CN110105666A - A kind of nucleating agent master batch and preparation method thereof for toughening modifying PP resin - Google Patents
A kind of nucleating agent master batch and preparation method thereof for toughening modifying PP resin Download PDFInfo
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- CN110105666A CN110105666A CN201910425867.4A CN201910425867A CN110105666A CN 110105666 A CN110105666 A CN 110105666A CN 201910425867 A CN201910425867 A CN 201910425867A CN 110105666 A CN110105666 A CN 110105666A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
The present invention discloses a kind of nucleating agent master batch and preparation method thereof for toughening modifying PP resin, using calcium salt and sulfate as raw material, reaction solution is filled in the pore structure of porous PP particle with ultrasonic technique, so that the calcium sulfate crystal whiskers uniform load generated improves dispersion effect of the calcium sulfate crystal whiskers in PP material on the gap and surface of PP particle；Calcium sulfate crystal whiskers after sonicated have the heterogeneous nucleating effect of certain induction beta-crystal, and the calcium sulfate crystal whiskers of generation form more heterogeneous nucleation points in PP material, the crystal of more fine uniforms is induced to occur；Using the calcium sulfate crystal whiskers inside PP particle as carrier, using ultrasonic technique by the calcium sulfate crystal whiskers surface after organic nucleating agent uniform load to modification, dispersibility of the compounding nucleating agent in PP master batch is improved, overcomes organic phosphate nucleating agent in resin matrix the problem of bad dispersibility.
Description
Technical field
The present invention relates to technical field of polymer, and in particular to a kind of nucleating agent master batch for toughening modifying PP resin and
Preparation method.
Background technique
PP is the resins for universal use of kind of function admirable, but its toughness is undesirable, thus limits application.It is desired in order to reach
High-toughness polypropylene can remove modified polypropene by method physically or chemically, and in the research of numerous polypropylene modifications, lead to
Crossing addition toughener and carrying out toughening modifying to PP is recent research hotspot, has result of study to show to add rubber bodies or rigidity
The toughener such as particle have Different Effects to the mechanical property of the entire co-mixing system of PP.
Calcium sulfate crystal whiskers have much for the research of polyacrylic toughening modifying, but are mostly directly straight with expanding material, PP resin
It is modified to connect melting mixing, but since calcium sulfate crystal whiskers large specific surface area, contact surface are big, calcium sulfate crystal whiskers is caused to prepare and applying
Easily reunite in the process, leads to the bad dispersibility in polypropylene PP resin, binding force is weak, and reinforcing effect is bad.
In addition the mechanical property for impact-resistant copolymerized PP and heat resistance are closely related with its crystallinity, crystal habit,
If PP spherulite size miniaturize, the shock resistance of PP polymer can be largely improved.And relative to α crystalline substance
For type, beta crystal impact copolymer polypropylene has superior mechanical property and hot property.It the use of nucleating agent is a kind of effective
The method for obtaining beta crystal.Under normal circumstances, grain density can be obviously increased by adding less nucleating agent, reduce crystal
Size.
There are many polypropylene nucleater type, can be divided mainly into inorganic and organic two major classes.Wherein organic phosphate series at
When core agent is used for PP, the product transparency, rigidity, crystallization rate and heat distortion temperature have raising by a relatively large margin, and heat resistance is excellent
It is different, be resistant to 400 DEG C or more of high temperature, processing conditions range of choice is wide, do not decomposed in forming process will not discharge it is unpleasant
Smell.The shortcoming of organic phosphate belongs to distributed nucleating agent, with resin precisely due to the fusing point of its most kind is excessively high
Limited compatibility, bad dispersibility are not easy mixture under usual conditions, product surface are easy to cause fault occur.
Summary of the invention
To solve above-mentioned the deficiencies in the prior art, the present invention proposes a kind of nucleation for toughening modifying PP resin
The preparation method of agent master batch improves the dispersion effect of calcium sulfate crystal whiskers, organic nucleating agent in PP master batch, facilitates to PP material
Carry out toughening modifying.
To realize the above-mentioned technical purpose, the invention discloses a kind of systems of nucleating agent master batch for toughening modifying PP resin
Preparation Method generates calcium carbonate crystal whisker using calcium salt and sulfate as raw material on the pore structure of porous PP particle, forms load carbon
After the PP particle of sour calcium pyroborate, then surface-modified dose of modification, organic nucleating agent is loaded to carbonic acid using ultrasonic technique
Calcium pyroborate surface, then through melting extrusion, pelletizing, obtain compounding nucleating agent master batch.
Further, the molar ratio of the calcium salt and sulfate is 1:1, and the calcium salt selects calcium nitrate, the sulfate
Select potassium sulfate.
Further, the porous PP particle is the spherical isotactic PP particle that inside is porous structure, and the partial size of particle exists
3-5mm, internal aperture is at 1-3 μm.
Further, the organic nucleating agent is organic phosphate nucleating agent, is specifically chosen organic phosphate nucleating agent NA-
10, one of NA-11 or NA-21.
A more step, the weight ratio of the organic nucleating agent and calcium sulfate crystal whiskers are (0.1-0.6): 1, the two it is described at
Specific gravity in core agent master batch is in 40-65%.
Further, the surface modifier is selected from silane coupling agent, titanate coupling agent agent, metatitanic acid aluminate coupling agent
And one of stearic acid, usage amount is in 2-4%.
Further, the preparation method of the nucleating agent master batch for toughening modifying PP resin, specific preparation step are as follows:
(1) it is respectively configured calcium salt and sulfate liquor, after mechanical stirring 5-15min, is slowly stirred 30-50min, stands 1-
2h obtains the suspension containing 20-40% calcium sulfate precipitation, and porous PP particle is added, after stirring 8-15min, ultrasonic disperse 30-
90min, still aging 18-30h after filtering, recycle filtrate, and it is brilliant that load calcium sulfate is made in 110-130 DEG C of dry 6-8h in filter cake
The PP particle of palpus；
(2) the PP particle for the load calcium sulfate crystal whiskers that step (1) obtains is placed in ethanol solution, is added and uses second
The dissolved stearic acid solution of alcohol, is placed in ultrasonic oscillation device, and mixing dispersion 20-40min stands 30-60min, filters, does
It is dry；
(3) organic nucleating agent is added in ethanol solution, stirring is completely dissolved to it, is added step (2) is modified
PP particle be placed in ultrasonic oscillation device after mixing evenly, mixing dispersion 40-90min, stand 10-20min after, large aperture
The screen to filtrate recycles filtrate, and sediment is washed 2-3 times, while recycling washing water, is incorporated into filtrate；
(4) filtrate by step (1) and step (3) recycling is added in spray dryer, and spray dried powder is prepared
Last powder, step (3) sediment is dry under the conditions of being placed in 120-140 DEG C, obtains compounding nucleating agent/PP particle；
(5) compounding nucleating agent/PP particle and spray-dried powders that step (4) obtains are added to double screw extruder
In, melting extrusion, and pelletizing is carried out, obtain the nucleating agent master batch of PP resin；Screw speed exists in 30-50r/min, melt temperature
225-230℃.Further, the aperture of the large aperture sieve used in step (3) is less than the partial size of the PP particle.
The invention also discloses a kind of nucleating agents for toughening modifying PP resin being prepared such as above-mentioned preparation method
Master batch.
Compared with the prior art, the invention has the following advantages:
(1) using calcium salt and sulfate as raw material, reaction solution is made to be filled in the pore structure of porous PP particle with ultrasonic technique
It is interior, so that on the one hand the calcium sulfate crystal whiskers uniform load generated improves calcium sulfate on the gap and surface of PP particle
Dispersion effect of the whisker in PP material, the calcium sulfate crystal whiskers on the other hand generated are smaller, formed in PP material more different
Phase nucleating point induces the crystal of more fine uniforms to occur, helps to improve the performance of polypropylene material.
(2) using the calcium sulfate crystal whiskers inside PP particle as carrier, using ultrasonic technique by organic nucleating agent uniform load extremely
Calcium sulfate crystal whiskers surface after modification, then through melting extrusion, on the one hand improve dispersion of the compounding nucleating agent in PP master batch
Property, so that organic nucleating agent and calcium sulfate crystal whiskers is realized fine dispersion in PP master batch, overcomes organic phosphate nucleating agent and setting
In aliphatic radical body the problem of bad dispersibility；On the other hand, the calcium sulfate crystal whiskers after sonicated have certain induction beta-crystal
Heterogeneous nucleating effect, make crystalling propylene temperature improve and crystalline rate increase, and then improve PP material toughening effect.
Specific embodiment
Embodiment 1
A kind of nucleating agent master batch for toughening modifying PP resin, specific preparation method step are as follows:
(1) it is respectively configured the calcium nitrate and potassium sulfate solution of equimolar amounts, after mechanical stirring 5min, is slowly stirred 30min,
2h is stood, the suspension containing 40% calcium sulfate precipitation is obtained, porous PP is added in the mass ratio for being 2:1 according to calcium sulfate/PP
Grain, after stirring 10min, ultrasonic disperse 90min, it is still aging for 24 hours, after filtering, recycle filtrate, filter cake is made in 120 DEG C of dry 6h
At the PP particle of load calcium sulfate crystal whiskers；
(2) the PP particle for the load calcium sulfate crystal whiskers that step (1) obtains is placed in ethanol solution, it is hard is added 3%
Resin acid, stearic acid are reentered after being dissolved using ethanol in proper amount, are placed in ultrasonic oscillation device, and mixing dispersion 30min stands 60min,
Filtering, it is dry；
(3) mass ratio for being 1:6 according to organic nucleating agent/calcium sulfate, nucleant agent N A-10 is added in ethanol solution,
Stirring is completely dissolved to it, and the modified PP particle of step (2) is placed in ultrasonic oscillation device by addition after mixing evenly, is mixed
Dispersion 60min is closed, after standing 20min, large aperture the screen to filtrate recycles filtrate, and sediment is washed 3 times, while recycling washing water,
It is incorporated into filtrate；
(4) filtrate by step (1) and step (3) recycling is added in spray dryer, and spray dried powder is prepared
Last powder, step (3) sediment is dry under the conditions of being placed in 130 DEG C, obtains compounding nucleating agent/PP particle；
(5) compounding nucleating agent/PP particle and spray-dried powders that step (4) obtains are added to double screw extruder
In, melting extrusion, and pelletizing is carried out, screw speed is in 35r/min, and for melt temperature at 225 DEG C, the nucleating agent for obtaining PP resin is female
Grain.
Embodiment 2
A kind of nucleating agent master batch for toughening modifying PP resin, specific preparation method step are as follows:
(1) it is respectively configured the calcium nitrate and potassium sulfate solution of equimolar amounts, after mechanical stirring 5min, is slowly stirred 30min,
Stand 2h, obtain the suspension containing 40% calcium sulfate precipitation, it is still aging for 24 hours, after filtering, recycle filtrate, filter cake is dry at 120 DEG C
Dry 6h, is made calcium sulfate crystal whiskers；
(2) calcium sulfate crystal whiskers that step (1) obtains are placed in ethanol solution, 3% stearic acid is added, stearic acid makes
It reenters, is placed in ultrasonic oscillation device after being dissolved with ethanol in proper amount, mixing dispersion 30min stands 60min, filters, dry；
(3) mass ratio for being 1:6 according to organic nucleating agent/calcium sulfate, nucleant agent N A-10 is added in ethanol solution,
Stirring is completely dissolved to it, is added step (2) modified calcium sulfate crystal whiskers；The quality for being simultaneously 2:1 according to calcium sulfate/PP
Than porous PP particle is added；
After mixing evenly, it is placed in ultrasonic oscillation device, mixing dispersion 60min, after standing 20min, large aperture sieve mistake
Filtrate is recycled in filter, and sediment is washed 3 times, while recycling washing water, is incorporated into filtrate；
(4) filtrate that step (3) are recycled is added in spray dryer, spray-dried powders powder is prepared, walked
Suddenly dry under the conditions of (3) sediment is placed in 130 DEG C, obtain compounding nucleating agent/PP particle；
(5) compounding nucleating agent/PP particle and spray-dried powders that step (4) obtains are added to double screw extruder
In, melting extrusion, and pelletizing is carried out, screw speed is in 35r/min, and for melt temperature at 225 DEG C, the nucleating agent for obtaining PP resin is female
Grain.
Embodiment 3
A kind of nucleating agent master batch for toughening modifying PP resin, specific preparation method step are as follows:
(1) it is respectively configured the calcium nitrate and potassium sulfate solution of equimolar amounts, after mechanical stirring 5min, is slowly stirred 30min,
Stand 2h, obtain the suspension containing 40% calcium sulfate precipitation, it is still aging for 24 hours, after filtering, recycle filtrate, filter cake is dry at 120 DEG C
Dry 6h, is made calcium sulfate crystal whiskers；
(2) calcium sulfate crystal whiskers that step (1) obtains are placed in ethanol solution, 3% stearic acid is added, stearic acid makes
It reenters, is placed in ultrasonic oscillation device after being dissolved with ethanol in proper amount, mixing dispersion 30min stands 60min, filters, dry；
(3) mass ratio for being 1:6 according to organic nucleating agent/calcium sulfate, calcium sulfate/porous PP particle are the mass ratio of 2:1,
It is added in double screw extruder, melting extrusion, and carries out pelletizing, screw speed is obtained in 35r/min, melt temperature at 225 DEG C
To the nucleating agent master batch of PP resin.
Embodiment 4
According in embodiment 1, embodiment 2 and embodiment 3 specific method preparation, respectively obtain A, B, C3 group it is different at
Core agent master batch obtains A group nucleating agent master batch using preparation method of the present invention according to embodiment 1, obtains according to 2 preparation method of embodiment
To B group nucleating agent master batch, C group nucleating agent master batch is obtained using the preparation method directly mixed according to embodiment 3, will be obtained later
Different nucleating agent master batches and pure PP resin prepare sample according to the ratio melting extrusion of 1:5, and carry out corresponding performance inspection
It surveys.
Tensile strength presses ASTM D-638 standard, and bending strength presses ASTM D-790 standard, carries out sample preparation test.Impact is strong
Degree test: according to GB/T 1843-1996, using the impact strength of balance weight impact testing machine measurement sample.Test result is shown in Table
1。
The test result of 1 MODIFIED PP material of table
As seen from the above table: in the identical situation of each component content, using the A group MODIFIED PP material of the method for the present invention preparation
Performance is better than two groups of materials of B, C, helps to improve organic nucleating agent, calcium sulfate crystal whiskers in PP tree using preparation method of the present invention
Dispersion effect in rouge promotes the growth of PP crystal, improves the shock resistance of PP material.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (9)
1. a kind of preparation method of the nucleating agent master batch for toughening modifying PP resin, which is characterized in that with calcium salt and sulfate
For raw material, calcium carbonate crystal whisker is generated on the pore structure of porous PP particle, forms the PP particle of load calcium carbonate crystal whisker, then is passed through
After surface modifying agent processing, organic nucleating agent is loaded to calcium carbonate crystal whisker surface using ultrasonic technique, then squeeze through melting
Out, pelletizing obtains compounding nucleating agent master batch.
2. a kind of preparation method of nucleating agent master batch for toughening modifying PP resin according to claim 1, feature
It is, the molar ratio of the calcium salt and sulfate is 1:1, and the calcium salt selects calcium nitrate, and the sulfate selects potassium sulfate.
3. a kind of preparation method of nucleating agent master batch for toughening modifying PP resin according to claim 1, feature
It is, the porous PP particle is the spherical isotactic PP particle that inside is porous structure, and the partial size of particle is in 3-5mm, internal holes
Diameter is at 1-3 μm.
4. a kind of preparation method of nucleating agent master batch for toughening modifying PP resin according to claim 1, feature
Be, the organic nucleating agent be organic phosphate nucleating agent, be specifically chosen organic phosphate nucleating agent NA-10, NA-11 or
One of NA-21.
5. a kind of preparation method of nucleating agent master batch for toughening modifying PP resin according to claim 1, feature
It is, the weight ratio of the organic nucleating agent and calcium sulfate crystal whiskers is (0.1-0.6): 1, the two is in the nucleating agent master batch
Specific gravity is in 40-65%.
6. a kind of preparation method of nucleating agent master batch for toughening modifying PP resin according to claim 1, feature
It is, the surface modifier is in silane coupling agent, titanate coupling agent agent, metatitanic acid aluminate coupling agent and stearic acid
One kind, usage amount is in 2-4%.
7. the preparation method of -6 any a kind of nucleating agent master batches for toughening modifying PP resin according to claim 1,
It is characterized in that, specific preparation step are as follows:
(1) it is respectively configured calcium salt and sulfate liquor, after mechanical stirring 5-15min, is slowly stirred 30-50min, stands 1-2h,
The suspension containing 20-40% calcium sulfate precipitation is obtained, porous PP particle is added, after stirring 8-15min, ultrasonic disperse 30-
90min, still aging 18-30h after filtering, recycle filtrate, and it is brilliant that load calcium sulfate is made in 110-130 DEG C of dry 6-8h in filter cake
The PP particle of palpus；
(2) the PP particle for the load calcium sulfate crystal whiskers that step (1) obtains is placed in ethanol solution, is added molten using ethyl alcohol
Stearic acid solution after solution, is placed in ultrasonic oscillation device, and mixing dispersion 20-40min stands 30-60min, filters, dry；
(3) organic nucleating agent is added in ethanol solution, stirring is completely dissolved to it, is added step (2) modified PP
Particle is placed in ultrasonic oscillation device after mixing evenly, mixing dispersion 40-90min, after standing 10-20min, large aperture sieve
Filtrate is recycled in filtering, and sediment is washed 2-3 times, while recycling washing water, is incorporated into filtrate；
(4) filtrate by step (1) and step (3) recycling is added in spray dryer, and spray-dried powders powder is prepared
End, step (3) sediment is dry under the conditions of being placed in 120-140 DEG C, obtains compounding nucleating agent/PP particle；
(5) compounding nucleating agent/PP particle and spray-dried powders that step (4) obtains are added in double screw extruder, are melted
Melt extrusion, and carry out pelletizing, obtains the nucleating agent master batch of PP resin；Screw speed is in 30-50r/min, and melt temperature is in 225-
230℃。
8. a kind of preparation method of nucleating agent master batch for toughening modifying PP resin according to claim 7, feature
It is, the aperture of the large aperture sieve used in step (3) is less than the partial size of the PP particle.
9. the nucleating agent master batch for toughening modifying PP resin that a kind of preparation method as described in claim 1-6 is prepared.
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| CN114717679A (en) * | 2022-02-22 | 2022-07-08 | 浙江安顺化纤有限公司 | Antibacterial PBAT short fiber and application thereof |
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Application publication date: 20190809 |