CN103361151A - Lubricant composite, preparation method thereof and trace lubricant made of same - Google Patents

Lubricant composite, preparation method thereof and trace lubricant made of same Download PDF

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Publication number
CN103361151A
CN103361151A CN2013103205865A CN201310320586A CN103361151A CN 103361151 A CN103361151 A CN 103361151A CN 2013103205865 A CN2013103205865 A CN 2013103205865A CN 201310320586 A CN201310320586 A CN 201310320586A CN 103361151 A CN103361151 A CN 103361151A
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lubricant
hydramine
carboxylic acid
acid
lubricant compositions
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CN103361151B (en
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张乃庆
吴启东
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Shenzhen Long Wei Technology Development Co., Ltd.
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Shanghai Jinzhao Energy Saving Technology Co Ltd
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Abstract

The invention provides a lubricant composite, a preparation method thereof and a method of preparing a lubricant made of the lubricant composite. The lubricant composite is characterized by being made of boric acid, hydramine, carboxylic acid and polyethylene glycol, wherein the mol ratio of boric acid to hydramine to carboxylic acid is 1:1 to 4: 1 to 1.5, and the weight of polyethylene glycol is 25 to 30% of the total weight of the reaction product of boric acid, hydramine and lauric acid. The trace lubricant prepared with the lubricant composite has the advantages of excellent lubricity, cooling ability, extreme pressure anti-wear property and good rust-proof ability. Just a little trace lubricant can satisfy the needs of lubricating, cooling, extreme pressure anti-wearing and rust preventing for the metal processing. The trace lubricant can be corporately used with a trace lubricant device, the usage amount of cutting fluid can be reduced by 90%, the oil spray system of the trace lubricant device will not be obstructed after being used for a long time, and has prominent effects on energy saving, discharge reducing and environmental protecting.

Description

A kind of lubricant compositions and preparation method thereof and with the agent of said composition preparation micro lubricating
Technical field
The invention belongs to lubrication technical field, relate to a kind of lubricant compositions and preparation method thereof and prepare the micro lubricating agent with said composition.
Background technology
It is lubricated that traditional metal cutting processing employing mineral oil or vegetables oil or cutting fluid are carried out a large amount of shower formulas, the usage quantity of lubricant is large, not only waste resource, cause the huge pollution of processing site and environment, also can have a strong impact on the healthy of operator simultaneously, for addressing these problems, in the recent period the research of Minimal Quantity Lubrication Technology obtained certain progress, it is large that Minimal Quantity Lubrication Technology has solved above lubricant usage quantity, the problem such as seriously polluted, but to the research of micro lubricating agent, the non-ferrous metals processings such as aluminium alloy have had larger breakthrough, and commercialization, but the micro lubricating agent research for ferrous metal, although certain progress is arranged, also there is certain problem in application facet, mainly be that the lubrication and cooling problem can not well solve.
It is disclosed a kind of stainless steel coolant for oil-less lubrication system of Chinese patent of CN101362981 and its production and use such as publication number, adopt: base oil 25%, compound phosphoric acid fat 50%, potassium borate 10%, tensio-active agent 10% and rust-preventive agent 5% is prepared from, add the stainless steel processing micro cutting liquid that uses after the 1-5 complete emulsification of water doubly during use, find through experiment, add man-hour machined surface smooth finish at stainless steel cutting better, also significantly reduce with oil mass, but because used working fluid is emulsion, often use after for some time the injection system with minimum quantity lubrication device to stop up, the lubricating system with trace amount fault is many, causes the workman that resentment is arranged in use.
In addition, be the disclosed a kind of Gear Processing micro cutting liquid of Chinese patent of CN102936530 such as publication number, adopt: the Gear Processing micro cutting liquid that water soluble polyether 40-70%, petroleum sodium sulfonate 3-5%, sodium-chlor 1-3%, Sulfothiorine 1-3%, tripoly phosphate sodium STPP 1-3%, Sodium Benzoate 0.2-0.5%, dimethyl silicone oil 0.05%-0.1% and excess water process, adding man-hour, also be significantly to reduce with oil mass, but sticking considering to be worth doing seriously on workpiece and the cutter affects cutter life after processing for some time.
Summary of the invention
In view of above defective, the objective of the invention is to overcome the deficiencies in the prior art, a kind of lubricant compositions and preparation method thereof is provided and prepares the micro lubricating agent with said composition.
For achieving the above object, a kind of lubricant compositions provided by the invention is characterised in that, is prepared from by boric acid, hydramine, carboxylic acid and polyoxyethylene glycol, and wherein, boric acid: hydramine: the mol ratio of carboxylic acid is 1:1~4:1~1.5; The weight of polyoxyethylene glycol is 25~30% of boric acid, hydramine and carboxylic acid gross weight.In addition, boric acid: the mol ratio of hydramine is preferred 1:3~4.
A kind of lubricant compositions provided by the invention also has such technical characterictic: hydramine is one or more the mixture in Monoethanolamine MEA BASF, diethanolamine, trolamine, α-amino isopropyl alcohol, the methyldiethanolamine.
In addition, a kind of lubricant compositions provided by the invention also has such technical characterictic: carboxylic acid is that carbonatoms is 8~18 saturated carboxylic acid or one or more the mixture in the unsaturated carboxylic acid.
In addition, a kind of lubricant compositions provided by the invention also has such technical characterictic: the molecular weight of polyoxyethylene glycol is 200~600.
In addition, the preparation method of above-mentioned a kind of lubricant compositions provided by the invention is characterized in that, adopts following steps:
Step 1, boric acid and hydramine are added in the reactor, be heated with stirring to 120~130 ℃, react the moisture that the reaction generation is discharged in decompression after 3~4 hours;
Herein, take the reaction of boric acid and Monoethanolamine MEA BASF as example, its reaction equation is as follows:
B(OH) 3+3HOCH 2CH 2NH 2B(OCH 2CH 2NH 2) 3+3H 2O
Step 2, carboxylic acid is added in the reactor behind the completing steps one, stir and be warming up to 170~180 ℃, react 1~2 hour, the moisture of reaction generation is discharged in decompression;
Herein, take the carboxylic acid that adds as lauric acid as example, its main reaction equation is as follows:
CH 3(CH 2) 10COOH+HOCH 2CH 2NH 2CH 3(CH 2) 10COOCH 2CH 2NH 2+H 2O
Owing to not strengthening acid catalysis, above reaction is also insufficient.
So actual mixture for triethanolamine borate ester, bay thanomin ester, lauric acid and a small amount of boric acid, Monoethanolamine MEA BASF of the compound that above reaction generates.
Step 3, the decompression of the reactor behind completing steps two are cooled to 100~110 ℃, add polyoxyethylene glycol and keep constant temperature to stir 1~2 hour, and moisture is removed in decompression, prepares a kind of lubricant compositions.
The main purpose of above-mentioned steps is to allow polyoxyethylene glycol and residue lauric acid react the generation nonionic surface active agent, makes the water-soluble better of solution.
Reaction process is as follows:
CH 3(CH 2) 10COOH+HO(CH 2CH 2O) nHCH 3(CH 2) 10COO(CH 2CH 2O) nH+H 2O
(wherein: n=3~14)
In addition, the present invention also provides a kind of using method of above-mentioned lubricant compositions, it is characterized in that: for the preparation of the micro lubricating agent.
In addition, the present invention also provides a kind of micro lubricating agent of adopting above-mentioned lubricant compositions preparation, it is characterized in that, and is composed of the following components:
Figure BDA00003574337200031
Get final product when in the preparation, above-mentioned each component being mixed to transparent or semitransparent shape.
In addition, above-mentioned micro lubricating agent provided by the invention also has such feature: phosphoric acid salt is one or more the mixture in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, Potassium tripolyphosphate, hexa metaphosphoric acid potassium, dipotassium hydrogen phosphate, the potassium primary phosphate.
In addition, above-mentioned micro lubricating agent provided by the invention also has such feature: defoamer is one or more the mixture in polyethers defoamer, dimethyl silicone oil, Siloxane-Oxyalkylene Copolymers, higher alcohols defoamer, polysiloxane defoamers, the fatty acid ester compounded thing of higher alcohols, polyoxyethylene polyoxypropylene tetramethylolmethane ether, polyoxyethylene polyoxy propyl alcohol amidogen ether, polypropylene glycerol aether and the polyoxypropylene.The higher alcohols defoamer can be selected from alcohol, phenylethyl alcohol oleic acid ester, toluylic acid bay alcohol ester, tributyl phosphate of C7~C9 etc.Polyether-modified silicon is polyether siloxane copolymers.
Effect and the effect of invention
The micro lubricating agent of the preparation of a kind of lubricant compositions of employing the present invention preparation, have excellent oilness, cooling, extreme pressure anti-wear and good rust-preventing characteristic, a small amount of micro lubricating agent just can be satisfied lubrication, extreme-pressure anti-wear and the antirust requirement of metal processing; Cooperate minimum quantity lubrication device to use, can save the usage quantity of cutting fluid more than 90%, also the injection system of minimum quantity lubrication device can not stopped up after using time for some time, and energy-saving and emission-reduction, environmental protection effect are remarkable.
Embodiment
Embodiment one
The agent of 1# micro lubricating
Step 1: by taking by weighing 61.83kg(1000mol) boric acid and 213.79kg(3500mol) Monoethanolamine MEA BASF adds in the reactor and is heated with stirring to 125 ℃, react the moisture that the reaction generation is discharged in decompression after 3.5 hours;
Step 2: take by weighing in the still of 250.4kg (1250mol) lauric acid adding step 1 reaction, stir and be warming up to 175 ℃, reacted 1.5 hours, decompression is discharged and is reacted the moisture that generates;
Step 3: when step 2 decompression is cooled to 105 ℃, add 147.29kg(above-mentioned steps raw material gross weight 28%) polyoxyethylene glycol (PEG400), keep constant temperature to stir 1.5 hours, moisture is removed in decompression.Prepare a kind of lubricant compositions.
Step 4: the lubricant compositions 100kg that gets the step 3 preparation adds the dipotassium hydrogen phosphate of 2.5kg, the defoamer dimethyl silicone oil of 0.3kg EDTA-2Na, 0.05kg, the water of 500kg, is micro lubricating agent working fluid when mixing into transparent or semitransparent shape.
The effect of embodiment one:
The agent of 1# micro lubricating is carried out the test of four ball extreme pressures, test-results: P with the GB/T12583 experimental technique D620 (kgf).
It is the stainless steel bar that Φ 68mm is cut in the sawing of 800m/min high-velocity zone that the agent of 1# micro lubricating is applied to linear velocity, originally carried out the lubrication by oil circulation cooling with emulsion, change now KS-2106 minimum quantity lubrication device (U-shaped nozzle, 2 fluid/pores) and a kind of micro lubricating agent into, result such as following table:
Project Before the transformation After the transformation
Cut a cutter required time 90 seconds 90 seconds
The saw blade mean lifetime 4/month 1/month
Lubricant consumes 25kg/ days 0.4kg/ my god
The job site Cutting fluid flows everywhere, and is on-the-spot dirty and messy Very clean
The agent of 1# micro lubricating is applied to the turbine hobbing processing of alteration 380mm, before with normal hydraulic oil oil bath lubrication processing.Use lubricating system with trace amount (KS-2105 minimum quantity lubrication device 3 nozzles+micro lubricating agent) correctional effect contrast table:
Project Before the transformation After the transformation
The every hobbing of turbine is the required time once 60 seconds 45 seconds
Hobber sharpening number of times Two class's mills once Three class's mills once
Lubricant consumes 4kg/ days 0.4kg/ my god
The job site The typical case is filthy Very clean
Aftertreatment The processing costs of workpiece oil contamination is large Without aftertreatment
Use lubricating system with trace amount and transform the sticking bits of nothing on post-treatment turbine and the hobber, the turbine surfaces temperature is normal, can take with hand.
Embodiment two
The agent of 2# micro lubricating
Step 1: by taking by weighing 61.83kg(1000mol) boric acid and 157.71kg(1500mol) diethanolamine adds in the reactor and is heated with stirring to 120 ℃, react the moisture that the reaction generation is discharged in decompression after 3 hours;
Step 2: take by weighing in the still of 426.72kg (1500mol) stearic acid adding step 1 reaction, stir and be warming up to 170 ℃, reacted 2 hours, decompression is discharged and is reacted the moisture that generates;
Step 3: when step 2 decompression is cooled to 100 ℃, add 161.57kg(above-mentioned steps raw material gross weight 25%) polyoxyethylene glycol (PEG200), keep constant temperature to stir 1.5 hours, moisture is removed in decompression.Prepare a kind of lubricant compositions.
Step 4: get the lubricant compositions 100kg adding 1kg Sodium hexametaphosphate 99 of step 3 preparation and the mixture of 1kg Sodium phosphate dibasic, the defoamer Siloxane-Oxyalkylene Copolymers of 0.5kg EDTA-4Na, 0.01kg, the water of 100kg, be micro lubricating agent working fluid when mixing into transparent or semitransparent shape.
Embodiment three
The agent of 3# micro lubricating
Step 1: by taking by weighing 61.83kg(1000mol) boric acid and 179.03kg(1200mol) trolamine adds in the reactor and is heated with stirring to 120 ℃, react the moisture that the reaction generation is discharged in decompression after 4 hours;
Step 2: take by weighing in the still of 282.47kg (1000mol) oleic acid adding step 1 reaction, stir and be warming up to 180 ℃, reacted 1 hour, decompression is discharged and is reacted the moisture that generates;
Step 3: when step 2 decompression is cooled to 110 ℃, add 157kg(above-mentioned steps raw material gross weight 30%) polyoxyethylene glycol (PEG600), keep constant temperature to stir 1 hour, moisture is removed in decompression.Prepare a kind of lubricant compositions.
Step 4: the lubricant compositions 100kg that gets the step 3 preparation adds 3kg hexa metaphosphoric acid potassium, the defoamer Siloxane-Oxyalkylene Copolymers of 0.1kg, the water of 1000kg, is micro lubricating agent working fluid when mixing into transparent or semitransparent shape.
Embodiment four
The agent of 4# micro lubricating
Step 1: by taking by weighing 61.83kg(1000mol) boric acid and 300.44kg(4000mol) α-amino isopropyl alcohol adds in the reactor and is heated with stirring to 130 ℃, react the moisture that the reaction generation is discharged in decompression after 3 hours;
Step 2: take by weighing in the still of 307.7kg (1200mol) palmitinic acid adding step 1 reaction, stir and be warming up to 175 ℃, reacted 1.8 hours, decompression is discharged and is reacted the moisture that generates;
Step 3: when step 2 decompression is cooled to 108 ℃, add 194.29kg(above-mentioned steps raw material gross weight 29%) polyoxyethylene glycol (PEG300), keep constant temperature to stir 2 hours, moisture is removed in decompression.Prepare a kind of lubricant compositions.
Step 4: get the lubricant compositions 100kg adding 1.8kg tripoly phosphate sodium STPP of step 3 preparation and the mixture of 1kg SODIUM PHOSPHATE, MONOBASIC, the defoamer polypropylene glycerol aether of 0.2kg EDTA-4Na, 0.02kg, the water of 600kg, be micro lubricating agent working fluid when mixing into transparent or semitransparent shape.
Embodiment five
The agent of 5# micro lubricating
Step 1: by taking by weighing 61.83kg(1000mol) boric acid and 130kg(1600mol) mixture of diethanolamine and Monoethanolamine MEA BASF, add in the reactor and be heated with stirring to 125 ℃, react the moisture that the reaction generation is discharged in decompression after 4 hours;
Step 2: take by weighing in the still of the sad adding step 1 reaction of 201.94kg (1400mol), stir and be warming up to 170 ℃, reacted 2 hours, the moisture that reaction generates is discharged in decompression;
Step 3: when step 2 decompression is cooled to 110 ℃, add 98.44kg(above-mentioned steps raw material gross weight 25%) polyoxyethylene glycol (PEG500), keep constant temperature to stir 2 hours, moisture is removed in decompression.Prepare a kind of lubricant compositions.
Step 4: the lubricant compositions 100kg that gets the step 3 preparation adds 2.2kg tripoly phosphate sodium STPP, the defoamer toluylic acid bay alcohol ester of 0.1kgEDTA-2Na, 0.08kg, the water of 200kg, is micro lubricating agent working fluid when mixing into transparent or semitransparent shape.
Because the micro lubricating agent of above-mentioned 2#~5# and 1# system are with a series of micro lubricating agent, it has the experiment effect suitable with the agent of 1# micro lubricating, does not do repeat specification herein.

Claims (9)

1. lubricant compositions is characterized in that: is prepared from by boric acid, hydramine, carboxylic acid and polyoxyethylene glycol, wherein,
Boric acid: hydramine: the mol ratio of carboxylic acid is 1:1~4:1~1.5;
The weight of polyoxyethylene glycol is 25~30% of boric acid, hydramine and carboxylic acid gross weight.
2. a kind of lubricant compositions as claimed in claim 1 is characterized in that:
Described boric acid: hydramine: the mol ratio of carboxylic acid is 1:3~4:1~1.5.
3. a kind of lubricant compositions as claimed in claim 1 is characterized in that:
Described hydramine is one or more the mixture in Monoethanolamine MEA BASF, diethanolamine, trolamine, α-amino isopropyl alcohol, the methyldiethanolamine.
4. a kind of lubricant compositions as claimed in claim 1 is characterized in that:
Described carboxylic acid is that carbonatoms is 8~18 saturated carboxylic acid or one or more the mixture in the unsaturated carboxylic acid.
5. a kind of lubricant compositions as claimed in claim 1 is characterized in that:
The molecular weight of described polyoxyethylene glycol is 200~600.
6. such as the preparation method of the described a kind of lubricant compositions of claim 1-5, it is characterized in that, adopt following steps:
Step 1, boric acid and hydramine are added in the reactor, be heated with stirring to 120~130 ℃, react the moisture that the reaction generation is discharged in decompression after 3~4 hours;
Step 2, carboxylic acid is added in the reactor behind the completing steps one, stir and be warming up to 170~180 ℃, react 1~2 hour, the moisture of reaction generation is discharged in decompression;
Step 3, the decompression of the reactor behind completing steps two are cooled to 100~110 ℃, add polyoxyethylene glycol and keep constant temperature to stir 1~2 hour, and moisture is removed in decompression.
7. with a kind of micro lubricating agent such as the arbitrary described a kind of lubricant compositions preparation of claim 1-5, it is characterized in that, composed of the following components:
Figure FDA00003574337100021
8. a kind of micro lubricating agent as claimed in claim 7 is characterized in that:
Described phosphoric acid salt is one or more the mixture in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, Sodium phosphate dibasic, SODIUM PHOSPHATE, MONOBASIC, Potassium tripolyphosphate, hexa metaphosphoric acid potassium, dipotassium hydrogen phosphate, the potassium primary phosphate.
9. a kind of micro lubricating agent as claimed in claim 7 is characterized in that:
Described defoamer is one or more the mixture in polyethers defoamer, dimethyl silicone oil, polyether-modified silicon, higher alcohols defoamer, polysiloxane defoamers, the fatty acid ester compounded thing of higher alcohols, polyoxyethylene polyoxypropylene tetramethylolmethane ether, polyoxyethylene polyoxy propyl alcohol amidogen ether, polypropylene glycerol aether and the polyoxypropylene.
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CN103601846A (en) * 2013-11-04 2014-02-26 上海金兆节能科技有限公司 Polyisobutene butane diacid amide and preparation method thereof as well as minimal quantity lubricating oil prepared from polyisobutene butane diacid amide
CN103740442A (en) * 2013-12-18 2014-04-23 张家港市林达外加剂厂 Rust-proof lubricating oil
CN104277895A (en) * 2014-09-25 2015-01-14 苏州长盛机电有限公司 Chain lubricating oil and preparation method thereof
CN105838513A (en) * 2016-05-18 2016-08-10 大连和田科技有限公司 Preparation method of high-solid content heavy-oil cleaning agent
CN108587755A (en) * 2018-06-30 2018-09-28 广西牛角科技有限公司 A kind of high heat conduction lubricating oil and preparation method thereof
CN110106013A (en) * 2019-06-10 2019-08-09 上海金兆节能科技有限公司 Boron nitrogen lubricant compositions and preparation method thereof and the combination prepare micro lubricating agent
CN110982061A (en) * 2019-11-05 2020-04-10 名畔科技(镇江)有限公司 Preparation method and application of polyethylene glycol long-chain alkylamide
CN111040828A (en) * 2019-12-25 2020-04-21 上海金兆节能科技有限公司 Trace lubricant of lubricating composition containing phosphorus, boron and nitrogen and preparation method thereof
CN112175689A (en) * 2020-10-13 2021-01-05 上海贝能环保科技有限公司 Antirust agent composition and preparation method thereof

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CN103601846A (en) * 2013-11-04 2014-02-26 上海金兆节能科技有限公司 Polyisobutene butane diacid amide and preparation method thereof as well as minimal quantity lubricating oil prepared from polyisobutene butane diacid amide
CN103601846B (en) * 2013-11-04 2015-11-11 上海金兆节能科技有限公司 Polyisobutene butylene diamide and preparation method thereof and prepare micro lubricating agent with this acid amides
CN103740442A (en) * 2013-12-18 2014-04-23 张家港市林达外加剂厂 Rust-proof lubricating oil
CN104277895A (en) * 2014-09-25 2015-01-14 苏州长盛机电有限公司 Chain lubricating oil and preparation method thereof
CN104277895B (en) * 2014-09-25 2016-08-24 苏州长盛机电有限公司 A kind of chain greasisng oil and preparation method thereof
CN105838513A (en) * 2016-05-18 2016-08-10 大连和田科技有限公司 Preparation method of high-solid content heavy-oil cleaning agent
CN108587755A (en) * 2018-06-30 2018-09-28 广西牛角科技有限公司 A kind of high heat conduction lubricating oil and preparation method thereof
CN108587755B (en) * 2018-06-30 2021-04-27 广西牛角科技有限公司 High-thermal-conductivity lubricating oil and preparation method thereof
CN110106013A (en) * 2019-06-10 2019-08-09 上海金兆节能科技有限公司 Boron nitrogen lubricant compositions and preparation method thereof and the combination prepare micro lubricating agent
CN110106013B (en) * 2019-06-10 2021-12-10 上海金兆节能科技有限公司 Boron-nitrogen lubricant composition, preparation method thereof and trace lubricant prepared by composition
CN110982061A (en) * 2019-11-05 2020-04-10 名畔科技(镇江)有限公司 Preparation method and application of polyethylene glycol long-chain alkylamide
CN111040828A (en) * 2019-12-25 2020-04-21 上海金兆节能科技有限公司 Trace lubricant of lubricating composition containing phosphorus, boron and nitrogen and preparation method thereof
CN112175689A (en) * 2020-10-13 2021-01-05 上海贝能环保科技有限公司 Antirust agent composition and preparation method thereof

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