CN104830403B - A kind of Hmp grease thickening thickening agent - Google Patents

A kind of Hmp grease thickening thickening agent Download PDF

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Publication number
CN104830403B
CN104830403B CN201510206670.3A CN201510206670A CN104830403B CN 104830403 B CN104830403 B CN 104830403B CN 201510206670 A CN201510206670 A CN 201510206670A CN 104830403 B CN104830403 B CN 104830403B
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bentonite
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under
thickening agent
thickening
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CN104830403A (en
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张怀滨
张有连
俞铁明
姜跃平
姜健
张怀辉
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CHANG'AN RENHENG CHEMICAL Co Ltd
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CHANG'AN RENHENG CHEMICAL Co Ltd
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Abstract

The invention discloses a kind of thickening agent thickened for Hmp grease, it is prepared from by following methods:By sodium bentonite under the conditions of 350 ~ 450 DEG C calcination 1h;Add in sulfuric acid solution and 30min is acidified under the conditions of 95 ~ 100 DEG C, flocculate, remove the gred, spent acid, drying are cleaned in filtering;Bentonite after acidifying is placed in ball mill and grinds 4h under 40KHz ul-trasonic irradiation;According to mBentonite:mCoverture=100:0.1 ~ 0.15 configuration quality fraction is 35 ~ 45% dimethyl stearyl benzylamine solution, and the Ultra-fine Bentonite of acquisition is placed in dimethyl stearyl benzylamine solution, 2h is stirred under the conditions of 80 DEG C, is filtered, and is dried, and milling crosses 200 mesh sieves, obtains thickening agent.The thickening agent of the present invention can be applied to prepare Hmp grease.

Description

A kind of Hmp grease thickening thickening agent
Technical field
The invention belongs to chemical field, more particularly to a kind of thickening agent, more specifically, the present invention are used to prepare height to be a kind of The thickening agent of thickening power is played during temperature lubricating grease.
Background technology
Hmp grease is generally used for more than 180 DEG C of use environment, and highest is even up to 800 DEG C or so, using being related to Multiple industries.If the phenomenons such as volatilization, dry and carbon deposit occurs under the high temperature conditions in the Hmp grease that equipment is used, it can make to set It is standby to be carried out under unlubricated state, considerable influence will be produced to equipment, the metal material of equipment can not only be produced at high temperature Thermal deformation, and its intensity can also reduce, and reduce the service life of equipment, lubrication accident occurs when serious, causes equipment to transport Row is stuck and rests.
The thickening agent that Hmp grease is used is generally complex lithium, polyureas and silica, and complex lithium and polyureas are increasingly high High price is brought to the use enterprise of Hmp grease greatly uses pressure, and silica is generally difficult to meet higher again Use requirement.At present, organobentonite is gradually shown solely with its exclusive characteristic in Hmp grease with thickening agent field Special advantage.
Bentonite grease is the important nonsoap grease of class, is to be thickened mineral lubricating oil or synthesis with modified alta-mud High temperature lubricating fat prod prepared by lubricating oil, not only with good heat resistance, while having good mechanical stability and glue Body stability.Heat-resisting bentonite grease and extreme-pressure bentonite grease lubricant using organobentonite as thickening agent can be answered widely For general agricultural machinery, general industry machinery, it is particularly suitable for metallurgical equipment, casting and steel rolling equipment, mine heavy-duty machinery is set The fields such as standby, large-scale truck, papermaking equipment, cement manufacture plant, high temp tunnel kiln car.In addition, bentonite grease Occupy critical role in aviation grease product.
The content of the invention
It is an object of the invention to provide a kind of Hmp grease thickening thickening agent.
To achieve these goals, the present invention uses following technical scheme:
A kind of Hmp grease thickening thickening agent, it is characterised in that be prepared from by following methods:
(1) by sodium bentonite under the conditions of 350~450 DEG C calcination 1h;
(2) prepare mass fraction be 17~19% sulfuric acid solution, add step (1) obtain bentonite, bentonite with The solid-liquid mass ratio of sulfuric acid solution is 2.10~2.30:30min is stirred under the conditions of 1,95~100 DEG C and carries out acidification reaction, is flocculated, Slagging-off, filtering;
(3) material for obtaining step (2) is introduced into standing groove, adds washings, is stirred 1~2 minute, time of repose 45min, extracts supernatant liquor, and cyclic washing 4~9 times is 4~5 to clear liquid pH value, filtered, drying;
(4) bentonite for obtaining step (3) is put into ball mill, is ground 4h under 40KHz ul-trasonic irradiation, is obtained super Thin bentonite;
(5) m is pressedBentonite:mCoverture=100:The Ultra-fine Bentonite that 0.1~0.15 ratio obtains step (4) adds quality Fraction for 35~45% organic covering agent solution in, stir 2h under the conditions of 80 DEG C;
(6) by the material obtained by step (5) through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, and 200 are crossed after milling Mesh sieve, obtains Hmp grease thickening thickening agent.
Further, the quality of step (3) described washings obtains 6 times of quality of material by step (2).
Calcination temperature described in step (1) is 380 DEG C.
Organic coverture described in step (5) is dimethyl stearyl hexadecyldimethyl benzyl ammonium.
Obtained Hmp grease thickening can be applied to prepare Hmp grease with thickening agent according to the method described above.
The specific steps of the above method are further described below:
1. calcination bentonite.Sodium bentonite is subjected to calcination at a certain temperature, removes a part of interlayer in bentonite Water and water is combined, increase bentonite bedding void, make its loose.Temperature is suitable, it is ensured that removes intermediary water and combines water, and not Can be too high and bentonite is sintered.Suitable temperature is 350~450 DEG C, preferably 380 DEG C.
2. acid activation.The sulfuric acid solution of certain mass fraction is prepared, adding step (1) by certain solid-liquid mass ratio obtains Bentonite, stirring 30min carries out acidification reaction under the conditions of 95~100 DEG C, flocculates, and removes the gred, filtering.The quality of sulfuric acid solution point Number is 17~19%, and the solid-liquid mass ratio of bentonite and sulfuric acid solution is 2.10~2.30:1.
3. clean spent acid.The material that step 2 is obtained is introduced into standing groove, adds a certain amount of water, is stirred 1~2 minute, Time of repose is 45min, extracts supernatant liquor out, and cyclic washing to clear liquid pH value is 4~5, is filtered, drying.The quality of water is step Rapid 2 obtain 6 times of quality of material.
4. ultrasonic grind.The bentonite that step 3 is obtained is put into ball mill, is ground under 40KHz ul-trasonic irradiation Grind 4h.Obtain Ultra-fine Bentonite.
5. organic coverture covering.The Ultra-fine Bentonite that step 4 is obtained in proportion adds the organic of certain mass fraction Cover in agent solution, 2h is stirred under the conditions of 80 DEG C.The mass ratio of Ultra-fine Bentonite and organic coverture is mBentonite:mCoverture=100: 0.1~0.15, the mass fraction of organic coverture aqueous solution is 35~45%, and organic coverture is dimethyl stearyl benzyl Ammonium.
6. by the material obtained by step 5 through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, and 200 mesh are crossed after milling Sieve, obtains Hmp grease thickening thickening agent.
The present invention first by sodium bentonite calcination, add bentonitic bedding void, using sodium bentonite sun from Sub- commutativity, by sulfuric acid activated, with the H of inorganic acid+Replace the Na between bentonite bed+, the space of structure cell is increased, is expanded Cavity, has dredged cavity, has increased specific surface area, enhanced surface-active, added ion exchange property so that acidifying Bentonite possesses the properties such as generation Inter layer adsorption, bonding and absorption electronic action.Meanwhile, reach the bentonitic purpose of purification.It is logical Ultrasonic grind is crossed, bentonitic specific surface area and electronegativity is further improved.Utilize the special chemistry of quaternary ammonium salt organic matter Structure, by intercalation modifying, forms organic covering on bentonite surface, improves bentonite for hydroxyl and carboxyl isopolarity group With good compatibility, good thickening effect is played during Hmp grease is prepared as thickening agent.
Embodiment
Embodiment 1
1050kg sodium bentonites are taken, the calcination 1h at 350 DEG C.
The sulfuric acid solution that 500kg mass fractions are 17% is prepared, stirring 30min is carried out at acid activation under the conditions of 95 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.1 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 35% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 2
1070kg sodium bentonites are taken, the calcination 1h at 370 DEG C.
The sulfuric acid solution that 500kg mass fractions are 17.4% is prepared, stirring 30min is carried out at acid activation under the conditions of 96 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.11 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 37% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 3
1090kg sodium bentonites are taken, the calcination 1h at 390 DEG C.
The sulfuric acid solution that 500kg mass fractions are 17.8% is prepared, stirring 30min is carried out at acid activation under the conditions of 97 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.12 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 39% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 4
1110kg sodium bentonites are taken, the calcination 1h at 410 DEG C.
The sulfuric acid solution that 500kg mass fractions are 18.2% is prepared, stirring 30min is carried out at acid activation under the conditions of 98 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.13 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 41% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 5
1130kg sodium bentonites are taken, the calcination 1h at 430 DEG C.
The sulfuric acid solution that 500kg mass fractions are 18.6% is prepared, stirring 30min is carried out at acid activation under the conditions of 99 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.14 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 43% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 6
1150kg sodium bentonites are taken, the calcination 1h at 450 DEG C.
The sulfuric acid solution that 500kg mass fractions are 19% is prepared, stirring 30min is carried out at acid activation under the conditions of 100 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.15 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 45% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 7
1150kg sodium bentonites are taken, the calcination 1h at 380 DEG C.
The sulfuric acid solution that 500kg mass fractions are 17% is prepared, stirring 30min is carried out at acid activation under the conditions of 95 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.1 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 45% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Embodiment 8
1050kg sodium bentonites are taken, the calcination 1h at 380 DEG C.
The sulfuric acid solution that 500kg mass fractions are 19% is prepared, stirring 30min is carried out at acid activation under the conditions of 95 DEG C Put.Flocculation, removes the gred, filtering.
6 times by quality of material is obtained add a certain amount of water cleaning spent acid, stir 60s, stand 45min, extract upper strata out Clear liquid, it is 4~5 to clean repeatedly to supernatant liquor pH value.Filtering, drying.
Bentonite after drying is put into ball mill, 4h is ground under 40KHz ul-trasonic irradiation, ultra-fine swelling is prepared Soil.
By mBentonite:mCoverture=100:0.15 adds the Ultra-fine Bentonite of acquisition the dimethyl 18 that mass fraction is 35% In alkyl benzyl ammonium salt solution, 2h is stirred under the conditions of 80 DEG C.
By the material after organic covering through flocculation, filtering is dried under the conditions of being transferred to 30 DEG C, 200 mesh sieves is crossed after milling, are obtained Obtain Hmp grease thickening thickening agent.
Product of the present invention is applied to after certain model Hmp grease as thickening agent, and Hmp grease technical indicator is seen below Table:
The thickening agent of the present invention can be used for preparing Hmp grease.

Claims (3)

1. a kind of Hmp grease thickening thickening agent, it is characterised in that be prepared from by following methods:
(1)By sodium bentonite under the conditions of 350 ~ 450 DEG C calcination 1h;
(2)The sulfuric acid solution that mass fraction is 17 ~ 19% is prepared, step is added(1)The bentonite of acquisition, bentonite is molten with sulfuric acid The solid-liquid mass ratio of liquid is 2.10 ~ 2.30:30min is stirred under the conditions of 1,95 ~ 100 DEG C and carries out acidification reaction, is flocculated, slagging-off, Filtering;
(3)By step(2)The material of acquisition is introduced into standing groove, adds washings, is stirred 1~2 minute, time of repose 45min, Supernatant liquor is extracted, cyclic washing 4~9 times is 4~5 to clear liquid pH value, filtered, drying;
(4)By step(3)The bentonite of acquisition is put into ball mill, and 4h is ground under 40KHz ul-trasonic irradiation, obtains ultra-fine swollen Profit soil;
(5)By mBentonite:mCoverture=100:0.1 ~ 0.15 ratio is by step(4)The Ultra-fine Bentonite of acquisition adds mass fraction In 35 ~ 45% organic covering agent solution, 2h is stirred under the conditions of 80 DEG C;Described organic coverture is dimethyl stearyl benzyl Base ammonium;
(6)By step(5)Obtained material is dried through flocculation, filtering under the conditions of being transferred to 30 DEG C, and 200 mesh sieves are crossed after milling, Obtain Hmp grease thickening thickening agent.
2. Hmp grease thickening thickening agent as claimed in claim 1, it is characterised in that:Step(3)The washings Quality is step(2)6 times of obtained quality of material.
3. Hmp grease thickening thickening agent as claimed in claim 1, it is characterised in that:Step(1)Described calcination temperature Spend for 380 DEG C.
CN201510206670.3A 2015-04-28 2015-04-28 A kind of Hmp grease thickening thickening agent Active CN104830403B (en)

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Publication number Priority date Publication date Assignee Title
CN111996064A (en) * 2020-09-23 2020-11-27 上海虎头化工有限公司 Ultrahigh-temperature lubricating grease and preparation method thereof
CN113308289B (en) * 2021-05-26 2022-05-31 安徽博洋润滑科技有限公司 Lubricating grease for drill chuck and preparation method thereof

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Denomination of invention: A Thickening Agent for High Temperature Lubricating Greases

Effective date of registration: 20231115

Granted publication date: 20170912

Pledgee: Changxin Zhejiang rural commercial bank Limited by Share Ltd.

Pledgor: ZHEJIANG CHANGAN RENHENG TECHNOLOGY CO.,LTD.

Registration number: Y2023980065649