CN106893272A - A kind of magnesium hydroxide crystal whisker is modified the preparation method and products thereof of polyadipate/butylene terephthalate composite - Google Patents
A kind of magnesium hydroxide crystal whisker is modified the preparation method and products thereof of polyadipate/butylene terephthalate composite Download PDFInfo
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- CN106893272A CN106893272A CN201510973456.0A CN201510973456A CN106893272A CN 106893272 A CN106893272 A CN 106893272A CN 201510973456 A CN201510973456 A CN 201510973456A CN 106893272 A CN106893272 A CN 106893272A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1535—Five-membered rings
- C08K5/1539—Cyclic anhydrides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- 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
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Abstract
The invention provides a kind of preparation method of the modified polyadipate/butylene terephthalate composite of magnesium hydroxide crystal whisker, comprise the following steps：Magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse obtains finely dispersed suspension；Coupling agent is dissolved in absolute ethyl alcohol, coupling agent solution is obtained；The finely dispersed suspension and the coupling agent solution are well mixed again, are flowed back；Room temperature, centrifugation are cooled to, then are dried in 80 DEG C of vacuum drying ovens, modified magnesium hydroxide crystal whisker is obtained；The modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer are placed in high speed blender together with polyadipate/butylene terephthalate and are mixed, granulated, target product is obtained.Significantly improved using the tensile strength of the modified polyadipate/butylene terephthalate of magnesium hydroxide crystal whisker obtained in preparation method of the present invention, extend its application field.
Description
Technical field
The present invention relates to the method for modifying of composite, more particularly to a kind of modified polyadipate of magnesium hydroxide crystal whisker
The preparation method of/butylene terephthalate composite, and magnesium hydroxide obtained in the preparation method is brilliant
Must modified polyadipate/butylene terephthalate composite.
Background technology
Polyadipate/butylene terephthalate is that one kind has aliphatic polyester excellent biodegradability energy and virtue concurrently
The aliphatic/aromatic copolyester of fragrant adoption ester excellent mechanical performance, the copolyesters has can be with common plasticses phase
The good physical and processing characteristics for matching in excellence or beauty.It is similar with commodity polymer material, polyadipate/terephthaldehyde
Sour fourth diester can also be processed by means such as injection, extrusion, blowing, molding, casting film-forming and blown films
Prepare.But the tensile strength of polyadipate/butylene terephthalate is less, limits the composite in power
Learn the application in performance requirement field higher.Therefore need to improve polyadipate/butylene terephthalate composite wood
The combination property of material simultaneously reduces production cost, and it is modified.
Magnesium hydroxide crystal whisker is into threadiness, and mono-crystalline structures, 0.5~5 μm of diameter of whiskers is long 200~2000 μm.
During the fiber magnesium hydroxide that activates in the high temperature, red phosphorus, coupling agent are added to polymer according to a certain percentage, add
Plus in the case of a certain amount of red phosphorus, with the increase of fiber magnesium hydroxide addition, oxygen index (OI) gradually increases.By
In poisonous and harmful substance is not produced to environment after magnesium hydroxide crystal whisker decomposition, a certain amount of magnesium hydroxide crystal whisker is added
Flame Retardancy can again improved, and the mechanical performance of material can be improved.
The content of the invention
In order to overcome above-mentioned problems of the prior art, in order to lift polyadipate/terephthalic acid (TPA)
The tensile strength of fourth diester, in order to pass through modified its application field of extension；The first aspect of the present invention, it is intended to carry
For a kind of preparation method of the modified polyadipate/butylene terephthalate composite of magnesium hydroxide crystal whisker.
Above-mentioned preparation method is comprised the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse obtains finely dispersed suspension；In addition,
Coupling agent is dissolved in absolute ethyl alcohol, coupling agent solution is obtained；Again by the finely dispersed suspension and the coupling
Agent solution is well mixed, and in backflow at 80 DEG C；Room temperature, centrifugation are cooled to, then are dried in 80 DEG C of vacuum
Dried in case, modified magnesium hydroxide crystal whisker is obtained；
(2) by the modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/to benzene
Dioctyl phthalate fourth diester is placed in high speed blender is mixed together；
(3) mixture of each reactant being well mixed in step (2) is placed in extruding pelletization in double screw extruder,
Modified polyadipate/butylene terephthalate the composite particles of magnesium hydroxide crystal whisker are obtained；
Wherein, the mass fraction proportioning of each reactant composition is as follows：
Preferably, in above-mentioned preparation method, the equal molecule of number of the polyadipate/butylene terephthalate
Measure is 3.6 × 104。
Preferably, in above-mentioned preparation method, the coupling agent is gamma-aminopropyl-triethoxy-silane (KH550)
Or titanate coupling agent (NZD-201).
Preferably, in above-mentioned preparation method, the antioxidant be selected from it is following any one：Diphenylamines, to benzene
Diamines or EEDQ.
Preferably, in above-mentioned preparation method, the heat stabilizer is maleic anhydride or epoxidized soybean oil.
It is further preferred that in above-mentioned preparation method, ultrasonic disperse duration described in step (1)
It is 10min.
It is further preferred that the duration that flowed back in above-mentioned preparation method, described in step (1) is 3
Hour.
The second aspect of the present invention, there is provided a kind of magnesium hydroxide crystal whisker is modified polyadipate/terephthalic acid (TPA) fourth
Diester composite, it is characterised in that the magnesium hydroxide crystal whisker is modified polyadipate/terephthalic acid (TPA) fourth two
Ester composite is as obtained in above-mentioned preparation method.
Using preparation method of the present invention, the modified polyadipate/terephthalic acid (TPA) of magnesium hydroxide crystal whisker is used
Fourth diester composite, products obtained therefrom is that the modified polyadipate/butylene terephthalate of magnesium hydroxide crystal whisker is multiple
Condensation material.The magnesium hydroxide crystal whisker be modified polyadipate/butylene terephthalate composite stretching it is strong
Degree is significantly improved, and the extension of its application field is realized by being modified.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following implementation
Mode.
A kind of magnesium hydroxide crystal whisker is modified the preparation method of polyadipate/butylene terephthalate composite.
Above-mentioned preparation method is comprised the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse obtains finely dispersed suspension；In addition,
Coupling agent is dissolved in absolute ethyl alcohol, coupling agent solution is obtained；Again by the finely dispersed suspension and the coupling
Agent solution is well mixed, and in backflow at 80 DEG C；Room temperature, centrifugation are cooled to, then are dried in 80 DEG C of vacuum
Dried in case, modified magnesium hydroxide crystal whisker is obtained；
(2) by the modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/to benzene
Dioctyl phthalate fourth diester is placed in high speed blender is mixed together；
(3) mixture of each reactant being well mixed in step (2) is placed in extruding pelletization in double screw extruder,
Modified polyadipate/butylene terephthalate the composite particles of magnesium hydroxide crystal whisker are obtained；
Wherein, the mass fraction proportioning of each reactant composition is as follows：
In a preferred embodiment, in above-mentioned preparation method, the polyadipate/terephthalic acid (TPA) fourth two
The number-average molecular weight of ester is 3.6 × 104。
In a preferred embodiment, in above-mentioned preparation method, the coupling agent is gamma-aminopropyl-triethoxy
Silane (KH550) or titanate coupling agent (NZD-201).
In a preferred embodiment, in above-mentioned preparation method, the antioxidant be selected from it is following any one：
Diphenylamines, p-phenylenediamine or EEDQ.
In a preferred embodiment, in above-mentioned preparation method, the heat stabilizer be maleic anhydride or
Epoxidized soybean oil.
In a further preferred embodiment, in above-mentioned preparation method, ultrasound described in step (1)
Dispersion duration is 10min.
In a further preferred embodiment, in above-mentioned preparation method, flowed back described in step (1)
Duration is 3 hours.
Embodiment 1
Using the modified polyadipate/butylene terephthalate composite of magnesium hydroxide crystal whisker, wherein, it is each anti-
Answer the mass fraction proportioning of thing component as follows：
And reacted according to the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse 10min obtains finely dispersed suspension；
In addition, by coupling agent (pressing the 0.5% of whisker mass fraction) gamma-aminopropyl-triethoxy-silane coupling agent (KH550)
Absolute ethyl alcohol is dissolved in, coupling agent solution is obtained；Unit for uniform suspension is well mixed in 80 DEG C with coupling agent solution again
Lower backflow 3h；Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens, so as to be obtained what is be modified
Magnesium hydroxide crystal whisker.
(2) by above-mentioned modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/right
Terephtha-late is placed in high speed blender is mixed together.
(3) above-mentioned well mixed each reactant is placed in extruding pelletization in double screw extruder, hydroxide is obtained
The whisker modified polyadipate of magnesium/butylene terephthalate composite particles.
(4) above-mentioned composite particles are obtained standard testing batten through injection moulding, it is standby.
Embodiment 2
Using the modified polyadipate/butylene terephthalate composite of magnesium hydroxide crystal whisker, wherein, it is each anti-
Answer the mass fraction proportioning of thing component as follows：
And reacted according to the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse 10min obtains finely dispersed suspension；
In addition, coupling agent (by the 0.5% of whisker mass fraction) titanate coupling agent NZD-201 is dissolved in into anhydrous second
Alcohol, obtains coupling agent solution；Unit for uniform suspension is well mixed in the 3h that flowed back at 80 DEG C with coupling agent solution again；
Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens, so as to modified magnesium hydroxide crystal whisker is obtained.
(2) by above-mentioned modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/right
Terephtha-late is placed in high speed blender is mixed together.
(3) above-mentioned well mixed each reactant is placed in extruding pelletization in double screw extruder, hydroxide is obtained
The whisker modified polyadipate of magnesium/butylene terephthalate composite particles.
(4) above-mentioned composite particles are obtained standard testing batten through injection moulding, it is standby.
Embodiment 3
Using the modified polyadipate/butylene terephthalate composite of magnesium hydroxide crystal whisker, wherein, it is each anti-
Answer the mass fraction proportioning of thing component as follows：
And reacted according to the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse 10min obtains finely dispersed suspension；
In addition, by coupling agent (pressing the 0.5% of whisker mass fraction) gamma-aminopropyl-triethoxy-silane coupling agent (KH550)
Absolute ethyl alcohol is dissolved in, coupling agent solution is obtained；Unit for uniform suspension is well mixed in 80 DEG C with coupling agent solution again
Lower backflow 3h；Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens, so as to be obtained what is be modified
Magnesium hydroxide crystal whisker.
(2) by above-mentioned modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/right
Terephtha-late is placed in high speed blender is mixed together.
(3) above-mentioned well mixed each reactant is placed in extruding pelletization in double screw extruder, hydroxide is obtained
The whisker modified polyadipate of magnesium/butylene terephthalate composite particles.
(4) above-mentioned composite particles are obtained standard testing batten through injection moulding, it is standby.
Embodiment 4
Using the modified polyadipate/butylene terephthalate composite of magnesium hydroxide crystal whisker, wherein, it is each anti-
Answer the mass fraction proportioning of thing component as follows：
And reacted according to the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse 10min obtains finely dispersed suspension；
In addition, by coupling agent (pressing the 0.5% of whisker mass fraction) gamma-aminopropyl-triethoxy-silane coupling agent (KH550)
Absolute ethyl alcohol is dissolved in, coupling agent solution is obtained；Unit for uniform suspension is well mixed in 80 DEG C with coupling agent solution again
Lower backflow 3h；Room temperature is cooled to, is centrifuged, dried in 80 DEG C of vacuum drying ovens, so as to be obtained what is be modified
Magnesium hydroxide crystal whisker.
(2) by above-mentioned modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/right
Terephtha-late is placed in high speed blender is mixed together.
(3) above-mentioned well mixed each reactant is placed in extruding pelletization in double screw extruder, hydroxide is obtained
The whisker modified polyadipate of magnesium/butylene terephthalate composite particles.
(4) above-mentioned composite particles are obtained standard testing batten through injection moulding, it is standby.
With unmodified polyadipate/butylene terephthalate consumption/part as comparative example, drawn using universal electrical
Force tester (SUN500 types, by Italian GALDABINI companies manufacture) to above-described embodiment 1-4 most
Preparation-obtained standard testing batten carries out tensile strength, elongation at break measure eventually, and it the results are shown in Table 1 institute
Show：
| Tensile strength/MPa | Elongation at break/% | |
| Embodiment 1 | 42.2 | 326.4 |
| Embodiment 2 | 34.2 | 354.3 |
| Embodiment 3 | 36.2 | 339.5 |
| Embodiment 4 | 28.6 | 341.9 |
| Comparative example | 22.0 | 315.7 |
Table 1
, polyadipate/to benzene two modified by magnesium hydroxide crystal whisker is can be seen that by the data of upper table 1
Formic acid fourth diester mechanical property is obviously improved.
Specific embodiment of the invention has been described in detail above, but, it is intended only as example, this hair
It is bright to be not restricted to particular embodiments described above.To those skilled in the art, it is any to the present invention
The equivalent modifications and replacement for carrying out are also all among scope of the invention.Therefore, essence of the invention is not being departed from
The impartial conversion and modification made under god and scope, all should be contained within the scope of the invention.
Claims (8)
1. the preparation method of the modified polyadipate/butylene terephthalate composite of a kind of magnesium hydroxide crystal whisker, its
It is characterised by, the preparation method is comprised the following steps：
(1) magnesium hydroxide crystal whisker is mixed with absolute ethyl alcohol, ultrasonic disperse obtains finely dispersed suspension；In addition,
Coupling agent is dissolved in absolute ethyl alcohol, coupling agent solution is obtained；Again by the finely dispersed suspension and the coupling
Agent solution is well mixed, and in backflow at 80 DEG C；Room temperature, centrifugation are cooled to, then are dried in 80 DEG C of vacuum
Dried in case, modified magnesium hydroxide crystal whisker is obtained；
(2) by the modified magnesium hydroxide crystal whisker, red phosphorus, antioxidant, heat stabilizer and polyadipate/to benzene
Dioctyl phthalate fourth diester is placed in high speed blender is mixed together；
(3) mixture of each reactant being well mixed in step (2) is placed in extruding pelletization in double screw extruder,
Modified polyadipate/butylene terephthalate the composite particles of magnesium hydroxide crystal whisker are obtained；
Wherein, the mass fraction proportioning of each reactant composition is as follows：
2. the modified polyadipate/butylene terephthalate composite wood of magnesium hydroxide crystal whisker according to claim 1
The preparation method of material, it is characterised in that the number-average molecular weight of the polyadipate/butylene terephthalate is
3.6×104。
3. the modified polyadipate/butylene terephthalate composite wood of magnesium hydroxide crystal whisker according to claim 1
The preparation method of material, it is characterised in that the coupling agent is that gamma-aminopropyl-triethoxy-silane or titanate esters are coupled
Agent.
4. the modified polyadipate/butylene terephthalate composite wood of magnesium hydroxide crystal whisker according to claim 1
The preparation method of material, it is characterised in that the antioxidant be selected from it is following any one：Diphenylamines, p-phenylenediamine
Or EEDQ.
5. the modified polyadipate/butylene terephthalate composite wood of magnesium hydroxide crystal whisker according to claim 1
The preparation method of material, it is characterised in that the heat stabilizer is maleic anhydride or epoxidized soybean oil.
6. the modified polyadipate/terephthalic acid (TPA) fourth of magnesium hydroxide crystal whisker according to any one of claim 1-5
The preparation method of diester composite, it is characterised in that ultrasonic disperse duration described in step (1)
It is 10min.
7. the modified polyadipate/terephthalic acid (TPA) fourth of magnesium hydroxide crystal whisker according to any one of claim 1-5
The preparation method of diester composite, it is characterised in that the duration that flowed back described in step (1) is 3
Hour.
8. the modified polyadipate/butylene terephthalate composite of a kind of magnesium hydroxide crystal whisker, it is characterised in that
The magnesium hydroxide crystal whisker be modified polyadipate/butylene terephthalate composite be by any of the above-described weigh
Obtained in preparation method described in profit requirement.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111849117A (en) * | 2020-07-17 | 2020-10-30 | 浙江王氏科技有限公司 | Flame-retardant plastic and processing technology thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111849117A (en) * | 2020-07-17 | 2020-10-30 | 浙江王氏科技有限公司 | Flame-retardant plastic and processing technology thereof |
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Application publication date: 20170627 |