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Patent Number/Link: 
5,725,613 Method to reduce oxidative deterioration of bulk materials

5,725,613

Mar. 10, 1998

United States Patent [19]

Reeves et al.

[54] METHOD TO REDUCE OXIDATIVE

DETERIORATION OF BULK MATERIALS

[75] Inventors: Robert A. Reeves. Arvada; Mark H.

Berggren. Golden; Charlie W.

Kenney. Littleton, all of Colo.

[73] Assignee: Hazen Research, Inc. Golden. Colo.

[21] AppL No.: 677,637

[22] Filed: Jul. 8, 1996

[51] Int. Cl.6 CI0L 9/00

[52] U.S. Cl 44/501; 44/591; 44/592;

44/620

[58] Field of Search 441501, 620

1111111111111111111111111111111111111111~lllllllllllmlI1IIIII1II

US005725613A

[11] Patent Number:

[45] Date of Patent:

OTHER PUBLICATIONS

Edwards. 1995. Catalysis Today, 23:59-66.

Keirn. "Industrial Uses of Carbon Dioxide". in Carbon

Dioxide as a Source ofCarbon, M. Aresta and G. Forti. eds..

D. Reidel Publishing Co.• 1987.23-31.

Rigsby et al.. "Coal self-heating: problems and solutions".

pp. 102-106.

Riley et aL. J. Coal Quality, Apr. 1987. pp. 64-67.

RipP. "Understanding coal pile hydrology can help BTU

loss in stored coal". pp. 146-150.

Sapienze et al.. "Carbon DioxidelWater for Coal Beneficiation".

in Mineral Matter and Ash in Coal, 1986 America

Chemical Society. pp. 50D-512.

Primary EXaminer-Ellen M. McAvoy

Attome)\ Agent, or Firm-Sheridan Ross P.C.

[56] References Cited [57] ABSTRACT

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4,599,250

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4,828,575

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5,087,269

U.S. PATENT DOCUMENTS

4/1966 Ellman et aI 3419

4/1978 Das 44/620

10/1979 Smith 44/1

8/1983 Li et aI. 44/1

8/1983 Bonnecaze 44/1

4/1985 Nakamura et aI 44/501

711986 Cargle et aI 4271220

9/1986 Chiang et aI 209/5

3/1987 Yan 44/1

1/1989 Siddoway et aI 44/501

5/1989 Bellow, Jr. et aI. 44/501

5/1989 Bixel et aI 44/501

2/1992 Clta et aI 44/501

Disclosed is a method to reduce oxidative deterioration of

bulk materials. Preferred embodiments of bulk materials

include solid fuel materials. such as coal. and bulk food

products. The method includes contacting a bulk material

with a heat transfer medium to reduce the temperature of the

bulk material below ambient temperature. and preferably

below about 100 C. In this manner, the rate of oxidation is

sufficiently low so that significant losses, such as the loss of

thermal values in of fuel material. are avoided. The heat

transfer medium can be solid or fluid and in a preferred

embodiment is liquid carbon dioxide or liquid nitrogen.

42 Claims, No Drawings

5,725,613

2

DEfAll..ED DESCRIPTION

The method includes directly contacting the bulk material

with a heat transfer medium to reduce the temperature of the

bulk material below an ambient temperature. In a preferred

embodiment. the temperature of the bulk material is reduced

5 to below about 10° C. In this manner. significant oxidative

deterioration of the bulk material is avoided. In the instance

of a solid fuel material. for example. loss of the thermal

value of the solid fuel material is reduced because the rate

of oxidative deterioration significantly slows with cooler

10 temperatures. Significant reductions in the rate of loss of

heating value can be attained for solid fuel material. For

example. fuel materials treated with the method of the

present invention can have a rate of loss of heating value of

less than about 0.5% per month.

The heat transfer medium can be solid. liquid or gas and

is substantially inert to the bulk material. In preferred

embodiments. the heat transfer medium can be carbon

dioxide. carbon monoxide. helium. nitrogen. argon or air. In

preferred embodiments. the heat transfer medium is carbon

20 dioxide or nitrogen. in particular. liquid and solid carbon

dioxide and liquid nitrogen.

The present invention includes conducting the process of

contacting a bulk material with a heat transfer medium at a

variety of times throughout the product life of the bulk

25 material. For example. the process can be conducted during

time periods when the bulk material is subject to a high

degree of mixing such as during size reduction steps and/or

loading or Unloading of the bulk material. In an alternative

embodiment. the step of contacting the bulk material with

30 the heat transfer medium can be conducted while the bulk

material is in a static state. such as in a storage pile.

Further embodiments of the present invention include

compositions which have been produced by conducting the

35 method of the present invention. Such compositions. for

example. include bulk materials in direct contact with a heat

transfer medium having temperatures within ranges according

to the method of the present invention.

The present invention concerns a method to reduce oxidative

deterioration of bulk materials. The term "bulk materials"

refers to any solid materials which are produced.

shipped and/or stored in quantities measured on a tonnage

basis. and preferably includes oxidizable and highly reactive

materials. Bulk materials can include solid fuel materials.

bulk food products. sulfide ores and carbon containing

materials. such as activated carbon and carbon black.

Solid fuel material. as used herein. generally refers to any

solid material which is combusted for some useful purpose.

More particularly. solid fuel materials can include coal.

upgraded coal products. and other solid fuels. The term coal

includes anthracite. bituminous coal. sub-bituminous coal

and lignite. The present invention is particularly suited for

55 bituminous coal. sub-bituminous coal and lignite. The term

upgraded coal product includes thermally-upgraded coal

products. coal products produced by beneficiation based

upon specific gravity separation. mechanically cleaned coal

products. and sized coal products such as stoker. breeze.

60 slack and fines. The present invention is particularly suited

for thermally-upgraded coal because of significantly

increased risk of oxidative deterioration and/or self-ignition.

Thermally upgraded products are likely to have a higher rate

of oxidation because of formation of reactive components

65 which increases the rate of oxidation. In addition. such

materials typically have had water removed to a significant

extent. If such materials are subsequently exposed to humid

BACKGROUND OF THE INVENTION

1

METHOD TO REDUCE OXIDATIVE

DETERIORATION OF BULK MATERIALS

FIELD OF THE INVENTION

The present invention relates to a method and composition

for reducing the oxidative deterioration of bulk materials.

In particular. the invention relates to reduction of

oxidative deterioration of solid fuel materials. such as coal.

When bulk materials contact the ambient environment.

they are subject to oxidative deterioration because of contact

with oxygen in air. Such oxidative deterioration can have

many negative effects. For example. when a solid fuel

material. such as coal. is being transported from a mine to a 15

utility or is in storage at a utility. it is subject to oxidation.

One negative aspect of such oxidative deterioration is a loss

in the thermal value of the coal. Depending on the type of

coal and its water content. among other factors. between 1%

and 5% of the thermal value of coal can be lost from the time

it is mined until the time at which it is consumed. These

losses are sizeable in the domestic United States utility

industry which consumes about 800 million tons of coal per

year. Such losses are particularly significant for low rank

coals such as lignite and sub-bituminous coals. especially

for such materials which have been upgraded by thermal

treatment to reduce moisture.

Moreover. low level oxidation of coal generates heat and

as such a reaction progresses. there is a significant risk of

certain coal materials self-igniting. resulting in a risk to

property and life.

Most efforts to reduce oxidative deterioration have

focused on reducing the risk of self-heating and thereby

self-ignition of coals. The problem has been addressed by a

variety of approaches. One such approach is by compacting

coal as it is transported or stored. By compacting coal.

significant reductions in coal surface area which contact the

ambient environment can be attained. Such a reduction of

surface area contact reduces the amount of coal available for 40

oxidation by the ambient environment Another approach

has been to flatten and trim coal piles to decrease the ability

of the coal pile to hold heat and therefore generate enough

heat through self-heating to self-ignite. In addition. contacting

coal materials with various fluids. such as hydrocarbon- 45

based materials. has been used.

While the more chronic problem of loss of economic

value of bulk materials. such as the loss of heating values in

coal. has been recognized and studied. adequate widespread

use of strategies for significantly reducing economic losses 50

from this problem have not been achieved. Therefore. a need

exists for reducing the oxidative deterioration of bulk materials.

SUMMARY OF THE INVENTION

The present invention includes a method to reduce oxidative

deterioration of bulk materials. particularly including

oxidizable and highly reactive bulk materials. In preferred

embodiments. the bulk materials in question include solid

fuel materials. bulk food products. sulfide ores and carbon

containing materials such as activated carbon and carbon

black. In further preferred embodiments. the solid fuel

material can be coal. upgraded coal products. oil shale. solid

biomass materials. refuse-derived (including municipal and

reclaimed refuse) fuels. coke. char. petroleum coke.

gilsonite. distillation by-products. wood by-product wastes.

shredded tires. peat and waste pond coal fines.

5,725.613

3 4

sidered. For example. warm air may be overly reactive with

some bulk materials. such as coal, but if the heat transfer

medium is cold air (e.g.. 4° C.). the degree of reactivity with

the coal may be acceptably low to be considered nonoxidizing.

Preferably, to be considered non-oxidizing. the

heat transfer medium of the present invention should not

oxidize the product or cause the product to become more

reactive to oxygen at a time subsequent to treatment with the

heat transfer medium. In a further embodiment. the heat

transfer medium can be inert (i.e.. non-reactive) to the bulk

material.

The heat transfer medium needs to be sufficiently cold so

that the temperature of the bulk material. prior to contact

with the heat transfer medium. can be reduced to within the

appropriate temperature range after contact. In a preferred

embodiment. the temperature of the heat transfer medium

prior to contact with the bulk medium is less than about -30°

C.. more preferably less than about -50° C. and most

preferably less than about -70° C.

The heat transfer medium can comprise carbon dioxide,

carbon monoxide, helium. nitrogen, argon. or air. More

preferably, the heat transfer medium can comprise carbon

dioxide, carbon monoxide. nitrogen or argon. In a preferred

embodiment, the heat transfer medium can comprise either

nitrogen or carbon dioxide. In a further preferred

embodiment, the heat transfer medium can comprise liquid

or solid carbon dioxide or liquid nitrogen. It will be recognized

that for a liquid or solid heat transfer medium which

is a gas at ambient temperatures of the bulk material, as the

heat transfer medium heats up, it will change phase to

become a gas. Such an evolution of gas over time, such as

the evolution of carbon dioxide gas from solid carbon

dioxide. has the benefit of excluding oxygen from contacting

the bulk material.

It will be appreciated that in the instance of a solid heat

transfer medium. smaller particle sizes will allow more

uniform cooling than for larger particle sizes. In the instance

of a solid heat transfer medium, the particle size of the

medium is preferably less than about 5 millimeter, more

preferably less than about 3 millimeter and most preferably

less than about 0.5 millimeter.

The step of contacting includes bringing the heat transfer

medium and the bulk material into sufficiently intimate

contact such that the bulk material is cooled to the desired

temperature. By contacting the bulk material directly with

the heat transfer medium. the heat transfer which occurs to

cool the bulk material is more efficient than through an

indirect heat transfer. Since the heat transfer medium is not

50 confined within, for example. tubes of a heat exchanger, a

more complete, effective and uniform cooling of the bulk

material can be achieved. Specific preferred methods for

contacting the heat transfer medium with the bulk material

are described in detail below.

It will be understood that the amount of heat transfer

medium needed to cool a given amount of bulk material will

depend on various factors, including the relative temperatures

of each. However, in a preferred embodiment. the

amount of heat transfer medium to be contacted with a bulk

material will be between about 0.5 and about 10 weight

percent. more preferably between about 1 and about 5

weight percent and even more preferably between about 1

and about 2 weight percent based on the weight of the bulk

material.

The step of contacting a bulk material with a heat transfer

medium of the present invention is preferably conducted

substantially in the absence of water. It will be recognized

environments, the materials will rewet thereby generating

heat through the heat of hydration.

Examples of other solid fuels embodied in the present

invention include, but are not limited to, oil shale. solid

biomass materials, refuse-derived (including municipal and 5

reclaimed refuse) fuels, coke. char, petroleum coke,

gilsonite. distillation by-products, wood by-product wastes,

shredded tires, peat and waste pond coal fines. The term

solid biomass can include, for example. wood wastes, agricultural

wastes. and grass. The term refuse-derived fuels can 10

include. for example, landfill material from which noncombustible

materials have been removed.

In one embodiment of the present invention. bulk materials

include bulk food products. Such bulk food products

include food products that tend to deteriorate in storage. 15

Since the food industry has concentrated on preservation of

high-end food products such as meats, dairy and vegetables,

there remains a need in the industry for low cost, effective

preservation of bulk food products such as bulk grains and

related by-products. According to the present invention. bulk 20

food products can include bulk grains. animal feed and

related by-products. Examples of such bulk grains include,

but are not limited to wheat. corn. soybeans, barley, oats, and

any other cereal grain that deteriorates in storage.

25 Examples of other oxidizable and highly reactive solid

bulk materials embodied in the present invention include,

but are not limited to sulfide ores. and carbon containing

materials. such as activated carbon and carbon black.

The present method includes directly contacting the bulk 30

material with a heat transfer medium to reduce the temperature

of the bulk material below ambient temperature. The

term ambient can refer to the temperature of the environment

in which the bulk material is produced. shipped and/or

stored. Alternatively, such term can include the temperature 35

at which the material existed prior to production. For

example. the temperature of coal in the earth is relatively

constant and will vary between about 10° C. and about 16°

C. In a preferred embodiment. the method of the present

invention includes reducing the temperature of the bulk 40

material with a heat transfer medium to below about 10° c..

preferably below about 5° c., more preferably below about

3° c.. and even more preferably between about 0° C. and

about 3° C. According to the present invention. reference to

the temperature of the bulk material can include the tem- 45

perature of an interior. such as the core of the material.

and/or a surface portion of the material. More particularly,

the temperature of the bulk material can refer to the temperature

of a portion of the material which is or can be in

contact with air or oxygen.

The appropriate temperature for cooling a bulk material

by contact with a heat transfer medium pursuant to the

present invention is selected such that unacceptable levels of

oxidative deterioration and/or self-heating are avoided. The

determination of the appropriate temperature may depend on 55

a variety offactors. including the nature of the bulk material,

the available time until consumption (i.e. storage time). the

rate of oxidation of the bulk material at various

temperatures. the cost of the heat transfer medium, and the

effects of extraneous factors on the product such as material 60

handling protocols.

The heat transfer medium of the present invention can be

solid or fluid (i.e.. liquid or gas). The heat transfer medium

is essentially non-oxidizing to the bulk material. It should be

noted that when considering whether the heat transfer 65

medium is non-oxidizing with regard to the bulk material.

the temperature of the heat transfer medium must be con5,725.613

6

In a further preferred embodiment of the present invention

where the heat transfer medium is not air. the step of

contacting the bulk material with a heat transfer medium

displaces ambient air from contact with the bulk material. In

5 this manner. the available oxygen for oxidation of the bulk

material is reduced.

In a further preferred embodiment of the present

invention. the heat transfer medium reacts with the surface

of the solid fuel material to passivate the solid fuel material

10 from oxidation by ambient air. Such a heat transfer medium

can. for instance. form new compounds on the surface of the

solid fuel material such that the surface is inactive. or less

reactive to oxidation by ambient air.

Methods of the present invention. including contacting a

15 bulk material with a heat transfer medium, can be conducted

at any time in the product life of the bulk material in question

to reduce oxidative deterioration in the future. For example.

in the case of solid fuel material such as coal. the step of

contacting can be conducted at any time from when the fuel

20 is removed from the ground or otherwise produced. until it

is ultimately consumed at a utility.

The method of contacting a bulk material with a heat

transfer medium is preferably conducted at a point in the

product life of the bulk material when the bulk material is

25 subject to a high degree of mixing or agitation for some

other purpose. In this manner. efficient contact of the bulk

material with the heat transfer medium can occur without the

added requirement of inducing substantial mixing or agitation

solely for the purpose of contact with the heat transfer

30 medium. In one embodiment. the step of contacting can

occur when the particle size of a bulk material is being

reduced. For example. in the instance of a solid fuel material

such as coal. the step of contacting can be conducted at the

mine at which the coal is recovered. Such a step of contact-

35 ing is advantageously conducted when run-of-mine coal is

initially crushed. As the run-of-mine coal is introduced into

a crusher. a stream of fluid heat transfer medium. preferably

liquid carbon dioxide or liquid nitrogen. can be introduced

at the same time. In this manner because the crusher induces

vigorous mixing of coal particles. intimate contact and

mixing of the heat transfer medium with the coal is also

achieved. In addition. or alternatively. a solid heat transfer

medium such as solid carbon dioxide can be introduced at a

mine location such as during a crushing step or subsequent

45 to the crushing as coal is loaded into a transport vehicle (i.e..

rail car or barge).

In a further preferred embodiment. the heat transfer

medium can be contacted with a bulk material when the bulk

material is subject to any material handling or processing

50 operation. such as when being transferred from one storage

or transport apparatus to another. such as during loading or

unloading from or to a transport vehicle or a storage facility.

For example. in the case of coal. which is transported by rail

or barge. when it arrives at a utility the coal is either

55 immediately consumed or sent to short- or long-term storage.

In any event. as the coal is unloaded from the rail or

barge vehicle. it is typically unloaded in such a manner that

the solid particulate coal becomes temporarily dispersed. At

this point in the unloading process. it is an advantageous

60 time for contacting with the heat transfer medium because of

the high degree of mixing available to achieve intimate

contact and efficient cooling. Thus. a fluid and/or solid heat

transfer medium. such as liquid or solid carbon dioxide or

liquid nitrogen. can be introduced at this point in a material

65 transfer process. For example. coal is typically unloaded

from a barge by scraping the coal from the cargo hold by a

bucket elevator or clamshell and is loaded onto a conveyor.

5

that many bulk materials and heat transfer media contain

some naturally occurring water. Reference to conducting the

present process in the absence of water refers to no water

being introduced in addition to any moisture naturally

occurring in the bulk material or heat transfer media.

A preferred embodiment of the present invention further

includes maintaining the bulk material at a cooled temperature

as described above for a time of at least about one day.

more preferably at least about one month and more preferably

at least about six months. For example. by maintaining

such temperatures for such time periods. oxidative deterioration

can be reduced during processing. transport and

storage of bulk materials.

The method of the present invention which includes

contacting a bulk material with a heat transfer medium to

effectively reduce the temperature. can be used in combination

with other techniques for reducing oxidative deterioration

and/or self-heating. For example. methods of the

present invention can further include sizing the bulk material

by removing small particles therefrom. In this manner. the

effective surface area of the bulk material available as an

oxidative surface is decreased. More particularly. this step

can include removing particles of the bulk material having

a particle size of less than about 5 millimeter.

In addition. methods of the present invention can also

include the step of compacting the bulk material. In this

manner. the available surface area for contact with ambient

air is reduced. More particularly. the step can include

compacting the bulk material to a bulk density of greater

than about 700 kgtm3

• and more preferably to a bulk density

of greater than about 1000 kglm3

•

Methods of the present invention will reduce the oxidative

deterioration of the bulk material in question. In the instance

where the bulk material is a solid fuel material. one measure

of the effectiveness of reducing oxidative deterioration is

measuring the rate of loss of the heating value of the fuel

material. For example. thermal loss can be measured by

comparing the moisture-ash-free heating value (MAP heating

value) of coal before and after storage. The MAPheating 40

value is computed by subtracting the dilution effects of

non-combustible ash and moisture from a heating value

measured on whole material by a laboratory calorimeter. The

MAP heating value is primarily a component of the hydrogen

and carbon in the coal. These two components are

oxidized to water vapor and carbon dioxide during storage.

Oxidation of hydrogen and carbon through low temperature

oxidation will reduce the MAP heating value.

In a preferred embodiment of methods of the present

invention. solid fuel material treated by methods of the

present invention has a rate of loss of heating value of less

than about 0.5% per month when stored at 2° C. in air. and

in a more preferred embodiment. the solid fuel material has

a rate of loss of heating value of less than about 0.1% per

month. and in a more preferred embodiment the solid fuel

material has a rate of loss of heating value of less than about

0.05% per month.

In the instance where the bulk material is a bulk food

product. such as bulk grain. other means of measuring the

effectiveness of reducing oxidative deterioration can be

employed. For example. a reduction in the concentration of

micro-organisms on grain could be used as a measurement

of the effectiveness of reducing oxidative deterioration in the

grain. The effectiveness of reducing oxidative deterioration

in a bulk food product could also be measured as a percentage

of spoilage of the food product over a given period of

time.

5}25.613

7 8

-58%

-85%

Percent reduction

O· C. by cooling

0.0034

0.0021

TABLE 1

24· C.

0.0081

0.0138

Rate of Oxygen Adsorption, k, for 24· C. and

O· C. Raw and Dried PRB Coal

Sample

Raw PRBCoal

Dtied PRB Coal

It will be noted that a reduction in the rate of oxygen

adsorption of 85% was achieved by cooling the dried coal

from 24° C. to 0° C. Similarly. a 58% reduction was seen

with the untreated raw coal. This example illustrates that

significant reductions in oxidative deterioration of fuel materials

can be achieved by practice of the present invention.

While various embodiments of the present invention have

been described in detail. it is apparent that modifications and

adaptations of those embodiments will occur to those skilled

in the art. It is to be expressly understood. however, that such

35 modifications and adaptations are within the scope of the

present invention, as set forth in the following claims.

What is claimed is:

1.A method to reduce oxidative deterioration of solid fuel

material comprising particles having a size of greater than

about 5 m.m. said method comprising the steps of:

directly contacting said solid fuel material with a heat

transfer medium. wherein said heat transfer medium is

not air; and

reducing a temperature of said solid fuel material below

about 10° C. through said contacting step.

2. A method as claimed in claim 1, wherein the temperature

of said solid fuel material is reduced to below about 5°

C.

3. A method. as claimed in claim 1, wherein the tempera50

ture of said solid fuel material is reduced to be between

about 0° C. and about 3° C.

4. Amethod, as claimed in claim 1. wherein said solid fuel

material is selected from the group consisting of coal,

upgraded coal products, oil shale. solid biomass materials,

55 refuse-derived fuels, coke, char, petroleum coke. gilsonite,

distillation by-products, wood by-product wastes, shredded

tires, peat and waste pond coal fines.

S. Amethod, as claimed in claim 1. wherein said solid fuel

material comprises coal and wherein said coal is selected

60 from the group consisting of bituminous coal. subbituminous

coal and lignite.

6. Amethod. as claimed in claim 1. wherein said solid fuel

material is an upgraded coal product and wherein said

upgraded coal product is selected from the group consisting

65 of thermally upgraded products, products beneficiated by

specific gravity separation, mechanically cleaned coal products

and sized coal products.

water bath maintained at 24° C. The other two vessels were

placed in an ice chest filled with ice and liquid water to

maintain the contents at 0° C. One of the dried samples was

placed in a 24°C. vessel and one in a 0° C. vessel. One

5 untreated sample was placed in a 24°C. vessel and in a 0°

C. vessel. The initial pressures within each vessel were

adjusted to 760 rom Hg (1 atmosphere at sea level). Air

pressure readings were read twice a day for 72 hours. Air

pressure decreases were reflective of oxygen adsorption by

10 the coal. Thus. air pressure decreases simulated the tendency

of coal to oxidize and therefore. the loss of thermal heating

value. The rates of oxygen adsorption are shown below in

Table 1.

EXAMPLES

Example 1

This example evaluates the rate of oxygen adsorption of

coal at different temperatures as a model to evaluate the

effect of cooling on oxidative deterioration of fuel materials.

Four loo-gram samples of o/.!-inch coal was obtained from

the Powder River Basin in Wyoming, U.S.A. 1Wo of the

samples were dried for 16 hours under a warminert nitrogen

atmosphere to reduce the moisture content of the coal from

approximately 27% to 6.27%. The remaining two samples

were not thermally treated. The samples contained, on a dry

basis, 7% ash. 44% volatile matter. 71% carbon, 4.8%

hydrogen, 0.6% sulfur and 11,820 BTUllb.

Each of the four samples of coal was placed in an airtight,

I-liter capacity. stainless steel test vessel. Each vessel was

fitted with an electronic solid-state pressure gauge capable

of measuring internal air pressure to within 0.015 psi. and a

septum fitting to allow air to be admitted to the vessel by

syringe. 1Wo of the vessels were placed in a circulating

At a transfer point, e,g., between two conveyors downstream

of the unloading process, a heat transfer medium such as

liquid carbon dioxide or liquid nitrogen can be added to the

coal before the coal is placed in storage.

In addition to conducting the method of the present

invention when the bulk material is subject to a high degree

of mixing or agitation, the step of contacting can be conducted

when the bulk material is static. For example, in the

instance of a solid fuel material, such as coal, which is in a

storage pile, the method of the present invention can include

contacting the heat transfer medium with the coal while it is

in storage or otherwise in a static condition. Such a step of

contacting can be achieved, for example. by inserting a pipe

or other distribution device into various points throughout a

storage pile and injecting an appropriate amount of, for 15

example, liquid carbon dioxide until appropriate cooling of

the coal pile is attained.

In the case wherein the bulk material is a bulk food

product, addition of a heat transfer medium is ideally

performed such that the food product is not crushed or 20

damaged. Therefore, the heat transfer medium can be contacted

with the bulk food product by adding such heat

transfer medium at a material handling transfer point during

the shipping and unloading of the food product.

25

In a further preferred embodiment. in the instance of solid

fuel materials, such as coal or upgraded coal products, the

heat transfer medium is liquid and/or solid carbon dioxide.

In this embodiment, carbon dioxide is recovered from the

flue gases at a utility by conventional stripping technology. 30

The carbon dioxide is then liquified or frozen solid and then

used, as described above, for contacting with coal or

upgraded coal product supplies which are incoming during

unloading from a transport vehicle or which are already in

storage.

Further embodiments of the present invention include

compositions which are produced by the processes of the

present invention. Such compositions include any of the

various bulk materials. as described above. which have been

contacted with an appropriate heat transfer medium, as 40

generally disclosed above, and cooled to a temperature

within the ranges as described above to reduce the oxidative

deterioration of the bulk material.

The following examples are provided for purposes of

illustration only and are not intended to limit the scope of the 45

invention.

5.725.613

9 10

* * * * *

26. A composition as claimed in claim 25, wherein the

temperature of said solid fuel material is reduced to below

about 50 C.

27. A composition, as claimed in claim 25. wherein the

5 temperature of said solid fuel material is reduced to be

between about 00 Co and about 3a C.

28. A composition, as claimed in claim 25, wherein said

solid fuel material is selected from the group consisting of

coal, upgraded coal products, oil shale, solid biomass

10 materials, refuse-derived fuels, coke, char. petroleum coke,

gilsonite, distillation by-products. wood by-product wastes.

shredded tires. peat and waste pond coal fines.

29. A composition, as claimed in claim 25, wherein said

solid fuel material comprises coal and wherein said coal is

15 selected from the group consisting of bituminous coal,

sub-bituminous coal and lignite.

30. A composition. as claimed in claim 25, wherein said

solid fuel material is an upgraded coal product and wherein

said upgraded coal product is selected from the group

20 consisting of thermally upgraded products. products beneficiated

by specific gravity separation, mechanically cleaned

coal products and sized coal products.

31. A composition, as claimed in claim 25. wherein said

heat transfer medium is selected from the group consisting

25 of carbon dioxide, carbon monoxide. helium, nitrogen,

argon and air.

32. A composition, as claimed in claim 25, wherein said

heat transfer medium comprises carbon dioxide.

33. A composition, as claimed in claim 25. wherein said

30 heat transfer medium comprises liquid carbon dioxide.

34. A composition, as claimed in claim 25. wherein said

solid fuel material has a rate of loss of heating value of less

than about O.5%/month.

35. A composition, as claimed in claim 25. wherein said

35 solid fuel material has a rate of loss of heating value of less

than about 0.1%/month.

36. A composition, as claimed in claim 25, wherein said

solid fuel material has a rate of loss of heating value of less

than about 0.05%/month.

37. A method to reduce oxidative deterioration of a bulk

material comprising particles having a size of less than 5

mm.. said method comprising the steps of:

directly contacting said bulk material with a heat transfer

medium; and

reducing a temperature of said bulk material below about

100 C. through said contacting step.

38. A method. as claimed in claim 37, wherein the

temperature of said bulk material is reduced to below about

50 C.

39. A method. as claimed in claim 37, wherein the

temperature of said bulk material is reduced to be between

about 00 C. and about 3a C.

40. A method, as claimed in claim 37, wherein said bulk

material comprises a bulk food or agricultural product.

55 41. A method, as claimed in claim 40, wherein said bulk

food product is selected from the group consisting of wheat,

corn, soybeans, barley, oats and animal feed.

42. A method, as claimed in claim 40. wherein said bulk

material is a carbon containing material selected from the

60 group consisting of activated carbon and carbon black.

7. A method, as claimed in claim 1, wherein said heat

transfer medium is selected from the group consisting of

carbon dioxide, carbon monoxide, helium, nitrogen, argon

and air.

8. A method, as claimed in claim 1, wherein said heat

transfer medium is selected from the group consisting of

carbon dioxide, carbon monoxide, nitrogen and argon.

9. A method, as claimed in claim 1, wherein said heat

transfer medium comprises carbon dioxide.

10. A method, as claimed in claim 1, wherein said heat

transfer medium comprises liquid carbon dioxide.

11. A method, as claimed in claim 1, wherein said heat

transfer medium comprises solid carbon dioxide.

12. A method, as claimed in claim 1, wherein said heat

transfer medium comprises liquid nitrogen.

13. A method. as claimed in claim 1, further comprising

removing particles of said fuel material having a particle

size of less than about 5 millimeter.

14. A method. as claimed in claim 1, further comprising

compacting said solid fuel material.

15. A method, as claimed in claim 1, further comprising

compacting said solid fuel material to a bulk density of

greater than about 700 kglm3

•

16. A method, as claimed in claim 1, further comprising

compacting said solid fuel material to a bulk density of

greater than about 1000 kg/m3

•

17. A method, as claimed in claim 1, wherein said solid

fuel material has a rate of loss of heating value of less than

about 0.5%/month.

18. A method, as claimed in claim 1, wherein said solid

fuel material has a rate of loss of heating value of less than

about 0.1%/month.

19. A method, as claimed in claim 1, wherein said solid

fuel material has a rate of loss of heating value of less than

about 0.05%/month.

20. A method, as claimed in claim 1, wherein said step of

contacting said heat transfer medium and said solid fuel

material displaces ambient air from contact with said fuel

material.

21. A method, as claimed in claim 1, wherein said heat 40

transfer medium reacts with the surface of said solid fuel

material to passivate said solid fuel material from oxidation

by ambient air.

22. A method. as claimed in claim 1, wherein said step of

contacting comprises contacting said heat transfer medium 45

with said solid fuel material during crushing of said solid

fuel material.

23. A method, as claimed in claim 1, wherein said step of

contacting comprises contacting said heat transfer medium

with said solid fuel material during a material handling or 50

processing operation.

24. A method, as claimed in claim 1, wherein said step of

contacting comprises contacting said heat transfer medium

with said solid fuel material while said solid fuel material is

in a static condition.

25. A composition comprising:

a solid fuel material, comprising particles having a size of

greater than about 5 mm; and

a heat transfer medium being in direct contact with said

solid fuel material, wherein said composition has a

temperature below about 100 C. and said heat transfer

medium is not air.

UNITED STATES PATENT AND TRADEMARK OFFICE

CERTIFICATE OF CORRECTION

PATENT NO. : 5,725,613

DATED : March 10, 1998

INVENTOR(S) : Reeves et al

It is certified that error appears in the above-identified patent and that said Letters Patent is hereby

corrected as shown below:

Column 9, line 3, after nitrogen delete "," and insert --and--.

Column 9, line 4, delete --and air--.

Column 10, line 25, after nitrogen delete "," and insert --and--.

Column 10, line 26, delete --and air--.

Signed and Sealed this

Twenty-seventh Day ofApril, 1999

Attest:

Attesting Officer

Q. TODD DICKINSON

Acrin!? Commissioner of PateUf.'lllnd Trademarks


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