Process of production of heat-resistant epoxide compound for glass-fiber materials

FIELD: polymer materials in rocket engineering.

SUBSTANCE: invention concerns process of producing heat-resistant epoxide compound for reinforced glass-fiber bodies used in fabrication of rigid armoring housings for removable charges of solid-fuel rocket engines. Compound is prepared by mixing 28-32% of epoxide dian resin having molecular mass 390-430, 28-32% of epoxide dian resin having molecular mass 480-540, and 14-18% of trimethylolpropane/epichlorohydrin condensation product, mixing being effected for 15-30 min at 80-100° C and stirrer rotation speed 125-158 rpm. When temperature drops to 60-80° C, mixture is supplemented by 24-27% of epoxycyanurate resin and stirred for further 15-30 min at stirrer rotation speed 125-158 rpm under residual pressure not higher than 20 mm Hg.

EFFECT: improved mechanical, adhesion, elastic, and working characteristics at higher vitrification temperature (135° C).

1 tbl, 6 ex

 

The invention relates to the field of rocket technology and concerns a method for obtaining glass-fibre reinforced plastics, in particular of the method of obtaining heat-resistant epoxy compound used in the manufacture of rigid breezepaw for supplementary charges RESF.

Known methods for producing epoxy compositions based on epoxy resins. For example, in the application of Japan No. 6244773 describes a method for epoxy compositions based on epoxy resin, which consists in the fact that Novolac epoxy resin, accelerator and lubricant to form a uniformly mixed in the melt, cooled, pulverized and the resulting powder material is mixed with other components.

The disadvantage of the above method is that the composition is cured, crushed and the crushed product is newly introduced as filler. The obtained product with a high modulus can lead to the emergence of hub tension in the finished material and, as a consequence, the destruction of the material on these high-stressed points.

A method of obtaining modified epoxy resins. For example, in patent No. 2071485 (RU) from 10.01.97, - (prototype) described a method of obtaining modified epoxy resins by reacting epoxygenase resin and on BNR rubber in a ratio of 14:1, respectively, and AK is ivator at a temperature of 25-70° C.

The disadvantage of this method is the low heat resistance of the cured material not exceeding the temperature plus 80°C.

The technical task of the present invention is to provide a heat-resistant epoxy resin compositions with the requirements of high temperature operation supplementary charges solid in terms of aerodynamic heating, which is determined by the glass transition temperature hardened compositions and which should be at the level of 130-135°C. such compositions should possess high mechanical characteristics (tensile strength, modulus and elongation).

The technical result is achieved by mixing epoxy resin with a molecular mass of 390-430 and 480-540 and condensation products of atrial with epichlorohydrin at a temperature of 80-100°C for 15-30 minutes at a rotation speed of the stirrer 125-158 rpm, followed by lowering the temperature to 60-80°C due to input cooling input epoxiconazole resin and stirring for 15-30 min at a rotation speed of the stirrer 125-158 rpm under vacuum at a residual pressure of not more than 20 mm RT. Art. in the following ratio, wt.%:

epoxy resin ED-20 with a molecular mass of 390-430 GOST 10587-84 - 28-32

epoxy resin ED-6 with a molecular mass of 480-540 GOST 10587-84 - 28-32

epoxysilane resin EDP-N TO-032000203306-97 - 24-27

the product of condensation of atrial with epichlorohydrin resin EET-1 TU 2225-527-00203521 - 14-18

Known mixing processes, in which the energy input components are spent not only on homogenization and dispersion, but also for the initiation of chemical interactions between system components with the formation of a new product is heat resistant epoxy compound with a long shelf life of up to one year. Therefore, the proposed method of producing heat-resistant epoxy compound allows to obtain a glass with a high glass transition temperature, high performance while also lowering the viscosity, reducing the technological process of preparation of a binder composition having improved sealing ability stellaemirate.

Obtained by the proposed method heat resistant compound has over existing epoxy compositions several advantages, namely, that the finished epoxy compound, consisting of four components, mixed, homogenized, plasticized, stable when stored within the warranty period of 1 year. Compositions prepared on the basis of heat-resistant epoxy compound used as a curing agent isomeinterface the CSOs anhydride (IMTFE), have high mechanical, adhesive, elastic and operational characteristics and a high glass transition temperature (130-135°C), and therefore, can withstand high temperature transient aerodynamic heating RD.

The table below shows examples of making heat-resistant epoxy compound.

Component nameContent, wt.%
The placeholderExample 1Example 2Example 3Example 4Example 5
1234567
Epoxy resin ED-20 with a molecular mass of 390-43014,028,032,029,230,031,0
On BNR rubber1,0-----
Activator1,25-5,0-----
Epoxy resin ED-16 with a molecular mass of 480-540-30,028,029,232,0280
The product of condensation of atrial with epichlorohydrin resin EET-1-15,015,016,614,016,0
Epoxysilane resin ACD-N-27,025,025,024,025,0
The glass transition temperature, °C80133130135132134

Example 1. of 28.0 g of epoxy resin ED-20 with a molecular weight of 420 and 30.0 g epoxy resin ED-16 with a molecular weight of 480 mixed with 15.0 g of the product of condensation of atrial with epichlorohydrin EET-1 at a temperature of 80°C for 15 minutes at a rotation speed of the agitator 125 rpm Then reduce the temperature due to the applied cooling, add 27,0 g epoxiconazole resin ECD-H and stirred at a temperature of 60°C for 30 min under vacuum at a residual pressure of 20 mm RT. century, when the rotation speed of the agitator 125 rpm

Example 2. of 32.0 g of epoxy resin ED-20 with a molecular weight of 400 and 28.0 g of epoxy resin ED-16 with a molecular weight of 500 mixed with 15.0 g of the product of condensation of atrial with epichlorohydrin EET-1 at a temperature of 90°C for 20 minutes at a rotation speed of the mixer 158 rpm Then reduce the pace is the atur due to the applied cooling, add 25,0 g epoxiconazole resin ECD-H and stirred at a temperature of 65°C for 20 min under vacuum at a residual pressure of 10 mm RT. century, when the rotation speed of the mixer 158 rpm

Example 3. 29,2 g of epoxy resin ED-20 with a molecular weight of 430 and 29.2 g of epoxy resin ED-16 with a molecular weight of 520 mixed with 16.6 g of the product of condensation of atrial with epichlorohydrin EET-1 at a temperature of 100°C for 30 minutes at a rotation speed of the agitator 125 rpm Then reduce the temperature due to the applied cooling, add 25,0 g epoxiconazole resin ECD-H and stirred at a temperature of 70°C for 15 min under vacuum at a residual pressure of 15 mm RT. century, when the rotation speed of the agitator 125 rpm

Example 4. 30.0 g epoxy resin ED-20 with a molecular weight of 415 and 32.0 g of epoxy resin ED-16 with a molecular weight of 510 mixed with 14.0 g of the product of condensation of atrial with epichlorohydrin EET-1 at a temperature of 85°C for 20 minutes at a rotation speed of the mixer 158 rpm Then reduce the temperature due to the applied cooling, add 24,0 g epoxiconazole resin ECD-H and stirred at a temperature of 65°C for 20 min under vacuum at a residual pressure of 10 mm RT. century, when the rotation speed of the mixer 158 rpm

Example 5. 31.0 g epoxy resin ED-20 with molecular the th weight 390 and 28.0 g of epoxy resin ED-16 with a molecular weight of 540 mixed with 18.0 g of the product of condensation of atrial with epichlorohydrin EET-1 at a temperature of 95° C for 25 minutes at a rotation speed of the agitator 125 rpm Then reduce the temperature due to the applied cooling, add 25,0 g epoxiconazole resin ECD-H and stirred at a temperature of 80°C for 30 min under vacuum at a residual pressure of 20 mm RT. century, when the rotation speed of the agitator 125 rpm

Heat resistant epoxy compound obtained by the proposed method has the following characteristics:

- appearance - viscous liquid yellow to dark yellow;

- mass fraction of epoxy group - 23%;

- viscosity on the ball viscometer with ⊘ tube 25-27 mm at a temperature of 50°C - 60;

- storage period at a temperature of 23°C - 12 months.

Physico-mechanical characteristics of the compositions using a heat-resistant epoxy resin, hardened isomethyltetrahydrophthalic anhydride, have significant advantages in comparison with prototype:

- temperature range from + 135°C to 50°C (for prototype from + 80°C to minus 48°C);

- the strength of the adhesive joint is 25.3-27,0 MPa (for prototype 16-20 MPa);

the glass transition temperature plus 135°C (for prototype 30°);

- good technical and operational characteristics, ensuring the quality of charge during the warranty period of storage.

Offer the procedure of obtaining heat-resistant compound for fiberglass is of great interest for use when booking charges to aircraft rocket engines, subjected to significant aerodynamic heating.

The method of obtaining heat-resistant epoxy compound, namely, that mix epoxy resin with a molecular mass of 390-430 and 480-540 and the product of condensation of atrial with epichlorohydrin at a temperature of 80-100°C for 15-30 min at a rotation speed of the stirrer 125-158 rpm, then after lowering the temperature to 60-80°enter epoxiconazol resin and stirred for 15-30 min at a rotation speed of the stirrer 125-158 rpm under vacuum at a residual pressure of not more than 20 mm RT. Art. in the following ratio, wt.%:

epoxy resin with a molecular weight of 390-43028-32
epoxy resin with a molecular weight of 480-54028-32
epoxysilane resin24-27
the product of condensation of atrial with epichlorohydrin14-18



 

Same patents:

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1 ex

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10 cl, 2 tbl, 14 ex

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81 cl, 15 tbl, 5 ex

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1 cl, 2 dwg, 2 tbl, 2 ex

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2 tbl

Compound // 2293099

FIELD: manufacture of building materials.

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1 tbl, 6 ex

FIELD: building industry and materials.

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2 tbl

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2 tbl, 3 ex

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2 cl, 2 tbl

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9 cl, 12 tbl, 11 ex

Compound // 2293099

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1 tbl, 6 ex

FIELD: building industry and materials.

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4 tbl, 2 dwg

Spackling compound // 2281269

FIELD: industry of building materials.

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2 tbl

Putty // 2280061

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EFFECT: improved and valuable properties of putty.

3 tbl

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SUBSTANCE: invention relates to polymeric compositions used for protection against corrosion. Polymeric composition comprises epoxidated rubber or dimethylsiloxane rubber as a polymeric binding agent, polyamide resin or polymethylsilazane as a nitrogen-containing hardening agent, talc or mica as a filling agent, aerosil as a thixotropic additive and electrolytic nickel powder or powder of the alloy system Al-Fe-Cu as a current-conducting additive. The composition can comprise additionally epoxy resin in the amount 10-20 mass. p. Invention provides preparing the composition showing high protective properties in all-climate conditions that allows increasing exploitation period of articles. Invention can be used for filling the internal lap cavity (before welding) formed in the pointed arc welding of metals and alloys.

EFFECT: improved and valuable properties of composition.

7 cl, 2 tbl

Putty // 2259380

FIELD: manufacture of building materials.

SUBSTANCE: putty appropriate leveling of concrete, plaster, and wooden surfaces contains 32-40% tereclite clay, 40-38% alcohol distillery dregs (moisture 85-90%), and 20-25% lime flour.

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2 tbl

Putty // 2259330

FIELD: putties used for finishing concrete and plastered surfaces.

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EFFECT: fast drying of putty.

2 tbl

FIELD: manufacture of building materials.

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3 cl, 2 tbl

The invention relates to the field of building materials, namely filler compositions, representing a highly filled paste, used in construction for interior decoration, and may find wide application in the field of production and modernization of such compositions
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EFFECT: paint with increased performance characteristics.

5 tbl, 4 ex

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