CN105838042A - Insulating pbt material used for electronic equipment and preparation method thereof - Google Patents
Insulating pbt material used for electronic equipment and preparation method thereof Download PDFInfo
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- CN105838042A CN105838042A CN201610230063.5A CN201610230063A CN105838042A CN 105838042 A CN105838042 A CN 105838042A CN 201610230063 A CN201610230063 A CN 201610230063A CN 105838042 A CN105838042 A CN 105838042A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses an insulating pbt material used for electronic equipment. The material comprises: by weight, 3-5 parts of polyimide, 6-8 parts of chlorinated paraffin, 0.4-1 part of dibasic lead phosphite, 70-80 parts of caprolactam, 10-13 parts of attapulgite, 1-1.4 parts of zinc acetate, 2-3 parts of gamma-aminopropyltriethoxysilane, 18-20 parts of oxalic acid, 300-370 parts of polybutylene terephthalate, 4-5 parts of aluminium-magnesium silicate, 2-3 parts of 2-bromo-4-methylphenol, 7-10 parts of trimellitate, 1-2 parts of fatty acid diethanol amide, 3-5 parts of polytetramethylene ether glycol, and 4.5-6 parts of hydroxystearic acid. The pbt material has good insulating property, and is widely used for electronic equipment.
Description
Technical field
The present invention relates to field of material technology, particularly relate to a kind of electronic equipment insulation pbt material and preparation method thereof.
Background technology
ZnO was widely studied in the last few years as a kind of photocatalyst-type anti-biotic agent, and it generates strong oxygen under photocatalysis
The active function groups of the property changed kills antibacterial.It has nontoxic, nonirritant, good stability, and difficult decomposition under high temperature, timeliness is long
For a long time, cheap, the advantage such as aboundresources, have broad application prospects；
The common carrier being presently used for loaded optic catalyst mainly has CNT (CNTs) and activated carbon, mesoporous material, Linesless charcoal
Black and zeolites etc. can obtain the nano-particle of size uniform by load, in turn ensure that functional nano-composites simultaneously
High stability.Nano-photocatalyst/porous mineral compound system, i.e. assembles Nano semiconductor photocatalyst or loads to mineral
In the hole of material or on surface, not only solve the agglomeration traits of nano-photocatalyst granule, reduce its consumption, also simultaneously
Utilize the high-specific surface area of porous mineral, strong characterization of adsorption to realize in water or the targeting enrichment of pollutants in air, urged by light
Agent is more effectively carried out light degradation；
Therefore nano-photocatalyst/porous mineral compound system can improve the disposal efficiency of catalysis material, reduces again
Its consumption and preparation cost, accomplished to have complementary advantages, and this support type composite had both remained the character of nano-particle itself,
Closed by the interface between nano-particle and matrix simultaneously, some new assembly effects can be produced again, make whole complex
System shows as distinctive synergistic enhancing effect, thus significantly improves the functional characteristic of material, but presently used carrier is the most all deposited
In the shortcoming such as expensive, surface activity point is low, therefore, research and develop a kind of novel carrier material and be the most increasingly subject to
The attention of scholars, find a kind of cheap, surface activity is high and the novel carriers of good stability seems the most necessary；
Polyamide due to its good mechanical property, barrier property, anti-wear performance, acid-proof alkaline and good processing characteristics,
Increasingly become indispensable material as engineering plastics and non-fibre material, its application relate to auto parts and components, cord fabric,
The fields such as tyre equatorial, electronic apparatus, household supplies, consumption becomes kinds most in polyamide product.But applying
Cheng Zhong, the polar group of polyamide 6 material makes it be prone to absorb moisture, causes dry state and low temperature impact strength is low, product
Easily there is the phenomenon such as plastic deformation, serious wear in product poor stability, friction, additionally, uses as mine engineering plastics, do not possess
Antistatic property, easily produces gas explosion etc., thus affects the stability of its product size, antiwear and friction reduction property and electrically
Can, which has limited its range of application；
Attapulgite, as a kind of natural nanometer fibrous clay mineral, has 2:1 type layer chain structure, in its crystal structure
There is a large amount of pore passage structure, and have that specific surface area is big, surface activity site is many, energy of adsorption
By force, excellent biocompatibility and the chemically and thermally feature such as stability, be a kind of economical and practical carrier material, giving birth to
The aspects such as thing, environment, new material have broad application prospects；Therefore it is an object of the invention to nano-photocatalyst with recessed
Convex rod stone is effectively combined, and is the most effectively distributed in polyamide, prepares a kind of novel composite.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of electronic equipment with insulation pbt material and
Its preparation method.
The present invention is achieved by the following technical solutions:
A kind of electronic equipment insulation pbt material, it is made up of the raw material of following weight parts:
Polyimides 3-5, chlorinated paraffin 6-8, dibasic lead phosphite 0.4-1, caprolactam 70-80, attapulgite 10-13,
Zinc acetate 1-1.4, gamma-aminopropyl-triethoxy-silane 2-3, ethanedioic acid 18-20, polybutylene terephthalate (PBT) 300-370,
Aluminium-magnesium silicate 4-5,2-bromo-4-methylphenol 2-3, trimellitate 7-10, fatty diglycollic amide 1-2, PolyTHF
Ether glycol 3-5, hydroxy stearic acid 4.5-6.
The preparation method of a kind of described electronic equipment insulation pbt material, comprises the following steps:
(1) above-mentioned aluminium-magnesium silicate is joined in the deionized water of its weight 20-34 times, insulated and stirred 10-20 at 60-70 DEG C
Minute, adding dibasic lead phosphite, stirring, to room temperature, obtains dispersion liquid；
(2) above-mentioned attapulgite is calcined 1-2 hour at 300-350 DEG C, join acidifying 3-5 in the hydrochloric acid of 3-5mol/l little
Time, souring temperature is 20-35 DEG C, precipitation is joined in above-mentioned dispersion liquid after filtration, does to water 80-90 DEG C of stirring, wears into
Fine powder, obtains activation attapulgite powder；
(3) take the 16-20% of above-mentioned ethanedioic acid weight, mix with PTMG, join compound weight 13-16
In dehydrated alcohol again, stir, obtain compound alcoholic solution；
(4) above-mentioned zinc acetate is joined in its weight 70-80 times, 46-50% ethanol solution, add above-mentioned activation concavo-convex
Rod soil powder, ultrasonic 10-20 minute, adds above-mentioned compound alcoholic solution, magnetic agitation 3-4 minute, sucking filtration, is existed by the product after sucking filtration
It is dried 3-5 hour at 110-116 DEG C, sends in Muffle furnace, calcine 1.7-2 hour at 600-640 DEG C, cooling, obtain zinc oxide
Load powder；
(5) above-mentioned zinc oxide load powder is joined in the dehydrated alcohol of its weight 60-70 times, add γ-aminopropyl three second
TMOS, rises high-temperature and is 80-90 DEG C, insulated and stirred 1.7-2 hour, and precipitation is washed 2-3 time, at 50-60 DEG C by sucking filtration
It is vacuum dried 20-30 minute, obtains amino modified zinc oxide load powder；
(6) above-mentioned 2-bromo-4-methylphenol is joined in the dehydrated alcohol of its weight 5-7 times, stir, add hydroxyl hard
Fat acid, insulated and stirred 30-40 minute at 70-80 DEG C, obtain premix material；
(7) take the 10-16% of above-mentioned caprolactam weight, the 20-30% of residue ethanedioic acid weight, load with amino modified zinc oxide
Powder mixes, and adds the distilled water of compound weight 8-10 times, is sent in reactor, rises high-temperature and is 190-200 DEG C, insulation
Reacting 3-4 hour, add above-mentioned premix material, stirring, to room temperature, is filtered to remove filtrate, precipitation is dried, grinds to form fine powder, obtain pre-
Poly-modified zinc oxide load powder；
(8) by above-mentioned polyimides, fatty diglycollic amide mixing, the deionized water of compound weight 10-15 times is joined
In, stir, obtain amide solution；
(9) above-mentioned pre-polymerization modified zinc oxide load powder is mixed with remaining caprolactam, add compound weight 4-7 times
Distilled water, is sent in reactor, rises high-temperature and is 200-230 DEG C, adds remaining ethanedioic acid, insulation reaction 3-3.5 hour,
Adding above-mentioned amide solution, stirring mixing 30-40 minute, discharging cools down, and is vacuum dried 1-2 hour, obtains polymerization at 50-60 DEG C
Modified zinc oxide load powder；
(10) being mixed with remaining each raw material by above-mentioned polymeric modification zinc oxide load powder, high-speed stirred is uniform, sends into twin screw
Extruder is extruded, and through tie rod, cooling, pelletizing, dried, to obtain final product.
The invention have the advantage that first attapulgite is calcined and acidification by the present invention, attapulgite can be increased
The silicone hydroxyl group on stone surface, gives attapulgite surface more negative charge, increases its absorbability to metal cation,
By the attapulgite in-situ precipitate of absorption Zn2+ ion is obtained presoma, obtain ZnO/ attapulgite composite wood by calcination
Material, with attapulgite as carrier, can improve the dispersibility of ZnO nanoparticle, it is thus achieved that have the composite of high antibacterial activity,
Attapulgite as layer chain silicate clay, the advantages such as tool specific surface area is big and lateral reactivity site is many, load nano-ZnO
After, considerably increasing the contact area of ZnO and microorganism, high adsorption activity based on attapulgite, antibacterial can be by antibacterial material
Material absorption is forming enrichment about so that ZnO nano granule is easier to directly contact with antibacterial, thus plays its antibacterial characteristics
Cause inactivation of bacteria, then this composite is participated in the pre-polymerization process of caprolactam, utilize caprolactam open-loop products
Aminocaproic acid reacts with the amino of composite material surface, makes composite material surface be grafted a certain amount of polyamide prepolymer aggressiveness, at it
Surface forms one layer of strong boundary layer；Participate in the polymerization process of polyamide the most again, due to the polyamides of composite material surface grafting
Amine performed polymer can participate in the ring-opening polymerisation of caprolactam, therefore, it is possible to form " micronetwork " structure with masterbatch as core, enters
And add intensity and the toughness of polyamide substrate material, and, beneficially composite is in the dispersion of polyamide substrate material；
The pbt material of the present invention has good insulating properties, is widely used in electronic equipment.
Detailed description of the invention
A kind of electronic equipment insulation pbt material, it is made up of the raw material of following weight parts:
Polyimides 3, chlorinated paraffin 6, dibasic lead phosphite 0.4, caprolactam 70, attapulgite 10, zinc acetate 1, γ ammonia
Propyl-triethoxysilicane 2, ethanedioic acid 18, polybutylene terephthalate (PBT) 300, aluminium-magnesium silicate 4,2 bromomethyl phenol 2, partially
Benzenetricarboxylic acid ester 7, fatty diglycollic amide 1, PTMG 3, hydroxy stearic acid 4.5.
The preparation method of a kind of described electronic equipment insulation pbt material, comprises the following steps:
(1) above-mentioned aluminium-magnesium silicate is joined in the deionized water of its weight 20 times, insulated and stirred 10 minutes at 60 DEG C, add
Dibasic lead phosphite, stirring, to room temperature, obtains dispersion liquid；
(2) above-mentioned attapulgite is calcined 1 hour at 300 DEG C, join in the hydrochloric acid of 3mol/l and be acidified 3 hours, acidifying temperature
Degree is 20 DEG C, precipitation is joined in above-mentioned dispersion liquid after filtration, does to water 80 DEG C of stirrings, wears into fine powder, must activate concavo-convex
Rod soil powder；
(3) take the 16% of above-mentioned ethanedioic acid weight, mix with PTMG, join the nothing of compound weight 13 times
In water-ethanol, stir, obtain compound alcoholic solution；
(4) above-mentioned zinc acetate is joined in its weight 70 times, the ethanol solution of 46%, adds above-mentioned activation attapulgite powder,
Ultrasonic 10 minutes, add above-mentioned compound alcoholic solution, magnetic agitation 3 minutes, sucking filtration, the product after sucking filtration is dried at 110 DEG C 3
Hour, send in Muffle furnace, calcine 1.7 hours at 600 DEG C, cooling, obtain zinc oxide load powder；
(5) above-mentioned zinc oxide load powder is joined in the dehydrated alcohol of its weight 60 times, add γ aminopropyl-triethoxy
Silane, rising high-temperature is 80 DEG C, insulated and stirred 1.7 hours, and precipitation is washed 2 times by sucking filtration, is vacuum dried 20 points at 50 DEG C
Clock, obtains amino modified zinc oxide load powder；
(6) above-mentioned 2 bromomethyl phenol are joined in the dehydrated alcohol of its weight 5 times, stir, add hydroxy stearic acid,
At 70 DEG C, insulated and stirred 30 minutes, obtain premix material；
(7) take the 10% of above-mentioned caprolactam weight, the 20% of residue ethanedioic acid weight, mix with amino modified zinc oxide load powder
Closing, add the distilled water of compound weight 8 times, be sent in reactor, rising high-temperature is 190 DEG C, and insulation reaction 3 hours adds
Entering above-mentioned premix material, stirring, to room temperature, is filtered to remove filtrate, precipitation is dried, grinds to form fine powder, obtains pre-polymerization modified zinc oxide and bears
Carry powder；
(8) by above-mentioned polyimides, fatty diglycollic amide mixing, join in the deionized water of compound weight 10 times,
Stir, obtain amide solution；
(9) above-mentioned pre-polymerization modified zinc oxide load powder is mixed with remaining caprolactam, add the steaming of compound weight 4 times
Distilled water, is sent in reactor, and rising high-temperature is 200 DEG C, adds remaining ethanedioic acid, insulation reaction 3 hours, adds above-mentioned acyl
Amine aqueous solution, stirring mixing 30 minutes, discharging cools down, and is vacuum dried 1 hour at 50 DEG C, obtains polymeric modification zinc oxide load powder
Material；
(10) being mixed with remaining each raw material by above-mentioned polymeric modification zinc oxide load powder, high-speed stirred is uniform, sends into twin screw
Extruder is extruded, and through tie rod, cooling, pelletizing, dried, to obtain final product.
Performance test:
Hot strength is 96MPa；
Notch impact strength (KJ/m2) 10.10；
Vertical combustion (1.6mm) FV-O；
The zinc oxide load powder wherein prepared is O.lg/L to colibacillary minimum inhibitory concentration.
Claims (2)
1. an electronic equipment insulation pbt material, it is characterised in that it is made up of the raw material of following weight parts:
Polyimides 3-5, chlorinated paraffin 6-8, dibasic lead phosphite 0.4-1, caprolactam 70-80, attapulgite 10-13,
Zinc acetate 1-1.4, gamma-aminopropyl-triethoxy-silane 2-3, ethanedioic acid 18-20, polybutylene terephthalate (PBT) 300-370,
Aluminium-magnesium silicate 4-5,2-bromo-4-methylphenol 2-3, trimellitate 7-10, fatty diglycollic amide 1-2, PolyTHF
Ether glycol 3-5, hydroxy stearic acid 4.5-6.
2. the preparation method of an electronic equipment as claimed in claim 1 insulation pbt material, it is characterised in that include with
Lower step:
(1) above-mentioned aluminium-magnesium silicate is joined in the deionized water of its weight 20-34 times, insulated and stirred 10-20 at 60-70 DEG C
Minute, adding dibasic lead phosphite, stirring, to room temperature, obtains dispersion liquid；
(2) above-mentioned attapulgite is calcined 1-2 hour at 300-350 DEG C, join acidifying 3-5 in the hydrochloric acid of 3-5mol/l little
Time, souring temperature is 20-35 DEG C, precipitation is joined in above-mentioned dispersion liquid after filtration, does to water 80-90 DEG C of stirring, wears into
Fine powder, obtains activation attapulgite powder；
(3) take the 16-20% of above-mentioned ethanedioic acid weight, mix with PTMG, join compound weight 13-16
In dehydrated alcohol again, stir, obtain compound alcoholic solution；
(4) above-mentioned zinc acetate is joined in its weight 70-80 times, 46-50% ethanol solution, add above-mentioned activation concavo-convex
Rod soil powder, ultrasonic 10-20 minute, adds above-mentioned compound alcoholic solution, magnetic agitation 3-4 minute, sucking filtration, is existed by the product after sucking filtration
It is dried 3-5 hour at 110-116 DEG C, sends in Muffle furnace, calcine 1.7-2 hour at 600-640 DEG C, cooling, obtain zinc oxide
Load powder；
(5) above-mentioned zinc oxide load powder is joined in the dehydrated alcohol of its weight 60-70 times, add γ-aminopropyl three second
TMOS, rises high-temperature and is 80-90 DEG C, insulated and stirred 1.7-2 hour, and precipitation is washed 2-3 time, at 50-60 DEG C by sucking filtration
It is vacuum dried 20-30 minute, obtains amino modified zinc oxide load powder；
(6) above-mentioned 2-bromo-4-methylphenol is joined in the dehydrated alcohol of its weight 5-7 times, stir, add hydroxyl hard
Fat acid, insulated and stirred 30-40 minute at 70-80 DEG C, obtain premix material；
(7) take the 10-16% of above-mentioned caprolactam weight, the 20-30% of residue ethanedioic acid weight, load with amino modified zinc oxide
Powder mixes, and adds the distilled water of compound weight 8-10 times, is sent in reactor, rises high-temperature and is 190-200 DEG C, insulation
Reacting 3-4 hour, add above-mentioned premix material, stirring, to room temperature, is filtered to remove filtrate, precipitation is dried, grinds to form fine powder, obtain pre-
Poly-modified zinc oxide load powder；
(8) by above-mentioned polyimides, fatty diglycollic amide mixing, the deionized water of compound weight 10-15 times is joined
In, stir, obtain amide solution；
(9) above-mentioned pre-polymerization modified zinc oxide load powder is mixed with remaining caprolactam, add compound weight 4-7 times
Distilled water, is sent in reactor, rises high-temperature and is 200-230 DEG C, adds remaining ethanedioic acid, insulation reaction 3-3.5 hour,
Adding above-mentioned amide solution, stirring mixing 30-40 minute, discharging cools down, and is vacuum dried 1-2 hour, obtains polymerization at 50-60 DEG C
Modified zinc oxide load powder；
(10) being mixed with remaining each raw material by above-mentioned polymeric modification zinc oxide load powder, high-speed stirred is uniform, sends into twin screw
Extruder is extruded, and through tie rod, cooling, pelletizing, dried, to obtain final product.
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| CN201610230063.5A CN105838042A (en) | 2016-04-14 | 2016-04-14 | Insulating pbt material used for electronic equipment and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444717A (en) * | 2008-12-05 | 2009-06-03 | 江苏工业学院 | Method for preparing concavo-convex rod soil/zinc oxide nanometer composite material |
| CN102952327A (en) * | 2011-08-25 | 2013-03-06 | 上海杰事杰新材料(集团)股份有限公司 | Resin composite material and its preparation method and use |
| CN104448299A (en) * | 2013-09-24 | 2015-03-25 | 骏马化纤股份有限公司 | In-situ-polymerized halogen-free flame-retardant nylon 6/attapulgite nano composite material and preparation method thereof |
-
2016
- 2016-04-14 CN CN201610230063.5A patent/CN105838042A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444717A (en) * | 2008-12-05 | 2009-06-03 | 江苏工业学院 | Method for preparing concavo-convex rod soil/zinc oxide nanometer composite material |
| CN102952327A (en) * | 2011-08-25 | 2013-03-06 | 上海杰事杰新材料(集团)股份有限公司 | Resin composite material and its preparation method and use |
| CN104448299A (en) * | 2013-09-24 | 2015-03-25 | 骏马化纤股份有限公司 | In-situ-polymerized halogen-free flame-retardant nylon 6/attapulgite nano composite material and preparation method thereof |
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