Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – At least one aryl ring which is part of a fused or bridged...
Reexamination Certificate
2002-06-28
2003-10-28
Toomer, Cephia A. (Department: 1714)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
At least one aryl ring which is part of a fused or bridged...
C524S612000, C524S590000, C524S494000, C524S186000
Reexamination Certificate
active
06639010
ABSTRACT:
A method for the manufacture of elastic, thixotropic organo-mineral systems, the products obtained therewith and their application.
In the field of mining and particularly for application underground, anchoring and fastening systems play a special part. The present invention therefore concerns a method for the manufacture of an organo-mineral system with which bore holes can be filled and anchors can be agglutinated. The substances according to the invention which may be used for this purpose possess advantageous properties.
Inflammability is of importance, especially for underground applications for anchoring and agglutinating systems. PU systems, polyurethane systems as well as the known polyester resin systems are flammable and during hardening develop a strong smell and gases which may be damaging to health. Epoxy resin systems which are in use at the present time are not sufficient to meet these requirements. The synthetic resins named above do however find application because until now it has not been possible to prepare a rapid setting anchor fastening system for overhead application, which can be injected into an overhead bore hole by means of a two component processing plant, without the material flowing out again. Also, apart from high strength, elasticity is also desirable so that the resin can accommodate possible roof movement.
WO A-94/04588 and/or DE-A-42 28 178 disclose primary and secondary amines as polymerising agents for the manufacture of polyurethane synthetic resins. Furthermore it is known that organo-mineral systems do not burn well and harden to form brittle-hard resins. Such an organo-mineral system, namely a water-glass/isocyanate system is described in EP-A-0 167 002. It is known that only a few materials dissolve in water-glass and/or can be emulsified therein. These are primarily short chained diols and triols. If one now adds to the A component diols and/or triois according to EP-A-0 167 002, then the elasticity of the product is not increased to any measurable extent. On the contrary an heterogeneous product is obtained because the reaction rate between water-glass and isocyanate and diol/triol is variable. A multi phase resin is obtained. If one uses on the isocyanate side a pre-polymer then an elastic resin will form at first but which will however become brittle after a few days.
It is an objective of the present invention to overcome the disadvantages to which the substances tend which are described in the state of the art and to prepare a material which is not flammable, which hardens rapidly, possesses thixotropic properties and can be processed in a machine as a two component system. After hardening, the material should exhibit a residual elasticity, which should be ecologically and toxicologically unobjectionable and if possible should be capable of being manufactured in a cost effective manner.
This objective is achieved by the following invention as it is defined in the claims.
In order to obtain a durable, elastic material, a reactive monomer dissolved or dispersed in water-glass is desirable, which is reactive with respect to isocyanate. In order to obtain thixotropic properties it is necessary to increase the rate of reaction to such an extent that if possible a gel-like condition is reached instantaneously, which prevents the reaction mixture from running out of a bore hole in overhead working. Surprisingly, it has now been found that in contrast to the usual polyoles, primary and secondary di and preferably trifunctional poly-oxy-alkylene amine can be dispersed in water-glass without swelling up (gelatinization). If, as is defined in the claims, one reacts this water-glass mixed with poly-oxy-alkylene amine with isocyanate and/or prepolymers then one will obtain homogeneous substances which will gelatinize instantaneously so that within the space of about 2 minutes a pudding like product is obtained into which an anchor can be set. It is assumed that the rates of reaction of the poly-oxy-alkylene amine on the one hand and of the water-glass on the other hand with the poly-isocyanate component are almost the same. The hardening which follows thereupon leads to a high strength elastic inflammable product.
The raw materials which are necessary for the manufacture of the substances according to the invention are described in detail in the following.
The compounds employed in the invention having terminal amino groups in which at least one free hydrogen atom on at least one amino group and at least one alkylene group interrupted by oxygen, nitrogen and/or sulphur atom are present are for example polyoxyalkylene amine or polyalkylene polyamine. These materials in addition to the oxygen and/or sulphur atoms which interrupt the alkylene groups may also contain nitrogen atoms.
The polyoxyalkylene amines which are employed in the invention have at their disposal a polyoxyalkylene chain and one or more terminal amino groups which exhibit at least one free hydrogen atom in the amino group. Polyoxyalkylene amines are preferred selected from compounds having the formula
in which R, signifies CH
3
OCH
2
CH
2
O, R′ signifies hydrogen or an alkyl residue with 1 to 4 carbon atoms, A signifies the residue of a trivalent alcohol, preferably trimethylol propane or glycerine. x′ signifies a number from 2 to 70, b signifies a number from 5 to 160, the sum of the numbers a+c represents a value of from 2 to 4, n represents a value of from 4 to 80, x, y or z represent a value of from 1 to 100 or mixtures thereof.
Formula II compounds are preferred in particular.
The poly-oxy-alkylene amines quoted above are known commercially by the trade name Jeffamine®.
Products which can be used according to formula I are Jeffamine® D-230, D-400, D-2000 or D-4000. Products according to formula II are Jeffamine® T-403, T-3000 and T-5000. Products according to formula III are Jeffamine® ED-600, ED.900, ED-2001, ED-4000 or ED-6000. Products according to formula IV are Jeffamine® DU-700 or DU-3000. Products according to formula V are for example Jeffamine® BuD-2000 and similar. Products according to formula VI are Jeffamine® M-600, M-1000, M-2005 or M-2070.
Secondary poly-oxy-alkylene amines for example are compounds in the Novamine® series.
Molecular weights of from 100 to 10 000 g/Mol are usable, the range from 400 to 6000 is preferred, particularly preferred are 200 to 5000, e.g. about 400 to 1000 or 4000 to 5000 or 1000 to 3000 g/Mol.
For the above and the following compounds with terminal amino groups which are used according to the invention it holds good that for a shorter length of chain and/or a lower molecular weight the catalytic properties are increased and the elasticity is reduced.
Polyoxyalkylenes where at least one amino group exhibiting a free hydrogen atom forms a part of an urea, guanidine, basic hetero cyclus such as Imidazol, Piperidin etc. may also be used. An example for this is the Jeffamine® BuD-2000 mentioned above.
Accordingly by the expression compounds having terminal amino groups all those compounds are to be understood in which at least one group containing nitrogen is linked to the end of the molecule in which at least one reactive i.e. free hydrogen atom is linked to a nitrogen atom.
Examples for polyalkylene amines are compounds having the formula
H
2
N—(R—NH)
n
—NH
2
in which R signifies an alkylene residue having 2 to 5 carbon atoms and n signifies a number of 1 to 50 or having the formula
A[(NH—R)
n
—NH
2
]
m
in which R and n have the above meanings, A signifies a hydrocarbon residue and m signifies a number of 3 to 20. Diethylene triamine, triethylene tetramine and tetraethylene pentamine are preferred. Diethylene triamine is particularly preferred.
The alkali silicate solutions which are commonly used in this sector of the trade can be employed for the manufacture of the organo-mineral system according to the invention Aqueous solutions of sodium and potassium water-glasses may be used from 28 to 60° B, having a Mol ratio of Na
2
O to SiO
2
or K
2
O to SiO
2
of 1:4 and a dry solids content of 35 to 60 wt
Minova International Limited
Nixon & Vanderhye P.C.
Toomer Cephia A.
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