CN109852454A - A kind of four polyurea grease of composite calcium-base and preparation method thereof - Google Patents

A kind of four polyurea grease of composite calcium-base and preparation method thereof Download PDF

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Publication number
CN109852454A
CN109852454A CN201910227265.8A CN201910227265A CN109852454A CN 109852454 A CN109852454 A CN 109852454A CN 201910227265 A CN201910227265 A CN 201910227265A CN 109852454 A CN109852454 A CN 109852454A
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China
Prior art keywords
base
polyurea grease
composite calcium
calcium
diisocyanate
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Withdrawn
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CN201910227265.8A
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Chinese (zh)
Inventor
耿飞
白涛
顾敏峰
左明明
左晓兵
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Changshu Institute of Technology
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Changshu Institute of Technology
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Priority to CN201910227265.8A priority Critical patent/CN109852454A/en
Publication of CN109852454A publication Critical patent/CN109852454A/en
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Abstract

The invention discloses a kind of four polyurea greases of composite calcium-base and preparation method thereof, and according to mass percentage, raw material is composed of the following components: base oil 70-82%, thickening agent 15-30%, additive 1-4%;Wherein, the thickening agent is made of diisocyanate, organic amine, acid anhydrides, calcium hydroxide.Four polyurea grease of composite calcium-base prepared by the present invention has good lubricity, adhesiveness, heat-resisting quantity and excellent mechanical stability, extreme pressure anti-wear and anti-water drenching.The present invention effectively improves the correlated performance of polyurea grease, expands its application range, and preparation method is simply easily operated, has good marketing and application potential.

Description

A kind of four polyurea grease of composite calcium-base and preparation method thereof
Technical field
The invention belongs to lubriation material technical field, a kind of four polyurea grease of composite calcium-base and its preparation side are provided Method.
Background technique
With the fast development of modern industry, the harsh working condition such as various high/low temperatures, high revolving speed is to industrial lubrication material More stringent requirements are proposed for material, and in recent years, all kinds of lubricating grease have obtained quick development.Wherein, compositing lithio ester, composite sulfoacid The high dropping point such as calcium grease, polyurea grease, long-life lubricating grease are studied extensively by scholars.
Metal soap base grease such as lithium base grease, Ba-grease, calcium-base grease etc. has lubricity good, inexpensive The advantages of, it is widely applied in industrial circle, but in use, the metal ion in metal soap base grease is often Catalysed oxidn can be generated to lubricating grease, so that the antioxygenic property of metal soap base grease is poor, so that working life contracts It is short, machinery rouge high frequency of replacement.
Polyurea grease has many excellent performances, but its there is also the defects of itself, after working at high temperature for a long time, gather Urea grease can generate hardening phenomenon, this needs to concentrate in the high-temperature mechanical equipment for rouge some, often make line clogging, To influence mechanical normal use, which also limits the uses of polyurea grease
In order to improve existing metal soap base grease and polyurea grease existing shortcoming and defect in use, expand The demand for the grease product that the use scope of big existing grease product develops higher performance is constantly increasing.
Summary of the invention
The object of the present invention is to provide a kind of four polyurea greases of composite calcium-base and preparation method thereof, to improve existing metal Soap base grease and polyurea grease existing shortcoming and defect in use, expand existing grease product uses model It encloses.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of four polyurea grease of composite calcium-base, according to mass percentage, raw material is composed of the following components:
Base oil 70-82%, thickening agent 15-30%, additive 1-4%;
Wherein, the thickening agent is made of diisocyanate, organic amine, binary acid, calcium hydroxide.
Preferably, each component of the thickening agent accounts for the percentage composition of four polyurea grease raw material of composite calcium-base are as follows:
Diisocyanate 6-10%, organic amine 4-7.1%, binary acid 1.5-3.5%, calcium hydroxide 5-7%.
The base oil is one of mineral oil, synthetic oil, vegetable oil or a variety of mixtures, preferably mineral oil.
The diisocyanate is toluene di-isocyanate(TDI), methyldiphenyl diisocyanate, diphenylmethane diisocyanates One of ester, xylylene diisocyanate, 4,4- methyl diphenylene diisocyanate are a variety of, preferably diphenyl-methane two Isocyanates.
The organic amine is the mixture of organic monoamine and organic diamine;The organic monoamine is octadecylamine, lauryl amine, ten One of tetramine, para-totuidine, cyclohexylamine, parachloroanilinum, m-chloroaniline, aniline or a variety of mixtures, preferably octadecylamine, Para-totuidine, cyclohexylamine;The organic diamine be p-phenylenediamine, o-phenylenediamine, the aromatic amine of 4,4- benzidine, ethylenediamine, One of propane diamine, the straight-chain fatty amine of 1,6- hexamethylene diamine, diaminodiphenylmethane or a variety of mixtures, preferably diamino Diphenyl-methane.
The acid anhydrides is succinic anhydride.
The additive is organic amine-phenolic antioxidant and anticorrosive antirust agent.
As optimal technical scheme, according to mass percentage, the raw material of four polyurea grease of composite calcium-base of the invention It is composed of the following components: base oil 72-80%, diisocyanate 6.5-9.5%, organic monoamine 4-5.5%, organic diamine 1- 2%, succinic anhydride 1.5-2.5%, calcium hydroxide 5.5-7%, additive 1-3%.
A kind of preparation method of four polyurea grease of composite calcium-base, comprising the following steps:
(1) base oil and organic diamine are added to reaction kettle, are warming up to 80 DEG C of progress heating stirring dissolutions;
(2) diisocyanate is added in the mixture that step (1) obtains, and dissolved, is transferred in reaction kettle, 80 DEG C carry out isothermal reaction 60min;
(3) organic monoamine is added in the mixture that step (2) obtains, and dissolved, in a kettle, in 80 DEG C of temperature Degree reaction 40min, is then warming up to 95 DEG C for reaction kettle and adds distilled water and react 40min under the conditions of this temperature;
(4) acid anhydrides is added in the mixture that solution is obtained to step (3), and dissolved, be then warming up to 120 in reaction kettle DEG C, carry out isothermal reaction 60min;
(5) calcium hydroxide and distilled water are weighed and be added to after Hybrid Heating dissolution reaction kettle, while by additive It is added in reaction kettle, the isothermal reaction 40min at 120 DEG C;
(6) reaction kettle is warming up to 205 DEG C of progress high temperature refining 15min, cools down, grind by stirring, degassing obtains institute State four polyurea grease of composite calcium-base.
The preparation principle of four polyurea grease of composite calcium-base of the invention are as follows:
The utility model has the advantages that four polyurea grease of composite calcium-base and preparation method thereof of the invention, has double phenyl ring using one kind The diaminodiphenylmethane of rock-steady structure is as the organic diamine in the preparation of four polyurea compounds and passes through a kind of method of simplicity Carboxylic acid calcium salt is introduced into four polyureas molecules to prepare a kind of four polyurea grease of composite calcium-base.Prepared composite calcium-base Four polyurea greases have good lubricity, adhesiveness, heat-resisting quantity and excellent mechanical stability, extreme pressure anti-wear and resist Water washout characteristics.Four polyurea grease of composite calcium-base of the invention not only increases technical deficiency existing for existing lubricating grease and expansion The application range of grease product.
Specific embodiment
The present invention is further elaborated below with reference to embodiment.
Embodiment 1
Four polyurea grease of composite calcium-base of the present embodiment, according to mass percentage, raw material is composed of the following components: Base oil 76%, diisocyanate 8.7%, octadecylamine 4.7%, diaminodiphenylmethane 1%, succinic anhydride 2%, calcium hydroxide 6.6%, organic amine-phenolic antioxidant 0.5%, anticorrosive antirust agent 0.5%;
Above-mentioned four polyurea grease of composite calcium-base the preparation method is as follows:
(1) base oil and organic diamine are added to reaction kettle, are warming up to 80 DEG C of progress heating stirring dissolutions;
(2) diisocyanate is added in the mixture that step (1) obtains, and dissolved, is transferred in reaction kettle, 80 DEG C carry out isothermal reaction 60min;
(3) organic monoamine is added in the mixture that step (2) obtains, and dissolved, in a kettle, in 80 DEG C of temperature Degree reaction 40min, is then warming up to 95 DEG C for reaction kettle and adds distilled water and react 40min under the conditions of this temperature;
(4) acid anhydrides is added in the mixture that solution is obtained to step (3), and dissolved, be then warming up to 120 in reaction kettle DEG C, carry out isothermal reaction 60min;
(5) calcium hydroxide and distilled water are weighed and be added to after Hybrid Heating dissolution reaction kettle, while by additive It is added in reaction kettle, the isothermal reaction 40min at 120 DEG C;
(6) reaction kettle is warming up to 205 DEG C of progress high temperature refining 15min, cools down, grind by stirring, degassing obtains institute State four polyurea grease of composite calcium-base.
Embodiment 2
Four polyurea grease of composite calcium-base of the present embodiment, according to mass percentage, raw material is composed of the following components: Base oil 78%, diisocyanate 8%, octadecylamine 4.2%, diaminodiphenylmethane 0.9%, succinic anhydride 1.9%, hydroxide Calcium 6%, organic amine-phenolic antioxidant 0.5%, anticorrosive antirust agent 0.5%.
The preparation method is the same as that of Example 1.
Embodiment 3
Four polyurea grease of composite calcium-base of the present embodiment, according to mass percentage, raw material is composed of the following components: Base oil 75%, diisocyanate 8.8%, octadecylamine 4.8%, diaminodiphenylmethane 1.1%, succinic anhydride 2.2%, hydrogen-oxygen Change calcium 7%, organic amine-phenolic antioxidant 0.6%, anticorrosive antirust agent 0.5%.
The preparation method is the same as that of Example 1.
Embodiment 4
Four polyurea grease of composite calcium-base of the present embodiment, according to mass percentage, raw material is composed of the following components: Base oil 72%, diisocyanate 9.5%, octadecylamine 5.5%, diaminodiphenylmethane 2%, succinic anhydride 2.5%, hydroxide Calcium 5.5%, organic amine-phenolic antioxidant 1.5%, anticorrosive antirust agent 1.5%.
The preparation method is the same as that of Example 1.
Embodiment 5
Four polyurea grease of composite calcium-base of the present embodiment, according to mass percentage, raw material is composed of the following components: Base oil 80%, diisocyanate 6.5%, octadecylamine 4%, diaminodiphenylmethane 1%, succinic anhydride 1.5%, calcium hydroxide 6%, organic amine-phenolic antioxidant 0.5%, anticorrosive antirust agent 0.5%.
The preparation method is the same as that of Example 1.
Comparative example
Using the mass ratio of base oil and thickening agent used when preparing four polyurea grease of composite calcium-base in embodiment 3 And used preparation method prepares four polyurea grease of composite calcium-base, by the organic diamine in the synthesis of four polyurea compounds Diaminodiphenylmethane replaces with ethylenediamine to prepare four polyurea grease of composite calcium-base.
Prepared composite calcium in four polyurea grease of composite calcium-base prepared by the embodiment of the present invention 1-3 and comparative example The performance test results of four polyurea grease of base are as shown in table 1 below:
Table 1
The four polyurea grease data of composite calcium-base as prepared by products obtained therefrom detection data of the present invention and common organic diamine Comparison is it can be seen that a kind of four polyurea grease of composite calcium-base of the present invention has good lubricity, adhesiveness, resistance to height Warm nature and excellent mechanical stability, extreme pressure anti-wear and anti-water drenching.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of four polyurea grease of composite calcium-base, it is characterised in that: according to mass percentage, raw material is by following components group At:
Base oil 70-82%, thickening agent 15-30%, additive 1-4%;
Wherein, the thickening agent is made of diisocyanate, organic amine, binary acid, calcium hydroxide.
2. four polyurea grease of composite calcium-base according to claim 1, it is characterised in that: each component of the thickening agent accounts for The percentage composition of four polyurea grease raw material of composite calcium-base are as follows:
Diisocyanate 6-10%, organic amine 4-7.1%, binary acid 1.5-3.5%, calcium hydroxide 5-7%.
3. four polyurea grease of composite calcium-base according to claim 1, it is characterised in that: the base oil be mineral oil, One of synthetic oil, vegetable oil or a variety of mixtures.
4. four polyurea grease of composite calcium-base according to claim 1 or 2, it is characterised in that: the diisocyanate is Toluene di-isocyanate(TDI), methyldiphenyl diisocyanate, '-diphenylmethane diisocyanate, xylylene diisocyanate, One of 4,4- methyl diphenylene diisocyanate is a variety of.
5. four polyurea grease of composite calcium-base according to claim 1 or 2, it is characterised in that: the organic amine is organic The mixture of monoamine and organic diamine.
6. four polyurea grease of composite calcium-base according to claim 5, it is characterised in that: the organic monoamine is 18 One of amine, lauryl amine, tetradecy lamine, para-totuidine, cyclohexylamine, parachloroanilinum, m-chloroaniline, aniline or a variety of mixing Object;The organic diamine be p-phenylenediamine, o-phenylenediamine, the aromatic amine of 4,4- benzidine, ethylenediamine, propane diamine, 1,6- oneself One of the straight-chain fatty amine of diamines, diaminodiphenylmethane or a variety of mixtures.
7. four polyurea grease of composite calcium-base according to claim 1 or 2, it is characterised in that: the acid anhydrides is succinic acid Acid anhydride.
8. four polyurea grease of composite calcium-base according to claim 1, it is characterised in that: the additive is organic amine- The mixture of phenolic antioxidant and anticorrosive antirust agent.
9. four polyurea grease of composite calcium-base according to claim 1, it is characterised in that: according to mass percentage, Raw material is composed of the following components: base oil 72-80%, diisocyanate 6.5-9.5%, organic monoamine 4-5.5%, organic diamine 1-2%, succinic anhydride 1.5-2.5%, calcium hydroxide 5.5-7%, additive 1-3%.
10. a kind of preparation method of four polyurea grease of composite calcium-base, it is characterised in that: the following steps are included:
(1) base oil and organic diamine are added to reaction kettle, are warming up to 80 DEG C of progress heating stirring dissolutions;
(2) diisocyanate is added in the mixture that step (1) obtains, and dissolved, is transferred in reaction kettle, 80 DEG C into Row isothermal reaction 60min;
(3) organic monoamine is added in the mixture that step (2) obtains, and dissolved, it is in a kettle, anti-in 80 DEG C of temperature 40min is answered, reaction kettle is then warming up to 95 DEG C and adds distilled water and reacts 40min under the conditions of this temperature;
(4) acid anhydrides is added in the mixture that solution is obtained to step (3), and dissolved, be then warming up to 120 DEG C in reaction kettle, Carry out isothermal reaction 60min;
(5) calcium hydroxide and distilled water are weighed and is added to reaction kettle after carrying out Hybrid Heating dissolution, while additive being added To reaction kettle, the isothermal reaction 40min at 120 DEG C;
(6) reaction kettle is warming up to 205 DEG C of progress high temperature refining 15min, cools down, grind by stirring, degassing obtains described multiple Close four polyurea grease of calcium base.
CN201910227265.8A 2019-03-25 2019-03-25 A kind of four polyurea grease of composite calcium-base and preparation method thereof Withdrawn CN109852454A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303977A (en) * 2020-03-24 2020-06-19 青岛中科润美润滑材料技术有限公司 Lubricating grease for continuous casting machine and preparation method thereof
CN115247094A (en) * 2022-08-12 2022-10-28 福建优立盛油脂有限公司 Polyurea-anhydrous calcium-based lubricating grease and preparation method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111303977A (en) * 2020-03-24 2020-06-19 青岛中科润美润滑材料技术有限公司 Lubricating grease for continuous casting machine and preparation method thereof
CN115247094A (en) * 2022-08-12 2022-10-28 福建优立盛油脂有限公司 Polyurea-anhydrous calcium-based lubricating grease and preparation method thereof

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