CN105778441A - Heat-preservation pbt material and preparing method thereof - Google Patents
Heat-preservation pbt material and preparing method thereof Download PDFInfo
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- CN105778441A CN105778441A CN201610231209.8A CN201610231209A CN105778441A CN 105778441 A CN105778441 A CN 105778441A CN 201610231209 A CN201610231209 A CN 201610231209A CN 105778441 A CN105778441 A CN 105778441A
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- 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
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Abstract
The invention discloses a heat-preservation pbt material.The heat-preservation pbt material is prepared from, by weight, 3-4 parts of scolecite, 3-5 parts of an alkyl ketene dimer, 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, 1-2 parts of fatty alcohol polyoxyethylen ether, 10-14 parts of dimethyl isophthalate, 2-3 parts of ammonium aluminum sulfate, 2-3 parts of tert-butyl hydroquine, 1-2 parts of borax, 2-4 parts of trichloroiminocyanuric acid and 1-2 parts of polystyrene.According to the heat-preservation pbt material, scolecite is added, micropores can be formed in the material, and thus very good heat preservation and heat insulation effects are achieved.
Description
Technical field
The present invention relates to field of material technology, particularly relate to a kind of 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 insulation pbt material and preparation method thereof.
The present invention is achieved by the following technical solutions:
One is incubated pbt material, and it is made up of the raw material of following weight parts:
Scolecite 3-4, alkyl ketene dimer 3-5, caprolactam 70-80, attapulgite 10-13, zinc acetate 1-1.4, γ-ammonia
Propyl-triethoxysilicane 2-3, ethanedioic acid 18-20, polybutylene terephthalate (PBT) 300-370, fatty alcohol-polyoxyethylene ether
1-2, dimethyl isophthalate 10-14, Burnt ammonium alum 2-3, the tert-butyl group are to biphenol 2-3, Borax 1-2, sym-closene
2-4, polystyrene 1-2.
The preparation method of a kind of described insulation pbt material, comprises the following steps:
(1) above-mentioned Borax is joined in the deionized water of its weight 10-13 times, stir, add scolecite, at 80-90
At DEG C, insulated and stirred is done to water, calcines 1-2 hour at 600-700 DEG C, and cooling obtains modified zeolite；
(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 washed 3-4 time after filtration, is dried at 80-90 DEG C, mixes with above-mentioned modified zeolite
Close, wear into fine powder, obtain multiplicity reactivation powder；
(3) take the 16-20% of above-mentioned ethanedioic acid weight, join in the dehydrated alcohol of its weight 25-30 times, stir；
(4) above-mentioned zinc acetate is joined in its weight 70-80 times, 46-50% ethanol solution, add above-mentioned multiplicity reactivation
Powder, ultrasonic 10-20 minute, drips the ethanol solution of above-mentioned ethanedioic acid, magnetic agitation 3-4 minute after dropping, and sucking filtration will be taken out
Product after filter is dried 3-5 hour at 110-116 DEG C, sends in Muffle furnace, calcines 1.7-2 hour at 600-640 DEG C, cold
But, zinc oxide load powder is obtained；
(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, adds the above-mentioned tert-butyl group to biphenol, stirring mixing
20-30 minute, sucking filtration, precipitation is washed 2-3 time, is vacuum dried 20-30 minute at 50-60 DEG C, obtains amino modified zinc oxide
Load powder；
(6) 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
React 3-4 hour, slowly cool to room temperature, be filtered to remove filtrate, precipitation is dried, grinds to form fine powder, obtain pre-polymerization modified oxidized
Zinc load powder；
(7) above-mentioned Burnt ammonium alum is joined in the deionized water of its weight 4-7 times, stir；
(8) 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 Burnt ammonium alum aqueous solution, stir, discharging cools down, and is vacuum dried 1-2 hour, obtains polymerization and change at 50-60 DEG C
Property zinc oxide load powder；
(9) above-mentioned polymeric modification zinc oxide load powder is mixed with polystyrene, preheats 4-10 minute at 100-110 DEG C,
Mixing with remaining each raw material, high-speed stirred is uniform, sends into double screw extruder extrusion, through tie rod, cooling, pelletizing, is dried place
Reason, 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 material of the present invention adds scolecite, can form micropore in the inside of material, serves good heat insulating effect.
Detailed description of the invention
One is incubated pbt material, and it is made up of the raw material of following weight parts:
Scolecite 3, alkyl ketene dimer 3, caprolactam 70, attapulgite 10, zinc acetate 1, γ aminopropyl-triethoxy silicon
Alkane 2, ethanedioic acid 18, polybutylene terephthalate (PBT) 300, fatty alcohol-polyoxyethylene ether 1, dimethyl isophthalate 10, sulfur
Acid aluminum ammonium 2, the tert-butyl group are to biphenol 2, Borax 1, sym-closene 2, polystyrene 1.
The preparation method of a kind of described insulation pbt material, comprises the following steps:
(1) above-mentioned Borax is joined in the deionized water of its weight 10 times, stir, add scolecite, protect at 80 DEG C
Temperature stirring is done to water, calcines 1 hour at 600 DEG C, and cooling obtains modified zeolite；
(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 washed 3 times after filtration, is dried, mixes with above-mentioned modified zeolite, wear into fine powder, obtain compound at 80 DEG C
Activation powder；
(3) take the 16% of above-mentioned ethanedioic acid weight, join in the dehydrated alcohol of its weight 25 times, stir；
(4) above-mentioned zinc acetate is joined in its weight 70 times, the ethanol solution of 46%, add above-mentioned multiplicity reactivation powder, ultrasonic
10 minutes, drip the ethanol solution of above-mentioned ethanedioic acid, magnetic agitation 3 minutes after dropping, sucking filtration, the product after sucking filtration is existed
It is dried 3 hours at 110 DEG C, sends 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, adds the above-mentioned tert-butyl group and biphenol, stirring are mixed 20 minutes, taken out
Filter, washes precipitation 2 times, is vacuum dried 20 minutes at 50 DEG C, obtains amino modified zinc oxide load powder；
(6) 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 is slow
Slow cool down, to room temperature, is filtered to remove filtrate, precipitation is dried, grinds to form fine powder, obtains pre-polymerization modified zinc oxide load powder；
(7) above-mentioned Burnt ammonium alum is joined in the deionized water of its weight 4 times, stir；
(8) 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 sulfur
Acid aluminum aqueous ammonium, stirs, and discharging cools down, and is vacuum dried 1 hour at 50 DEG C, obtains polymeric modification zinc oxide load powder
Material；
(9) above-mentioned polymeric modification zinc oxide load powder is mixed with polystyrene, preheat 4 minutes at 100 DEG C, each with residue
Raw material mixes, and high-speed stirred is uniform, sends into double screw extruder extrusion, through tie rod, cooling, pelletizing, dried, to obtain final product.
Performance test:
Hot strength is 95.1MPa；
Notch impact strength (KJ/m2) 10.08；
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 insulation pbt material, it is characterised in that it is made up of the raw material of following weight parts:
Scolecite 3-4, alkyl ketene dimer 3-5, caprolactam 70-80, attapulgite 10-13, zinc acetate 1-1.4, γ-ammonia
Propyl-triethoxysilicane 2-3, ethanedioic acid 18-20, polybutylene terephthalate (PBT) 300-370, fatty alcohol-polyoxyethylene ether
1-2, dimethyl isophthalate 10-14, Burnt ammonium alum 2-3, the tert-butyl group are to biphenol 2-3, Borax 1-2, sym-closene
2-4, polystyrene 1-2.
2. the preparation method of an insulation pbt material as claimed in claim 1, it is characterised in that comprise the following steps:
(1) above-mentioned Borax is joined in the deionized water of its weight 10-13 times, stir, add scolecite, at 80-90
At DEG C, insulated and stirred is done to water, calcines 1-2 hour at 600-700 DEG C, and cooling obtains modified zeolite；
(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 washed 3-4 time after filtration, is dried at 80-90 DEG C, mixes with above-mentioned modified zeolite
Close, wear into fine powder, obtain multiplicity reactivation powder；
(3) take the 16-20% of above-mentioned ethanedioic acid weight, join in the dehydrated alcohol of its weight 25-30 times, stir；
(4) above-mentioned zinc acetate is joined in its weight 70-80 times, 46-50% ethanol solution, add above-mentioned multiplicity reactivation
Powder, ultrasonic 10-20 minute, drips the ethanol solution of above-mentioned ethanedioic acid, magnetic agitation 3-4 minute after dropping, and sucking filtration will be taken out
Product after filter is dried 3-5 hour at 110-116 DEG C, sends in Muffle furnace, calcines 1.7-2 hour at 600-640 DEG C, cold
But, zinc oxide load powder is obtained；
(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, adds the above-mentioned tert-butyl group to biphenol, stirring mixing
20-30 minute, sucking filtration, precipitation is washed 2-3 time, is vacuum dried 20-30 minute at 50-60 DEG C, obtains amino modified zinc oxide
Load powder；
(6) 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
React 3-4 hour, slowly cool to room temperature, be filtered to remove filtrate, precipitation is dried, grinds to form fine powder, obtain pre-polymerization modified oxidized
Zinc load powder；
(7) above-mentioned Burnt ammonium alum is joined in the deionized water of its weight 4-7 times, stir；
(8) 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 Burnt ammonium alum aqueous solution, stir, discharging cools down, and is vacuum dried 1-2 hour, obtains polymerization and change at 50-60 DEG C
Property zinc oxide load powder；
(9) above-mentioned polymeric modification zinc oxide load powder is mixed with polystyrene, preheats 4-10 minute at 100-110 DEG C,
Mixing with remaining each raw material, high-speed stirred is uniform, sends into double screw extruder extrusion, through tie rod, cooling, pelletizing, is dried place
Reason, to obtain final product.
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Cited By (2)
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| CN108745319A (en) * | 2018-06-27 | 2018-11-06 | 邱小艳 | A kind of antibacterial sorbing material and preparation method thereof |
| CN115152387A (en) * | 2022-07-07 | 2022-10-11 | 山东实力农业股份有限公司 | Fertilizing method for saving fertilizer and increasing yield of fruit and vegetable crops |
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| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745319A (en) * | 2018-06-27 | 2018-11-06 | 邱小艳 | A kind of antibacterial sorbing material and preparation method thereof |
| CN115152387A (en) * | 2022-07-07 | 2022-10-11 | 山东实力农业股份有限公司 | Fertilizing method for saving fertilizer and increasing yield of fruit and vegetable crops |
| CN115152387B (en) * | 2022-07-07 | 2023-03-28 | 山东实力农业股份有限公司 | Fertilizing method for saving fertilizer and increasing yield of fruit and vegetable crops |
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Application publication date: 20160720 |