C.I.E. - PHOENIX - Process for treatment and recovery of caustic soda spent solution used for die cl

PHOENIX

℗

Process for treatment and recovery of caustic soda SPENT SOLUTION USED FOR DIE CLEANING Patented process

The process is divided into two phases, that can also be made separately

Dirty dies

Die cleaning bath

PHOENIX℗ REVALUATION PROCESS

Neutral water dump

Al2O3.H2O

Exhaust treatment with production of pure and recyclable Alumina hydrate (Al2O3.H2O) as secondary raw material (Already existing approval) The resulting water could be sent to dump without further depuration.

Dirty dies

Die cleaning bath

NaOH Neutralization & Regeneration

NaOH Concentration

Recyclable Solids

Al(OH)3

CaCO3

Exhaust treatment with production of Alumina hydrate (Phoenix Revaluation) On site recovery and recycling with a yield of more than 95%.

In this case the process is zero waste water PHOENIX℗: Save more than 50% of current running cost C.I.E. s.r.l. Via 1° Maggio 20/22 20070 San. Zenone al Lambro (MI) - Italy Tel. +39 02 9810470 – Fax +39 02 98175079 - E-mail: info@cieeng.com – web: www.cieeng.com

PHOENIX

℗

REVALUATION

Neutralization and upgrading process for spent Die cleaning solutions PHOENIX℗ REVALUATION

: Saving of 56% to 80% on operating costs!!!!!

Patented process

Dirty dies

PHOENIX

℗

is a process designed and developed by CIE for the Neutralization of spent alkaline baths from aluminum pickling (like washing extrusion dies.) with production of aluminum hydroxide, no longer considered toxic, but as pure, recyclable and reusable PHOENIX ℗ is based on chemical neutralization with CO2, followed by filtration to separate the hydroxide in solid form and then by the direct discharge of the neutralized liquid without further treatment.

PHOENIX ℗ The relocation of hydroxide is conveyed with prices and contracts agreed STANDARD WORKING PARAMETERS OF DIE CLEANING:

Die Cleaning Plant

NaOH spent bath: 150 -:- 250 g/l Al spent bath: 30 -:- 70 g/l

PHOENIX℗ REVALUATION PROCESS

Neutral water dump

Al(OH)3

PHOENIX℗ REVALUATION:

Benefits and Process Overwiew

1) Elimination of disposal costs 2 ) Environmentally friendly (No hazardous waste) 3 ) Production of recyclable solids: pure resalable Aluminum hydroxide as raw material for various industrial uses (refractories, ceramics, fire retardants, pigments for paints, bases for flocculants) 4) Simple, convenient and no dangerous chemical to be used 5) Operating costs below 40 € per tonne of spent bath 6) Further recovery of 20% of operating costs from the resale of aluminum hydroxide

CO 2

Neutralization

Spent Die Cleaning solution

Partial water recovering

Filtrazione Direct dump Ph 8,5 Recyclable Solids

Al(OH)3 C.I.E. s.r.l. Via 1° Maggio 20/22 20070 San. Zenone al Lambro (MI) - Italy Tel. +39 02 9810470 – Fax +39 02 98175079 - E-mail: info@cieeng.com – web: www.cieeng.com

PHOENIX

℗

REVALUATION

Neutralization and upgrading process for spent Die cleaning solutions PHOENIX℗ REVALUATION:

PROCESS TECHNOLOGY

PHOENIX℗ REVALUATION process has been studied for on-site treatment of spent Die cleaning solutions by avoiding outside disposal or on-site depuration

Process principles The spent solution (rinse and baths), after filtration to remove oil and carbon residue, are placed in a reactor . By insufflation of CO2 until a determined pH, we have the precipitation of aluminum hydroxide and the neutralization of NaOH according to the following reactions : 2 NaOH + CO2  Na2CO3 + H2O 2 NaAlO2 + CO2 + 3 H2O  Na2CO3 + 2Al(OH)3 After homogenizing and conditioning, the mud will be sent to filter press where there is the separation of Pure Al(OH) 3.

The filtered water is recovered as new Die cleaning bath because it contains 5-10% of NaOH equivalent. This saves from 90% to 95% of fresh NaOH. The surplus of the filtrate is finally neutralized with other CO2 using the following reaction : Na2CO3 + CO2 + H2O  2 NaHCO3 and finally discharged without other treatment.

Aluminium Hydroxide destination: The sludge produced is presented free of impurities, metals and other pollutants, it is white and is composed of Al (OH) 3 with pure carbon content below 2%. It is a mud with 30% of dry neutral.

It can therefore be sold to concerned sector companies that, after drying and grinding, can use it as the equivalent of 65% for alumina refractories, ceramics, porcelain, fire retardants, pigments for paints or bases or aluminum sulfate or polyclorides used for flocculation.

The PHOENIX℗ REVALUATION plant is also extensible without modification to achieve the catalytic process for the regeneration and the total recovery of caustic soda exhausted (PHOENIX℗ CATALYST).

The PHOENIX℗ REVALUATION process, lends itself particularly to small and medium spent volume productions, between 5 and 10 tons per week (corresponding on average to 150 to 300 die per week to wash.)

PHOENIX ℗ REVALUATION: Costs and Savings per tonne of Exhaust The costs of management of Phoenix Revaluation proces is given by : -CO2 257 Kg x 0,15 € /Kg = 38,5 € -Energy (7 Kwh x 0,15 €/kwh) = 1,5 €

TOTAL = 40 €/tonne of spent solution The relocation of aluminum hydroxide Al(OH)3 was established by chemical analysis and practical tests of compatibility in the field of porcelain which uses large quantities and the current rating of the resale price is around 60 €/ton of 100% pure dried hydroxide. Since the spent solution contains about 13 -15% of hydroxide, it follows that the recovery will amount to

8 €/tonne of exhaust.

THE REAL COST will therefore be given 40 - 8 = 32 € / tonne of spent solution Given that the disposal of spent solution outside has a cost ranging from 70 to 150 €/tonne, it follows that saving will be from 38 € to 118 € / tonne of spent solution (56-80%) Chemical analysis of aluminium hydroxide (100%) by Phoenix revaluation process -Aspect: - Al(OH)3 -Na -CO3

white powder 98,2 % - Specific gravity: 0,49 % - Ph: 1,29 % - SiO2, Fe2O3

2,42 g/cm3 9,8 less then 0,02 %

C.I.E. s.r.l. Via 1° Maggio 20/22 20070 San. Zenone al Lambro (MI) - Italy Tel. +39 02 9810470 – Fax +39 02 98175079 - E-mail: info@cieeng.com – web: www.cieeng.com

PHOENIX

℗

CATALYST

Catalitic Process for Caustic Soda recovering by spent die cleaning solutions

WHAT IS PHOENIX℗ CATALYST? PHOENIX℗

D I E Dirty Dies

C L E A N I N G S H O P

is a special Process studied and developed by C.I.E. for treatment of spent Alkaline DIE CLEANING SOLUTIONS PHOENIX℗ is based on chemical neutralization with solid separation of Al(OH)3

by CO2 and a catalytic process for the regeneration of Caustic Soda. ℗ PHOENIX license is allowed by C.I.E. to its customers with a specific confidential agreement ℗ PHOENIX is the process without any liquid discharge Z.L.D. (Zero Liquid Discharge)

PHOENIX℗ PROCESS Die Cleaning Bath NaOH Neutralization & Regeneration

NaOH Concentration

Recyclable Solids

Patented Process Al(OH)3

CaCO3

STANDARD WORKING PARAMETERS OF DIE CLEANING SOLUTIONS: NaOH conc. of fresh bath : 200 -:- 300 g/l NaOH conc.of spent bath : 150 -:- 250 g/l Al conc. of spent bath : 30 -:- 70 g/l

PHOENIX℗ Lay-out Catalyst (powder) Spent solution inner heating shell inner heating shell

CO 2

Filtration NaOH Regeneration

NaOH Concentration

Neutralization

1° step

Recyclable Solids

NaOH 25 ÷30 %

3° step

2° step Al(OH)3

CaCO3

C.I.E. s.r.l. Via 1° Maggio 20/22 20070 San. Zenone al Lambro (MI) - Italy Tel. +39 02 9810470 – Fax +39 02 98175079 - E-mail: info@cieeng.com – web: www.cieeng.com 1/2

PHOENIX

℗

CATALYST

Catalitic Process for Caustic Soda recovering by spent die cleaning solutions PHOENIX℗ - Chemical Reaction 1st Step

+ CO2 NEUTRALIZATION

Na2CO3 + Al(OH)3

NaOH + NaAlO2 R.Temp

2nd Step

CATALYTIC REGENARATION Na2CO3 + H2O

(solid)

CCO *

NaOH + CaCO3

T = 80 °C

(solid)

* CCO = Catalytic Calcium Oxide

3rd Step

- H2O NaOH CONCENTRATION

NaOH

NaOH 12-15%

60°- 70 °C

25÷30%

PHOENIX℗ - Performances 1) 95% recovery of NaOH contained into the spent die cleaning solutions 2) Environmental friendly managing (NO MORE hazardous wastes) 3) Save up to 50% of die cleaning costs 4) Simple,cheap and NON hazardous chemicals to use 5) Produce only NON hazardous solids,recyclable again as raw materials for industry (Aluminium Hydroxide and Calcium Carbonate)

C.I.E. s.r.l. Via 1° Maggio 20/22 20070 San. Zenone al Lambro (MI) - Italy Tel. +39 02 9810470 – Fax +39 02 98175079 - E-mail: info@cieeng.com – web: www.cieeng.com 2/2