High-strength epoxide composition and preparation method thereof

FIELD: chemistry.

SUBSTANCE: invention refers to the high-strength epoxide composition used for impregnation at production of high-strength glass-, carbon,- organic-, and boron plastics working in the wide temperature range and used in different industrial sectors (machinery construction, shipbuilding, aircraft and space industries, for production of the parts of complicated configuration e.g. thin- and thick-walled casings). The invention refers also to the method for preparation of the said composition including the following components (weight parts): 10-100 - diglycidyl resorcinol ether, 10-100 - product of epichlorohydrin condensation with triphenol, 6-12 - oligoether cyclocarbonates with mass ratio of cyclocarbonate groups in the range from 18 to 29, 28-50 - curing agent (primary aromatic amine), 0.5-2.5 - curing agent (tertiary amine), 0.25-1.25 - mixture of carbon and silicate nanomaterials. The mass ratio of diglycidyl resorcinol ether to product of epichlorohydrin condensation with triphenol is in the range from 1 : 9 to 9 : 1. Metaphenylen diamine or 4,4'-diaminodiphenylmethane or their eutectic mixtures in ratio from 40 : 60 to 60 : 40 are used as primary aromatic amine. Mono-, di and trimethylsubstituted pyridine or monovinylsubstituted pyridine are used as tertiary aromatic amine. The carbon nanomaterial is fullerene C2n, wherein n is no less than 30, the silicate nanomaterial is organobentonite, the fullerene : organobentonite ratio is in the range from 1 : 3 to 3 : 1. The method of composition preparation consists in stirring of nanomaterials mixture with oligoether cyclocarbonates by ultrasonic action at frequency 22-44 kHz during 30-45 min. Then the obtained suspension is mixed with beforehand prepared mixture of diglycidyl resorcinol ether and product of epichlorohydrin condensation with triphenol. After that the curing agent in the form of aromatic primary and tertiary amine mixture is added. The ready composition is cured in step mode with maximal curing temperature 155°C.

EFFECT: invention allows obtaining of the composition with high physical, mechanical and dissipative properties.

2 cl, 2 tbl, 6 ex

 

The invention relates to the field of creation of high-strength composite materials on the basis of fibrous fillers and epoxy resins and can be used to create reinforced plastics structural purpose, used in various branches of engineering and shipbuilding, aviation and space industries, as well as for making parts of complex configuration, for example, thin - and thick-walled buildings.

Modern manufacture of products made of composite materials is mainly based on the use of pre-impregnated reinforcement materials - prepregs. The selection of binder components for the preparation of high performance prepreg is a complex and multistep process, as a binder for them must meet a whole range of material and process requirements.

From the technological side, the main requirement of the prepreg is high viability (low reactivity) of the binder at temperatures of storage and its high reactivity at temperatures of formation of products. Note that these technological requirements in the kinetic aspect means that the binder should have a high activation energy of the curing process.

A characteristic feature of these products atwere the help of epoxy resins by the method of polycondensation in the presence of primary and secondary amines, is the content in mesosaline fragments of the secondary alcohol groups and fixed nodes chemical grid tertiary amino groups. The presence of these groups in the grid structure affects the kinetics and mechanism of the formation of a mesh structure, and properties of the obtained materials. Indeed, these groups can act as active sites for physical grid, resulting in high values of cohesive strength mesh material. In the presence of aromatic amines in fact formed chetyrehskatnye chemical sites, which give the mesh a polymer higher dissipative properties, and heat resistance and glass transition temperature Tarticle(Oleinik E.F. Advances in Polymer Science. 1980. V.80. P.49).

A characteristic feature of the products of the curing of epoxy resins polymerization method in the presence of tertiary amines is education trechcwetnym nodes and flexible ether linkages, which increases the relaxation ability of the binder, but significantly reduces its dissipative properties, and heat resistance and Tarticle. Note that curing of the tertiary amine may or may not be included in the three-dimensional structure. In the latter case, it may play an additional role as a plasticizer (Li X., Neville K. reference guide for epoxy resins. M.: Energy. 1973).

Tert is cnie amines are widely used in epoxy resin as a main hardeners of epoxy resins (for example, triethanolaminato used in the industrial composition of EDB - 10), and as additives to epoxy compositions to reduce the viscosity and regulating the speed of the curing reaction.

It is known the use of epoxy resin mixtures of primary and tertiary amines. So, for epoxy resins based on polyglycidyl ether and polyphenol used a mixture of piperazine with ethanolamine (U.S. Pat. U.S. No. 4110313, 1978, CL 528/90).

Known composition containing diglycidyl ether of diphenylolpropane (DEDTP), diaminodiphenylsulfone (DDFS) and 1% dimethylbenzylamine. The rate of curing this composition increases, but Tarticlesignificantly reduced (Galy I. et al. J. Polymer Engineering and Science. 1986, V.26. No21, P.1514).

Known technical solution relating to the fiberglass-based epoxy resin containing a curing part of the primary, secondary and tertiary amines. So for epoxy resins on the basis of phenylglycidyl ether, and mixtures thereof with haratyuinian ether was used a mixture of triethyltetramine with triethylamine (U.S. Pat. U.S. No. 2783214, 1957, CL 260-28); for epoxy resins based on glycidyloxy ethers of polyphenols and polyalcohol used a mixture of alkylamines followed with tertiary monohydroxylation (U.S. Pat. U.S. No. 2907748, 1959, CL 260-47); for epoxy resins based on polyglycidyl ether and polyphenol applied the mixture is officescape cycloaliphatic amine and tertiary amine (U.S. Pat. U.S. No. 4088633, 1978, CL 528/99; 4185132, 1980, CL 427/137); or a mixture of piperazine with ethanolamine (U.S. Pat. U.S. No. 4110313, 1978, CL 528/90).

The kinetics of curing the oligomeric diepoxides diaminodiphenylsulfone in the presence of 2-methylimidazole described in the article by N. Pirogov. (Plastic masses, 1994, No. 3, p.3-6).

The closest to the technical nature of the claimed invention is a composition containing diglycidyl ether of resorcinol (DEXA), diaminopyridine, monosubstituted methylpyridin(β-picoline). (Smirnov, Y., Mosquitoes B.A. Chemical engineering vasopressin mesh epoxy-amine polymers II. Structure and properties of interconnected polycondensation and polymerization nets. Plastic masses, 2001, No. 11, P6-12).

The main disadvantages of this composition is its low viability and relatively low strength and dissipative characteristics.

All of the above technical solutions, the method of obtaining the polymer compositions were mechanical mixing of the components in the reactor.

The closest to the technical nature of the claimed method for producing polymer compositions is a method comprising preparing a polymer binder, in which the first polymeric binder components containing fulleroid in the form of a suspension in acetone, stirred by ultrasonic in which the effects and then mixed with epoxy oligomer and introduce amine curing agent (U.S. Pat. Of the Russian Federation No. 2223988, CL 08L 63/00, SC 13/02 dated 19.11.2001,).

The method involves the use of a solvent that has a negative impact on the quality of the solidified polymer compositions and products based on them, especially manufactured by the method of "wet" winding.

The present invention is the creation of the epoxy composition with high physical-mechanical and dissipative properties in a wide temperature range, which would provide a sustainable technological processes of obtaining the appropriate glass-, carbon-, organo - and bioplastics known methods, including "dry" and "wet" winding and method of making the composition.

The technical result from the use of the invention is to improve the strength and modulus of elasticity tensile, fracture toughness and glass transition temperature by reducing the viscosity of the composition and increase its viability during processing temperatures (20-70°C).

This result is achieved by the fact that the high-strength composition for impregnation in obtaining glass-, carbon-, organo - and bioplastics, including diglycidyl ether of resorcinol, the hardener is a mixture of an aromatic primary and tertiary amines, primary aromatic amine contains metafemale the diamine or 4,4'-diaminodiphenylmethane or eutectic mixture in a ratio of from 40:60 to 60:40, as the tertiary amine is mono-, di-, trimethylammonium pyridine or monofilament pyridine further comprises the condensation product of epichlorhydrin with triphenols ratio diglycidylether ether of resorcinol and condensation products of epichlorohydrin with triphenols is from 1:9 to 9:1, oligomerisation with mass fraction cyclocarbonate groups from 18 to 29 and a mixture of carbon nanomaterials and silicate types, consisting of fullerene C2nwhere n is not less than 30, and organobentonite at a ratio of 1:3 to 3:1 in the following ratio of components in mass parts:

diglycidyl ether of resorcinol10-100
the condensation product of epichlorohydrin with triphenols100-10
the above oligomerisation6-12
the above primary aromatic
Amin or above
eutectic mixture of aromatic amines28-50
the above tertiary aromatic amine 0,5-2,5
the above mixture of nanomaterials0,25-1,25

A method of obtaining a high-strength epoxy composition for impregnation in obtaining glass-, carbon-, organo - and bioplastic is that the mixture of nanomaterials consisting of fullerene and organobentonite, mixed with oligoethercyclocarbonates by ultrasonic treatment at a frequency of 22-44 kHz for 30-45 min and the resulting suspension is mixed with the previously prepared mixture diglycidylether ether of resorcinol and condensation products of epichlorohydrin with triphenols, then enter the hardener is a mixture of an aromatic primary and tertiary amines, then the finished composition utverjdayut in a stepwise mode with a maximum temperature of curing 155°C.

The invention is illustrated by examples.

Example 1.

Getting suspension - a mixture of nanomaterials oligomerisation.

10 parts by weight of oligomerisation - monacileobaa of polyoxypropyleneglycol with mass fraction cyclocarbonate groups 25-29 mark "Lapolt 301 (TU 2226-303-10488057-94) pour of 0.75 parts by weight of a mixture of nanomaterials consisting of fullerene C84(THE 31968474.1319.001-2000) and organobentonite (TU 952752-2000) in the ratio 2:1 and the mixture is dispersed is stirred by ultrasonic treatment with preparing the aqueous emitter of USSN (TU 25-7401,0027-88) for 45 min at a frequency of exposure to 22 kHz.

Previously in the reactor, equipped with a mechanical stirrer, heating and cooling, with constant stirring download 50 parts by weight of diglycidylether ether of resorcinol (technical product - resin pack-637 THE 6-05-241-194-79) and 50 parts by weight of the product of the interaction of epichlorohydrin with triphenols (technical product - resin ETF THAT 2225-316-09201208-949), warmed to 55-60°C (at a ratio of resin 1:1), the mixture is stirred for 20-25 min and injected into the reactor prepared suspension of nanomaterials in "Lapolt 301"; the contents of the reactor are stirred for at least 30 min, and then injected into the reactor hardener - first 40 parts by weight of a melt of a primary aromatic amine - eutectic mixture of metaphenylenediamine (GOST 5826-68) and 4,4'-diaminodiphenylmethane (TU 6-14-415-70) in a ratio of 40:60, the mixture is stirred for 30 min, cooled to a temperature of 35-40°C and injected 1.5 parts by weight of tertiary amine - disubstituted pyridine-2,4-lutidine (CAS N 141866).

Prepared epoxy resin composition is thoroughly mixed, vaccuming under pressure (-0,9-1) kgf/cm2within 15 min, after which it is poured into metal molds and utverjdayut in a stepwise mode:

Temperature °CThe exposure time, hours
501,5
853,0
12520
1552,0

Examples 2-6 carried out analogously to example 1, but the ratio and the name of the components shown in table 1. In examples 2 and 3 ultrasonic treatment under stirring nanomaterials with oligoethercyclocarbonates produced using an ultrasonic disperser of UZDN-2T (CFT) with frequency and exposure time of 30 kHz to 35 minutes, 44 kHz - 30 min, respectively.

In addition, table 1 shows the formulations of the inventive compositions for each example.

Table 1
The composition of the epoxy kompzicii
Formulations bisoprolol epoxy composition
№ p/pName of the componentName (brand) of the components, their ratio examples
123456
1.Diglycidyl ether Rezo is the Qing, parts by weightUE-637
50
UE-637
10
UE-2130
83
UE-637
90
UE-637
90
UE-2130
83
2.The condensation product of epichlorohydrin with triphenols (PCAT) parts by weightETF
50
ETF
90
ETF
17
ETF
10
ETF
10
ETF
17
3.The ratio of DER:PCAT1:11:95:19:11:15:1
4.Oligomerisation, parts by weightLaprolan 301 GLaprolan 803Laprolan 301 GLaprolan 803A mixture of libralato 301 G and 803 in the ratio of 5:95A mixture of libralato 301 G and 803 in the ratio of 50:50
101268 106
5.A mixture of nanomaterials - fullerene C2nwhere n is not less than 30 and organobentonite (ABOUT), parts by weightFullerene C-84 with ABOUT 0,75Fullerene C-60 with ABOUT 0,25Fullerene C-60 with ABOUT a 1.25Fullerene C-84 with ABOUT 0,5Fullerene C-84 with ABOUT 0,75Fullerene C-60 with ABOUT a 1.25
6.The ratio of the fullerene and ABOUT2:11:13:11:32:13:1
7.Primary aromatic amine, parts by weightAntactica a mixture of MFDA andMFDA 28Antactica a mixture of MDF and4.4 DBP FMAntactica a mixture of MFDA and 4,DAD
F
Antactica a mixture of MFDA and DD
F
DD FM ratioDD FM in the ratio of 60:4050 M in the ratio of 60:40
40:60354035
40
8.Tertiary aromatic amine, parts by weight2,4-lutidine4-vinylpyridin2,4,6-kallidinβ-picoline2,4-lutidine2,4,6-kallidin 0,5
1,50,52,01,5
2,5

Properties of the proposed compositions of examples 1-6 in comparison with known presented in table 2.

Table 2.
The performance properties of the composition
№ p/pName of indicators and the method of its determinationValue
ExamplesPrototype: Plastic masses. 2001. No. 2. p.19-25
123456
1.The tensile strength, MPa, GOST 11262-80153158156152155154118
2.The modulus of tensile elasticity, GPA, GOSTwith 3.273,523,43,063,283,352,45
3.Fracture toughness, γ×10-2J/m2Characterizes the dissipative St is in the composition; the determination by the method of "splitting" as the value of the surface of the destruction of γ in equation Griffiths,* namely the energy value, dyslipidaemia when the crack opening38,448,136,335,838,736,722,5 is 30.5
4.The glass transition temperature, °C, is determined using DSC165170160150166160130
5.Viability, τηmin composition at a temperature of processing was defined as the time to reach the viscosity of 1200 MPa·s at a rotational viscometer, REATEST-II230185190220225195140
* equation Griffiths: σCR.=2γ/πlCR.
- kN. Berry J. P. Destruction. M.: Mir, 1976, Vol.7, part II, p.8-62
where: E is the modulus of elasticity;
lCR.- p is Ramer defects;
γ is the fracture toughness (dissipative parameter).

As can be seen from table 2, the proposed high-strength epoxy composition produced by the proposed method has significantly higher performance in comparison with the known, namely increased indicators:

- limits of tensile strength at 17-30%;

the modulus of tensile elasticity of more than 30%;

- toughness and fracture - 25-60%;

- glass transition temperature - 20-40°C;

- viability - 1.3-1.7 times.

The set of indices produced by the proposed method the proposed epoxy composition allows its use for effective and technologically advanced manufacturing processes, high-strength, glass-, carbon-, organic-, bioplastique products, operating in a wide temperature range, in particular, for facilities and space technology.

1. High strength epoxy composition for impregnation in obtaining glass, coal, organic and bioplastics, including diglycidyl ether of resorcinol, the hardener is a mixture of an aromatic primary and tertiary amines, wherein the primary aromatic amine it contains metaphenylenediamine or 4,4'-diaminodiphenylmethane or eutectic mixture in a ratio of from 40:60 to 60:40, as t is knogo Amin - mono-, di-, trimethylammonium pyridine or monofilament pyridine, optionally, a condensation product of epichlorohydrin with triphenols ratio diglycidylether ether of resorcinol and condensation products of epichlorohydrin with triphenols is from 1:9 to 9:1, oligomerisation with mass fraction cyclocarbonate groups from 18 to 29 and a mixture of carbon nanomaterials and silicate types, consisting of fullerene C2nwhere n is not less than 30, and organobentonite in the ratio from 1:3 to 3:1 in the following, wt. including:

diglycidyl ether of resorcinol10-100
the condensation product of epichlorohydrin with triphenols10-100
the above oligomerisation6-12
the above primary aromatic amine or
above the eutectic mixture of aromatic amines28-50
the above tertiary aromatic amine0,5-2,5
the above mixture of nanomaterials0,2-1,25

2. A method of obtaining a high-strength epoxy composition for impregnation in obtaining glass, coal, organic and bioplastics according to claim 1, which consists in the fact that the mixture of nanomaterials consisting of fullerene and organobentonite, mixed with oligoethercyclocarbonates by ultrasonic treatment at a frequency of 22-44 kHz for 30-45 min, and the resulting suspension is mixed with the previously prepared mixture diglycidylether ether of resorcinol and condensation products of epichlorohydrin with triphenols, then enter the hardener - the above mixture of aromatic primary and tertiary amines, then the finished composition utverjdayut in a stepwise mode with a maximum temperature of curing 155°C.



 

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3 cl, 3 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: first version of invention claims composition of the following component ratio, wt %: N,N,N',N'-tetraglycidyl-4,4'-diamino-3,3'-dichlordiphenylmethane 24.8÷42.1 and triglycidyl-aminophenol as polyfunctional epoxy resins 11.5÷25.8, polycrystalline powder of N,N'-hexamethylenebismaleimide as bismaleimide 25.8÷41.3, polycrystalline powder of 4,4'-diaminodiphenylsulfone as solidifier 17.4÷22.6. Second version of invention claims composition of the following component ratio, wt %: N,N,N',N'-tetraglycidyl-4,4'-diamino-3,3'-dichlordiphenylmethane 21.6÷49.5 and triglycidyl bisphenol-A ether as polyfunctional epoxy resins 16.1÷32.4, polycrystalline powder of N,N'-hexamethylenebismaleimide as bismaleimide 3.5÷27.0, polycrystalline powder of 4,4'-diaminodiphenylsulfone as solidifier 19.0÷25.8. Method of obtaining the claimed compositions involves addition of polycrystalline 4,4'-diaminodiphenylsulfone powder to homogenous polyfunctional epoxy resin melt during stirring at 120÷130°C in minimum time sufficient for its complete dissolution. Then the temperature of obtained homogenous melt is lowered to 90÷100°C. By further stirring polycrystalline powder of N,N'-hexamethylenebismaleimide is added to the melt in minimum time sufficient for its complete dissolution. Prepreg includes components at the following ratio, wt %: the claimed epoxybismaleimide binding agent 20-48 and fiber filler 52-80. An article is produced by the claimed prepreg modelling.

EFFECT: improved durability of binding agent and increased vitrifying temperature and flexural strength of article.

6 cl, 2 tbl, 10 ex

FIELD: technological processes.

SUBSTANCE: glue strips are applied with preset pitch onto glass tissue cloth in longitudinal direction, then they are dried, and glass tissue with applied glue strips is cut into preforms in direction that is perpendicular to glue strips, honeycomb packet is assembled from prepared preforms by laying with displacement of every preform in respect to glue strips that are adjacent by half of pitch, preforms of honeycomb packet are glued at preset temperature and pressure, and honeycomb unit is produced by means of honeycomb packet extension, then prepared extended honeycomb unit is soaked with polymer binder, it is hardened in accordance with preset mode, at that as glass tissue thin glass tissue is used on the basis of fibres made of alumina-borosilicate alkali-free glass of "А-5Пx90" or "А-4Пx90" type, for glue strips phenol-polyvinyl-acetal glue is used of BF-2 type with viscosity of 45 by viscosity gage VZ-246, gluing of honeycomb packet preforms is carried out under vacuum of 0.12-0.16 kgf/cm2 according to temperature-time mode: heating up to temperature of 80°C with further pause of 30 minutes, heating up to temperature of 150°C with further pause of 60 minutes, heating up to temperature of 170°C with further pause of 120 minutes, as polymer binder for soaking, bakelite lacquer is used of LBS-1 brand with viscosity of 15 by viscosity gage VZ-246, hardening of honeycomb unit soaked with polymer binder is carried out in accordance with the following mode: heating up to temperature of 100°C with further pause of 30 minutes, heating up to temperature of 150°C with further pause of 90 minutes, heating up to temperature of 170°C with further pause of 120 minutes.

EFFECT: provision of honeycomb filler compression strength; expansion of assortment of manufactured honeycomb filler and increase of manufacturability.

1 tbl, 6 ex

FIELD: technological processes.

SUBSTANCE: method includes the following: viscose or polyacrylonitrile technical thread is soaked with the mixture of epoxy resin ED-20 and hardener polyethylene polyamine with mass ratio 9:1. Then bundle is formed out of separately soaked technical threads with the number of threads of 100-140 and is thermally treated at the temperature of 30-70°C. At the same time the shaped bundle is exposed to ultraviolet radiation with power of 0.70-0.80 Watt/m3 at the wave length of λ=253.7 for 8-12 minutes, and then hardened.

EFFECT: increases breaking stress during static bending of materials with polyacrylonitrile technical thread.

2 tbl

FIELD: construction engineering; mechanical engineering; rocketry; space engineering for fire safety of articles.

SUBSTANCE: proposed binder contains components at the following ratio, parts by mass: epoxy-dian resin, 100; aniline-phenol-formaldehyde resin used as hardening agent, 80-100; urethane prepolymer used as modifying agent, 50-65; 3,3'-dichloro-4,4'-diamino-diphenyl methane used as hardening agent, 8-15; 2,2'-bis(3,5-dibromo hydroxyphenyl) propane, 120-140; solvent, 225-290. Used as solvent is alcohol-acetone mixture at mass ratio of alcohol to acetone of 1:1.

EFFECT: reduction of gelatinization time; production of prepreg on base of this binder at high life time and difficultly combustible plastic at high ultimate strength.

8 ex

FIELD: resins, chemical technology.

SUBSTANCE: invention relates to technology for preparing molded articles, in particular, a polishing disk comprising fabric interlayers that are impregnated with a thermoreactive synthetic resin-base binding agent. Binding agent used for impregnation represents thermoreactive resin alcoholic solution or mixture of resins, or mixture if resins with a hardening agent. Before the impregnation process 1-15% of additive is added to the solution chosen from group of fatty acid amides or fatty acid substituted amides as measured for amount of resin or mixture of resins, or mixture of resin with a hardening agent. Invention provides simplifying process for stacking articles, possibility for their repeated separation one from another and without decreasing their quality.

EFFECT: improved preparing method.

7 cl, 1 ex

FIELD: chemistry of polymers.

SUBSTANCE: invention relates to a polymeric binding agent for composition materials used as structural materials in machine engineering, aircraft construction and instrument making. Binding agent comprises the following ratio of components, mas. p. p.: epoxy resin ED-20, 50-60; phenolformaldehyde resin RFN-60, 40-50, and additive, 6-7. Mixture of triethanolamine (6 mas. p.) and salicylal-5-methoxy-8-aminoquinoline (0.5 mas. p.) is used as an additive. Invention provides decreasing hardening time, to enhance bending strength and reduce the friction coefficient of the proposed composition material.

EFFECT: improved and valuable technical properties of material.

2 tbl, 3 ex

FIELD: chemistry; production of composite materials.

SUBSTANCE: epoxy binder consists of the following components in the given mass ratios: 100 epoxy diane resin, 60-80 iso-methyltetrahydrophtalic anhydride, 1.0-2.0 hardener. The hardener used is an alkanolamine with general formula where R= (CH2)2, (CH2)6; R2=C6H5OCH2, CH2=CHCH2OCH2, HOCH2, ClCH2.

EFFECT: improved operational characteristics of the binder, lower temperature and time of hardening, wide assortment of binders on epoxy resin base.

4 tbl, 9 ex

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