REACTOR FOR PRODUCTION OF ALKOXYLATED RESIN DEMULSIFIER
The production of alkoxylated phenolic resin demulsifiers involves two main steps: the synthesis of
phenolic resin followed by its alkoxylation using alkylene oxides (e.g., ethylene oxide, propylene oxide).
Here’s a detailed process flow:
1. Phenolic Resin Synthesis
This step involves the reaction of phenol with formaldehyde in the presence of a catalyst to form a resol
resin (if an excess of formaldehyde is used under basic conditions). The reaction is an exothermic
reaction resulting in resol resin containing methylol group (-CH2OH) and ether linkages.
Key Process Parameters/Typical reaction conditions:
Reactant;
- Phenol: Source of hydroxyl groups.
- Formaldehyde: Provides methylol groups (-CH₂OH).
Molar Ratio: Phenol:Formaldehyde = 1:1.5 (to form resol resin)
Catalyst: 3% - 5% (w/w) of phenol-formaldehyde
Operating Temperature: 70–80 °C.
Operating Pressure: Atmospheric pressure – 1.5 bar (due to volatile reactants like formaldehyde)
Reaction Time: 2–4 hours.
pH Range: 8 – 10
Agitation speed: 50 – 300 rpm (depend on the viscosity of the reaction mixture)
2. Alkoxylation of Phenolic Resin
The phenolic resol resin is reacted with an alkylene oxide (e.g., ethylene oxide, propylene oxide) to
introduce alkoxy groups. This step determines the hydrophilic-lipophilic balance (HLB) and the resin’s
performance as a demulsifier. It is also an exothermic reaction.
Key Process Parameters/Typical reaction conditions:
Reactant;
- Phenolic Resin: Acts as the alkoxylation substrate.
- Ethylene Oxide: Source of alkoxy group
Molar Ratio: Alkylene oxide:Resin = 2–10:1 (depending on desired properties).
Catalyst: 0.5 - 3% (w/w) of the phenolic resin
Operating Temperature: 100–120 °C.
Operating Pressure: 2–6 bar (to maintain the alkylene oxide in liquid form).
Reaction Time: 2–4 hours.
pH Range: 7.5–9.5
Agitation Speed: 200 – 600 rpm
3. Purification
The crude alkoxylated resin is purified to remove unreacted alkylene oxide, catalyst residues, and by-
products:
• Vacuum Distillation: Removes unreacted alkylene oxides.
• Filtration: Removes solid residues if present.
For these reactions, the choice of the reactor depends on factors like reaction kinetics, scalability, heat
management, and process safety. Also, it employs reactors that can handle highly exothermic reactions,
maintain precise temperature and pressure control, and allow uniform mixing of reactants.
REACTOR COMPONENTS AND SPECIFICATIONS
The production of alkoxylated resin demulsifiers typically uses a PRESSURIZED BATCH REACTOR designed
for handling alkylene oxides and facilitating the alkoxylation process under controlled conditions.
Key Considerations for Reactor Selection:
Reaction Type: phenolic resin synthesis and Alkoxylation are typically exothermic, requiring
reactors with excellent heat management and thermal Stability.
Pressure and Temperature: Reactors with precise pressure and temperature control are essential
for handling alkylene oxides.
Agitation: System should be setup to have an efficient stirring mechanism in order to avoid
localized overheating and uneven reaction of alkylene oxide.
Mixing and heat transfer: Efficient mixing and heat transfer are essential for uniform reaction
conditions and to prevent hotspots. Also prevents side reactions and maintains uniform resin
quality.
Scale of Production: Reactors that suit small-scale setups and research development. Scalable
from lab to industrial scale
Material Compatibility: Use corrosion-resistant materials (e.g., stainless steel, glass-lined) to
withstand the reactants and products.
Safety: The reactor should be designed with safety features, such as pressure relief, temperature
control, and emergency shutdown systems. For alkoxylation, ensure the reactor is designed to
handle flammable and reactive alkylene oxides safely.
Environment protection: ensure the system is design to control emission of formaldehyde.
Essential components and features of the reactor:
1. Temperature control
- Reactor should be equipped with heating and cooling system using an external jacketed
or internal coil system to maintain precise reaction temperature.
- Heating medium: Steam or hot water
- Cooling medium: Chilled water or glycol-water mixture.
2. Pressure capability
- Constructed to withstand pressure ranging from 2 – 6 bar to handle volatile and reactive
alkylene oxide like ethylene or propylene oxide requiring pressurized operations.
- High pressure increases the rate of alkoxylation.
3. Agitation system
- The reactor must have an efficient stirring mechanism to ensure thorough and uniform
mixing of vicious resin and alkylene oxide to prevent localized overheating and uneven
reaction.
- Rushon turbine or impeller (anchor or paddle).
- Agitation speed: 100 – 600 rpm (adjustable based on resin viscosity)
4. Inert gas purge system
- A sealed reactor with inert gas blanketing.
- Nitrogen or argon blanket can be use to prevent oxidation and explosion risk.
5. Reactant Feed Port
- For phenol, formaldehyde, water, and Alkylene oxide.
- Can include a metering system for precise control of formaldehyde and Alkylene oxide
addition
6. Sampling port
- Constructed for in-process monitoring of reaction progress (e.g. Viscosity, hydroxyl
value)
7. Drain ports
- Construct a drain ports resin removal or cleaning purposes.
Safety components and features of the reactor
1. Pressure monitoring
- Install pressure gauge and alarm system to monitor pressure.
- Use a pressure relief valve or rupture disk to release excess pressure safely.
2. Emergency cooling system
- Construct a cooling system to quench the reaction in case of runaway condition.
Auxiliary components
1. Catalyst addition
- The reactor includes port for precise catalyst dosing during the reaction.t
2. Vacuum system
- To remove unreacted alkylene oxides or water from the system post reaction.
3. Condenser or vapor vent system
- Installed reflux condenser to condense and recycle volatile reactants (e.g.
Formaldehydes).
- Or equipped with a scrubber or absorber to capture and neutralize formaldehyde vapor.
- This also minimize loss and environmental emissions.
4. Filtration unit
- Installed to remove solid residues or impurities such as unreacted resin or catalyst by-
product
Material of Construction
Stainless Steel (SS316):
- Common for handling Alkylene oxides, phenol, formaldehyde, and alkaline or acidic
catalysts.
- Resistant to corrosion and high temperatures.
Lining:
- Glass lining or PTFE Flat Gasket
- Preferred for enhanced corrosion resistance.
- Provides smooth surfaces to prevent product sticking or fouling.
Capacity
Lab Scale: 100–1000 ml.
