CN108641149A - A kind of preparation method and applications of lignin fibre rubber composite material - Google Patents
A kind of preparation method and applications of lignin fibre rubber composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L15/00—Compositions of rubber derivatives
- C08L15/005—Hydrogenated nitrile rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention discloses a kind of preparation method and applications of lignin fibre rubber composite material, this method is used clay, calcium carbonate, dacron fibre ball milling；Lignin fibre, ethoxylated dodecyl alcohol are immersed in supersound process, isolated centrifugal deposition object in acid solution, are transferred to after washing in high-pressure stirring reaction kettle, aromatic naphtha is added and is stirred to react to obtain high-pressure stirring reactant；Dioctyl sebacate, methyl acrylate are added in distilled water to stir evenly to form mixed liquor, then heat up and dibenzothiazyl disulfide is added obtains isothermal holding mixed liquor through standing isothermal holding；Internal mixing and plasticizing after finally above-mentioned product is mixed, then obtained mixing mixing glue and hydrogenated nitrile-butadiene rubber, methyl silicone rubber be kneaded jointly, sulfidization molding, drying, obtain finished product rubber composite material.The rubber composite material being prepared, tensile property is good, lear energy is strong, has a good application prospect on mechanical equipment inner piece.
Description
Technical field
The present invention relates to technical field of rubber material, and in particular to a kind of preparation side of lignin fibre rubber composite material
Method and its application.
Background technology
Lignin fibre is that natural timber passes through the obtained organic fiber of chemical treatment, and appearance is flocculence, it is white or
Canescence passes through screening, division, high-temperature process, bleaching, the fiber for chemical treatment, neutralizing, being sieved into different length and fineness degree
To adapt to the needs of different application material.It is chemically very steady at typical condition since treatment temperature is up to 250 DEG C or more
Fixed substance is not general solvent, acid, caustic corrosion, has nontoxic, tasteless, pollution-free, "dead" fine quality, no
Environment is influenced, it is harmless, belong to green product, this is not available for other minerals fibers.The microcosmic knot of fiber
Structure is with sigmoid, and rough, porous, infall is flat, there is good toughness, dispersibility and chemical stabilization
Property, water absorbing capacity is strong, there is very outstanding thickening cracking resistance.
Rubber refers to the high elastic polymer material for having reversible deformation, high resilience at room temperature, in the external force of very little
Effect is lower to be generated compared with large deformation, and resilient after external force is removed.Rubber belongs to entirely without styling polymer, its vitrifying
Transition temperature is low, and molecular weight is often very big, is more than hundreds of thousands.Rubber is divided into two kinds of natural rubber and synthetic rubber.Natural rubber
It is made of the extraction colloid post-processing from the plants such as rubber tree, kok-saghyz；Synthetic rubber then by various monomers it is aggregated reaction and
.Rubber can be divided into general purpose rubber and specific rubber again by performance and purposes, be widely used in daily life, medical treatment at present
The fields such as health, communications and transportation, agricultural, scientific experimentation, national defence.With the development of society, people put forward the performance of rubber product
Higher requirement is gone out, existing rubber material can not meet the needs of high-grade, precision and advanced scientific and technical product, generally require to it
It is modified.
Invention content
In order to solve the above technical problems, the present invention provide a kind of lignin fibre rubber composite material preparation method and its
Using this method is used clay, calcium carbonate, dacron fibre ball milling；Lignin fibre, laruyl alcohol are gathered
Ethylene oxide ether is immersed in supersound process, isolated centrifugal deposition object in acid solution, will be transferred to high pressure after the washing of centrifugal deposition object
In stirred autoclave, aromatic naphtha is added and is stirred to react to obtain high-pressure stirring reactant；Dioctyl sebacate, methyl acrylate are added
Enter and stir evenly to form mixed liquor into distilled water, then heating up and dibenzothiazyl disulfide is added obtains through standing isothermal holding
To isothermal holding mixed liquor；Internal mixing and plasticizing after finally above-mentioned product is mixed, then the mixing mixing glue and hydrogenated butyronitrile that will obtain
Rubber, methyl silicone rubber be kneaded jointly, sulfidization molding, drying, obtain finished product rubber composite material.The rubber composite wood being prepared
Material, tensile property is good, lear energy is strong, has a good application prospect on mechanical equipment inner piece.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of lignin fibre rubber composite material, includes the following steps：
（1）It will be in 3-5 parts of 6-8 parts of clay, 3-5 parts of calcium carbonate, dacron fibre input planetary ball mills
Ball-milling treatment is carried out, ball-milled powder is obtained；
（2）22-24 parts of lignin fibre, 16-20 parts of ethoxylated dodecyl alcohol are immersed in the HCl of a concentration of 0.1 mol/L
It is ultrasonically treated in solution, will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through high speed centrifugation
Centrifugal deposition object is isolated, centrifugal deposition object is washed with distilled water 2-4 times and is transferred in high-pressure stirring reaction kettle, virtue is added
5-9 parts of hydrocarbon ils, set the pressure of high-pressure stirring reaction kettle as 15 MPa, temperature be 150 DEG C, in 250-260 revs/min of rate
Under be stirred to react 30 minutes, obtain high-pressure stirring reactant；
（3）By 15-25 parts of dioctyl sebacate, 16-18 parts of methyl acrylate be added in the distilled water of 60-80 times of quality according to
80-100 revs/min of rate stirs evenly to form mixed liquor, and mixeding liquid temperature is slowly raised to 80-90 DEG C, two sulphur are added
Change 6-8 parts of bisbenzothiazole, stands isothermal holding 30 minutes, obtain isothermal holding mixed liquor；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 80-90 DEG C, anti-aging agent 1-3 is then added in internal mixing and plasticizing 10-15 minutes
Part, 1-3 parts of vulcanizing agent continue internal mixing and plasticizing 6-8 minutes, and mixing mixing glue is obtained after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 55-65 parts of hydrogenated nitrile-butadiene rubber, the common throwing of 50-60 parts of methyl silicone rubber
Enter in open mill, set the roll spacing of open mill as 3 mm, open mill temperature is 50-60 DEG C, and mixing time is 18-20 minutes, thin
Lead to 2-3 postcooling and obtains whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, then by sulfur product at 120 DEG C
Lower forced air drying 80-100 minutes after being cooled to room temperature, obtains finished product rubber composite material.
Further, the step（1）The ratio of grinding media to material of middle ball mill is 15:1, drum's speed of rotation is 200-220 revs/min
Clock, Ball-milling Time are 8-10 hours.
Further, the step（2）The frequency of middle supersound process is 12-16 kHz, and the power of supersound process is 180-
The time of 200 W, supersound process are 50-60 minutes.
Further, the step（4）In anti-aging agent be selected from N- (1,3- dimethylbutyls)-N '-diphenyl-para-phenylene diamines,
4,4 '-thiobis（6- tertiary butyl -3- methylphenols）, N, any one in N- nickel dibutyl dithiocarbamates.
Further, the step（4）In vulcanizing agent be selected from toluene diisocyanate dimer, four vulcanization two morphines
Any one in quinoline, dual-tert-butyl peroxy isopropyl base benzene.
Further, the step（6）The curing temperature of middle plateform vulcanizer is 135-145 DEG C, sulfide stress 7-9
MPa, vulcanization time are 35-45 minutes.
At the same time, the invention also discloses lignin fibre rubber composite materials made from above-mentioned preparation method in machinery
Application on equipment inner piece.
Compared with prior art, the present invention advantage is：
（1）The preparation method of the lignin fibre rubber composite material of the present invention is used clay, calcium carbonate, poly terephthalic acid
Second diester fiber ball milling；Lignin fibre, ethoxylated dodecyl alcohol are immersed in supersound process, isolated centrifugation in acid solution
Deposit will be transferred to after the washing of centrifugal deposition object in high-pressure stirring reaction kettle, aromatic naphtha is added be stirred to react to obtain high pressure and stir
Mix reactant；Dioctyl sebacate, methyl acrylate are added to and stir evenly to form mixed liquor in distilled water, is then heated up simultaneously
Dibenzothiazyl disulfide is added and obtains isothermal holding mixed liquor through standing isothermal holding；Mixing after finally above-mentioned product is mixed
Plasticizing, then obtained mixing mixing glue and hydrogenated nitrile-butadiene rubber, methyl silicone rubber be kneaded jointly, sulfidization molding, drying, obtain into
Product rubber composite material.The rubber composite material being prepared, tensile property is good, lear energy is strong, in mechanical equipment
It has a good application prospect on backing member.
（2）Present invention employs lignin fibre, ethoxylated dodecyl alcohol, dioctyl sebacate, methyl acrylates etc.
Raw material participation prepares lignin fibre rubber composite material, and effective performance boost has been carried out to rubber composite material, although this
A little materials are not first Application in rubber composite material, but are aided with corresponding processing mode after amount combination according to a certain ratio,
Increasing substantially in performance is brought to the rubber composite material being finally prepared, this is not in previous research
Once it reported, for realizing that it is conclusive that the technique effect of the present invention plays the role of.
Specific implementation mode
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
（1）Ball will be carried out in 3 parts of 6 parts of clay, 3 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 200 revs/min, and Ball-milling Time is 8 hours, obtains ball milling powder
End；
（2）22 parts of lignin fibre, 16 parts of ethoxylated dodecyl alcohol are immersed in the HCl solution of a concentration of 0.1 mol/L
It is ultrasonically treated, the frequency of supersound process is 12 kHz, and the power of supersound process is 180 W, and the time of supersound process is 50
Minute, it will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition that is centrifuged at a high speed out
Centrifugal deposition object is washed with distilled water 2 times and is transferred in high-pressure stirring reaction kettle by object, and 5 parts of aromatic naphtha is added, and sets high pressure
The pressure of stirred autoclave is 15 MPa, temperature is 150 DEG C, is stirred to react 30 minutes, obtains under 250 revs/min of rate
High-pressure stirring reactant；
（3）15 parts of dioctyl sebacate, 16 parts of methyl acrylate are added in the distilled water of 60 times of quality according to 80 revs/min
Rate stir evenly to form mixed liquor, mixeding liquid temperature is slowly raised to 80 DEG C, 6 parts of dibenzothiazyl disulfide is added,
Isothermal holding 30 minutes are stood, isothermal holding mixed liquor is obtained；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 80 DEG C, N- (1,3- dimethyl butyrates are then added in internal mixing and plasticizing 10 minutes
Base) 1 part of-N '-diphenyl-para-phenylene diamines, 1 part of toluene diisocyanate dimer continue internal mixing and plasticizing 6 minutes, it is mixed after plastic emitting
Close mixing glue；
（5）By step（4）Obtained mixing mixing glue and 55 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 50 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 50 DEG C, and mixing time is 18 minutes, thin logical 2-3 postcooling
Obtain whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
135 DEG C, sulfide stress 7MPa, vulcanization time be 35 minutes, then by sulfur product at 120 DEG C forced air drying 80 minutes,
After being cooled to room temperature, finished product rubber composite material is obtained.
The performance test results of rubber composite material obtained are as shown in table 1.
Embodiment 2
（1）Ball will be carried out in 4 parts of 7 parts of clay, 4 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 210 revs/min, and Ball-milling Time is 9 hours, obtains ball milling powder
End；
（2）23 parts of lignin fibre, 18 parts of ethoxylated dodecyl alcohol are immersed in the HCl solution of a concentration of 0.1 mol/L
It is ultrasonically treated, the frequency of supersound process is 14 kHz, and the power of supersound process is 190 W, and the time of supersound process is 55
Minute, it will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition that is centrifuged at a high speed out
Centrifugal deposition object is washed with distilled water 3 times and is transferred in high-pressure stirring reaction kettle by object, and 7 parts of aromatic naphtha is added, and sets high pressure
The pressure of stirred autoclave is 15 MPa, temperature is 150 DEG C, is stirred to react 30 minutes, obtains under 255 revs/min of rate
High-pressure stirring reactant；
（3）20 parts of dioctyl sebacate, 17 parts of methyl acrylate are added in the distilled water of 70 times of quality according to 90 revs/min
Rate stir evenly to form mixed liquor, mixeding liquid temperature is slowly raised to 85 DEG C, 7 parts of dibenzothiazyl disulfide is added,
Isothermal holding 30 minutes are stood, isothermal holding mixed liquor is obtained；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 85 DEG C, 4,4 '-thiobis are then added in internal mixing and plasticizing 12 minutes（Uncle 6-
Butyl -3- methylphenols）2 parts, 2 parts of four two morpholines of vulcanization continuation internal mixing and plasticizing 7 minutes, obtain mixing mixing glue after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 60 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 55 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 55 DEG C, and mixing time is 19 minutes, thin logical 2-3 postcooling
Obtain whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
140 DEG C, sulfide stress be 8 MPa, vulcanization time be 40 minutes, then by sulfur product at 120 DEG C forced air drying 90 minutes,
After being cooled to room temperature, finished product rubber composite material is obtained.
The performance test results of rubber composite material obtained are as shown in table 1.
Embodiment 3
（1）Ball will be carried out in 5 parts of 8 parts of clay, 5 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 220 revs/min, and Ball-milling Time is 10 hours, obtains ball milling
Powder；
（2）24 parts of lignin fibre, 20 parts of ethoxylated dodecyl alcohol are immersed in the HCl solution of a concentration of 0.1 mol/L
It is ultrasonically treated, the frequency of supersound process is 16 kHz, and the power of supersound process is 200 W, and the time of supersound process is 60
Minute, it will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition that is centrifuged at a high speed out
Centrifugal deposition object is washed with distilled water 4 times and is transferred in high-pressure stirring reaction kettle by object, and 9 parts of aromatic naphtha is added, and sets high pressure
The pressure of stirred autoclave is 15 MPa, temperature is 150 DEG C, is stirred to react 30 minutes, obtains under 260 revs/min of rate
High-pressure stirring reactant；
（3）25 parts of dioctyl sebacate, 18 parts of methyl acrylate are added in the distilled water of 80 times of quality according to 100 revs/min
The rate of clock stirs evenly to form mixed liquor, and mixeding liquid temperature is slowly raised to 90 DEG C, dibenzothiazyl disulfide 8 is added
Part, isothermal holding 30 minutes are stood, isothermal holding mixed liquor is obtained；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 90 DEG C, N, N- dibutyl dithios is then added in internal mixing and plasticizing 15 minutes
3 parts of carbamic acid nickel, 3 parts of dual-tert-butyl peroxy isopropyl base benzene continue internal mixing and plasticizing 8 minutes, and mixing mixing glue is obtained after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 65 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 60 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 60 DEG C, and mixing time is 20 minutes, and thin logical 3 postcoolings obtain
To whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
145 DEG C, sulfide stress is 9 MPa, and vulcanization time is 45 minutes, and then by sulfur product, forced air drying 100 divides at 120 DEG C
Clock after being cooled to room temperature, obtains finished product rubber composite material.
The performance test results of rubber composite material obtained are as shown in table 1.
Comparative example 1
（1）Ball will be carried out in 4 parts of 7 parts of clay, 4 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 210 revs/min, and Ball-milling Time is 9 hours, obtains ball milling powder
End；
（2）18 parts of ethoxylated dodecyl alcohol is immersed in the HCl solution of a concentration of 0.1 mol/L and is ultrasonically treated, is surpassed
The frequency of sonication is 14 kHz, and the power of supersound process is 190 W, and the time of supersound process is 55 minutes, then will be ultrasonic
Processing mixed liquor is neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition object that is centrifuged at a high speed out, by centrifugal deposition object
It is washed with distilled water 3 times and is transferred in high-pressure stirring reaction kettle, 7 parts of aromatic naphtha is added, set the pressure of high-pressure stirring reaction kettle
Power is 15 MPa, temperature is 150 DEG C, is stirred to react under 255 revs/min of rate 30 minutes, obtains high-pressure stirring reactant；
（3）20 parts of dioctyl sebacate, 17 parts of methyl acrylate are added in the distilled water of 70 times of quality according to 90 revs/min
Rate stir evenly to form mixed liquor, mixeding liquid temperature is slowly raised to 85 DEG C, 7 parts of dibenzothiazyl disulfide is added,
Isothermal holding 30 minutes are stood, isothermal holding mixed liquor is obtained；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 85 DEG C, 4,4 '-thiobis are then added in internal mixing and plasticizing 12 minutes（Uncle 6-
Butyl -3- methylphenols）2 parts, 2 parts of four two morpholines of vulcanization continuation internal mixing and plasticizing 7 minutes, obtain mixing mixing glue after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 60 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 55 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 55 DEG C, and mixing time is 19 minutes, thin logical 2-3 postcooling
Obtain whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
140 DEG C, sulfide stress be 8 MPa, vulcanization time be 40 minutes, then by sulfur product at 120 DEG C forced air drying 90 minutes,
After being cooled to room temperature, finished product rubber composite material is obtained.
The performance test results of rubber composite material obtained are as shown in table 1.
Comparative example 2
（1）Ball will be carried out in 4 parts of 7 parts of clay, 4 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 210 revs/min, and Ball-milling Time is 9 hours, obtains ball milling powder
End；
（2）23 parts of lignin fibre is immersed in the HCl solution of a concentration of 0.1 mol/L and is ultrasonically treated, is ultrasonically treated
Frequency be 14 kHz, the power of supersound process is 190 W, and the time of supersound process is 55 minutes, will be then ultrasonically treated mixed
It closes liquid and is neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition object that is centrifuged at a high speed out, centrifugal deposition object is distilled
Water washing 3 times is simultaneously transferred in high-pressure stirring reaction kettle, and 7 parts of aromatic naphtha is added, and sets the pressure of high-pressure stirring reaction kettle as 15
MPa, temperature are 150 DEG C, are stirred to react under 255 revs/min of rate 30 minutes, obtain high-pressure stirring reactant；
（3）20 parts of dioctyl sebacate, 17 parts of methyl acrylate are added in the distilled water of 70 times of quality according to 90 revs/min
Rate stir evenly to form mixed liquor, mixeding liquid temperature is slowly raised to 85 DEG C, 7 parts of dibenzothiazyl disulfide is added,
Isothermal holding 30 minutes are stood, isothermal holding mixed liquor is obtained；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 85 DEG C, 4,4 '-thiobis are then added in internal mixing and plasticizing 12 minutes（Uncle 6-
Butyl -3- methylphenols）2 parts, 2 parts of four two morpholines of vulcanization continuation internal mixing and plasticizing 7 minutes, obtain mixing mixing glue after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 60 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 55 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 55 DEG C, and mixing time is 19 minutes, thin logical 2-3 postcooling
Obtain whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
140 DEG C, sulfide stress be 8 MPa, vulcanization time be 40 minutes, then by sulfur product at 120 DEG C forced air drying 90 minutes,
After being cooled to room temperature, finished product rubber composite material is obtained.
The performance test results of rubber composite material obtained are as shown in table 1.
Comparative example 3
（1）Ball will be carried out in 4 parts of 7 parts of clay, 4 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 210 revs/min, and Ball-milling Time is 9 hours, obtains ball milling powder
End；
（2）23 parts of lignin fibre, 18 parts of ethoxylated dodecyl alcohol are immersed in the HCl solution of a concentration of 0.1 mol/L
It is ultrasonically treated, the frequency of supersound process is 14 kHz, and the power of supersound process is 190 W, and the time of supersound process is 55
Minute, it will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition that is centrifuged at a high speed out
Centrifugal deposition object is washed with distilled water 3 times and is transferred in high-pressure stirring reaction kettle by object, and 7 parts of aromatic naphtha is added, and sets high pressure
The pressure of stirred autoclave is 15 MPa, temperature is 150 DEG C, is stirred to react 30 minutes, obtains under 255 revs/min of rate
High-pressure stirring reactant；
（3）17 parts of methyl acrylate is added in the distilled water of 70 times of quality and stirs evenly shape according to 90 revs/min of rate
At mixed liquor, mixeding liquid temperature is slowly raised to 85 DEG C, 7 parts of dibenzothiazyl disulfide is added, stood isothermal holding 30 and divide
Clock obtains isothermal holding mixed liquor；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 85 DEG C, 4,4 '-thiobis are then added in internal mixing and plasticizing 12 minutes（Uncle 6-
Butyl -3- methylphenols）2 parts, 2 parts of four two morpholines of vulcanization continuation internal mixing and plasticizing 7 minutes, obtain mixing mixing glue after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 60 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 55 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 55 DEG C, and mixing time is 19 minutes, thin logical 2-3 postcooling
Obtain whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
140 DEG C, sulfide stress be 8 MPa, vulcanization time be 40 minutes, then by sulfur product at 120 DEG C forced air drying 90 minutes,
After being cooled to room temperature, finished product rubber composite material is obtained.
The performance test results of rubber composite material obtained are as shown in table 1.
Comparative example 4
（1）Ball will be carried out in 4 parts of 7 parts of clay, 4 parts of calcium carbonate, dacron fibre input planetary ball mills
The ratio of grinding media to material of mill processing, ball mill is 15:1, drum's speed of rotation is 210 revs/min, and Ball-milling Time is 9 hours, obtains ball milling powder
End；
（2）23 parts of lignin fibre, 18 parts of ethoxylated dodecyl alcohol are immersed in the HCl solution of a concentration of 0.1 mol/L
It is ultrasonically treated, the frequency of supersound process is 14 kHz, and the power of supersound process is 190 W, and the time of supersound process is 55
Minute, it will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through the centrifugal deposition that is centrifuged at a high speed out
Centrifugal deposition object is washed with distilled water 3 times and is transferred in high-pressure stirring reaction kettle by object, and 7 parts of aromatic naphtha is added, and sets high pressure
The pressure of stirred autoclave is 15 MPa, temperature is 150 DEG C, is stirred to react 30 minutes, obtains under 255 revs/min of rate
High-pressure stirring reactant；
（3）20 parts of dioctyl sebacate is added in the distilled water of 70 times of quality and is stirred evenly according to 90 revs/min of rate
Mixed liquor is formed, mixeding liquid temperature is slowly raised to 85 DEG C, 7 parts of dibenzothiazyl disulfide is added, stands isothermal holding 30
Minute, obtain isothermal holding mixed liquor；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 85 DEG C, 4,4 '-thiobis are then added in internal mixing and plasticizing 12 minutes（Uncle 6-
Butyl -3- methylphenols）2 parts, 2 parts of four two morpholines of vulcanization continuation internal mixing and plasticizing 7 minutes, obtain mixing mixing glue after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 60 parts of hydrogenated nitrile-butadiene rubber, the common input mill of 55 parts of methyl silicone rubber
In machine, the roll spacing of open mill is set as 3 mm, and open mill temperature is 55 DEG C, and mixing time is 19 minutes, thin logical 2-3 postcooling
Obtain whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, and the curing temperature of vulcanizing press is
140 DEG C, sulfide stress be 8 MPa, vulcanization time be 40 minutes, then by sulfur product at 120 DEG C forced air drying 90 minutes,
After being cooled to room temperature, finished product rubber composite material is obtained.
The performance test results of rubber composite material obtained are as shown in table 1.
By the rubber composite material obtained of embodiment 1-3 and comparative example 1-4 respectively according to the method for GB/T 528-2009
It tests its tensile strength and elongation at break, test its tearing strength according to the method for GB/T 529-2008.
Table 1
| Tensile strength（MPa） | Elongation at break（%） | Tearing strength（KN/m） | |
| Embodiment 1 | 25.2 | 462 | 82.3 |
| Embodiment 2 | 25.6 | 479 | 83.4 |
| Embodiment 3 | 25.5 | 475 | 83.1 |
| Comparative example 1 | 20.7 | 420 | 72.6 |
| Comparative example 2 | 20.0 | 426 | 71.8 |
| Comparative example 3 | 20.6 | 431 | 73.4 |
| Comparative example 4 | 21.3 | 414 | 70.5 |
The preparation method of the lignin fibre rubber composite material of the present invention is used clay, calcium carbonate, poly terephthalic acid second
Diester fiber ball milling；Lignin fibre, ethoxylated dodecyl alcohol are immersed in supersound process in acid solution, isolated centrifugation is sunk
Product object, is transferred to after centrifugal deposition object is washed in high-pressure stirring reaction kettle, and aromatic naphtha is added and is stirred to react to obtain high-pressure stirring
Reactant；Dioctyl sebacate, methyl acrylate are added to and stir evenly to form mixed liquor in distilled water, then heat up and is added
Enter dibenzothiazyl disulfide and obtains isothermal holding mixed liquor through standing isothermal holding；Mixing is moulded after finally above-mentioned product is mixed
Change, then obtained mixing mixing glue and hydrogenated nitrile-butadiene rubber, methyl silicone rubber are kneaded jointly, sulfidization molding, drying, obtain finished product
Rubber composite material.The rubber composite material being prepared, tensile property is good, lear energy is strong, in mechanical equipment liner
It has a good application prospect on part.Also, present invention employs lignin fibre, ethoxylated dodecyl alcohol, decanedioic acid two
The raw materials participation such as monooctyl ester, methyl acrylate prepares lignin fibre rubber composite material, has been carried out effectively to rubber composite material
Performance boost, it is auxiliary according to a certain ratio after amount combination although these materials are not first Application in rubber composite material
With corresponding processing mode, increasing substantially in performance is brought to the rubber composite material being finally prepared, this
It is never to report in previous research, for realizing that it is conclusive that the technique effect of the present invention plays the role of.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of lignin fibre rubber composite material, which is characterized in that include the following steps：
（1）It will be in 3-5 parts of 6-8 parts of clay, 3-5 parts of calcium carbonate, dacron fibre input planetary ball mills
Ball-milling treatment is carried out, ball-milled powder is obtained；
（2）22-24 parts of lignin fibre, 16-20 parts of ethoxylated dodecyl alcohol are immersed in the HCl of a concentration of 0.1 mol/L
It is ultrasonically treated in solution, will then be ultrasonically treated mixed liquor and be neutralized to neutrality with sodium hydroxide solution, then through high speed centrifugation
Centrifugal deposition object is isolated, centrifugal deposition object is washed with distilled water 2-4 times and is transferred in high-pressure stirring reaction kettle, virtue is added
5-9 parts of hydrocarbon ils, set the pressure of high-pressure stirring reaction kettle as 15 MPa, temperature be 150 DEG C, in 250-260 revs/min of rate
Under be stirred to react 30 minutes, obtain high-pressure stirring reactant；
（3）By 15-25 parts of dioctyl sebacate, 16-18 parts of methyl acrylate be added in the distilled water of 60-80 times of quality according to
80-100 revs/min of rate stirs evenly to form mixed liquor, and mixeding liquid temperature is slowly raised to 80-90 DEG C, two sulphur are added
Change 6-8 parts of bisbenzothiazole, stands isothermal holding 30 minutes, obtain isothermal holding mixed liquor；
（4）By step（1）-（3）Obtained ball-milled powder, high-pressure stirring reactant and isothermal holding mixed liquor is transferred to adding pressure type
In mixer, the temperature of adding pressure type mixer is set as 80-90 DEG C, anti-aging agent 1-3 is then added in internal mixing and plasticizing 10-15 minutes
Part, 1-3 parts of vulcanizing agent continue internal mixing and plasticizing 6-8 minutes, and mixing mixing glue is obtained after plastic emitting；
（5）By step（4）Obtained mixing mixing glue and 55-65 parts of hydrogenated nitrile-butadiene rubber, the common throwing of 50-60 parts of methyl silicone rubber
Enter in open mill, set the roll spacing of open mill as 3 mm, open mill temperature is 50-60 DEG C, and mixing time is 18-20 minutes, thin
Lead to 2-3 postcooling and obtains whole epoxy glue；
（6）By step（5）Obtained whole epoxy glue is placed in sulfidization molding on vulcanizing press, then by sulfur product at 120 DEG C
Lower forced air drying 80-100 minutes after being cooled to room temperature, obtains finished product rubber composite material.
2. the preparation method of lignin fibre rubber composite material according to claim 1, which is characterized in that the step
（1）The ratio of grinding media to material of middle ball mill is 15:1, drum's speed of rotation is 200-220 revs/min, and Ball-milling Time is 8-10 hours.
3. the preparation method of lignin fibre rubber composite material according to claim 1, which is characterized in that the step
（2）The frequency of middle supersound process is 12-16 kHz, and the power of supersound process is 180-200 W, and the time of supersound process is 50-
60 minutes.
4. the preparation method of lignin fibre rubber composite material according to claim 1, which is characterized in that the step
（4）In anti-aging agent be selected from N- (1,3- dimethylbutyls)-N '-diphenyl-para-phenylene diamines, 4,4 '-thiobis（6- tertiary butyl -3- first
Base phenol）, N, any one in N- nickel dibutyl dithiocarbamates.
5. the preparation method of lignin fibre rubber composite material according to claim 1, which is characterized in that the step
（4）In vulcanizing agent selected from toluene diisocyanate dimer, four two morpholines of vulcanization, in dual-tert-butyl peroxy isopropyl base benzene
Any one.
6. the preparation method of lignin fibre rubber composite material according to claim 1, which is characterized in that the step
（6）The curing temperature of middle plateform vulcanizer is 135-145 DEG C, and sulfide stress is 7-9 MPa, and vulcanization time is 35-45 minutes.
7. according to lignin fibre rubber composite material made from any one of the claim 1-6 preparation methods in mechanical equipment
Application on inner piece.
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| CN101528831A (en) * | 2006-08-25 | 2009-09-09 | 萨克特本化学有限责任公司 | Titanium dioxide-containing composite |
| CN107057145A (en) * | 2017-05-27 | 2017-08-18 | 南京东润特种橡塑有限公司 | A kind of fiber reinforced rubber and preparation method thereof |
| CN107337817A (en) * | 2017-08-11 | 2017-11-10 | 广州市政鑫橡塑有限公司 | A kind of anti-slip sole special (purpose) rubber composition and preparation method thereof on ice |
| CN107474329A (en) * | 2017-08-17 | 2017-12-15 | 浙江久运汽车零部件有限公司 | A kind of anti-corrosive rubber cushion pad |
| CN107501643A (en) * | 2017-09-25 | 2017-12-22 | 芜湖凯奥尔环保科技有限公司 | A kind of preparation method of rubber composite |
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2018
- 2018-03-29 CN CN201810272700.4A patent/CN108641149A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101528831A (en) * | 2006-08-25 | 2009-09-09 | 萨克特本化学有限责任公司 | Titanium dioxide-containing composite |
| CN107057145A (en) * | 2017-05-27 | 2017-08-18 | 南京东润特种橡塑有限公司 | A kind of fiber reinforced rubber and preparation method thereof |
| CN107337817A (en) * | 2017-08-11 | 2017-11-10 | 广州市政鑫橡塑有限公司 | A kind of anti-slip sole special (purpose) rubber composition and preparation method thereof on ice |
| CN107474329A (en) * | 2017-08-17 | 2017-12-15 | 浙江久运汽车零部件有限公司 | A kind of anti-corrosive rubber cushion pad |
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