CN107245166A - A kind of preparation method of the ternary zinc-magnesium aluminum hydrotalcite heat stabilizer of nano silicon core-shell particles intercalation modifying - Google Patents
A kind of preparation method of the ternary zinc-magnesium aluminum hydrotalcite heat stabilizer of nano silicon core-shell particles intercalation modifying Download PDFInfo
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- CN107245166A CN107245166A CN201710596342.8A CN201710596342A CN107245166A CN 107245166 A CN107245166 A CN 107245166A CN 201710596342 A CN201710596342 A CN 201710596342A CN 107245166 A CN107245166 A CN 107245166A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- 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
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Abstract
The invention discloses a kind of preparation method of the ternary zinc-magnesium aluminum hydrotalcite heat stabilizer of nano silicon core-shell particles intercalation modifying, the present invention prepares zinc-magnesium aluminum hydrotalcite using co-precipitation centrifugation hydro-thermal method, then its presoma and nano silicon core-shell particles reaction are prepared to the ternary zinc-magnesium aluminum hydrotalcite of intercalation modifying, introducing of the nucleocapsid than the nano silicon core-shell particles for 30/70, the heat stabilizer of gained and PVC blend is set to have higher heat endurance good, and because the reaction of GMA epoxide groups in core-shell particles shell and PVC carboxyls makes gained hydrotalcite thermal stabilizer be difficult well to reunite with polymer matrix compatability, initial stage for that can significantly improve PVC in PVC suppresses discoloration, processing rheological property and resistance to elevated temperatures, good weatherability long-time stability are good.
Description
Technical field
The present invention relates to hydrotalcite thermal stabilizer production field, and in particular to a kind of nano silicon core-shell particles intercalation
The preparation method of modified ternary zinc-magnesium aluminum hydrotalcite heat stabilizer.
Background technology
Polyvinyl chloride(PVC)It is one of important general-purpose plastics, because its is nonflammable, performance is good and the low advantage of price,
It is widely used in the various fields such as tubing, plastic door-window, electric wire.But PVC heat endurances are very poor, and in process
Processing temperature is higher than PVC decomposition temperature, there is unstable chlorine atom on PVC strands, and it easily occurs in the case of heated
Dehydrochlorination, causes to form the polyene structure with conjugated double bond in PVC so that the color of PVC material changes, simultaneously
The physical and chemical properties of PVC material are deteriorated.Thus, it is necessary to which it is thermally-stabilised to improve its to add heat stabilizer in process
Performance.The species of PVC heat stabilizer is more, at present, the low-toxicity green environment-benign heat stabilizer based on Ca/Zn stabilizers into
For development trend.The hydrogen chloride that the interlayer carbanion and laminate of hydrotalcite can be produced with PVC degradeds reacts, therefore
PVC long-term thermal stabilities can be improved, are widely used in PVC auxiliary heat stabilizers.Hydrotalcite layers ion has commutative
Property, therefore feature anion can be introduced to interlayer preparation feature hydrotalcite to improve PVC performances.
Study dihydrogen phosphate intercalation zinc-magnesium aluminum hydrotalcite and compounded with PVC in the prior art, research finds phosphorus
The initial stage that acid dihydride root intercalation zinc-magnesium aluminum hydrotalcite can not only significantly improve PVC suppresses discoloration, meanwhile, biphosphate
The dispersiveness in polyvinyl chloride base material is improved after root intercalation modifying zinc-magnesium aluminum hydrotalcite and is improved between polyvinyl chloride
Compatibility, polyvinyl chloride mechanical property improves, but processing rheological property is in a slight decrease and long-term thermal stability is not good.
The content of the invention
It is an object of the invention to provide a kind of ternary zinc-magnesium aluminium neatly of nano silicon core-shell particles intercalation modifying
The preparation method of stone heat stabilizer, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this:
A kind of preparation method of the ternary zinc-magnesium aluminum hydrotalcite heat stabilizer of nano silicon core-shell particles intercalation modifying, it is special
Levy and be, comprise the following steps:
(1)Absolute ethyl alcohol and deionized water are made into alcohol-water solution with volume ratio 95: 5, are with dilute nitric acid solution regulation pH value
3-4, the lower addition nano silicon ultrasonic disperse of stirring mixes to obtain suspension;
(2)Silane coupler is added into above-mentioned suspension and bleeding agent stirs and evenly mixs ultrasonic disperse 20-30min, is spray-dried
Obtain modified manometer silicon dioxide;
(3)Modified manometer silicon dioxide, polymer monomer, assistant for emulsifying agent, initiator are well mixed in room according to a certain percentage
The lower magnetic agitation 30min of temperature, adjusts pH to 8-9, adds after emulsifying agent SDS stirs and ultrasound point is carried out under 1200W power
15min is dissipated, 70-80 DEG C is warming up to, with 300r/min 5-6 hours obtained nano silicon nucleocapsid grains of speed stirring reaction
Son;
(4)Weigh a certain amount of Magnesium dichloride hexahydrate, zinc chloride, Aluminium chloride hexahydrate to be dissolved in deionized water, stirring is obtained
Even mixing salt solution, then weigh a certain amount of sodium hydroxide and sodium carbonate is dissolved in deionized water, stirring obtains mixed ammonium/alkali solutions,
Two kinds of mixed solutions are controlled to add nucleation in rotating liquid-film reactor simultaneously with 1 drop/s speed, and forced circulation 2min is obtained
White nucleation slurries;
(5)By step(4)Obtained white nucleation slurries were centrifuged, washing in crystallization under reflux temperature 6 hours, obtained zinc
Magnalium hydrotalcite wet cake;
(6)By step(5)Zinc-magnesium aluminum hydrotalcite wet cake ultrasonic disperse in water, 2h is stirred at 90 DEG C, it is then slow plus
Enter step(3)Nano silicon core-shell particles, adjust pH=4 with dilute nitric acid solution, reaction are finally stirred at reflux at 100 DEG C
12 h, stand natural cooling, and suction filtration, washing to neutrality is dried for 60 DEG C and discharged.
The step(1)The mass fraction of nano silicon is 25-30% in middle suspension.
Step(2)Described in silane coupler be KH570, addition be nano silicon consumption 3-5%, it is described
Bleeding agent be AEO, addition be nano silicon consumption 0.6-0.9%.
The step(3)The nucleocapsid of middle nano silicon core-shell particles is than 30: 70;Described polymer monomer includes single
Body butyl acrylate (BA), methyl methacrylate (MMA) and GMA (GMA), wherein GMA mass point
The mass ratio that number is 1%, MMA and BA is 4: 6;Described assistant for emulsifying agent is hexadecane, and addition is the 10- of monomer total amount
13%;Described initiator is azodiisobutyronitrile, and addition is the 0.5-0.8% of monomer total amount;Described emulsifying agent SDS additions
Measure the 6-8% for monomer total amount.
The step(4)Middle n(MgCl2·6H2O)∶n(ZnCl2)∶n(AlCl3·6H2O)=1∶1∶1;Described hydroxide
The mol ratio 2 of sodium and metal cation;Described sodium carbonate and the mol ratio of metal cation are 1.
The step(5)In zinc-magnesium aluminum hydrotalcite wet cake solid content be 23-25%.
The step(6)The addition of middle nano silicon core-shell particles is the 3- of zinc-magnesium aluminum hydrotalcite wet cake consumption
4%。
The present invention has following beneficial effect:The present invention prepares zinc-magnesium aluminum hydrotalcite using co-precipitation-centrifugation-hydro-thermal method, so
Its presoma and nano silicon core-shell particles reaction are prepared to the ternary zinc-magnesium aluminum hydrotalcite of intercalation modifying afterwards, nucleocapsid ratio is
The introducing of 30/70 nano silicon core-shell particles, makes the heat stabilizer of gained and PVC blend have higher heat
Stability is good, and due to the reaction of GMA epoxide groups and PVC carboxyls in core-shell particles shell make gained hydrotalcite thermal stabilizer with
Polymer matrix compatability be difficult well reunite, for can be significantly improved in PVC suppress PVC initial stage discoloration,
Processing rheological property and resistance to elevated temperatures, good weatherability long-time stability are good.
Embodiment
A kind of preparation method of the ternary zinc-magnesium aluminum hydrotalcite heat stabilizer of nano silicon core-shell particles intercalation modifying,
It is characterised in that it includes following steps:
(1)Absolute ethyl alcohol and deionized water are made into alcohol-water solution with volume ratio 95: 5, are with dilute nitric acid solution regulation pH value
3-4, the lower addition nano silicon ultrasonic disperse of stirring mixes to obtain suspension;
(2)Silane coupler is added into above-mentioned suspension and bleeding agent stirs and evenly mixs ultrasonic disperse 20-30min, is spray-dried
Obtain modified manometer silicon dioxide;
(3)Modified manometer silicon dioxide, polymer monomer, assistant for emulsifying agent, initiator are well mixed in room according to a certain percentage
The lower magnetic agitation 30min of temperature, adjusts pH to 8-9, adds after emulsifying agent SDS stirs and ultrasound point is carried out under 1200W power
15min is dissipated, 70-80 DEG C is warming up to, with 300r/min 5-6 hours obtained nano silicon nucleocapsid grains of speed stirring reaction
Son;
(4)Weigh a certain amount of Magnesium dichloride hexahydrate, zinc chloride, Aluminium chloride hexahydrate to be dissolved in deionized water, stirring is obtained
Even mixing salt solution, then weigh a certain amount of sodium hydroxide and sodium carbonate is dissolved in deionized water, stirring obtains mixed ammonium/alkali solutions,
Two kinds of mixed solutions are controlled to add nucleation in rotating liquid-film reactor simultaneously with 1 drop/s speed, and forced circulation 2min is obtained
White nucleation slurries;
(5)By step(4)Obtained white nucleation slurries were centrifuged, washing in crystallization under reflux temperature 6 hours, obtained zinc
Magnalium hydrotalcite wet cake;
(6)By step(5)Zinc-magnesium aluminum hydrotalcite wet cake ultrasonic disperse in water, 2h is stirred at 90 DEG C, it is then slow plus
Enter step(3)Nano silicon core-shell particles, adjust pH=4 with dilute nitric acid solution, reaction are finally stirred at reflux at 100 DEG C
12 h, stand natural cooling, and suction filtration, washing to neutrality is dried for 60 DEG C and discharged.
The step(1)The mass fraction of nano silicon is 25-30% in middle suspension.
Step(2)Described in silane coupler be KH570, addition be nano silicon consumption 3-5%, it is described
Bleeding agent be AEO, addition be nano silicon consumption 0.6-0.9%.
The step(3)The nucleocapsid of middle nano silicon core-shell particles is than 30: 70;Described polymer monomer includes single
Body butyl acrylate (BA), methyl methacrylate (MMA) and GMA (GMA), wherein GMA mass point
The mass ratio that number is 1%, MMA and BA is 4: 6;Described assistant for emulsifying agent is hexadecane, and addition is the 10- of monomer total amount
13%;Described initiator is azodiisobutyronitrile, and addition is the 0.5-0.8% of monomer total amount;Described emulsifying agent SDS additions
Measure the 6-8% for monomer total amount.
The step(4)Middle n(MgCl2·6H2O)∶n(ZnCl2)∶n(AlCl3·6H2O)=1∶1∶1;Described hydroxide
The mol ratio 2 of sodium and metal cation;Described sodium carbonate and the mol ratio of metal cation are 1.
The step(5)In zinc-magnesium aluminum hydrotalcite wet cake solid content be 23-25%.
The step(6)The addition of middle nano silicon core-shell particles is the 3- of zinc-magnesium aluminum hydrotalcite wet cake consumption
4%。
Claims (7)
1. a kind of preparation method of the ternary zinc-magnesium aluminum hydrotalcite heat stabilizer of nano silicon core-shell particles intercalation modifying, its
It is characterised by, comprises the following steps:
(1)Absolute ethyl alcohol and deionized water are made into alcohol-water solution with volume ratio 95: 5, are with dilute nitric acid solution regulation pH value
3-4, the lower addition nano silicon ultrasonic disperse of stirring mixes to obtain suspension;
(2)Silane coupler is added into above-mentioned suspension and bleeding agent stirs and evenly mixs ultrasonic disperse 20-30min, is spray-dried
Obtain modified manometer silicon dioxide;
(3)Modified manometer silicon dioxide, polymer monomer, assistant for emulsifying agent, initiator are well mixed in room according to a certain percentage
The lower magnetic agitation 30min of temperature, adjusts pH to 8-9, adds after emulsifying agent SDS stirs and ultrasound point is carried out under 1200W power
15min is dissipated, 70-80 DEG C is warming up to, with 300r/min 5-6 hours obtained nano silicon nucleocapsid grains of speed stirring reaction
Son;
(4)Weigh a certain amount of Magnesium dichloride hexahydrate, zinc chloride, Aluminium chloride hexahydrate to be dissolved in deionized water, stirring is obtained
Even mixing salt solution, then weigh a certain amount of sodium hydroxide and sodium carbonate is dissolved in deionized water, stirring obtains mixed ammonium/alkali solutions,
Two kinds of mixed solutions are controlled to add nucleation in rotating liquid-film reactor simultaneously with 1 drop/s speed, and forced circulation 2min is obtained
White nucleation slurries;
(5)By step(4)Obtained white nucleation slurries were centrifuged, washing in crystallization under reflux temperature 6 hours, obtained zinc
Magnalium hydrotalcite wet cake;
(6)By step(5)Zinc-magnesium aluminum hydrotalcite wet cake ultrasonic disperse in water, 2h is stirred at 90 DEG C, it is then slow plus
Enter step(3)Nano silicon core-shell particles, adjust pH=4 with dilute nitric acid solution, reaction are finally stirred at reflux at 100 DEG C
12 h, stand natural cooling, and suction filtration, washing to neutrality is dried for 60 DEG C and discharged.
2. a kind of ternary zinc-magnesium aluminum hydrotalcite heat of nano silicon core-shell particles intercalation modifying according to claim 1
The preparation method of stabilizer, it is characterised in that the step(1)The mass fraction of nano silicon is 25- in middle suspension
30%。
3. a kind of ternary zinc-magnesium aluminum hydrotalcite heat of nano silicon core-shell particles intercalation modifying according to claim 1
The preparation method of stabilizer, it is characterised in that step(2)Described in silane coupler be KH570, addition is nano-silica
The 3-5% of SiClx consumption, described bleeding agent is AEO, and addition is the 0.6- of nano silicon consumption
0.9%。
4. a kind of ternary zinc-magnesium aluminum hydrotalcite heat of nano silicon core-shell particles intercalation modifying according to claim 1
The preparation method of stabilizer, it is characterised in that the step(3)The nucleocapsid of middle nano silicon core-shell particles is than 30: 70;Institute
The polymer monomer stated includes monomer butyl acrylate (BA), methyl methacrylate (MMA) and glycidyl third
The mass ratio that ester (GMA), wherein GMA mass fractions are 1%, MMA and BA is 4: 6;Described assistant for emulsifying agent is hexadecane, is added
Dosage is the 10-13% of monomer total amount;Described initiator is azodiisobutyronitrile, and addition is the 0.5-0.8% of monomer total amount;
Described emulsifying agent SDS additions are the 6-8% of monomer total amount.
5. a kind of ternary zinc-magnesium aluminum hydrotalcite heat of nano silicon core-shell particles intercalation modifying according to claim 1
The preparation method of stabilizer, it is characterised in that the step(4)Middle n(MgCl2·6H2O)∶n(ZnCl2)∶n(AlCl3·6H2O)
=1∶1∶1;Described sodium hydroxide and the mol ratio 2 of metal cation;Described sodium carbonate and the mol ratio of metal cation are
1。
6. a kind of ternary zinc-magnesium aluminum hydrotalcite heat of nano silicon core-shell particles intercalation modifying according to claim 1
The preparation method of stabilizer, it is characterised in that the step(5)In zinc-magnesium aluminum hydrotalcite wet cake solid content be 23-
25%。
7. a kind of ternary zinc-magnesium aluminum hydrotalcite heat of nano silicon core-shell particles intercalation modifying according to claim 1
The preparation method of stabilizer, it is characterised in that the step(6)The addition of middle nano silicon core-shell particles is zinc-magnesium aluminium
The 3-4% of hydrotalcite wet cake consumption.
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Cited By (5)
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CN110373048A (en) * | 2019-07-06 | 2019-10-25 | 王志胜 | A kind of polymolecularity light stablizes the preparation method of titanium dioxide |
CN112169803A (en) * | 2020-11-10 | 2021-01-05 | 林爱琴 | Porous carbon-loaded nano metal oxide for water treatment and preparation method thereof |
CN113754420A (en) * | 2021-09-11 | 2021-12-07 | 刘浩 | Fire-resistant and wear-resistant ceramic tile and preparation method thereof |
CN114534743A (en) * | 2022-03-07 | 2022-05-27 | 耒阳金悦科技发展有限公司 | Palladium catalyst for hydrogenation of 1, 4-butylene glycol and preparation process thereof |
CN115246955A (en) * | 2021-04-28 | 2022-10-28 | 中国石油化工股份有限公司 | Acid absorbent with layered structure and preparation method and application thereof |
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CN113754420A (en) * | 2021-09-11 | 2021-12-07 | 刘浩 | Fire-resistant and wear-resistant ceramic tile and preparation method thereof |
CN114534743A (en) * | 2022-03-07 | 2022-05-27 | 耒阳金悦科技发展有限公司 | Palladium catalyst for hydrogenation of 1, 4-butylene glycol and preparation process thereof |
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