Improvements in the Manufacture of Hypophosphites.
Year: 1889

page_text: Date of Application, 18th Dec., 1889
Complete Specification Left, 5th Sept., 1890-Accepted, 1st Nov., 1890
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Hypophosphites.
I, JAMES ALFRED KENDALL, of 19 Ellison Road, Streatham Common, in the
County of Surrey, Chemist, do hereby declare the nature of this invention to be as
follows:-
The manufacture of hypophosphites has been hitherto carried on by heating
phosphorus with milk of lime or with water and the hydrates or sulphides of the
alkalis or alkaline earths, which gives a product of hypophosphite in solution.
I have found that the operation may be greatly facilitated by mixing the phosphorus
with charcoal before adding it to the milk of lime or other hydrate or sulphide of an
alkali or alkaline earth.
To carry out my process I take charcoal in powder, placed in a suitable vessel with
sufficient water to make it into a cream or thin paste and I then add phosphorus. I
beat till the phosphorus is thoroughly melted, and strongly agitate till the phosphorus
and charcoal are thoroughly mixed. I then cool the mixture, continuing the agitation
at the same time.
Milk of lime or other solution or mixture having been prepared in another vessel
I add the charcoal and phosphorus mixture. The whole is heated till the reaction is
complete. It is convenient to agitate the materials during the reaction.
The product is then filtered and the solution is evaporated in the usual way.
Dated this 18th day of December 1889.
CARPMAEL & Co.,
Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Hypophosphites.
1, JAMES ALFRED KENDALL of 19 Ellison Road, Streatham Common, in the
County of Surrey, Chemist, do hereby declare the nature of this invention and in
what manner the same is to be performed to be particularly described and ascertained
in and by the following statement :-
The manufacture of hypophosphites has been hitherto carried on by heating
phosphorus with milk of lime or with water and the bydrates or sulphides of the
alkalies or alkaline earths, which gives a product of hypophosphites in solution.
I have found that the operation may be greatly facilitated by mixing the phosphorus
with charcoal before adding it to the milk of lime or other hydrate or sulphide of an
alkali or alkaline earth.
To carry out my process I take charcoal in powder placed in a suitable vessel with
sufficient water to make it into a cream or thin paste and I then add phosphorus. I
heat these materials until the phosphorus is thoroughly melted and I then close the
vessel by a cover and strongly agitate the materials until they are thoroughly mixed
into a thin paste, I then cool the mixture, continuing the agitation at the same time.
For effecting the mixing of the materials (aforesaid) I prefer to use revolving
stirrers worked by steam or other motive power.
For every 100 parts of phosphorus thus made into a mixture with charcoal powder
I prefer to use about 10 parts of the latter substance (although a smaller quantity
may be used but less advantageously) and I use about 250 parts of water.
Wood charcoal 1 prefer to use but powdered coke may also be employed.
When utilizing the above described mixture for the production of hypophosphites
I prefer to use hydrate of lime mixed with water and for the quantities of phosphorus etc.
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page_text: mentioned above I take about 160 parts of hydrate of lime and from 1200 to 1700
parts of water or thereabouts.
The lime and water are heated to about 80°-100° C. in a suitable vessel and the
phosphorus, mixture is added thereto. The heating of the lime mixture is continued
until the phosphorus is dissolved. The vessel in which this operation is carried on is
provided with a suitable pipe through which the gases which are evolved in the
reaction may be conveyed away.
The hypophosphite of lime resulting from the above described operations is obtained
by filtering the liquid mixture and evaporating the filtered liquor. By this means
crystallized hyrophosphite of lime is obtained.
When it is desired to make hypophosphite of baryta the process is carried out just
in the same way as that already described except that 277 parts of hydrate of baryta
is substituted for the 160 parts of hydrate of lime.
For the commercial manufacture of hypophosphites the use of hydrate of lime is
much preferable to the use of alkalies or alkaline or earthy sulphides.
Having now particularly described and ascertained the nature of my said invon-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. In the manufacture of hypophosphites, intimately mixing phosphorus with
charcoal or like carbonaceous matter substantially as described and then heating the
same with the hydrato of lime together with water.
2. In the manufacture of hypophosphites the preparation and use of an intimate
mixture of phosphorus and charcoal or like carbonaceous matter substantially as
described.
Tad this th law of Santambay 1900