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Crystallizer

Crystallization
• Crystallization is an important operation in the chemical
industry as a method of purification and as a method of
providing crystalline materials in the desired size range

• A process where solid particles are formed from a


homogeneous phase.

• It is a solid-liquid separation process

• For control
1) Yield of crystal’s
2) Purity of crystal’s
3) Sizes and shapes of crystal’s
Theory of crystallization :
1) Super saturation of the solution
a) It can be done by three ways.
b) Heating the solution
c) Cooling the solution Salting out
2) Nucleation
This takes place in several steps.
During their random motion, the atoms/ molecules/ ions will come
closer to one another and forms aggregates called as CLUSTERS.
These clusters will combine to form an EMBRYO. In this stage only the
lattice formation begins.
This embryo’s combine to form NUCLEI. From nuclei crystals are
formed

3) Crystal Growth
Once the crystals are formed, nuclei formation stops and crystal
growth begins.
Crystallization
The crystallization process consists of two major events:

Nucleation
Is the step where the solute molecules dispersed in the solvent start
together into clusters

The crystal growth


Is the subsequent growth of the nuclei that succeed in achieving the
critical cluster size
Crystallizer Design
Procedure
Crystallizer Design Procedure
The Following Step are outline for the Design of Crystallizer:
1) Choose the type of crystallizer that must meet the
requirement for
a) Product Size
b) Product Quality
c) Process economics
2) Make a list of temp and physical properties required for
calculation.
3) Make a Material balance, Heat balance and Flow sheet.
4) Decide what retention time is required to make the required
product.
a) By experience
b) From growth and nucleation rate
Reference:
Handbook of Industrial Crystallization
Cont.…
5. Size the body on the basis of controlling volume for crystal
retention with due consideration for minimum cross-section
required for vapor release.
6. Size the heat transfer surface.
7. Size the Vapor Pipe.
8. Select the Circulate pump.
9. Select the Agitator.

Reference:
Handbook of Industrial Crystallization
By Allan Myerson
Crystallizer Designing
Parameters
1) Retention time
2) Minimum Active Volume
3) Sizing
4) Height of Cylinder
5) Height of Cone
Equipment Sizing:
Calculation Flow Diagram

Retention time
𝐿50
𝜏=
3.67𝐺
Equipment Sizing:
Calculation Flow Diagram

Retention time
Minimum Active Volume
𝐿50
𝜏= 𝑉𝑅 = 𝜏𝑉14
3.67𝐺
Equipment Sizing:
Calculation Flow Diagram

Retention time
Minimum Active Volume
𝐿50
𝜏= 𝑉𝑅 = 𝜏𝑉14
3.67𝐺

Sizing
𝑉𝑅 = 𝑉𝑐𝑜𝑛𝑒 + 𝑉𝑐𝑦𝑙𝑖𝑛𝑑𝑒𝑟

𝜋 2
𝑉𝑅 = 0.1868𝐷3 + 𝐷 (1.5𝐷)
4
Equipment Sizing:
Calculation Flow Diagram

Retention time
Minimum Active Volume
𝐿50
𝜏= 𝑉𝑅 = 𝜏𝑉14
3.67𝐺

Height of Cone
𝐷 0.1𝐷
ℎ = tan 550 ( − )
2 2 Sizing
𝑉𝑅 = 𝑉𝑐𝑜𝑛𝑒 + 𝑉𝑐𝑦𝑙𝑖𝑛𝑑𝑒𝑟

𝜋 2
𝑉𝑅 = 0.1868𝐷3 + 𝐷 (1.5𝐷)
Height of Cylinder 4
ℎ = 1.5𝐷
Mechanical Engineering Design
The selected material for the crystallizer is (stainless steel
316) due to its high corrosion resistance.

• Shell Thickness
3
𝑡
𝑃𝑐 = 𝐾𝑐 𝐸
𝐷𝑜
• Tori spherical Head Thickness

𝑃𝑒
𝑒 = 4𝑅𝑠
𝐸
Mechanical Engineering Design

• Cone Thickness

3
𝑡𝑐𝑜𝑛𝑒
𝑃𝑐 = 𝐾𝑐 𝐸
𝐷𝐿

• Corrosion Allowance: 2 mm
Mechanical Engineering Design

• Leg Support, Angle Type

𝑊𝑡 𝐻 𝑅
𝑆1𝑡 = 2 [𝑐𝑜𝑠𝛼 −𝐾1 + 6𝐾2 + (−𝐾3 + 6𝐾4 )
𝑡 𝑅 𝑡

𝑊𝑡 𝐻 𝑅
𝑆1𝑐 = [𝑐𝑜𝑠𝛼 −𝐾1 − 6𝐾2 + (−𝐾3 − 6𝐾4
𝑡2 𝑅 𝑡
Mechanical Engineering Design

Figure A.5.4.5.Angle Leg Dimensions


Swirl Breaker
Pipe and Nozzle Sizing

To calculate the diameters of the pipe the following


equation is used.
𝐷𝑖,𝑜𝑝𝑡 = 3.9𝑞0.45 𝜌0.13
Importance of crystallization :
1) Purification of drugs .
2) Improve bio-availability of the drug and choose the most
stable form.
3) A crystalline powder is easily handled ,stable , possesses
good flow properties and an attractive appearance .
Application of crystallization :
1) Purification of drug
2) Better processing characteristics
3) Ease for handling
4) Improved physical stability
5) Sustained release
6) Improved bioavailability
7) Preparation of organic and inorganic API
8) Separation of API from Galenical extracts
9) Manufacturing of pure API by high yield