CN106810832A - Modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent and preparation method thereof - Google Patents
Modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent and preparation method thereof Download PDFInfo
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- CN106810832A CN106810832A CN201611216121.5A CN201611216121A CN106810832A CN 106810832 A CN106810832 A CN 106810832A CN 201611216121 A CN201611216121 A CN 201611216121A CN 106810832 A CN106810832 A CN 106810832A
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- crosslinking agent
- polyethylene terephthalate
- cyclic structure
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- 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
- B29C2948/9258—Velocity
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
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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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
Modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent and preparation method thereof, is related to a kind of plastic material and preparation method thereof, and recycled PET is dried；By micro- crosslinking masterbatch attrition grinding, then mix, finally obtain final product reworked material with double screw extruder extruding pelletization.Technical scheme can simultaneously realize enhancing, the effect of toughness reinforcing recycled PET.On the other hand, condensed ring is one kind of aromatic rings, and two rings share two carbon atoms.The crosslinking agent of condensed cyclic structure, because the heat resistance of phenyl structure can be improved with the increase of phenyl ring in molecule, therefore this kind of crosslinking agent has good heat resistance, and certain facilitation can be played in the process of modified PET.And isomerism cross-linking method is introduced into the regenerative process that can make recycled PET the toughness and intensity that compatilizer need not be added to make regenerative PET very well, great market popularization value.
Description
Technical field
It is more particularly to a kind of containing condensed cyclic structure crosslinking agent the present invention relates to a kind of plastic material and preparation method thereof
Modified polyethylene terephthalate of isomerism and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) has good fibre forming property, mechanical property, resistance in thermoplastics type's polyester
The performances such as mill property, creep resistance, low water absorbable and electric insulation, and it is cheap, in fiber, Packaging Bottle, film, engineering plastics
Etc. aspect be widely used.PET is used as engineering plastics, and its crystalline rate is slow, is limited the shortcomings of shock resistance difference
Make its application, it is therefore desirable to which it is modified.
In the crosslinking agent with condensed cyclic structure in the present invention, described condensed ring is one kind of aromatic rings, and two rings are shared
Two carbon atoms.The crosslinking agent of condensed cyclic structure, because the heat resistance of phenyl structure can be improved with the increase of phenyl ring in molecule,
Therefore this kind of crosslinking agent has good heat resistance, and certain facilitation can be played in the process of modified PET.This kind
Crosslinking agent can realize enhancing, resistance to combustion, heat-resisting and other effects while toughness reinforcing, solve to cause stretching strong because of one side performance boost
The decline problem of the performances such as degree, makes PET have preferable overall mechanical properties, such that it is able to reach the purpose of modified recovery
Conventional recovery method carries out toughness reinforcing by increasing elastic body toughening agent, it will usually cause the tensile property of PET resin to decline,
So as to influence overall mechanical property.
The content of the invention
It is an object of the invention to provide a kind of modified poly terephthalic acid of isomerism containing condensed cyclic structure crosslinking agent
Glycol ester and preparation method thereof, crosslinking agent of the present invention has good heat resistance, can be played in the process of modified PET
Certain facilitation.And isomerism cross-linking method be introduced into the regenerative process that can make recycled PET need not add it is compatible
Agent can also make the toughness and intensity of regenerative PET fine.
The purpose of the present invention is achieved through the following technical solutions：
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, the poly terephthalic acid second two
Alcohol ester contains condensed ring crosslinking agent, and its structure is as follows：
；
Polyethylene terephthalate is as follows into being grouped into based on mass weight part：Reclaim polyethylene terephthalate
100 parts；10~30 parts of toughener；10~30 parts of crosslinking masterbatch；10~20 parts of inorganic filler；3~20 parts of heat stabilizer.
The modified polyethylene terephthalate of the described isomerism containing condensed cyclic structure crosslinking agent, contains condensed ring knot
There is addition reaction system by acenaphthene formula cyclopentadienone, poly- methyl vinyl silicon oil and vinyltrimethoxy silane in the initiator of structure
.
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, and the toughener is KT-
At least one in 22, KT-915.
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, and described crosslinking masterbatch are
It is made up of A material B material and product aqua three step part；
A expects composition:Polyethylene terephthalate
Contain condensed cyclic structure crosslinking agent
Initiator（The different hydrogen propyl benzene (CHP) of peroxidating）
B expects composition：Polyethylene terephthalate
Catalyst（Dibutyl tin laurate）
Antioxidant（Antioxidant 1010）
Produce aqua composition：Acid and metal oxide.
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, the acid in the product aqua
It is at least one in stearic acid, inorganic acid.
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, the gold in the product aqua
Category oxide is at least one in zinc oxide, tin oxide.
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, and described filler is carbonic acid
At least one in calcium, talcum powder.
Isomerism containing condensed cyclic structure crosslinking agent is modified polyethylene terephthalate, and the heat stabilizer is Asia
Triphenyl phosphate.
The modified polyethylene terephthalate preparation method of isomerism containing condensed cyclic structure crosslinking agent, methods described
Comprise the following steps：
A, 95 parts of A material is weighed by mass fraction, extruding pelletization in double screw extruder is put into after 4.5 parts of B material mixing, then again with
0.5 part of product aqua（Stearic acid and zinc oxide 1:1 mixture）The well mixed double screw extruder extruding pelletization that is put into forms friendship
Connection masterbatch；
B, the micro- crosslinking masterbatch in A portions are first put into Universalpulverizer place into planetary ball mill grinding until crosslinking masterbatch
Particle diameter reach 10~50 μm untill；
C, hard PET material forced air drying 6~8 hours under the conditions of 80 DEG C will be reclaimed, by weight ratio by micro- crosslinking masterbatch, heat
Stabilizer, recovery hard PET, inorganic filler mix 4~6 minutes in putting into high-speed mixer, make its uniform mixing；
D, the above-mentioned material being well mixed in high-speed mixer is added to screw slenderness ratio for 36, rotating speed is 200r/min's
In double screw extruder, the average grain diameter of micro- crosslinking masterbatch is controlled 10 using the Strong shear power of twin-screw in the molten state
~50 μm, while crosslinking material is well mixed with heat stabilizer, reclaimed materials and inorganic filler, by above-mentioned compound extruding pelletization
Obtain the regeneration hard PET containing crosslinking PET.
The modified polyethylene terephthalate preparation method of the described isomerism containing condensed cyclic structure crosslinking agent, institute
The extruder temperature for stating double screw extruder is controlled between 260 DEG C -280 DEG C.
Advantages of the present invention is with effect：
The present invention can simultaneously realize enhancing, the effect of toughness reinforcing recycled PET.On the other hand, condensed ring is one kind of aromatic rings, two rings
Share two carbon atoms.The crosslinking agent of condensed cyclic structure, because the heat resistance of phenyl structure can be with the increase of phenyl ring in molecule
Improve, therefore this kind of crosslinking agent has good heat resistance, certain promotion can be played in the process of modified PET and is made
With.And being introduced into the regenerative process that can make recycled PET for isomerism cross-linking method need not add the compatilizer can also to make again
The toughness and intensity of raw PET are fine, great market popularization value.
Brief description of the drawings
Fig. 1 is the synthetic reaction equation of acenaphthene formula cyclopentadienone；
Fig. 2 and Fig. 3 are the synthetic reaction equations of many phenylethylene base silanes.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Embodiment 1-3, the weight distribution ratio of each component is as shown in table 1 in each embodiment.Each component is weighed by proportioning,
Mix 5 minutes in homogenizer, be placed in the raw material of compound in double screw extruder and make material, extruder temperature by discharging
Between 260 DEG C -280 DEG C, rotating speed is 200r/min for control.Batten is prepared, by corresponding standard testing（It is shown in Table 2）, performance knot
Fruit is shown in Table 3.
Table 1：Formula composition (part of embodiment 1-3）
Table 2：Mechanics Performance Testing standard
| Test event | Testing standard |
| Tensile strength MPa | GB/T 1040.1-2006 |
| Elongation at break % | GB/T 1040.1-2006 |
| Bending strength MPa | ASTM D-790 |
| Bending modulus MPa | ASTM D-790 |
| GB/T 1043-93 |
Table 3：The Mechanics Performance Testing of PET feed backs in embodiment 1-3
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Tensile strength MPa | 55 | 56 | 57 |
| Elongation at break % | 50% | 80% | 78% |
| Bending strength MPa | 84 | 88 | 96 |
| Bending modulus MPa | 5200 | 5800 | 6500 |
| 0.4 | 0.5 | 0.6 |
Comparative example 1-4, the weight distribution ratio of each component is as shown in table 4 in each comparative example.Each component is weighed by proportioning, Yu Gao
Fast stirrer for mixing 4 minutes, be placed in the raw material of compound in double screw extruder by discharging makes material, the temperature 260 of extruder
DEG C -280 DEG C, rotating speed 150r/min.Batten is prepared, by corresponding standard testing（It is shown in Table 2）, results of property is shown in Table 5.
Table 4：The formula composition of comparative example 1-4
Table 5：The Mechanics Performance Testing of recycled PET in comparative example 1-4
| Test event | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Tensile strength MPa | 55 | 56 | 57 | 60 |
| Elongation at break % | 50% | 80% | 78% | 48% |
| Bending strength MPa | 84 | 88 | 96 | 85 |
| Bending modulus MPa | 5200 | 5800 | 6500 | 6000 |
| 0.4 | 0.5 | 0.6 | 0.9 |
From the mechanical experimental results of the embodiment 1-3 of table 3 and comparative example 1-4, we understand：Use toughener merely
When, the tensile property of material can be reduced while recycled PET impact property is improved；And obtained micro- crosslinking masterbatch
Particle diameter is crushed to after 10~50 μm will be crosslinked the twin-screw extrusion that big L/D ratio is put into material and recycled PET, inorganic filler etc. again
Shear-mixed in machine, its tensile property can also be improved while recycled PET impact property is improved；Realize to recycled PET
Material carries out the effect of activeness and quietness simultaneously.Introducing containing condensed cyclic structure crosslinking agent simultaneously also has certain side to process
Help, play efficient crosslinked action.
The present invention is further illustrated above by specific embodiment, but these embodiments are only exemplary
, any limitation is not constituted to protection scope of the present invention.It will be appreciated by those skilled in the art that without departing from spirit of the invention
In the case of protection domain, technical solutions and their implementation methods of the present invention can be carried out various equivalencings, modification or
Improve, these all should fall within the scope of protection of the present invention.Protection scope of the present invention is defined by appended claim.
Claims (10)
1. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：It is described poly-
Ethylene glycol terephthalate contains condensed ring crosslinking agent, and its structure is as follows：
；
Polyethylene terephthalate is as follows into being grouped into based on mass weight part：Reclaim polyethylene terephthalate
100 parts；10~30 parts of toughener；10~30 parts of crosslinking masterbatch；10~20 parts of inorganic filler；3~20 parts of heat stabilizer.
2. the modified polyethylene terephthalate of the isomerism containing condensed cyclic structure crosslinking agent according to claim 1
Ester, it is characterised in that：Initiator containing condensed cyclic structure is by acenaphthene formula cyclopentadienone, poly- methyl vinyl silicon oil and vinyl three
There is addition reaction and be obtained in methoxy silane.
3. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：The increasing
Tough dose is KT-22, at least one in KT-915.
4. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：Described
Crosslinking masterbatch are made up of A material B material and product aqua three step part；
A expects composition:Polyethylene terephthalate
Contain condensed cyclic structure crosslinking agent
Initiator（The different hydrogen propyl benzene (CHP) of peroxidating）
B expects composition：Polyethylene terephthalate
Catalyst（Dibutyl tin laurate）
Antioxidant（Antioxidant 1010）
Produce aqua composition：Acid and metal oxide.
5. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：The product
Acid in aqua is at least one in stearic acid, inorganic acid.
6. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：The product
Metal oxide in aqua is at least one in zinc oxide, tin oxide.
7. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：It is described to fill out
Expect to be at least one in calcium carbonate, talcum powder.
8. the modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent, it is characterised in that：The heat
Stabilizer is triphenyl phosphite.
9. the modified polyethylene terephthalate preparation method of isomerism containing condensed cyclic structure crosslinking agent, its feature exists
In：The described method comprises the following steps：
A, 95 parts of A material is weighed by mass fraction, extruding pelletization in double screw extruder is put into after 4.5 parts of B material mixing, then again with
0.5 part of product aqua（Stearic acid and zinc oxide 1:1 mixture）The well mixed double screw extruder extruding pelletization that is put into forms friendship
Connection masterbatch；
B, the micro- crosslinking masterbatch in A portions are first put into Universalpulverizer place into planetary ball mill grinding until crosslinking masterbatch
Particle diameter reach 10~50 μm untill；
C, hard PET material forced air drying 6~8 hours under the conditions of 80 DEG C will be reclaimed, by weight ratio by micro- crosslinking masterbatch, heat
Stabilizer, recovery hard PET, inorganic filler mix 4~6 minutes in putting into high-speed mixer, make its uniform mixing；
D, the above-mentioned material being well mixed in high-speed mixer is added to screw slenderness ratio for 36, rotating speed is 200r/min's
In double screw extruder, the average grain diameter of micro- crosslinking masterbatch is controlled 10 using the Strong shear power of twin-screw in the molten state
~50 μm, while crosslinking material is well mixed with heat stabilizer, reclaimed materials and inorganic filler, by above-mentioned compound extruding pelletization
Obtain the regeneration hard PET containing crosslinking PET.
10. the modified poly terephthalic acid second of the isomerism containing condensed cyclic structure crosslinking agent according to claim requirement 9
Diol ester preparation method, it is characterised in that：The extruder temperature of the double screw extruder is controlled between 260 DEG C -280 DEG C.
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|---|---|---|---|
| CN201611216121.5A CN106810832A (en) | 2016-12-26 | 2016-12-26 | Modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent and preparation method thereof |
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| CN201611216121.5A CN106810832A (en) | 2016-12-26 | 2016-12-26 | Modified polyethylene terephthalate of isomerism containing condensed cyclic structure crosslinking agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073234A (en) * | 2019-12-30 | 2020-04-28 | 浙江新力新材料股份有限公司 | Heat-resistant flame-retardant PET composite material, preparation method thereof and application thereof in preparation of patch board |
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|---|---|---|---|---|
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| JPS5421377B1 (en) * | 1970-04-17 | 1979-07-30 | ||
| CN1275143A (en) * | 1998-06-22 | 2000-11-29 | Ck韦特科公司 | Silane vulcanized thermoplastic elastomers |
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| CN101798495A (en) * | 2009-02-10 | 2010-08-11 | 上海诺科化工新材料有限公司 | Method for synthesizing water-solubility or water-dispersity adhesives by recycling polyester waste materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073234A (en) * | 2019-12-30 | 2020-04-28 | 浙江新力新材料股份有限公司 | Heat-resistant flame-retardant PET composite material, preparation method thereof and application thereof in preparation of patch board |
| CN111073234B (en) * | 2019-12-30 | 2022-04-08 | 浙江新力新材料股份有限公司 | Heat-resistant flame-retardant PET composite material, preparation method thereof and application thereof in preparation of patch board |
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