CN109266017A - The preparation method of high-intensitive, high performance rubber material - Google Patents
The preparation method of high-intensitive, high performance rubber material Download PDFInfo
- Publication number
- CN109266017A CN109266017A CN201811144992.XA CN201811144992A CN109266017A CN 109266017 A CN109266017 A CN 109266017A CN 201811144992 A CN201811144992 A CN 201811144992A CN 109266017 A CN109266017 A CN 109266017A
- Authority
- CN
- China
- Prior art keywords
- rubber
- mixing
- stalk
- semi
- stage
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of high-intensitive, high performance rubber material, include the following steps: to provide stalk, and carry out nanosizing processing to stalk；Stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing, obtain the first mixture；Ball milling is carried out to the first mixture, obtains the first solid additive；Glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil and processing aid are mixed, the second mixture is obtained；High-speed stirred is carried out to the second mixture, obtains Second addition；Methyl phenyl vinyl silicone rubber is provided；P-methylphenyl vinylsiloxane rubber carries out multistage mixing；Second addition is added into the rubber compound being kneaded by second stage, then carries out phase III mixing, obtains semi-finished product silicon rubber；Double of finished product silicon rubber carries out heat-treated under medium temperature；First stage cure is carried out to medium temperature treated semi-finished product silicon rubber, obtains semi silicon sulfide rubber；And second stage vulcanization is carried out to semi silicon sulfide rubber.
Description
Technical field
The invention belongs to advanced technical field of rubber material, are related to a kind of preparation of high-intensitive, high performance rubber material
Method.
Background technique
Filling molecule is as reinforcing agent in macromolecule matrix, the composite material that processability is excellent, biodegradable
It is a big hot spot of high molecular material area research in recent years.The filler that initial people use is mainly inorganic mineral, than
Such as carbon black, kaolinite, silicate and clay.But most of such filler can endanger environment, or even human body can be threatened strong
Health.Twentieth century middle and later periods, the shallow lake that northern US area scholar once utilized starch to replace carbon black research that crosslinking is added in rubber
The variation of the reinforcing effect of rubber after powder xanthate, the results showed that, the reinforcement that starch xanthate and intermediate carbon black generate is made
With identical.The process of rubber due to starch derivatives addition and changed, to be opened for the preparation of powdered rubber
Issue a kind of both simple and economic feasible new way.Crosslinking xanthan acid diester containing 3-5% starch and 95~97% rubber
Starch/rubber co-precipitate can not only be blended easily with various rubber chemicals, but also can be processed into various
The rubber product that various kinds is had excellent performance.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of high-intensitive, high performance rubber material, to overcome existing
There is the problem of technology.
To achieve the above object, the present invention provides a kind of preparation methods of high-intensitive, high performance rubber material, including
Following steps: stalk is provided, and nanosizing processing is carried out to stalk；Stalk, alumina silicate fibre of the mixing by nanosizing processing
And carbon black, obtain the first mixture；Ball milling is carried out to the first mixture, obtains the first solid additive；Mix glutamic acid lanthanum
(DAGLa), vulcanizing agent, hydroxy silicon oil and processing aid obtain the second mixture；High-speed stirred is carried out to the second mixture,
Obtain Second addition；Methyl phenyl vinyl silicone rubber is provided；P-methylphenyl vinylsiloxane rubber carries out multistage mixing,
Wherein, when p-methylphenyl vinylsiloxane rubber carries out first stage mixing, the first solid additive is added into rubber compound,
Second stage mixing then is carried out to the rubber compound of the first solid additive of addition；Into the rubber compound being kneaded by second stage
Second addition is added, then carries out phase III mixing, obtains semi-finished product silicon rubber；Double of finished product silicon rubber carries out at medium temperature
Reason；First stage cure is carried out to medium temperature treated semi-finished product silicon rubber, obtains semi silicon sulfide rubber；And double of silicon sulfide
Rubber carries out second stage vulcanization, obtains high-intensitive, high performance rubber material.
Preferably, in above-mentioned technical proposal, nanosizing processing is carried out to stalk and includes the following steps: to crush stalk, and
Stalk after crushing is mixed with nanosizing processing auxiliary agent, obtains mixed solution, wherein it includes hydrogen-oxygen that nanosizing, which handles auxiliary agent,
Change sodium solution and hydrogen peroxide；Mixed solution is stirred by ultrasonic；Filtering ultrasonic agitation after mixed solution, obtain by
The stalk of nanosizing processing.
Preferably, in above-mentioned technical proposal, wherein include stalk 30-50g in every 100mL mixed solution, sodium hydroxide is molten
Liquid 40-60mL, remaining is hydrogen peroxide, ultrasonic agitation specifically comprises the processes of: ultraviolet light irradiation is carried out in ultrasonic agitation, ultraviolet light shines
Penetrating power is 30-50W, and ultrasonic agitation power is 800-1000W, and the ultrasonic agitation time is 5-8h.
Preferably, in above-mentioned technical proposal, in the first mixture, in parts by weight, the stalk handled by nanosizing
10-30 parts are accounted for, alumina silicate fibre accounts for 10-30 parts, and carbon black accounts for 40-50 parts.
Preferably, in above-mentioned technical proposal, ball milling is carried out to first mixture specifically comprises the processes of: ball milling speed is
1000-1500r/min, ratio of grinding media to material 10:1-15:1, Ball-milling Time 25-35h, wherein in mechanical milling process, every ball milling 3 is small
When, suspend ball milling 20-30min.
Preferably, in above-mentioned technical proposal, in the second mixture, in parts by weight, glutamic acid lanthanum (DAGLa) accounts for 5-10
Part, vulcanizing agent account for 1-4 parts, 4-8 parts of hydroxy silicon oil, carry out high-speed stirred to the second mixture specifically comprises the processes of: mixing temperature
It is 60-80 DEG C, mixing machine revolving speed is 500-800rpm, incorporation time 10-15min.
Preferably, in above-mentioned technical proposal, the first stage is kneaded specifically comprises the processes of: melting temperature is 130-140 DEG C, is kneaded
Time is 10-20min；Second stage is kneaded specifically comprises the processes of: melting temperature is 140-150 DEG C, mixing time 5-10min；
Phase III is kneaded specifically comprises the processes of: melting temperature is 145-155 DEG C, mixing time 10-20min, wherein in every 100 weight
Part methyl phenyl vinyl silicone rubber in include 50-60 parts of the first solid additive, 8-12 parts of Second addition.
Preferably, in above-mentioned technical proposal, double of finished product silicon rubber carries out heat-treated under medium temperature specifically comprises the processes of: to semi-finished product
Silicon rubber is heat-treated, and heat treatment temperature is 130-150 DEG C, heat treatment time 20-30h.
Preferably, in above-mentioned technical proposal, the tool of first stage cure is carried out to medium temperature treated semi-finished product silicon rubber
Body technology are as follows: high temperature and pressure vulcanization, sulfide stress 5-8MPa, curing temperature are carried out to medium temperature treated semi-finished product silicon rubber
It is 160-180 DEG C.
Preferably, in above-mentioned technical proposal, second stage vulcanization is carried out to semi silicon sulfide rubber specifically comprises the processes of: will be partly
Sulphurated siliastic is put into baking oven, and curing temperature is 175-185 DEG C, vulcanization time 4-5h.
Compared with prior art, the preparation method of high-intensitive, high performance rubber material of the invention has following beneficial
Effect: silastic material is a kind of very important high molecular material, and many prior arts are all directed to silastic material and carry out
Research, wherein prior art CN105860536A discloses a kind of flame-retardant Ceramic silicon rubber, the defect of the prior art
Be: preparation process is complicated, and it is long that rubber is manufactured the time, due to need it is counter refined, so needs open kneading machine twice, lead
Cause a large amount of energy waste.Composition proportion falls behind, and has been solely focused on ceramic packing for the humidification of silicon rubber, but has not had
Pay attention to mixed problem of the ceramic packing in rubber, causes some ceramic packings to become the reinforced phase in rubber material, still
Some ceramic packings form reunion in rubber, cause the mechanical property at the certain positions of rubber poor, eventually lead to modified rubber
Differ larger between the actual strength of material and theoretical strength.The application is directed to problem of the prior art, proposes a kind of improvement
Rubber material preparation method.The application preparation process is relatively easy, and manufacturing cost is lower, and the rubbery intensity of the application is high,
Rubber material intensity and theoretical value are closer.
Detailed description of the invention
Fig. 1 is the preparation method flow chart of high-intensitive, high performance rubber material according to the present invention.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention
Shield range is not limited by the specific implementation.
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " includes " or its change
Changing such as "comprising" or " including " etc. will be understood to comprise stated element or component, and not exclude other members
Part or other component parts.
Fig. 1 is the preparation method flow chart of high-intensitive, high performance rubber material according to the present invention.As shown, this
The preparation method of high-intensitive, the high performance rubber material of invention includes the following steps:
Step 101: stalk being provided, and nanosizing processing is carried out to stalk；
Step 102: stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing obtain the first mixture；
Step 103: ball milling being carried out to the first mixture, obtains the first solid additive；
Step 104: mixing glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil and processing aid obtain the second mixing
Object；
Step 105: high-speed stirred being carried out to the second mixture, obtains Second addition；
Step 106: methyl phenyl vinyl silicone rubber is provided；
Step 107: p-methylphenyl vinylsiloxane rubber carries out multistage mixing, wherein in p-methylphenyl vinyl
When silicon rubber carries out first stage mixing, the first solid additive is added into rubber compound, then to addition the first solid addition
The rubber compound of agent carries out second stage mixing；
Step 108: Second addition is added into the rubber compound being kneaded by second stage, it is mixed then to carry out the phase III
Refining, obtains semi-finished product silicon rubber；
Step 109: double of finished product silicon rubber carries out heat-treated under medium temperature；
Step 110: first stage cure being carried out to medium temperature treated semi-finished product silicon rubber, obtains semi silicon sulfide rubber；
And
Step 111: second stage vulcanization being carried out to semi silicon sulfide rubber, obtains high-intensitive, high performance rubber material.
Embodiment 1
The preparation method of high-intensitive, high performance rubber material of the invention includes the following steps: offer stalk, and to straw
Stalk carries out nanosizing processing；Stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing, obtain the first mixture；
Ball milling is carried out to the first mixture, obtains the first solid additive；Mix glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil with
And processing aid, obtain the second mixture；High-speed stirred is carried out to the second mixture, obtains Second addition；Methylbenzene is provided
Base vinylsiloxane rubber；P-methylphenyl vinylsiloxane rubber carries out multistage mixing, wherein in p-methylphenyl vinyl silicon
When rubber carries out first stage mixing, the first solid additive is added into rubber compound, then to adding the first solid additive
Rubber compound carry out second stage mixing；Second addition is added into the rubber compound being kneaded by second stage, then carries out
Phase III is kneaded, and obtains semi-finished product silicon rubber；Double of finished product silicon rubber carries out heat-treated under medium temperature；To medium temperature treated semi-finished product
Silicon rubber carries out first stage cure, obtains semi silicon sulfide rubber；Second stage vulcanization is carried out to semi silicon sulfide rubber, obtains height
Intensity, high performance rubber material.Nanosizing processing is carried out to stalk to include the following steps: to crush stalk, and will crush it
Stalk afterwards is mixed with nanosizing processing auxiliary agent, obtains mixed solution, wherein it includes sodium hydroxide solution that nanosizing, which handles auxiliary agent,
And hydrogen peroxide；Mixed solution is stirred by ultrasonic；Mixed solution after filtering ultrasonic agitation, obtains by nanosizing
The stalk of reason.It wherein, include stalk 30g, sodium hydroxide solution 40mL in every 100mL mixed solution, remaining is hydrogen peroxide, ultrasound
Stirring specifically comprises the processes of: ultraviolet light irradiation is carried out in ultrasonic agitation, ultraviolet light irradiation power is 30W, and ultrasonic agitation power is
800W, ultrasonic agitation time are 5h.In the first mixture, in parts by weight, 10 parts are accounted for by the stalk that nanosizing is handled, silicon
Sour aluminum fiber accounts for 10 parts, and carbon black accounts for 40 parts.Ball milling is carried out to the first mixture specifically comprises the processes of: ball milling speed 1000r/
Min, ratio of grinding media to material 10:1, Ball-milling Time 25h, wherein in mechanical milling process, every ball milling 3 hours suspends ball milling 20min.?
In second mixture, in parts by weight, glutamic acid lanthanum (DAGLa) account for 5 parts, vulcanizing agent account for 1 part, 4 parts of hydroxy silicon oil, it is mixed to second
It closes object and carries out high-speed stirred specifically comprises the processes of: mixing temperature is 60 DEG C, and mixing machine revolving speed is 500rpm, and incorporation time is
10min.First stage is kneaded specifically comprises the processes of: melting temperature is 130 DEG C, mixing time 10min；Second stage is kneaded specific
Technique are as follows: melting temperature is 140 DEG C, mixing time 5min；Phase III is kneaded specifically comprises the processes of: and melting temperature is 145 DEG C,
Mixing time is 10min, wherein including the first solid additive 50 in the methyl phenyl vinyl silicone rubber of every 100 parts by weight
Part, 8 parts of Second addition.Double of finished product silicon rubber carries out heat-treated under medium temperature specifically comprises the processes of: double of finished product silicon rubber carries out heat
Processing, heat treatment temperature are 130 DEG C, heat treatment time 20h.First stage is carried out to medium temperature treated semi-finished product silicon rubber
Vulcanization specifically comprises the processes of: high temperature and pressure vulcanization, sulfide stress 5MPa, sulphur are carried out to medium temperature treated semi-finished product silicon rubber
Changing temperature is 160 DEG C.Second stage vulcanization is carried out to semi silicon sulfide rubber specifically comprises the processes of: semi silicon sulfide rubber is put into baking
Case, curing temperature are 175 DEG C, vulcanization time 4h.
Embodiment 2
The preparation method of high-intensitive, high performance rubber material of the invention includes the following steps: offer stalk, and to straw
Stalk carries out nanosizing processing；Stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing, obtain the first mixture；
Ball milling is carried out to the first mixture, obtains the first solid additive；Mix glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil with
And processing aid, obtain the second mixture；High-speed stirred is carried out to the second mixture, obtains Second addition；Methylbenzene is provided
Base vinylsiloxane rubber；P-methylphenyl vinylsiloxane rubber carries out multistage mixing, wherein in p-methylphenyl vinyl silicon
When rubber carries out first stage mixing, the first solid additive is added into rubber compound, then to adding the first solid additive
Rubber compound carry out second stage mixing；Second addition is added into the rubber compound being kneaded by second stage, then carries out
Phase III is kneaded, and obtains semi-finished product silicon rubber；Double of finished product silicon rubber carries out heat-treated under medium temperature；To medium temperature treated semi-finished product
Silicon rubber carries out first stage cure, obtains semi silicon sulfide rubber；Second stage vulcanization is carried out to semi silicon sulfide rubber, obtains height
Intensity, high performance rubber material.Nanosizing processing is carried out to stalk to include the following steps: to crush stalk, and will crush it
Stalk afterwards is mixed with nanosizing processing auxiliary agent, obtains mixed solution, wherein it includes sodium hydroxide solution that nanosizing, which handles auxiliary agent,
And hydrogen peroxide；Mixed solution is stirred by ultrasonic；Mixed solution after filtering ultrasonic agitation, obtains by nanosizing
The stalk of reason.It wherein, include stalk 50g, sodium hydroxide solution 60mL in every 100mL mixed solution, remaining is hydrogen peroxide, ultrasound
Stirring specifically comprises the processes of: ultraviolet light irradiation is carried out in ultrasonic agitation, ultraviolet light irradiation power is 50W, and ultrasonic agitation power is
1000W, ultrasonic agitation time are 8h.In the first mixture, in parts by weight, 30 parts are accounted for by the stalk that nanosizing is handled,
Alumina silicate fibre accounts for 30 parts, and carbon black accounts for 50 parts.Ball milling is carried out to the first mixture specifically comprises the processes of: ball milling speed 1500r/
Min, ratio of grinding media to material 15:1, Ball-milling Time 35h, wherein in mechanical milling process, every ball milling 3 hours suspends ball milling 30min.?
In second mixture, in parts by weight, glutamic acid lanthanum (DAGLa) account for 10 parts, vulcanizing agent account for 4 parts, 8 parts of hydroxy silicon oil, to second
Mixture carries out high-speed stirred specifically comprises the processes of: mixing temperature is 80 DEG C, and mixing machine revolving speed is 800rpm, and incorporation time is
15min.First stage is kneaded specifically comprises the processes of: melting temperature is 140 DEG C, mixing time 20min；Second stage is kneaded specific
Technique are as follows: melting temperature is 150 DEG C, mixing time 10min；Phase III is kneaded specifically comprises the processes of: melting temperature 155
DEG C, mixing time 20min, wherein including that the first solid adds in the methyl phenyl vinyl silicone rubber of every 100 parts by weight
60 parts of agent, 12 parts of Second addition.Double finished product silicon rubber carries out heat-treated under medium temperature specifically comprises the processes of: double of finished product silicon rubber into
Row heat treatment, heat treatment temperature are 150 DEG C, heat treatment time 30h.First is carried out to medium temperature treated semi-finished product silicon rubber
Stage vulcanization specifically comprises the processes of: high temperature and pressure vulcanization is carried out to medium temperature treated semi-finished product silicon rubber, sulfide stress is
8MPa, curing temperature are 180 DEG C.Second stage vulcanization is carried out to semi silicon sulfide rubber specifically comprises the processes of: by semi-cure silicon rubber
Glue is put into baking oven, and curing temperature is 185 DEG C, vulcanization time 5h.
Embodiment 3
The preparation method of high-intensitive, high performance rubber material of the invention includes the following steps: offer stalk, and to straw
Stalk carries out nanosizing processing；Stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing, obtain the first mixture；
Ball milling is carried out to the first mixture, obtains the first solid additive；Mix glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil with
And processing aid, obtain the second mixture；High-speed stirred is carried out to the second mixture, obtains Second addition；Methylbenzene is provided
Base vinylsiloxane rubber；P-methylphenyl vinylsiloxane rubber carries out multistage mixing, wherein in p-methylphenyl vinyl silicon
When rubber carries out first stage mixing, the first solid additive is added into rubber compound, then to adding the first solid additive
Rubber compound carry out second stage mixing；Second addition is added into the rubber compound being kneaded by second stage, then carries out
Phase III is kneaded, and obtains semi-finished product silicon rubber；Double of finished product silicon rubber carries out heat-treated under medium temperature；To medium temperature treated semi-finished product
Silicon rubber carries out first stage cure, obtains semi silicon sulfide rubber；Second stage vulcanization is carried out to semi silicon sulfide rubber, obtains height
Intensity, high performance rubber material.Nanosizing processing is carried out to stalk to include the following steps: to crush stalk, and will crush it
Stalk afterwards is mixed with nanosizing processing auxiliary agent, obtains mixed solution, wherein it includes sodium hydroxide solution that nanosizing, which handles auxiliary agent,
And hydrogen peroxide；Mixed solution is stirred by ultrasonic；Mixed solution after filtering ultrasonic agitation, obtains by nanosizing
The stalk of reason.It wherein, include stalk 35g, sodium hydroxide solution 45mL in every 100mL mixed solution, remaining is hydrogen peroxide, ultrasound
Stirring specifically comprises the processes of: ultraviolet light irradiation is carried out in ultrasonic agitation, ultraviolet light irradiation power is 35W, and ultrasonic agitation power is
850W, ultrasonic agitation time are 6h.In the first mixture, in parts by weight, 15 parts are accounted for by the stalk that nanosizing is handled, silicon
Sour aluminum fiber accounts for 15 parts, and carbon black accounts for 45 parts.Ball milling is carried out to the first mixture specifically comprises the processes of: ball milling speed 1200r/
Min, ratio of grinding media to material 12:1, Ball-milling Time 30h, wherein in mechanical milling process, every ball milling 3 hours suspends ball milling 25min.?
In second mixture, in parts by weight, glutamic acid lanthanum (DAGLa) account for 6 parts, vulcanizing agent account for 2 parts, 5 parts of hydroxy silicon oil, it is mixed to second
It closes object and carries out high-speed stirred specifically comprises the processes of: mixing temperature is 65 DEG C, and mixing machine revolving speed is 600rpm, and incorporation time is
12min.First stage is kneaded specifically comprises the processes of: melting temperature is 132 DEG C, mixing time 12min；Second stage is kneaded specific
Technique are as follows: melting temperature is 142 DEG C, mixing time 6min；Phase III is kneaded specifically comprises the processes of: and melting temperature is 148 DEG C,
Mixing time is 12min, wherein including the first solid additive 55 in the methyl phenyl vinyl silicone rubber of every 100 parts by weight
Part, 9 parts of Second addition.Double of finished product silicon rubber carries out heat-treated under medium temperature specifically comprises the processes of: double of finished product silicon rubber carries out heat
Processing, heat treatment temperature are 135 DEG C, heat treatment time 25h.First stage is carried out to medium temperature treated semi-finished product silicon rubber
Vulcanization specifically comprises the processes of: high temperature and pressure vulcanization, sulfide stress 6MPa, sulphur are carried out to medium temperature treated semi-finished product silicon rubber
Changing temperature is 165 DEG C.Second stage vulcanization is carried out to semi silicon sulfide rubber specifically comprises the processes of: semi silicon sulfide rubber is put into baking
Case, curing temperature are 170 DEG C, vulcanization time 4.5h.
Embodiment 4
The preparation method of high-intensitive, high performance rubber material of the invention includes the following steps: offer stalk, and to straw
Stalk carries out nanosizing processing；Stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing, obtain the first mixture；
Ball milling is carried out to the first mixture, obtains the first solid additive；Mix glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil with
And processing aid, obtain the second mixture；High-speed stirred is carried out to the second mixture, obtains Second addition；Methylbenzene is provided
Base vinylsiloxane rubber；P-methylphenyl vinylsiloxane rubber carries out multistage mixing, wherein in p-methylphenyl vinyl silicon
When rubber carries out first stage mixing, the first solid additive is added into rubber compound, then to adding the first solid additive
Rubber compound carry out second stage mixing；Second addition is added into the rubber compound being kneaded by second stage, then carries out
Phase III is kneaded, and obtains semi-finished product silicon rubber；Double of finished product silicon rubber carries out heat-treated under medium temperature；To medium temperature treated semi-finished product
Silicon rubber carries out first stage cure, obtains semi silicon sulfide rubber；Second stage vulcanization is carried out to semi silicon sulfide rubber, obtains height
Intensity, high performance rubber material.Nanosizing processing is carried out to stalk to include the following steps: to crush stalk, and will crush it
Stalk afterwards is mixed with nanosizing processing auxiliary agent, obtains mixed solution, wherein it includes sodium hydroxide solution that nanosizing, which handles auxiliary agent,
And hydrogen peroxide；Mixed solution is stirred by ultrasonic；Mixed solution after filtering ultrasonic agitation, obtains by nanosizing
The stalk of reason.It wherein, include stalk 40g, sodium hydroxide solution 50mL in every 100mL mixed solution, remaining is hydrogen peroxide, ultrasound
Stirring specifically comprises the processes of: ultraviolet light irradiation is carried out in ultrasonic agitation, ultraviolet light irradiation power is 40W, and ultrasonic agitation power is
900W, ultrasonic agitation time are 7h.In the first mixture, in parts by weight, 20 parts are accounted for by the stalk that nanosizing is handled, silicon
Sour aluminum fiber accounts for 20 parts, and carbon black accounts for 45 parts.Ball milling is carried out to the first mixture specifically comprises the processes of: ball milling speed 1200r/
Min, ratio of grinding media to material 13:1, Ball-milling Time 30h, wherein in mechanical milling process, every ball milling 3 hours suspends ball milling 25min.?
In second mixture, in parts by weight, glutamic acid lanthanum (DAGLa) account for 8 parts, vulcanizing agent account for 3 parts, 6 parts of hydroxy silicon oil, it is mixed to second
It closes object and carries out high-speed stirred specifically comprises the processes of: mixing temperature is 70 DEG C, and mixing machine revolving speed is 700rpm, and incorporation time is
13min.First stage is kneaded specifically comprises the processes of: melting temperature is 135 DEG C, mixing time 15min；Second stage is kneaded specific
Technique are as follows: melting temperature is 145 DEG C, mixing time 8min；Phase III is kneaded specifically comprises the processes of: and melting temperature is 150 DEG C,
Mixing time is 15min, wherein including the first solid additive 55 in the methyl phenyl vinyl silicone rubber of every 100 parts by weight
Part, 10 parts of Second addition.Double of finished product silicon rubber carries out heat-treated under medium temperature specifically comprises the processes of: double of finished product silicon rubber carries out heat
Processing, heat treatment temperature are 140 DEG C, heat treatment time 25h.First stage is carried out to medium temperature treated semi-finished product silicon rubber
Vulcanization specifically comprises the processes of: high temperature and pressure vulcanization, sulfide stress 7MPa, sulphur are carried out to medium temperature treated semi-finished product silicon rubber
Changing temperature is 170 DEG C.Second stage vulcanization is carried out to semi silicon sulfide rubber specifically comprises the processes of: semi silicon sulfide rubber is put into baking
Case, curing temperature are 180 DEG C, vulcanization time 4.5h.
Comparative example 1
Difference from Example 1 is: not including alumina silicate fibre in the first mixture.
Comparative example 2
Difference from Example 1 is: when p-methylphenyl vinylsiloxane rubber carries out first stage mixing, simultaneously
The first solid additive and Second addition are added into rubber compound.
Comparative example 3
Difference from Example 1 is: double of finished product silicon rubber does not carry out heat-treated under medium temperature.
Comparative example 4
Difference from Example 1 is: not carrying out second stage mixing to rubber compound.
Comparative example 5
Difference from Example 1 is: in every 100mL mixed solution include stalk 70g, sodium hydroxide solution 10mL,
Remaining is hydrogen peroxide.
Comparative example 6
Difference from Example 1 is: ultrasonic agitation specifically comprises the processes of: shines in ultrasonic agitation without ultraviolet light
It penetrates, ultrasonic agitation power is 500W, and the ultrasonic agitation time is 12h.
Comparative example 7
Difference from Example 1 is: in parts by weight, accounting for 50 parts by the stalk that nanosizing is handled, aluminium silicate fiber
Dimension accounts for 50 parts, and carbon black accounts for 50 parts.
Comparative example 8
Difference from Example 1 is: carrying out ball milling to first mixture specifically comprises the processes of: ball milling speed is
1800r/min, ratio of grinding media to material 20:1, Ball-milling Time 40h.
Comparative example 9
Difference from Example 1 is: in the second mixture, in parts by weight, glutamic acid lanthanum (DAGLa) accounts for 12
Part, vulcanizing agent account for 1 part, 2 parts of hydroxy silicon oil.
Comparative example 10
Difference from Example 1 is: carrying out high-speed stirred to second mixture specifically comprises the processes of: mixing temperature is
30 DEG C, mixing machine revolving speed is 1000rpm, incorporation time 20min.
Comparative example 11
Difference from Example 1 is: the first stage is kneaded specifically comprises the processes of: melting temperature is 145 DEG C, mixing time
For 30min；Second stage is kneaded specifically comprises the processes of: melting temperature is 135 DEG C, mixing time 15min；Phase III is kneaded tool
Body technology are as follows: melting temperature is 140 DEG C, mixing time 30min.
Comparative example 12
Difference from Example 1 is: including first solid in the methyl phenyl vinyl silicone rubber of every 100 parts by weight
70 parts of body additives, 20 parts of Second addition.
Comparative example 13
Difference from Example 1 is: double of finished product silicon rubber carries out heat-treated under medium temperature specifically comprises the processes of: to semi-finished product
Silicon rubber is heat-treated, and heat treatment temperature is 160 DEG C, heat treatment time 10h.
Comparative example 14
Difference from Example 1 is: the tool of first stage cure is carried out to medium temperature treated semi-finished product silicon rubber
Body technology are as follows: high temperature and pressure vulcanization, sulfide stress 10MPa, curing temperature are carried out to medium temperature treated semi-finished product silicon rubber
It is 190 DEG C.
Comparative example 15
Difference from Example 1 is: carrying out second stage vulcanization to semi silicon sulfide rubber specifically comprises the processes of: will be partly
Sulphurated siliastic is put into baking oven, and curing temperature is 165 DEG C, vulcanization time 2h.
Tensile strength (MPa), elongation at break and tearing strength (N/ are tested to embodiment 1-4 and comparative example 15
mm).It the results are shown in Table 1.
Table 1
The aforementioned description to specific exemplary embodiment of the invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
1. a kind of preparation method of high-intensitive, high performance rubber material, it is characterised in that: high-intensitive, the high performance rubber
The preparation method of glue material includes the following steps:
Stalk is provided, and nanosizing processing is carried out to the stalk；
Stalk, alumina silicate fibre and carbon black of the mixing by nanosizing processing, obtain the first mixture；
Ball milling is carried out to first mixture, obtains the first solid additive；
Glutamic acid lanthanum (DAGLa), vulcanizing agent, hydroxy silicon oil and processing aid are mixed, the second mixture is obtained；
High-speed stirred is carried out to second mixture, obtains Second addition；
Methyl phenyl vinyl silicone rubber is provided；
Multistage mixing is carried out to the methyl phenyl vinyl silicone rubber, wherein to the methyl phenyl vinyl silicon rubber
When glue carries out first stage mixing, the first solid additive is added into rubber compound, then to the first solid additive of addition
Rubber compound carries out second stage mixing；
Second addition is added into the rubber compound being kneaded by second stage, then carries out phase III mixing, obtain half at
Product silicon rubber；
Heat-treated under medium temperature is carried out to the semi-finished product silicon rubber；
First stage cure is carried out to medium temperature treated semi-finished product silicon rubber, obtains semi silicon sulfide rubber；And
Second stage vulcanization is carried out to the semi silicon sulfide rubber, obtains high-intensitive, high performance rubber material.
2. high-intensitive, high performance rubber material as described in claim 1, it is characterised in that: carry out nanometer to the stalk
Change processing includes the following steps:
Stalk is crushed, and the stalk after crushing is mixed with nanosizing processing auxiliary agent, obtains mixed solution, wherein described
It includes sodium hydroxide solution and hydrogen peroxide that nanosizing, which handles auxiliary agent,；
Mixed solution is stirred by ultrasonic；
Mixed solution after filtering ultrasonic agitation, obtains the stalk handled by nanosizing.
3. high-intensitive, high performance rubber material as claimed in claim 2, it is characterised in that: wherein, every 100mL mixing is molten
It include stalk 30-50g, sodium hydroxide solution 40-60mL in liquid, remaining is hydrogen peroxide, ultrasonic agitation specifically comprises the processes of: in ultrasound
Ultraviolet light irradiation is carried out when stirring, ultraviolet light irradiation power is 30-50W, and ultrasonic agitation power is 800-1000W, ultrasonic agitation
Time is 5-8h.
4. high-intensitive, high performance rubber material as described in claim 1, it is characterised in that: in first mixture,
In parts by weight, 10-30 parts are accounted for by the stalk that nanosizing is handled, alumina silicate fibre accounts for 10-30 parts, and carbon black accounts for 40-50 parts.
5. as described in claim 1 high-intensitive, high performance rubber material, it is characterised in that: to first mixture into
Row ball milling specifically comprises the processes of: ball milling speed 1000-1500r/min, ratio of grinding media to material 10:1-15:1, Ball-milling Time 25-
35h, wherein in mechanical milling process, every ball milling 3 hours suspends ball milling 20-30min.
6. high-intensitive, high performance rubber material as described in claim 1, it is characterised in that: in second mixture,
In parts by weight, glutamic acid lanthanum (DAGLa) account for 5-10 parts, vulcanizing agent account for 1-4 parts, 4-8 parts of hydroxy silicon oil, to it is described second mixing
Object carries out high-speed stirred specifically comprises the processes of: mixing temperature is 60-80 DEG C, and mixing machine revolving speed is 500-800rpm, incorporation time
For 10-15min.
7. high-intensitive, high performance rubber material as described in claim 1, it is characterised in that: the first stage is kneaded specific work
Skill are as follows: melting temperature is 130-140 DEG C, mixing time 10-20min；Second stage is kneaded specifically comprises the processes of: melting temperature is
140-150 DEG C, mixing time 5-10min；Phase III is kneaded specifically comprises the processes of: melting temperature is 145-155 DEG C, when mixing
Between be 10-20min, wherein in the methyl phenyl vinyl silicone rubber of every 100 parts by weight include the first solid additive 50-60
Part, 8-12 parts of Second addition.
8. high-intensitive, high performance rubber material as described in claim 1, it is characterised in that: to the semi-finished product silicon rubber
Carry out heat-treated under medium temperature specifically comprises the processes of: the semi-finished product silicon rubber is heat-treated, heat treatment temperature is 130-150 DEG C,
Heat treatment time is 20-30h.
9. as described in claim 1 high-intensitive, high performance rubber material, it is characterised in that: to medium temperature treated half at
Product silicon rubber carries out first stage cure specifically comprises the processes of: to medium temperature, treated that semi-finished product silicon rubber carries out high temperature and pressure sulphur
Change, sulfide stress 5-8MPa, curing temperature is 160-180 DEG C.
10. high-intensitive, high performance rubber material as described in claim 1, it is characterised in that: to the semi silicon sulfide rubber
Carry out second stage vulcanization specifically comprises the processes of: the semi silicon sulfide rubber is put into baking oven, curing temperature is 175-185 DEG C,
Vulcanization time is 4-5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811144992.XA CN109266017B (en) | 2018-09-29 | 2018-09-29 | Preparation method of high-strength and high-performance rubber material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811144992.XA CN109266017B (en) | 2018-09-29 | 2018-09-29 | Preparation method of high-strength and high-performance rubber material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109266017A true CN109266017A (en) | 2019-01-25 |
| CN109266017B CN109266017B (en) | 2021-12-24 |
Family
ID=65198824
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811144992.XA Active CN109266017B (en) | 2018-09-29 | 2018-09-29 | Preparation method of high-strength and high-performance rubber material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109266017B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010600A (en) * | 2010-11-26 | 2011-04-13 | 广州天赐有机硅科技有限公司 | Conductive liquid silicon rubber-based adhesive and preparation method for composition thereof |
| CN105647190A (en) * | 2016-01-14 | 2016-06-08 | 上海大学 | Preparation method of ceramic silicon rubber composite material used for fire-resistant insulated cable |
| CN107141810A (en) * | 2017-05-18 | 2017-09-08 | 国家电网公司 | A kind of modified silicon rubber and preparation method thereof |
| CN107418217A (en) * | 2017-08-30 | 2017-12-01 | 长沙科成高分子材料有限公司 | A kind of fire-retardant tear-proof silicon rubber and preparation method thereof |
-
2018
- 2018-09-29 CN CN201811144992.XA patent/CN109266017B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010600A (en) * | 2010-11-26 | 2011-04-13 | 广州天赐有机硅科技有限公司 | Conductive liquid silicon rubber-based adhesive and preparation method for composition thereof |
| CN105647190A (en) * | 2016-01-14 | 2016-06-08 | 上海大学 | Preparation method of ceramic silicon rubber composite material used for fire-resistant insulated cable |
| CN107141810A (en) * | 2017-05-18 | 2017-09-08 | 国家电网公司 | A kind of modified silicon rubber and preparation method thereof |
| CN107418217A (en) * | 2017-08-30 | 2017-12-01 | 长沙科成高分子材料有限公司 | A kind of fire-retardant tear-proof silicon rubber and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 丛后罗，等: "秸秆复合材料研究进展", 《秸秆复合材料研究进展》 * |
| 周长忍，主编: "《生物材料学》", 30 April 2004, 中国医药科技出版社 * |
| 李永河，主编: "《橡胶硫化技术》", 31 May 2012, 黄河水利出版社 * |
| 饶友，等: "羟基硅油对过氧化物硫化硅橡胶性能的影响", 《有机硅材料》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109266017B (en) | 2021-12-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106867258A (en) | A kind of high temperature resistant resistance oil silicone rubber material and preparation method thereof | |
| CN106398229A (en) | High-elongation silica gel and preparation method thereof | |
| CN102020831B (en) | Composite material for wind power generation blades | |
| CN107603178A (en) | A kind of heat-resisting biodegradable plastic material | |
| CN109370496A (en) | A kind of automobile epoxy structural rubber and preparation method thereof | |
| CN105670223A (en) | Epoxy resin composition and composite material for wind power generator blade | |
| CN107234860A (en) | A kind of uncured type damping shock absorption film | |
| CN106398230A (en) | High-hardness and air-pressure-resistant silica gel and preparation method thereof | |
| JP2017052942A (en) | Rubber composition | |
| CN109266017A (en) | The preparation method of high-intensitive, high performance rubber material | |
| CN107381611A (en) | A kind of artificial stone is with modified nano calcium carbonate powder and preparation method thereof and resin based artificial stone material | |
| CN102676007A (en) | Nano hollow heat-dissipating carbon coating and manufacturing method thereof | |
| CN107601541A (en) | A kind of production method of nano-calcium carbonate | |
| CN112778950B (en) | Efficient intermediate-temperature fast-curing epoxy structural adhesive for die assembly and bonding of wind power generation blades and preparation method thereof | |
| CN108641303B (en) | Epoxy resin gasket | |
| CN110922924A (en) | Graphene modified epoxy resin adhesive and preparation method thereof | |
| CN105647033A (en) | Sealing material for high-pressure medium delivery valves | |
| CN109022089A (en) | A kind of method of swollen soft straws used for preparing fuel | |
| CN109762267A (en) | A kind of papermaking waste/PVC composite material | |
| CN104558983B (en) | The preparation method of organobentonite Modified PolytetrafluoroethylOil Oil Seal material | |
| CN104927114A (en) | Automobile chassis bushing rubber material and preparing method thereof | |
| CN101585977B (en) | Preparation method of polypropylene reinforced plasticized modifier | |
| CN107446164B (en) | Modified calcium carbonate for filling biodegradable plastics and preparation method thereof | |
| CN105255077B (en) | Silicon fluoride modifying carbon fibers strengthen polyvinylidene fluoride material and preparation method | |
| CN106047221A (en) | Adhesive with excellent adhesive property for inflatable boats |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20211207 Address after: 200000 No. 38, Fengsheng Road, Tinglin Town, Jinshan District, Shanghai Applicant after: SHANGHAI DAWNFLUO RUBBER TECHNOLOGY CO.,LTD. Address before: 362212 room 1008, building 23, haisijing City, Huazhou village, Chidian Town, Jinjiang, Quanzhou City, Fujian Province Applicant before: QUANZHOU JIETE CHEMICAL TECHNOLOGY Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230803 Address after: East side of Building 3, No. 18 Fengsheng Road, Tinglin Town, Jinshan District, Shanghai, April 2015 Patentee after: Shanghai Chengcheng New Materials Co.,Ltd. Address before: 200000 No. 38, Fengsheng Road, Tinglin Town, Jinshan District, Shanghai Patentee before: SHANGHAI DAWNFLUO RUBBER TECHNOLOGY CO.,LTD. |
|
| TR01 | Transfer of patent right |