.
Form P-1
Fee: Rs.
Insert (in full) the name,
address, and nationality
of the applicant or
applicants.
Insert title of the invention.
Insert who is the inventor.
State here whether the
specification accompanying this
“complete”.
Insert number of sheets of the
Description, Claim(s), Abstract,
and Drawing(s).
Insert address for
Service in Pakistan
.
Insert name,
designation and
address of the
signatory. In case of
Agent, also include
latest tele-
communication
details.
Signature: _____________________
1. Name: Dr. Muhammad Younas
Designation: Associate Professor______
Address: University of Engineering & Technology, Peshawar
Signature: ___________________
3. Name: Engr. Waheed Zeb
Designation: PhD Scholar
Address: University of Engineering & Technology, Peshawar
Patent Ordinance, 2000
Application for patent when the true and first
inventor is sole or joint applicant
(Section 13(1) Rule 8(1))
(To be accompanied in duplicate by a provisional specification
on Form P-3 or the Complete Specification of Form P-3A)
We,
Dr. Muhammad Younas, University of Engineering & Technology, Peshawar (Pakistani)
Engr. Waheed-Ur-Rehman, PCSIR Laboratories Complex, Peshawar (Pakistani)
Engr. Waheed Zeb, University of Engineering & Technology, Peshawar
(Pakistani)
hereby declare that: -
” Integrated Membrane Process for Concentration of Fruit Juices”
(i) we are in possession of an invention
for “Integrated Membrane Process for Concentration of Fruit Juices”
(ii) that I (or we) (or the Said) (Muhammad Younas, Waheed-Ur-Rehman &
Waheed Zeb) claim to be the true and first inventor
thereof;
(iii) that the invention is not in use in Pakistan by any other person;
(iv) that the complete specification filed with this application is,
and any amended specification which may hereafter be filed in this behalf will be,
true of the invention to which this application relates;
(v) that following are particulars of my application,-
10 Nos.
Description:
(Total)
Claim (s): 07 Nos.
Abstract: 01 page
Drawing (s): 03 Nos.
University of Engineering & Technology, Peshawar, Pakistan
I (or we) respectfully request that a patent may be granted to me (or us)
for the said Invention.
Dated this, 5th day of December, 2017,
Signature: ___________________
2. Name: Engr. Waheed-Ur-Rehman
Designation: Junior Engineer
Address: PCSIR Labs. Complex, Peshawar
Page 1 of 10
To
Controller of Patents
The Patent Office
Karachi
Form P-3 A Patent Ordinance, 2000
Fee: Rs. Application for complete specification
(Section 14)
(To be supplied in duplicate with Forms P-2, P-2A, P-2B or P-2C
or
Forms P-1, P-1A, P-1B or P-1C
(if a Provisional Specification is not accompanying))

Insert title verbally “Process for the extraction of antimony metal from low grade Krinj
Agreeing with that in the stibnite ore”
application form.

Insert (in full) the name, Engr. Waheed-ur-Rehman, PCSIR Labs. Complex Peshawar (Pakistani)
address, and nationality Dr Muhammad Riaz, PCSIR Labs. Complex Peshawar (Pakistani)
of the applicant or Engr. Muhammad Ishaq, SNGPL, Peshawar (Pakistani)
applicants.

Description: (including this page) 10 Nos. (Total)

Insert number of sheets of the Claim (s): 07 Nos.
Description, Claim(s), Abstract,
and Drawing(s). Abstract: 01 page
Drawing (s): 03 Nos.

Insert address for PCSIR Laboratories Complex Jamrud Road Peshawar, (KPK),
Service in Pakistan Pakistan

Here begin full description of the The following specification particularly describes and ascertains the nature of the
invention. nature of this invention and the manner in which it is to be performed:-

Page 2 of 10
 Abstract

Antimony is a silvery white, brittle and crystalline solid which is extensively consumed in lead
acid batteries, antimonial lead alloys, flame retardants and a variety of metallic products. The
antimony content of commercial ores range from 5-60% and determines the method of
extraction, either pyrometallurgical or hydrometallurgical. The present invention relates to the
extraction of antimony metal from lower grade stibnite ore of Krinj (Chitral) without the use of
iron scrap, thus eliminating the second step of iron removal in conventional direct reduction
method. A tilting gas fired furnace with digital temperature control system was designed to
optimize the operating parameters for extraction of antimony metal. Weight ratios of flux and
reductant, operating time and operating temperature were optimized. Highest percentage
recovery and purity were achieved using soda ash as a flux and charcoal as a reductant, at a
temperature of 900 oC for 2 hours.

Page 3 of 10
 Introduction

Antimony is obtained from stibnite (Sb2S3) ore containing 20–60 percent Sb, by the
pyrometallurgical and hydrometallurgical treatment. The pyrometallurgical methods include
precipitation smelting and reduction smelting. Sulphide concentrates serve as the raw material
for precipitation smelting, which is based on the replacement of antimony in the sulphide by
iron:
Sb2S3 + 3Fe ⇄ 2Sb + 3FeS
The iron is introduced into the charge as scrap, and the smelting is carried out in reverberatory or
short rotating furnaces at 1300-1400°C. The extraction of antimony in the form of crude metal
exceeds 90 percent. The reduction smelting of antimony is based on the reduction of antimony
oxides to the metal using charcoal or coal dust and on the slagging of waste rock. Reduction
smelting is preceded by oxidative roasting at 550°C with an excess of air. The calcine contains
the non-volatile tetroxide of antimony. Electric furnaces can be used in both precipitation and
reduction smelting. Pyrometallurgical or electrolytic refining is used to produce pure antimony.
In pyrometallurgical refining, impurities of iron and copper are removed as sulphur compounds
by introducing antimonite (Sb2S3); arsenic (as sodium arsenate) and sulphur are then recoved by
passing air under the soda slag. In electrolytic refining with a soluble anode, crude antimony is
purified of iron, copper, and other metals remaining in the electrolyte (with Cu, Ag, and Au
remaining in the slurry. A solution consisting of SbF 3, H2SO4, and HF serves as the electrolyte.
The content of impurities in refined antimony does not exceed 0.5–0.8 percent. To obtain high-
purity antimony, zone refining is carried out in an atmosphere of inert gas, or antimony is
obtained from previously purified antimony trioxide or antimony trichloride.
The present invention focuses on direct production of metal from ore without the use of
iron scrap, thus eliminating the second step of iron removal in conventional reduction method.

Page 4 of 10
 Example

The Krinj stibnite ore which was used in our studies had an antimony content of 22.00%. About
1 Kg of ore was crushed in jaw crusher to a size of 0.5 in to 2 in. The crushed ore was ground in
a disc grinder to a mesh size of -60+80 (-246µm+175µm). The ground stibnite ore was uniformly
blended with 700 grams of soda ash as a flux and 140 grams of charcoal as a reducing agent. The
final recipe was kept in a graphite crucible in a tilting gas fired furnace. The furnace as shown in
figure-3 consisted of an outer mild steel shell which was internally lined with high alumina
refractory castable. Ceramic wool insulation was provided in-between the shell and refractory
castable. Natural gas was used as a fuel, while air was provided by a blower to aid in
combustion. Air and gas were mixed in a burner nozzle. An R-type thermocouple was installed in
the furnace for temperature detection. Its output was fed to a digital temperature controller. There
the desired temperature was already set. The error generated in the controller due to the
difference in set point temperature and measured temperature, caused a solenoid valve on natural
gas line to open or close. At the same time the error value caused the blower to start or stop. Thus
as the temperature exceeded the set point value, the controller simultaneously closed the solenoid
valve and stopped the blower. So a stable temperature was maintained in the furnace. A graphite
crucible resting on a high alumina frustum was used for smelting purpose. The furnace could be
tilted to pour the molten product in sand moulds. The sample was smelted at controlled
temperature of 900 oC for a period of 2 hours. After smelting the molten metal along with slag
was poured into sand mould. When the metal and slag cooled and solidified, the mould was
broken to get pure metal. 81.00 percent of antimony was recovered with a purity of 99.00
percent.

Page 5 of 10
Figure-1: Process Block Diagram

Ore

Crushing

Grinding

Smelting

Casting

Antimony
metal

Page 6 of 10
Figure-2: Equipment Block Diagram

Jaw crusher

Disc grinder

Blender

Smelting furnace

Casting molds

Antimony metal

Page 7 of 10
 Graphite Cruicible
TIC
Temperature Controller

Refractory Castable
Air

Blower
SV Solenoid Valve
High Alumina Frustum
Mixer Burner
Natural Gas
Pilot Valve

Figure-3: Diagram of Antimony Extraction Furnace

Page 8 of 10
Table-1: Chemical Composition of Stibnite

Compound Percentage (%)

Sb2S3 30.56
SiO2 26.06
SO3 33.92
Others 9.46

We claim:
Page 9 of 10
1. The process for extraction of antimony metal from stibnite ore, wherein stibnite
ore is of lower grade containing 22% antimony metal.
2. The process as claimed in claim 1, wherein stibnite ore is ground to a particle size
of -246µm+175µm in disc grinder.
3. The process as claimed in claim 1, wherein ground stibnite ore is blended with
soda ash and charcoal.
4. The process as claimed in claim 3, wherein soda ash acts as a flux and charcoal as
a reducing agent.
5. The process as claimed in claim 1, wherein smelting of stibnite ore is carried out
in the presence of flux and reducing agent.
6. The process as claimed in claim 5, and as shown in figure 3, wherein smelting
furnace is gas fired with an arrangement of air blower and temperature control
system.
7. The process as claimed in claim 5, wherein the smelting temperature is 900 oC for
a period of 2 hours.
8. The process as claimed in claim 5, wherein 81.00 % of antimony metal is
recovered with a purity of 99.00%.

Signature: _____________________ Signature: ___________________

1. Name: Engr. Waheed-ur-Rehman 2. Name: Dr. Muhammad Riaz___
Designation: Junior Engineer______ Designation: Chief Scientific Officer
Address: PCSIR Labs. Complex, Peshawar Address: PCSIR Labs. Complex, Peshawar

Signature: ___________________ Signature: ___________________

3. Name: Engr. Muhammad Ishaq 4. Name: Asma Yamin
Designation: Billing Engineer Designation: Senior Scientific Officer
Address: SNGPL, Peshawar Address: PCSIR Labs. Complex, Peshawar

Dated: 06h May, 2013

Page 10 of 10