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CN108440958A - A kind of activeness and quietness high temperature resistant Load materials and preparation method - Google Patents

A kind of activeness and quietness high temperature resistant Load materials and preparation method Download PDF

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Publication number
CN108440958A
CN108440958A CN201810200867.XA CN201810200867A CN108440958A CN 108440958 A CN108440958 A CN 108440958A CN 201810200867 A CN201810200867 A CN 201810200867A CN 108440958 A CN108440958 A CN 108440958A
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parts
aramid fibre
heterocyclic aramid
high temperature
activeness
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CN108440958B (en
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王朝辉
傅一
陈谦
左志武
陈宝
张长林
周骊威
李林
陈渊召
李振霞
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Changan University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/10Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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    • D06M11/64Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/68Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/80Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/12Aldehydes; Ketones
    • D06M13/127Mono-aldehydes, e.g. formaldehyde; Monoketones
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
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    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides
    • D06M2101/36Aromatic polyamides

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  • Epoxy Resins (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

The present invention provides a kind of activeness and quietness high temperature resistant Load materials and preparation methods, are made by following material:20~30 parts of divinyl sulfone, 1 (2 amine ethyl) 20~40 parts of piperazine, 140~160 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, 130~150 parts of curing agent.The problem of for physical treatment in the prior art, chemical treatment, hyperbranched polysulfones amine is made using 1 (2 amine ethyl) piperazine, divinyl sulfone;Heterocyclic Aramid Fibre is handled using reducing medium and nitrification medium, obtains the Heterocyclic Aramid Fibre that surface carries amino;The hyperbranched polysulfones amine of gained is grafted to the Heterocyclic Aramid Fibre surface through nitrification processing, fiber is uniformly dispensed to tiling, forms skeleton;Mould material prepared by epoxy resin and curing agent is uniformly cast on the fiber reinforcement of tiling, activeness and quietness high temperature resistant Load materials are obtained after solidification.The raw material of this material is easy to get, and reaction process is controllable, reduces technology difficulty, and material possesses excellent mechanical property.

Description

A kind of activeness and quietness high temperature resistant Load materials and preparation method
Technical field
The invention belongs to pavement material fields, are related to Load materials, and in particular to a kind of activeness and quietness high temperature resistant road material Material and preparation method.
Background technology
Paving steel bridge deck adhesive layer mainly has two class material of pitch class and reaction resin class at present.Epoxy resin is as anti- The representative of answering property resinous material is introduced into the country very early.However, epoxy resin is mostly normal temperature cured type material, it is tough after solidification Property it is low, and high temperature resistance exists certain insufficient, therefore the toughening of epoxy resin becomes the focus and difficult point of its application.Use fiber Modified epoxy is important one of toughening methods.Heterocycle fiber have high intensity, high temperature resistant, it is resistant to chemical etching the features such as, However fiber surface itself is smooth, chemism is low, and need to pass through surface treatment could generate good bonding effect with resin matrix Fruit.Currently used fiber surface modification method includes chemical method and physical method.Chemical method includes surface etch, surface Grafting, rare-earth element modified etc., physical method include corona treatment, gamma Rays processing, ultrasonic immersing processing etc..So And chemical modification reaction process is not easy to control, physical method equipment requirement is high, of high cost, and both methods all can be in difference Fiber is caused to damage in degree, reduces the intensity of fiber itself, and then influences its modified effect to epoxy resin.
Therefore, there is an urgent need for developing a kind of activeness and quietness high temperature resistant Load materials, preparation process is simple, reaction process is controllable, Epoxy resin modification difficulty can be reduced, epoxy resin cure intensity, toughness and high temperature resistance are improved.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of activeness and quietness high temperature resistant road material Material and preparation method solve the feature that toughness is low, high temperature resistance is poor after epoxy resin cure.
In order to solve the above-mentioned technical problem, the present invention is realised by adopting the following technical scheme:
A kind of activeness and quietness high temperature resistant Load materials are made in terms of parts by weight of following raw material:Divinyl sulfone be 20~ 30 parts, 1- (2- amine ethyl) piperazine be 20~30 parts, Heterocyclic Aramid Fibre is 140~150 parts, epoxy resin is 100 parts, solidification Agent is 130~140 parts.
The present invention also has following distinguishing feature:
Preferably, it in terms of parts by weight, is made of following raw material:Divinyl sulfone is 30 parts, 1- (2- amine ethyl) piperazine is 20 parts, Heterocyclic Aramid Fibre be 150 parts, epoxy resin is 100 parts, curing agent is 140 parts.
Preferably, the structural formula of the Heterocyclic Aramid Fibre is:
Wherein:N value ranges are 100~200.
Preferably, the curing agent is methyl tetrahydro phthalic anhydride.
The present invention also protects a kind of preparation method of activeness and quietness high temperature resistant Load materials, the preparation method to use institute as above The formula for the activeness and quietness high temperature resistant Load materials stated, this approach includes the following steps:
Step 1 prepares hyperbranched polysulfones amine:
1- (2- amine ethyl) piperazine, divinyl sulfone and chloroform is added in reaction bulb, seals, 5~10min of inflated with nitrogen, The heating stirring 120h at 40 DEG C uses methanol extraction after reaction, and obtained sediment methanol and acetone are respectively washed successively It washs 3~4 times, is dried in vacuo, obtains white powdery solids, obtain hyperbranched polysulfones amine;
Step 2, Heterocyclic Aramid Fibre surface treatment:
Heterocyclic Aramid Fibre is immersed in successively in acetone, petroleum ether and deionized water, cleaning 3h is heated to reflux respectively, takes Go out Heterocyclic Aramid Fibre, is then dried in vacuo 12h at 80 DEG C, obtains Heterocyclic Aramid Fibre;Then again by Heterocyclic Aramid Fibre It is immersed in nitrification medium, nitration reaction 6h at 10 DEG C takes out Heterocyclic Aramid Fibre, rinsed well with deionized water, and dry; Dried Heterocyclic Aramid Fibre is immersed in reducing medium, react at room temperature for 24 hours, take out Heterocyclic Aramid Fibre, spend from Sub- water is rinsed well, and dry, obtains the Heterocyclic Aramid Fibre that surface carries amino;
Step 3, the processing of Heterocyclic Aramid Fibre surface grafting:
Heterocycle aramid fiber of the surface obtained in hyperbranched polysulfones amine made from institute's step 1 and step 2 with amino is fine Dimension is dissolved in dimethyl sulfoxide (DMSO), and drying tunnel is entered after infiltration, and drying tunnel temperature is 160 DEG C, carries out graft reaction and dries, obtains surface The modification Heterocyclic Aramid Fibre of grafting;
Step 4: preparing Load materials:
First, the modification Heterocyclic Aramid Fibre of surface grafting is uniformly dispensed into tiling, forms fiber reinforcement;
Then, curing agent is added into epoxy resin be mixed to form mould material;
Finally, gained mould material is uniformly cast on the fiber reinforcement of tiling, solidification temperature is 80 DEG C, and enhancing is made Toughening high temperature resistant Load materials.
Preferably, in terms of parts by weight, the nitrification medium is 40 parts of fuming nitric aicds, 2 parts of concentrated sulfuric acids, 370 parts of acetic acid The mixture that acid anhydride and 100 parts of glacial acetic acid are uniformly mixed to get.
Preferably, the reducing medium is according to following proportioning mixed solution obtained:Per 0.12g potassium dihydrogen phosphates, 0.36g dipotassium hydrogen phosphates and 0.55g sodium borohydrides correspondence are dissolved in 200mL tetrahydrofurans.
Further, hyperbranched polysulfones amine obtained in step 1 is subjected to amino-terminated processing as follows:
30mL chloroforms are added into hyperbranched polysulfones amine, then 2mL triethylamines are dissolved in 15mL chloroforms, and by three second The chloroformic solution of amine is added in hyperbranched polysulfones amine, and agitating solution simultaneously instills 10mL chlorobenzoyl chlorides in mixed liquor, stirs at room temperature Mix reaction 10h, precipitated with 500mL tetrahydrofurans, sediment through suction filtration, washing, it is dry after obtain that amino-terminated that treated is super Branched polysulfones amine, structural formula are:
Compared with prior art, the present invention having the following technical effect that:
(I) hyperbranched polysulfones amine is used for fibre modification field by the present invention for the first time.Hyperbranched polysulfones amine raw material is easy to get, a step Synthesis, easy to operate, process controllability is good.
(II) a kind of Heterocyclic Aramid Fibre that uses of the present invention full aromatic heterocycle polyamide containing pyridine ring that be main chain, energy are molten For solution in the organic solvents such as dimethyl sulfoxide (DMSO) and n,N-Dimethylformamide, fusing point is more than 360 DEG C, has high intensity, high-modulus, resistance to The excellent properties such as high temperature, resistant to chemical etching.
(III) the hyperbranched polysulfones amine degree of branching is high, has three-dimensional chondritic, molecule is with Amino End Group, vinyl, primaquine A large amount of active function groups such as base, secondary amino group have good mobility and dissolubility, can successfully be grafted to Heterocyclic Aramid Fibre Surface;The Heterocyclic Aramid Fibre surface-active for being grafted hyperbranched polysulfones amine improves, and it is viscous between epoxy resin to can effectively improve it Connect effect.
(IV) the hyperbranched polysulfones amine of Heterocyclic Aramid Fibre surface grafting can be taken with epoxy resin-base in the present invention It connects, forms semi-intercrossing network.Forming composite material using hyperbranched polysulfones amine, Heterocyclic Aramid Fibre and epoxy resin can reach excellent Different epoxy resin roughening effect.
(V) Heterocyclic Aramid Fibre that hyperbranched polysulfones amine is grafted in Load materials prepared by the present invention can effectively improve ring After oxygen resin solidification the shortcomings that toughness low and high temperature poor performance, various types of deck paving adhesive layers can be widely used in.
Explanation is further explained in detail to the particular content of the present invention with reference to embodiments.
Specific implementation mode
In compliance with the above technical solution, specific embodiments of the present invention are given below, it should be noted that the present invention not office It is limited to following specific examples, all equivalent transformations made on the basis of the technical solutions of the present application each falls within the protection model of the present invention It encloses.
Embodiment 1:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 20 parts of divinyl sulfone, 1- (2- amine ethyl) 40 parts of piperazine, 150 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 140 Part.
Wherein, the structural formula of Heterocyclic Aramid Fibre is:
Wherein:N value ranges are 100~200.
The Heterocyclic Aramid Fibre is a kind of full aromatic heterocycle polyamide of main chain containing pyridine ring, can be dissolved in dimethyl sulfoxide (DMSO) It is more than 360 DEG C with organic solvents, fusing points such as n,N-Dimethylformamide.
Epoxy resin is bisphenol A type epoxy resin, and appearance yellowish, epoxide number 0.41, year is 14.2Pas, Number-average molecular weight is 487.
Curing agent is methyl tetrahydro phthalic anhydride.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment includes the following steps:
Step 1 prepares hyperbranched polysulfones amine:
1- (2- amine ethyl) piperazine, divinyl sulfone and chloroform is added in reaction bulb, seals, 5~10min of inflated with nitrogen, The heating stirring 120h at 40 DEG C uses methanol extraction after reaction, and obtained sediment methanol and acetone are respectively washed successively It washs 3~4 times, is dried in vacuo, obtains white powdery solids, obtain hyperbranched polysulfones amine;
Step 2, Heterocyclic Aramid Fibre surface treatment:
Heterocyclic Aramid Fibre is immersed in successively in acetone, petroleum ether and deionized water, cleaning 3h is heated to reflux respectively, takes Go out Heterocyclic Aramid Fibre, is then dried in vacuo 12h at 80 DEG C, obtains Heterocyclic Aramid Fibre;Then again by Heterocyclic Aramid Fibre It is immersed in nitrification medium, nitration reaction 6h at 10 DEG C takes out Heterocyclic Aramid Fibre, rinsed well with deionized water, and dry; Dried Heterocyclic Aramid Fibre is immersed in reducing medium, react at room temperature for 24 hours, take out Heterocyclic Aramid Fibre, spend from Sub- water is rinsed well, and dry, obtains the Heterocyclic Aramid Fibre that surface carries amino;
Step 3, the processing of Heterocyclic Aramid Fibre surface grafting:
Heterocycle aramid fiber of the surface obtained in hyperbranched polysulfones amine made from institute's step 1 and step 2 with amino is fine Dimension is dissolved in dimethyl sulfoxide (DMSO), and drying tunnel is entered after infiltration, and drying tunnel temperature is 160 DEG C, carries out graft reaction and dries, obtains surface The modification Heterocyclic Aramid Fibre of grafting;
Step 4: preparing Load materials:
First, the modification Heterocyclic Aramid Fibre of surface grafting is uniformly dispensed into tiling, forms fiber reinforcement;
Then, curing agent is added into epoxy resin be mixed to form mould material;
Finally, gained mould material is uniformly cast on the fiber reinforcement of tiling, solidification temperature is 80 DEG C, and enhancing is made Toughening high temperature resistant Load materials.
Wherein:
In terms of parts by weight, nitrification medium is 40 parts of fuming nitric aicds, 2 parts of concentrated sulfuric acids, 370 parts of acetic anhydrides and 100 parts of ice The mixture that acetic acid is uniformly mixed to get.
Reducing medium is according to following proportioning mixed solution obtained:Per 0.12g potassium dihydrogen phosphates, 0.36g phosphoric acid hydrogen two Potassium and 0.55g sodium borohydrides correspondence are dissolved in 200mL tetrahydrofurans.
Embodiment 2:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 30 parts of divinyl sulfone, 1- (2- amine ethyl) 30 parts of piperazine, 150 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 140 Part.
The selection of raw material and specification are same as Example 1 in the present embodiment.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment is same as Example 1.
Embodiment 3:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 30 parts of divinyl sulfone, 1- (2- amine ethyl) 20 parts of piperazine, 150 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 140 Part.
The selection of raw material and specification are same as Example 1 in the present embodiment.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment is in addition to step 1, other steps and embodiment Step in 1 is identical.
The step of the step of the present embodiment one and embodiment 1 one, difference lies in by hyperbranched poly obtained in step 1 Sulfone amine carries out amino-terminated processing as follows:
30mL chloroforms are added into hyperbranched polysulfones amine, then 2mL triethylamines are dissolved in 15mL chloroforms, and by three second The chloroformic solution of amine is added in hyperbranched polysulfones amine, and agitating solution simultaneously instills 10mL chlorobenzoyl chlorides in mixed liquor, stirs at room temperature Mix reaction 10h, precipitated with 500mL tetrahydrofurans, sediment through suction filtration, washing, it is dry after obtain that amino-terminated that treated is super Branched polysulfones amine, structural formula are:
Embodiment 4:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 30 parts of divinyl sulfone, 1- (2- amine ethyl) 20 parts of piperazine, 140 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 140 Part.
The selection of raw material and specification are same as Example 1 in the present embodiment.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment is same as Example 3.
Embodiment 5:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 30 parts of divinyl sulfone, 1- (2- amine ethyl) 20 parts of piperazine, 160 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 140 Part.
The selection of raw material and specification are same as Example 1 in the present embodiment.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment is same as Example 3.
Embodiment 6:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 30 parts of divinyl sulfone, 1- (2- amine ethyl) 20 parts of piperazine, 150 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 130 Part.
The selection of raw material and specification are same as Example 1 in the present embodiment.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment is same as Example 3.
Embodiment 7:
The present embodiment provides a kind of activeness and quietness high temperature resistant Load materials, in terms of parts by weight, is made of following raw material: 30 parts of divinyl sulfone, 1- (2- amine ethyl) 20 parts of piperazine, 150 parts of Heterocyclic Aramid Fibre, 100 parts of epoxy resin, curing agent 150 Part.
The selection of raw material and specification are same as Example 1 in the present embodiment.
The preparation method of the activeness and quietness high temperature resistant Load materials of the present embodiment is same as Example 3.
Comparative example 1:
This comparative example provides a kind of Load materials, in terms of parts by weight, is made of following raw material:100 parts of epoxy resin, 140 parts of curing agent.
The selection of middle raw material and specification are same as Example 1 in this comparative example.
This comparative example difference from Example 3 is, is not modified processing to epoxy resin.
The preparation method of the Load materials of this comparative example carries out in accordance with the following steps:Curing agent system is added into epoxy resin Standby mould material, by the evenly laid out cast of gained mould material, solidification temperature is 80 DEG C to get to a kind of Load materials.
Comparative example 2:
This comparative example provides a kind of Load materials, in terms of parts by weight, is made of following raw material:30 parts of divinyl sulfone, 1- (2- amine ethyl) 20 parts of piperazine, 100 parts of epoxy resin, 140 parts of curing agent.
The selection of middle raw material and specification are same as Example 1 in this comparative example.
This comparative example difference from Example 1 is, is modified to epoxy resin only with hyperbranched polysulfones amine.
The preparation method of the Load materials of this comparative example carries out in accordance with the following steps:
Step 1 is identical as the step of embodiment 3 one.
Step 2 prepares Load materials:
The step is corresponding with the step of embodiment 3 four, and detailed process is:By epoxy resin, curing agent and hyperbranched poly Sulfone amine tiles after stirring evenly, and cures to get to a kind of Load materials under the conditions of 80 DEG C.
There is no the step two in embodiment 3 and step 3 in the preparation process of this comparative example.
Comparative example 3:
This comparative example provides a kind of Load materials, in terms of parts by weight, is made of following raw material:Heterocyclic Aramid Fibre 150 parts, 100 parts of epoxy resin, 140 parts of curing agent.
The selection of middle raw material and specification are same as Example 1 in this comparative example.
This comparative example difference from Example 3 is, is modified to epoxy resin only with Heterocyclic Aramid Fibre.
The preparation method of the Load materials of this comparative example carries out in accordance with the following steps:
Step 1 is identical as the step of embodiment 3 two.
Step 2 prepares Load materials:
The step is corresponding with the step of embodiment 3 four, and detailed process is:Curing agent preparation is added into epoxy resin to pour Material is noted, gained mould material is uniformly cast on the fiber reinforcement of tiling, solidification temperature is 80 DEG C and is used to get to a kind of road Material.
There is no the step one in embodiment 3 and step 3 in the preparation process of this comparative example.
Performance test:To verify tensile strength, fracture elongation, shearing strength and the adhesion strength of Load materials, according to According to《Test methods for building waterproof coatings》The relevant regulations of (GB/T 16777-2008) are to institute in the embodiment of the present invention and comparative example Load materials are made and carry out basic performance tests, the results are shown in Table 1.
1 the performance test results of table
Known to analytical table 1:
(A) in the case of Heterocyclic Aramid Fibre, epoxy resin and constant curing agent component, divinyl sulfone and 1- (2- amine Ethyl) piperazine feed molar ratio be 3:Highest output capacity can be reached when 2.
(B) compared with the epoxy resin of non-modified processing, activeness and quietness high temperature resistant Load materials tensile strength and fracture Elongation percentage improves, and illustrates that the strength of materials improves;It is bent under the conditions of -20 DEG C, 90 ° and does not crack, illustrate the toughness enhancing of material;Phase Than in room temperature (25 DEG C) condition, shearing strength is not obvious with adhesive strength decline under the conditions of high temperature (70 DEG C), illustrates material High temperature resistance enhances.
(C) compared with the epoxy resin handled through hyperbranched polysulfones amine, activeness and quietness high temperature resistant Load materials have more preferable Performance, this is because Heterocyclic Aramid Fibre can effectively improve the intensity of epoxy resin.
(D) compared with the epoxy resin handled through Heterocyclic Aramid Fibre, activeness and quietness high temperature resistant Load materials have more preferable Performance, this is because through hyperbranched polysulfones amine be modified there are a large amount of active group, these bases on Heterocyclic Aramid Fibre surface Group can be chemically bonded with epoxy resin, effectively increase the adhesive strength of Heterocyclic Aramid Fibre and epoxy resin.
(E) indices of comparative example 1~7, it can be found that the indices of embodiment 3 are optimal.

Claims (8)

1. a kind of activeness and quietness high temperature resistant Load materials, which is characterized in that in terms of parts by weight, be made of following raw material:Diethyl Alkene sulfone is 20~30 parts, 1- (2- amine ethyl) piperazine is 20~30 parts, Heterocyclic Aramid Fibre is 140~150 parts, epoxy resin is 100 parts, curing agent be 130~140 parts.
2. activeness and quietness high temperature resistant Load materials as described in claim 1, which is characterized in that in terms of parts by weight, by following Raw material is made:Divinyl sulfone is 30 parts, 1- (2- amine ethyl) piperazine is 20 parts, Heterocyclic Aramid Fibre is 150 parts, epoxy resin is 100 parts, curing agent be 140 parts.
3. the activeness and quietness high temperature resistant Load materials as described in claim 1 to 2 any claim, which is characterized in that described The structural formula of Heterocyclic Aramid Fibre be:
Wherein:N value ranges are 100~200.
4. the activeness and quietness high temperature resistant Load materials as described in claim 1 to 2 any claim, which is characterized in that described Curing agent be methyl tetrahydro phthalic anhydride.
5. a kind of preparation method of activeness and quietness high temperature resistant Load materials, which is characterized in that the preparation method is used as right is wanted The formula of the activeness and quietness high temperature resistant Load materials described in 1 to 2 any claim is sought, this approach includes the following steps:
Step 1 prepares hyperbranched polysulfones amine:
1- (2- amine ethyl) piperazine, divinyl sulfone and chloroform, sealing, 5~10min of inflated with nitrogen, 40 are added in reaction bulb Heating stirring 120h at DEG C, after reaction use methanol extraction, obtained sediment methanol and acetone successively respectively washing 3~ 4 times, vacuum drying obtains white powdery solids, obtains hyperbranched polysulfones amine;
Step 2, Heterocyclic Aramid Fibre surface treatment:
Heterocyclic Aramid Fibre is immersed in successively in acetone, petroleum ether and deionized water, cleaning 3h is heated to reflux respectively, takes out miscellaneous Then ring aramid fiber is dried in vacuo 12h at 80 DEG C, obtains Heterocyclic Aramid Fibre;Then Heterocyclic Aramid Fibre is impregnated again In nitrifying medium, nitration reaction 6h at 10 DEG C takes out Heterocyclic Aramid Fibre, is rinsed well with deionized water, and dry;It will do Dry good Heterocyclic Aramid Fibre is immersed in reducing medium, is reacted at room temperature for 24 hours, is taken out Heterocyclic Aramid Fibre, use deionized water It rinses well, and dry, obtains the Heterocyclic Aramid Fibre that surface carries amino;
Step 3, the processing of Heterocyclic Aramid Fibre surface grafting:
Heterocyclic Aramid Fibre of the surface obtained in hyperbranched polysulfones amine made from institute's step 1 and step 2 with amino is molten In dimethyl sulfoxide (DMSO), drying tunnel is entered after infiltration, drying tunnel temperature is 160 DEG C, carries out graft reaction and dries, obtains surface grafting Modification Heterocyclic Aramid Fibre;
Step 4: preparing Load materials:
First, the modification Heterocyclic Aramid Fibre of surface grafting is uniformly dispensed into tiling, forms fiber reinforcement;
Then, curing agent is added into epoxy resin be mixed to form mould material;
Finally, gained mould material is uniformly cast on the fiber reinforcement of tiling, solidification temperature is 80 DEG C, and activeness and quietness is made High temperature resistant Load materials.
6. the preparation method of activeness and quietness high temperature resistant Load materials as claimed in claim 5, which is characterized in that with parts by weight Meter, the nitrification medium are that 40 parts of fuming nitric aicds, 2 parts of concentrated sulfuric acids, 370 parts of acetic anhydrides and 100 parts of glacial acetic acid uniformly mix Obtained mixture.
7. the preparation method of activeness and quietness high temperature resistant Load materials as claimed in claim 5, which is characterized in that the reduction Medium is according to following proportioning mixed solution obtained:Per 0.12g potassium dihydrogen phosphates, 0.36g dipotassium hydrogen phosphates and 0.55g boron hydrogen Change sodium correspondence to be dissolved in 200mL tetrahydrofurans.
8. the preparation method of activeness and quietness high temperature resistant Load materials as claimed in claim 5, which is characterized in that by step 1 In hyperbranched polysulfones amine obtained carry out amino-terminated processing as follows:
30mL chloroforms are added into hyperbranched polysulfones amine, then 2mL triethylamines are dissolved in 15mL chloroforms, and by triethylamine Chloroformic solution is added in hyperbranched polysulfones amine, and agitating solution simultaneously instills 10mL chlorobenzoyl chlorides in mixed liquor, and stirring is anti-at room temperature Answer 10h, precipitated with 500mL tetrahydrofurans, sediment through suction filtration, washing, it is dry after obtain that amino-terminated that treated is hyperbranched Polysulfones amine, structural formula are:
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109486457A (en) * 2018-10-19 2019-03-19 长安大学 A kind of high temperature resistant height glues high-strength and high ductility interlaminar bonding material and preparation method
CN110423452A (en) * 2019-08-02 2019-11-08 长安大学 A kind of road high-strength durable material for quickly repairing and preparation method
CN110551383A (en) * 2019-08-02 2019-12-10 齐鲁交通发展集团有限公司 Reinforced and toughened road rapid repair material and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4137221A (en) * 1974-07-11 1979-01-30 Teijin Limited Heat-curable and solvent-soluble ester group-containing polymer compositions and process for their preparation
US4973631A (en) * 1989-10-06 1990-11-27 Virginia Tech Intellectual Properties Inc. Novel phosphorus containing epoxy networks
CN102675886A (en) * 2012-05-07 2012-09-19 湖北大学 Fiber-reinforced epoxy asphalt material and preparation method thereof
CN104927051A (en) * 2015-06-17 2015-09-23 西南石油大学 Nanometer polymer blocking agent for water-based drilling fluid and preparation method thereof
US9193611B2 (en) * 2011-04-29 2015-11-24 Basf Se Composite membranes comprising a sulfonated polyarylether and their use in forward osmosis processes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4137221A (en) * 1974-07-11 1979-01-30 Teijin Limited Heat-curable and solvent-soluble ester group-containing polymer compositions and process for their preparation
US4973631A (en) * 1989-10-06 1990-11-27 Virginia Tech Intellectual Properties Inc. Novel phosphorus containing epoxy networks
US9193611B2 (en) * 2011-04-29 2015-11-24 Basf Se Composite membranes comprising a sulfonated polyarylether and their use in forward osmosis processes
CN102675886A (en) * 2012-05-07 2012-09-19 湖北大学 Fiber-reinforced epoxy asphalt material and preparation method thereof
CN104927051A (en) * 2015-06-17 2015-09-23 西南石油大学 Nanometer polymer blocking agent for water-based drilling fluid and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109486457A (en) * 2018-10-19 2019-03-19 长安大学 A kind of high temperature resistant height glues high-strength and high ductility interlaminar bonding material and preparation method
CN109486457B (en) * 2018-10-19 2020-12-08 长安大学 High-temperature-resistant high-viscosity high-strength high-toughness interlayer bonding material and preparation method thereof
CN110423452A (en) * 2019-08-02 2019-11-08 长安大学 A kind of road high-strength durable material for quickly repairing and preparation method
CN110551383A (en) * 2019-08-02 2019-12-10 齐鲁交通发展集团有限公司 Reinforced and toughened road rapid repair material and preparation method thereof
CN110551383B (en) * 2019-08-02 2021-03-26 山东高速集团有限公司 Reinforced and toughened road rapid repair material and preparation method thereof

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