Kolbe-Schmitt Process

Salicylic Acid Production Plant

Capacity: 40 tons/hour | 13,200 tons/year

Purity: 99.9% Pharmaceutical Grade

Location: Jazan Industrial City, Saudi Arabia

ROI: 62% | Payback: 1.6 years

Material Efficiency

99.5% conversion in CSTR

Energy Optimized

Total duty: 189 MW

Economically Viable

Production cost: $0.98/kg

Safety First

Comprehensive HAZOP analysis

Project Overview

Project Details

UniversityJazan University
DepartmentChemical Engineering
Project TypeSenior Design Project 2025
StudentsMohammed Ahmed Dighriri
Marzoug Mohammed Musa Hazzazi
SupervisorDr. Saleh Matar

Salicylic Acid Applications

Pharmaceutical (60%)
Chemical Industry (30%)
Industrial Resins (10%)

Process Description

The industrial synthesis of salicylic acid primarily follows the Kolbe-Schmitt reaction, which carboxylates sodium phenoxide to produce the final product. The process begins with sodium phenoxide preparation in a CSTR reactor, followed by flash separation, carboxylation in an autoclave reactor, dilution, acidification, and purification steps including centrifugation and drying.

Key Reactions

Reaction 1: Sodium Phenoxide Formation (CSTR)

C₆H₅OH + NaOH → C₆H₅ONa + H₂O

Conditions: 100°C, Atmospheric Pressure
Conversion: 99.5%

Reaction 2: Carboxylation (Autoclave)

C₆H₅ONa + CO₂ → HOC₆H₄COONa

Conditions: 125°C, 4.9 bar
Conversion: 70%

Reaction 3: Acidification

2HOC₆H₄COONa + H₂SO₄ → 2HOC₆H₄COOH + Na₂SO₄

Conditions: 70°C to 20°C
Conversion: 99%

Interactive Process Flow Diagram

Phenol Storage S1 NaOH Storage S2 CSTR R-101 Flash Tank FT-101 Autoclave R-102 CO₂ Compressor Dilution Tank M-101 Acidification R-103 H₂SO₄ Centrifuge FF-101 Dryer DE-101 Sublimation SB-101 Crystallizer C-101 Product 99.9% Pure

Legend

Storage Tank
Reactor
Separator
Equipment

Equipment Design Specifications

CSTR

CSTR (R-101)

Volume: 1.267 m³

Dimensions: Ø1.024 × 1.536 m

Material: Carbon Steel 310

Agitator: Turbine, 196 RPM

Power: 0.362 hp

Flash Tank

Flash Tank (FT-101)

Diameter: 0.819 m

Length: 2.457 m

Material: Stainless Steel 316

Thickness: 5 mm

Pressure: 101.3 kPa

Autoclave

Autoclave (R-102)

Volume: 25 m³ (est.)

Pressure: 4.9 bar

Temperature: 125°C

Material: Stainless Steel 316L

Design: High Pressure

Acidification Tank

Acidification Tank (R-103)

Volume: 2.548 m³

Dimensions: Ø1.293 × 1.9395 m

Material: Stainless Steel 316L

Thickness: 8 mm

Residence Time: 20 min

Centrifuge

Centrifuge (FF-101)

Type: Basket Type

Capacity: 2.1 m³/batch

Separation: 95% water & phenol removal

Material: Stainless Steel

Dryer

Dryer (DE-101)

Type: Vacuum Tray Dryer

Tray Area: 190 m²

Capacity: 1,898 kg/h

Temperature: 20-70°C

Sublimation Tank

Sublimation Tank (SB-101)

Volume: 20 m³

Pressure: 10 kPa (vacuum)

Temperature: 150-200°C

Type: Jacketed Vacuum Vessel

Crystallizer

Crystallizer (C-101)

Volume: 20 m³

Type: Desublimer

Temperature: 25°C

Cooling Load: 330 kW

Material Balance Analysis

Overall Material Balance

Feed Streams

Phenol: 1,809 kg/h

NaOH: 699 kg/h

CO₂: 1,148 kg/h

H₂SO₄: 591 kg/h

Total Feed: 4,247 kg/h

Product Streams

Salicylic Acid: 1,665 kg/h

Byproducts: 856 kg/h Na₂SO₄

Waste Water: 4,642 kg/h

Unreacted CO₂: 600 kg/h

Total Output: 7,763 kg/h

Stream Compositions

Stream Phenol NaOH Sodium Phenolate Water CO₂ Sodium Salicylate H₂SO₄ Salicylic Acid Na₂SO₄ Total (kg/h)
S1 (Phenol Feed) 1,809 - - 3,015 - - - - - 4,824
S2 (NaOH Feed) - 699 - 1,399 - - - - - 2,098
S3 (CSTR Outlet) 1809 84 4,847 47,28 - - - - - 6,924
S5 (Flash Liquid) 164 84 4,847 95 - - - - - 2,282
S8 (Autoclave Outlet) 164 84 606 95 614 4,678 - - - 6,241
S12 (Acidification Outlet) 3,939 84 1,454 44,967 - 468 591 3,960 856 18,746
S17 (Final Product) 158 84 - 54 - 468 - 3,960 856 6,127
S19 (Pure SA) - - - 2 - - - 1,665 - 1,667

Unit-wise Material Balance

ComponentInput (kg/h)Output (kg/h)
Phenol1,809164
NaOH6993.5
Sodium Phenolate-2,020
Water4,4134,728
Total6,9216,916

Energy Balance & Utility Requirements

Total Energy Consumption

Unit-wise Energy Duties

CSTR 18,975 kW
Flash Tank 69,844 kW
Autoclave 13,006 kW
Acidification -35,001 kW
Dryer 4,623 kW
Sublimation 328 kW

Detailed Energy Calculations

CSTR Energy Balance

Q = Q₁ + ΔHRXN + Q₂

Q₁ (Feed Cooling): -2.86 × 10⁶ kJ/h

ΔHRXN: 2.64 × 10⁷ kJ/h

Q₂ (Product Heating): 4.48 × 10⁷ kJ/h

Total Q: 6.83 × 10⁷ kJ/h = 18,975 kW

Flash Tank Duty

Q = nphenol × ΔHvap + nwater × ΔHvap

Q = (2.203 kmol/h × 54,200 kJ/kmol) + (6,177.96 kmol/h × 40,680 kJ/kmol)

Q = 2.51 × 10⁸ kJ/h = 69,844 kW

Economic Analysis

Total Capital Investment

$3,771,926

Fixed Capital: $3,279,936
Working Capital: $491,990

Annual Production Cost

$12,900,000

Variable: $7,045,000
Fixed: $3,704,990

Revenue & Profit

$16,500,000

Gross Profit: $3,600,000
Net Profit: $2,340,000

Key Metrics

62% ROI

Payback: 1.6 years
Prod. Cost: $0.98/kg

Equipment Cost Breakdown

EquipmentCost (USD)% of Total
Dryer189,65026.3%
Centrifuge118,72016.5%
Autoclave95,55013.3%
Acidification Tank74,06010.3%
Storage Tanks68,9409.6%
CSTR59,7708.3%
Dilution Tank30,9104.3%
Distillation Column36,9505.1%
Others69,4406.3%

HAZOP Study & Safety Analysis

HAZOP Guide Words

NO

Negation of design intent

LESS

Quantitative decrease

MORE

Quantitative increase

PART OF

Qualitative decrease

AS WELL AS

Qualitative increase

REVERSE

Logical opposite

OTHER THAN

Complete substitution

Safety Considerations

Process Safety

  • Autoclave designed for 4.9 bar with 1.4 safety factor
  • Phenol storage with nitrogen blanketing and vapor recovery
  • Dust explosion protection in dryer and packaging areas
  • Emergency relief systems on all pressure vessels

Personal Protection

  • Full PPE required in phenol handling areas
  • Eye wash stations within 15 seconds reach
  • Emergency decontamination showers
  • Self-contained breathing apparatus for firefighting

Environmental Controls

  • Phenol wastewater treatment to <0.5 ppm discharge
  • CO₂ recovery system for unreacted gas
  • Sodium sulfate by-product recovery
  • Scrubbers for acid vapor containment

HAZOP Team Structure

HAZOP Leader

Plans sessions, controls discussion, motivates team

Process Engineer

Provides process description and design intentions

Chemist

Provides chemical hazards and reaction details

Plant Engineer

Provides site-specific operational experience

References

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  5. Krik-Othmar, Encyclopedia of Chemical Technology, Third Edition. Volume 1. John wiley and Sons, New York, NY, 1980.
  6. Stanely M. Walas, "Chemical Process Equipment Selection and Design", Butteworth-Heinemann USA, 1988.
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Project Credits

Project Development

Authors:

  • Mohammed Ahmed Dighriri (202003311)
  • Marzoug Mohammed Musa Hazzazi (202003782)

Supervisor: Dr. Saleh Matar

Institution: Jazan University
College of Engineering and Computer Science
Chemical Engineering Department

Project Objective

This senior design project was submitted in partial fulfillment of the requirements for the Bachelor of Science degree in Chemical Engineering (May 2025).

The project demonstrates comprehensive application of chemical engineering principles including:

  • Process design and simulation
  • Equipment sizing and mechanical design
  • Material and energy balance calculations
  • Economic analysis and feasibility studies
  • Safety and hazard analysis (HAZOP)
  • Instrumentation and control systems

Acknowledgments

The authors express gratitude to:

  • Dr. Saleh Matar for supervision and guidance
  • Jazan University for facilities and support
  • Chemical Engineering Department faculty
  • Family and friends for continuous support