CN106519386A - Preparing method of high-performance HDPE/PET microfiber strengthened blend - Google Patents
Preparing method of high-performance HDPE/PET microfiber strengthened blend Download PDFInfo
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- CN106519386A CN106519386A CN201610968492.2A CN201610968492A CN106519386A CN 106519386 A CN106519386 A CN 106519386A CN 201610968492 A CN201610968492 A CN 201610968492A CN 106519386 A CN106519386 A CN 106519386A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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Abstract
The invention discloses a preparing method of a high-performance HDPE/PET microfiber strengthened blend. The method includes the steps that non-volatile, low-toxicity and high-reactivity diallyl phthalate serves as a comonomer, a GMA serves as a stem grafting monomer, preparation of an HDPE-g-(DAP-co-GMA) graft and capacity increasing of the HDPE/PET blend are carried out, PET disperse orientation and fiber forming are carried out through an appropriate method, the structure is better preserved in a follow-up product, and therefore the aim of strengthening HDPE through PET microfibers on site is achieved. By means of the prepared high-performance HDPE/PET microfiber strengthened blend, the HDPE tensile strength is obviously improved, and the preparing method is of important significance in expanding the application field of the HDPE.
Description
Technical field
The invention belongs to Reactive polymer processing field, it is related to a kind of high-performance, high-density polyethylene (HDPE)/poly-
Ethylene glycol terephthalate (PET) fento strengthens the novel preparation method of blend.
Background technology
The blending and modifying of HDPE and PET is all the emphasis of people's research all the time, adds PET to be expected to realize in HDPE
The high performance of HDPE and engineering plastics.But research all the time finds that the blending of HDPE and PET can not be very
The mechanical strength of HDPE is effectively improved, this aspect is because both HDPE and PET for incompatible polymer, and compatibility is low to be led
Cause blend poor mechanical property；Another aspect is because that the blend of current overwhelming majority HDPE and PET is based on HDPE
Phase, PET are what particle dispersion phase was constituted, when co-mixing system is stressed effect, undertake the main or HDPE of stress, therefore
The mechanical strength of HDPE/PET blends is still close to the mechanical strength of HDPE so that the humidification of PET still embodies not
Out, so HDPE mechanical strengths improve it is unobvious.
In recent years, people's research finds to carry out processing by appropriate processing method by PET to make which deposit in the form of fento
It is the mechanical strength that HDPE can be effectively improved in HDPE matrixes.Shen Jingwei et al. (high density polyethylene (HDPE)s/poly- terephthaldehyde
The form and mechanical property of sour glycol ester in-situ fibrillation enhancing composite, modern chemical industry, 2006,26 (6)：40 44.) with
Phase based on HDPE, PET are prepared for HDPE/PET fento reinforcing materials for dispersion phase, and research finds the mass percent as PET
For 25%, the tensile strength of the fento reinforcing material for being obtained improves 33% than pure HDPE, and Young's modulus improves 66%；King
Will steel et al. (preparation of recycled PET fiber reinforcement HDPE composite and performance study, plastics industry, 2015,43 (10)：35-
39.) being prepared for HDPE/rPET fentos strengthens blend, as a result shows, when rPET contents are 20% in co-mixing system, material to be blended
The mechanical property of material is best.Li Zhongming et al. (Li Z M, Yang W, Huang R, et al.Tensile properties of
poly(ethylene terephthalate)and polyethylene in-situmicrofiber reinforced
Composite formed via slit die extrusion and hot stretching [J] .Mater Lett,
2002,56(5)：HDPE/PET in-situ fibrillations are prepared for using the method for " extrusion-hot stretching-quenching " 756-762.) multiple
Condensation material, when PET contents are 15%～25%, preferably, enhancing effect is also relatively good for the fiber of formation.The equal table of research above
It is bright PET is carried out into in-situ micro-fibrilization in HDPE/PET blends effectively to play humidifications of the PET in HDPE matrixes,
Improve the mechanical strength of HDPE.
But because HDPE and PET is incompatible blend, the quality of Miscibility directly determines final blend
The quality of performance, therefore it is compatible between HDPE and PET to improve during HDPE/PET is blended must to add compatilizer
Property.The compatilizer of traditional HDPE/PET systems is maleic anhydride (MAH), GMA (GMA), acrylic acid
(AA) the polycthylene grafted thing or above-mentioned polar monomer of isopolarity monomer is with styrene (St), trimethylolpropane propylene
Acid esters (Tris), divinylbenzene (DVB) they are polycthylene grafted thing obtained under conditions of co-monomer, but above-mentioned polar monomer
Or there are a series of shortcomings such as volatile, toxicity is big, expensive in co-monomer.
So a kind of environmental protection of exploitation, the compatilizer of low cost have great meaning improving HDPE and PET compatibility
Justice.
The content of the invention
The purpose of the present invention is to overcome in prior art that poor compatibility, compatilizer in HDPE/PET systems be volatile, toxicity
Greatly, expensive the shortcomings of, there is provided a kind of high-performance HDPE/PET fento strengthens the preparation method of blend.This method is using difficult
Volatilization, the diallyl phthalate (DAP) that toxicity is low, reactivity is high are co-monomer, and GMA is grafted monomers, are prepared
Bulking agent of HDPE-g- (DAP-co-GMA) grafts as HDPE/PET systems.
The present invention relates to a kind of adopt New Compatilizer HDPE-g- (DAP-co-GMA) graft, high-performance is prepared high
Density polyethylene (HDPE)/polyethylene terephthalate (PET) fento strengthens the new method of blend.
According to the first aspect of the invention, the invention provides a kind of high-performance HDPE/PET fento strengthens blend
Preparation method, comprises the following steps：
1) preparation of HDPE-g- (DAP-co-GMA) graft
On extruder, mixed material GMA, adjacent benzene two are injected in melt zone using measuring pump
Formic acid diallyl, initiator, control mixed material add speed, prepare the high percent graftings of HDPE-g- (DAP-co-GMA) and connect
Branch thing；Extruder by hopper to die temperature is：150～160 DEG C, 165～170 DEG C, 170～180 DEG C, 180～185 DEG C, 185
～190 DEG C, 180～185 DEG C；The screw speed of the extruder is 60～100 revs/min；
2) preparation of increase-volume PP Pipe Compound
HDPE, HDPE-g- (DAP-co-GMA) graft, PET are carried out into drying and processing；By HDPE after drying, HDPE-g-
(DAP-co-GMA) graft, PET and antioxidant 1010 are mixed, and carry out extruding pelletization in an extruder and obtain increase-volume after mixing
PP Pipe Compound；Extruder by hopper to die temperature is：110～120 DEG C, 240～250 DEG C, 260～280 DEG C, 270～280 DEG C,
270～280 DEG C, 260～270 DEG C；The screw speed of the extruder is 80～120 revs/min；
The HDPE, HDPE-g- (DAP-co-GMA) graft, PET, antioxidant 1010 are counted proportioning by weight and are：
HDPE is 55～85 parts；PET is 10～30 parts；HDPE-g- (DAP-co-GMA) is 5～15 parts；Antioxidant 1010
For 0.3～0.5 part；
3) fento strengthens the preparation of blend
By step 2) drying of increase-volume PP Pipe Compound, stretching and drawing is carried out using wire drawing draw-gear then, by draw-gear
Rotating speed restrained stretching ratio；Material after stretching cooling and shaping in 15～25 DEG C of tank；
4) pelletizing
By step 3) after the material boundling of cooling and shaping, it is cut into the particle of certain draw ratio.
5) injection mo(u)lding
By step 4) particle is molded into test bars after the drying, and mechanics is carried out after batten is processed 12h at 100 DEG C
Performance test；Injection machine by hopper to mouth mold each section of temperature be 140～150 DEG C, 150～160 DEG C, 160～170 DEG C, 170
～180 DEG C；
The HDPE refers to high density polyethylene (HDPE)；PET refers to polyethylene terephthalate.
Preferably, in 210 DEG C of temperature, the melt flow rate (MFR) measured under load 2.16kg is 2～8g/ to the HDPE
The number-average molecular weight of 10min, the PET is 20,000～80,000.
Preferably, step 1) HDPE-g- (DAP-co-GMA) graft preparation in GMA and
Diallyl phthalate constitutes mix monomer, and mix monomer is 0.05～0.15 with HDPE mass ratioes, phthalic acid two
Allyl ester is 0.2～0.8 with the monomer mole ratio of GMA, initiator for mix monomer quality 0.5
～0.8%, in the present invention, mix monomer percent grafting is that 0.5～5%, GMA grafting efficiencies are more than 60%.
Preferably, step 1) described in initiator be dibenzoyl peroxide, cumyl peroxide, 2,5- dimethyl-
One or more in 2,5- bis(t-butylperoxy)s hexane or di-t-butyl peroxide.
Preferably, step 3) in by the rotating speed restrained stretching ratio of draw-gear, draw ratio control is 4～16.
Preferably, step 4) in by the material boundling of cooling and shaping after, be cut into the particle of certain draw ratio, the draw ratio
For 10～45, and follow-up equipment processing charging is not affected, so that fento is intact during following process and possesses
The characteristics of long fiber reinforcement.
The diallyl phthalate (DAP) that this method adopts difficult volatilization, toxicity is low, reactivity is high for co-monomer,
GMA is grafted monomers, prepares HDPE-g- (DAP-co-GMA) grafts as the bulking agent of HDPE/PET systems.DAP is used as altogether
Monomer not only overcomes the shortcoming existing for the co-monomers such as St, DVB, and connects on HDPE strands during melt blending
The DAP of branch can also function to compatibilization by there is ester exchange reaction with PET to HDPE/PET systems, and St, DVB etc. are single altogether
But there is no such effect in body, substantially increase the increase-volume synergy of co-monomer.
The present invention principle be：With HDPE as continuous phase, in co-mixing system process of the PET as dispersion phase, PET is cutting
Cut and stretching action under form fento, by control appropriate processing conditions and it is final granulate when particle draw ratio, make fento
It is able to preserve and produce matrix the effect of long fiber reinforcement during following process；Again through uniform temperature, certain hour
Heat treatment, improve the degree of crystallinity of fento, eliminate internal stress, so as to strengthen fento In-sltu reinforcement effect, and then reach and significantly carry
The purpose of high matrix material performance.
In the present invention, HDPE refers to high density polyethylene (HDPE)；PET refers to polyethylene terephthalate；MAH refers to Malaysia
Acid anhydrides；GMA refers to GMA；DAP is diallyl phthalate；AA refers to acrylic acid；St is referred to
Styrene；Tris refers to trimethylolpropane acrylates；DVB refers to divinylbenzene.
Specific embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this
Invention is further described.It should be understood that these descriptions are simply exemplary, and it is not intended to limit the scope of the present invention.
The HDPE being previously mentioned in following instance：The trade mark 8008, Lanzhou Petrochemical production, MFR=7.6g/10min (190 DEG C,
2.16kg)；Diallyl phthalate (DAP) is produced for Shouguang Nuomeng Chemical Co., Ltd., purity more than 95%；Methyl-prop
Olefin(e) acid ethylene oxidic ester (GMA) is produced for Jiangxi Rui Xiang Chemical Co., Ltd.s, purity more than 99%；Cumyl peroxide
(DCP) produce for Tian Lian Fine Chemical Co., Ltd, purity more than 99%；PET is the limited public affairs of Jiangsu Hydron razor-edge chemical industry
Department sells；Antioxidant 1010 is Shanghai vapour Bagao bridge Chemical Co., Ltd. product；PET：Yizheng petrochemical industry Co., Ltd,
BG802, inherent viscosity are 0.83 ± 0.02.
Embodiment 1
(1) preparation of HDPE-g- (DAP-co-GMA) graft
On extruder of the rotating speed for 120rpm, using measuring pump, in melt zone injection mixed material, (GMA is total with DAP
Quality is 0.4 for the monomer mole ratio of 10%, the DAP and GMA of HDPE mass, and initiator DCP consumption is GMA and DAP gross masses
0.5%), control mixed material add speed, prepare the high percent grafting grafts of HDPE-g- (DAP-co-GMA).Extruder
By hopper to die temperature it is：160℃、170℃、180℃、185℃、190℃、185℃.
(2) preparation of increase-volume PP Pipe Compound
HDPE, HDPE-g- (DAP-co-GMA) graft, PET are carried out into drying and processing.By dried material and antioxygen
Agent is mixed by following mass percent, finally carries out extruding pelletization in an extruder.Extruder is by hopper to mouth mold temperature
Spend and be：120℃、250℃、260℃、270℃、280℃、270℃.
The parts by weight of material are：
HDPE is 55～85 parts；PET is 10～30 parts；HDPE-g- (DAP-co-GMA) is 5～15 parts；Antioxidant 1010
For 0.3～0.5 part；
(3) fento strengthens the preparation of blend
After above-mentioned increase-volume PP Pipe Compound is dried, stretching and drawing is carried out using special wire drawing draw-gear, by drawing dress
The rotating speed restrained stretching ratio put, the cooling and shaping in 15～25 DEG C of tank of the material after stretching obtain the thing that draw ratio is 4
Material.
(4) pelletizing
After by the material boundling of cooling and shaping, the particulate material that draw ratio is 10 is cut into.
(5) injection mo(u)lding
Test bars are molded into after the particulate material that above-mentioned draw ratio is 10 is dried, and batten is processed into 12h at 100 DEG C
After carry out Mechanics Performance Testing.Injection machine is 150 DEG C, 160 DEG C, 170 DEG C, 180 DEG C by each section of temperature of hopper to mouth mold.
Example two
The monomer mole ratio of DAP in one step of example (1) and GMA is changed into into 0.2, other are with example one.
Example three
The monomer mole ratio of DAP in one step of example (1) and GMA is changed into into 0.8, other are with example one.
Example four
GMA in one step of example (1) is changed into into the 5% of HDPE gross masses with DAP monomer gross mass, other are with example one.
Example five
GMA in one step of example (1) is changed into into the 15% of HDPE gross masses with DAP monomer gross mass, other are with example one.
Example six
Change stretching and drawing speed in one step of example (3), obtain the material that draw ratio is 6, other are with example one.
Example seven
Change stretching and drawing speed in one step of example (3), obtain the material that draw ratio is 9, other are with example one.
Example eight
Change stretching and drawing speed in one step of example (3), obtain the material that draw ratio is 16, other are with example one.
Example nine
Change pelletizing draw ratio in one step of example (4), obtain the material that draw ratio is 15, other are with example one.
Example ten
Change pelletizing draw ratio in one step of example (4), obtain the material that draw ratio is 30, other are with example one.
Example 11
Change pelletizing draw ratio in one step of example (4), obtain the material that draw ratio is 45, other are with example one.
Example 12
It is DCP and DTBH by initiator in one step of example (1), respectively accounts for the 50% of weight, other is with example one.
Example 13
Without the pure HDPE8008 of any modification.
Example 14
DAP and GMA mix monomers in one step of example (1) are changed to into the maleic anhydride (MAH) of phase homogenous quantities, other are with real
Example six.
Performance detection：With reference to power of the method for testing in GB/T1040-1992 to each fiber reinforced blends of embodiment
Performance test is learned, data are listed in table 1
1 embodiment performance test of table
From data above, the present invention adopts New Compatilizer HDPE-g- (DAP-co-GMA) graft, is prepared for
High performance HDPE/PET fentos strengthen blend so that the tensile strength of HDPE is significantly improved, and this should for extension HDPE's
It is extremely important with field.
Strengthen the novel preparation method of blend above to a kind of high-performance HDPE/PET in-situ micro-fibril provided by the present invention
It is described in detail.Although embodiments of the present invention are described in detail, it should be understood that, without departing from this
In the case of the spirit and scope of invention, embodiments of the present invention can be made with various changes, replace and change.
Claims (6)
1. a kind of high-performance HDPE/PET fento strengthens the preparation method of blend, comprises the following steps：
1) preparation of HDPE-g- (DAP-co-GMA) graft
On extruder, mixed material GMA, phthalic acid are injected in melt zone using measuring pump
Diallyl, initiator, control mixed material add speed, prepare the high percent grafting grafts of HDPE-g- (DAP-co-GMA)；
Extruder by hopper to die temperature is：150～160 DEG C, 165～170 DEG C, 170～180 DEG C, 180～185 DEG C, 185～190
DEG C, 180～185 DEG C；The screw speed of the extruder is 60～100 revs/min；
2) preparation of increase-volume PP Pipe Compound
HDPE, HDPE-g- (DAP-co-GMA) graft, PET are carried out into drying and processing；By HDPE after drying, HDPE-g-
(DAP-co-GMA) graft, PET and antioxidant 1010 are mixed, and carry out extruding pelletization in an extruder and obtain increase-volume after mixing
PP Pipe Compound；Extruder by hopper to die temperature is：110～120 DEG C, 240～250 DEG C, 260～280 DEG C, 270～280 DEG C,
270～280 DEG C, 260～270 DEG C；The screw speed of the extruder is 80～120 revs/min；
The HDPE, HDPE-g- (DAP-co-GMA) graft, PET, antioxidant 1010 are counted proportioning by weight and are：
HDPE is 55～85 parts；PET is 10～30 parts；HDPE-g- (DAP-co-GMA) is 5～15 parts；Antioxidant 1010 is 0.3
～0.5 part；
3) fento strengthens the preparation of blend
By step 2) drying of increase-volume PP Pipe Compound, stretching and drawing is carried out using wire drawing draw-gear then, turning by draw-gear
Fast restrained stretching ratio；Material after stretching cooling and shaping in 15～25 DEG C of tank；
4) pelletizing
By step 3) after the material boundling of cooling and shaping, it is cut into the particle of certain draw ratio；
5) injection mo(u)lding
By step 4) particle is molded into test bars after the drying, and mechanical property is carried out after batten is processed 12h at 100 DEG C
Test；Injection machine by hopper to mouth mold each section of temperature be 140～150 DEG C, 150～160 DEG C, 160～170 DEG C, 170～
180℃；
The HDPE refers to high density polyethylene (HDPE)；PET refers to polyethylene terephthalate.
2. a kind of high-performance HDPE/PET fento according to claim 1 strengthens the preparation method of blend, and its feature exists
In：In 210 DEG C of temperature, the melt flow rate (MFR) measured under load 2.16kg is 2～8g/10min to the HDPE, the PET's
Number-average molecular weight is 20,000～80,000.
3. a kind of high-performance HDPE/PET fento according to claim 1 strengthens the preparation method of blend, and its feature exists
In：Step 1) HDPE-g- (DAP-co-GMA) graft preparation in GMA and phthalic acid two
Allyl ester constitutes mix monomer, and mix monomer and HDPE mass ratioes are 0.05～0.15, diallyl phthalate and methyl
The monomer mole ratio of glycidyl acrylate is 0.2～0.8, initiator for mix monomer quality 0.5～0.8%.
4. a kind of high-performance HDPE/PET fento according to claim 1 strengthens the preparation method of blend, and its feature exists
In：Step 1) described in initiator be dibenzoyl peroxide, cumyl peroxide, the double (tert-butyl groups of 2,5- dimethyl -2,5-
Peroxy) one or more in hexane or di-t-butyl peroxide.
5. a kind of high-performance HDPE/PET fento according to claim 1 strengthens the preparation method of blend, and its feature exists
In：Step 3) in by the rotating speed restrained stretching ratio of draw-gear, draw ratio control is 4～16.
6. a kind of high-performance HDPE/PET fento according to claim 1 strengthens the preparation method of blend, and its feature exists
In：Step 4) in by the material boundling of cooling and shaping after, be cut into the particle of certain draw ratio, the draw ratio is 10～45.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110054872A (en) * | 2019-04-23 | 2019-07-26 | 华南理工大学 | A kind of PET/PE blend alloy and its preparation method and application |
| WO2024050418A1 (en) * | 2022-08-31 | 2024-03-07 | Dow Global Technologies Llc | Low viscosity functionalized ethylene copolymer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1346845A (en) * | 2001-09-25 | 2002-05-01 | 四川大学 | Process and apparatus for preparing polyolefin/polyglycol terephthalate in-situ micro-fibril reinforced composite material |
| CN105733098A (en) * | 2016-02-23 | 2016-07-06 | 常州大学 | Method for preparing high-performance PP/PET blend |
-
2016
- 2016-10-28 CN CN201610968492.2A patent/CN106519386A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1346845A (en) * | 2001-09-25 | 2002-05-01 | 四川大学 | Process and apparatus for preparing polyolefin/polyglycol terephthalate in-situ micro-fibril reinforced composite material |
| CN105733098A (en) * | 2016-02-23 | 2016-07-06 | 常州大学 | Method for preparing high-performance PP/PET blend |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110054872A (en) * | 2019-04-23 | 2019-07-26 | 华南理工大学 | A kind of PET/PE blend alloy and its preparation method and application |
| WO2024050418A1 (en) * | 2022-08-31 | 2024-03-07 | Dow Global Technologies Llc | Low viscosity functionalized ethylene copolymer |
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Application publication date: 20170322 |