CN106589786B - One kind isomerism modified polyacetal of crosslinking agent containing L-POSS and preparation method thereof - Google Patents
One kind isomerism modified polyacetal of crosslinking agent containing L-POSS and preparation method thereof Download PDFInfo
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Abstract
A kind of isomerism modified polyacetal of crosslinking agent containing L-POSS and preparation method thereof is related to a kind of polyformaldehyde and preparation method thereof, will first recycle POM in drying；Homemade micro- crosslinking masterbatch are smashed and ground, high-speed mixer and mixing then is put into dried recycling hard POM, micro- crosslinking masterbatch, heat stabilizer and inorganic filler by weight ratio, finally with double screw extruder extruding pelletization up to reworked material.The present invention can realize the effect of enhancing, toughening recycling POM simultaneously.On the other hand, the crosslinking agent of the structure containing L-POSS is with Si-O for inorganic kernel, and inorganic kernel can assign its good heat resistance, flame resistance, splendid water resistance, radiativity and electrical property, can play certain facilitation in process.And being introduced into for isomerism cross-linking method can make it is not necessary that compatilizer is added or keeps the toughness for regenerating POM and intensity fine in the regenerative process for recycling POM, great market popularization value.
Description
Technical field
The present invention relates to a kind of polyformaldehyde and preparation method thereof, more particularly to a kind of isomerism of crosslinking agent containing L-POSS
Modified polyacetal and preparation method thereof.
Background technique
L-POSS crosslinking agent is the synthetic method reacted using L-POSS with silane compound, synthesizes novel silane crosslinking
Agent.Product is the derivative of silane, is catalyzed silane generates under initiation active site and-LPOSS formation polyaddition reaction,
The crosslinking agent with double crosslinked actions is formed, at the same time, because L-POSS is different from traditional organic matter, it is using Si-O as nothing
Machine kernel, inorganic kernel can assign its good heat resistance, flame resistance, splendid water resistance, radiativity and electrical property, so
The novel silane crosslinking agent containing L-POSS of synthesis also has greatly improved in these performances, therefore this silane crosslinker can be
High temperature, the lower presence of high radiation, and its crosslinking agent performance of doing more independent than silane is more preferable, and the cost of crosslinking agent is also directly done than POSS
Much smaller, cross-linking effect is more preferable, performance also gets a promotion.
Polyformaldehyde (English: polyformaldehyde) also known as acetal resin, there is good physics, mechanically and chemically property
Can, especially there is excellent crocking resistance, is the third-largest general-purpose plastics.Suitable for make anti-attrition wear part, driving parts,
And chemical industry, the parts such as instrument.Property it is good, fatigue durability is prominent, is not easy to be corroded by chemical mediator etc..In recent years, as industry is sent out
The demand of exhibition, concern of the people to the study on the modification of polyformaldehyde also more.Polyformaldehyde (POM) is to be lower than other many engineering plastics
Cost, substituting some markets traditionally captured by metal, such as substituting zinc, brass, aluminium and steel make many components,
Since the advent of the world, POM have been widely used for the fields such as electronics, machinery, machinery, instrument, daily light industry, automobile, building materials, agricultural.
In the application of many frontiers, such as medical technology, sports apparatus etc., POM also shows preferable growing trend.
On the other hand, POM is corroded by strong acid, and weatherability is poor, poor adhesion, and thermal decomposition is close with softening temperature, and limit oxygen refers to
The disadvantages of number is small, and shock resistance is poor limits its application, it is therefore desirable to be modified to it, this patent passes through L-POSS crosslinking agent
The preparation method of the modified POM of isomerism cross-linking method that activeness and quietness is carried out to it is modified.
Summary of the invention
The purpose of the present invention is to provide a kind of isomerism modified polyacetal of crosslinking agent containing L-POSS and preparation method thereof,
The crosslinking agent of present invention structure containing L-POSS be with Si-O be inorganic kernel, inorganic kernel can assign its good heat resistance,
Flame resistance, splendid water resistance, radiativity and electrical property can play certain facilitation in process, can be real simultaneously
The effect of POM is recycled in now enhancing, toughening.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of isomerism modified polyacetal of crosslinking agent containing L-POSS, the L-POSS crosslinking agent are using L-POSS
The method reacted with silane compound, product are the derivatives of silane；Its structure are as follows:
；
Isomerism modified polyacetal is based on mass weight part, component are as follows:
100 parts of polyformaldehyde of recycling；
10~30 parts of toughener；
10~30 parts of crosslinking masterbatch；
10~20 parts of inorganic filler；
3~20 parts of heat stabilizer.
One kind isomerism modified polyacetal of crosslinking agent containing L-POSS, the synthetic cross-linking agent include two ranks
Section, is to form raw material first, and silane generates active site and forms chemical reaction to introduce L-POSS followed by under catalytic action
Prepare silane crosslinker containing L-POSS.
One kind isomerism modified polyacetal of crosslinking agent containing L-POSS, the toughener are POM/POE, POM/
At least one of EVA.
One kind isomerism modified polyacetal of crosslinking agent containing L-POSS, the crosslinking masterbatch are by A material B material and produce water
Three step part of agent composition；
A expects composition: polyformaldehyde
The crosslinking agent of structure novel containing L-POSS
Initiator (cumyl peroxide (DCP))
B expects composition: polyformaldehyde
Catalyst (dibutyl tin dilaurate)
Antioxidant (antioxidant 1010)
Produce aqua composition: acid and metal oxide；Producing the acid in aqua is at least one of stearic acid, inorganic acid；Gold
Category oxide is at least one of zinc oxide, tin oxide.
One kind isomerism modified polyacetal of crosslinking agent containing L-POSS, the filler are calcium carbonate, in talcum powder
At least one.
One kind isomerism modified polyacetal of crosslinking agent containing L-POSS, the heat stabilizer are phosphorous triphenyl phosphate
Ester.
A kind of isomerism modified polyacetal preparation method of crosslinking agent containing L-POSS, the described method comprises the following steps:
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
It is uniformly mixed again with 0.5 part of production aqua (mixture of stearic acid and zinc oxide 1:1) and is put into double screw extruder extruding pelletization shape
At crosslinking masterbatch；
B, micro- crosslinking masterbatch in the portion A are first put into Universalpulverizer and place into grinding in planetary ball mill until crosslinking
Until the partial size of masterbatch reaches 10~50 μm；
C, hard POM material will be recycled forced air drying 6~8 hours under the conditions of 80 DEG C, it is by weight ratio that micro- crosslinking is female
Material, heat stabilizer, recycling hard POM, 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 heat stabilizer, reclaimed materials and inorganic filler, and above-mentioned mixture is squeezed
It is granulated out and obtains the regeneration hard POM containing crosslinking POM.
One kind isomerism modified polyacetal preparation method of crosslinking agent containing L-POSS, the double screw extruder
Extruder temperature controls between 160 DEG C -180 DEG C.
The advantages and effects of the present invention are:
The present invention can realize the effect of enhancing, toughening recycling POM simultaneously.On the other hand, the crosslinking agent of the structure containing L-POSS
It is with Si-O for inorganic kernel, inorganic kernel can assign its good heat resistance, flame resistance, splendid water resistance, radiativity
And electrical property, certain facilitation can be played in process.And the introducing of isomerism cross-linking method can make to recycle
The toughness for regenerating POM and intensity can also be made fine it is not necessary that compatilizer is added in the regenerative process of POM, great marketing valence
Value.
Detailed description of the invention
Fig. 1 is the reaction equation of the synthesis high temperature resistant crosslinking agent of L-POSS and vinyltrimethoxysilane.
Specific embodiment
The following describes the present invention in detail with reference to examples.
Embodiment 1-3, the weight distribution ratio of each component is as shown in table 1 in each embodiment.Each component is weighed according to the ratio,
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 is between 160 DEG C -180 DEG C, revolving speed 200r/min.Batten is prepared, by corresponding standard testing (see Table 2), performance knot
Fruit is shown in Table 3.
Table 1: the formula composition (part) of embodiment 1-3
Table 2: Mechanics Performance Testing standard
| Test item | 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 |
| The strong KJ/m of notch shock2 | GB/T 1043-93 |
Table 3: the Mechanics Performance Testing of POM feed back in embodiment 1-3
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Tensile strength MPa | 58 | 64 | 68 |
| Elongation at break % | 56% | 68% | 70% |
| Bending strength MPa | 80 | 85 | 90 |
| Bending modulus MPa | 82 | 86 | 98 |
| The strong KJ/m of notch shock2 | 64 | 89 | 88 |
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 according to the ratio,
It is mixed 4 minutes in high-speed mixer, the raw material of mixture is placed in double screw extruder by discharging makes material, the temperature of extruder
160 DEG C -180 DEG C of degree, revolving speed 150r/min.Batten is prepared, by corresponding standard testing (see 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 POM is recycled in comparative example 1-4
| Test item | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Tensile strength MPa | 58 | 64 | 68 | 80 |
| Elongation at break % | 56% | 68% | 70% | 69% |
| Bending strength MPa | 80 | 85 | 90 | 85 |
| Bending modulus MPa | 82 | 86 | 98 | 79 |
| The strong KJ/m of notch shock2 | 64 | 89 | 88 | 96 |
From the mechanical experimental results of table 3 embodiment 1-3 and comparative example 1-4, we are known: simple using increasing
When tough dose, the tensile property of material can be reduced while improving and recycling POM impact property；And it is micro- crosslinking obtained is female
The partial size of material is crushed to the twin-screw that crosslinking material and recycling POM, inorganic filler etc. are put into big L/D ratio again after 10~50 μm
Shear-mixed in extruder can also be improved its tensile property while improving and recycling POM impact property；It realizes to recycling
POM material carries out the effect of activeness and quietness simultaneously.Introducing simultaneously containing L-POSS structure crosslinking agent also has one to process
Efficient crosslinked action is played in fixed help.
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 (6)
1. a kind of isomerism modified polyacetal of crosslinking agent containing L-POSS, which is characterized in that the L-POSS crosslinking agent is to adopt
The method reacted with L-POSS with silane compound, product are the derivatives of silane；Its structure are as follows:
；
Isomerism modified polyacetal is based on mass weight part, component are as follows:
100 parts of polyformaldehyde of recycling；
10~30 parts of toughener；
10~30 parts of crosslinking masterbatch；
10~20 parts of inorganic filler；
3~20 parts of heat stabilizer；
The crosslinking masterbatch are made of A material B material and production three step part of aqua；
A expects composition: polyformaldehyde
L-POSS crosslinking agent
Initiator, the initiator are cumyl peroxide DCP
B expects composition: polyformaldehyde
Catalyst, the catalyst are dibutyl tin dilaurate
Antioxidant, the antioxidant are antioxidant 1010
Produce aqua composition: acid and metal oxide；Producing the acid in aqua is at least one of stearic acid, inorganic acid；Metal oxygen
Compound is at least one of zinc oxide, tin oxide；
The L-POSS crosslinking agent includes two stages, is to form raw material first, and silane generates followed by under catalytic action
Active site prepares crosslinking agent containing L-POSS to introduce L-POSS formation chemical reaction.
2. one kind isomerism modified polyacetal of crosslinking agent containing L-POSS according to claim 1, which is characterized in that institute
Stating toughener is at least one of POM/POE, POM/EVA.
3. one kind isomerism modified polyacetal of crosslinking agent containing L-POSS according to claim 1, which is characterized in that described
Filler is at least one of calcium carbonate, talcum powder.
4. one kind isomerism modified polyacetal of crosslinking agent containing L-POSS according to claim 1, which is characterized in that described
Heat stabilizer is triphenyl phosphite.
5. a kind of preparation method of the isomerism of crosslinking agent containing L-POSS modified polyacetal according to claim 1, special
Sign is, the described method comprises the following steps:
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
0.5 part of production aqua mixing is uniformly mixed and is put into double screw extruder extruding pelletization formation crosslinking masterbatch, and the production aqua is 1:
1 stearic acid and the mixture of zinc oxide；
B, by A walk in crosslinking masterbatch be first put into Universalpulverizer and place into planetary ball mill and grind until crosslinking masterbatch
Until partial size reaches 10~50 μm；
C, polyformaldehyde material will be recycled forced air drying 6~8 hours under the conditions of 80 DEG C, it is by weight ratio that crosslinking masterbatch, heat is steady
Determine agent, recycling polyformaldehyde, 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, in the molten state using the Strong shear power of twin-screw by the control of the average grain diameters of crosslinking masterbatch 10~
50 μm, while crosslinking masterbatch being uniformly mixed with heat stabilizer, recycling polyformaldehyde and inorganic filler, above-mentioned mixture is squeezed out
Granulation obtains the isomerism modified polyacetal of crosslinking agent containing L-POSS.
6. one kind isomerism modified polyacetal preparation method of crosslinking agent containing L-POSS according to claim 5, feature
It is, the extruder temperature of the double screw extruder controls between 160 DEG C -180 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5623030A (en) * | 1994-12-01 | 1997-04-22 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Curable composition and process for producing molded articles using the same |
| CN1796441A (en) * | 2004-12-30 | 2006-07-05 | 中国科学院化学研究所 | Trapezoidal organic poly sesquisiloxane and preparation method |
| CN103657456A (en) * | 2013-12-18 | 2014-03-26 | 北京工商大学 | Preparation method of ethanol-permselective POSS (polyhedral oligomeric silsesquioxanes)/silicone rubber composite membrane |
| CN104903404A (en) * | 2013-01-09 | 2015-09-09 | 株式会社大赛璐 | Curable resin composition, and cured product of same |
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- 2016-12-27 CN CN201611223474.8A patent/CN106589786B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5623030A (en) * | 1994-12-01 | 1997-04-22 | Kanegafuchi Kagaku Kogyo Kabushiki Kaisha | Curable composition and process for producing molded articles using the same |
| CN1796441A (en) * | 2004-12-30 | 2006-07-05 | 中国科学院化学研究所 | Trapezoidal organic poly sesquisiloxane and preparation method |
| CN104903404A (en) * | 2013-01-09 | 2015-09-09 | 株式会社大赛璐 | Curable resin composition, and cured product of same |
| CN103657456A (en) * | 2013-12-18 | 2014-03-26 | 北京工商大学 | Preparation method of ethanol-permselective POSS (polyhedral oligomeric silsesquioxanes)/silicone rubber composite membrane |
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