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Urea (Polyurea) Greases

Article in Russian Journal of Applied Chemistry · June 2018

DOI: 10.1134/S1070427218060010

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ISSN 1070-4272, Russian Journal of Applied Chemistry, 2018, Vol. 91, No. 6, pp. 885−894. © Pleiades Publishing, Ltd., 2018.
Original Russian Text © A.S. Lyadov, Yu.M. Maksimova, A.S. Shakhmatova, V.V. Kirillov, O.P. Parenago, 2018, published in Zhurnal Prikladnoi Khimii, 2018,
Vol. 91, No. 6, pp. 761−771.

REVIEWS

Urea (Polyurea) Greases

A. S. Lyadova,b,*, Yu. M. Maksimovaa,c, A. S. Shakhmatovaa,c,
V. V. Kirillovb, and O. P. Parenagoa
a Topchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences, Moscow, 119191 Russia
b Elektrogorsk Institute of Oil Refining, Elektrogorsk, Moscow oblast, 142530 Russia
c Peoples’ Friendship University of Russia, Moscow, 117198 Russia

*e-mail: [email protected]

Received June 6, 2018

Abstract—The review deals with greases in which organic ureas of various compositions and structures are
used as thickeners. The nature of compounds participating in the synthesis of organic ureas and the main types
of polyurea thickeners are considered. The physicochemical, tribological, and operation properties of plastic
polyurea lubricants are discussed.
DOI: 10.1134/S1070427218060010

Today it is impossible to imagine the operation Table 2 illustrates the diversity of the modern
of any friction unit without using greases. Greases assortment of greases [1]. By combining base oil,
are semisolid lubricants consisting, as a rule, of two thickener, and additives, it is possible to obtain an
main components: base oil and thickener. The use and unlimited number of lubricant formulations for
composition of greases was mentioned for the first various purposes with a wide spectrum of operation
time in the survived sources from the Ancient Egypt. characteristics.
In the XIX century, soaps came into active use as Vigorous progress of technologies and engineering
thickeners. These thickeners still play an important and the development of high-capacity installations
role in production of greases. The brief history of the and aggregates made the requirements to lubricants
origination and development of greases is given in considerably more stringent. Often lubricants with soap
Table 1. thickeners no longer met these requirements, which led
Table 1. Origination chronology for various types of greases
Date Event

About 1400 BC The use of animal fat and limestone for lubrication of axes of Hittite chariots was started. In the same
period, lubricants based on olive oil and limestone were used in Ancient Egypt
1845 A lubricant consisting of mineral oil, animal fat, and limestone was invented in the United States
1853 The first sodium lubricant based on beef fat appeared in the United Kingdom
1912 The production of calcium lubricants with the dispersion medium based on mineral oil was started
in Japan
1938 Lithium lubricants were developed. They quickly conquered the world and were used as
multipurpose lubricants
1954 Invention of complex aluminum lubricants for operation at high temperatures
1955 Invention of urea greases in the United States

885
886 LYADOV et al.

Table 2. Base oils, thickeners, and additives for modern lubricants

Base oils Thickeners Additives

Mineral oils Sodium soaps Antioxidant

Synthetic oils Calcium soaps Antiscuff
Diesters Lithium soaps Friction modifiers
Silicone liquids Aluminum soaps Corrosion inhibitors
Phosphate esters Lithium complex Metal deactivators
Fluorinated silicones Calcium complex Dyes
Chlorinated silicones Aluminum complex Structural modifiers
Polyglycols Bentonite
Silicon oxide
Carbon/graphite
Poluyurea
Polyethylene
Indanthrene dyes
Phthalocyanine dyes

to the development of lubricants with novel thickeners,

e.g., with those on urea base. The first urea thickener
was patented in 1955 [2], and lubricants thickened
with organic ureas have found wide use owing to their
better physicochemical, tribological, and operation
characteristics compared to soap lubricants [3].
This review deals with greases in which organic Urea group Urea
ureas of various compositions and structures are used
as thickeners. The simplest representative of ureas is unsubstituted
urea. Compounds containing two urea groups are termed
THICKENERS BASED ON ORGANIC UREAS diureas, and those containing more than two urea groups,
polyureas. Among ureas, diureas are used as thickeners
Organic ureas are compounds containing the most widely. These compounds can be prepared by the
following group of atoms: reaction of diisocyanates with amines [4]:

This reaction is exothermic and readily occurs with- traditionally termed polyureas. True polyureas can also
out any additional actions. Despite the fact that diureas be used as thickeners. They are prepared by copolymer-
are used in most cases as thickeners, these additives are ization of appropriate diisocyanates and diamines:

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

 UREA (POLYUREA) GREASES 887

The following isocyanates are used for preparing diisocyanate), PIC (polyisocyanate), and TDI (toluene
polyureas most widely: MDI (diphenylmethane diisocyanate):

MDI TDI

MDI, in particular, the 4,4′ isomer, is the most the lubricant industry after the end of the World War II.
produced diisocyanate in the world (market share about Despite the fact that the technology of their production
60%). Commercial PIC (polyisocyanate) is a mixture was developed in the United States, urea greases became
of products: 55% MDI, 25% triisocyanates, and 20% the most widely used in Japan, where their market share
polyisocyanates [5]. TDI is mainly produced as 2,4 is still about 21%. Data on the production of various
isomer, and its market share is about 30%. types of lubricants in various countries and regions are
Among amines, primary amines, namely, aniline, given in Table 3. As can be seen, PU lubricants were
individual aliphatic amines (octylamine, dodecylamine, initially produced only in Japan, China, and North
octadecylamine produced under trade name Rofamin-t America. In 2011, the situation slightly changed, and
or Flotamin), or their mixtures, are used for preparing production of these lubricants was started in Europe
urea thickeners most widely. (Fig. 1) [6].
The total production share of urea greases in the
COUNTRIES AND REGIONS PRODUCING
world, according to different estimates, does not exceed
POLYUREA LUBRICANTS
4–5%. Today in Russia there is only one enterprise
The development of plastic polyurea lubricants (PU having its own production of PU lubricants for various
lubricants) is one of the most significant discoveries in purposes, Elektrogorsk Institute of Oil Refining. The

Table 3. Distribution of lubricant production between countries and regions

Country, region Production share, %

North America Li 36 Li Complex 35 Al 9 PU 6

Europe Li 60 Li Complex 11 Ca 7 Ca Complex 7
China Li 73 Ca Complex 8 PU 3 Li Complex 7
Japan Li 59 PU 23 Ca 11 Li Complex 1
India Li 82 Na 7 Ca 4 Li Complex 4
Southeast Asia Li 55 Ca 22 Al 4 Li Complex 17
Countries of Caribbean Basin Li 76 Ca 12 Ca 3 Li Complex 5
Africa and Central Asia Li 81 Li Complex 7 Ca 3 Na 3

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

888 LYADOV et al.

Other
Aluminum
Polyurea
Calcium
Lithium

Asia Europe North

America

Fig. 1. Share of PU lubricants in the total lubricant production volume for different regions (as for 2011).

total production capacity of this enterprise is 500 t 23% of all the urea greases produced in the world
annually, which meets the demand of the Russian are consumed by agricultural enterprises, because these
Federation for this product and allows the import of lubricants are versatile and can be used in friction units
analogs to be fully abandoned. of various structures. Thus, farmers can ensure reliable
The main companies producing urea greases in the operation of diverse agricultural machines by purchasing
world and supplying them to the Russian market are only a single lubricant. The share of machine-building
Clariant, Mobil, and BASF. There are also several tens and automotive industries is 17% each, and the share of
of smaller companies producing these lubricants. The the metallurgical industry is 10%. The best illustration
final consumers of PU lubricants and their distribution is the example of metallurgical industry, where soap
are shown in Fig. 2. lubricants are replaced by urea greases, because the
modern continuous casting mills with centralized
feeding system mainly use urea greases as exhibiting
high heat resistance, good pumpability, and excellent
water resistance. That is why metallurgical enterprises
are the major consumers of urea greases in Russia.
Machine
building
Agriculture BASE OILS FOR UREA GREASES
17%
23%
Base oils of any group are suitable for preparing
greases with thickeners based on organic ureas, except
Other polyorganosiloxanes, which in the pure form cannot be
17% thickened with ureas. However, numerous lubricants
Metallurgical based on polysiloxanes are available. Mixtures of poly-
industry siloxanes with mineral or synthetic base oils are used
23% for their production. It should be noted that producers
Automotive of greases started to actively use silicone liquids for
y 6%

industry preparing products intended for operation under severe

Mining

17% conditions (high or ultralow temperatures, aggressive

industr

medium, etc.). The nature of the base oil significantly in-

fluences the rheological and operation properties of urea
greases. Also, the base oil should be chosen very thor-
oughly, because isocyanates owing to their high reactiv-
ity can react with oil components, which can negatively
Fig. 2. Final consumers of polyurea lubricants in the world.
affect the physicochemical and operation properties of
RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018
 UREA (POLYUREA) GREASES 889

a lubricant. Greases based on poly-α-olefin oils thick- TECHNOLOGY FOR PRODUCING

ened with ureas of various compositions and structures UREA GREASES
have found wide use. As shown in [7], such lubricants
can operate under the conditions of high temperatures There are two essentially different technologies for
and velocities. The low-temperature properties of urea producing urea greases. The first technology consists
greases based on poly-α-olefin oils were studied in [8]. in thickening of base oils using a ready urea powder.
A powder of an organic urea is dispersed in the base
ADDITIVES IMPROVING THE OPERATION oil, and the oil is heated with vigorous stirring to a
PROPERTIES OF UREA GREASES definite temperature, usually 100–140°С. In the process,
the oil undergoes thickening with the formation of a
Antiwear, antiscuff, and corrosion-protecting ad- grease. Then, the resulting mixture is passed through
ditives are commonly introduced into the urea grease a homogenizer and cooled [20, 21]. The resulting
formulations. The performance of the additives is often product is packed. This process is very simple in
manifested in urea greases more strongly than in soap implementation; however, there are problems with the
lubricants. availability of the polyurea powder. In the world, there
When formulating greases with polyurea thickeners, are several companies producing thickening powders
it should be taken into account that organic ureas can based on ureas, but their cost is extremely high, because
both deteriorate and improve the antiwear and antiscuff the process for synthesizing and isolating pure polyureas
properties, which often requires introduction of various is money-consuming and requires large amounts of
friction modifiers into the lubricant formulation. Both solvents. Some processes involve the use of an auxiliary
known additives (graphite, molybdenum disulfide, solvent, in which the ready urea is dissolved and then
Teflon, zinc dithiophosphate, etc.) and new additives introduced into the base oil, after which the solvent is
that have not been used previously, e.g., hexagonal removed at reduced pressure.
boron nitride [9], organic compounds of tungsten and The second technology involves preparation of a urea
molybdenum containing no phosphorus and sulfur thickener in situ in the base oil from the diisocyanate
[10], naphthyl phenyl diphosphate [11], nanosized and appropriate amines. To this end, a solution of the
molybdenum disulfide [12], nanosized silicon oxide base oil with the corresponding amines is prepared in
[13], molybdenum carbamate complexes [14], etc., are the main reactor, and a suspension of the diisocyanate
used as antiwear agents. All these compounds showed in a dispersion medium is added at a definite rate. When
antiwear and, in some cases, also antiscuff activity in preparing lubricants, particular attention is paid to the
urea greases. temperature conditions and stirring efficiency, because
Introduction of antioxidant additives into urea these parameters can influence the operation properties
greases is not always necessary, because ureas of the lubricants [22, 23]. Sometimes a small amount
themselves are capable to inhibit oxidation processes of water is added after thickening to remove traces of
[15]. Additives based on boron compounds enhance toxic diisocyanate from the ready lubricant. This water
the colloidal stability of urea greases. It is assumed that is then removed in the course of keeping the lubricant
boron compounds form with ureas a complex exhibiting at elevated temperature. The unchanged diisocyanate
higher thickening power [16]. The effect of ionic liquids reacts with water to form harmless carbamic acid.
on the physicochemical and tribological properties of Figure 3 schematically shows an installation
urea greases is being studied [17, 18]. For example, developed by STRATCO for production of urea greases.
Wang and Wu [19] have shown that introduction of a A specific feature of this installation is a reactor allowing
phosphorus-containing ionic liquid into urea greases thickening of base oil by introducing pure diisocyanate
formulation allows considerable improvement of the without preliminarily making an emulsion. In the process,
tribological properties of a friction unit at high operation the reactants are stirred with the created turbulent flow.
temperatures. Wang and Wu attribute this effect to the The operation characteristics of lubricants prepared in
formation of a protective film consisting of iron oxide this reactor are better than those of lubricants of similar
and FePO4 on tribocontact sites. composition, prepared in common mixing reactors [24].

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

890 LYADOV et al.

Fig. 3. Scheme of an installation developed by STRATCO for production of urea greases: (1) vertical reactor, (2) intermediate vessel,
(3) pumps, (4) filter, (5) homogenizer, and (6) product output for packaging.

The physicochemical and operation characteristics (1) IR spectroscopy. The IR spectrum of urea greases
of urea greases prepared using ready organic ureas and has the following characteristic absorption bands
those synthesized in the base oil in situ were compared belonging to polyureas: 3310–3323 and 1610 cm–1 [28].
in some studies [25, 26]. It is, however, impossible to
(2) Thermal gravimetric analysis and differential
make unambiguous conclusions on what technology is
scanning calorimetry furnish information on the heat
preferable.
resistance of lubricants and on the presence or absence
PHYSICOCHEMICAL METHODS USED FOR of ash upon combustion of such lubricants.
CHARACTERIZATION OF UREA GREASES (3) Scanning electron microscopy allows studying
Determination of physicochemical characteristics is the morphology of lubricant thickeners.
an essential step in the development of new lubricants. Figure 4 shows an electron micrograph of urea
There are a number of parameters whose determination thickener isolated from a lubricant [29].
is obligatory, and procedures for their determination Along with laboratory studies, rig and industrial
are prescribed by the corresponding standards [GOST trials are also important. They are performed in cases
(State Standard), ASTM, DIN]. The main parameters when the lubricant being developed meets all the
that should be determined are as follows: requirements and the conclusion on its suitability for
– external appearance; industrial operation should be formulated. There are
– penetration at 25°С, 0.1 mm (GOST 5346–78); numerous procedures for diverse rig trials of lubricants,
– dropping point (GOST 6793–74); developed taking into account the parameters whose
determination is necessary. An example is a rig for
– ultimate strength (GOST 7143–73);
studying the pumpability of a lubricant in centralized
– colloidal stability (GOST 7142–74); feeding systems developed by SKF [30]. The final step
– corrosion action on metals (GOST 9.080–77); of the development of a lubricant involves industrial
– mechanical impurities. trials on specific friction units at enterprises that produce
Along with physicochemical studies, there are lubricants or use them [31].
approximately 30 standard mechanodynamical tests
PHYSICOCHEMICAL, TRIBOLOGICAL,
and numerous tests developed by lubricant producers.
AND OPERATION PROPERTIES
For example, the Kluber company developed 17 own OF UREA GREASES
mechanodynamic tests [27].
Along with the determination of these parameters, The greases with different types of thickeners are
there are numerous modern methods allowing compre- compared in Table 4. As can be seen, urea grease surpass
hensive study of lubricants on different levels. lubricants with other thickeners in all the parameters,

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

 UREA (POLYUREA) GREASES 891

Table 4. Comparison of greases thickened with various thickeners

Common soap lubricants Complex lubricants Urea
Property
Ca Li Na Al Ca Ba Li greases

Drop point 80 175 170 260 260 260 260 250

Maximal operation temperature 65 125 125 150 150 150 160 180
Low-temperature properties ++ ++ + ++ ++ ++ ++ +++
Water resistance +++ ++ + +++ +++ +++ +++ +++
Oxidation resistance + ++ ++ +++ +++ + ++ +++

which allows their operation in various friction units in of the hydrocarbon substituents in the diurea structure.
a wide range of conditions. A study of the tribological properties of lubricants has
The structure of the urea thickener can significantly shown that the wear spot diameter tends to increase with
influence the physicochemical and tribological charac- an increase in the number of carbon atoms in the diurea
teristics of lubricants. The properties of lubricants in molecule. This fact well agrees with the results obtained
relation to the structure of organic urea are compared in studying the colloidal stability of the lubricants.
in Table 5 [29]. The lubricants thickened with diureas The results of studying the influence exerted by the
have the best operation properties. The use of aromatic degree of oligomerization of urea on physicochemical
diureas allows preparation of the most stable lubricants. and tribological properties of lubricants are described
Diureas containing both aromatic and aliphatic substitu- in [41]. Lubricants based on the same oil, thickened
ents are used very frequently for preparing multipurpose with di-, tetra-, hexa-, and octaureas, were prepared.
urea greases, which allows reaching better operation Diphenylmethane 4,4′-diisocyanate was used. An
characteristics. increase in the number of units in the oligourea
Numerous studies deal with the influence of molecule led to an increase in the colloidal stability
and ultimate strength, but the penetration and wear spot
the composition and structure of organic ureas on
the physicochemical, tribological, and operation
characteristics of greases thickened with them [32–40].
Studies are also performed to evaluate the stability of
urea greases under various operation conditions in
relation to the design of the friction unit and external
conditions of the tribocontact [41–49].
The length of hydrocarbon substituents in diureas
influences the lubricant properties. For example, the
ultimate strength, which is an important parameter of
greases, under equal other conditions increases with
an increase in the number of carbon atoms in the
hydrocarbon substituents in the amine moiety of the
diurea molecule, which suggests formation of a stronger
structural framework of the grease. Similar trend was
observed for the colloidal stability. With an increase
in the number of atoms in the diurea molecule, the
colloidal stability is improved, which is manifested in a
decrease in the amount of oil separated in the course of
testing the lubricants at elevated temperatures. The drop Fig. 4. TEM image of aliphatic diurea separated from urea
point tends to increase with an increase in the length greases.

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

892 LYADOV et al.

Table 5. Comparison of urea greases differing in the type of the organic urea
Maximal Water Ultimate
Urea type operation Lubricant characteristics
resistance strength
temperature, °C

Diurea: The most stable lubricant, optimal for use

aromatic 180 ++++ ++++ as embedded grease
aliphatic 180 +++ +++ Multipurpose lubricant, can be
recommended for use in centralized
feeding systems
alicyclic 180 +++ +++ Multipurpose lubricant
Triurea 180 ++ + Tends to solidification
Tetraurea 180 ++ + Tends to softening in friction

Table 6. Compatibility of various types of greasesa

Ca 12-hy- Li 12-hy-
Al Ba Ca Ca Ca Li Li
Thickener type droxy- Bentonite droxy- Urea
complex complex stearate complex sulfonate stearate complex
stearate stearate
Al complex I I С I P I I I С С
Ba complex I I С I С I I I I P
Ca stearate I I Х С I С С С P С С
Ca
C С С Х P P С С С С С
12-hydroxystearate
Ca complex I I I P Х I I I I С С
Ca sulfonate P С С P I Х I P P С С
Bentonite I I С С I I Х I I I С
Li stearate I I С С I P I Х С С С
Li
I I P С I P I С Х I С
12-hydroxystearate
Li complex С I С С С С I С I Х С
Urea С P С С С С С С С С Х
a (C) Compatible, (P) partially compatible, and (I) incompatible.

diameter increased also, which is a negative factor for greases are comparable with other lubricants with the
the operation of greases. same base oils, and their water resistance is close to that
Because organic ureas are thermally stable compounds of soap lubricants [50].
(Fig. 5) and start to decompose at temperatures higher One more important advantage of urea greases is
than 200°С, the choice of appropriate base oils allows their compatibility with other kinds of lubricants [51].
preparation of greases suitable for operation at high As seen from Table 6, urea greases are compatible
temperatures. with all the kinds of lubricants except those thickened
with the barium complex with which they are partially
The radiation resistance of organic ureas is higher compatible. This fact is important for practice, because
than that of other lubricants, especially soap lubricants. the lubricants can be replaced without cleaning the
Therefore, urea greases were recommended for use in friction units and centralized systems for feeding
atomic power engineering. In adhesion properties, urea lubricating materials.

RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

 UREA (POLYUREA) GREASES 893

Δm, % 5. TU (Technical Specification) 113-03-38-106–90.

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RUSSIAN JOURNAL OF APPLIED CHEMISTRY Vol. 91 No. 6 2018

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