1
Mmh 25,1886.1 THE JOURNAL OF THE SOCIETY OF DYERS AND COLOURISTS. PI ON SOME DERIVATIVES OF PHOSPHINE. COMMUNICATION FROM W. R. RICHARDSON. THIS well-known dyestuff, which is.obtained in small quantities as a by-product in the manufacture of magenta by the arsenic-acid process, occurs in com- merce as an orange powder, easily soluble in water and is used to some extent in the dyeing of silk and cotton. It belon s to the class of the basic colouring matters, and has t e e n shown b Fischer to consist oi the hydrochloride of diamido-pgenylacridine- C H NHZ l6 The phos hine used in these experiments was purified by. hscher's method. The aqueous solution was re'cipitated with caustic soda, the base washed and gied and extracted with benzene. On evapora- ting the latter solution, a molecular compound of chrysaniline and benzene separates out, which, when crystallised again from boiling alcohd, yields pure chr saniline. $hen diazotised-i.e., treated in hydrochloric acid solution with the theoretical uantity of sodium nitrite-chryaaniline yields a 8iazo compound, the platinum double salt of which I have obtained in the form of small yellow needles, almost insoluble in water and alcohol. Two analyses showed that this saltpossesses the composition, C,,Hl,N4C1,. PtCl,, which yields theoretically 27'16%Pt. Found I. 26'99 ; 11. 26'74. The solution of tetrazo henylacridine, when boiled with dilute sulphuric aci:, deposits a flocculent pre- cipitate, which may be purified by crystallising from alcohol, and consists probably of the corresponding phenol (phos-phenol) C DHllN(OH),. When treated with nitric acid, it yields nitro derivatives, the salts of which are yellow dyes. On acting upon the solution of this tetrazo com- pound with solutions of' the phenols and their sul- phonic acids, an interesting series of colouring mat- ters results. Salicylic acid yields an orange, which is s aringlysoluble in water, and dyes wool in a bath acicfulated with sulphuric acid. The dyestuffs pro- duced with the naphthol sulphonic acids are bluish- red, and dye cotton and wool without a mordant, while the shades produced are fast to light and soa I have also fixed these colours on cotton by Ho& da s process, but the shades produced are only dull. &he product obtained froin tetrazo henylacridine and p-na htholsulphonate of soda in t i e usual inan- ner may g e purified by crystallising from water. An analysis showed it to possess the expected composition of phenylacridinetetrazonaphthol-p-sulphonate of soda :- SOaNa I C~,H,LOH 8.70% S. CioH,-OH \ Calculated for ClBHIINH4 b 8Na Found .............................................. 8.03 ,, The last-named colouring matter dyes wool a very blue shade of red. With barium chloride it yields a crystalline precipitate of the barium salt. Acids separate the free acid as a flocculent precipitate, sparingly soluble in water.-Zurich-Tec?hlzical Labo- ratory of the FedeTal Polytechnic. 11.-ALKALIES, ACIDS, AND DRUCtS. The Limits of the Change of Sodaum Carbonate into Sodium Hydrate b means of Lime. G. Lunge and J. Schniid. Berl. ierichte, 1885, 18, 3286. THE soda solutions when working under usual atnio- spheric pressure were heated t,o a boil in bright iron pans, with an excess of lime, for an hour each, the evaporated water being replaced b more. The experi- ments made under pressure were L n e in copper tubes with screw taps. In order to stir, as is necesary, some pebbles were inserted in the tubes, and the furnace, used for heating, was hung up by two stron so that durin the hour's heating it could f ew : : : : tinually moveffrom one side to the other. The follow- ing are the results :- A-EXPERIMENTS UNDER USUAL ATMOSPHERIC PRESSURE. Contents of Solution After Causticiaing 100 parta of Soda before Causticising. (as NaOH). are present. Percentage Na,CO, Expenment I. 11. 2 ..................... 99.4 .................. 99.3 6 ..................... 99.0 .................. 99.2 10 ..................... 97.2 .................. 97.4 12 ..................... 96.8 .................. 96.2 14 ..................... 94.5 .................. 95.4 16 ..................... 93.7 .................. 94.0 20 ..................... 90.7 .................. 91.0 B.-UNDER HIGH PRESSURE (Lea, 148-150' C.). Contents of Solution After Causticising 100 parts of Soda before Causticisin (as NaOH). are present. Percentage Na,C& Experiment I. 11. 10 .................. 97'06 .................. 97'6 12 .................. 96.35 .................. 96.8 14 .................. 95% .................. 96.6 16 .................. 95.4 ................. 94.8 20 .................. 91.66 .................. 91.61 The experiments show that a hi h ressure does not facilitate the change. Very like?y, towever, a more thorough agitation than that usually practised when making on a large scale would beneficially affect the change.-E. H. Manufacture of Chloride of Zinc. Chem. Zeit. 1885, 105, 1905. IN makin chloride of zinc it is usual to use chiefly odd cuttings of sheet zinc, carefully sorted, so as not to con- tain any galvanised iron. These are dissolved in hydro- chloric acid ; it is best to avoid doing so in iron vessels, and to employ stone or even wooden ones. If stone ones are used, iron stirringrods must be avoided, also as the writer is acquainted with two very serious explosions having arisen from sparks produced by an incautioua knock ainst the stone. The vessel must be fitted with a woodg cliimney, by means of which the va ours can escape. If the hydrochloric acid is not too wea\, a solu- tion will be obtained of from 98"to 110' Tw., which is only slightly acid, and can often be used. particularly for -- dyeing straight away. This solution contains also other metals. dhieflv iron. If a pure white chloride of zinc powder is wanGd, the iron and manganese must be removed b neutralising with soda, heating to 40" or 50' C., and abbing chloride of lime in solution. The iron and manganese are then preci itated ; they settle quickly, and the clear solution may ge filtered or decanted off, and evaporated down in enamelled vessels. These should have a ca acity of about 100-200 litres, and be heated direct by &e. Dry down until the thermometer rises to about 240' C. ; add a little chlorate of potash, as the liquor will have become somewhat ye1 bw again, from the or anic matter of the atmosphere, and then add ve carefdly by means of a long tube-funnel, having the e$in the hot solution, some hydrochloric acid (free of iron) in order to hinder

ALKALIES, ACIDS, AND DRUGS

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M m h 25,1886.1 THE JOURNAL OF THE SOCIETY OF DYERS AND COLOURISTS. PI

ON SOME DERIVATIVES OF PHOSPHINE. COMMUNICATION FROM W. R. RICHARDSON.

THIS well-known dyestuff, which is.obtained in small quantities as a by-product in the manufacture of magenta by the arsenic-acid process, occurs in com- merce as a n orange powder, easily soluble in water and is used t o some extent in the dyeing of silk and cotton. It belon s to the class of the basic colouring matters, and has t e e n shown b Fischer to consist oi the hydrochloride of diamido-pgenylacridine-

C H NHZ l 6

The phos hine used in these experiments was purified by. hscher's method. The aqueous solution was re'cipitated with caustic soda, the base washed and g i e d and extracted with benzene. On evapora- ting the latter solution, a molecular compound of chrysaniline and benzene separates out, which, when crystallised again from boiling alcohd, yields pure chr saniline.

$hen diazotised-i.e., treated in hydrochloric acid solution with the theoretical uantity of sodium nitrite-chryaaniline yields a 8iazo compound, the platinum double salt of which I have obtained in the form of small yellow needles, almost insoluble in water and alcohol. Two analyses showed that this saltpossesses the composition, C,,Hl,N4C1,. PtCl,, which yields theoretically 27'16%Pt. Found I. 26'99 ; 11. 26'74.

The solution of tetrazo henylacridine, when boiled with dilute sulphuric aci:, deposits a flocculent pre- cipitate, which may be purified by crystallising from alcohol, and consists probably of the corresponding phenol (phos-phenol) C DHllN(OH),. When treated with nitric acid, it yields nitro derivatives, the salts of which are yellow dyes.

On acting upon the solution of this tetrazo com- pound with solutions of' the phenols and their sul- phonic acids, an interesting series of colouring mat- ters results. Salicylic acid yields an orange, which is s aringlysoluble in water, and dyes wool in a bath acicfulated with sulphuric acid. The dyestuffs pro- duced with the naphthol sulphonic acids are bluish- red, and dye cotton and wool without a mordant, while the shades produced are fast to light and soa I have also fixed these colours on cotton by Ho& da s process, but the shades produced are only dull.

&he product obtained froin tetrazo henylacridine and p-na htholsulphonate of soda in t i e usual inan- ner may g e purified by crystallising from water. An analysis showed it to possess the expected composition of phenylacridinetetrazonaphthol-p-sulphonate of soda :-

SOaNa I

C~,H,LOH 8.70% S.

CioH,-OH \

Calculated for ClBHIINH4

b 8Na Found .............................................. 8.03 ,,

The last-named colouring matter dyes wool a very blue shade of red. With barium chloride it yields a crystalline precipitate of the barium salt. Acids separate the free acid as a flocculent precipitate, sparingly soluble in water.-Zurich-Tec?hlzical Labo- ratory of the FedeTal Polytechnic.

11.-ALKALIES, ACIDS, AND DRUCtS. The Limits of the Change of Sodaum Carbonate into

Sodium Hydrate b means of Lime. G. Lunge and J. Schniid. Berl. ierichte, 1885, 18, 3286.

THE soda solutions when working under usual atnio- spheric pressure were heated t,o a boil in bright iron pans, with an excess of lime, for an hour each, the evaporated water being replaced b more. The experi- ments made under pressure were L n e in copper tubes with screw taps. In order to stir, as is necesary, some pebbles were inserted in the tubes, and the furnace, used for heating, was hung up by two stron so that durin the hour's heating it could few:::: tinually moveffrom one side to the other. The follow- ing are the results :- A-EXPERIMENTS UNDER USUAL ATMOSPHERIC

PRESSURE. Contents of Solution After Causticiaing 100 parta of Soda before Causticising. (as NaOH). are present. Percentage Na,CO, Expenment I. 11.

2 ..................... 99.4 .................. 99.3 6 ..................... 99.0 .................. 99.2

10 ..................... 97.2 .................. 97.4 12 ..................... 96.8 .................. 96.2 14 ..................... 94.5 .................. 95.4 16 ..................... 93.7 .................. 94.0 20 ..................... 90.7 .................. 91.0

B.-UNDER HIGH PRESSURE (Lea, 148-150' C.). Contents of Solution After Causticising 100 parts of Soda before Causticisin (as NaOH). are present. Percentage Na,C& Experiment I. 11.

10 .................. 97'06 .................. 97'6 12 .................. 96.35 .................. 96.8 14 .................. 95% .................. 96.6 16 .................. 95.4 ................. 94.8 20 .................. 91.66 .................. 91.61

The experiments show that a hi h ressure does not facilitate the change. Very like?y, towever, a more thorough agitation than that usually practised when making on a large scale would beneficially affect the change.-E. H.

Manufacture of Chloride of Zinc. Chem. Zeit. 1885, 105, 1905.

IN makin chloride of zinc it is usual to use chiefly odd cuttings of sheet zinc, carefully sorted, so as not to con- tain any galvanised iron. These are dissolved in hydro- chloric acid ; it is best to avoid doing so in iron vessels, and to employ stone or even wooden ones. If stone ones are used, iron stirringrods must be avoided, also as the writer is acquainted with two very serious explosions having arisen from sparks produced by an incautioua knock ainst the stone. The vessel must be fitted with a woodg cliimney, by means of which the va ours can escape. If the hydrochloric acid is not too wea\, a solu- tion will be obtained of from 98"to 110' Tw., which is only slightly acid, and can often be used. particularly for - - dyeing straight away.

This solution contains also other metals. dhieflv iron. If a pure white chloride of zinc powder is wanGd, the iron and manganese must be removed b neutralising with soda, heating to 40" or 50' C., and abbing chloride of lime in solution. The iron and manganese are then preci itated ; they settle quickly, and the clear solution may ge filtered or decanted off, and evaporated down in enamelled vessels. These should have a ca acity of about 100-200 litres, and be heated direct by &e. Dry down until the thermometer rises to about 240' C. ; add a little chlorate of potash, as the liquor will have become somewhat ye1 bw again, from the or anic matter of the atmosphere, and then add ve carefdly by means of a long tube-funnel, having the e$in the hot solution, some hydrochloric acid (free of iron) in order to hinder