Wax Processing and

Purification
 Introduction

The word "wax" usually refers to a variety of organic

substances that are solid at ambient temperature but become
free-flowing liquids at slightly higher temperatures.
The chemical composition of waxes is complex, but normal
alkanes are always present in high proportion and molecular
weight profiles tend to be wide.
According to the chemical composition waxes are basically
esters of long chain fatty acids and long chain monohydric or
polyhydric alcohols, each containing 16-34 carbon atoms(C
atoms).
Naturally they are produced by plants and animals
and also found in petroleum.
Their melting point ranges from 35-100 degree
centigrade.
They are soluble in organic solvents and in-soluble in
water.
In general, these are found in nature as a mixture of
esters.
So we can say that :
Waxes are the mixed esters of higher monohydric
or polyhydric alcohols other than glycerol with fatty
acids.
Classification of waxes
Waxes can be classified as Natural and Synthetic

1. Natural Waxes

Animal Waxes
Vegetable waxes
Mineral waxes
 Mineral waxes
Mineral waxes are paraffin waxes which are obtained from petroleum.
For example:
Paraffin wax - made of long-chain alkane hydrocarbons
Microcrystalline wax - with very fine crystalline structure
Petroleum jelly-Petrolatum or petroleum jelly is essentially a mixture
of microcrystalline wax and oil.
Ceresin waxes -wax like the paraffin consists of a group of
hydrocarbons relates to methane with low acid number so that it's
important in rubber compounding.
Mountain wax - extracted from lignite and brown coal
Ozocerite - found in lignite beds
Peat waxes-dark waxy substance extracted from peat using organic
solvents.
 Paraffin wax
Paraffin wax refers to a mixture of alkanes that falls within the 20
n 40 range; they are found in the solid state at room temperature
and begin to enter the liquid phase past approximately 37C.
Paraffin wax is a mixture of saturated aliphatic hydrocarbons (with
the general formula CnH2n+2). Pure paraffin wax is an excellent
electrical insulator, with an electrical resistivity of between 1013 and
1017 ohm meter.
Microcrystalline waxes
Microcrystalline waxes are a type of wax produced by de-oiling
petrolatum, as part of the petroleum refining process. In contrast to
the more familiar paraffin wax which contains mostly unbranched
alkanes, microcrystalline wax contains a higher percentage of
isoparaffinic (branched) hydrocarbons and naphthenic hydrocarbons
 Petrolatum (petroleum jelly )
Petrolatum is usually a soft product containing approximately 20%
oil and melting between 38C (100F) and 60C (140F). Petrolatum
or petroleum jelly is essentially a mixture of microcrystalline wax
and oil.
It is produced as an intermediate product in the refining of
microcrystalline wax or compounded by blending appropriate waxy
products and oils.
Petrolatum colors range from the almost black crude form to the
highly refined yellow and white pharmaceutical grades.
 2. Synthetic Waxes

Synthetic waxes are produced primarily from ethylene. These

materials are less variable than natural products and less inclined to
price fluctuations since supply is not dependent on weather, rain fall
etc. which can affect Carnauba production.

Polyethylene waxes
Polypropylene wax
Tetrafluoroethylen (PTFE)
Ethylene-Acrylic Acid (EAA)
An important operation in the production of lubricating oils is the
dewaxing of the corresponding petroleum fractions and residues,
since it is only possible to manufacture lubricating and industrial
oils with low pour points and with viscosities, suitable for use at
low temperatures, from crudes containing paraffin. The
manufacture of petroleum waxes includes the following
technological processes :
Production of slack waxes and petrolatum's by dewaxing
petroleum products.
De-oiling and fractional crystallization of slack waxes and
petrolatum's.
Purification of crude paraffin waxes.
Blending of paraffin waxes with additives.
 Dewaxing Processes Methods
Dewaxing Crystallizer
1. Large and well-developed crystals can be readily pressed and
filtered.
2. The needle-shaped crystalline types can be easily sweated
3. Microcrystalline paraffin waxes cannot be separated by filter
pressing, but are readily separated by centrifuging.

Dewaxing processes using solvents

In these processes, organic solvents are used as diluents which, at
the temperature of filtering, dissolve paraffin waxes only to a very
slight extent, while they are good for dissolving the other
components of lubricating oils. Rotary filters are mostly used to
separate crystallized paraffin wax.
1. Methyl ethyl ketone dewaxing
2. The propane dewaxing process
3. Dewaxing with a mixture of petroleum jelly,
propylene and acetone
4. Dewaxing with chlorinated hydrocarbons
5. Dilchill dewaxing process
6. Filter aids
 LUBE DEWAXING PROCESSES

Lube feedstocks typically contain increased wax content resulting from

deasphalting and refining processes.
Waxes are normally solid at ambient temperatures and must be removed to
manufacture lube oil products with the necessary low temperature properties.
Catalytic dewaxing and solvent dewaxing (the most prevalent) are processes
currently in use; older technologies include cold settling, pressure filtration, and
centrifuge dewaxing.
 SOLVENT DEWAXING
Solvent dewaxing is used to remove wax from either distillate or residual base stock
at any stage in the refining process. There are several processes in use for solvent
dewaxing, but all have the same general steps, which are:
(1) mixing the feedstock with a solvent,
(2) precipitating the wax from the mixture by chilling,
and
(3) recovering the solvent from the wax and dewaxed oil for recycling by distillation
and steam stripping.
 Usually two solvents are used: toluene, which dissolves the oil and maintains
fluidity at low temperatures, and methyl ethyl ketone (MEK), which dissolves
little wax at low temperatures and acts as a wax precipitating agent.
Other solvents sometimes used include benzene, methyl isobutyl
ketone,propane, petroleum naphtha, ethylene dichloride, methylene chloride,
and sulfur dioxide.
In addition, there is a catalytic process used as an alternate to solvent
dewaxing.
SOLVENT DEWAXING UNIT
 SOLVENT DEWAXING UNIT (SDU)
Good qualities of dewaxing solvent blends:

High solvent power for oil & low solvent power for wax

Low visc. at operating temperature to get low pressure drop & to help in
precipitation /crystallization
Good filterability
Low freezing point & temperature effect of dewaxing
High thermal/chemical stability
Boiling point much lower than that of feed
Low latent heat/specific heat
 De-oiling and fractional crystallization of slack
waxes and petrolatums
Oil and low-melting fractions removed from the slack wax. The
process is called de-oiling.
De-oiling is fractional crystallization of slack or paraffin waxes
by their melting point.
Slack waxes obtained from light distillates by cooling and
pressing were formerly-oiled exclusively by a
process called sweating.
Slack Wax, feedstock, is obtained from the dewaxing of refined
or unrefined vacuum distillate fractions. If the material has been
separated from residual oil fractions it is frequently called
Petrolatum.

The slack waxes are de-oiled by sweating processes to produce

commercial waxes with low oil content. The oil that is
separated from these processes is known as Foot Oil. The
refined petroleum waxes are known as Paraffin Waxes.

Microcrystalline Waxes have higher molecular weight than the

paraffin waxes and consist of substantial amounts of iso and
cycloalkanes.
 PARAFFINE WAX
A waxy crystalline substance that in the pure form is white, odorless and
translucent and has the approximate chemical formula of C20H42 (and above). It
is obtained from petroleum by distillation and is then purified by sweating or
solvent refining. Paraffin, which is not a true wax, consists mainly of a mixture
of saturated straight-chain solid hydrocarbons. Its melting points range from
50C to 57C.

MICROCRYSTALLINE WAX
Microcrystalline waxes consist of odorless, tasteless, non-polar hydrocarbons
with relatively high melting points. Multi wax grades vary in color from white to
yellow, and in such physical properties as hardness and melting point.

VASELINE (PETROLEUM JELLY)

Vaseline is a well-known brand of petrolatum (Petroleum Jelly). Petrolatum is a
flammable, semi-solid mixture of hydrocarbons, having a melting-point usually
ranging from a little below to a few degrees above 37C. It is colorless or of a
pale yellow color, translucent and devoid of taste and smell.
 PROCESS FLOW DESCRIPTION - I
Paraffin Wax & Microcrystalline Wax

The slack wax, as by-product, is obtained in the lube oil process of

the refinery plant. Slack wax is a mixture of oil and wax, which
serves as the wax industry's feedstock and that is further refined and
blended to create value-added petroleum wax products.
 SWEATING PROCESS

The sweating chamber, a steel structure covered with insulation, contains rectangular
trays with cone shape bottom, which are equipped with approx. 50 mesh screen plate in
its lower part and coils for alternate cooling and heating purpose. These trays are
installed inside of the sweating chamber by an arrangement of several vertical lines of
which each has approx. 8 ~10 trays.

In the first step of this process, the fresh water is filled in each tray until the level
reaches slightly over the screen mesh before the feed wax feeds to keep 10 ~ 20 cm
thick beds and then the cooling water is circulated through the coil. After the feed is
completely crystallized, the filled water is drained off.

The crystallized wax is then sweated while simultaneously draining the liquid
drippings, so called foot oil, from each tray in the sweating chamber. The later fractions
of foot oil is recycled through sweating process.
When the congealing point of the liquid drippings indicates that
melting temperature of desired wax product has been obtained,
sweating and drainage are stopped. Consequently, the remaining
solid bed of wax in the sweating chamber is rapidly melted by
heater and then flows to semi-finished product tanks.
To produce refined wax from a product wax requires that the
wax should be treated with activated clay for color and odor
removal is filtered in filter press or rotary drum filter. In order to
obtain the low oil content required in final wax products,
sometimes two or three repeated treatments are required.
Process Flow Diagram (Wax-Sweating Process)
 PROCESS FLOW DESCRIPTION - II
Vaseline (Petroleum Jelly)

In the process, either petrolatum and lube base oil from oil refinery or
paraffin and micro wax produced from the sweating process as
described are used as feedstock.
The process, as semi-continuous process, can be divided either by the
blending ratios of the feedstock or treatment methods.

ACID TREATMENT PROCESS

The feedstock from storage tanks are exactly
pre-measured in proportion to each required
fraction and then transferred by metering
pumps to the acid treatment tank where they
are blended and mixed to give certain desired
properties such as melt point and penetration.
After the transfer is completed, the blended is mixed and heated up to 80 5
C by hot water through heating coils equipped within the tank.
In case the blended meets the targeted qualities by sampling check, it proceeds
to the next stage acid treatment. The sulfuric acid (H2SO4) solution with
concentration of approx. 0.5 wt % is gradually injected into the tank with
maintaining the pre-conditioned temperature and blending. In the reaction with
sulfuric acid, most of traces of aromatics, resins and impurities are removed.
As a form of finishing process, the treatment of the molten wax with activated
earth (Clay) to neutralize acidity remaining from earlier sulphuric acid
treatment and/or to improve color and reduce odor and taste of the finished
wax, also to remove traces of possibly harmful compounds (Polycyclic
Aromatic Hydrocarbons). In the next filtration, the finishing product is filtered
in filter press or rotary drum filter.
This earth treatment may be repeated several times until the product meets the
requirement of color and neutralization
Process Flow Diagram (Vaseline-Acid Treatment Process)
APPLICATIONS
 Purification of Waxes
The purity of paraffin waxes is an important aspect in their grading.
The required extent of purity, obviously, depends on the type of the
field of application. Paraffin waxes used for candle manufacture, for
instance, must be white and stable to color changes.
Paraffin waxes applied in food conservation and packaging must be
odorless and free from compounds damaging the human organism,
above all from polycyclic aromatic substances. Similar, but even
more strict specifications are applied for paraffin products to be used
for medical purposes.
Purification processes are based on:
1. Treatment with chemicals
2. Adsorption
3. Hydrogenation.
 By treatment with chemicals

It is a common feature of all chemical purification processes that

to achieve the desired grade, rather vigorous conditions have to
be used.
The agents include potassium hydroxide, sodium hydroxide,
sodium carbonate, ammonia, alkaline solution of magnesia, zinc
oxide.
In this process, among many other intermediate reactions,
oxidation, condensation, polymerization, sulfonation and resin-
forming take place. The final effect of the purification depends
on the composition of the initial product.
 By adsorption processes

The simplest process, essentially purification by adsorption, is by

mixing with bleaching earth.
After a satisfactory contact time, i.e. after equilibrium has been
established, the paraffin wax is separated by filtration and the used
bleaching earth is discarded.
Various types of fullers earth activated carbon, silica gel, bauxites,
betonies, natural or synthetic aluminum silicates are suitable
adsorbents.
 By hydrogenation

The essence of all refining hydrogenation processes can be

summarized as follows :
1. A suitable mixture of the feedstock and hydrogen is heated to
the required reaction temperature.
2. The gas-phase or liquid-phase or gas-liquid phase reaction
mixture enters the reactor packed with catalyst where the desired
reactions and side reactions proceed.
3. The contents of the reactor are cooled, the hydrogen-rich gas
phase is separated in a high-pressure separator, hydrogen sulfide
formed in the reactions is removed and the gas is recycled into the
process.
4. After reduction of pressure, the gases dissolved in the liquid
reaction product are removed by flash distillation
 Blending of paraffin waxes

Paraffin waxes in their various fields of application require many

different specifications. These can only partly be satisfied by a
suitable choice of feedstock and the above-discussed
manufacturing processes, or even by some modifications of these
processes. In order to fully meet the great variety of demands,
and to further increase the assortment of paraffin wax grades,
manufacturers resort to blending.

The two groups used as additives to paraffin waxes are

1. Microcrystalline paraffin waxes
2. Polymers
Application of Waxes
 Colour
Paraffin wax is generally white in color, whereas microcrystalline
wax and petrolatum range from white to almost black. A fully
refined wax should be virtually colorless when examined in the
molten state. Absence of color is of particular importance in wax
used for pharmaceutical purposes or for the manufacture of food
wrappings.
 Applications of waxes

They are many uses in

Pharmaceuticals
Cosmetics
plastics
textiles
foods
Corrugated board
 Suitable Ingredients for

Polishes
Paste types , used for
i. Floors
ii. Furniture
iii. Cars
iv. footwear
Waxes are also used for

candle making
 Coatings for waxed paper or cloth.
Food-grade paraffin wax
Food packing industry is the largest consumer of wax today
Coating of fruit and cheese
For lining of cans and barrels
Manufacturing of anti-corrosives
Due to thermoplastic nature used for molding and making of
replicas
Blends of waxes are used for dentists when making dentures
Used engineers when mass-producing precision casting
Shiny coating used in candy -making although edible
 Coating for many kinds of hard cheese, like Edam cheese
Sealant for jars, cans, and bottle
Solid propellant for hybrid rocket motors
Component of surf wax, used for grip on surfboards in surfing
Component of glide wax, used on skis and snowboards.
Bone wax is used to help mechanically control bleeding from
bone surfaces during surgical procedures
Chewing gum additive
Wax baths for beauty and therapy purposes .
Micro wax: food additive, a glazing agent.