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US993331A - Process for the manufacture of formates. - Google Patents

Process for the manufacture of formates. Download PDF

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US993331A
US993331A US30274406A US1906302744A US993331A US 993331 A US993331 A US 993331A US 30274406 A US30274406 A US 30274406A US 1906302744 A US1906302744 A US 1906302744A US 993331 A US993331 A US 993331A
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formates
lumps
formate
manufacture
caustic alkali
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US30274406A
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Arnold Wiens
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/10Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide

Definitions

  • caustic alkali is, before use, finely pow-' the alkali is used in large pieces (for instance, of a size varying between that of a pea and that of the fist) and withoutadmixture of the alkali with such substances as lime or coal.
  • Figure 1 represents a vertical longitudinal section of an apparatus suitable for carrying out the invention
  • Fig. 2 represents a vertical apparatus.
  • 6 indicates a vessel having a jacket (1 into which a heating means, for instance, superheated steam, may be introduced, as, for example, through an inlet pipe 72. provided with a cutoff valve 71.
  • a heating means for instance, superheated steam
  • the vessel 6 the lumps (Z of caustic alkali are placed.
  • a shaft 0, provided with stirrer arms 6 is rotated to stir the lumps d.
  • the gas is introduced by the pipe f and is led away by the pipe 9.
  • m indicates an inlet pipe provided with a cut-off valve 72., for the admission of any cooling-medium to the jacket a, for the purpose hereinafter described.
  • the caustic alkali in its usual commercial form, should be broken up into fairly large pieces (ranging, for instance, from the size of a pea to the size of the fist), which pieces, without depriving them of their moisture, (amounting to about 4%) are put into the apparatus wherein they are subjected to the action of carbon monoxid under pressure and at an initial temperature of from 100 C. to 120 Q, this being the temperature of the heat ing medium.
  • the pieces are stirred by suitable means, formates are immediately formed while heat is at the same time evolved.
  • I may employ 100 kilograms of caustic soda. Carbon monoxid, at eight atmospheres pressure and at a temperature of about 20 C. may then be supplied, the pressure being maintained until the entire quantity of caustic soda has been converted into formate. After about twothirds of the amount of caustic alkali e1nployed has thus been converted, water is ad- 'mitted into the apparatus through the pipe '0 in quantity not exceeding 2% of the caustic alkali employed. TlllS is done for the purpose of causing the mass which at that time has been reduced to powder, to agglomerate. I The agglomeration or ballin'g together of the particles of formate, due to the admission of the water, withdraws then, in large measure from any of the caustic alkali that has not thus far been con-. i
  • the process for the manufacture of formates which consists in subjecting caustic alkali in lump form to the action of carbon monoxid under pressure at an initial temperature ofabout 100 to 120 C.,,thereby converting the outer surface of said lumps into formate, progressively separating the formate from the outer surfaces of the lumps'by agitation so as to give the carbon monoxid access to the portions within, and, after about two-thirds of the lumps of caustic alkali have been converted into formates agglomerating the formed formates by adding about 2% of water, thereafter subjecting the mass to the further action of the carbon monoxid, and maintaining the tem perature below the decomposition temperature of the formed formate during the progress of the reaction.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

- A. WIENS.
PROCESS FOR THE MANUFACTURE OF FORMATES. APPLICATION FILED 11:12.24, 1906.
Patented May 23, 1911.
ARNOLD WIENS, OF BITTEREELD, GERMANY.
PROCESS FOR THE MANUFACTURE OF FORMATES.
Specification of Letters Patent.
Patented May 23, 1911.
Application filed February 24, 1906. Serial No. 302,744.
To all whom it may concern:
Be it known that I, ARNOLD Wrens, a subject of the German Emperor, residing at I Bitterfeld, in the Empire of Germany, have invented a certain new and useful Process for the Manufacture of Formates, of which the following is a specification.
In the manufacture of formates from caustic alkalies and carbon monoxid, it has hitherto been considered necessary that the caustic alkali should be used in a finely divided condition. In some instances, the
caustic alkali is, before use, finely pow-' the alkali is used in large pieces (for instance, of a size varying between that of a pea and that of the fist) and withoutadmixture of the alkali with such substances as lime or coal.
In the accompanying drawings, Figure 1 represents a vertical longitudinal section of an apparatus suitable for carrying out the invention; Fig. 2 represents a vertical apparatus.
transverse section thereof.
Referring to the drawing, 6 indicates a vessel having a jacket (1 into which a heating means, for instance, superheated steam, may be introduced, as, for example, through an inlet pipe 72. provided with a cutoff valve 71. In the vessel 6, the lumps (Z of caustic alkali are placed. A shaft 0, provided with stirrer arms 6 is rotated to stir the lumps d. The gas is introduced by the pipe f and is led away by the pipe 9.
m indicates an inlet pipe provided with a cut-off valve 72., for the admission of any cooling-medium to the jacket a, for the purpose hereinafter described.
t indicates a charging door for the introducti'on of the lumps of alkali and 'v indicates means for introducing water into the In carrying out the invention, it has been found suflicient that the caustic alkali, in its usual commercial form, should be broken up into fairly large pieces (ranging, for instance, from the size of a pea to the size of the fist), which pieces, without depriving them of their moisture, (amounting to about 4%) are put into the apparatus wherein they are subjected to the action of carbon monoxid under pressure and at an initial temperature of from 100 C. to 120 Q, this being the temperature of the heat ing medium. Experience has shown that when the pieces are stirred by suitable means, formates are immediately formed while heat is at the same time evolved. The'formate formed at the surfaces of the pieces of caustic alkali separates therefrom, with theresult that the gas will constantly act upon particles of alkali free from formates and that the whole amount of caustic alkali will, in a short time, be converted into formate. After the beginning of the reaction, cooling will be effected by circulating through the apparatus, (2'. 6,, through the cooling jacket a) cold water,
cold air, or the like, so that a rise in tem perature above the decomposition point of the formateyi. 0., about 270 (1., is avoided.
In one operation, I may employ 100 kilograms of caustic soda. Carbon monoxid, at eight atmospheres pressure and at a temperature of about 20 C. may then be supplied, the pressure being maintained until the entire quantity of caustic soda has been converted into formate. After about twothirds of the amount of caustic alkali e1nployed has thus been converted, water is ad- 'mitted into the apparatus through the pipe '0 in quantity not exceeding 2% of the caustic alkali employed. TlllS is done for the purpose of causing the mass which at that time has been reduced to powder, to agglomerate. I The agglomeration or ballin'g together of the particles of formate, due to the admission of the water, withdraws then, in large measure from any of the caustic alkali that has not thus far been con-. i
formates, which consists in subjecting the caustic alkali in lump form-to the action of carbon monoxid under pressure at an lnltial temperature of about 100 to 120 0., thereby converting the outer surface of said lumps into formates and completing the conversion of said lumps into formate by progressively separating the formate mechanically from their outer surfaces so as to give the carbon monoxid access to the poras to separate therefrom the formed formate,
-' the carbon monoxid access to the tions within; substantially-as described.
2. The process for the manufacture of formates, which consists in subjecting the caustic alkali in lump form to the'action of carbon monoxid under pressure at an initial temperature of about 100 to 120 0., thereby converting the outer surface ofsaid lumps into formates, completing the conversion of said lumps into formate by progressively separating the formate mechani-' cally from their outer surfaces so as to give ortions within, and, during the progress the reaction, maintaining'the temperature below the decomposition temperature of the formed formate; substantially as described.
3. The process for the manufacture of formates, which consists in subjecting caustic alkali in lump form to the action of carbon monoxid under pressure at an initial temperature of about. 100 to 120 C. thereby converting the outer surface of said lumps into for-mate, agitating the lumps so by converting the outer surface of said lumps into formate, progressively separating the formate from the outer surfaces of the lumps by agitation so as to glve the carbon monoxid access to the portions within, and, after about two-thirds of the lumps of caustic alkali have been converted into formates, agglomerating the formed formates by adding about 2% of water, and thereafter'subjecting the mass to the further action of'the carbon monoxid; substantially as described. v
5. The process for the manufacture of formates, which consists in subjecting caustic alkali in lump form to the action of carbon monoxid under pressure at an initial temperature ofabout 100 to 120 C.,,thereby converting the outer surface of said lumps into formate, progressively separating the formate from the outer surfaces of the lumps'by agitation so as to give the carbon monoxid access to the portions within, and, after about two-thirds of the lumps of caustic alkali have been converted into formates agglomerating the formed formates by adding about 2% of water, thereafter subjecting the mass to the further action of the carbon monoxid, and maintaining the tem perature below the decomposition temperature of the formed formate during the progress of the reaction.
In testimony whereof I have hereunto signed my name to this specification in the
US30274406A 1906-02-24 1906-02-24 Process for the manufacture of formates. Expired - Lifetime US993331A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2737446A (en) * 1952-04-24 1956-03-06 Degussa Process for the production of finely divided silica and alkali formates
WO1983002109A1 (en) * 1981-12-07 1983-06-23 Crown Zellerbach Corp Lime slaker

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2737446A (en) * 1952-04-24 1956-03-06 Degussa Process for the production of finely divided silica and alkali formates
WO1983002109A1 (en) * 1981-12-07 1983-06-23 Crown Zellerbach Corp Lime slaker

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