Sodium Hydroxide → Accelerator DM

HRID 1979783Notes

Reaction equation

HRID 1979783 reaction equation
[OH-].[Na+].ClCl.[SH:5][C:6]1[S:7][C:8]2[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=2[N:10]=1.[Na]>>[CH:12]1[CH:13]=[CH:14][C:8]2[S:7][C:6]([S:5][S:5][C:6]3[S:7][C:8]4[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=4[N:10]=3)=[N:10][C:9]=2[CH:11]=1

Participants

4

Reactant 3

HCID 14798Sodium Hydroxide2×HCID 24526Chlorine2×HCID 178527777HCID 178527777, compound2×

Product 1

HCID 8447Accelerator DMYield 99.4%

Procedure

A 55 gal. reactor was filled with 40 gallons sodium mercaptobenzothiazole (9.69 g./100 ml.). The agitator was set at 335 RPM and a Beckman pH combination probe and a Beckman redox combination probe were immersed in the solution. Sodium hydroxide solution, 1.95N, was pumped in at 0.26 gal./min. and vaporized chlorine fed in until the pH was 8.9 and the redox potential was +90 mv. Sodium mercaptobenzothiazole solution (0.69 g./100 ml.) was then pumped in at 25° C. at a rate of 47.5 gal./min. The sodium hydroxide solution and chlorine flow were controlled to maintain the pH between 8.9 and 9.4 and the redox potential between +90 mv. and 150 mv. A slurry of benzothiazyl disulfide at 49° C. was continuously withdrawn at the overflow. After a steady state condition was obtained, benzothiazyl disulfide was produced at a yield of 99.4% having a purity of 96%.

Workup

  1. temperatureto maintain the pH between 8.9 and 9.4
  2. customA slurry of benzothiazyl disulfide at 49° C. was continuously withdrawn at the overflow
  3. customAfter a steady state condition was obtained

Sources & evidence

ORD record
ord-0f84c835103d46e48a0078596c83d436
Source dataset
uspto-grants-1984_11
Patent number
US04482720

Reaction notes

Loading…