RU1783823C - Method of joining smooth metallic surface - Google Patents

Abstract

FIELD: automobile industry. SUBSTANCE: method involves application at least on one of surfaces anaerobic composition consisting of (poly)ethylene glycol dimethacrylate or its mixture with monomethylacrylate, hydroperoxide initiator, amine or sulfimide accelerator and stabilizing system followed by surface joining in the presence of epilam of the formula CF₃(OC₃F₆)_mOCF₂C(O)(CF₂)_n-C(O)R, where m 35; n 2-4; R OH, NH. N(O)NH...N(O)(CH₃)_2i; taken at concentration 0.05-10.00 mas. p. per 100 mas. p. (poly)ethylene glycol dimethacrylate and its mixture with monomethylacrylate. Steel specimens (roughness -NH...NH(CH₃)_2i-NH₂ 0.09-0.15 mcm) were worked preliminary with epilam, then anaerobic composition is applied and surfaces were joined, or anaerobic composition containing epilam is applied on steel surfaces. Hardening is carried out at the room temperature. Properties of join at roughness 0.09-0.15 mcm: fixation time is 15-45 min, strength limit at uniform break off after 3 h is 13.0 MPa, after 24 h 8.3 MPa. EFFECT: improved method of joining. 1 tbl

Description

 The invention relates to methods for joining smooth metal surfaces with anaerobic compositions, namely, to improving the method for joining smooth surfaces with known anaerobic compositions containing dimethacrylate (poly) ethylene glycol as a monomer or a mixture thereof with monomethacrylate, an initiating system comprising a hydroperoxide initiator, an amine and sulfimide and a stabilizing system.

 Based on the known methods, industrial brands Unigerm-6 (TU 6-01-1285-84), Unigerm-7 (TU 6-01-1312-85), Unigerm-8 and Unigerm-9 (TU 6-01-1326- 86), Anaterm-1u (TU 6-01-1308-85), Anaterm-117 (TU 6-01-2-1304-85). Anaterm-260 (TU 6-01-2-712-86). Anaterm-6K and Anaterm-8K (TU 6-01-2-726-86).

 The method of joining smooth surfaces is that an anaerobic composition is applied to one of the surfaces and the surfaces to be joined are combined.

 In the manufacture of automobiles and agricultural machinery, as well as in other engineering industries where conveyor assembly is used, the most important requirement is the requirement for a quick and reliable connection of parts. At the same time, the fixation time (time to reach manual strength) should not exceed 1 hour. A set of functional strength (at least 50% of full strength) should be carried out in no more than 3 hours, and full strength should be achieved within 24 hours.

 The method of joining smooth surfaces using these anaerobic compositions satisfies these requirements when connecting surfaces with a roughness Ra of 1.5-2.2 μm. However, when connecting surfaces of higher processing purity (roughness Ra 0.09-0.15 μm), it no longer meets the requirements of conveyor production. The fixation time is 5-8 hours, a set of functional strength is carried out in 18-24 hours, and full strength is achieved in 48 hours. Therefore, the scope of the method is limited.

 The connection of such surfaces can be accelerated using activators, for example, metal salts of variable valency, aldimines, thiourea, etc. For this, the surfaces are pretreated with a solution of the activator in a volatile organic solvent, after the evaporation of the solvent, an anaerobic composition is applied and the surfaces are combined.

 The use of activators in the conditions of conveyor production is not technologically advanced due to environmental pollution by vapors of highly toxic solvents. The preliminary introduction of activators into the composition is impossible due to the premature polymerization of the composition. In addition, when using activators, the strength characteristics of the compound are reduced.

 The aim of the invention is to expand the scope of the method by accelerating the process of connecting surfaces with a roughness Ra of 0.09-0.15 microns.

(CF₂)_n-C

где m 35; n 2-4;
R -OH, -NH.N

,
-NH. NH

, -NH₂ взятого в количестве 0,05-10,00 мас.ч. на 100 мас.ч. диметакрилата (поли)этиленгликоля или его смеси с монометакрилатом.The goal is achieved in that in a method for joining smooth metal surfaces by applying at least one of the surfaces of an anaerobic composition containing dimethacrylate (poly) ethylene glycol or a mixture thereof with monomethacrylate, a hydroperoxide initiator, an amine and sulfimide accelerator and a stabilizing system, followed by combining surfaces, in contrast to the known, the connection is carried out in the presence of an epilam of the following formula:
CF ₃ (OC ₃ F ₆ ) _m OCF

(CF ₂ ) _n -C

where m 35; n 2-4;
R-OH, -NH.N

,
-NH. NH

, -NH ₂ taken in an amount of 0.05-10.00 parts by weight per 100 parts by weight (poly) ethylene glycol dimethacrylate or a mixture thereof with monomethacrylate.

 You can connect smooth surfaces in the presence of an epilam by pre-treating the surfaces to be glued with an epilam followed by applying an anaerobic composition and combining the surfaces, as well as by introducing the epilam into an anaerobic composition, applying this composition to one of the surfaces and combining the surfaces.

-(CF₂)_n-COOH, где m

35, n 2-4.Used epilams (TU 6-02-1229-82 with amendment N 1) of the following composition:
CF ₃ (OC ₃ F ₆ ) _m -OCF ₂ -

- (CF ₂ ) _n -COOH, where m

35, n 2-4.

-(CF₂)_n-C

где m

35, n 2-4.Epilam 6-MFK-180
CF ₃ (OC ₃ F ₆ ) _m -OCF ₂ -

- (CF ₂ ) _n -C

where m

35, n 2-4.

-(CF₂)_n-C

где m

35, n 2-4.Epilam 4AS9T
CF ₃ (OC ₃ F ₆ ) _m -OCF ₂ -

- (CF ₂ ) _n -C

where m

35, n 2-4.

-(CF₂)_n-C

, где m

35, n 2-4,
аминофен.Epilam 4AC9
CF ₃ (OC ₃ F ₆ ) _m OCF ₂ -

- (CF ₂ ) _n -C

where m

35, n 2-4,
aminophen.

 Epilams are non-toxic, heavy, non-volatile liquids that are odorless, therefore, in the case of preliminary processing of glued surfaces with epilams, they do not evaporate and do not pollute the environment, but remain on the surface in the form of a monomolecular layer. When epilams are introduced in the indicated amounts into anaerobic compositions, they do not cause premature polymerization of the compositions during storage and do not reduce the strength characteristics of the compound.

 The (meth) acrylic monomers used are (poly) ethylene glycol dimethacrylates: ethylene glycol dimethacrylate (DMEG, TU 6-01-843-78), triethylene glycol dimethacrylate (TGM-3, STP2-9-88), tetraethylene glycol dimethacrylate (TGM-4, TGM-4 STP-2-9-88) and their other mixtures with monomethacrylates-octyl methacrylate (OMAC, STP2-15-79), ethylene glycol methacrylate (MEG, TU 6-01-1240-80), methoxyethylene glycol methacrylate (MDEM, STP2-17- 79), decylmethacrylate (DMAK, STP2-15-79), etc.

 The initiating system provides curing of the anaerobic composition when it enters a narrow gap in case of violation of contact with oxygen.

 The initiating system includes the hydroperoxide initiator cumyl hydroperoxide (GPC, TU 6-01-879-79), tert-butyl hydroperoxide (GPTB, TU 6-01-463-76) and others, the sulfimide accelerator o-benzenesulfimide (OBSI, TU 64-6-126-79), dibenzenesulfimide (DBSI, TU 6-09-10-923-73) and others, amine accelerator dimethylaniline (DMA, GOST 5855-79), dimethyl p-toluidine (DMPT, TU 6- 09-2497-77), dimethyl-p-anisidine (DMAN, TU 6-09-1752-72), etc.

 The inhibitory system ensures the viability of the anaerobic composition and protects it from premature polymerization during storage.

 The inhibitory system includes 2,2,6,6-tetramethyl-4-oxopiperidin-1-ox-sil (TMOP, 6-06-31-304-79), hydroquinone (GC, GOST 19627-74), benzoquinone ( BKh, TU 6-09-156-70), naphthoquinone (HX, TU 6-09-2520-72), oxalic acid (ShK, GOST 22180-76), 4,4'-bis- (dimethylamino) triphenylmethane-xolate (MOH, malachite green, TU 6-09-1551-77), disodium salt of ethylenediamine-N, N, N ', N'-tetraacetic acid (Trilon B, GOST 10652-73), etc.

 It is also possible to add plasticizers, thickeners, dyes, fillers, metal salts of constant valency to the anaerobic composition.

 Anaerobic compositions are prepared by mixing its constituent components in a glass reactor at room temperature until completely dissolved.

The connection of smooth metal surfaces is as follows. In one case, steel samples according to GOST 14760-69 (samples have a joint area of 5 cm ² ) with a roughness Ra of 0.09-0.15 μm are pre-treated with epilam, then anaerobic composition is applied (the amount of epilam is taken from the calculation of 0.05-10 wt parts per 100 parts by weight of monomers) and the surfaces are combined. In another case, an anaerobic composition containing 0.05-10 parts by weight is applied to steel samples. epilame per 100 parts by weight monomers, and surfaces combine. Curing is carried out at room temperature.

The following characteristics of the compound are then determined:
fixation time, the fixation time is the time after which the connected surfaces cannot be manually shifted relative to each other;
ultimate strength at uniform separation (σ _neg ) according to GOST 14760-69 3 hours (σ _neg ¹ ) and 24 hours (σ _neg ² ) after the beginning of curing on samples with a surface roughness Ra of 0.09-0.015 μm;
for comparison, the tensile strength was determined with uniform separation (σ _spr ³ ) on steel samples with a surface roughness of Ra 1.5-2.2 μm 24 hours after joining the surfaces.

PRI me R 1. On steel samples according to GOST 14760-69 applied anaerobic composition of the following composition, parts by weight TGM-3.75; MEG 25; CCP 1.5; DMPT 0.6; OBI 0.8; sodium chloride 0.5; ALK 0.001; TMOP 0.001 and epilame 4AC9 0.05. The surfaces were aligned, curing was carried out at room temperature. The following characteristics of the compound were determined: fixation time on surfaces with a roughness Ra 0.09-0.15 μm; tensile strength with uniform separation on surfaces with a roughness Ra of 0.09-0.15 μm after 3 hours (σ _sp ¹ ) and 4 hours (σ _sp ² ); full bond strength (σ _neg ³ ) on surfaces with a roughness Ra of 1.5-2.2 μm after 24 hours. The test results are shown in the table.

 PRI me R 2. On steel samples in accordance with GOST 14760-69 applied anaerobic composition of the following composition, wt.h. TGM-4.60; OMAC 40; GPTB 2; DBSI 1.5; DMAN 1.2; dioctyl phthalate (DOP plasticizer) 20; rubber SKN-30, KTPA (thickener) 1.5; MOH 0.02; HX 0.05; TMOP 0.05; Trilon B 0.08; magnesium acetate 1.5; powder ftoroplast F-4 (filler) 18; Aerosil A-300 (thixotropic agent) 4 and 4AC9T 2 epilam. The surfaces were combined, curing was carried out at room temperature. The tests were carried out as in example 1. The test results are shown in the table.

 PRI me R 3. On the surface of steel samples in accordance with GOST 14760-69 applied epilame 6MFK-180 at the rate of 0.015 g (10 parts by weight per 100 parts by weight of monopolymers) epilam per 1 sample. Then, 0.15 g of anaerobic composition of the following composition was applied to each sample, parts by weight DMEC 55; MDEM 15; DMAK 30; CCP 0.2; DMA 0.2; OBI 0.2; MOH 0.02; GC 0.05; TMOP 0.03; dye 0.01; Aerosil A-300 (thixotropic agent) 3.5. The surfaces were aligned, curing was carried out at room temperature. The tests were carried out as in example 1. The test results are shown in the table.

 PRI me R 4. On the surface of steel samples according to GOST 14760-69 applied epilame 6MFK-180 at the rate of 0.0015 g (1 part by weight per 100 parts by weight of monomer) epilam per 1 sample. Then, 0.15 g of anaerobic composition of the following composition was applied to each sample, parts by weight TGM-3 100; GPC 1; DMPT 2; OBSI 2; ShchKO 1; TMOP 0.05; HX 0.05. The surfaces were aligned, curing was carried out at room temperature. The tests were carried out as in example 1. The test results are shown in the table.

 PRI me R s 5-7. In the well-known industrially developed anaerobic compositions Unigerm-6, Unigerm-9, Anaterm-8K epilums were added in the amount corresponding to the proposed method. The compositions were thoroughly mixed and applied to the surface of steel samples according to GOST 14760-69. The surfaces were aligned, curing was carried out at room temperature. The tests were carried out as in example 1. The test results are shown in the table.

 PRI me R s 8-10 (known). The industrialized anaerobic compositions Unigerm-6, Unigerm-9, Anaterm-8K were applied to the surface of steel samples according to GOST 14760-69. The surfaces were aligned, curing was performed at room temperature. The tests were carried out as in example 1. The test results are shown in the table.

 As can be seen from the table (examples 1-7), when connecting metal surfaces with high purity (roughness Ra 0.09-0.15 μm) according to the proposed method, the fixation time does not exceed 1 h, together with the anaerobic epilam composition, and a set of functional strength (at least 50% of full strength) occurs in less than 3 hours. In this case, full strength on samples with a surface roughness of Ra 0.09-0.15 μm is achieved in 24 hours (93-100% of the total strength obtained on samples with a surface roughness of Ra 1.5-2.2 μm).

 When connecting metal surfaces with high purity by known methods, fast and reliable joining of parts is not achieved (examples 8-10).

 Thus, the use of epilam allows you to accelerate the connection of surfaces of high purity processing known anaerobic compositions. This makes the compositions more universal, expands the scope of their application.

Claims (1)

METHOD FOR CONNECTING SMOOTH METAL SURFACES by applying to at least one of the surfaces of an anaerobic composition containing (poly) ethylene glycol dimethacrylate or its mixture with monomethacrylate, a hydroperoxide initiator, an amine and sulfimide accelerator, and a stabilizing system with in order to accelerate the process of joining surfaces with a roughness of Ra0.09 - 0.15 μm, the connection is carried out in the presence of an epilam of the following formula:

where m35; n2-4;

-NH ₂
taken in an amount of 0.05 to 10.00 wt. hours per 100 parts by weight (poly) ethylene glycol dimethacrylate or a mixture thereof with monomethacrylate.

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