前苏联专利SU869561A3 Polymeric composition

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专利摘要:
A hardenable composition for use as an adhesive in sealing, spackling, filling, stamping and the like composed of a first component of a monomeric, oligomeric or polymeric compound and a hardening promoting agent, wherein the first component or the hardening promoting agent is encased in a protective casing to prevent rupturing of the casing or hardening of the composition, and a casing rupturing agent composed of microspheres which break under pressure into fragments which have angular edges or are acutely tapered.
公开号:SU869561A3
申请号:SU762387553
申请日:1976-08-11
公开日:1981-09-30
发明作者:Хинтервальднер Рудольф
申请人:за витель Иностранец (ФРГ)；
IPC主号:

专利说明:

(54) POLYMER COMPOSITION
The invention relates to the preparation of a polymer paste-like thixotropic composition used as a putty, adhesives, compaction and coatings.
Dry building mortars and masses for putty based on calcined gypsum, containing microencapsulated auxiliary substances fl.
However, despite the long period of swelling, dissolution and intense mechanical stresses, the capsules are slightly destroyed, which does not allow to obtain a mass with stable properties and high viscosity values.
The closest in technical essence and the obtained result to the 20 proposed is a sealing or adhesive composition containing a liquid polymer and a hardener, and one of the components can be encapsulated G2 .25
However, this composition has an increased cure time. When using compositions with added fillers to impart high viscosity and thixotropy, sex occurs
capsules and there is a partial cure, loss of adhesion or leaks.
The purpose of the invention is to reduce the curing time and increase the viability.
The goal is achieved by the fact that a polymer composition comprising a polymer and a hardener, one of the components being encapsulated, contains as the polymer a compound selected from the group including unsaturated polyester resin, polyvinyl acetate, polysulfide, urea formaldehyde resin, epoxy resin, chloroprene rubber, poly (meth) acryl lats, polyurethane, silicone polymer, and additionally hollow microspheres of silicate or organic polymer with a diameter of 20-500 microns in the following ratio of components , weight:
Polymer 100
Hardener 2-100
Hollow microspheres 1-600
In the composition according to the invention, the polymeric compounds or the hardener are encapsulated, i.e. surrounded by a protective sheath, the hollow microspheres are
by means of swelling of the protective sheath, since angular and / or sharp parts form as a result of mechanical forces on the composition, as well as fillers.
Intermediate free cavities formed after the destruction of hollow microspheres can contribute to the improvement of reactivity to achieve a high distribution coefficient of reactive and auxiliary substances, since they create internal free flow areas, i.e. uniformity and thoroughness of the masses are achieved. It is possible to equalize the pressure stresses of the expansion force.
Hollow microspheres can be obtained from inorganic and organic substances. They have a hollow spherical shape and their degradation products should produce, in particular, angular and / or sharp particles, chips, and so on.
Inorganic hollow microspheres can be obtained from glass, ceramics, expanded and / or expanded mineral fillers, such as perlite, silicate, calcium silicate, and organic - from synthetic materials, such as thermosetting plastic, such as aminoplasts and phenoplasts.
The grain sizes of the hollow micro-bodies can vary over a wide range and their diameters are preferably 1,500 microns. In addition, they have low bulk and specific weights, preferably 1.0 g / cm, in particular 0.7 g / cm, lower than the specific gravity of the masses in which they are contained. Mixtures of hollow microspheres of different diameters may also be contained. The amounts of hollow micro-bodies in masses can also vary within wide limits, in particular from 1 to 600 wt.% In terms of unloaded starting materials. The content of the hollow microspheres depends on the content of the microcapsules, the capacity of the protective agent swelling agent, the degree of filling, and the like. However, one-component masses containing microencapsulated substances should contain at least 10-100, preferably from 30 to 70 wt.%, In terms of unloaded basic substances (polymeric compounds).
As hardeners, reaction initiators for individual vulcanization, polymerization, polycondensation, and / or polyaddition systems can be used — well-known reactive compounds that can initiate reactions. Along with coreactants, hardeners, such as polyamides, polyamidoamines, known compounds that form peroxides, hydroxides, peracids, their derivatives and salts; oxidizing agents, for example lead dioxide, manganese dioxide; isocyanates and their derivatives, mercaptans and mercapto compounds.
The composition may contain solvents that are used due to swelling and / or softening of physically curable systems for reactivating dry films. Reaction accelerators for validating components, such as compounds that easily donate electrons and thus perform such tasks as accelerated peroxide decomposition, include heavy metal salts, amines, amides, imines, imides, mercapts, azo compounds, and t .P.
The composition may also contain preservatives that impart hydrophobicity, retarders and / or accelerators for curing setting masses,
Not regulated under normal conditions, the reaction processes of highly reactive substances, for example, in connection with too short storage and processing time, using the proposed composition are manageable, and substances can be applied by temporarily activating protective shells.
In this way, one-component systems are obtained which are reactivated and cured at.
Reactivated one-component masses containing microencapsulated reactive substances remain inactive during their preparation and / or storage. The choice of reactive substances, which should be temporarily disinfected by means of protective shells so that they can be added to other reagents, depends on the encapsulation technology, on the type of application and economy. Such reactive substances are present in protective shells, which are contained in insignificant amounts in the system. In the encapsulated form it is better to use a hardener.
The composition may contain auxiliary additives: oils, resins, asphalt, bitumens, solvents, dyes, pigments, thixotropics, inorganic and / or organic fillers and fibers, stabilizers. And / or inhibitors.
The hollow micro-bodies, microcapsules and / or fillers used in the masses can be additionally coated with substances forming a sticky bridge, such as silanes, chromium complexes, in order to achieve stronger combinations on the surface. However, to deactivate with respect to chemical sorption processes, they can be coated.
substances, for example, fatty acids, esters of fatty acids. For the preparation of the proposed compositions, mixing aggregates are suitable, which during mixing do not develop too high shear and / or frictional mixtures, they include planetary, drum and screw mixers.
When preparing compositions with high viscosity and / or thixotropy, in particular when there are angular and / or sharp filler particles, special care is required. Microcapsules are pre-moistened and / or added as the first substance. After that, add hollow microspheres. The hollow micro-bodies perform an additional function, the size of their hollow bodies is approximately one or three times the size of the microcapsules, and they perform a protective function in relation to the microcapsules, which is characteristic, in particular, of viscosity and / or dioxotropy additives. preferably in the presence of angular and / or sharp filling particles.
Compositions are stored in cartouches, Hobbocks, etc., for months. Test results show that an activated container of hollow microspheres as a means of swelling the protective shell Hc1 is much higher than the pressure or pressure itself in combination with an angular and / or sharp filler.
In addition, when the content of the prison and / or angular filler can be reduced, the number of hollow micro-bodies.
Example 2. An adhesive composition is obtained in the form of an adhesive for a pin.
Adhesive 1 contains, by weight.h .: unsaturated polyester resin 100; microencapsulated 40% peroxide with a size of 50 μm 10; hollow microspheres from bloated stable. They are used to make adhesives, putty seals and coatings.
Example 1. Get 4 mixtures of colored, toluene-containing microcapsules, PEELH microspheres and quartz sand.
Mixture 1 consists of 100 weight.h. microcapsules, the size of 100 microns, a mixture of 2 - 100 weight.h. microcapsules, the size of the der 100 MK, 10 weight.h.
0 quartz sand, the value of der 100300 microns, a mixture of 3 - out of 100 weight.h. microcapsules, the value of der JOO MK, 10 weight.h. hollow microspheres of swollen silicate, size 1005 300 microns, a mixture of 4 - 100 weight.h. microcapsules, the size of the der 100 MK, 5 weight.h. hollow microspheres, the value of der 100-300 microns, 5 weight.h. quartz sand, the value of der 100-300 microns.
0
5 parts by weight Each of these mixtures is placed between two thick glass plates, which are gradually subjected to increasing pressure over the entire surface. After reaching 5 the test pressure, it is held for 60 seconds unchanged and then removed again.
Table 1 presents the results of rupture or destruction of the capsules,%:
Table 1
addition of silicate, the value of der ZOOmk, 30; magnesium oxide 2; zinc oxide 2; grafted olefin copolymer with 2.1% acrylic acid 8; silica, the value of der 100 microns, 20.
Adhesive II contains, by weight.h .: unsaturated polyester resin 100; microencapsulated 40% peroxide with a value of 50 microns of 10; magnesium oxide 2; zinc oxide 2 grafted copolymer of olefin with 2.1% acrylic acid 8; quartz sand with a size of 300 microns 30; Curvatured earth with a value of 10 μm, 20.
Adhesive III contains, by weight.h .: unsaturated polyester resin, 100; microencapsulated 40% peroxide with a value of 50 microns
10) magnesium oxide 2; zinc oxide 2 graft copolymer of olefin with 2.1% acrylic acid B; silica with a size of 10 microns of 50.
The adhesive masses for the pin are placed in the cartridges. After drilling holes in concrete in quality class VZOO
PRI me R 3. Prepare adhesives for pre-coating.
Glue J contains, by weight.h .: methyl methacrylate, microencapsulated with a value of 200 microns 25; resin bonding agent 15; highly dispersed silicic acid 4; benzene peroxide in 40% plasticizer 6; a mixture of solvents gasoline + toluene in a ratio of 1: 1 50.
Glue II is prepared in the same way as glue 1, 10 parts by weight of Hb are added. microspheres.
Example 4: Glue, fast solutions are prepared.
Clay I contains, by weight.h .: styrene containing unsaturated resin 100; microencapsulated peroxide with a particle size of 100 microns, 40% 15; cobalt octoate 2; hollow microspheres with a particle size of 300 microns 40; MDO 1; ZnO 3} highly dispersed silicic acid 1; graft copolymer powder containing 6%
they are washed and filled with an adhesive mass for a pin. After that, the usual steel bolts are manually inserted into the drilled holes, and the main rods - by means of machines.
The results of the experiments are presented in table 2.
Table 2
acrylic acid, 5f quartz peso with a particle size of 0.1-0.3 mm 33.
Example 5. Get sealing mass.
Sealing mass 1 contains, by weight.h .: polysulfide 100 microencapsulated lead dioxide with a rene value of 100-300 microns 5; hollow microspheres with a grain size of 300 microns 30; chlorinated plasticizer 30; highly dispersed silicic acid 5; coating filler (chalk) 45.
Sealing mass II is similar to mass 1, only instead of 30 parts by weight. microspheres are used in 30 parts by weight. silica sand with a particle size of 0.3 microns.
Example 6. Get putty, filling and ramming mass.
: Putty contains, by weight.h .: acrylic polymer (in the form of a solution in afttrilovy monomer) 100; microencapsulated peroxide, 40% 8; microspheres with a particle size of 300 microns 50 G quartz sand with a particle size of 0.5 mm 150; highly dispersed silicic acid 2,
Example 7: Two adhesives and coatings are obtained.
Clay I contains, by weight.h,: epoxy resin encapsulated with an epoxy number of 0.5 with a particle size of 300 microns of 100; polyamidoamine (hardener; carrier) 100; microspheres with a particle size of 300 microns 40; highly dispersed acid 5; coated chalk 50.
Clay II is similar to glue, however 40. weight.h. the microspheres are replaced with the same amount of silica sand with a particle size of 0.3 mm.
Example 8. A wood glue is obtained containing, by weight.h .: 50% PVA dispersion 100; Vanadium acetylacetonate microcapsules (10% solution in glycol-butyl ether) 5; microspheres with a particle size of 100-300 microns 35; light spar 30.
Example 9: Chloroprene based adhesives are prepared.
Glue I contains, by weight.h .: polychloroprene glue 100; toluene microcapsules with a particle size of 100 microns 25; hollow microspheres 25.
Clay II contains, by weight.h .: polychloroprene glue 100; microcapsules from toluene 25.
Example 10. Compositions are obtained for glass-reinforced plastics, containing, by weight, polyester unsaturated resin 100; microencapsulated peroxide 40% with a particle size
40 microns 4; chalk 100; zinc stearite 5; magnesium oxide 1; microspheres with a particle size of 0.1-0.3 mm.40.
Example 11. Preparing a mass for pre-coating of a thread containing, by weight.h .: microencapsulated neopentyl glycol dimethacrylate; der value 200 microns 100; microencapsulated with 50% p-dichlorobenzoyl peroxide, nucleus 100 µm 5; hollow micro-objects of silicate with a diameter of 300 microns 50; water 50.
This aqueous suspension is coated with a thread of 10 screws.
After the water has evaporated, the precoated screws are screwed into the counter piece, for example a nut. When screwing in, hollow micro-objects and microcapsules are destroyed. After 3 a break-off time of 250 cm-kp is set. For comparison, the experiment is repeated without the addition of microorganisms. These precoated screws have a break off time of 80 cm-kp. Microscopic examination establishes that the destruction of the capsules is 50%.
Example 12. An adhesive mass is obtained for the putty of the following composition, parts by weight: unsaturated resin, 70% in ethyl methacrylate, viscosity
10.000 cp 100; microencapsulated benzoyl peroxide, 40%, grain size 2000 microns 4; hollow micro-objects of silicate with a diameter of 200 microns 100.
The mass is applied to the aluminum strip and sealed with a 6 cm plane. Thereafter, at a pressure of 20 kp / cm, force is applied to the joined metal strip, whereby they are activated. After 24 h, a tensile strength is established for stretching and shearing of 50 kp / cm.
Example 13. A tamping mass is prepared with the following composition, weight.h .: microencapsulated epoxy resin, degree of epoxy.
5 0.53, with a grain size of 500 100; amine hardener 50; H is equivalent to 0.3; an accelerator, for example 2,4,5-tris- {N, N-dimethyl-aminomethyl) -phenol, 4; hollow micro-objects of swollen silicate, grain size 300 micron 600.
0
The tamping mass is rammed into the perforated hole in the concrete, the microencapsulated resin is destroyed and thus hardened (step polymerization).
five
Example 14. A putty mass is obtained in a planetary mixer at a speed of 15 rpm of the following composition, parts by weight: an unsaturated, highly active resin with a content;
0 styrene 35%, acid number 25, viscosity 800 cP / 20s, 100; 2,4-dichlorobenzoyl peroxide, 50% in a solvent, microencapsulated, grain size 250 micron 3; pyrogenic cream5 acid 4; hollow micro-objects of swollen silicate; grain size 75 microns; specific gravity 0.175 g / cm 1; heavy spar (BaSO) S; titanium dioxide 5; Talc 100.
0
The mass is applied to the defatted metal sheet with a metal spatula. It is activated by pressure, and after 30 minutes it solidifies and can be sanded with sanding paper. To compare the
5 crush the mass, but without the addition of hollow micro-bodies. After 90 minutes, it remains soft.
Additions of hollow microspheres in the adhesive substance I compared with adhesive substance III (example 2) form a larger activatable capacity than the means of swelling the protective sheath, and thus, due to the improved mixing, they increase the first
5 speed of hardening and give rise. shanenye exits.
The binder contained in adhesives I and II is used as a carrier and binder for fixing the microcapsules on the surface (Example 3). 10 bolts (M10) are coated with these adhesives in such a way that after drying the screws remain 50% full. After that, the nuts are fitted and attracted with a preload of 3 micron tension. In the case of screwing onto the bolts previously coated with adhesive substance I, the layer of the latter is partially removed, while bolts coated with adhesive II have a layer with equalizing and sealing properties in the screws. Break-off moments after 3 hours of bolts with glue I: 200 cm-1sp variation coefficient 40%, bolt with glue II: 310 cm-kp, variation coefficient nt 18%. In example 4, concrete stones are used as test bodies, placed in a low-temperature refrigerating chamber at -21 ° C for a day and then applied to adhesive surfaces. Adhesives 1 and II. Make four samples. Concrete stones are pressed into the vessel with adhesives and the samples are again placed in a refrigerator at -21 ° C. After 4 hours, glue I cures, fracture resulting from the breaking load occurs outside the glue line. Adhesive II, after two days, is partially rented. Experimental samples can be separated by hand (in the glue line). In Example 5, sealing masses are placed between two flange surfaces that are screwed together. After one day, the sealing mass is fully vulcanized, while sealing mass II remains plastic and. In Example 6, the mass is used to putty a concrete surface. After 8 hours, the mass is fully vulcanized, the surfaces are sanding. The drilling hole is also filled with a mass, and it is filled with a steel chisel. The mass is vulcanized after 4 hours. In Example 7, the compositions are used to glue concrete. The glue is worn with a spatula followed by pressing. The composition is also used to form a coating on the surface of an artificial stone. In case of pasting of concrete / concrete with glue I, a monolithic joint is obtained in a day. Fracture occurs outside the glue line. Clay II cures only after 6 days, with the fracture occurring in the area of the glue line. Composition I after a day gives a homogeneous coating, while as composition. II sticky. In Example 8, wood glue is used to seal the pins of beechwood. After storage for 8 days, the glued samples are kept for 4 weeks in cold water. Without the use of microencapsulated vanadium acetylacetonate, after 2 weeks, the glue line is torn off. In example 9, rubber profiles are coated with adhesives. After removal of the solvent, the profiles are stored for 2 weeks. Profiles with reactivated layers of glue are then laid on the surface of the beechwood and knock hard with a hammer. The profiles covered with glue I after 10 minutes are connected with the beech tree, while with glue II there appear only separate points of adhesion. - In example 10, the composition is compressed at a pressure of 4 kp / cm. The composition with the hollow microspheres is cured after 5 minutes, and without the hollow microspheres remains sticky and soft. Table 3 presents the raw materials and composition of the proposed composition. The table introduces the basics of the means of swelling of protective shells (hollow micro-bodies): No. 1 - boron silicates, grain diameter 20-70 microns; 2 magnesium / calcium silicates, grain diameter 70-300 microns; No. 3 - aluminum corundum, grain diameter 250-1000 microns; 4 - epoxy resin, grain diameter 60200 microns; No. 5 - phenolic resins, grain diameter 5-15.0 microns; No. 6 polyester resin, grain diameter 20-50 microns; No. 7 - boron silicates, coated, for example, with silane, fatty acid ester, etc., grain diameter 20-50 microns.
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& As As follows from the examples given in Table 3, the proposed composition can be used to obtain coatings, adhesives, and putties, while ensuring the high physicomechanical characteristics of the materials obtained. The composition is stable, has a reduced cure time. The invention has a polymer composition comprising a polymer and a hardener, and one of the components is encapsulated because, in order to decrease the curing time and increase its viability, it contains as the polymer a compound selected from the group consisting of an unsaturated polyester resin, polyvinyl acetate , polysulfide, urea-formaldehyde resin, epoxy resin, chloroprene rubber, poly (meth) acrylate, polyurethane and silicone polymer, and additionally, micro-spheres from silicate or org polymer-ethnic 20500 microns in diameter at the following component ratio in parts by weight .; Polymer 100 Hardener 2-100 Hollow micro. Spheres 1-600 Sources of information taken into account during the examination 1. German patent number 2200163, cl. C.04 To 13/14, published 1974. 2. The patent of France 2064220, cl. C 09 J 3/00, published 1971 (prototype).

权利要求:
Claims (1)
[1]
Claims
A polymer composition comprising a polymer and a hardener, wherein one of the components is encapsulated> o-t, characterized in that, in order to reduce cure time and 15 increase viability, it contains as a polymer a compound selected from the group including • unsaturated polyester resin, component parts, parts by weight:
Polymer Hardener Hollow Microspheres
100 2-100
1-600

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

DE2536319A|DE2536319C3|1975-08-14|1975-08-14|Hardenable composition and method for hardening it|

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