CA1339651C - Super-heavy oil emulsion fuel - Google Patents

Abstract

Disclosed is an O/W type emulsion fuel comprising [A]
100 parts by weight of super-heavy oil, [B] 30-80 parts by weight of water, [C] a nonionic surface active agent having an HLB value of 9-19 and [D] an anionic surface active agent, a naturally-occurring hydrophilic polymer substance or a water-soluble synthetic polymer. The emulsion can be formed by mechanically stirring the components and has a low viscosity.
By forming the emulsion, super-heavy oil such as petroleum-based asphalt or bitumen is made flowable and can be used as a fuel.

Description

13~3~51 Super-Heavy Oil Emulsion Fuel Industrial Utilization Field This invention relates to a super-heavy oil emulsion fuel.

[Description of the Prior Art]
Buried deposits of fossil fuel resources such as oil sand, bitumen and natural asphalt which are not contained in petroleum, coal or LNG are drawing attention as a result of their extremely vast amounts. In addition, with respect to petroleum-based substances also, asphalt and other heat-treated residues from which oil distillates such as naphtha have been removed are also in large excess. These super-heavy oils are oily substances which contain approximately 60-70% or more of a heavy fraction of 420-450~C or more which is normally the product of distillation under reduced pressure, and either do not flow as is or have high viscosity of several tens of thousands centepoise or more.
As a result, when using as a fuel, if not heated to high temperatures, problems relating to handling and atomization occur. In addition, such fuels are also susceptible to resulting in blocking of pipes, etc. making them very difflcult to use.
[Disclosure of the Inventlon]
The lnventors discovered that a super-heavy oil, oil droplets ln water type (O/W type) of emulsion fuel in whlch super-heavy oll (O) is emulsifled ln water (W) can be prepared when a sultable surface active agent, called also a surface actlvatlng agent, ls used. Thls emulsion fuel exhibits a vlscoslty which is comparatively close to that of water and allows adequate atomlzatlon at high temperatures of, for example, 40-90~C making lt extremely easy to handle. O~W type emulslon fuels are more preferable the lower the water (W) content, ln other words, the greater the oll (O) content, since fuel loss ls less. In order for emulslon fuels to be handled in the same manner as ordinary llquld fuel olls, long-term stability which allows the fuel to wlthstand transport and storage ls requlred. Although there are numerous reports ln the past of uslng olls of satisfactory fluidity such as kerosene, heavy oil A, heavy oll B and heavy oll C by emulslfylng super~heavy oil which has an extremely large heavy fraction and elther does not flow or has a viscosity of several ten thousand centipoise and then using it as a fuel.

X

1~3~b~i The inventors discovered that a low viscosity O/W
type emulsion fuel can be prepared by appropriately combining a nonionic surface active agent having an HLB (hydrophilic lipophilic balance) value of 9-19 selected from those defined in (I)-(VII) hereinunder with either (i) an anionic surface active agent selected from those defined in (i)-(vii) herein-under or (ii) a naturally-occurring hydrophilic polymer defined in (A)-(D) hereinunder or a hydrophilic synthetic polymer defined in (a)-(f) hereinunder, by stirring the components by a mechanical force of a line mixer etc.
Thus, an embodiment of the invention provides a low viscosity, O/W type super-heavy oil emulsion fuel comprising 100 parts (by weight standard, the same applies to all to follow) of super-heavy oil, 30-80 parts, and preferably 33-50 parts, of water, 0.01-4 parts by weight of an anionic surface active agent selected from those defined in (i) to (vii) below and a nonionic surface active agent having an HLB of 9-19 selected from those defined in (I)-(VII) below at an anionic surface active agent /
nonionic surface active agent weight ratio of 1/99-75/25, preferably 10/90-40/60.
(Anionic surface active agent) (i) This group consists of formalin condensation products of sulfonic acid or sulfonate salts of cyclical aromatic compounds such as naphthalene, alkylnaphthalene, alkylphenol or alkyl-benzene, in which the average degree of condensation of formalin is 1.2-100, and preferably 2-20. The salts are lower amines such as ammonium, 13336~1 monoethanolamine, diethanolamine, triethanolamine and triethylamine or alkali metals or alkaline earth metals such as sodium, potassium, magnesium and calcium.
(ii) This group consists of the formalin condensation products of lignin sulfonic acid, lignin sulfonate salts, its derivative and lignin sulfonate and sulfonates of aromatic compounds, naphthalene and alkylnaphthalene, and their salts. In any of the cases above, the salts are lower amines such as ammonium, monoethanolamine, diethanolamine, triethanolamine and triethylamine, or alkali metals or alkaline earth metals such as sodium, potassium, calcium and magnesium. The average degree of condensation of formalin is 1.2-50, and preferably 2-20.
For the lignin, the introduction of, for example, a few carboxyl groups results in superior performance particularly at high temperatures.
(iii) This group consists of copolymers and their salts of polystyrene sulfonic acid and its salts as well as styrene sulfonic acid and other copolymerizing monomers in which the molecular weight is 500-500,000, and preferably 2000-100,000. The salts are lower amines such as ammonium, monoethanolamine, diethanolamine, triethanolamine and triethylamine, or alkali metals or alkaline earth metals such as sodium, potassium, calcium and magnesium. Typical examples of copolymerizing monomers include acrylate, methacrylate, vinyl acetate, acrylic ester, olefins, allyl alcohols as well as their ethylene oxide addition products, and AMPS.
(iv) This group consists of dicyclopentadiene sulfonate polymers and their salts in which the molecular weight of the polymer is 500-500,000, and preferably 2000-100,000.
The salts are lower amines such as ammonium, monoethanolamine, diethanolamine, triethanolamine and triethylamine, or alkali metals or al~aline earth metals such as sodium, potassium, calcium and magnesium.
(v) This group consists of copolymers and their acids and salts of maleic anhydride and/or itaconic anhydride and other copolymerizing monomers in which the molecular weight is 500-500,000, and preferably 1500-100,000. Salts are ammonium as well as alkali metals such as sodium, and potassium. Examples of the copolymerizing monomer include olefins (ethylene, propylene, butylene, pentene, hexene, heptene, octene, nonene, decene, undecene, dodecene, tridecene, tetradecene, pentadecene, hexadecene), styrene, 13~g6~1 vinyl acetate, acrylic ester, methacrylate and acrylate.
(vi) This group consists of the maleic compounds and their salts of liquid polybutadiene in which the molecular weight of liquid butadiene is 500-200,000, and preferably 1000-50,000. The copolymer is preferred to have so high a content of maleic anhydride units as to be soluble in water, more preferably 40-70%.
Salts include ammonium as well as alkali metals such as sodium and potassium.
(vii) This group consists of the following anionic surface activating agents having 1 or 2 hydrophilic groups within the same molecule.
(a) Sulfuric ester salts of alcohols having 4-18 carbon atoms in which the salts are lower amines such as ammonium, monoethanolamine, diethanolamine, triethanolamine or triethylamine, or alkali metals or alkaline earth metals such as sodium, potassium, magnesium or calcium. Typical examples include sodium dodecyl sulfate and sodium octyl sulfate.
(b) Alkanes, alkenes and/or alkylaryl sulfonates or their salts having 4-18 carbon atoms in which the salts are lower amines such as ammonium, monoethanolamine, diethanolamine, triethanolamine and triethylamine, or alkali metals or 133~651 alkaline earth metals such as sodium, potassium, magnesium and calcium. Typical examples include sodium dodecylbenzyl-sulfonate, sodium butylnaphthalenesulfonate and sodium dodecanesulfonate.
(c) Sulfates or phosphate esters and their salts of the alkylene oxide addition products of compounds having 1 or more activated hydrogens within the same molecule. Examples of the salts include ammonium, sodium, potassium, magnesium and calcium. Typical examples include the sodium sulfuric ester salt of polyoxyethyelene (3 mol)nonylphenyl ether and the sodium phosphoric ester salt of polyoxyethylene(3 mol) dodecyl ether.
(d) Sulfosuccinate salts which are esters of saturated or unsaturated fatty acids having 4-22 carbon atoms in which the salts are ammonium, sodium or potassium. Typical examples include sodium or ammonium dioctylsulfosuccinate and sodium dibutylsulfosuccinate.
(e) Alkyldiphenylether disulfonates and their salts. The alkyl groups have 8-18 carbon atoms and the salts are ammonium, sodium, potassium, magnesium and calcium.
(f) Rosin acids and their salts in which the salts are ammonium, sodium and potassium. Tall oil and acid mixture, 13396~1 which is an acid mixture of rosin acid and higher fatty acids, and its salts are also included.
(g) Alkanes or alkene fatty acids having 4-18 carbon atoms and their salts in which the salts are ammonium, potassium and sodium.

<Nonionic Surface Activating Agents with HLB of 9-19>
(I) This groups consists of the alkylene oxide addition products of compounds having phenolic hydroxyl groups such as phenol, cresol, butylphenol, nonylphenol, dinonylphenol, dodecylphenol, para-cumylphenol and bis-phenol A, in which the alkylene oxide is ethylene oxide and/or propylene oxide, butylene oxide or styrene oxide.
(II) This group consists of the alkylene oxide addition products of the formalin condensation products of compounds having phenolic hydroxyl groups such as alkylphenol, phenol, meta-cresol, styrenated phenol and benzylated phenol, in which a condensation degree is 1.2-100~ or preferably ~ . . ..

2-20. The alkylene oxide is ethylene oxide and/or propylene oxide, butylene oxide or styrene oxide.
(III) This group consists of the alkylene oxide addition products of monovalent aliphatic alcohols and/or aliphatic amines having 2-50, preferably 12 to 20, carbon atoms, in which the alkylene oxide 13~6~1 is ethylene oxide and/or propylene oxide, butylene oxide or styrene oxide.
(IV) This group consists of the block or random addition polymers of ethylene oxide and propylene oxide and/or butylene oxide and styrene oxide.
(V) This group consists of the alkylene oxide addition products of polyvalent alcohols such as glycerine, trimethylolpropane, pentaerythritol, sorbitol, sucrose, polyglycerine, ethylene glycol, polyethylene glycol, propylene glycol and polypropylene glycol, or the esters of those polyvalent alcohols and fatty acids having 8-18 carbon atoms. The alkylene oxide is ethylene oxide and/or propylene oxide, butylene oxide or styrene oxide.
(VI) Alkylene oxide addition products of polyvalent amines having a multiple number of active hydrogen atoms such as ethylenediamine, tetraethylenediamine and polyethyleneimine (molecular weight: 600-1,000,000). The alkylene oxide is ethylene oxide and/or propylene oxide, butylene oxide or styrene oxide.
(VII) The products of the reaction resulting from the addition of an alkylene oxide to a mixture of 1 mole of triglyceride-type oil and 1 or 2 or more types of polyvalent 1 ~3~65 1 alcohols selected from the group consisting of glycerine, trimethylolpropane, pentaerythritol, sorbitol, sucrose, ethylene glycol, polyethylene glycol with a molecular weight of 1000 or less, propylene glycol, and polypropylene glycol having a molecular weight of 1000 or less, and/or 0.1-5 moles of water. The alkylene oxide is ethylene oxide and/or propylene oxide, butylene oxide or styrene oxide.

From among the anionic surface activating agents selected from the groups indicated in (i)-(vii) above, the formalin condensation products of lignin sulfonic acid and lignin sulfonate with naphthalene sulfonate and their salts, and the formalin condensation product of naphthalene sulfonate demonstrated particularly superior performance overall. The action of anionic surface active agents involves adsorbing onto the interface of the particles of the super-heavy oil thereby giving an electrical charge to the particles while simultaneously assisting in reducing the size of the particles resulting in prevention of aggregation of the particles. Although nonionic surface active agents are strongly susceptible to the effects of temperature, when anionic surface active ~ ~ 3 ~ fi 5 1 agents are added, the effects of temperature are weakened resulting in improved storage stability of the emulsion.
The action of the above nonionic surface activating agents involves adsorbing onto the interface of the particles of the super-heavy oil and preventing aggregatiOn of the particles as a result of protective action while simultaneously assisting in reducing the size of the particles.
In the case of anionic surface activating agent alone, storage stability is inadequate. Similarly, in the case of nonionic surface activating agent alone, a stable emulsion fuel cannot be obtained since such agents are strongly susceptible to the effects of temperature. By adding anionic surface activating agent to nonionic surface activating agent to reduce their dependence on temperature, it is possible to prepare a stable emulsion fuel.
The amount of anionic surface activating agent may be 0.005-2.2 wt.%, and preferably 0.06-0.61 wt% based on the total emulsion fuel.
more types o~ anionic surface activating agen~ and nonionic surface activating agentsrespectively may also be used. In addition, the anionic surface activating agent and nonionic surface activa~ing agent may be added separately or may be 1 ~ .3 added in the form of a mixture mixed in advance.
Although the optimum HLB value of the nonionic surface activàting agent varies according to the temperature at the time of emulsion, a value of 9-19 is preferable with a value of 12-17 being more preferable. From among the nonionic surface activating agents indicated above, the surface activating agent indicated in (VII) above is the most superior, followed by (II) and (III) which also demonstrate superior performance.
Another embodiment of the invention provides a stable O/W emulsion fuel comprising 100 parts of super-heavy oil, 30-80 parts, and preferably 33-50 parts of water, 0.05-4 parts of nonionic surface activating agent having an HLB value of 9-19, and preferably 12-17, which is selected from those defined in (I)-(VII) above, and 0.003-1 part, and preferably 0.01-0.1 part of a naturally-occurring hydrophilic polymer substance defined in (A)-(D) below, and/or 0.01-1 part of a water-soluble synthetic polymer defined in (a)-(f) below.

1~3~651 <Naturally-Occurring Hydrophilic Polymer Substances>
(A) Microorganism-Originating Hydrophilic Polymer Substances (Polysaccharides) (a) Xanthan Gum (b) Bluran (c) Dextran (B) Plant-Originating Hydrophilic Polymer Substances (Polysaccharides) (a) Kelp-originating (1) Agar (2) Galaginan (3) Phaseleran (4) Arginate and its salts (Na, K, NH4, Ca, Mg) (b) Seed-originating (1) Locust Bean Gum (2) Gua Gum (3) Fatsia Gum (4) Tamarind Gum (c) Tree-originating (Sap) (1) Arabian Gum (2) Karaya Gum (3) Tragacanth Gum 133g~1 td) Fruit-originating (1) Pectin (C) Animal-Originating Hydrophilic Polymer Substances (Proteins) (1) Gelatin (2) Casein (D) Natural Polymer Derivatives (1) Cellulose derivatives (such as carboxymethylcellulose) (2) Processed starch <Hydrophilic Synthetic Polymers~
The following describes water-soluble synthetic polymers which increase viscosity when dissolved in water.
(a) Homopolymers of acrylate and its derivatives as well as copolymers of other monomers.
/ R

\ Co2M n where R: H, methyl, ethyl M: H, Na, K, Li, NH4 ~Rl Z:-CH2-C- and monomers which can copolymerize with this monomer and its salts (NH4, Na, K, Li).
Examples include maleic acid (anhydride), itaconic acid (anhydride), ~-olefins, acrylamide, vinylsulfonate, allylsulfonate, methallylsulfonate, acrylamide methylpropylsulfonate and its salts (NH4, Na, K), and dialkyl(methyl or ethyl)ethylaminomethacrylate and its salts (chlorine, diethylsulfate, dimethylsulfate).
n: 50-100,000 (b) Copolymers of acrylamide and other monomers which can copolymerize with its derivatives.

CO n NH
R
where R: H, CH2CH2OH
Z:_CH2-CH- and monomers which can be polymerized with CO this monomer, and their salts (NH4, Na, K, Li).
lNH
R
Examples include vinylsulfonate, allylsulfonate, methallylsulfonate, acrylamide methylpropylsulfonate, dialkyl(methyl or ethyl)ethylaminomethacrylate, ~-olefins 1 3~65~

(C2-C18) and vinylallyl alcohols.
n: 50-100,000 (c) Salts of copolymers of maleic anhydride, itaconic anhydride and other monomers that can copolymerize. The salt includes that with ammonium, potassium and sodium.

tM~ Z--where M: Maleic anhydride, itaconic anhydride Z: ~-olefins (ethylene, propylene, butylene, isobutylene, octene, decene, dodecene, etc.), styrene n: 50-100,000 (d) Homopolymers and copolymers of vinyl alcohol.

~ OH / nwhere Z: Vinyl acetate, styrene n: 30-100,000 (e) Homopolymers and copolymers of vinylpyrrolidone.
t t N
n / \ O
CH2 C ~
CH2_CH2 ~3~6~.

where Z: Monomers which can copolymerize with vinylpyrrolidone and their salts (NH4, Na, K, Li).
Examples include acrylamide, vinylsulfonate, methallylsulfonate, maleic anhydride, itaconic anhydride, styrene and ~-olefins (C2-C18).
n: 50-100,000 (f) Polyethyleneoxide (PEO) with a molecular weight of 10,000-3,000,000, and preferably 20,000-1,000,000.

It is preferable to use naturally-occurring hydrophilic polymer substances so that 0.003-1 part, and preferably 0.01-0.1 part are contained in 100 parts of super-heavy oil, and use hydrophilic synthetic polymers so that 0.01-1 part are contained in 100 parts of super-heavy oil. If the amount that is added is excessive, since the viscosity of the system will be too high and since this is also economically disadvantageous, it is desirable to demonstrate effectiveness with as small an amount as possible. From among the hydrophilic polymer substances indicated above, xanthan gum is especially superior such that superior performance will be exhibited with the addition of a small amount.

6 ~ 1 When anionic surface activating agent is further added to the nonionic surface activating agent - hydrophilic polymer substance and/or aqueous synthetic polymer system, a super-heavy oil emulsion fuel results with even greater long-term stability. The anionic surface activating agents indicated in (i)-(vii) above are typical examples of the anionic surface activating agent of this invention.
From among the anionic surface activating agents indicated above, (i) and (ii) exhibited superior performance overall.
When the powerful protective action of the hydrophilic polymer substance is added to the action of the anionic and nonionic surface activating agents, the super-heavy oil emulsion fuel becomes a stable system at low viscosity for an extended period of time.
For systems which use anionic surface activating agent, nonionic surface activating agent and a hydrophilic polymer substance, as well as for systems which use a nonionic surface activating agent and a hydrophilic polymer substance, these can either be used by blending together in advance or used separately. In addition, although these can be added to either water or oil, adding to water results in ~ 3 ~

easier handling.
In regard to mechanical methods for preparing the emulsion fuel, as long as an efficient stirring method is used, any method of this type is satisfactory, and two or more methods may be combined. High-shearing types of stirring devices are particularly desirable. Examples of these include line mixers, arrow blade turbine blade mixers, propeller blade mixers, full margin type blade mixers and paddle blade mixers. High shearing refers to shearing of llOO/sec. or greater, and preferably a range of 4000-30,000/sec.
The action of anionic surface activating agents involves adsorbing onto the interface of the particles of the super-heavy oil thereby giving an electrical charge to the particles while simultaneously assisting in reducing the size of the particles resulting in prevention of aggregation of the particles. Although nonionic surface active agents are strongly susceptible to the effects of temperatuare, when anionic surface active agents are added, the effects of temperature are weakened resulting in improved storage stability of the emulsion. In addition, storage stability is further improved by adding the action 1 339 (DS-I

of a hydrophilic polymer substance.
In the case of anionic surface activating agent alone, although the viscosity of the system decreases, storage stability is worsened. Similarly, in the case of nonionic surface activating agent alone, viscosity increases with time since such agents are strongly susceptible to the effects of temperature and as such, an emulsion fuel that is stable for an extended period of time cannot be prepared.
However, when anionic surface activating agent and nonionic surface activating agent are used in combination, a stable emulsion fuel can be obtained. The weight ratio of anionic surface activating agent and nonionic surface activating agent (anionic surface activating agent / nonionic surface activating agent) which demonstrate superior performance is 1/99-75/25, and preferably 10/90-40/60. An added amount of anionic surface activating agent of 0.005-2.2 parts to 100 parts of emulsion fuel is preferable, and 0.06-0.61 parts is more preferable.
The oil which is referred to as super-heavy oil in this invention includes the oils indicated below which have a high viscosity at room temperature and do not flow unless heated to high temperatures.

1~3965~

(1) Petroleum-based asphalts as well as its mixtures.
(2) Various types of treated petroleum-based asphalt, their intermediate products, residues and oil mixtures.
(3) High fluid point oils or crude oils which do not flow at room temperature.
(4) Petroleum-based tar pitch as well as its mixtures.

(5) Bitumen, oil sand and natural asphalt.

Brief Description of Drawings Fig. 1 is a schematic view of a centrifuge tube used in evaluation of the dispersion state after allowing to stand undisturbed.
1: Surface Layer 2: Intermediate Layer 3: Sedimentation Layer Examples The following describes examples of this invention, this invention is not limited to these examples.

Example 1 A specific amount of Middle East type asphalt softening temperature; 50~C) or Asabaska bitumen (sof~ening 1~96~

temperature: 12.5~C), water and surface activating agent were weighed so as to total 300g. This mixture was then placed in an 800ml centrifuge tube and heated to 75~C.
After reaching a constant temperature, the mixture was stirred with a TX Homomixer*(Tokushu Kikako Ltd., equipped with low viscosity stirring blades) to prepare the emulsion fuel. This was then maintained at a temperature of 60~C.
After reaching a constant temperature, the viscosity was measured. A portion of the emulsion fuel was maintained at a temperature of 50~C and observed after 1 day, 7 days, 21 days, 1 month and 3 months. A portion was removed and the amount that passed through a 100 mesh strainer was measured.
Viscosity measurements were made using a Vismetron*Model VS-AI No. 2 (Shibaura Systems Co., Ltd.) at a rotor speed of 60 rpm and the amount that passed through the strainer was determined by placing approximately lOg of the sample on a ~70mm, 100 mesh stainless steel strainer in a 50~C
atmosphere and calculating the amount remaining in the strainer after 10 minutes. Those results àre indicated in Table 1.
Furthermore, overall evaluation was made by comprehensively evaluating viscosity of the emulsion, amount *Trade-mark 133~51 that passed through the strainer, and visual observation of the dispersion state after the emulsion was allowed to stand. Evaluation was made using the symbols ~ >O>~>X with an evaluation of ~ of better being recognized as at least demonstrating some degree of effectiveness.
However, in the case of the dispersion state after standing, evaluation was made by observing the three layers consisting of the surface layer 1, intermediate layer 2 and se~imentation layer 3 as indicated in Fig. 1 and evaluating each of the respective surface layer, intermediate layer and sedimentation layer separately.
In surface layer 1, the size of the oil droplets on the surface were observed as well as the size of the oil film that formed when these were large. Dispersion state was evaluated in the order of no oil droplets > some oil droplets > small oil film > large oil film with no oil droplets indicating the most satisfactory evaluation.
In intermediate layer 2, the quality of the emulsification state was observed. Evaluation was made in the order of good emulsification > slightly creamy >
creamy > separated > major separation > complete separation with good emulsification indicating the most satisfactory evaluation.
In sedimentation layer 3, evaluation was made in the order of no sediment > soft sediment > hard sediment with no sediment indicating the most satisfactory evaluation. Soft sediment refers to sediment that is soft and can be redispersed easily. Hard sediment refers to sediment that is hard and for which redispersion is difficult.

Example 2 A specific amount of Asabaska bitumen (softening temperature: 12.5~C, Canada), water and each of the surface activating agents indicated in Table 2 were weighed so as to total 300g. This mixture-was then placed in an 800ml centrifuge tube and heated to 45~C. After reaching a constant temperature, the mixture was stirred with a TK
Homo~ixer, equipped with low viscosity stirring blades, to prepare the emulsion fuel. This was then placed in a 40~C
constant temperature bath. After reaching a constant temperature, the viscosity was measured. A portion of the emulsion fuel was maintained at a temperature of 40~C and its state was observed after 1 day, 3 days and 7 days. A
portion was removed and the amount that passed through a 100 mesh strainer was measured. Viscosity measurements were ià3S~

made using a Vismetron Model VS-AI No. 2 (Shibaura Systems Co., Ltd.) at a rotor speed of 60 rpm and the amount that passed through the strainer was determined by placing approximately lOg of the sample on a ~70mm, 100 mesh stainless steel strainer in a 40~C atmosphere and calculating the amount r~m~i~ing in the strainer after 10 minutes. Those results are indicated in Table 1. Further, overall evaluation and observation of the dispersion state were performed with the same methods as in Example 1-.

Example 3 A specific amount of Middle East type asphalt (softening temperature: 50~C), water, surface activating agent, hydrophilic polymer substance and/or aqueous synthetic polymer substance were weighed so as to total 300g. This mixture was then placed in an 800ml centrifuge tube and heated to 75~C. After reaching a constant temperature, the mixture was stirred with a TK Homomixer (Tokushu Kikako Ltd., equipped with low viscosity stirring blades) to prepare the emulsion fuel. This was then maintained at a temperature of 60~C. After reaching a constant temperature, the viscosity was measured. A portion *Trade-mark ~333~1 of the emulsion fuel was maintained at a temperature of 50~C
and observed after 1 day, 7 days, 21 days, 1 month and 3 months. A portion was removed and the amount that passed through a lO0 mesh strainer was measured. Viscosity measurements were made using a Vismetron Model VS-AI No. 2 (Shibaura Systems Co., Ltd.) at a rotor speed of 60 rpm and the amount that passed through the strainer was determined by placing approximately lOg of the sample on a ~70mm, 100 mesh stainless steel strainer in a 50~C atmosphere and calculating the amount rem~i~ing in the strainer after 10 minutes. Those results are indicated in Table 3. Further, overall evaluation and observation of the dispersion state were performed with the same methods as in Example l.

Example 4 A specific amount of Asabaska bitumen (softening temperature: 12.5~C, Canada), water, surface activating agent, hydrophilic polymer substance and/or aqueous synthetic polymer substance were weighed so as to total 300g. This mixture was then placed in an 800ml centrifuge tube and heated to 40~C. After reaching a constant temperature, the mixture was stirred with a TK Ho-momixer (Tokushu Kikako Ltd.) to prepare the emulsion fuel. This 1~3565:~

was then placed in a 40~C constant temperature bath. After reaching a constant temperature, the viscosity was measured.
A portion of the emulsion fuel was maintained at a temperature of 40~C and its state was observed after 1 day, 7 days, 21 days, 1 month and 3 months. A portion was removed and the amount that passed through a 100 mesh strainer was measured. Viscosity measurements were made using a Vismetron Model VS-AI No. 2 (Shibaura Systems Co., Ltd.) at a rotor speed of 60 rpm and the amount that passed through the strainer was determined by placing approximately lOg of the sample on a ~70mm, 100 mesh stainless steel strainer in a 40~C atmosphere and calculating the amount remaining in the strainer after 10 minutes. Those results are indicated in Table 4. Further, overall evaluation and observation of the dispersion state were performed with the same methods as in Example 3.

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Claims (17)

1. An O/W type low viscosity emulsion fuel consisting essentially of super-heavy oil, 30-80 parts by weight of water per 100 parts by weight of the super-heavy oil, 0.01-4 parts by weight of at least one anionic surface active agent selected from the group (i)-(vii) defined hereinunder per 100 parts by weight of the super-heavy oil, and at least one nonionic surface active agent having an HLB of 9-19 and selected from the group consisting of (I)-(VII) defined hereinunder at a weight ratio of the anionic surface active agent / the nonionic surface active agent of 1/99-75-25:
(i) formalin condensation products of sulfonic acid or sulfonate salts of cyclical aromatic compounds selected from the group consisting of naphthalene, alkylnaphthalene, alkylphenol and alkylbenzene, in which the average degree of condensation of formalin is 1.2-100 and the salts are ammonium, lower amine, alkali metal or alkaline earth metal salts;
(ii) formalin condensation products of lignosulfonate or lignosulfonate salts and formalin condensation products of lignosulfonate and sulfonates of aromatic compounds, in which the salts are ammonium, lower amine, alkali metal or alkaline earth metal salts and the average degree of condensation of formalin is 1.2-50, (iii) copolymers and their salts of polystyrene sulfonic acid having a molecular weight of 500-500,000, in which the salts are ammonium, lower amine, alkali metal or alkaline earth metal salts;

53a (iv) dicyclopentadiene sulfonate polymers having a molecular weight of 500-500,000 and their salts in which the salts are ammonium, lower amine, alkali metal or alkaline earth metal salts;
(v) copolymers of an unsaturated dicarboxylic anhydride and a copolymerizable monomer, their corresponding acids and salts, wherein the unsaturated dicarboxylic anhydride is maleic anhydride or itaconic anhydride, the copolymerizable monomer is olefin, styrene, vinyl acetate, methacrylate or acrylate and the salts are ammonium or alkali metal salts;
(vi) liquid polybutadiene modified with maleic anhydride and its salts in which the liquid butadiene has a molecular weight of 500-200,000 and the salts are ammonium or alkali metal salts;
(vii) the following anionic surface activate agents having 1 or

2 hydrophilic groups within the same molecule;
(a) sulfuric ester salts of alcohols having 4-18 carbon atoms in which the salts are lower amine, ammonium, alkali metal or alkaline earth metal salts;
(b) alkane, alkene or alkylaryl sulfonates or their salts having 4-18 carbon atoms in which the salts are lower amine, ammonium, alkali metal or alkaline earth metal salts;
(c) sulfates or phosphate esters and their salts of alkylene oxide addition products of compounds having 1 or more activated hydrogens within the same molecule wherein the salts are ammonium, potassium, magnesium, alkali metal or alkaline earth metal salts;

(d) sulfosuccinate salts which are esters of saturated or unsaturated fatty acids having 4-22 carbon atoms in which the salts are ammonium, sodium or potassium;
(e) alkyldiphenylether disulfonates and their salts, in which the alkyl groups have 8-18 carbon atoms and the salts are ammonium, sodium, potassium, magnesium or calcium;
(f) rosin acids and their salts in which the salts are ammonium, sodium and potassium;
(g) alkane or alkene fatty acids having 4-18 carbon atoms and their salts in which the salts are ammonium, potassium or sodium;
(I) alkylene oxide addition products of compounds having phenolic hydroxyl groups, in which the alkylene oxide is ethylene oxide, propylene oxide, butylene oxide or styrene oxide;
(II) alkylene oxide addition products of formalin condensation products of compounds having phenolic hydroxyl groups, in which the condensation degree is 1.2-100 and the alkylene oxide is ethylene oxide, or propylene oxide, butylene oxide or styrene oxide;
(III) alkylene oxide addition products of monovalent aliphatic alcohols or aliphatic amines having 2-50 carbon atoms, in which the alkylene oxide is ethylene oxide, or propylene oxide, butylene oxide or styrene oxide;

(IV) block or random addition polymers of at least two oxides selected from the group consisting of ethylene oxide, propylene oxide, butylene oxide and styrene oxide;
(V) alkylene oxide addition products of polyvalent alcohols or esters of the polyvalent alcohols and fatty acids having 8-18 carbon atoms, wherein the alkylene oxide is ethylene oxide, propylene oxide, butylene oxide or styrene oxide;
(VI) alkylene oxide addition products of polyvalent amines having at least two active hydrogen atoms, wherein the alkylene oxide, propylene oxide, butylene oxide or styrene oxide; and (VII) products resulting from the addition of an alkylene oxide to a mixture of 1 mole of triglyceride-type oil and 0.1 to 5 moles of at least one type of polyvalent alcohols selected from the group consisting of glycerine, trimethylolpropane, pentaerythritol, sorbitol, sucrose, ethylene glycol, polyethylene glycol having a molecular weight of 1,000 or less, propylene glycol, and polypropylene glycol having a molecular weight of 1,000 or less, or 0.1-5 moles of water, wherein the alkylene oxide is ethylene oxide, propylene oxide, butylene oxide or styrene oxide.

2. An O/W type emulsion fuel consisting essentially of:
super-heavy oil, 30-80 parts by weight of water, 0.05-4 parts by weight of at least one nonionic surface active agent (I)-(VII) described in claim 1, and at least one member selected from the group consisting of:
0.003-1 part by weight of a naturally-occurring hydrophilic polymer substance defined in (A)-(D) hereinunder, and 0.01-1 part by weight of a hydrophilic synthetic polymer defined in (a)-(f) hereinunder, each per 100 parts by - 56a -weight of the super-heavy oil:
(A) microorganism-originating hydrophilic selected from the group consisting of:
(a) xanthan gum, (b) bluran, and (c) dextran;
(B) plant-originating hydrophilic polysaccharides selected from the group consisting of:
(a) kelp-originating polymer substances selected from the group consisting of:
(1) agar, (2) galaginan, (3) phaseleran, and (4) arginate and its Na, K, NH4, Ca or Mg salt;
(b) seed-originating polymer substances selected from the group consisting of:
(1) locust bean gum, (2) gua gum, (3) fatsia gum, and (4) tamarind gum;
(c) tree-originating polymer substances selected from the group consisting of:
(1) arabian gum, (2) karaya gum, and (3) tragacanth gum;
(d) fruit-originating polymer substance being (1) pectin;

(C) animal-originating hydrophilic proteins selected from the group consisting of:
(1) gelatin, and (2) casein; and (D) national polymer derivatives selected from the group consisting of:
(1) cellulose derivatives, and (2) processed starch;
(a) acrylate polymers represented by the formula:

[wherein R is H, methyl or ethyl;

M is H, Na, K, Li or NH4;

Z is or a monomer selected from the group consisting of:
maleic acid, maleic anhydride, itaconic acid, itaconic anhydride, .alpha.-olefin, acrylamide, vinylsulfonate, allylsulfonate, methallylsulfonate, acrylamide methylpropylsulfonate and their NH4, Na or K salts and dilower-alkylethylaminomethacrylate and its chlorine, diethylsulfate or dimethylsulfate salt; and n is 50-100,000];
(b) acrylamide polymers represented by the formula:

[wherein R is H or CH2CH2OH;

Z is or a monomer selected from the group consisting of vinylsulfonate, allysulfonate, methallylsulfonate, acrylamide methylpropylsulfonate, dilower-alkylethylamino-methacrylate, .alpha.-olefin having 2-18 carbon atoms and vinylallyl alcohol; and n is 50-100,000];
(c) salts of copolymers of the formula:

[wherein M is a unit derived from maleic anhydride or itaconic anhydride;
Z is a unit derived from .alpha.-olefin having 2 to 12 carbon atoms or styrene; and n is 50-100,000], wherein the salts are ammonium, potassium or sodium salts;
(d) vinyl alcohol polymers of the formula:

[wherein Z is vinyl acetate or styrene; and n is 30-100,000];
(e) polymers of vinylpyrrolidone of the formula:

[wherein Z is a unit derived from monomers selected from the group consisting of acrylamide, vinylsulfonate, methallylsulfonate, maleic anhydride, itaconic anhydride, styrene and C2-C18 .alpha.-olefins and their NH4, Na, K or Li salts; and n is 50-100,000]; and (f) polyethyleneoxide having a molecular weight of 10,000-3,000,000.

3. A super-heavy oil emulsion fuel as described in claim 2 which comprises 0.005-4 parts by weight of the anionic surface active agent described in claim 1 per 100 parts by weight of super-heavy oil, in addition to the nonionic surface active agent.

4. A super-heavy oil emulsion fuel as described in claim 2 or 3, in which the hydrophilic polymer substance is xanthan gum and the amount of xanthan gum is 0.01-0.1 parts by weight per 100 parts by weight of the super-heavy oil.

5. A super-heavy oil emulsion fuel as described in claim 1, 2 or 3, in which the HLB of the nonionic surface active agent is from 12-17.

6. A super-heavy oil emulsion fuel as described in claim 1, 2 or 3, in which the super-heavy oil has a softening point of 50°C or lower.

7. A super-heavy oil emulsion fuel as described in claim 1 or 3, in which the weight ratio of the anionic surface active agent to the nonionic surface active agent is from 10:90 to 40:60.

8. A super-heavy oil emulsion fuel as described in claim 1, 2 or 3, in which the nonionic surface active agent is (VII) as described in claim 1.

9. A super-heavy oil emulsion fuel as described in claim 1 or 3, in which the anionic surface active agent is (i) or (ii) as described in claim 1.

10. A super-heavy oil emulsion fuel as described in claim 1 or 3, in which the anionic surface active agent is (i) or (ii) as described in claim 1, and the nonionic surface active agent is (VII) as described in claim 1.

11. A super-heavy oil emulsion fuel as described in claim 2 or 3, in which the nonionic surface active agent is (VII) of (II) or (III) as described in claim 1, and the hydrophilic polymer substance is xanthan gum as described in claim 2.

12. A super-heavy oil emulsion fuel as described in claim 1, 2 or 3, in which the amount of water is 33-50 parts per 100 parts by weight of the super-heavy oil.

13. A super-heavy oil emulsion fuel as described in claim 1, 2 or 3, in which the super-heavy oil has a high viscosity at room temperature and does not flow unless heated to high temperatures and is selected from the group consisting of petroleum-based asphalt, crude oil, petroleum-based tar pitch, bitumen, oil sand and natural asphalt.

14. An O/W type low viscosity emulsion fuel consisting essentially of:
a super-heavy oil which itself does not flow at room temperature due to high viscosity and is selected from the group consisting of petroleum-based asphalt, crude oil, petroleum-based tar pitch, bitumen, oil sand and natural asphalt;
30 to 50 parts by weight of water per 100 parts by weight of the super-heavy oil;
0.01 to 2.2 parts by weight of an anionic surface active agent per 100 parts by weight of the super-heavy oil; and a nonionic surface active agent in such an amount that the weight ratio of the anionic surface active agent /
nonionic surface active agent is from l/99 to 75/25, wherein:
the said anionic surface active agent is a member selected from the group consisting of ammonium, lower amine, alkali metal or alkaline earth metal salt of lignosulfonate, formalin condensate of lignosulfonate, formalin condensate of naphthalene sulfonate, formalin condensate of cresol sulfonate, or formalin condensate of butylnaphthalene sulfonate, and the said nonionic surface active agent has an HLB 9-19 and is selected from the group consisting of polyoxyethylene nonylphenyl ether, ethylene oxide adduct of nonylphenol formalin condensate, polyoxyethylene monovalent aliphatic C12-C20 alcohol, polyoxyethylene sorbitan C8-C18 fatty acid ester, polyoxypropylene polyoxyethylene block copolymer, ethylene oxide and propylene oxide block copolymer of tetraethyleneamine, and ethylene oxide adduct of a mixture of 1 mole of triglyceride oil and 0.1 to 5 moles of glycerin.

15. The emulsion fuel as described in claim 14, wherein the amount of the nonionic surface active agent is 0.05 to 4 parts by weight per 100 parts by weight of the super-heavy oil and the fuel also comprises 0.003 to 1 part by weight of xanthan gum per 100 parts by weight of the super-heavy oil.

16. The emulsion fuel as described in claim 14 or 15, wherein the anionic surface active agent is sodium lignosulfonate and the nonionic surface active agent is an ethylene oxide adduct of a mixture of 1 mole of beef tallow and 0.1 to 5 moles of glycerin.

17. An 0/W type viscosity emulsion fuel consisting essentially of:
[A] super-heavy oil;
[B] 30-80 parts by weight of water per 100 part by weight of the super-heavy oil;

- 63a -[C] a nonionic surface active agent having an HLB
value of 9-19 and being selected from those defined in (I)-(VII) in claim 1; and [D] either (i) an anionic surface active agent selected from those defined in (i)-(vii) in claim 1, or (ii) at least one member selected from the group consisting of a naturally-occurring hydrophilic polymer substance defined in (A)-(D) in claim 2 and a hydrophilic synthetic polymer defined in (a)-(f) in claim 2, wherein:
when the component [D] is the anionic surface active agent (i), the amount of the anionic surface active agent is 0.01-4 parts by weight per 100 parts by weight of the super-heavy oil and the amount of the nonionic surface active agent is such that an anionic surface active agent/nonionic surface active agent weight ratio is 1/99-75/25, and when the component [D] is other than the anionic surface active agent, the amounts of the nonionic surface active agent, the naturally-occurring hydrophilic polymer substance and the hydrophilic synthetic polymer are 0.05-4, 0.003-1 and 0.01-1 part, respectively, each by weight per 100 parts by weight of the super-heavy oil.