Formaldehyde → HCID 131710685, compound

HRID 597118Notes

Reaction equation

HRID 597118 reaction equation
[CH2:1]([C:10]1[CH:15]=[CH:14][C:13]([OH:16])=CC=1)[CH2:2][CH2:3][CH2:4][CH2:5]CCCC.[CH2:17]=[O:18].[OH-:19].[Na+].S(=O)(=O)(O)O.P(=O)(O)(O)O.[C:31]1([CH3:38])[C:32](C)=[CH:33][CH:34]=[CH:35][CH:36]=1>>[CH2:17]([CH:14]([CH2:13][OH:16])[CH2:15][CH2:10][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:38][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[OH:19])[OH:18]

Participants

7

Reactant 6

HCID 712Formaldehyde3×HCID 1004Phosphoric AcidHCID 1118Sulfuric AcidHCID 17524-NonylphenolHCID 7237O-XyleneHCID 14798Sodium Hydroxide

Product 1

HCID 131710685HCID 131710685, compound

Conditions

Temperature
40 °C

Procedure

220g of p-nonyl phenol, 50 g of aqueous (30%) formaldehyde and 50 g of (90%) paraformaldehyde are dissolved or suspended accompanied by stirring at 40° C and over a period of half an hour 80 g of 33% caustic soda solution are added. The temperature rises to 60° C. This temperature is maintained initially by cooling then later by heating, until the free formaldehyde content drops to 1.8 - 2%, which takes 4-5 hours. 75g of xylene are then added, followed by cooling to 40° C and the pH is adjusted to 8.0 to 7.5 with about 105 g of 60% sulphuric acid. The temperature must be held at 40° C by cooling. Subsequently the pH is adjusted to from 6.4 to 6.6 with 2 to 3 g of 50% phosphoric acid. The solution is left to settle, separated and discarded. The dimethylol nonyl phenol solution, after adding xylene as the entraining agent, is freed of water by circulation distillation as described in Examples 1-4 under reduced pressure and at a tank temperature of 50°- 60° C. Inorganic salts are removed by subsequent filtration. 390 g of the solution are obtained.

Workup

  1. additionare added
  2. customrises to 60° C
  3. temperatureThis temperature is maintained initially
  4. temperatureby cooling
  5. custommust be held at 40° C
  6. temperatureby cooling
  7. waitThe solution is left
  8. customseparated
  9. additionThe dimethylol nonyl phenol solution, after adding xylene as the entraining agent
  10. distillationis freed of water by circulation distillation
  11. customas described in Examples 1-4 under reduced pressure and at a tank temperature of 50°- 60° C
  12. customInorganic salts are removed by subsequent filtration

Sources & evidence

ORD record
ord-8ab4708364504d73a66a157e27cd8d14
Source dataset
uspto-grants-1977_03
Patent number
US04013605

Reaction notes

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