughness high-strength polypropylene material through in-situ compatibilization Download PDFInfo
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- CN103665723A CN103665723A CN201310667825.4A CN201310667825A CN103665723A CN 103665723 A CN103665723 A CN 103665723A CN 201310667825 A CN201310667825 A CN 201310667825A CN 103665723 A CN103665723 A CN 103665723A
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- ductility
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- polypropylene material
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- situ compatibilization
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92514—Pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92914—Degassing unit
Abstract
The invention relates to a method for preparing high-toughness high-strength polypropylene material through in-situ compatibilization. The method comprises the steps of uniformly mixing polypropylene, ethylene-octylene copolymer, grafted polar monomers and initiators in a mixer, then uniformly mixing superfine inorganic mineral powder, surface treating agents, dispersion lubricating agents and antioxidants in a mixer, adding the mixtures into an extruder separately, reacting and mixing at 170-230 DEG C, extrusion granulating, and carrying out post-devolatilization on the materials in a drum tackifying machine, wherein a vacuum pump is started to carry out primary devolatilization during the extrusion process. According to the method, modified fillers and auxiliaries are added in the polypropylene grafting reaction extruding process, the method belongs to the in-situ compatibilization process for improving the toughness and the strength, the traditional process in which the polypropylene grafted polymer is firstly prepared and then secondary modification is carried out is simplified, the cost is saved and the dispersion uniformity of the fillers and the compatibility with base resin are ensured.
Description
Technical field
The present invention relates to polypropylene modified material preparation technology, particularly the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility.
Background technology
Along with the development of synthesis technology, polypropylene (PP) resin is applied to every field more and more widely with its excellent performance, and demand increases sharply, and market outlook are good.With respect to other engineering plastics, due to strength of PP and low-temperature flexibility poor, in some field, can not directly apply, be generally for specific requirement, carry out corresponding modification, as enhancing modified, toughening modifying, flame-retardant modified etc.But itself belongs to non-polar resin polypropylene, poor with the interface binding power of modified filler, need to add the consistency that compatilizer could improve itself and filler, avoid occurring that fillers dispersed is inhomogeneous, the phenomenons such as layering.Therefore polyacrylic polar is the content of polymer circle research always.At present, the way of material modification circle is in modifying process, adds grafts, polypropylene grafted maleic anhydride for example, and polypropylene grafted vinylformic acid etc. improve the bonding force of polypropylene and filler as compatilizer.But this method is limited to the preparation of odorlessness grafts on the one hand, increased on the other hand later stage modified process, cost is higher, and because the vector resin that grafts is used is different from the base resin trade mark in modifying process, affects design of material and material property.
Summary of the invention
Problem and defect in view of above-mentioned prior art existence, the preparation method who the object of this invention is to provide the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility, present method is carried out polar process (graft reaction) and physically modified in same forcing machine, simplify modified process, in extrusion and after cooling granulation, carry out devolatilization processing, farthest reduce the smell of material simultaneously.
The technical scheme that the present invention takes is: the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility, it is characterized in that, and the method comprises the following steps:
Step 1: by polypropylene, ethylene-octene copolymer,, grafting of polar monomers and initiator mix in mixing machine, each composition weight umber is:
Polypropylene 100
Ethylene-octene copolymer 5-10
Grafting of polar monomers 1-5
Initiator 0.2-1.0.
Step 2: ultra-fine inorganic breeze, surface treatment agent, dispersed lubricant and oxidation inhibitor are mixed in mixing machine, and each composition weight umber is:
Inorganic mineral powder 10-30
Dispersed lubricant 0.1-0.5
Oxidation inhibitor 0.1-0.4
Surface treatment agent 0.1-0.5.
Step 3: by the mixture through step 1 gained from forcing machine front end spout, mixture through step 2 gained joins respectively forcing machine from extruding pusher side spout, and after extrusion temperature is that under 170-230 ℃ of processing condition, reaction mixes, extruding pelletization, obtains the high-strength polypropylene material of In Situ Compatibilization high-ductility.
Of the present invention in extrusion, open vacuum pump, make the reach-0.08Mpa of vacuum tightness in forcing machine, material is carried out to preliminary devolatilization with this understanding; , after extruding pelletization, at pressure, be simultaneously 130Pa, devolatilization temperature is, under the processing condition of 80 ℃, material to be carried out in rotary drum tackify machine to later stage devolatilization processing.
Advantage of the present invention is: the present invention is in polypropylene grafted reaction extrusion, add modified filler and auxiliary agent, belong to the high-strength technique of In Situ Compatibilization high-ductility, simplify traditional modified technique and first prepared Graft Polypropylene, then carry out the method for twice-modified processing, provide cost savings, and guaranteed the dispersed of filler and with the consistency of base resin.
This adopts and vacuumizes de-brightness technique clearly in the polypropylene grafted reaction process later stage, after having made grain, adopts the technique of follow-up de-brightness, has both guaranteed the sufficient percentage of grafting of material, has solved again the problem that produces intense stimulus smell in production and application process.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Forcing machine of the present invention adopts big L/D ratio forcing machine, and its length-to-diameter ratio is not less than 40(as CTE-64 forcing machine, length-to-diameter ratio 44), two aspirating holes are increased in machine barrel rear end, and each aspirating hole is connected with vacuum pump.In extrusion, open vacuum pump, make the reach-0.08Mpa of vacuum tightness in forcing machine, material is carried out to preliminary devolatilization with this understanding, unnecessary initiator and grafting of polar monomers are discharged; , after extruding pelletization, at pressure, be simultaneously 130Pa, devolatilization temperature is, under the processing condition of 80 ℃, material to be carried out in rotary drum tackify machine to later stage devolatilization processing, further discharges unnecessary small molecule monomer, guarantees the low smell of material.
The present invention's grafting of polar monomers used is one or more mixing in norbornene dicarboxylic anhydride, maleic anhydride, glycidyl methacrylate, butyl methacrylate, hydroxyethyl methylacrylate, methyl methacrylate.
The present invention's initiator used is peroxide type initiator, select 2,5-dimethyl-2, two (t-butyl peroxy) hexanes, two 2 4-[two (2 of 5-, 4-dichloro-benzoyl) superoxide, peroxidation two (4-toluyl), dicumyl peroxide, two (tert-butyl hydroperoxide sec.-propyl) benzene, 1,1-di-t-butyl methyl-3, one or more mixing in 5,5-trimethyl-cyclohexane.
The present invention's inorganic mineral powder used is one or more mixing in nano-calcium carbonate, nanomete talc powder, nano-sized magnesium hydroxide, nanometer hydroxide, nano imvite, nano-silicon lime stone, nano kaoline.
The present invention's surface treatment agent used is one or more mixing in 3-triethoxysilyl-1-propylamine, γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, stearic acid, titanic acid ester, Aluminate, zirconate.
The present invention's dispersed lubricant used is one or more mixing in ethylene bis stearamide, PE wax, montanic acid, calcium stearate, stearic acid.
The present invention's oxidation inhibitor used is the composite antioxidant that phosphite ester kind antioxidant and Hinered phenols antioxidant form, and the weight ratio of phosphite ester kind antioxidant and Hinered phenols antioxidant is 1:0.3～1:0.7.
Embodiment mono-: the method comprises the following steps:
Step 1: polypropylene, ethylene-octene copolymer, maleic anhydride and tasteless dicumyl peroxide are mixed in mixing machine, and each composition weight umber is:
Polypropylene 100
Ethylene-octene copolymer 5
Maleic anhydride 1
Tasteless dicumyl peroxide 0.2.
Step 2: nanomete talc powder, ethylene bis stearamide, composite antioxidant and γ-aminopropyl triethoxysilane are mixed in mixing machine, and each composition weight umber is:
Nanomete talc powder (1200 order) 10
Ethylene bis stearamide 0.2
Composite antioxidant 0.2
γ-aminopropyl triethoxysilane 0.1.
Wherein composite antioxidant is comprised of phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010, and its weight ratio is 1:0.3.
Step 3: by the mixture through step 1 gained from forcing machine front end spout, mixture through step 2 gained joins respectively forcing machine from extruding pusher side spout, and be that under 200 ℃ of processing condition, reaction mixes at extrusion temperature, open vacuum pump simultaneously, make the reach-0.08Mpa of vacuum tightness in forcing machine, material is carried out to preliminary devolatilization with this understanding.After extruding pelletization, at pressure, be 130Pa, devolatilization temperature is under the processing condition of 80 ℃, material is carried out in rotary drum tackify machine to later stage devolatilization and processes 2 hours, obtains the high-strength polypropylene material of In Situ Compatibilization high-ductility.
Embodiment bis-:
Step 1: polypropylene, ethylene-octene copolymer, maleic anhydride, tasteless dicumyl peroxide are mixed in mixing machine, and each composition weight umber is:
Polypropylene 100
Ethylene-octene copolymer 7
Maleic anhydride 3
Tasteless dicumyl peroxide 0.5.
Step 2: nanomete talc powder, ethylene bis stearamide, composite antioxidant and titanic acid ester are mixed in mixing machine, and each composition weight umber is:
Nanomete talc powder (1200 order) 15
Ethylene bis stearamide 0.35
Composite antioxidant 0.3
Titanic acid ester 0.2.
Wherein composite antioxidant is comprised of phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010, and its weight ratio is 1:0.5.
Step 3: by the mixture through step 1 gained from forcing machine front end spout, mixture through step 2 gained joins respectively forcing machine from extruding pusher side spout, and be that under 220 ℃ of processing condition, reaction mixes at extrusion temperature, open vacuum pump simultaneously, make the reach-0.08Mpa of vacuum tightness in forcing machine, material is carried out to preliminary devolatilization with this understanding.After extruding pelletization, at pressure, be 130Pa, devolatilization temperature is under the processing condition of 80 ℃, material is carried out in rotary drum tackify machine to later stage devolatilization and processes 3 hours, obtains the high-strength polypropylene material of In Situ Compatibilization high-ductility.
Embodiment tri-:
Step 1: polypropylene, ethylene-octene copolymer, maleic anhydride, tasteless dicumyl peroxide are mixed in mixing machine, and each composition weight umber is:
Polypropylene 100
Ethylene-octene copolymer 9
Maleic anhydride 5
Tasteless dicumyl peroxide 0.8.
Step 2: nanomete talc powder, ethylene bis stearamide, composite antioxidant and titanic acid ester are mixed in mixing machine, and each composition weight umber is:
Nanomete talc powder (1200 order) 25
Ethylene bis stearamide 0.4
Composite antioxidant 0.3
Titanic acid ester 0.4.
Wherein composite antioxidant is comprised of phosphite ester kind antioxidant 168 and Hinered phenols antioxidant 1010, and its weight ratio is 1:0.5.
Step 3: by the mixture through step 1 gained from forcing machine front end spout, mixture through step 2 gained joins respectively forcing machine from extruding pusher side spout, and be that under 230 ℃ of processing condition, reaction mixes at extrusion temperature, open vacuum pump simultaneously, make the reach-0.08Mpa of vacuum tightness in forcing machine, material is carried out to preliminary devolatilization with this understanding.After extruding pelletization, at pressure, be 130Pa, devolatilization temperature is under the processing condition of 80 ℃, material is carried out in rotary drum tackify machine to later stage devolatilization and processes 4 hours, obtains the high-strength polypropylene material of In Situ Compatibilization high-ductility.
After testing, the performance index of above three embodiment are as shown in table 1.
Table 1
As can be seen from the above table, the high-strength polypropylene material of In Situ Compatibilization high-ductility that adopts present method to prepare has higher modulus and hardness, and thermotolerance, compares with conventional plastic modification preferably, and operation is simple.The high-strength polypropylene material of In Situ Compatibilization high-ductility prepared by present method has good over-all properties, can meet the requirement in the fields such as automobile, household electrical appliances.
Claims (8)
1. a preparation method for the high-strength polypropylene material of In Situ Compatibilization high-ductility, is characterized in that, the method comprises the following steps:
Step 1: polypropylene, ethylene-octene copolymer, grafting of polar monomers and initiator are mixed in mixing machine, and each composition weight umber is:
Polypropylene 100
Ethylene-octene copolymer 5-10
Grafting of polar monomers 1-5
Initiator 0.2-1.0;
Step 2: ultra-fine inorganic breeze, surface treatment agent, dispersed lubricant and oxidation inhibitor are mixed in mixing machine, and each composition weight umber is:
Inorganic mineral powder 10-30
Dispersed lubricant 0.1-0.5
Oxidation inhibitor 0.1-0.4
Surface treatment agent 0.1-0.5;
Step 3: by the mixture through step 1 gained from forcing machine front end spout, mixture through step 2 gained joins respectively forcing machine from extruding pusher side spout, and after extrusion temperature is that under 170-230 ℃ of processing condition, reaction mixes, extruding pelletization, obtains the high-strength polypropylene material of In Situ Compatibilization high-ductility.
2. the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility as claimed in claim 1, is characterized in that, in extrusion, opens vacuum pump, makes the reach-0.08Mpa of vacuum tightness in forcing machine, and material is carried out to preliminary devolatilization with this understanding; , after extruding pelletization, at pressure, be simultaneously 130Pa, devolatilization temperature is, under the processing condition of 80 ℃, material to be carried out in rotary drum tackify machine to later stage devolatilization processing.
3.
described grafting of polar monomers is one or more mixing in norbornene dicarboxylic anhydride, maleic anhydride, glycidyl methacrylate, butyl methacrylate, hydroxyethyl methylacrylate, methyl methacrylate.
4. the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility as claimed in claim 1, it is characterized in that, described initiator is peroxide type initiator, select 2,5-dimethyl-2, two (t-butyl peroxy) hexanes, two 2 4-[two (2 of 5-, 4-dichloro-benzoyl) superoxide, peroxidation two (4-toluyl), dicumyl peroxide, two (tert-butyl hydroperoxide sec.-propyl) benzene, 1,1-di-t-butyl methyl-3, one or more mixing in 5,5-trimethyl-cyclohexane.
5. the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility as claimed in claim 1, it is characterized in that, described inorganic mineral powder is one or more mixing in nano-calcium carbonate, nanomete talc powder, nano-sized magnesium hydroxide, nanometer hydroxide, nano imvite, nano-silicon lime stone, nano kaoline.
6. the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility as claimed in claim 1, it is characterized in that, described surface treatment agent is one or more mixing in 3-triethoxysilyl-1-propylamine, γ-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, stearic acid, titanic acid ester, Aluminate, zirconate.
7. the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility as claimed in claim 1, is characterized in that, described dispersed lubricant is one or more mixing in ethylene bis stearamide, PE wax, montanic acid, calcium stearate, stearic acid.
8. the preparation method of the high-strength polypropylene material of a kind of In Situ Compatibilization high-ductility as claimed in claim 1, it is characterized in that, described oxidation inhibitor is the composite antioxidant that phosphite ester kind antioxidant and Hinered phenols antioxidant form, and the weight ratio of phosphite ester kind antioxidant and Hinered phenols antioxidant is 1:0.3～1:0.7.
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| CN201310667825.4A CN103665723A (en) | 2013-12-07 | 2013-12-07 | Method for preparing high-toughness high-strength polypropylene material through in-situ compatibilization |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001521A (en) * | 2015-04-30 | 2015-10-28 | 南京鸿瑞塑料制品有限公司 | Ionomer modified polypropylene composite material generated by in-situ reaction and preparing method thereof |
| CN109535627A (en) * | 2018-11-21 | 2019-03-29 | 常宁市广富木业有限公司 | High strength wood-plastic composite board material composition and preparation method thereof |
| CN109535325A (en) * | 2018-10-15 | 2019-03-29 | 宁波工程学院 | The method of solwution method preparation norbornene graft polypropylene |
| CN111359377A (en) * | 2018-12-26 | 2020-07-03 | 绍兴福膜新材料有限公司 | Devolatilization method and devolatilization system |
| CN111393784A (en) * | 2019-12-18 | 2020-07-10 | 宁波能之光新材料科技股份有限公司 | Easily-dispersible high-interface-bonding-strength polyolefin filling master batch and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001521A (en) * | 2015-04-30 | 2015-10-28 | 南京鸿瑞塑料制品有限公司 | Ionomer modified polypropylene composite material generated by in-situ reaction and preparing method thereof |
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| CN109535627A (en) * | 2018-11-21 | 2019-03-29 | 常宁市广富木业有限公司 | High strength wood-plastic composite board material composition and preparation method thereof |
| CN111359377A (en) * | 2018-12-26 | 2020-07-03 | 绍兴福膜新材料有限公司 | Devolatilization method and devolatilization system |
| CN111359377B (en) * | 2018-12-26 | 2022-04-15 | 绍兴福膜新材料有限公司 | Devolatilization method and devolatilization system |
| CN111393784A (en) * | 2019-12-18 | 2020-07-10 | 宁波能之光新材料科技股份有限公司 | Easily-dispersible high-interface-bonding-strength polyolefin filling master batch and preparation method thereof |
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Application publication date: 20140326 |