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February 15, 1965

NATIONAL DISTILLERS & CHEMICAL CORP., Jaward H. Murib, and Charles A. Bonecutter, Plaintiffs,
David L. LADD, Commissioner of Patents, Defendant

The opinion of the court was delivered by: JACKSON

This is an action brought pursuant to U.S.C. § 145 in which the plaintiff, National Distillers and Chemical Corporation, as assignee, and the plaintiffs, Jawad H. Murib and Charles A. Bonecutter, as applicants, of application for patent Serial No. 748,156, filed July 14, 1958, entitled 'Preparation of Boron Compounds', seek by their complaint a judgment from the Court authorizing the defendant, Commission of Patents, to grant plaintiffs a patent containing claims 2, 3, 4, 7 and 8 of the aforementioned application.

The invention relates to a catalytic method for the preparation of boron hydrides, specially haloboron-hydrides and diborane, by the vapor phase reduction of boron trihalides (such as boron trichloride) with hydrogen in the presence of a Group Ib metal (such as copper or silver) which serves as a catalyst. The reaction is carried out at temperatures of from 250 degrees to about 950 degrees C for a period of time which ranges from 0.01 to 2.5 seconds. Hydrogen may be used in large excess, such as 1 to 60 moles per mole of boron trihalide, and the amount of Group Ib metal may vary widely from relatively small catalytic amounts based on the weight of the boron trihalide reactant to large amounts, as when a bed of such metal is used. The reduction reaction results in a product mixture consisting mainly of haloboronhydrides, diborane, boron halide, hydrogen and hydrogen halide. A critical feature of the reaction is that no substantial formation of the corresponding halide of the Group Ib metal occurs.

 '7. A catalytic process for preparation of boron hydrides by direct reaction of a boron trihalide with hydrogen which comprises passing a mixture of a boron trihalide and hydrogen into contact with a catalytic amount of a Group Ib metal at from about 250 to about 950 degrees C for from about 0.01 to about 2.5 seconds to produce boron hydrides by direct reaction of the hydrogen and boron trihalide without substantial formation of the corresponding halide of said Group Ib metal, and continuing passage of such a mixture of boron trihalide and hydrogen into contact with said catalytic amount of Group Ib metal at said conditions of temperature and contact time until the amount of boron hydrides produced greatly exceeds the amount of boron hydride theoretically producible if said catalytic amount of Group Ib metal reacted with boron trihalide to produce the corresponding halide of said Group Ib metal in presence of hydrogen whereby there is produced a reaction mixture comprising essentially haloboronhydrides, diborane, boron halide, hydrogen, and hydrogen halide and containing no Group Ib metal halide.'

 This claim was rejected by the Patent Office on the ground that the differences between the subject matter it contained and that of the prior art would have been obvious at the time the invention was made to a person having ordinary skill in the art to which the subject matter pertains. 35 U.S.C. 103. The prior art relied upon by the Patent Office at trial was a United States patent to Winternitz, No. 2,875,028 (1959); an article by Schlessinger and Burg in the Journal of the American Chemical Society, Vol. 53, pp. 4321-4332 (1931); and an article by Weintraub in Industrial and Engineering and Chemistry, Vol. 3, pp. 299-301 (1911).

 The Winternitz patent discloses a process for the vapor phase preparation of boron hydrides. A mixture of boron trichloride and hydrogen is passed through a reaction chamber where it reacts with finely divided aluminum (or copper) at a temperature between 350 degrees and 700 degrees C for from a few thousandths of a second to several seconds. Aluminum chloride is formed during the reaction, and is collected in a container as the mixture subsequently passes through another chamber.

 The Schlessinger and Burg publication describes passing a mixture of boron trichloride across an arc in order primarily to produce elementary boron at a temperature of 2000 degrees centigrade. The process was described by the testimony of its co-author Dr. Burg as 'essentially a cold process', or one occurring 'at nearly room temperature'. Instead of an electric arc, Schlessinger and Burg apparently employed a 'glow discharge'. Dr. Burg further characterized the temperature of operation as 'far less than what I would call a good red heat'.

 The Weintraub article discloses a method for preparing elemental boron based on the decomposition of boron chloride by hydrogen 'at good red heat'. The heat is provided by 'an arc discharge taking place between two * * * copper electrodes' which occurs 'in an atmosphere of boron chloride and hydrogen'.

 At trial the claims were asserted to be unpatentable on two separate grounds. The first was that they were obvious in view of Winternitz, and the second was that they were obvious in view of Schlessinger et al. combined with Weintraub.

 With respect to Winternitz, the Patent Office seems at first to admit that a stoichiometric reaction is involved. Realizing that plaintiffs' claims, however, seem to contemplate a catalytic reaction, the Patent Office relies upon the occasional use by Winternitz of the word 'promoter' to designate the copper or aluminum. From the usual signification of that word, the Patent Office argues that the metal really is employed as a catalyst, since 'promoters' are customarily thought of as performing a catalytic function. Additionally, the Patent Office contends that since he uses an excess of metal, Winternitz would have remaining a portion of the metal 'unconsumed and reuseable', thus likening the metal to a catalyst, which normally is not consumed in the reaction it initiates.

 With respect to the second ground of rejection, the Patent Office takes the position that Schlessinger, et al. disclose an electric arc process which uses the apparatus of Weintraub; that Weintraub states that he uses a 'good red heat'; that this heat is within the temperature range of applicant's claims; and that Weintraub's use of copper electrodes meets the requirements for the presence in plaintiffs' process of a Group Ib metal.

 In response to the rejection upon Winternitz, the plaintiffs introduced evidence by which they sought to demonstrate that the Winternitz process was not in fact 'catalytic', and that Winternitz indeed produced metal halides as a necessary part of his reaction. The plaintiffs also sought to show that the word 'promoter' was used erroneously by Winternitz in his specification.

 In response to the second ground of rejection, plaintiffs adduced testimony by Dr. Burg, co-author of the Schlessinger-Burg publication, by which plaintiffs sought to establish that the principal purpose of using an electric discharge was not to provide heat, but electrons, and that the reaction was essentially 'electric' in the sense that the energy of the electrons passing through the vapor caused the reaction to occur. Dr. Burg testified further that it would not have been reasonable to assume that the Schlessinger-Burg publication indicated operation at a 'red heat'. Finally, plaintiffs evidence sought to demonstrate that the copper electrodes used to produce the arc did not perform a catalytic function.

 With regard to the rejection based upon Winternitz, the Court must find as a fact that the reaction of Winternitz is not really catalytic. From the disclosure as a whole it is indisputable that the finely divided aluminum participates directly in the reaction and thereby forms aluminum chloride. This is the exact antithesis of the language in the plaintiffs' claim, which specifies ...

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