CN106832894B - A kind of isomerism of the crosslinking agent containing condensed cyclic structure is modified to recycle nylon and preparation method thereof - Google Patents
A kind of isomerism of the crosslinking agent containing condensed cyclic structure is modified to recycle nylon and preparation method thereof Download PDFInfo
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- CN106832894B CN106832894B CN201611224964.XA CN201611224964A CN106832894B CN 106832894 B CN106832894 B CN 106832894B CN 201611224964 A CN201611224964 A CN 201611224964A CN 106832894 B CN106832894 B CN 106832894B
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such 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
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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
- C08L2312/00—Crosslinking
Abstract
A kind of isomerism of the crosslinking agent containing condensed cyclic structure is modified to recycle nylon and preparation method thereof, it is related to a kind of recycling nylon and preparation method thereof, the specific method of modifying of the present invention is: will recycle nylon first forced air drying 3~4 hours under the conditions of 80 DEG C, it will be by condensed cyclic structure crosslinking agent and dried recycling nylon, initiator, catalyst, antioxidant, micro- crosslinking masterbatch made from the melting mixings extruding pelletizations such as production aqua are first put into Universalpulverizer and place into grinding in planetary ball mill until the partial size of micro- crosslinking masterbatch reaches 10~50 μm, then by weight ratio by dried recycling nylon, micro- crosslinking masterbatch, 4~6min of high-speed mixer and mixing is put into toughener and inorganic filler, finally with double screw extruder, extruding pelletization has the regeneration nylon of isomeric structur to obtain the final product at 180 DEG C~240 DEG C.The present invention realizes the effect of the mechanical properties such as toughening, enhancing recycling nylon, keeps the performance of reworked material fine, great market popularization value.
Description
Technical field
The present invention relates to a kind of recycling nylon and preparation method thereof, more particularly to a kind of the same of crosslinking agent containing condensed cyclic structure
Modified recycling nylon of matter isomery and preparation method thereof.
Background technique
Fypro is commonly called as nylon (Nylon), and nylon is widely used in terminal consumer products, belongs to crystallinity polymerization
Object, there are firm hydrogen bonds between the amide group on strand, and crystallinity and fusing point are higher, have excellent mechanical property
Can, however waste and old nylon resin, because of aging action, mechanical property especially impact resistance can not show a candle to nylon virgin material.
With the shortage of petroleum resources and getting worse for environmental protection, market competition is extremely fierce, regenerates nylon resin
Application gradually increase, many nylon products production commercial city starts to reduce cost using regeneration nylon material, however recycling nylon
Because aging action, mechanical property especially erosion-resisting characteristics can not show a candle to nylon virgin material, need to be modified rear can be carried out again resin
Secondary utilization, therefore we need the crosslinking agent of a kind of novel technological means and excellent properties efficiently to carry out discarded nylon
Modified and recycling.
The application for a patent for invention that China Patent Publication No. is CN105219074A has used the enhancing of isomerism cross-linking method to increase
Tough recycling nylon, the crosslinking agent used are vinyltrimethoxysilane, and silane crosslinker Applicable temperature is small, cannot be to crosslinking
The big plastic material of temperature is modified, and heat resistance is bad, and activity is lower under high temperature, is applied to higher melting-point plastics
Such as the crosslinking of nylon, since the reaction temperature of crosslinking agent and the melting temperature of nylon be not within the scope of same temperature, so crosslinking
Effect can be undesirable, therefore we need a kind of biggish crosslinking agent of crosslinking temperature to improve the deficiency of the preparation method, into one
Step break through because under material melt temp is high or crosslinking agent high temperature activity it is low due to cannot use suffered by limitation.
Summary of the invention
The purpose of the present invention is to provide a kind of modified recycling nylon of the isomerism of crosslinking agent containing condensed cyclic structure and its systems
Preparation Method, the present invention in crosslinking agent can be than not due to introducing multiple phenyl ring i.e. condensed cyclic structure, heat resistance in structure
Silane crosslinker containing benzene ring structure correspondinglys increase, when this crosslinking agent for nylon salvage material it is cross-linking modified when, handing over
While connection nylon material promotes its mechanical property, moreover it is possible to play the role of improving nylon heat resistance, to obtain high-performance
Recycle modified nylon material.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of modified recycling nylon of the isomerism of the crosslinking agent containing condensed cyclic structure, the crosslinking agent is with condensed cyclic structure
Crosslinking agent, structural formula are as follows:
；
The composition of modified recycling nylon material forms as follows based on mass weight part:
100 parts of nylon of recycling；
3~20 parts of toughener；
10~30 parts of micro- crosslinking masterbatch；
5~10 parts of inorganic filler.
A kind of modified recycling nylon of the isomerism of crosslinking agent containing condensed cyclic structure, the toughener are POE, EVA
At least one of, preferably POE.
A kind of modified recycling nylon of the isomerism with crosslinking agent containing condensed cyclic structure, micro- crosslinking masterbatch are
It is made of A material, B material and production aqua three parts；
A expects composition: nylon
Crosslinking agent
Initiator
B expects composition: nylon
Catalyst
Antioxidant
Produce aqua composition: acid and metal oxide are with the mixing of (1:1) ratio；
The inorganic filler is at least one of calcium carbonate, talcum powder, preferably calcium carbonate；
The initiator be at least one of benzoyl peroxide (BPO) and cumyl peroxide (DCP), preferably
Cumyl peroxide；
The antioxidant is at least one of antioxidant 1010, antioxidant 1076, preferably antioxidant 1010；
The catalyst is dibutyl tin dilaurate, triethylamine, Tri-n-Propylamine, tri-n-butylamine, N, N- dimethyl butyrate
At least one of amine, preferably dibutyl tin dilaurate；
The production aqua is that acid and metal oxide are mixed in a certain proportion, preferably stearic acid and zinc oxide.
A kind of modified recycling nylon preparation method of the isomerism of the crosslinking agent containing condensed cyclic structure, the specific steps of the method
It is as follows:
A, 95 parts of A material are weighed by mass fraction, is put into extruding pelletization in double screw extruder after 4.5 parts of B material mixing, then
Aqua (mixture that stearic acid and zinc oxide molar ratio are 1:1) is produced with 0.5 part again and is uniformly mixed that be put into double screw extruder crowded
It is granulated out and forms micro- crosslinking masterbatch；
B, micro- crosslinking masterbatch in the portion A are first put into Universalpulverizer and place into planetary ball mill grinding until micro- friendship
Until the partial size of connection masterbatch reaches 10~50 μm；
C, will recycling nylon material forced air drying 3~4 hours under the conditions of 80 DEG C, by weight ratio by micro- crosslinking masterbatch,
Toughener, recycling nylon, inorganic filler are put into high-speed mixer and are mixed 4~6 minutes, mix it uniformly；
D, the above-mentioned material being uniformly mixed in a high speed mixer is added to screw slenderness ratio is 36, revolving speed 200r/
In the double screw extruder of min, utilize the Strong shear power of twin-screw by the average grain diameter control of micro- crosslinking masterbatch in the molten state
System is uniformly mixed at 10~50 μm, while by crosslinking material with toughener, recycling nylon and inorganic filler, and above-mentioned mixture is squeezed
It is granulated out and obtains regeneration nylon.
A kind of modified recycling nylon preparation method of the isomerism of crosslinking agent containing condensed cyclic structure, the twin-screw squeeze
The extruder temperature of machine controls between 180 DEG C~240 DEG C out.
The advantages and effects of the present invention are:
Crosslinking agent of the invention is the silane crosslinker containing more benzene ring structures, its is resistance to for most molecules containing benzene ring structure
Hot property is relatively preferable, and the crosslinking agent in the present invention is heat-resisting due to introducing multiple phenyl ring i.e. condensed cyclic structure in structure
Property can be than be correspondinglyd increase without the silane crosslinker of benzene ring structure, when this crosslinking agent is for the cross-linking modified of nylon salvage material
When, while cross-link nylon material promotes its mechanical property, moreover it is possible to play the role of improving nylon heat resistance, to obtain
High-performance recycles modified nylon material.
Isomerism cross-linking method (activeness and quietness) modification of the present invention is to improve a kind of effective way of plastics mechanical property,
Technological operation is simple and can produce recycled plastic in enormous quantities, meets the industrial requirement in market, therefore, for existing
Defect this method of technology is modified recycling nylon by a kind of isomerism cross-linking method of crosslinking agent containing condensed cyclic structure, to reach
Improve recycling nylon mechanical property.
Detailed description of the invention
Fig. 1 is the molecular structural formula of condensed cyclic structure crosslinking agent.
Specific embodiment
The following describes the present invention in detail with reference to examples.
The weight distribution ratio of each component is as shown in table 1 in embodiment 1-3 and comparative example.Each component is weighed according to the ratio, in
It is mixed 5 minutes in high-speed mixer, discharges, the raw material of mixture is placed in double screw extruder and makes material, extruder temperature control
System is between 180 DEG C~240 DEG C, revolving speed 200r/min.Batten is prepared, by corresponding standard testing (see Table 2), results of property
It is shown in Table 3.
Table 1: the formula composition (part) of embodiment 1-3 and comparative example
Table 2: Mechanics Performance Testing standard
Table 3: the Mechanics Performance Testing of nylon is regenerated in embodiment 1-3 and comparative example
From the mechanical experimental results in the embodiment 1-3 and comparative example of table 3 it can be seen that female not using micro- crosslinking
When material, the addition of other modified additives can reduce the tensile property of material while improving and recycling nylon impact property,
And the partial size of micro- crosslinking masterbatch obtained is crushed to after 10~50 μm and again puts into micro- crosslinking masterbatch and recycling nylon etc. greatly
Shear-mixed in the double screw extruder of draw ratio makes crosslinking material form isomerism dispersed structure, this method with reclaimed materials
It can also be improved its tensile property while improving and recycling nylon impact property, realize isomerism cross-linking method to recycling Buddhist nun
Imperial material carries out the effect of activeness and quietness simultaneously.
The present invention is further illustrated above by specific embodiment, but these embodiments are only exemplary
, any restrictions are 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 where protection scope, technical solutions and their implementation methods of the present invention can be carried out a variety of equivalencings, modification or
It improves, these should all fall within the scope of protection of the present invention.Protection scope of the present invention is subject to the attached claims.
Claims (4)
1. a kind of modified recycling nylon of the isomerism of crosslinking agent containing condensed cyclic structure, which is characterized in that the crosslinking agent is to have
The crosslinking agent of condensed cyclic structure, structural formula are as follows:
；
The composition of modified recycling nylon material forms as follows based on mass weight part:
100 parts of nylon of recycling；
3~20 parts of toughener；
10~30 parts of micro- crosslinking masterbatch；
5~10 parts of inorganic filler；
Micro- crosslinking masterbatch are expected by A, B expects and produce aqua three parts forms；
A expects composition: nylon
Crosslinking agent
Initiator, the initiator are at least one of benzoyl peroxide BPO and cumyl peroxide DCP；
B expects composition: nylon
Catalyst, the catalyst are dibutyl tin dilaurate, triethylamine, Tri-n-Propylamine, tri-n-butylamine, N, N- diformazan
At least one of base butylamine,
Antioxidant, the antioxidant are at least one of antioxidant 1010, antioxidant 1076；
Produce aqua composition: acid and metal oxide are mixed with the molar ratio of 1:1；
The inorganic filler is at least one of calcium carbonate, talcum powder.
2. a kind of modified recycling nylon of the isomerism of crosslinking agent containing condensed cyclic structure according to claim 1, feature exist
In the toughener is at least one of POE, EVA.
3. a kind of modified recycling nylon of the isomerism of crosslinking agent containing condensed cyclic structure according to claim 1, feature exist
In specific step is as follows for the preparation method of the modified recycling nylon of the isomerism of the crosslinking agent containing condensed cyclic structure:
A, weigh 95 parts of A material by mass fraction, be put into extruding pelletization in double screw extruder after 4.5 parts of B material mixing, then again with
The mixing of 0.5 part of production aqua is uniformly mixed and is put into double screw extruder extruding pelletization and forms micro- crosslinking masterbatch, and the production aqua is
The mixture that stearic acid and zinc oxide molar ratio are 1:1；
B, by A walk in micro- crosslinking masterbatch be first put into Universalpulverizer and place into planetary ball mill grinding until micro- crosslinking mother
Until the partial size of material reaches 10~50 μm；
C, nylon material will be recycled forced air drying 3~4 hours under the conditions of 80 DEG C, by weight ratio by micro- crosslinking masterbatch, toughening
Agent, recycling nylon, inorganic filler are put into high-speed mixer and are mixed 4~6 minutes, mix it uniformly；
D, the above-mentioned material being uniformly mixed in a high speed mixer is added to screw slenderness ratio is 36, and revolving 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 micro- crosslinking masterbatch being uniformly mixed with toughener, recycling nylon and inorganic filler, above-mentioned mixture is squeezed out
It is granulated and obtains the modified recycling nylon of isomerism of the crosslinking agent containing condensed cyclic structure.
4. a kind of modified recycling nylon of the isomerism of crosslinking agent containing condensed cyclic structure according to claim 3, feature exist
In the extruder temperature of the double screw extruder of the preparation method controls between 180 DEG C~240 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611224964.XA CN106832894B (en) | 2016-12-27 | 2016-12-27 | A kind of isomerism of the crosslinking agent containing condensed cyclic structure is modified to recycle nylon and preparation method thereof |
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| CN201611224964.XA CN106832894B (en) | 2016-12-27 | 2016-12-27 | A kind of isomerism of the crosslinking agent containing condensed cyclic structure is modified to recycle nylon and preparation method thereof |
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| CN106832894A CN106832894A (en) | 2017-06-13 |
| CN106832894B true CN106832894B (en) | 2019-06-21 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105219074A (en) * | 2015-11-09 | 2016-01-06 | 沈阳化工大学 | Isomerism crosslinking toughen and intensify reclaims nylon and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219074A (en) * | 2015-11-09 | 2016-01-06 | 沈阳化工大学 | Isomerism crosslinking toughen and intensify reclaims nylon and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 含有稠环侧链的聚硅氧烷的合成及其对加成型高温硫化硅橡胶性能的影响;杜作栋,尹上;《高分子学报》;19881226(第6期);第422-427页 |
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