CN106632916A - Anticorrosion grafted composite elastic material and preparation method thereof - Google Patents
Anticorrosion grafted composite elastic material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3472—Five-membered rings
- C08K5/3475—Five-membered rings condensed with carbocyclic rings
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
Abstract
The invention discloses an anticorrosion grafted composite elastic material. The anticorrosion grafted composite elastic material is prepared from the following raw materials in parts by weight: 0.3 to 1 part of zinc acetylacetonate, 3 to 4 parts of 4-dimethylamino-pyridine, 1 to 2 parts of triethylamine, 0.1 to 0.3 part of 2-bromopropionyl bromide, 3 to 4 parts of polyethylene glycol, 1 to 2 parts of chlorinated-1-allyl, 1 to 2 parts of 3-methylimidazole, 50 to 60 parts of methyl methacrylate, 10 to 13 parts of carbon nanotubes, 40 to 51 parts of n-butyl acrylate, 0.7 to 1 part of copper bromide, 1.6 to 2 parts of pentamethyldiethylenetriamine, 1 to 2 parts of copper powder, 3 to 4 parts of dibutyl maleate, 0.6 to 1 part of benzotriazole, 2 to 3 parts of calcium propionate, 4 to 6 parts of methyl nylon acid, 0.1 to 0.2 part of p-methylbenzene sulfonic acid, 0.6 to 1 part of ethoxylated ammonium alkylphenol sulfate, 6 to 8 parts of tetrahydrofuran, absolute ethyl alcohol, ethylene glycol, dimethylformamide, 95 to 98 percent nitric acid, thionyl chloride and a proper amount of chloroform. By adding the benzotriazole, the calcium propionate, the methyl nylon acid and the like, the anticorrosion property of a finished material can be enhanced effectively, and the storage stability of the finished product is enhanced.
Description
Technical field
The present invention relates to elastomeric material technical field, more particularly to a kind of anti-corrosion grafting composite elastic material and its preparation side
Method.
Background technology
Thermoplastic elastomer (TPE) is a kind of special macromolecular material, both with elasticity, and with plasticity, can extensively be applied
In the key areas of the national economy such as packaging material, auto parts, adhesive, clothes, biomedicine.Thermoplastic elastomer (TPE) has one
Individual common the characteristics of, i.e., be nearly all phase-separated system, and at room temperature one is mutually rubber phase, and another phase is hard phase.Vitrifying
The very low rubber of transition temperature is used as matrix, and the higher hard phase of glass transition temperature is then dispersed in rubber as dispersion phase
Play a part of physical crosslinking point in matrix.For thermoplastic elastomer (TPE), mutually make elastomer that there is intensity firmly, and rubber mutually makes
Elastomer has ductility, and by control ratio between the two the elastomer of different mechanical properties can be obtained.But, with biography
System vulcanized rubber is compared, and thermoplastic elastomer (TPE) also has disadvantages that, this kind of elastomer is susceptible to permanent compression set, its shape
Stability, heat resistance and solvent resistance are also bad.Therefore, in order to obtain the thermoplastic elastic material of superior performance, need
Controllable optimization design is carried out to the chain structure of thermoplastic elastomer (TPE) so as to hard mutually to bring out the best in each other with rubber, preferably played each
From effect；
CNT possesses excellent mechanical property and electric property, and heat endurance is high, and with larger draw ratio, and density is very
It is low, so be considered as to prepare the preferable Nano filling of high performance material even so, dispersed very poor due to CNT,
Easily aggregation is reunited in polymeric matrix, is had a great impact to the performance of composite, therefore greatly limit carbon
The large-scale application of nanotube, in order to improve the degree of scatter of CNT, can be with Bian things when composite is prepared
Reason or the method for chemistry are processed, such as using surfactant, dissolve blending, solution blending, surface is modified, be co-precipitated, surpass
The method such as sound dispersion and in-situ polymerization, CNT is made into Nano filling introducing elastic matrix increases can its modulus, and this is
The hydrodynamics effect and the interaction between polymer and filler caused after due to adding CNT increased bullet
What the crosslink density of gonosome was caused.Generally, introduce Nano filling after, elastic composite occur Payne effects and
Mullins effects, the elastic composite based on CNT is no exception.It should be noted that Payne effects are referred to
The storage modulus of elastic composite declines to a great extent as strain amplitude increase occurs, typical non-linear behavior occurs,
At present being that the network being made up of filler in material is gradually destroyed as strain increases most reasonably is explained to this phenomenon, this
Individual network is not only formed by the interaction between filler and filler, also including between polymer and filler and polymer
Interact.It is exactly Mullins effects to occur delayed strain softening phenomenon when elastic composite carries out second stretching
Should, this hysteresis is due to introducing the Nano filling that cannot be deformed upon, material is generated in drawing process
Energy dissipation, destroys a part and the polymer molecular chain of contribution function is played to elastomeric network and is caused.For such
Composite, crystallization can be formed due to molecular chain orientation and plays a part of similar physical crosslinking points when stretching at room temperature, this
The molten point of a little crystallizations is about 48 DEG C, therefore its strain can not be replied at once after the stress for applying is removed.When temperature is raised sample
After the crystal training formed in product is melted, the conformation of polymer molecular chain is just gradually recovered under the driving of entropic elasticity.Due to carbon nanometer
Pipe can absorb near infrared light, it is also possible to which heat is produced in the presence of electric current raises the temperature of sample, promotes as physics
The crystallization of crosslinking points is dissolved, here it is there is the origin of shape memory.There is many being similar to prepare using CNT again later
The report of the thermoplastic elastomer composite material of shape memory function；
Inorganic nano-filler introducing polymeric matrix can be made into the material in mechanical property, electric conductivity, heat endurance and breathed freely
The aspects such as property increase significantly and improve.For such nano composite material, their macro property and Nano filling
Distance between size, interfacial interaction and filler is closely related.CNT is introduced by bullet by the method for physical blending
The research of gonosome has a lot, however, for the research that glycerol polymerization prepares elastomer is carried out as initiation point using CNT
Also rarely have and be related to, carrying out one kettle way glycerol polymerization by the method for chemistry can effectively increase phase between Nano filling and matrix
Interaction so as in being better dispersed in matrix, significantly increases its interface interaction power, so as to further improve its performance, therefore
Prepare this kind of high-performance thermoplastic elastomer and there is important practical significance.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of anti-corrosion grafting composite elastic material and its
Preparation method.
The present invention is achieved by the following technical solutions：
A kind of anti-corrosion is grafted composite elastic material, and it is by made by following weight parts raw material：
DMAP 3-4, triethylamine 1-2,2- bromine isobutyl acylbromide 0.1-0.3, zinc acetylacetonate 0.3-1, polyethylene glycol
3-4, chlorination 1- pi-allyl -3- methylimidazole 1-2, methyl methacrylate 50-60, CNT 10-13, n-butyl acrylate
40-51, copper bromide 0.7-1, pentamethyl-diethylenetriamine 1.6-2, copper powder 1-2, dibutyl maleate 3-4, BTA
0.6-1, calcium propionate 2-3, nylon acid methyl esters 4-6, p-methyl benzenesulfonic acid 0.1-0.2, ethoxylated alkylphenol ammonium sulfate 0.6-1,
Tetrahydrofuran 6-8, absolute ethyl alcohol, ethylene glycol, dimethylformamide, the nitric acid of 95-98%, thionyl chloride, appropriate chloroform.
A kind of described anti-corrosion is grafted the preparation method of composite elastic material, comprises the following steps：
（1）By above-mentioned polyethylene glycol at 80-90 DEG C insulated and stirred 5-10 minute, add above-mentioned chlorination 1- pi-allyls -3- methyl
Imidazoles, insulated and stirred 10-20 minute, obtains alcohol dispersion liquid；
（2）Above-mentioned CNT is added in its weight 100-130 times, 95-98% nitric acid, 140-150 DEG C is sent to
In oil bath, insulated and stirred 10-12 hour, suction filtration washes precipitate with deionized water 2-3 time, and at 54-60 DEG C 1-2 is vacuum dried
Hour, obtain acidifying CNT；
（3）Above-mentioned acidifying CNT, calcium propionate are mixed, in being added to the thionyl chloride of compound weight 20-30 times,
Insulated and stirred 20-25 hour, is distilled off thionyl chloride at 60-70 DEG C, in being added to the ethylene glycol of its weight 10-15 times, send
Enter in 110-120 DEG C of oil bath, be incubated 46-50 hours, suction filtration is washed precipitation dimethylformamide 2-3 time, in 40-50
1-2 hours are vacuum dried at DEG C, hydroxyl carbon nano tube is obtained；
（4）Above-mentioned hydroxyl carbon nano tube is added in alcohol dispersion liquid, it is 60-70 DEG C to rise high-temperature, adds above-mentioned levulinic
Ketone zinc, insulated and stirred 10-20 minute, suction filtration washes precipitation absolute ethyl alcohol, deionization 3-4 time, and air drying obtains modified
Hydroxyl carbon nano tube；
（5）Above-mentioned modified hydroxyl carbon nano tube is added in the chloroform of its total amount 17-20 times, above-mentioned 4- dimethylaminos are added
Pyridine, triethylamine, in being sent to ice-water bath, are added dropwise above-mentioned 2- bromine isobutyl acylbromides, and stirring reaction 3-4 hour discharges, at room temperature
Insulation reaction 46-50 hour, suction filtration washs filter cake chloroform, deionized water 2-3 time successively, is vacuum dried at 40-50 DEG C
1-2 hours, obtain initiator carbon nano-tube modified；
（6）Above-mentioned BTA is added in nylon acid methyl esters, it is 80-85 DEG C to rise high-temperature, adds above-mentioned ethoxylation
Alkyl phenol ammonium sulfate, insulated and stirred 3-4 minute, obtains ester dispersion liquid；
（7）By above-mentioned methyl methacrylate, n-butyl acrylate, carbon nano-tube modified initiator, pentamethyl-diethylenetriamine,
Copper bromide, the mixing of ester dispersion liquid, in being added to the dimethylformamide of compound weight 10-16 times, add above-mentioned copper powder, are passed through
Nitrogen, freeze-drying 20-30 minutes, in being sent to 65-70 DEG C of oil bath, insulated and stirred 1-2 hour adds above-mentioned tetrahydrochysene furan
Mutter, stir, in adding the methyl alcohol of mixed system weight 2-3 times, add remaining each raw material, stand 2-3 hours, suction filtration will
Precipitation dimethylformamide, deionized water are washed 3-4 time successively, and 10-12 hours are vacuum dried at 40-50 DEG C, obtain described
Composite elastic material.
It is an advantage of the invention that：The present invention is to carry out acidification to CNT in red fuming nitric acid (RFNA) first, then by shape
Into carboxyl carry out chloride with thionyl chloride, then there is acylation reaction with ethylene glycol, so as to introduce in carbon nano tube surface
Hydroxyl, most relief hydroxyl react with 2- bromine isobutyl acylbromides, thus initiation point can be modified in carbon nano tube surface, carry out
Controllable glycerol polymerization, finally on carbon Nanosurface graft acrylic acid N-butyl and methyl methacrylate copolymer；Carbon
Nanotube is connected with the graft polymers as matrix by chemical bond, therefore has stronger interfacial interaction, can be with
In being effectively dispersed in polymer, reunion will not be formed, and introduce CNT as polynary physical crosslinking point, when answering masterpiece
When on these thermoplastic elastomer composite materials, scattered CNT is hooked as physical crosslinking due to there are these
Point, stress can be shifted successfully, and so as to avoid stress concentration occurs to early Materials Fracture, therefore the tensile property of finished product are obtained
Very big lifting is arrived, while CNT can significantly increase the mechanical property of material as rigid physical crosslinking point；
BTA, calcium propionate, nylon acid methyl esters that the present invention is added etc., can effectively improve the anti-corrosive properties of finished-product material
Can, improve the bin stability of finished product.
Specific embodiment
A kind of anti-corrosion is grafted composite elastic material, and it is by made by following weight parts raw material：
DMAP 3, triethylamine 1,2- bromine isobutyl acylbromides 0.1, zinc acetylacetonate 0.3, polyethylene glycol 3, the allyl of chlorination 1
Ylmethyl imidazoles 1, methyl methacrylate 50, CNT 10, n-butyl acrylate 40, copper bromide 0.7, pentamethyl divinyl
Triamine 1.6, copper powder 1, dibutyl maleate 3, BTA 0.6, calcium propionate 2, nylon acid methyl esters 4, p-methyl benzenesulfonic acid
0.1st, ethoxylated alkylphenol ammonium sulfate 0.6, tetrahydrofuran 6, absolute ethyl alcohol, ethylene glycol, dimethylformamide, 95% nitric acid,
Thionyl chloride, appropriate chloroform.
A kind of described anti-corrosion is grafted the preparation method of composite elastic material, comprises the following steps：
（1）By above-mentioned polyethylene glycol at 80 DEG C insulated and stirred 5 minutes, add the above-mentioned allyl methyl imidazoles of chlorination 1, insulation to stir
Mix 10 minutes, obtain alcohol dispersion liquid；
（2）Above-mentioned CNT is added in 100 times of its weight, 95% nitric acid, in being sent to 140 DEG C of oil bath, insulation
Stirring 10 hours, suction filtration washes precipitate with deionized water 2 times, is vacuum dried 1 hour at 54 DEG C, obtains acidifying CNT；
（3）Above-mentioned acidifying CNT, calcium propionate are mixed, in being added to the thionyl chloride of 20 times of compound weight, at 60 DEG C
Lower insulated and stirred 20 hours, is distilled off thionyl chloride, in being added to the ethylene glycol of 10 times of its weight, is sent to 110 DEG C of oil
In bath, 46 hours are incubated, suction filtration washes precipitation dimethylformamide 2 times, are vacuum dried 1 hour at 40 DEG C, obtain hydroxylating
CNT；
（4）Above-mentioned hydroxyl carbon nano tube is added in alcohol dispersion liquid, it is 60 DEG C to rise high-temperature, adds above-mentioned acetylacetone,2,4-pentanedione
Zinc, insulated and stirred 10 minutes, suction filtration washes precipitation absolute ethyl alcohol, deionization 3 times, and air drying obtains modified hydroxyl carbon
Nanotube；
（5）Above-mentioned modified hydroxyl carbon nano tube is added in the chloroform of 17 times of its total amount, above-mentioned 4 dimethylamino pyrrole is added
Pyridine, triethylamine, in being sent to ice-water bath, are added dropwise above-mentioned 2 bromine isobutyl acylbromide, and stirring reaction 3 hours, discharging is incubated at room temperature
Reaction 46 hours, suction filtration successively washs filter cake chloroform, deionized water 2 times, is vacuum dried 1 hour at 40 DEG C, must cause
Agent is carbon nano-tube modified；
（6）Above-mentioned BTA is added in nylon acid methyl esters, it is 80 DEG C to rise high-temperature, adds above-mentioned ethoxylated alkyl
Phenol ammonium sulfate, insulated and stirred 3 minutes, obtains ester dispersion liquid；
（7）By above-mentioned methyl methacrylate, n-butyl acrylate, carbon nano-tube modified initiator, pentamethyl-diethylenetriamine,
Copper bromide, the mixing of ester dispersion liquid, in being added to the dimethylformamide of 10 times of compound weight, add above-mentioned copper powder, are passed through nitrogen
Gas, freeze-drying 20 minutes, in being sent to 65 DEG C of oil bath, insulated and stirred 1 hour adds above-mentioned tetrahydrofuran, stirs,
In adding the methyl alcohol of 2 times of mixed system weight, remaining each raw material is added, stand 2 hours, suction filtration, by precipitation dimethyl formyl
Amine, deionized water are washed successively 3 times, are vacuum dried 10 hours at 40 DEG C, obtain the composite elastic material.
Performance test：
Elongation at break：513%；
Tensile strength：7.2N/mm2。
Claims (2)
1. a kind of anti-corrosion is grafted composite elastic material, it is characterised in that it is by made by following weight parts raw material：
DMAP 3-4, triethylamine 1-2,2- bromine isobutyl acylbromide 0.1-0.3, polyethylene glycol 3-4, chlorination 1- pi-allyls-
3- methylimidazole 1-2, methyl methacrylate 50-60, CNT 10-13, n-butyl acrylate 40-51, copper bromide 0.7-
1st, pentamethyl-diethylenetriamine 1.6-2, copper powder 1-2, dibutyl maleate 3-4, BTA 0.6-1, calcium propionate 2-3, Buddhist nun
Imperial acid methyl esters 4-6, p-methyl benzenesulfonic acid 0.1-0.2, ethoxylated alkylphenol ammonium sulfate 0.6-1, zinc acetylacetonate 0.3-1, four
Hydrogen furans 6-8, absolute ethyl alcohol, ethylene glycol, dimethylformamide, the nitric acid of 95-98%, thionyl chloride, appropriate chloroform.
2. a kind of anti-corrosion as claimed in claim 1 is grafted the preparation method of composite elastic material, it is characterised in that including following
Step：
（1）By above-mentioned polyethylene glycol at 80-90 DEG C insulated and stirred 5-10 minute, add above-mentioned chlorination 1- pi-allyls -3- methyl
Imidazoles, insulated and stirred 10-20 minute, obtains alcohol dispersion liquid；
（2）Above-mentioned CNT is added in its weight 100-130 times, 95-98% nitric acid, 140-150 DEG C is sent to
In oil bath, insulated and stirred 10-12 hour, suction filtration washes precipitate with deionized water 2-3 time, and at 54-60 DEG C 1-2 is vacuum dried
Hour, obtain acidifying CNT；
（3）Above-mentioned acidifying CNT, calcium propionate are mixed, in being added to the thionyl chloride of compound weight 20-30 times,
Insulated and stirred 20-25 hour, is distilled off thionyl chloride at 60-70 DEG C, in being added to the ethylene glycol of its weight 10-15 times, send
Enter in 110-120 DEG C of oil bath, be incubated 46-50 hours, suction filtration is washed precipitation dimethylformamide 2-3 time, in 40-50
1-2 hours are vacuum dried at DEG C, hydroxyl carbon nano tube is obtained；
（4）Above-mentioned hydroxyl carbon nano tube is added in alcohol dispersion liquid, it is 60-70 DEG C to rise high-temperature, adds above-mentioned levulinic
Ketone zinc, insulated and stirred 10-20 minute, suction filtration washes precipitation absolute ethyl alcohol, deionization 3-4 time, and air drying obtains modified
Hydroxyl carbon nano tube；
（5）Above-mentioned modified hydroxyl carbon nano tube is added in the chloroform of its total amount 17-20 times, above-mentioned 4- dimethylaminos are added
Pyridine, triethylamine, in being sent to ice-water bath, are added dropwise above-mentioned 2- bromine isobutyl acylbromides, and stirring reaction 3-4 hour discharges, at room temperature
Insulation reaction 46-50 hour, suction filtration washs filter cake chloroform, deionized water 2-3 time successively, is vacuum dried at 40-50 DEG C
1-2 hours, obtain initiator carbon nano-tube modified；
（6）Above-mentioned BTA is added in nylon acid methyl esters, it is 80-85 DEG C to rise high-temperature, adds above-mentioned ethoxylation
Alkyl phenol ammonium sulfate, insulated and stirred 3-4 minute, obtains ester dispersion liquid；
（7）By above-mentioned methyl methacrylate, n-butyl acrylate, carbon nano-tube modified initiator, pentamethyl-diethylenetriamine,
Copper bromide, the mixing of ester dispersion liquid, in being added to the dimethylformamide of compound weight 10-16 times, add above-mentioned copper powder, are passed through
Nitrogen, freeze-drying 20-30 minutes, in being sent to 65-70 DEG C of oil bath, insulated and stirred 1-2 hour adds above-mentioned tetrahydrochysene furan
Mutter, stir, in adding the methyl alcohol of mixed system weight 2-3 times, add remaining each raw material, stand 2-3 hours, suction filtration will
Precipitation dimethylformamide, deionized water are washed 3-4 time successively, and 10-12 hours are vacuum dried at 40-50 DEG C, obtain described
Composite elastic material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370192A (en) * | 2018-10-12 | 2019-02-22 | 安徽徽合台智能科技有限公司 | A kind of lignin enhancing pc material and preparation method thereof |
| CN109537098A (en) * | 2018-10-26 | 2019-03-29 | 董荣志 | A kind of polythiophene conductive fiber and preparation method thereof |
-
2016
- 2016-12-15 CN CN201611161825.7A patent/CN106632916A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370192A (en) * | 2018-10-12 | 2019-02-22 | 安徽徽合台智能科技有限公司 | A kind of lignin enhancing pc material and preparation method thereof |
| CN109537098A (en) * | 2018-10-26 | 2019-03-29 | 董荣志 | A kind of polythiophene conductive fiber and preparation method thereof |
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Application publication date: 20170510 |