Universal cross linking compound and polymer

Details Universal cross linking compound and polymer Universal cross linking compound and polymer

2000-05-16

2002-09-17

Szekely, Peter (Department: 1714)

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

Processes of preparing a desired or intentional composition...

C524S059000, C524S071000

Reexamination Certificate

active

06451886

ABSTRACT:

REFERENCE TO MICROFICHE APPENDIX
This application is not referenced in any microfiche appendix.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention teaches new and unexpected cross linking of several chemically different types of polymers by combining selected chemical moieties into a mixture which will cross link the chemically different polymer types. This invention further teaches the development of a new type of polymer with or without the cross linking chemical mixture which offers unexpected results. Both or either the new cross linking mixture and or the new polymer may be useful in many different industrial applications. Examples as to modify asphalts or bitumens are shown herein to illustrate utility of the teachings.
2. Prior Art
Previous to the invention disclosed herein, most known prior art centered upon various techniques for modification of asphalt by polymer combinations with no regard for direction of polymer chemistry to encompass all possible aspects of polymer structure. Rather, prior polymer art generally teaches one facet of polymer chemistry and structure as related to polymer usage such as modified asphalt. The art disclosed herein will set forth unexpected results by understanding the effects of combining the various possible polymer chemistry and structure interactions and relationships to polymer modified asphalt. This understanding of the various polymer chemistries and structures will be further augmented and disclosed herein by the unexpected results obtained with the use of a universal cross linking agent. By universal cross linking agent, it is meant that combinations of chemical moieties disclosed herein form mixtures which may be adjusted in ratio or by inclusion or exclusion of any chemical moiety disclosed herein to form a cross linking agent to optimize the effect of a cross link of various polymer chemistries and structures to themselves for industrial applications such as with asphalt or bitumen.
It has long been known in the rubber industry that from vulcanization, elemental sulfur will under go revision upon prolonged heating. It is also known that phenolic resin derivatives and in particular phenol formaldehyde derivatives do not as easily under go revision as sulfur. It is further understood in the art that the presence of Group VII-A elements (the so called Halides) of the Periodic Table of Elements will enhance the resistance of degradation of phenolic resin vulcanization to revision. The Group VII-A Elements may be present as attached to the phenolic ring of a phenol aldehyde or introduced separately in a salt form with Group IV-A Elements of the Periodic Table. Typical of this understanding is the paper entitled “The Vulcanization of Butyl Rubber with Phenol Formaldehyde Derivatives” by P. O. Tawney, J. R. Little and P. Viohl and presented at the Division of Rubber Chemistry meeting of the American Chemical Society on May 14-16, 1958 in Cincinnati, Ohio and is here in incorporated by reference. As will be shown in this disclosure, a direct application of the use of Group IV-A salts of Group VII-A Elements of the Periodic Table of Elements through the salt form will not yield satisfactory results when combined in phenol aldehyde polymer asphalt mixtures. Taught in this disclosure will be the unexpected results of combining metal sulfates and metal chloride (salts with phenol aldehyde resols resins in the presence of polymer asphalt mixtures).
U.K. Patent No. 368,236 issued to Robert Bosch Aktiengesellschaft found they could use phenol aldehyde condensation products catalyzed in the usual way with optional rubber and asphalt. The product is a plastic, not asphaltic in final usage, suitable for acid and electrical resistance applications. This art lacks discussing mix temperature parameters or processing except to state the use of a mixing machine or by rollers.
Russian Patent No. 732340 issued to Main Pipelines Construction teaches that a phenol formaldehyde resin may be used in a primer composition for pipe coatings. The teachings limit the phenol formaldehyde resin to 2.0% to 10.0% by weight in the formula. All materials are dissolved in a hydrocarbon solvent at room temperature or with gentle heating. There is no disclosure for cross linking the phenol formaldehyde resin or that it is of the reactive type.
The Russian Patent No. 761527 issued to Polymer Construction Material teaches the use of pentachlorophenol resin in solvent based systems. The teachings of the art limit bitumen to 65.0% to 70.0% in terms of weight percent. It is not stated that the pentachlorophenol is of a reactive form or made reactive for use in cross linking reactions. Pentachlorophenol is normally not reactive and is used to improve aging and or tack. The butyl rubber is described in detail as follows: the molecular weight ranges from 13,000 to 27,000 containing 1.5% to 1.9% vinyl groups, 0.20% to 0.25% secondary amino groups and 0.25% to 0.30% hydroxyl groups. The product of the process is for pipe coatings.
In German Patent No. DE 3630132A issued to J. Haas is taught that cross linking agents may be formed by combining sulfur in plasticizer oil with oxidants, vulcanization auxiliary agents or other combinations. This art also teaches that the sulfur containing vapor may be collected as filter material and reused in the next batch.
The U.S. Pat. No. 3,275,585 issued to Baum et al. and assigned to Mobil Oil Corporation disclosed the aldehyde as the main source of polymeric material and does not teach or disclose the use of any type or rubber or other elastomeric materials. The use level of the aldehyde of from 1 to 25% and preferably 5 to 15% based upon the weight of the asphalt. A strong mineral acid catalyst, hydrochloric or toluene sulfonic acid for example, is at the 0.1% to 5.0% and preferably 0.1 to 2.0% use level based upon the weight of the asphalt. There is no discussion of reactions of, with or by cross linked carboxylic acid terminated vinyl aromatic/conjugated diene polymers with a universal cross linking compound suitable for cross linking various polymer types.
In U.S. Pat. No. 3,547,805, inventor Montgomery teaches the use of alkali metals to polymerizing in situ conjugated dienes and vinyl substituted aromatic compounds. The preferred alkali metal is sodium. The preferred diene is 1,3-butadiene. The preferred vinyl substituted aromatic compound is styrene. Characteristics of the process are changes or increases in ring and ball softening point and higher penetration ratio. The penetration ratio is defined in column 3, line 1 through line 3 as the ratio of the penetration at 39.2° F. (4° C.) to the penetration at times 100 as determined by ASTM Test Method D5-61.
Prior art by Krivohlavek, U.S. Pat. No.5,256,710 teaches that carboxylated styrene butadiene and similar types of rubber polymers without carboxylation in use with one and two step phenolic curing resins with or with out the presence of sulfur or sulfur donors or accelerators activated by or catalyzed by heat or amines (Hexamethylene tetraamines as a specific example) may be used to modify or cross link polymer modified asphalt. This work did not address further polymer chemistry or the use of metal chlorides or sulfates. Klutz in U.S. Pat. No. 5,278,207 and U.S. Pat. No. 5,322,867 teaches the use of various poly amine compounds to crosslink carboxylic acids grafted to pre formed styrene butadiene block copolymers to be used in asphalt modification. In the art disclosed by Klutz, various acrylic acid or methacrylate or melaic moieties are used as a source for grafting a carboxylic acid or anhydride to the polymer backbone. Gorbathy, U.S. Pat. Nos. 5,288,773 and 5,336,805 and 5,348,994 disclose the potential for sulfonation of styrene butadiene block copolymers and subsequent cross linking by amines or metallic compounds in the presence of asphalt.
Gorbathy also taught in U.S. Pat. No. 5,336,705 the utility of acrylic acid terpolymers with sulfonated rubber such as EPDM and styrene butadiene in the presence of oxidized asphalt and neutralized (or cross linked) by c

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