CN109880220A - Self-repair type environment-protective rubber material and preparation method thereof - Google Patents
Self-repair type environment-protective rubber material and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of self-repair type environment-protective rubber material and preparation method thereof, it is made of following raw material: 75-100 parts of nanometer silicon rubber/fluorubber blend compounds, 15-20 parts of emulsifiers, 55-80 parts of polyethylene, 25-50 parts of alumina powders, 15-20 parts of diethyl phthalates, 35-50 parts of nitric acid magnesium dusts, 15-25 parts of nitric acid aluminium powders, 5-15 parts of adhesive；The present invention is prepared for a kind of self-repair type environment-friendly rubber, since its molecular weight is larger, molecule is with the presence of random coil Coiling-type, due to the effect of a large amount of branches when by external force, improve stronger mechanical performance, generate strong recovery tendency, there are excellent self-healing properties, by the way that silicon rubber and fluorubber are carried out ball milling, using epoxy resin as curing agent, a kind of silicon rubber/fluorubber blend compounds are formed, the good chemical stability of silicon rubber and electrical property had not only been remained, but also remain the excellent high temperature resistance of fluorubber.
Description
Technical field
The invention belongs to technical field of rubber material, specially self-repair type environment-protective rubber material and preparation method thereof.
Background technique
Rubber (Rubber) refers to the high elastic polymer material with reversible deformation, high resilience at room temperature, very
Larger deformation can be generated under small external force, remove resilient after external force.Rubber belongs to entirely without styling polymer, it
Glass transition temperature (Tg) it is low, molecular weight is often very big, is greater than hundreds of thousands.The rubber of early stage is taken from rubber tree, rubber
The latex of the plants such as grass, be made after processing with elasticity, insulating properties, impermeable water and air material.It is elastomeric macromolecule
Compound.Rubber is divided into natural rubber and two kinds of synthetic rubber.Natural rubber is to extract glue from the plants such as rubber tree, kok-saghyz
Matter post-processing is made；Synthetic rubber is then obtained by the aggregated reaction of various monomers.
With the development of science and technology, the performance requirement of the isolation protective material of the industries such as electric power, electronic apparatus is higher (such as
Service life, reactance voltage, heatproof, antifatigue etc.), but the rubber material bad mechanical strength occurred in existing market, impact resistance
Performance is weaker and self-healing properties are poor, is unable to satisfy the requirement of these special dimensions.
Summary of the invention
In order to overcome above-mentioned technical problem, the present invention provides a kind of self-repair type environment-protective rubber material and its preparation side
Method.By the way that modified magnalium hydrotalcite and nanometer silicon rubber/fluorubber blend compounds are added, it is prepared for a kind of self-repair type environmental protection rubber
Glue, since its molecular weight is larger, molecule is with the presence of random coil Coiling-type, due to the work of a large amount of branches when by external force
With improving stronger mechanical performance, generate strong recovery tendency, there is excellent self-healing properties.
The purpose of the present invention can be achieved through the following technical solutions:
Self-repair type environment-protective rubber material is made of following raw material: 75-100 parts of nanometer silicon rubber/fluorubber are simultaneously
With glue, 15-20 parts of emulsifiers, 55-80 parts of polyethylene, 25-50 parts of alumina powders, 15-20 parts of diethyl phthalates, 35-
50 parts of nitric acid magnesium dusts, 15-25 parts of nitric acid aluminium powders, 5-15 parts of adhesive；
The self-repair type environment-protective rubber material is made by the following method:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, adds after at the uniform velocity stirring 15min
Enter nitric acid aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) carbonic acid is added into mixed solution
Hydrogen sodium is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；(C)
Mixed solution is transferred in the autoclave with stirring, dynamic crystallization 8h in 80 DEG C of baking ovens is put into, is taken out, is filtered after standing 12h,
High speed centrifugation is carried out with the revolving speed of 10000r/min, sediment is washed with deionized, is dried, magnalium hydrotalcite is made；Nitric acid
Magnesium, deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, is at the uniform velocity stirred
At slurries, single month silicic acid glycerol vinegar is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times,
It is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol
Vinegar weight ratio is 1: 5: 1；
Step S3, mixer will be added after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding
In, by open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, emulsifier and adhesive is added, mixing is equal
It is added in mixer after even and sizing material is made through open mill compression molding；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
Hydrotalcite is a kind of layer dihydroxy metal oxide, is a kind of anion type laminated compound, due to its uniqueness
Layer structure so have good thermal stability and memory performance, prepare magnalium hydrotalcite with the precipitation method, it is brilliant to pass through dynamic
Change and the magnalium hydrotalcite content of static burn in preparation is higher than conventional method and purity is higher, but magnalium hydrotalcite surface
Hydroxyl can interact with magnesium-aluminum metal cation, generate octahedral ligand structure, be not easy to disperse so as to cause magnalium hydrotalcite
And do not have compatibility, magnalium hydrotalcite is modified by single month silicic acid glycerol vinegar, the carboxylic on single month silicic acid glycerol vinegar surface
Base reacts with magnalium hydrotalcite surface hydroxyl so that magnalium hydrotalcite not will form octahedral ligand structure, metal sun from
Son combines negative electrical charge to reach stable state, to obtain easily dispersing to be provided with the modification magnalium hydrotalcite of good affinity.
Further, the nanometer silicon rubber/fluorubber blend compounds are made by the following method:
(1) 50mL dimethyl silicone polymer pours into three-necked flask, and 100mL methyl vinyl silicon oil, 60 DEG C of water-baths are added
3g stannous chloride is added after heating 50min, at the uniform velocity stirring 15min, is transferred in beaker, is heated to 80 DEG C, it is different that 5mL is added
Propyl alcohol controls vacuum degree -0.10MPa to be transferred in reaction kettle after the revolving speed high-speed stirred 30min of 1200r/min, and temperature is
It 100 DEG C, is taken out after reacting 2h, 10mL glycerol is added, at the uniform velocity stirred 10min after standing 30min, obtain complex colloid；
(2) complex colloid is added in mixer, sets roll spacing 3.5mm, 80 DEG C of temperature, is added after forming packet roller
10mLKH550 is kneaded 30min, and 15g sulphur is added, and is kneaded 25min, takes out, and is transferred to addition 15g sodium thiosulfate in beaker,
It is added in mixer after stirring 30min with the revolving speed of 800r/min, is taken out after being kneaded 30min, stand 1h, be added in centrifuge,
Carry out high speed centrifugation with the revolving speed of 12000r/min, with washes of absolute alcohol three times after, be placed in 80 DEG C of drying boxes dry 4h, system
Obtain nanometer silicon rubber；
(3) nanometer silicon rubber and 20g fluorubber are mixed, is poured the mixture into ball mill, with the revolving speed of 1600r/min
High speed ball milling is carried out, is added after ball milling in the beaker equipped with 100mL dehydrated alcohol, 10g epoxy resin, ultrasound is added
30min extracts the air in mixed liquor out, is transferred in vacuum oven, controls vacuum degree -0.09MPa, and temperature is 65 DEG C, does
Nanometer silicon rubber/fluorubber the blend compounds are made in dry 12h.
Silicon rubber has good weather resistance and excellent chemical stability, but silicon rubber is using silicon oxygen bond as main chain
Polymer, surface is there are great amount of hydroxy group, easily generation agglomeration, and fluorubber on the carbon atom of its main chain or side chain due to containing
There is fluorine atom, so having excellent heat resistance, inoxidizability, oil resistivity, but since fluorubber branch is largely assembled, is formed
Random special construction causes fluorubber resistance to low temperature poor；The silicon rubber of preparation exists with nano shape, can preferably with
Fluorubber copolymerization, forms a kind of nanometer of silicon rubber/fluorubber blend compounds.
The emulsifier be one or more of soybean lecithin, lauric monoglyceride, methyl glycol fatty acid ester, it is described
Adhesive is one or more of polyphenylene oxide, fluororesin, polyphenylene sulfide.
The preparation method of self-repair type environment-protective rubber material, includes the following steps:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, adds after at the uniform velocity stirring 15min
Enter nitric acid aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) carbonic acid is added into mixed solution
Hydrogen sodium is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；(C)
Mixed solution is transferred in the autoclave with stirring, dynamic crystallization 8h in 80 DEG C of baking ovens is put into, is taken out, is filtered after standing 12h,
High speed centrifugation is carried out with the revolving speed of 10000r/min, sediment is washed with deionized, is dried, magnalium hydrotalcite is made；Nitric acid
Magnesium, deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, is at the uniform velocity stirred
At slurries, single month silicic acid glycerol vinegar is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times,
It is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol
Vinegar weight ratio is 1: 5: 1；
Step S3, mixer will be added after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding
In, by open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, emulsifier and adhesive is added, mixing is equal
It is added in mixer after even and sizing material is made through open mill compression molding；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
Further, extrusion device described in step S5 includes extrusion mechanism, transport establishment and feeding mechanism, the charging
Mechanism is mounted on the left of extrusion mechanism, and the transport establishment is mounted on the right side of extrusion mechanism, the transport establishment and extrusion mechanism
Connection；
The extrusion mechanism includes extruded tube, die head, motor, feed inlet, the first support column, pedestal, fixed link, baffle,
The extruded tube is fixed by the connecting rod in baffle upper surface, and the extruded tube right lateral surface connects die head, and the extruded tube is left
Side surface connects motor, and the motor is fixed on baffle upper surface, and the feed inlet is mounted on extruded tube surface, the feed inlet
Bottom end is mounted on inside extruded tube, and the baffle lower surface connects the first support column, and first support top end is fixed on gear
Intralamellar part, first support column bottom end connect pedestal, are fixed between first support column by fixed link；
The transport establishment includes driving drum, conveyer belt, water inlet pipe, pond, support rod, non-slip mat, the transmission rolling
Cylinder is fixed on supporting bar top, and the conveyer belt is coated on driving drum surface, and the connection of support rod bottom end lower surface is anti-skidding
Pad, the pond are mounted below conveyer belt center, and described water inlet pipe one end is mounted on basin bottom, and the water inlet pipe is another
One end is mounted on inside extruded tube, and the transport establishment is connect by water inlet pipe with extrusion mechanism；
The feeding mechanism includes deduster, blower, feed pipe, pedestal, the second support column, discharge gate, feed opening, described
Deduster is fixed on above pedestal by the second support column, and surface, the feed opening are mounted on the assembling on the base
Deduster left end upper surface, the feed opening bottom are mounted on inside deduster, and the feed pipe is mounted on above deduster, institute
It states discharge gate to connect with feed pipe, the discharge gate and feed inlet are oppositely arranged.
Further, described driving drum or so is oppositely arranged, and described support rod or so is oppositely arranged.
Further, the feed pipe left end connects deduster, and the feed pipe right end connects discharge gate.
Beneficial effects of the present invention:
(1) of the invention by the way that modified magnalium hydrotalcite and nanometer silicon rubber/fluorubber blend compounds are added, it is prepared for one kind certainly
Repairing type environment-friendly rubber, since its molecular weight is larger, molecule is with the presence of random coil Coiling-type, due to big when by external force
The effect for measuring branch, improves stronger mechanical performance, generates strong recovery tendency, there is excellent self-healing properties；
(2) by the way that silicon rubber and fluorubber are carried out ball milling, using epoxy resin as curing agent, formed a kind of silicon rubber/
Fluorubber blend compounds had not only remained the good chemical stability of silicon rubber and electrical property, but also remained the excellent resistance to height of fluorubber
Warm nature energy is prepared for a kind of comprehensive silicon rubber of performance/fluorubber blend compounds；
(3) present invention carries out rubber material preparation by extrusion device when preparing self-repair type environment-protective rubber material, should
Device is provided with dust-extraction unit and is dusted to rubber material, and impurity is avoided to be mixed into rubber to influence self-repair type environment-friendly rubber
The performance of material, device extrusion effect is good, can shorten process time, improves rubber extruding efficiency.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, will be described below to embodiment required
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is extrusion device structural schematic diagram；
Fig. 2 is extrusion device extruded tube structural schematic diagram；
In figure: 1, extrusion mechanism；11, extruded tube；12, die head；13, motor；14, feed inlet；15, the first support column；16,
Pedestal；17, fixed link；18, baffle；2, transport establishment；21, driving drum；22, conveyer belt；23, water inlet pipe；24, pond；25,
Support rod；26, non-slip mat；3, feeding mechanism；31, deduster；32, blower；33, feed pipe；34, pedestal；35, the second support
Column；36, discharge gate；37, feed opening.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Please refer to Fig. 1, shown in 2, extrusion device includes extrusion mechanism 1, transport establishment 2 and feeding mechanism 3, feeding mechanism 3
It is mounted on 1 left side of extrusion mechanism, transport establishment 2 is mounted on 1 right side of extrusion mechanism, and transport establishment 2 connect with extrusion mechanism 1；
As shown in Figure 1, 2, extrusion mechanism 1 includes extruded tube 11, die head 12, motor 13, feed inlet 14, the first support column
15, pedestal 16, fixed link 17, baffle 18, extruded tube 11 are fixed by the connecting rod in 18 upper surface of baffle, 11 right side table of extruded tube
Face connects die head 12, and 11 left-hand face of extruded tube connects motor 13, and motor 13 is fixed on 18 upper surface of baffle, and feed inlet 14 is installed
On 11 surface of extruded tube, 14 bottom end of feed inlet is mounted on inside extruded tube 11, and 18 lower surface of baffle connects the first support column 15, the
One support column, 15 top is fixed on inside baffle 18, and 15 bottom end of the first support column connects pedestal 16, is led between the first support column 15
Fixed link 17 is crossed to be fixed；
As shown in Figure 1, transport establishment 2 include driving drum 21, conveyer belt 22, water inlet pipe 23, pond 24, support rod 25,
Non-slip mat 26, driving drum 21 are fixed on 25 top of support rod, and driving drum 21 or so is oppositely arranged, and conveyer belt 22 is coated on biography
Dynamic 21 surface of roller, support rod 25 or so are oppositely arranged, and 25 bottom end lower surface of support rod connects non-slip mat 26, and pond 24 is mounted on
Below 22 center of conveyer belt, 23 one end of water inlet pipe is mounted on 24 bottom of pond, and 23 other end of water inlet pipe is mounted on extruded tube
Inside 11, transport establishment 2 is connect by water inlet pipe 23 with extrusion mechanism 1；
As shown in Figure 1, feeding mechanism 3 include deduster 31, blower 32, feed pipe 33, pedestal 34, the second support column 35,
Discharge gate 36, feed opening 37, deduster 31 are fixed on 34 top of pedestal by the second support column 35, and blower 32 is mounted on pedestal 34
Upper surface, feed opening 37 are mounted on 31 left end upper surface of deduster, and 37 bottom of feed opening is mounted on inside deduster 31, feed pipe
33 are mounted on 31 top of deduster, and 33 left end of feed pipe connects deduster 31, and 33 right end of feed pipe connects discharge gate 36, discharge gate
36 and feed inlet 14 be oppositely arranged.
Embodiment 1
Self-repair type environment-protective rubber material is made of following raw material: 75 parts of nanometer silicon rubber/fluorubber are used in combination
Glue, 15 parts of methyl glycol fatty acid esters, 55 parts of polyethylene, 25 parts of alumina powders, 15 parts of diethyl phthalates, 35 parts of magnesium nitrates
Powder, 15 parts of nitric acid aluminium powders, 5 parts of polyphenylene oxide；
The self-repair type environment-protective rubber material is made by the following method:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, adds after at the uniform velocity stirring 15min
Enter nitric acid aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) carbonic acid is added into mixed solution
Hydrogen sodium is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；(C)
Mixed solution is transferred in the autoclave with stirring, dynamic crystallization 8h in 80 DEG C of baking ovens is put into, is taken out, is filtered after standing 12h,
High speed centrifugation is carried out with the revolving speed of 10000r/min, sediment is washed with deionized, is dried, magnalium hydrotalcite is made；Nitric acid
Magnesium, deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, is at the uniform velocity stirred
At slurries, single month silicic acid glycerol vinegar is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times,
It is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol
Vinegar weight ratio is 1: 5: 1；
Step S3, mixer will be added after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding
In, by open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, methyl glycol fatty acid ester and polyphenyl is added
Ether is added in mixer sizing material is made through open mill compression molding after mixing；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
Nanometer silicon rubber/fluorubber blend compounds are made by the following method:
(1) 50mL dimethyl silicone polymer pours into three-necked flask, and 100mL methyl vinyl silicon oil, 60 DEG C of water-baths are added
3g stannous chloride is added after heating 50min, at the uniform velocity stirring 15min, is transferred in beaker, is heated to 80 DEG C, it is different that 5mL is added
Propyl alcohol controls vacuum degree -0.10MPa to be transferred in reaction kettle after the revolving speed high-speed stirred 30min of 1200r/min, and temperature is
It 100 DEG C, is taken out after reacting 2h, 10mL glycerol is added, at the uniform velocity stirred 10min after standing 30min, obtain complex colloid；
(2) complex colloid is added in mixer, sets roll spacing 3.5mm, 80 DEG C of temperature, is added after forming packet roller
10mLKH550 is kneaded 30min, and 15g sulphur is added, and is kneaded 25min, takes out, and is transferred to addition 15g sodium thiosulfate in beaker,
It is added in mixer after stirring 30min with the revolving speed of 800r/min, is taken out after being kneaded 30min, stand 1h, be added in centrifuge,
Carry out high speed centrifugation with the revolving speed of 12000r/min, with washes of absolute alcohol three times after, be placed in 80 DEG C of drying boxes dry 4h, system
Obtain nanometer silicon rubber；
(3) nanometer silicon rubber and 20g fluorubber are mixed, is poured the mixture into ball mill, with the revolving speed of 1600r/min
High speed ball milling is carried out, is added after ball milling in the beaker equipped with 100mL dehydrated alcohol, 10g epoxy resin, ultrasound is added
30min extracts the air in mixed liquor out, is transferred in vacuum oven, controls vacuum degree -0.09MPa, and temperature is 65 DEG C, does
Nanometer silicon rubber/fluorubber the blend compounds are made in dry 12h.
Embodiment 2
Self-repair type environment-protective rubber material is made of following raw material: 80 parts of nanometer silicon rubber/fluorubber are used in combination
Glue, 16 parts of methyl glycol fatty acid esters, 60 parts of polyethylene, 30 parts of alumina powders, 18 parts of diethyl phthalates, 40 parts of magnesium nitrates
Powder, 18 parts of nitric acid aluminium powders, 10 parts of polyphenylene oxide；
The self-repair type environment-protective rubber material is made by the following method:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, adds after at the uniform velocity stirring 15min
Enter nitric acid aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) carbonic acid is added into mixed solution
Hydrogen sodium is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；(C)
Mixed solution is transferred in the autoclave with stirring, dynamic crystallization 8h in 80 DEG C of baking ovens is put into, is taken out, is filtered after standing 12h,
High speed centrifugation is carried out with the revolving speed of 10000r/min, sediment is washed with deionized, is dried, magnalium hydrotalcite is made；Nitric acid
Magnesium, deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, is at the uniform velocity stirred
At slurries, single month silicic acid glycerol vinegar is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times,
It is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol
Vinegar weight ratio is 1: 5: 1；
Step S3, mixer will be added after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding
In, by open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, methyl glycol fatty acid ester and polyphenyl is added
Ether is added in mixer sizing material is made through open mill compression molding after mixing；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
Embodiment 3
Self-repair type environment-protective rubber material is made of following raw material: 95 parts of nanometer silicon rubber/fluorubber are used in combination
Glue, 18 parts of methyl glycol fatty acid esters, 70 parts of polyethylene, 40 parts of alumina powders, 18 parts of diethyl phthalates, 40 parts of magnesium nitrates
Powder, 20 parts of nitric acid aluminium powders, 12 parts of polyphenylene oxide；
The self-repair type environment-protective rubber material is made by the following method:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, adds after at the uniform velocity stirring 15min
Enter nitric acid aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) carbonic acid is added into mixed solution
Hydrogen sodium is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；(C)
Mixed solution is transferred in the autoclave with stirring, dynamic crystallization 8h in 80 DEG C of baking ovens is put into, is taken out, is filtered after standing 12h,
High speed centrifugation is carried out with the revolving speed of 10000r/min, sediment is washed with deionized, is dried, magnalium hydrotalcite is made；Nitric acid
Magnesium, deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, is at the uniform velocity stirred
At slurries, single month silicic acid glycerol vinegar is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times,
It is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol
Vinegar weight ratio is 1: 5: 1；
Step S3, mixer will be added after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding
In, by open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, methyl glycol fatty acid ester and polyphenyl is added
Ether is added in mixer sizing material is made through open mill compression molding after mixing；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
Embodiment 4
Self-repair type environment-protective rubber material is made of following raw material: 100 parts of nanometer silicon rubber/fluorubber are used in combination
Glue, 20 parts of methyl glycol fatty acid esters, 80 parts of polyethylene, 50 parts of alumina powders, 20 parts of diethyl phthalates, 50 parts of magnesium nitrates
Powder, 25 parts of nitric acid aluminium powders, 15 parts of polyphenylene oxide；
The self-repair type environment-protective rubber material is made by the following method:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, adds after at the uniform velocity stirring 15min
Enter nitric acid aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) carbonic acid is added into mixed solution
Hydrogen sodium is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；(C)
Mixed solution is transferred in the autoclave with stirring, dynamic crystallization 8h in 80 DEG C of baking ovens is put into, is taken out, is filtered after standing 12h,
High speed centrifugation is carried out with the revolving speed of 10000r/min, sediment is washed with deionized, is dried, magnalium hydrotalcite is made；Nitric acid
Magnesium, deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, is at the uniform velocity stirred
At slurries, single month silicic acid glycerol vinegar is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times,
It is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol
Vinegar weight ratio is 1: 5: 1；
Step S3, mixer will be added after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding
In, by open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, methyl glycol fatty acid ester and polyphenyl is added
Ether is added in mixer sizing material is made through open mill compression molding after mixing；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
Comparative example 1
The self-repair type environment-protective rubber material of this comparative example preparation compared with Example 1, lacks modified magnalium in step S2
Hydrotalcite.
Comparative example 2
The self-repair type environment-protective rubber material of this comparative example preparation compared with Example 1, lacks step (3), does not prepare and receive
Rice silicon rubber/fluorubber blend compounds.
Comparative example 3
This comparative example is one of market rubber material.
Temperature resistant range is carried out to self-repair type environment-friendly rubber prepared by embodiment 1-4 and comparative example 1-3, tensile property, is returned
Elasticity and elongation at break are detected, as a result as shown in table 1 below:
Temperature resistant range: self-repair type environment-protective rubber material is tested according to GB/T15256-1994.
Tensile property: self-repair type environment-protective rubber material is tested according to GB/T528-1998.
Resilience: self-repair type environment-protective rubber material is tested according to GB/T1681-1991.
Breaking strength: self-repair type environment-protective rubber material is tested according to GB/T582-2009.
Table 1
The resistance to heat rating of self-repair type environment-protective rubber material of embodiment 1-4 preparation is at -63 DEG C -254 as can be seen from Table 1
Between DEG C, the resistance to heat rating of comparative example 1-3 is between -48 DEG C -220 DEG C；The self-repair type environment-friendly rubber material of embodiment 1-4 preparation
Tensile strength is expected between 6.1-8.7MPa range, and the tensile strength of comparative example 1-3 is between 5.3-5.9MPa range；Embodiment
The self-repair type environment-protective rubber material resilience of 1-4 preparation is stronger, and self-repair type environment-protective rubber material prepared by comparative example 1,2 returns
Elasticity is weaker, and 3 resilience of comparative example is general；The self-repair type environment-protective rubber material breaking strength of embodiment 1-4 preparation is in 230-
Within the scope of 261kg, comparative example 1-3 breaking strength is within the scope of 208-223kg；So self-repair type environmental protection rubber prepared by the present invention
Glue material has excellent mechanical performance, and resistance to temperature change can by force and screen resilience is strong, and self-healing properties are higher, and it is special to be suitable for
Industrial circle.
The extrusion device course of work is as follows:
It feeds intake from feed opening 37, deduster 31 is started to work, and material is dusted by deduster 31, passes through charging
Pipe 33 and discharge gate 36 enter feed inlet 14, enter extruded tube 11 later, and motor 13 starts turning, and extrusion mechanism 1 is driven to run,
Water in pond 24 is entered in extruded tube 11 by water inlet pipe 23, and material is extruded mixing, extruded tube 11 inside extruded tube 11
Start rotation and material is discharged by die head 12, material falls into 22 surface of conveyer belt, and driving drum 21 rotates clockwise, and drives and passes
Band 22 is sent to rotate clockwise, so that material is detached from transport establishment 2.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (6)
1. self-repair type environment-protective rubber material, which is characterized in that be made of following raw material: 75-100 parts of nano-silicon rubbers
Glue/fluorubber blend compounds, 15-20 parts of emulsifiers, 55-80 parts of polyethylene, 25-50 parts of alumina powders, 15-20 parts of phthalic acids
Diethylester, 35-50 parts of nitric acid magnesium dusts, 15-25 parts of nitric acid aluminium powders, 5-15 parts of adhesive；
The self-repair type environment-protective rubber material is made by the following method:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in deionized water, nitre is added after at the uniform velocity stirring 15min
Sour aluminium powder, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) sodium bicarbonate is added into mixed solution,
60 DEG C are warming up to, 10min is stirred, 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；It (C) will mixing
Solution is transferred in the autoclave with stirring, is put into dynamic crystallization 8h in 80 DEG C of baking ovens, is taken out, and is filtered after standing 12h, with
The revolving speed of 10000r/min carries out high speed centrifugation, and sediment is washed with deionized, and dries, and magnalium hydrotalcite is made；Magnesium nitrate,
Deionized water and sodium bicarbonate weight ratio are 1: 8: 2；
Step S2, modified magnalium hydrotalcite: magnalium hydrotalcite is added equipped in the beaker in deionized water, at the uniform velocity stirring is slurried
Single month silicic acid glycerol vinegar is added in liquid, 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized three times, is placed in
Dry 5h in 100 DEG C of drying boxes, is made modified magnalium hydrotalcite；Magnalium hydrotalcite, deionized water and single month silicic acid glycerol vinegar weight
Amount is than being 1: 5: 1；
Step S3, it will be added in mixer after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding,
By open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, emulsifier and adhesive is added, after mixing
It is added in mixer and sizing material is made through open mill compression molding；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
2. self-repair type environment-protective rubber material according to claim 1, which is characterized in that the nanometer silicon rubber/fluorine rubber
Glue blend compounds are made by the following method:
(1) 50mL dimethyl silicone polymer pours into three-necked flask, and 100mL methyl vinyl silicon oil, 60 DEG C of heating water baths are added
3g stannous chloride is added after 50min, at the uniform velocity stirring 15min, is transferred in beaker, is heated to 80 DEG C, 5mL isopropyl is added
Alcohol controls vacuum degree -0.10MPa to be transferred in reaction kettle after the revolving speed high-speed stirred 30min of 1200r/min, and temperature is
It 100 DEG C, is taken out after reacting 2h, 10mL glycerol is added, at the uniform velocity stirred 10min after standing 30min, obtain complex colloid；
(2) complex colloid is added in mixer, sets roll spacing 3.5mm, 80 DEG C of temperature, adds 10mLKH550 after forming packet roller,
It is kneaded 30min, 15g sulphur is added, is kneaded 25min, is taken out, addition 15g sodium thiosulfate in beaker is transferred to, with 800r/min
Revolving speed stirring 30min after be added mixer in, be kneaded 30min after take out, stand 1h, be added centrifuge in, with 12000r/
The revolving speed of min carries out high speed centrifugation, with washes of absolute alcohol three times after, be placed in 80 DEG C of drying boxes dry 4h, nano-silicon be made
Rubber；
(3) nanometer silicon rubber and 20g fluorubber are mixed, is poured the mixture into ball mill, carried out with the revolving speed of 1600r/min
High speed ball milling is added after ball milling in the beaker equipped with 100mL dehydrated alcohol, and 10g epoxy resin is added, and ultrasonic 30min takes out
Air in mixed liquor out, is transferred in vacuum oven, controls vacuum degree -0.09MPa, and temperature is 65 DEG C, dry 12h, system
Obtain the nanometer silicon rubber/fluorubber blend compounds.
3. the preparation method of self-repair type environment-protective rubber material, which comprises the steps of:
Step S1, prepared by magnalium hydrotalcite: (a) nitric acid magnesium dust being added in 100mL deionized water, after at the uniform velocity stirring 15min
Nitric acid aluminium powder is added, 40 DEG C of heating water baths are spare to being completely dissolved to obtain mixed solution；(b) 10g is added into mixed solution
Sodium bicarbonate is warming up to 60 DEG C, stirs 10min, and 10% sodium hydroxide solution is added and adjusts mixed solution pH until pH is 8-10；
(C) mixed solution is transferred in the autoclave with stirring, is put into dynamic crystallization 8h in 80 DEG C of baking ovens, taken out, stand mistake after 12h
Filter carries out high speed centrifugation with the revolving speed of 10000r/min, sediment is washed with deionized, dry, magnalium hydrotalcite is made；
Step S2, modified magnalium hydrotalcite: 20g magnalium hydrotalcite is taken to be added in the beaker being equipped in 100mL deionized water, at the uniform velocity
Slurries are stirred into, mono- month silicic acid glycerol vinegar of 5g is added in 60 DEG C of heating water baths, stirs 45min, and vacuum filtration is washed with deionized water
It washs three times, is placed in 100 DEG C of drying boxes dry 5h, modified magnalium hydrotalcite is made；
Step S3, it will be added in mixer after nanometer silicon rubber/fluorubber blend compounds, alumina powder and polyethylene co-grinding,
By open mill compression molding, rubber master batch is made；
Step S4, rubber master batch is taken out into beaker, diethyl phthalate, emulsifier and adhesive is added, after mixing
It is added in mixer and sizing material is made through open mill compression molding；
Step S5, sizing material is placed in extrusion device, extrusion molding, the self-repair type environment-protective rubber material is made.
4. the preparation method of self-repair type environment-protective rubber material according to claim 3, which is characterized in that institute in step S5
Stating extrusion device includes extrusion mechanism (1), transport establishment (2) and feeding mechanism (3), and the feeding mechanism (3) is mounted on extrusion
On the left of mechanism (1), the transport establishment (2) is mounted on the right side of extrusion mechanism (1), the transport establishment (2) and extrusion mechanism (1)
Connection；
The extrusion mechanism (1) includes extruded tube (11), die head (12), motor (13), feed inlet (14), the first support column
(15), pedestal (16), fixed link (17), baffle (18), the extruded tube (11) are fixed by the connecting rod the table on baffle (18)
Face, extruded tube (11) right lateral surface connect die head (12), and extruded tube (11) left-hand face connects motor (13), described
Motor (13) is fixed on baffle (18) upper surface, and the feed inlet (14) is mounted on extruded tube (11) surface, the feed inlet
(14) bottom end is mounted on extruded tube (11) inside, and baffle (18) lower surface connects the first support column (15), and described first
Dagger (15) top is fixed on baffle (18) inside, and the first support column (15) bottom end connects pedestal (16), and described first
It is fixed between dagger (15) by fixed link (17)；
The transport establishment (2) includes driving drum (21), conveyer belt (22), water inlet pipe (23), pond (24), support rod
(25), non-slip mat (26), the driving drum (21) are fixed on support rod (25) top, and the conveyer belt (22) is coated on transmission
Roller (21) surface, support rod (25) the bottom end lower surface connect non-slip mat (26), and the pond (24) is mounted on conveyer belt
(22) below center, described water inlet pipe (23) one end is mounted on pond (24) bottom, water inlet pipe (23) other end peace
Internal mounted in extruded tube (11), the transport establishment (2) is connect by water inlet pipe (23) with extrusion mechanism (1)；
The feeding mechanism (3) includes deduster (31), blower (32), feed pipe (33), pedestal (34), the second support column
(35), discharge gate (36), feed opening (37), the deduster (31) are fixed on pedestal (34) by the second support column (35)
Side, the blower (32) are mounted on pedestal (34) upper surface, and the feed opening (37) is mounted on deduster (31) left end upper surface,
Feed opening (37) bottom is mounted on deduster (31) inside, and the feed pipe (33) is mounted on above deduster (31), institute
It states discharge gate (36) to connect with feed pipe (33), the discharge gate (36) and feed inlet (14) are oppositely arranged.
5. the preparation method of self-repair type environment-protective rubber material according to claim 4, which is characterized in that the transmission rolling
Cylinder (21) left and right is oppositely arranged, and support rod (25) left and right is oppositely arranged.
6. the preparation method of self-repair type environment-protective rubber material according to claim 4, which is characterized in that the feed pipe
(33) left end connection deduster (31), feed pipe (33) right end connect discharge gate (36).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111423795A (en) * | 2020-05-25 | 2020-07-17 | 朱小丽 | Environment-friendly waterproof building coating for wall surface and preparation method thereof |
| CN113024925A (en) * | 2021-03-15 | 2021-06-25 | 四川汇利实业有限公司 | Modified PE film capable of improving self-repairing performance and preparation method thereof |
| CN113043691A (en) * | 2021-03-15 | 2021-06-29 | 四川汇利实业有限公司 | Oral liquid multilayer composite hard tablet and preparation method thereof |
| CN114347617A (en) * | 2021-03-15 | 2022-04-15 | 四川汇利实业有限公司 | Self-repairing PET-AL-PE composite film for flexible package and preparation method thereof |
-
2019
- 2019-03-19 CN CN201910209029.3A patent/CN109880220A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111423795A (en) * | 2020-05-25 | 2020-07-17 | 朱小丽 | Environment-friendly waterproof building coating for wall surface and preparation method thereof |
| CN113024925A (en) * | 2021-03-15 | 2021-06-25 | 四川汇利实业有限公司 | Modified PE film capable of improving self-repairing performance and preparation method thereof |
| CN113043691A (en) * | 2021-03-15 | 2021-06-29 | 四川汇利实业有限公司 | Oral liquid multilayer composite hard tablet and preparation method thereof |
| CN114347617A (en) * | 2021-03-15 | 2022-04-15 | 四川汇利实业有限公司 | Self-repairing PET-AL-PE composite film for flexible package and preparation method thereof |
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Application publication date: 20190614 |