8/20/15

LECTURE20:
PHOSPHOROUS
PHOSPHORIC ACID

CHEMICAL TECHNOLOGY (CH-206)

Department of Chemical Engineering

PHOPHOROUS (P)
8/20/15

In 1669, Hennig Brand discovered phosphorous.

In 1680, Robert Boyle was the first to use phosphorus
to ignite sulfur-tipped wooden splints.
It is used in explosives, poisons and nerve agents is
referred as "the Devil's element".
It is a component of DNA, RNA, ATP, and also the
phospholipids that form all cell membranes.
It is not found in its free element form on Earth, due to
its high reactivity.
Phosphorus as a mineral is present in oxidized state,
as inorganic phosphate rocks.
Phosphorous is primarily extracted from calcium
phosphate rocks consider as an expensive mineral..

PHOPHOROUS (P)
Elemental phosphorus exists in two major forms

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White

phosphorus
Red phosphorus,

White phosphorus was first made commercially, for the match

industry in the 19th century, by distilling off phosphorus
vapour from precipitated phosphates, mixed with ground
coal or charcoal, which was heated in an iron pot, in
retort.
precipitated phosphates were made from ground up bones
that had been degreased and treated with strong acids.

The

CO and other flammable gases produced during the reduction

process were burnt off in a flare stack.
This process became obsolete when the submerged arc furnace for
phosphorus production was introduced to reduce phosphate rock.
The production was further increased, electric furnace method.

PHOSPHATE ROCK
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Phosphate rock is a natural mineral found as a geological

deposit in the form of sedimentary rocks containing various
amounts of calcium phosphates.
India alone is estimated to have about 140 million tons of
rock phosphate deposits, most of which are however, of low
grade and with substantial impurities unsuitable for the
production of phosphate fertilizers.
Phosphate rock is used as a phosphatic fertilizer after grinding
called phosphorite or mineral phosphate, or as a primary source
of phosphorus.
The ground rock (60-100mesh size) phosphate can be applied
directly to the acidic soil.
For neutral or alkaline soils acid-treated rock phosphate (like
superphosphate) is used.

Crops

like rubber, tea, coffee, apples and fruit plantations of oranges

are suitable for direct application of rock phosphate.

PHOSPHATE ROCK
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Francolite (calcium carbonate-fluorapatite) of

formula [Ca5(PO4,CO3)3(F,OH)] is the most
predominant mineral of phosphate.
Four kinds of phosphate rocks are recognized, with the
phosphorus content varying from 2 to 21%:

hard

rock phosphate,
soft rock phosphate,
land pebble phosphate and
river pebble phosphate.

Phosphate rock contains phosphorous in an apatite form

which is water insoluble.
The citrate solubility can vary from 5 to 17 % of the
total phosphorus, depending on the chemical nature of
the rock and the size to which it is ground.

PHOSPHATE ROCK
The efficiency of the ground rock phosphate can
be increased by

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Mixing

with soluble phosphorus and fertilizers

Mixing with elemental sulfur or sulfur-producing
compounds
Using phosphate solubilizing micro-organisms

More than 90% of rock phosphate is used for

production of superphosphate and phosphoric
acid.
Less than 8 % is used directly as soil fertilizer
and about 2 % as animal and poultry feed.

PHOSPHATE ROCK:
PURIFICATION
8/20/15

Clays (kaolinite, illite, smectites and attapulgite),

quartz and other silicates (feldspars), carbonates
(calcite and dolomite), secondary phosphates
(phosphates bearing iron and aluminum) and
iron oxides (geothite, hematite and magnetite)
are the common impurities which are associated
with phosphate rock.
The ore is upgraded and the impurities are
removed by Floatation method.
Calcium phosphate is obtained after removal of
various impurities present in phosphate rock.

PHOSPHATE ROCK:
PURIFICATION
8/20/15

Froth floatation is generally employed with

siliceous ores when other less expensive or less
complicated techniques fail to produce phosphate
concentrates suitable for chemical processing.
Prior to its conditioning for floatation, the
floatation feed of phosphate rocks is delimed.

PHOSPHATE ROCK:
PURIFICATION
8/20/15

In the floatation of phosphate ores, apatite particles are

generally directly transferred to the froth fraction (direct
floatation) by using anionic collectors such as fatty acids.
The anionic collectors selectively attach themselves to the
phosphate particles, render them hydrophobic and lift
them to the surface by the froth and air bubbles formed.
The mineral bearing froth may simply overflow the cells
or paddles or may be skimmed off.
Quartz and other silicates are removed from the bottom
of the floatation cells.
A second stage of floatation may be required to remove
silica from the phosphate-rich float by cationic collectors
(usually amines), when silica is floated and the
phosphate particles settle to the underflow.

PHOSPHATE ROCK:
PURIFICATION
8/20/15

A selective floatation of carbonates from

phosphate rock is rather difficult owing to the
similarity in the physicochemical properties of
the carbonate and phosphate minerals.
Several treatments have been proposed,
including floatation, calcination, acid washing,
magnetic separation and heavy media separation
for the removal of free carbonates from the
phosphates.

10

PHOSPHATE ROCK:
PURIFICATION
Process

Main products

By- products

and reagents

and derivatives

Acidulation

Phosphate rock,
Sulfuric acid,
phosphoric acid,
hydrochloric acid
ammonia, potassium
chloride

Superphosphate,
phosphoric acid (wet
process) triple
super phosphate , mono
ammonium phosphate,
diammonium phosphate

Fluorine compounds
vanadium, uranium
(limited)

Electricfurnace
reduction

Phosphate rock,
siliceous flux, coke
(for reduction),
electrical energy,
condensing water

Phosphorus, phosphorus
pentoxide and halides,
phosphoric acid, triple
superphosphate, various
Na,K,NH4,Ca salts;
mono potassium
phosphate

Fluorine
compounds, CO,
slag
(for RR ballast
aggregate, fillers,
ferrophosphorus

Calcium
metaphosphate

Phosphate rock,
phosphorus, air or
oxygen, fuel

Calcium metaphosphate

11
Fluorine compounds

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Raw materials

YELLOW PHOSPHOROUS
Raw materials
Basis:

1 ton Phosphorus
Calcium phosphate
6804 kg
Sand
2018 kg
Coke
1202 kg
Carbon electrode consumption
22.68 kg
Electricity
13000 kWH

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Reaction
2Ca3(PO4)2 + 10C + 6SiO2 CaSiO3 + P4 + 10CO
12

YELLOW PHOSPHOROUS
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11500C
15000C

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YELLOW PHOSPHOROUS
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14

11500C and 1500 0C

YELLOW PHOSPHOROUS

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Rock phosphate is crushed as fine powder.

The powdered rock phosphate is mixed with sand and
coke powder in the required proportion and charged
into electric furnace having electrodes at bottom.
The base of furnace is heated with carbon blocks as the
temperature increases due to electrical heating.
Reaction of rock phosphate with sand starts at about
11500C resulting into calcium silicate and P2O5.

Further increasing the temperature to 15000C carbon

particle reacted with P2O5 there by phosphorous and
CO formed which is collected from top outlet.
15

YELLOW PHOSPHOROUS

The carbon and silicon impurities are removed due to

oxidation.
Pure phosphorous which is pale yellow colour is
washed with water before it is casted into sticks.

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Residual calcium silicate settles down at bottom in

form of slag which is taken out time to time from the
outlet provided at bottom of the furnace.
Product gases which is mixture of phosphorous and
CO is cooled in a water cooler thereby phosphorous
solidify and CO gas is separated.
Purification of phosphorous is carried out by melting
it and treating with chromic acid (mixture of K 2Cr2O7
and H2SO4).

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YELLOW PHOSPHOROUS
RECOVERY OF THE PRODUCTS

SiF4 + 3H2O H2SiO3 + 2H2SiF6

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The fumes emerging from the furnace are first freed

from any mineral and other fine reagents which may
have been carried up at less than 3000C so that the
phosphorous is not condensed out.
The remaining gases consist of phosphorous, CO and
SiF4, are sent to a bottom of tower in which water is
sprayed from two different heights. The temperature
should not go below 600C.
The phosphorous condenses out but does not solidify,
is collected under water which reacts with the SiF 4
gas, converting into metasilicic and fluorosilicic acids.

17

YELLOW PHOSPHOROUS
RECOVERY OF THE PRODUCTS

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The fluorinated components are subsequently recovered

from the solution.
CO which is completely freed from phosphorous and
fluorine compounds is then cooled, dried and
subsequently used as a fuel.
The slags consisting of CaSiO3, which are produced in
the furnace and subsequently discharged from outlet
provided at base of furnace, are good additives for
cements, air-port runway construction and antiskid
conglomerates.
The liquid phosphorous, after decolouration with
activated carbon is filtered and solidify to yellow
phosphorous.
It is stored under water.

18

RED PHOSPHOROUS
Raw material
Yellow

phosphorous

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Batch process
Yellow

phosphorous obtain from earlier process is taken into

iron pot provided with safety outlet and thermometer
jackets.
Conversion of yellow phosphorous to red phosphorous is
exothermic reaction and strict maintenance of temperature
in range 2400C to 2500C is required as conversion do not
take place below 2400C and above 2500C accident chances
are there.
After complete conversion product is washed with NaOH
solution as yellow phosphorous is soluble but red
phosphorous is not soluble in NaOH

19

RED PHOSPHOROUS
Continuous process
In

the process liquid white phosphorous is

maintained at boiling point for 5-6 hrs to achieve 35
to 50% conversion.
The product is taken into screw conveyer in which
unreacted phosphorous vaporizes which is
recrystallize and recycled.
The red phosphorous is of high purity and therefore
doesn't require further purification.

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20

RED PHOSPHOROUS
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Block diagram of manufacturing process

21

Process diagram of manufacturing process

PHOSPHOROUS: PROPERTIES

Appearance
Odour
:
Boiling point
Melting point
Density

:
:

P
30 gm/mole

:
White, red and black solid
Irritating odour
:
280.5 0C
:
44.2 0C
:
2.2 2.34 gm/mL

Solubility
:
Insoluble in water and
soluble in carbon disulfide
White phosphorus is a highly reactive, waxy, white-yellow,
transparent solid with acrid fumes. It emits a weak green glow
(luminescence) in the presence of oxygen. White phosphorus
ignites spontaneously in air.

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Molecular formula
Molecular weight

22

PHOSPHOROUS: APPLICATIONS
Red phosphorus is used in fireworks, smoke bombs and pesticides.
Black phosphorus no significant commercial uses due to least reactivity.
White phosphorus and zinc phosphate are mainly used as a poison for rats.
Used in making incendiary bombs, tracer bullets and for producing smoke
screen
Used in fertilizers.
Used in the manufacture of PCl 3, PCl5, P2O5 and phosphorus bronze.

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Organophosphorus compounds used in detergents, pesticides and nerve agents,

and matches.
Phosphorus is one of the most essential mineral in the body and is ranked
second to calcium.

About

80% of all phosphorus is present in human body in the form of calcium phosphate
in the teeth and bones.
It also participates in several vital functions of the body, such as energy metabolism,
synthesis of DNA and the absorption and utilization of calcium.
Phosphorus plays a role in facilitating optimal digestion.
It helps in the normal functioning of the kidneys and ensures proper discharge of wastes.
Adequate levels in body is essential to maintain normal brain functions
23
Phosphorus helps maintain a good hormonal equilibrium.

PHOSPHORIC ACID
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Phosphoric acid (H3PO4), also known as orthophosphoric

acid, it is a mineral (inorganic) acid.
Orthophosphoric acid molecules can combine with
themselves to form a variety of compounds which are
also referred to as phosphoric acids.
Phosphoric acid is used for specialty application, such as
anticorrosive and food industry.
The continuous process of phosphoric acid production
uses liquid white phosphorous at the boiling condition
for 5 to 6 hrs so that about 3550 % white phosphorous
is converted to red phosphorous.
The hot red phosphorous is taken in a screw conveyer
which along with inert gases gives a solid pure red
phosphorous as product.

24

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
The modern manufacturing methods of
phosphoric acid are following:

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Blast

furnace process
Electric furnace process
Oxidation and hydration of phosphorous
Wet process or strong sulfuric acid leaching

25

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

Raw materials
Basis:

1 ton phosphoric acid (100%)

Phosphate rock
2290kg
Sand (Silica) 6800kg
Coke 3175kg (reducing agent as
well as fuel)
Briquette binder 227kg
Air 450000 ft3

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Reactions
Ca3(PO4)2 + 3SiO2 + 5C 2P + 5CO + 3CaSiO3
2P + 5CO + 5O2 P2O5 + 5CO2
P2O5 + 3H2O 2H3PO4

(85-90% yield)

26

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

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27

Block diagram for manufacturing of Phosphoric acid using blast furnace

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

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28

Process diagram for manufacturing of Phosphoric acid using blast furnace

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

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Phosphate rock is pulverized and mixed with coke powder

and binder is compressed to 5000 psi resulting into the
briquettes.
Briquettes are dried and charged along with sand and
additional coke powder from top of the blast furnace.
The preheated air (1000 1100 0C) is charged from bottom
of the blast furnace via tuyere.

tuyere is cooled copper conical pipe numbering 12 small

furnace and up to 42 large furnace through which hot air is
blown in to the furnace.

Preheated air leads to burning of briquettes giving

temperature rise up to 13700C.
About 760kg of coke is consumed in reduction of phosphate
rock to phosphorous and remaining generates heat by
combustion with air.

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PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

8/20/15

Reaction is completed in the furnace itself producing P 2O5 and

calcium silicates as slag.
The product gases also contain CO and N 2 along with dust
particles.
For purification, it is passed through cyclone separator and
phosphorous condenser.
Thus, P2O5 and elemental phosphorous are separated out.

Hot P2O5 gases are cooled in the heat exchanger.

Superheated steam is produced and a part of gas is taken into

regenerative blast furnace.
As a result the entire phosphorous and P 2O5 is cooled and
purified before taken into hydrating towers.
Purification of phosphoric acid includes removal of arsenic by
hydrogen sulfide treatment followed by filtration.

30

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

Engineering Aspects:

Blast furnace is made of high temperature resistant

refractories brick.
Blast furnace have accessories of hot blast stove for supply
of compressed preheated air having temperature 1000
11000C, briquette press for preparation of briquettes of
Phosphate rock and coke, dust collector (cyclone separator)
for removal of dust particles from product stream.
Also, two outlets for removal of slag and ferrophosphorous
are provided at the bottom of the furnace.
The top of the blast furnace is closed as it operates at high
top pressure.

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31

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
BLAST FURNACE PROCESS

There are two different systems are used for charging of briquettes,
coke and silica.

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One is having double bell system which is often equipped with movable
throat armour and other is bell less top.

32

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

One utilized lintel or support ring at the bottom of the shaft upon
which the higher level of the furnace rests.
The other is free standing construction requiring and independent
support for the blast furnace top and gas system.
The required expansion both thermal as well as pressure for the
installation is below for the lintel i.e. in bosh/belly area in lintel
type furnace, while compensator for expansion in the free
standing furnace is at the top.

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BLAST FURNACE PROCESS

There are two construction techniques to support the blast
furnace.

33

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
ELECTRIC FURNACE PROCESS

Raw materials

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Basis:

1 ton phosphoric acid (100%)

Phosphate rock
2225kg
Sand (silica)
680kg
Coke breeze
400kg
Caron electrode
8kg
Air
100000 ft3
Electricity
4070KWH

Reactions

Ca3(PO4)2 + 3SiO2 + 5C 2P + 5CO + 3CaSiO3 H = 364.8 kcals

2P + 5CO + 5O2 P2O5 + 5CO2
P2O5 + 3H2O 2H3PO4 87-92% yield

H = 44.9 kcals

34

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
ELECTRIC FURNACE PROCESS

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Block diagram for manufacturing of Phosphoric acid using electric furnace

35

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
ELECTRIC FURNACE PROCESS

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Process diagram for manufacturing of Phosphoric acid using electric furnace

36

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
ELECTRIC FURNACE PROCESS

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Phosphate rock after proper grinding and

primary purification is taken into sintering oven
where it is nodulized and granulized so that fast
oxidation of the separated phosphorous takes
place.
Temperature of 10950C is maintained in electric
furnace so that maximum amount of elemental
phosphorous extracted out and oxidation takes
place.
Since fluoride of phosphorous and calcium are
the common impurity which reacts with sand
giving flourosilicates as the slag.

37

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

PHOSPHATE ROCK AND ELECTRIC FURNACE

The gases from the furnace, phosphorous and CO

are removed by the suction process and the
oxidation product P2O5 is taken into hydration
column which gives P2O5 to H3PO4 at about 850C.

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Purification of phosphoric acid is carried out by

H2S to remove Arsenic, H2SO4 to remove calcium
salts and Silica to remove fluorides.
All the byproducts are removed before
concentrating the acid and filtering it as final
product.

38

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

PHOSPHATE ROCK AND ELECTRIC FURNACE

Advantages of electric arc furnace over

other methods

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It

can handle low-grade phosphate rock, provided the

major impurity is silica.
Presence of iron and aluminum oxides are not
objectionable as in the wet process.
Siliceous rocks containing 24% phosphorus as P2O5
are acceptable.
The by-product CO, is used as a fuel for calcination.

39

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

OXIDATION AND HYDRATION OF PHOSPHOROUS

Raw materials
Basis:

1 ton phosphoric acid (100%)

Phosphorus
300kg
Air
46000 ft3
Steam
Water

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Reactions
2P + 2O2 P2O5
P2O5 + 3H2O 2H3PO4 (94 97% yield)
40

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

OXIDATION AND HYDRATION OF PHOSPHOROUS

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19800C

Block diagram for manufacturing of Phosphoric acid

41

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

OXIDATION AND HYDRATION OF PHOSPHOROUS

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19800C

42

Process diagram for manufacturing of Phosphoric acid

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

OXIDATION AND HYDRATION OF PHOSPHOROUS

The molten phosphorous is sprayed into combustion chamber

along with preheated air and superheated steam.
Combustion of phosphorous increases the temperature up to
19800C.
Furnace is made of acid proof structural bricks, graphite,
carbon and stainless steel.
The gases from furnace which mainly contains P2O5, steam, N2
and small quantity of oxygen is taken into a hydration column
where counter current mixing of dilute phosphoric acid and the
gases gives the product concentrated H3PO4 of 75% to 85%
concentration.
Remaining acid is trapped into packed column or electrostatic
precipitator.

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43

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

WET PROCESS OR FROM STRONG SULFURIC ACID

Raw materials

Basis: 1 ton phosphoric acid (100%)

Phosphate rock
1635kg
Sulfuric acid
1360kg

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Reaction
Ca10F2(PO4)6 + 10H2SO4 + 20H2O 10CaSO4.2H2O + 2HF + 6H3PO4

There are two processes i.e. dihydrate and hemihydrates (CaSO4.2H2O and
CaSO4.1/2H2O) are used for production of phosphoric acid.

44

PHOSPHORIC ACID: MANUFACTURING

PROCESSES
WET PROCESS OR FROM STRONG SULFURIC ACID

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45

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4 to 8hrs
75-800C.

Process diagram for

manufacturing of
Phosphoric acid

46

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

WET PROCESS OR FROM STRONG SULFURIC ACID

The grinded phosphate rock is reacted with dilute phosphoric

acid to produce melt, which in a reactor as mixed with
concentrated sulfuric acid for 4 to 8hrs in the temperature
range of 75-800C.
Excess air is required to control the temperature.
Resulting gases includes HF and P2O5 which in the absorption
tower is separated and finally treated to give fluorosilicates and
dilute phosphoric acid.
The main product in the liquid form which is phosphoric acid
and calcium sulfate is filtered and washed.
Thus, gypsum and phosphoric acid are separated and after
minor purification the phosphoric acid is concentrated into the
evaporator.

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47

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

WET PROCESS OR FROM STRONG SULFURIC ACID

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Throughout the plant, corrosion resistant materials

of construction must be used.
The most common ones are structural carbon or
nickel alloy for evaporator heat exchangers; rubber
or carbon-brick for reactor linings; polyester-fiber
glass in pipes, ducts, and small vessels.
Yield of phosphoric acid based on phosphorus
content of raw material is 95%

48

PHOSPHORIC ACID: MANUFACTURING

PROCESSES

WET PROCESS OR FROM STRONG SULFURIC ACID

Engineering Aspects

Selection of phosphate rock

Grinding of rock materials
Handling and storage of
phosphate rock
Amount of sulfuric acid
Filtration of gypsum
Purification
Sludge disposal

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49

PHOSPHORIC ACID: PROPERTIES

Molecular formula :

H3PO4

Molecular weight : 97.994gm/mole

Appearance :
White solid or colourless viscous liquid
above 420C
Boiling point : 1580C (decompose)
Melting point : 42.350C (anhydrous)
29.320C (hemihydrate)
Density : 1.885gm/mL (liquid)
1.685gm/mL (85%
solution)
2.030gm/mL (crystal at 250C)
Solubility : Soluble in water
Viscosity :
147cP (100%)

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50

PHOSPHORIC ACID: APPLICATIONS

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Used for preparation of hydrogen halides

Used as a "rust converter", by direct application to rusted iron, steel tools, or
surfaces. It converts reddish-brown iron(III) oxide, Fe2O3 (rust) to black ferric
phosphate, FePO4

Food-grade phosphoric acid is used to acidify foods and beverages such as

various colas.
Used in dentistry and orthodontics as an etching solution, to clean and
roughen the surfaces of teeth where dental appliances or fillings will be placed.
As an ingredient in over-the-counter anti-nausea medications that also contain
high levels of sugar (glucose and fructose).
Used in many teeth whiteners to eliminate plaque.
Used as an external standard for NMR and HPLC
As a chemical oxidizing agent for activated carbon production
As the electrolyte in phosphoric acid fuel cells and is used with distilled water
(23 drops per gallon) as an electrolyte in oxyhydrogen (HHO) generators.
Also, used as an electrolyte in copper electro polishing for burr removal and
51
circuit board planarization.

PHOSPHORIC ACID:
APPLICATIONS
8/20/15

As a flux by hobbyists (such as model railroaders) as an aid to

soldering.
As common wet etching agent in compound semiconductor processing,
Hot phosphoric acid is used in micro fabrication to etch silicon nitride
(Si3N4). It is highly selective in etching Si3N4 instead of SiO2, silicon
dioxide.
As a cleaner by construction trades to remove mineral deposits,
cementitious smears, and hard water stains.
As a chelant in some household cleaners aimed at similar cleaning
tasks.
Used in hydroponics pH solutions to lower the pH of nutrient
solutions.
As a pH adjuster in cosmetics and skin-care products.
As a dispersing agent in detergents and leather treatment.
As an additive to stabilize acidic aqueous solutions within specified
pH range

52

ACKNOWLEDGEMENT
Slides are developed from the following references:
Austin

G. T., "Shreves Chemical Process Industries",

Fifth edition, Tata McGraw Hill, NY.
Kent J.A., "Riegel's Handbook of Industrial
Chemistry, CBS Publishers.
Gopala Rao M. & Marshall Sittig, "Drydens Outlines of
Chemical Technology for the 21st Century", Affiliated
East West Press, New Delhi.
Mall I. D., "Petrochemical Process Technology",
Macmillan India Ltd., New Delhi.
http://nptel.ac.in/courses/103106108/24

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