US1628279A - Sensitive layer on alpha suitable base and process of making same - Google Patents

Description

Patented May 10, 1927.

UNITED STATES PATENT OFFICE.

MAXIMILIAN PAUL SCHMIDT AND WILI-IELM KRIEGER, OF BIEBRIOH-ON-THE-RHINE,

GERMANY, ASSIGNORS TO KALLE & 60., AKTIENG-ESELLSCHAFT, OF BIEBRICH-ON- THE-RHINE, GERMANY, A CORPORATION OF GERMANY.

SENSITIVE LAYER ON A SUITABLE BASE AND PROCESS OF MAKING SAME.

No Drawing. Application filed .Tune 19, 1925, Serial No. 38,288, and in Germany May 28, 1924.

In U. S. Patent No. 1,444,469 of Gustav Kogel, filed September 12, 1922, a process is described for the production of layers sensitive to light and of great technical value,

particularly for making light copy paper, by means of the so-called diazo-anhydrides. By the application of these layers it is possible to obtain directly positive pictures from positives.

In U. S. Patent No. 1,444,469 it is set out that diazo compounds can be applied on the base simultaneously with the azo-dyestuff components, without impairing there by the effect of the picture to be produced.

Further it has been shown that the coupling of the diazoand azo-components can be effected by means of a gaseous alkali, for instance ammonia, which permits the development of the picture without having to 20 use any liquid.

It has been proposed to use an acid for preventing a premature coupling of the components during their storage. Thus it is possible to apply diazo compounds of dili'er- '25 ent kind together with azo components. If

diazo compounds other than diazo-anhydrides are chosen, it is necessary to add thereto .a considerable quantity of an acid, for instance sulphuric acid, in order to prevent a premature coupling of the components, but this addition impairs considerably the durability of the paper-fibre. Moreover the simplediazo compounds involve the disadvantage that they .are scarcely colored so that it is very difficult -to see when the bleaching is finished.

Now we have found that there can be obtained papers which are equally durable or nearly as durable and capable of being stored as those described in U. S. Patent No. 1,444,-

469 without having to add a considerable quantity of an acid, b using as diazo components compounds W ich may be regarded as diazo anhydrides in a broad sense and which may be presumed to have been produced from diazonium compounds with elimination of water. We prefer to use diazo compounds formed from amino compounds containing at least one other amino group substituted or not.

These diazo compounds possess, like the diazo anhydrides already mentioned, the

necessary stability and they are also more or less colored.

As such diazo components there may be used amino-diazo compounds, for instance the diazo con'ipounds 'lrom p-diamiues andderi-vatives thereof and also aminodiphe nylamines such, for instance as phenyliminoquinonediazide (comp. Hantzsch & Reddelin, Die Diazoverbindungen Berlin 1921, page ft), dialkylamino-oaniline and its sulphonic acid.

For our new process there may also be used the diazo compounds obtained from aminocarbazoles, being also amino compounds, in which one of the amino groups is substituted by carbon atoms standing in a closed nucleus, aminofiuorene, aminodiphenylcueoxide and similar stable diazo bodies, which arealso colored and behave in a like manner.

As described in the above mentioned U. Patent No. 1,444,469 metallic salts may simultaneously be added to the layer sensitive to light, and the new process may be carried out according to any of the various methods described in the previous patent. 1ustead of incorporating the metallic salts into the light-sensitive layer there may also be used the metal compounds of the diazoor azo-components in question or of both components in case they contain salt-forming groups or, when combined with metal salts, form double salts. In this case it is advantageous to develop the picture after exposure to light by means of a gaseous alkali, which latter may be produced according to any known method The development of the picture may however also be effected in an aqueous alkaline bath and then the metal salts added to the alkali bath.

The other amino groups of the amino compounds, from which the diazo compounds are formed, can be substituted or not.

The diazo anhydrides already claimed in U. S. Patent No. 1,444,469 are excluded from what we claim in our present application.

The following examples illustrate our invention:

1. 13.6 parts by weight of o-aminodimethylaniline are diazotized in the usual manner and in this diazo solution, which has a deep yellow color, 8 parts of resorcylic acid and parts of nickel sulfate are dissolved. The solution is made up to one liter and used for being spread on the desired base (paper).

The layers obtained after drying yield, when exposed to light and treated with an alkali, brownish-orange copies.

2. 10 parts by weight of phenyliminoquinonediazidesulfate, 9 parts by weight ot resorcylic acid and parts by weight oi nickel sulfate (NiSQ tFH O) are dissolved in 1000 parts by volume of water and the base is painted over with this solution.

The layers so obtained are exposed to light in the usual manner and by then treat ing them with an alkaline agent, such as gaseous ammonia or sodium carbonate, 1mmediate brown positive copies are produced.

3. 10 parts by weight of 1')-iminoquinonediazidesulfonic acid, which is obtained by diazotizing p-phenylenediaminesulfonic acid, are dissolved in 1000 parts by volume of water together with 20 parts of l-amino- S-oxynaphthalene-3.6-disulfonic acid (H- acid) and the base is painted over with this solution.

The layers so obtained after being exposed to light and subsequently developed with an alkaline agent, for instance gaseous ammonia, yield dark bluish-violet positive copies.

4t. 12 parts by weight of dimethyliminoquinoned.iazidesulfonic acid, which may be obtained by diazotizing p-dimethylaminoaniline sultonic acid, and 20 parts by weight of fi-naphthol-3.6-disulfonic acid are I dissolved in 1000 parts by volume of water and the base is painted over with this solution.

In the same way as described in Example 2, brown positive copies are obtained.

10 parts by weight of phenyliminoquinonediazidesultate, obtained by diazotizing -aminodiphenylamine, are dissolved in .1000 parts by volume of water together with 20 parts by weight of ,8-naphthol-3.6- disultonic acid and applied upon a suitable base for instance paper. The layers so obtained when treated as indicated in EX- amples 3 and l yield dark violet positive copies.-

(5. 9 parts by weight of 3-aminocarbazole are diazotized in the usual manner and in this diazo solution are dissolved: 8 parts by weight of resorcylic acid and 15 parts of nickel sulfate. The resulting solution is made up to one liter and spread on a base. The layers so obtained, after being dried, exposed to light under a positive or negative and developed with an alkali, yield brown copies.

lVe do not claim any diazo compounds described and claimed in U. S. patent of liogel No. 1,44%, l09, tiled Sept. 12, 192

\Ve claim:

1. Process for producing sensitive layers on a suitable base, consisting in covering the base with a diazo compound being formed from amino compounds containing at least one other amino group and an azo dyestutt component.

2. Process for producing sensitive layers on a suitable base, consisting in covering the base with a diazo compound being formed from amino compounds containing at least one other amino group. an azo-dyestutl' component and a metal salt.

3. Process For producing sensitive layers on a suitable base, consisting in covering the base with a diazo compound being formed from amino compounds containing at least one other amino group substituted or not, an alkali and a metal salt.

4-. As new products, sensitive layers on a suitable base, consisting of diazo compounds being formed from amino compounds containing at least one other amino group, and an aZo-dyestuti con'iponent.

5. As new products, sensitive layers on a suitable base, consisting of diazo compounds being formed "from amino compounds ('ol". taining at least one other amino group, and a metal salt.

6. As new products, sensitive layers on a suitable base, consisting of diazo compounds being formed "from amino con'ipounds containing at least one other amino group, and an alkali.

7. As new products, sensitive layers on a suitable base, consisting of diazo compounds being formed from amino compounds containing at least one other amino group, an axe dyestutt' component: and a metal salt.

8. As new products, sensitive layers on a suitable base, consisting of (liazo compounds being formed from amino compounds con taining at least one other amino group, an alkali and a metal salt.

In testimony whereof we hereunto allix our signatures.

Dr. MAXIMILIAN PAUL SCHMIDT. Dr. WlLllELll'l KRIEGER.

DISCLAIMER 1,628,279.Ma:m'milian Paul Schmidt and Wilhelm Krieger, Biebrich-on-the-Rhine, Germany. SENSITIVE LAYER ON A SUITABLE BASE AND PROCESS OF MAKING SAME. Patent dated May 10, 1927. Disclaimer filed February 3, 1940, by the assignee, Kalle ct C0. Alctiengesellschajt.

Hereby disclaims claims 3, 5, 6, and 8 of said Letters Patent,

The comma and Words aminofiuorene, aminodiphenyleneoxide, appearing on page 1, lines 69 and 70 of said Letters Patent, and

From the scope of claims 1, 2, 4, and 7 of said Letters Patent, those diazo compounds being formed from amino compounds containing at least one other amino group which compounds may not be regarded as diazo anliydrides in a broad sense and which compounds may not be presumed to have been produced from diazonium compounds with elimination of water.

[Ojfict'al Gazette February 27, 1940.]