CN109337656A - A kind of automotive antifreezing liquid and preparation method thereof - Google Patents
A kind of automotive antifreezing liquid and preparation method thereof Download PDFInfo
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- CN109337656A CN109337656A CN201811297790.9A CN201811297790A CN109337656A CN 109337656 A CN109337656 A CN 109337656A CN 201811297790 A CN201811297790 A CN 201811297790A CN 109337656 A CN109337656 A CN 109337656A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/20—Antifreeze additives therefor, e.g. for radiator liquids
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Abstract
The invention discloses a kind of automotive antifreezing liquid and preparation method thereof, by mass percentage, a kind of automotive antifreezing liquid includes following components: 60% ethylene glycol, 2 ~ 4% glycerol, 2 ~ 4% DMF, 1.5 ~ 2.0% triethanolamine, 0.2 ~ 0.3% hydrolyzed maleic anhydride, 0.4 ~ 0.5% sodium polyphosphate, 0.01 ~ 0.03% EDETATE DISODIUM, the linear tetramer of 0.1 ~ 0.2% c-NMF, 0.1 ~ 0.2% metal-organic framework material MOF-5, 0.05 ~ 0.08% PEO-PPO-PEO triblock copolymer, 0.05 ~ 0.08% Emulsifier EL-60 and 0.008 ~ 0.012% methylene blue, surplus is deionized water, it is cooled down with reducing Liquid is in common use environment the advantages of icing possibility.
Description
Technical field
The present invention relates to a kind of automotive antifreezing liquid and preparation method thereof.
Background technique
The engine-cooling system of internal combustion vehicle is the liquid-cooled sealing and circulating body being made of cylinder, collet and water tank
System.The working condition of cooling system directly affects the normal operation of vehicle and the service life of vehicle.
Therefore, the anti-icing fluid for developing a kind of reduction coolant liquid icing possibility in commonly using use environment has centainly
Production application value.
Summary of the invention
The first object of the present invention is to provide a kind of automotive antifreezing liquid, and having reduces coolant liquid ties in common use environment
The advantages of ice possibility.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of automotive antifreezing liquid, by mass percentage, including following components: 60% ethylene glycol, 2~4% glycerol,
2~4% DMF, 1.5~2.0% triethanolamine, 0.2~0.3% hydrolyzed maleic anhydride, 0.4~0.5% poly phosphorus
Sour sodium, 0.01~0.03% EDETATE DISODIUM, the linear tetramer of 0.1~0.2% c-NMF, 0.1~0.2% metal
Organic framework materials MOF-5,0.05~0.08% PEO-PPO-PEO triblock copolymer, 0.05~0.08% polyoxy second
Alkene castor oil and 0.008~0.012% methylene blue, surplus is deionized water.
Further preferably are as follows: by mass percentage, including following components: 60% ethylene glycol, 3% glycerol, 3%
DMF, 1.8% triethanolamine, 0.24% hydrolyzed maleic anhydride, 0.48% sodium polyphosphate, 0.02% EDETATE SODIUM
Salt, the linear tetramer of 0.16% c-NMF, 0.16% metal-organic framework material MOF-5,0.06% PEO-PPO-
PEO triblock copolymer, 0.056% Emulsifier EL-60 and 0.010% methylene blue, surplus are deionized water.
The second object of the present invention is to provide a kind of preparation method of automotive antifreezing liquid.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation method of automotive antifreezing liquid, comprising the following steps: by the ethylene glycol of formula ratio, glycerol, DMF, three second
Hydramine, PEO-PPO-PEO triblock copolymer, Emulsifier EL-60, methylene blue and deionized water are mixed and are uniformly dispersed,
Hydrolyzed maleic anhydride, sodium polyphosphate, EDETATE DISODIUM, the linear tetramer of c-NMF and the metal that formula ratio is added have machine frame
Frame material MOF-5 is dispersed with stirring and uniformly obtains solution, filters to take filtrate；Filtrate is increased to 85~95 DEG C from room temperature and keeps the temperature 1
~2hr, then be cooled to -65~-55 DEG C and keep the temperature 1~2hr, then be warming up to room temperature and keep the temperature 1~2hr, it filters again, filtrate is
For a kind of automotive antifreezing liquid.
Further preferably are as follows: in heating to filtrate and cooling treatment process, heating and cooling rate be 45~55 DEG C/
hr。
Further preferably are as follows: the following steps are included: by the ethylene glycol of formula ratio, glycerol, DMF, triethanolamine, PEO-PPO-
PEO triblock copolymer, Emulsifier EL-60, methylene blue and deionized water are mixed and are uniformly dispersed, and formula ratio is added
Hydrolyzed maleic anhydride, sodium polyphosphate, EDETATE DISODIUM, c-NMF the linear tetramer and metal-organic framework material MOF-5,
It is dispersed with stirring and uniformly obtains solution, filter to take filtrate；It is set to be increased to 90 DEG C from room temperature with the heating rate of 50 DEG C/hr filtrate
And 1.5hr is kept the temperature, then so that it is cooled to -60 DEG C with the rate of temperature fall of 50 DEG C/hr and keep the temperature 1.5hr, then with the heating of 50 DEG C/hr
Rate is allowed to warm to room temperature and keeps the temperature 1.5hr, filters again, and filtrate is a kind of automotive antifreezing liquid；
By mass percentage, a kind of automotive antifreezing liquid includes following components: 60% ethylene glycol, 3% glycerol,
3% DMF, 1.8% triethanolamine, 0.24% hydrolyzed maleic anhydride, 0.48% sodium polyphosphate, 0.02% EDTA
Disodium salt, the linear tetramer of 0.16% c-NMF, 0.16% metal-organic framework material MOF-5,0.06% PEO-
PPO-PEO triblock copolymer, 0.056% Emulsifier EL-60 and 0.010% methylene blue, surplus are deionization
Water.
In conclusion the invention has the following advantages: reduction water freezing point breaches the prior art to -69~-73 DEG C
In minimum (- 68 DEG C), reduce the icing possibility of coolant liquid, suitable for broader environment temperature, applicability is wider；It is anti-
Corrosivity is good, even if being still able to maintain preferable anticorrosive property after placing for a long time under low temperature (test temperature is -60 DEG C).
Specific embodiment
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the protection scope of invention.
It is indicated except no special, the room temperature of the application refers to environment temperature, is 20~30 DEG C.
Embodiment 1: a kind of automotive antifreezing liquid is prepared by following steps:
By ethylene glycol, glycerol, DMF, triethanolamine, PEO-PPO-PEO triblock copolymer (F127 type), polyoxyethylene castor
Sesame oil, methylene blue and deionized water are mixed and are uniformly dispersed, be added hydrolyzed maleic anhydride, sodium polyphosphate, EDETATE DISODIUM,
The linear tetramer and metal-organic framework material MOF-5 of c-NMF (i.e. cis- N-METHYLFORMAMIDE), is dispersed with stirring and uniformly obtains
Solution filters to take filtrate.So that it is increased to 90 DEG C from room temperature with the heating rate of 50 DEG C/hr filtrate and keeps the temperature 1.5hr, then with
The rate of temperature fall of 50 DEG C/hr makes it be cooled to -60 DEG C and keeps the temperature 1.5hr, then is allowed to warm to room with the heating rate of 50 DEG C/hr
Temperature simultaneously keeps the temperature 1.5hr, filters again, filtrate is a kind of automotive antifreezing liquid.
By mass percentage, which includes following components: 60% ethylene glycol, 3% glycerol,
3% DMF, 1.8% triethanolamine, 0.24% hydrolyzed maleic anhydride, 0.48% sodium polyphosphate, 0.02% EDTA
Disodium salt, the linear tetramer of 0.16% c-NMF, 0.16% metal-organic framework material MOF-5,0.06% PEO-
PPO-PEO triblock copolymer, 0.056% Emulsifier EL-60 and 0.010% methylene blue, surplus are deionization
Water.
Embodiment 2: a kind of automotive antifreezing liquid, difference from example 1 is that, by mass percentage, the one kind
Automotive antifreezing liquid includes following components: 60% ethylene glycol, 2% glycerol, 2% DMF, 1.5% triethanolamine, 0.2%
Hydrolyzed maleic anhydride, 0.4% sodium polyphosphate, 0.01% EDETATE DISODIUM, 0.1% c-NMF the linear tetramer,
0.1% metal-organic framework material MOF-5,0.05% PEO-PPO-PEO triblock copolymer (F127 type), 0.05%
Emulsifier EL-60 and 0.008% methylene blue, surplus is deionized water.
Embodiment 3: a kind of automotive antifreezing liquid, difference from example 1 is that, by mass percentage, the one kind
Automotive antifreezing liquid includes following components: 60% ethylene glycol, 4% glycerol, 4% DMF, 2.0% triethanolamine, 0.3%
Hydrolyzed maleic anhydride, 0.5% sodium polyphosphate, 0.03% EDETATE DISODIUM, 0.2% c-NMF the linear tetramer,
0.2% metal-organic framework material MOF-5,0.08% PEO-PPO-PEO triblock copolymer (F127 type), 0.08%
Emulsifier EL-60 and 0.012% methylene blue, surplus is deionized water.
Embodiment 4: a kind of automotive antifreezing liquid, difference from example 1 is that, a kind of automotive antifreezing liquid by with
Lower step preparation: by the ethylene glycol of formula ratio, glycerol, DMF, triethanolamine, PEO-PPO-PEO triblock copolymer (F127
Type), Emulsifier EL-60, methylene blue and deionized water mix and be uniformly dispersed, be added formula ratio hydrolyzed maleic anhydride,
Sodium polyphosphate, EDETATE DISODIUM, c-NMF the linear tetramer and metal-organic framework material MOF-5, be dispersed with stirring uniform
To solution, filtrate is filtered to take.So that it is increased to 85 DEG C from room temperature with the heating rate of 45 DEG C/hr filtrate and keeps the temperature 2hr, then with
The rate of temperature fall of 45 DEG C/hr makes it be cooled to -55 DEG C and keeps the temperature 2hr, then is allowed to warm to room temperature with the heating rate of 45 DEG C/hr
And 2hr is kept the temperature, it filters again, filtrate is a kind of automotive antifreezing liquid.
Embodiment 5: a kind of automotive antifreezing liquid, difference from example 1 is that, a kind of automotive antifreezing liquid by with
Lower step preparation: by the ethylene glycol of formula ratio, glycerol, DMF, triethanolamine, PEO-PPO-PEO triblock copolymer (F127
Type), Emulsifier EL-60, methylene blue and deionized water mix and be uniformly dispersed, be added formula ratio hydrolyzed maleic anhydride,
Sodium polyphosphate, EDETATE DISODIUM, c-NMF the linear tetramer and metal-organic framework material MOF-5, be dispersed with stirring uniform
To solution, filtrate is filtered to take.So that it is increased to 95 DEG C from room temperature with the heating rate of 55 DEG C/hr filtrate and keeps the temperature 1hr, then with
The rate of temperature fall of 55 DEG C/hr makes it be cooled to -65 DEG C and keeps the temperature 1hr, then is allowed to warm to room temperature with the heating rate of 55 DEG C/hr
And 1hr is kept the temperature, it filters again, filtrate is a kind of automotive antifreezing liquid.
Embodiment 6: a kind of automotive antifreezing liquid, difference from example 1 is that, a kind of automotive antifreezing liquid by with
Lower step preparation: by the ethylene glycol of formula ratio, glycerol, DMF, triethanolamine, hydrolyzed maleic anhydride, sodium polyphosphate, EDTA bis-
Sodium salt, the linear tetramer of c-NMF, metal-organic framework material MOF-5, PEO-PPO-PEO triblock copolymer (F127 type),
Emulsifier EL-60, methylene blue and deionized water mixing, are dispersed with stirring and uniformly obtain solution, as a kind of automotive antifreezing
Liquid.
Performance test
One, freezing point is tested
1, test sample: embodiment 1-6 and reference substance 1-4.
Reference substance 1: a kind of anti-icing fluid, by the way that the deionized water of the ethylene glycol of 60wt% and 40wt% is mixed.
Reference substance 2: a kind of anti-icing fluid, by the way that the deionized water of the ethylene glycol of 68wt% and 32wt% is mixed.
Reference substance 3: a kind of anti-icing fluid, by the way that the deionized water of the ethylene glycol of 70wt% and 30wt% is mixed.
Reference substance 4: a kind of anti-icing fluid, by by the triethanolamine of the ethylene glycol of 60wt%, 1.8wt%, 0.24wt%
Hydrolyzed maleic anhydride, the sodium polyphosphate of 0.48wt%, the EDETATE DISODIUM of 0.02wt% and 37.46wt% deionized water
It mixes.
2, it test content: is surveyed referring to national oil chemical industry standard SH/T0090 " engine coolant kryoscopy "
The freezing point of test agent.
3, test result: as shown in table 1.Table 1 is shown:
(1) reference substance 1-3 is only aqueous and ethylene glycol, and the ethylene glycol content in reference substance 1-3 successively increases；Freezing point test
It was found that the freezing point of reference substance 1-3 is respectively -50, -68 and -63 DEG C, illustrate to increase with ethylene glycol content, ethylene glycol and aqueous systems
Freezing point first increases and reduces afterwards, and the freezing point value in the ethylene glycol of 68wt% and the deionized water mixed system of 32wt% is minimum,
I.e. -68 DEG C, the knot of this test discovery and the prior art (" how proper use of anti-icing fluid " that such as Cheng Lili et al. is delivered)
Fruit is consistent；
(2) reference substance 1 is identical with the content of ethylene glycol in reference substance 4；Compared to reference substance 1, also containing specific in reference substance 4
Triethanolamine, hydrolyzed maleic anhydride, sodium polyphosphate, the EDETATE DISODIUM of ratio, but test discovery reference substance 4 and reference substance 1
Freezing point be -50 DEG C, illustrate that the substance additionally added has no significant effect the freezing point of sample；
(3) content of ethylene glycol is identical in reference substance 1, reference substance 4 and embodiment 1-6；Compared to reference substance 1 and reference substance 4,
The freezing point of embodiment 1-6 drops to -69~-73 DEG C from -50 DEG C, declines more obvious and slightly attainable better than the prior art
Optimum level (reference substance 2).
1 freezing point test result of table
Two, corrosion test
1, test sample: embodiment 1-6 and reference substance 1, reference substance 4.
Reference substance 1: a kind of anti-icing fluid, by the way that the deionized water of the ethylene glycol of 60wt% and 40wt% is mixed.
Reference substance 4: a kind of anti-icing fluid, by by the triethanolamine of the ethylene glycol of 60wt%, 1.8wt%, 0.24wt%
Hydrolyzed maleic anhydride, the sodium polyphosphate of 0.48wt%, the EDETATE DISODIUM of 0.02wt% and 37.46wt% deionized water
It mixes.
2, test content: referring to " the code test side of engine coolant corrosion test in glassware ASTM D 1384
Method " it is tested for the property.
3, test result: as shown in table 2.Table 2 is shown: comparing reference substance 1, the corrosion of embodiment 1-6 and reference substance 4 is more
It is small, it complies with standard, wherein the corrosion of embodiment 1-6 is minimum.
2 corrosion test result (unit: mgcm of table-2)
Three, stability test
1, test sample: embodiment 1-6 and reference substance 1, reference substance 4.
Reference substance 1: a kind of anti-icing fluid, by the way that the deionized water of the ethylene glycol of 60wt% and 40wt% is mixed.
Reference substance 4: a kind of anti-icing fluid, by by the triethanolamine of the ethylene glycol of 60wt%, 1.8wt%, 0.24wt%
Hydrolyzed maleic anhydride, the sodium polyphosphate of 0.48wt%, the EDETATE DISODIUM of 0.02wt% and 37.46wt% deionized water
It mixes.
2, test content: taking 10g sample respectively, places it at -50 DEG C 60 days, then tests its corruption by corrosion test
Corrosion energy.
3, test result: as shown in table 3.Table 3 is shown: after being placed 60 days at -50 DEG C, embodiment 1-6 and reference substance 4
Corrosion resistance be deteriorated, wherein embodiment 1 corrosion resistance be deteriorated degree it is smaller.
3 stability test result (unit: mgcm of table-2)
The specific implementation of the invention is not to be limited to these illustrations for the above content, and technology belonging to the present invention is led
For the those of ordinary skill in domain, without departing from the inventive concept of the premise, a number of simple deductions or replacements can also be made,
It all shall be regarded as belonging to present invention scope of patent protection determined by the appended claims.
Claims (5)
1. a kind of automotive antifreezing liquid, which is characterized in that by mass percentage, including following components: 60% ethylene glycol, 2 ~ 4%
Glycerol, 2 ~ 4% DMF, 1.5 ~ 2.0% triethanolamine, 0.2 ~ 0.3% hydrolyzed maleic anhydride, 0.4 ~ 0.5% polyphosphoric acids
Sodium, 0.01 ~ 0.03% EDETATE DISODIUM, the linear tetramer of 0.1 ~ 0.2% c-NMF, 0.1 ~ 0.2% metal organic frame
Material MOF-5,0.05 ~ 0.08% PEO-PPO-PEO triblock copolymer, 0.05 ~ 0.08% Emulsifier EL-60 and
0.008 ~ 0.012% methylene blue, surplus are deionized water.
2. a kind of automotive antifreezing liquid according to claim 1, which is characterized in that by mass percentage, including with the following group
Point: 60% ethylene glycol, 3% glycerol, 3% DMF, 1.8% triethanolamine, 0.24% hydrolyzed maleic anhydride, 0.48% it is more
Polyphosphate sodium, 0.02% EDETATE DISODIUM, the linear tetramer of 0.16% c-NMF, 0.16% metal-organic framework material
MOF-5,0.06% PEO-PPO-PEO triblock copolymer, 0.056% Emulsifier EL-60 and 0.010% methylene
Indigo plant, surplus are deionized water.
3. a kind of preparation method of automotive antifreezing liquid as claimed in claim 1 or 2, which comprises the following steps: will
Ethylene glycol, glycerol, DMF, triethanolamine, PEO-PPO-PEO triblock copolymer, the Emulsifier EL-60, methylene of formula ratio
Base indigo plant and deionized water are mixed and are uniformly dispersed, be added the hydrolyzed maleic anhydride of formula ratio, sodium polyphosphate, EDETATE DISODIUM,
The linear tetramer and metal-organic framework material MOF-5 of c-NMF, is dispersed with stirring and uniformly obtains solution, filter to take filtrate；It will filter
Liquid is increased to 85 ~ 95 DEG C from room temperature and keeps the temperature 1 ~ 2hr, then is cooled to -65 ~ -55 DEG C and keeps the temperature 1 ~ 2hr, then be warming up to room temperature simultaneously
1 ~ 2hr is kept the temperature, is filtered again, filtrate is a kind of automotive antifreezing liquid.
4. a kind of preparation method of automotive antifreezing liquid according to claim 3, which is characterized in that heating and drop to filtrate
In warm treatment process, heating and cooling rate are 45 ~ 55 DEG C/hr.
5. a kind of preparation method of automotive antifreezing liquid according to claim 4, which comprises the following steps: will
Ethylene glycol, glycerol, DMF, triethanolamine, PEO-PPO-PEO triblock copolymer, the Emulsifier EL-60, methylene of formula ratio
Base indigo plant and deionized water are mixed and are uniformly dispersed, be added the hydrolyzed maleic anhydride of formula ratio, sodium polyphosphate, EDETATE DISODIUM,
The linear tetramer and metal-organic framework material MOF-5 of c-NMF, is dispersed with stirring and uniformly obtains solution, filter to take filtrate；It will filter
Liquid makes it be increased to 90 DEG C from room temperature and keeps the temperature 1.5hr with the heating rate of 50 DEG C/hr, then is made with the rate of temperature fall of 50 DEG C/hr
It is cooled to -60 DEG C and keeps the temperature 1.5hr, then is allowed to warm to room temperature with the heating rate of 50 DEG C/hr and keeps the temperature 1.5hr, again
Filtering, filtrate is a kind of automotive antifreezing liquid；
By mass percentage, a kind of automotive antifreezing liquid includes following components: 60% ethylene glycol, 3% glycerol, 3%
DMF, 1.8% triethanolamine, 0.24% hydrolyzed maleic anhydride, 0.48% sodium polyphosphate, 0.02% EDETATE DISODIUM,
The linear tetramer of 0.16% c-NMF, 0.16% metal-organic framework material MOF-5,0.06% PEO-PPO-PEO tri- are embedding
Section copolymer, 0.056% Emulsifier EL-60 and 0.010% methylene blue, surplus are deionized water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330835A (en) * | 2019-08-12 | 2019-10-15 | 厦门欧化实业有限公司 | The freeze proof table printing ink of grease resistance and its processing method, process equipment |
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| CN109790447A (en) * | 2016-07-12 | 2019-05-21 | 布拉斯通产品公司 | Heat-transfer fluid and for the method for inhibiting corrosion in heat transfer system |
| CN106350028A (en) * | 2016-08-15 | 2017-01-25 | 中山大桥化工集团有限公司 | Automotive antifreeze fluid and preparation method thereof |
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| CN110330835A (en) * | 2019-08-12 | 2019-10-15 | 厦门欧化实业有限公司 | The freeze proof table printing ink of grease resistance and its processing method, process equipment |
| CN110330835B (en) * | 2019-08-12 | 2022-07-26 | 厦门欧化实业有限公司 | Oil-resistant and anti-freezing surface printing ink and processing method and processing equipment thereof |
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