الفهرس 
IntroductionOnly 14 pages are availabe for public view
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Abstract
Lithium greases either simple lithium greases or lithium complex greases are most favorable and widely used in manufacturing of multipurpose greases due to their excellent properties such as good temperature resistance, excellent water resistance and excellent mechanical stability. In the last decade the prices of lithium are extremely increased due to the expansion of electric cars and cell phone batteries production and the lithium rarity in earth. For these reasons the industrial sectors tend to use alternative greases to substitute lithium greases.
Our study aims to produce new locally prepared multipurpose greases using local raw materials in order to overcome the problems of providing lithium and its high price.
The thesis is divided into three parts:
PART I
Preparation of Calcium suphonate grease
In this part calcium sulphonate greases were prepared as multipurpose grease from heavy and light alkyl benzenes via sulphonation, neutralization, carbonation and grease formulation steps. First step sulphonation process
Sulphonation step was carried out after failure of trying to use commercial sulphonic acid in the market in the production of Over-Based Calcium Sulphonates (OBCS).
This process was carried out on Heavy Alkyl Benzene (HAB) using conc. H2SO4 98%, and studied the reaction at different conditions such as temperature,
Summary
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Acid/HAB ratio and digestion time using several trials. The optimum condition has been determined from the highest yield of Heavy Alkyl Benzene Sulphonic Acid (HABSA). The optimum temperature was 55⁰-60⁰C, digestion time four hours and Acid /HAB ratio 1.7/1.
By knowing the optimum temperature and digestion time, some sulphonation trials were carried out on Light Alkyl Benzene (LAB) using conc. H2SO4 98% with different Acid/LAB ratios at temperature 55⁰-60⁰C and digestion time four hours. The optimum Acid /LAB ratio was 1.5/1.
These several sulphonation trials were carried out in order to produce alkyl benzene sulphonic acid that is effective in the manufacture of OBCS. The prepared
Heavy Alkyl Benzene Sulphonic Acid (HABSA) and Light Alkyl Benzene Sulphonic Acid (LABSA) were evaluated by testing kinematic viscosity, color, water content, free sulphuric acid and anionic active matter.
Second step neutralization process
The neutralization of the prepared Heavy Alkyl Benzene Sulphonic Acid (HABSA) and Light Alkyl Benzene Sulphonic Acid (LABSA) by CaO in presence of methanol as promoter were carried out. Four neutralization trials have done for each Heavy Alkyl Benzene Sulphonic Acid (HABSA) and Light Alkyl Benzene Sulphonic Acid (LABSA) in different solvents and temperatures. These trials were carried out in order to produce calcium sulphonate that is effective in manufacture of Over-Based Calcium Sulphonates (OBCS). The prepared calcium sulphonate were evaluated by testing Total Base Number (TBN), sulfated ash, Ca % by weight and appearance. The most effective trial was the one which produced calcium sulphonate with higher Total Base Number (TBN).
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Third step carbonation process
This process was carried out in order to produce Over-Based Calcium Sulphonates (OBCS) which used in manufacture of calcium sulphonate grease, by passing CO2 gas on the prepared calcium sulphonate with excess calcium oxide in presence of methanol as promoter. The prepared Heavy Alkyl Benzene Over-Based Calcium Sulphonates (HAB-OBCS) and Light Alkyl Benzene Over-Based Calcium Sulphonates (LAB-OBCS) were evaluated by testing Total Base number (TBN), Ca% wt, detergency, dispersive power, colloidal stability, copper strip corrosion, appearance and solubility in oil.
Fourth step formulations of calcium sulphonate grease.
Simple calcium sulphonate greases were formulated using Heavy Alkyl Benzene Over-Based Calcium Sulphonates (HAB-OBCS), Light Alkyl Benzene Sulphonic Acid (LABSA) with different base oils in order to produce greases with consistency of National Lubricating Grease of America (NLGI) grades 1, 2 and 3.
Calcium sulphonate complex greases were formulated using Heavy Alkyl Benzene Over-Based Calcium Sulphonates (HAB-OBCS), Light Alkyl Benzene Sulphonic Acid (LABSA), complexing acids (like boric acid, phosphoric acid and 12-hydroxy strearic acid) and different base oils in order to produce grease with consistency of National Lubricating Grease of America (NLGI) grades 1, 2 and 3.
Both simple calcium sulphonate greases and calcium sulphonate complex greases were evaluated compared with samples of lithium greases as multipurpose greases. The evaluation has done by testing dropping point, unworked cone penetration, worked cone penetration, four ball welding load, four ball scare diameter, rust and washing %.
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The results of the properties of formulated grease showed excellent results of heat resistance, mechanical stability, water resistance, anti-wear and extreme pressure properties compared to lithium grease currently used in the market.
PART II Preparation of Bentonite Grease
In this part, another multipurpose grease substitute for lithium grease with dropping point over 300⁰C was prepared which can act as thermal greases.
Several trials were carried out on organoclay locally available used in the field of paints with base oil SN 260/290 in laboratory were carried out in order to determine the optimum manufacturing conditions. These conditions were gelling concentration, activator types and its concentration.
The optimum gelling concentration was determined by measuring the time required for densification between a mixture of base oil and organoclay using methanol 99% as activator. The proper gelling concentration was between 20% -40% organoclay in base oil.
The optimum activator type and its concentration were determined by using different activators (methanol, ethanol and acetone) at different concentrations with respect to organoclay. The optimum activator was noticed at the concentration of 20% methanol of the used organoclay.
The effect of adding water to methanol activator was studied to know the possibility of using commercial methanol in the production and also to decrease the toxic effect of methanol. The optimum water content was at percent of 10% water to methanol.
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The prepared bentonite grease from locally available organoclay and supplied with Egyptian pound (Viscogel B4) had excellent properties compared with lithium grease. The extreme pressure properties of the prepared greases were improved using Molybdenum disulfide (MoS2) as an additive. The prepared grease was evaluated on laboratory scale by testing dropping point, un-worked cone penetration, worked cone penetration, four ball welding load, four ball scar diameter, rust and washing %.
Some trials to prepare organobentonite were done using Egyptian bentonite and hexadecyltrimethyl ammonium chloride. The prepared greases using this organobentonite yielded greases with low (dropping point) compared with lithium greases i.e., couldn’t substitute lithium greases. This is due to the nature of Egyptian bentonite which contains other ingredients beside smectite minerals which lowering the absorption power of bentonite and Egyptian bentonite is mainly composed of Ca smectite which is lower in swelling power than Na smectite.
The prepared bentonite grease using prefabricated Organobentonite [The imported organoclay locally available and supplied by Egyptian pound (Viscogel B4) was tested in client Mechanical and Electrical Department (MED) factory. The tested grease was approved by client. The successful grease was manufactured in Misr Petroleum Company (MPC) factory. The locally produced bentonite greases are approved to be sold in the market.
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PART III Preparation of Waxing compound (Wax-Grease Mixture)
Many metal producers tend to protect their production using waxing compounds. In Egypt they using waxing compound composed of (microcrystalline wax, petrolatum and BS 5000). These components are imported and no longer present in Egyptian market. The only available wax is paraffin wax. But there is a great difference in behavior between imported microcrystalline wax and local paraffin wax. This is due to the great adhesion properties of microcrystalline wax compared to paraffin wax.
To overcome this problem Misr Petroleum Company (MPC) grease formulators used wax-lithium grease compound as metal coating. The paraffin wax- lithium grease compound (mixture) had good laboratory results but it caused problems during working in industry rather than the great price of lithium.
In this part wax-grease mixtures (waxing compounds) were prepared according to the following:
The initial formulation of waxing mixture which composed of (microcrystalline wax, petrolatum and BS5000).
Calcium 12-hydroxy stearate- paraffin wax mixture at different soap concentrations.
Lithium 12- hydroxy stearate – paraffin wax mixture with different soap concentrations.
Aluminum stearate – paraffin wax mixture using already prepared soap (locally produced aluminum stearate) at different concentrations.
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The above mixtures were prepared in order to make comprehensive evaluation of wax- grease mixtures as metal coatings.
The prepared mixtures were evaluated by testing DROP melting point, cone penetration, copper strip corrosion and adhesion power tests.
The results revealed the followings:
The initial formulation had good adhesion power with metal but the client needed more heat resistance properties (i.e. higher DROP melting point).
Calcium 12-hydroxy stearate- paraffin wax mixture had low heat resistance and mechanical stability during storage.
Lithium 12-hydroxy stearate – paraffin wax mixture had better laboratory results compared to initial formulation. But it had some problems during working in factory due to its very high melting point it decomposed during melting process before spraying on the metal surface. The decomposition of the mixture produces brown fumes and bad odor in addition to the main problem of using lithium because of its price and unavailability.
Aluminum grease –paraffin wax mixture gives excellent laboratory results (suitable DROP melting point, suitable cone penetration, excellent copper strip corrosion resistance and excellent adhesion power).
The newly and locally prepared Aluminum base waxing was subjected to a field trial in Egyptian Copper Company (ECC) copper rolling factory. The waxing compound was approved by client. The product was manufactured easily in Misr Petroleum Company (MPC) grease factory.
The locally produced aluminum base waxing compound was approved to be sold in the market.
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Feasibility study
PART I
The cost of the prepared calcium sulphonate grease prepared using local raw materials was calculated compared to lithium grease. The cost of simple calcium sulphonate grease was 58% of lithium grease cost. The cost of calcium sulphonate complex grease was 53% of lithium grease cost.
PART II
The cost of the prepared bentonite grease prepared using local raw materials was calculated compared to lithium grease. The cost of bentonite grease was 42% of the lithium grease cost.
PART III
The Cost of the local Aluminum grease- wax compound is about 40% of the cost of wax gel grease prepared from imported materials. The Cost of the local Aluminum grease- wax compound is about 30% of the cost of wax- lithium grease compound.