CN110408363A - A kind of preparation method of the auxiliary additive convenient for grease transport - Google Patents
A kind of preparation method of the auxiliary additive convenient for grease transport Download PDFInfo
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- CN110408363A CN110408363A CN201910756376.8A CN201910756376A CN110408363A CN 110408363 A CN110408363 A CN 110408363A CN 201910756376 A CN201910756376 A CN 201910756376A CN 110408363 A CN110408363 A CN 110408363A
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- C—CHEMISTRY; METALLURGY
- 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
- C09K3/00—Materials not provided for elsewhere
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17D—PIPE-LINE SYSTEMS; PIPE-LINES
- F17D1/00—Pipe-line systems
- F17D1/08—Pipe-line systems for liquids or viscous products
- F17D1/16—Facilitating the conveyance of liquids or effecting the conveyance of viscous products by modification of their viscosity
- F17D1/17—Facilitating the conveyance of liquids or effecting the conveyance of viscous products by modification of their viscosity by mixing with another liquid, i.e. diluting
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Abstract
This application discloses a kind of preparation methods of auxiliary additive convenient for grease transport.Include: that dipropylene glycol methyl ether and N, N- diethyl ethanamine are added in tetrahydrofuran, acryloyl chloride is slowly added dropwise;After 1h, temperature is warmed to room temperature, the reaction was continued, and 12h filters out the sediment that reaction generates after reaction;The product in filtrate is washed out with petroleum ether;Then, in methyl alcohol by 4~10 parts and 5~20 parts of the polyethylene imine dissolutions of above-mentioned product, it is stirred to react 20h, after stopping reaction, reaction product elder generation rotary evaporation is removed into partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry i.e. acquisition solvent;Solvent and mica powder are add to deionized water ball milling together, are prepared into suspension to get the auxiliary additive.
Description
Technical field
This application involves technical field of organic chemistry, in particular to a kind of auxiliary additive convenient for grease transport
Preparation method.
Background technique
According to statistics, China consumes about 22,000,000 tons of grease every year at present, wherein 15% about 3,300,000 ton becomes waste grease.
Currently, mainly there are 3 kinds of modes in China to the comprehensive utilization of waste oil: first is that carrying out simple processing purification to waste oil, directly making
For low-grade industrial oleic acid, stearic acid and commercial grease etc.;Second is that preparing non-phosphide detergent using waste oil;Third is that by waste oil
Alcoholysis preparing biological diesel oil (fatty acid methyl ester).
Waste oil is comprehensively utilized although having, the transport of waste oil is still a difficult problem.
Triglyceride can be contained in waste grease, further include alkane, alkene, the fatty acid of low-carbon, ketone, free-fat
Acid, glycerol, monoglyceride, diglyceride, dimer etc..This position, a little substances have exhaust gas grease, and viscosity is big, specific heat
Greatly, the features such as seriously rancid.It is not easy to transport, is not easy to store.
Therefore, a kind of auxiliary additive is developed, is able to solve the transportation problem of waste grease, it appears very necessary.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparations of auxiliary additive convenient for grease transport
Method
Additive of the present invention is suspension, and the preparation method includes the preparation of solvent and the system of suspension
It is standby, comprising: dipropylene glycol methyl ether and N, N- diethyl ethanamine are added in tetrahydrofuran, acryloyl chloride part is slowly added dropwise;After 1h,
Temperature is warmed to room temperature, the reaction was continued, and 12h filters out the sediment that reaction generates after reaction;It is washed out in filtrate with petroleum ether
Product;
Then, in methyl alcohol by 4~10 parts and 5~20 parts of the polyethylene imine dissolutions of above-mentioned product, it is stirred to react 20h,
After stopping reaction, reaction product elder generation rotary evaporation is removed into partial solvent, the product of concentration is settled out in petroleum ether, centrifugation,
It is dry to obtain solvent;
Solvent and mica powder are add to deionized water ball milling together, are prepared into the suspension.
Further, the method are as follows: 2~5 parts of dipropylene glycol methyl ether and N, N- diethyl are added in tetrahydrofuran
2~5 parts of ethamine, in nitrogen protection, temperature is slowly added dropwise 2~5 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is risen into room
Temperature, the reaction was continued, and 12h filters out the sediment that reaction generates after reaction;The product in filtrate is washed out with petroleum ether;
Then, in methyl alcohol by 4~10 parts and 5~20 parts of the polyethylene imine dissolutions of above-mentioned product, it is stirred to react simultaneously
Reaction product elder generation rotary evaporation after stopping reaction, is removed partial solvent, the product of concentration is settled out in petroleum ether by 20h, from
The heart, dry i.e. acquisition solvent;
It is add to deionized water ball milling together by 100 parts and 2~10 parts of mica powder of solvent, is prepared into the suspension
Liquid.
Specifically, the molecular weight of the dipropylene glycol methyl ether is 500~5000.
Specifically, the molecular weight of the polyethylene imine is 1500~5000.
Specifically, the reaction condition are as follows: reactant in confined conditions by it is freeze-thaw-Freeze-thaw cycle processing after,
At 40~50 DEG C, reacted.
Specifically, the ball milling condition are as follows: ball milling speed is 10~20rad/min, and temperature is 10~20 DEG C, and the time is
6~12 hours.
Further, described the preparation method comprises the following steps: 2~5 parts of dipropylene glycol methyl ether and N, N- are added in tetrahydrofuran
2~5 parts of diethyl ethanamine, in nitrogen protection, temperature is slowly added dropwise 2~5 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, by temperature
It is warmed to room temperature, the reaction was continued, and 12h filters out the sediment that reaction generates after reaction;The production in filtrate is washed out with petroleum ether
Object;
Then, in methyl alcohol by 6~15 parts and 5~20 parts of the polyethylene imine dissolutions of above-mentioned product, reactant is closed
Under the conditions of by it is freeze-thaw-Freeze-thaw cycle processing after, at 40~50 DEG C, while being stirred to react 20h, stop reaction after, will be anti-
It answers product elder generation rotary evaporation to remove partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry i.e. acquisition solvent;
Ball milling together, ball milling condition are add to deionized water by 100 parts and 2~10 parts of mica powder of solvent are as follows: ball milling speed
Degree is 10~20rad/min, and temperature is 10~20 DEG C, and the time is 6~12 hours, is prepared into the suspension.
A typical method of the invention are as follows: 3 parts of dipropylene glycol methyl ether and N, N- diethyl second are added in tetrahydrofuran
3 parts of amine, in nitrogen protection, temperature is slowly added dropwise 2 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is warmed to room temperature, is continued
12h is reacted, after reaction, filters out the sediment that reaction generates;The product in filtrate is washed out with petroleum ether;
Then, in methyl alcohol by 8 parts and 10 parts of the polyethylene imine dissolutions of above-mentioned product, reactant passes through in confined conditions
After crossing freeze-thaw-Freeze-thaw cycle processing, at 42 DEG C, while it being stirred to react 20h, after stopping reaction, reaction product is first rotated
Evaporation removes partial solvent, and the product of concentration is settled out in petroleum ether, is centrifuged, dries i.e. acquisition solvent;
Ball milling together, ball milling condition are add to deionized water by 100 parts and 2~10 parts of mica powder of solvent are as follows: ball milling speed
Degree is 20rad/min, and temperature is 15 DEG C, and the time is 6 hours, is prepared into the suspension
The utility model has the advantages that auxiliary additive of the present invention is thermal sensitivity auxiliary agent, having can be sent out under different temperature stimulation
The property of raw hydrophilic-hydrophobic phase co-conversion.The temperature sensitive suspension have dispersion performance it is good and can by temperature regulation come
The characteristics of controlling temperature sensitive suspension rheological property;This temperature sensitive suspension controls its mobile performance by regulating and controlling temperature.
At 20 degree hereinafter, the viscosity of main body (waste grease) can be increased, and has the tendency that solidification, restore at 30 degree or so
Mobility, 30 DEG C or more the mobility that can greatly increase main body (exhaust gas grease).
Specific embodiment
In order to make those skilled in the art more fully understand application scheme, below in conjunction with the embodiment of the present application, originally
Number as described in the examples refers both to mass fraction.
Embodiment 1
2 parts of the dipropylene glycol methyl ether and 2 parts of N, N- diethyl ethanamine that molecular weight is 500 are added in tetrahydrofuran, in nitrogen
Gas shielded, temperature are slowly added dropwise 2 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is warmed to room temperature, the reaction was continued 12h.Instead
After answering, the sediment that reaction generates is filtered out;The product in filtrate is washed out with petroleum ether.
Then, in methyl alcohol by 5 parts and 5 parts of polyethylene imine (molecular weight 1800) dissolutions of above-mentioned product, reactant
In confined conditions after freeze-thaw-Freeze-thaw cycle processing, at 40 DEG C, while it being stirred to react 20h, it, will after stopping reaction
Reaction product elder generation rotary evaporation remove partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry obtain it is molten
Agent.
Embodiment 2
5 parts of the dipropylene glycol methyl ether and 5 parts of N, N- diethyl ethanamine that molecular weight is 5000 are added in tetrahydrofuran, in nitrogen
Gas shielded, temperature are slowly added dropwise 5 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is warmed to room temperature, the reaction was continued 12h.Instead
After answering, the sediment that reaction generates is filtered out;The product in filtrate is washed out with petroleum ether.
Then, in methyl alcohol by 15 parts and 20 parts of polyethylene imine (molecular weight 1800) dissolutions of above-mentioned product, reaction
Object after freeze-thaw-Freeze-thaw cycle processing, at 40 DEG C, while being stirred to react 20h in confined conditions, after stopping reaction,
By reaction product elder generation rotary evaporation remove partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry obtain it is molten
Agent.
Embodiment 3
3 parts of dipropylene glycol methyl ether and 3 parts of N, N- diethyl ethanamine are added in tetrahydrofuran, in nitrogen protection, temperature 0
2 parts of acryloyl chloride are slowly added dropwise under the conditions of DEG C;After 1h, temperature is warmed to room temperature, the reaction was continued, and 12h is filtered out anti-after reaction
The sediment that should be generated;The product in filtrate is washed out with petroleum ether;
Then, in methyl alcohol by 8 parts and 10 parts of the polyethylene imine dissolutions of above-mentioned product, reactant passes through in confined conditions
After crossing freeze-thaw-Freeze-thaw cycle processing, at 42 DEG C, while it being stirred to react 20h, after stopping reaction, reaction product is first rotated
Evaporation removes partial solvent, and the product of concentration is settled out in petroleum ether, is centrifuged, dries i.e. acquisition solvent;
Embodiment 4
4 parts of the dipropylene glycol methyl ether and 4 parts of N, N- diethyl ethanamine that molecular weight is 5000 are added in tetrahydrofuran, in nitrogen
Gas shielded, temperature are slowly added dropwise 3 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is warmed to room temperature, the reaction was continued 12h.Instead
After answering, the sediment that reaction generates is filtered out;The product in filtrate is washed out with petroleum ether.
Then, in methyl alcohol by 15 parts and 20 parts of polyethylene imine (molecular weight 1800) dissolutions of above-mentioned product, reaction
Object after freeze-thaw-Freeze-thaw cycle processing, at 40 DEG C, while being stirred to react 20h in confined conditions, after stopping reaction,
By reaction product elder generation rotary evaporation remove partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry obtain it is molten
Agent.
Embodiment 5
4 parts of the dipropylene glycol methyl ether and 4 parts of N, N- diethyl ethanamine that molecular weight is 5000 are added in tetrahydrofuran, in nitrogen
Gas shielded, temperature are slowly added dropwise 3 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is warmed to room temperature, the reaction was continued 12h.Instead
After answering, the sediment that reaction generates is filtered out;The product in filtrate is washed out with petroleum ether.
Then, in methyl alcohol by 5 parts and 20 parts of polyethylene imine (molecular weight 1800) dissolutions of above-mentioned product, reactant
In confined conditions after freeze-thaw-Freeze-thaw cycle processing, at 40 DEG C, while it being stirred to react 20h, it, will after stopping reaction
Reaction product elder generation rotary evaporation remove partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry obtain it is molten
Agent.
Embodiment 6
3 parts of the dipropylene glycol methyl ether and 3 parts of N, N- diethyl ethanamine that molecular weight is 3000 are added in tetrahydrofuran, in nitrogen
Gas shielded, temperature are slowly added dropwise 3 parts of acryloyl chloride under the conditions of being 0 DEG C;After 1h, temperature is warmed to room temperature, the reaction was continued 12h.Instead
After answering, the sediment that reaction generates is filtered out;The product in filtrate is washed out with petroleum ether.
Then, in methyl alcohol by 10 parts and 20 parts of polyethylene imine (molecular weight 1800) dissolutions of above-mentioned product, reaction
Object after freeze-thaw-Freeze-thaw cycle processing, at 40 DEG C, while being stirred to react 20h in confined conditions, after stopping reaction,
By reaction product elder generation rotary evaporation remove partial solvent, the product of concentration is settled out in petroleum ether, be centrifuged, dry obtain it is molten
Agent.
Embodiment 7~12
A pilling is add to deionized water with 10 parts of mica powder respectively by 100 parts of the resulting solvent of Examples 1 to 6 respectively
Mill, ball milling condition are as follows: ball milling speed 20rad/min, temperature are 15 DEG C, and the time is 6 hours, are prepared into the suspension
Embodiment 13
3 100 parts of resulting solvent of embodiment is add to deionized water ball milling together, ball milling with 2 parts of mica powder respectively
Condition are as follows: ball milling speed 20rad/min, temperature are 15 DEG C, and the time is 6 hours, are prepared into the suspension
Embodiment 14
3 100 parts of resulting solvent of embodiment is add to deionized water ball milling together, ball milling with 4 parts of mica powder respectively
Condition are as follows: ball milling speed 20rad/min, temperature are 15 DEG C, and the time is 6 hours, are prepared into the suspension
Embodiment 15
3 100 parts of resulting solvent of embodiment is add to deionized water ball milling together, ball milling with 6 parts of mica powder respectively
Condition are as follows: ball milling speed 20rad/min, temperature are 15 DEG C, and the time is 6 hours, are prepared into the suspension
Embodiment 16
3 100 parts of resulting solvent of embodiment is add to deionized water ball milling together, ball milling with 8 parts of mica powder respectively
Condition are as follows: ball milling speed 20rad/min, temperature are 15 DEG C, and the time is 6 hours, are prepared into the suspension
Embodiment 17
3 100 parts of resulting solvent of embodiment is add to deionized water ball milling together, ball milling with 10 parts of mica powder respectively
Condition are as follows: ball milling speed 20rad/min, temperature are 15 DEG C, and the time is 6 hours, are prepared into the suspension
Embodiment 18 is applied
The resulting suspension of embodiment 7~17 is added in waste grease, additional amount be waste grease quality 2~
10%.
10 DEG C of viscosity (cp) | 30 DEG C of viscosity (cp) | 40 DEG C of viscosity (cp) | |
Waste grease (untreated) | 3000 | 2800 | 2500 |
Waste grease (embodiment 7) | 4000 | 310 | 200 |
Waste grease (embodiment 11) | 3300 | 280 | 180 |
Waste grease (embodiment 15) | 3800 | 330 | 190 |
Waste grease (embodiment 17) | 3300 | 220 | 170 |
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application.
Claims (8)
1. a kind of preparation method of the auxiliary additive convenient for grease transport, which is characterized in that the additive is suspension,
The preparation method includes the preparation of solvent and the preparation of suspension, comprising:
Dipropylene glycol methyl ether and N, N- diethyl ethanamine are added in tetrahydrofuran, acryloyl chloride part is slowly added dropwise;It, will be warm after 1h
Degree is warmed to room temperature, and the reaction was continued, and 12h filters out the sediment that reaction generates after reaction;The production in filtrate is washed out with petroleum ether
Object;Then, in methyl alcohol by 4~10 parts and 5~20 parts of the polyethylene imine dissolutions of above-mentioned product, it is stirred to react 20h, stopped anti-
Reaction product elder generation rotary evaporation is removed partial solvent, the product of concentration is settled out in petroleum ether, is centrifuged, dries i.e. by Ying Hou
Obtain solvent;Solvent and mica powder are add to deionized water ball milling together, are prepared into the suspension.
2. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that in tetrahydro
2~5 parts of dipropylene glycol methyl ether and 2~5 parts of N, N- diethyl ethanamine are added in furans, in nitrogen protection, under the conditions of temperature is 0 DEG C
It is slowly added dropwise 2~5 parts of acryloyl chloride;After 1h, temperature is warmed to room temperature, the reaction was continued, and 12h filters out reaction and produce after reaction
Raw sediment;The product in filtrate is washed out with petroleum ether;Then, by 4~10 parts of above-mentioned product and polyethylene imine 5~20
Part dissolution in methyl alcohol, while being stirred to react 20h, and after stopping reaction, reaction product elder generation rotary evaporation is removed partial solvent, by
The product of concentration settles out in petroleum ether, is centrifuged, dries i.e. acquisition solvent;100 parts and 2~10 parts of mica powder of solvent are added to
Ball milling together in deionized water is prepared into the suspension.
3. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that described
The molecular weight of dipropylene glycol methyl ether is 500~5000.
4. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that described
The molecular weight of polyethylene imine is 1500~5000.
5. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that described
Reaction condition are as follows: reactant after freeze-thaw-Freeze-thaw cycle processing, at 40~50 DEG C, is reacted in confined conditions.
6. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that ball milling item
Part are as follows: ball milling speed is 10~20rad/min, and temperature is 10~20 DEG C, and the time is 6~12 hours.
7. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that in tetrahydro
2~5 parts of dipropylene glycol methyl ether and 2~5 parts of N, N- diethyl ethanamine are added in furans, in nitrogen protection, under the conditions of temperature is 0 DEG C
It is slowly added dropwise 2~5 parts of acryloyl chloride;After 1h, temperature is warmed to room temperature, the reaction was continued, and 12h filters out reaction and produce after reaction
Raw sediment;The product in filtrate is washed out with petroleum ether;Then, by 6~15 parts of above-mentioned product and polyethylene imine 5~20
Part dissolution in methyl alcohol, reactant in confined conditions by it is freeze-thaw-Freeze-thaw cycle processing after, at 40~50 DEG C, simultaneously
It is stirred to react 20h, after stopping reaction, reaction product elder generation rotary evaporation is removed into partial solvent, by the product of concentration in petroleum ether
In settle out, be centrifuged, dry i.e. acquisition solvent;A pilling is add to deionized water by 100 parts and 2~10 parts of mica powder of solvent
Mill, ball milling condition are as follows: ball milling speed is 10~20rad/min, and temperature is 10~20 DEG C, and the time is 6~12 hours, is prepared into institute
The suspension stated.
8. the preparation method of the auxiliary additive according to claim 1 convenient for grease transport, which is characterized in that in tetrahydro
3 parts of dipropylene glycol methyl ether and 3 parts of N, N- diethyl ethanamine are added in furans, in nitrogen protection, temperature is slowly dripped under the conditions of being 0 DEG C
Add 2 parts of acryloyl chloride;After 1h, temperature is warmed to room temperature, the reaction was continued, and 12h filters out the precipitating that reaction generates after reaction
Object;The product in filtrate is washed out with petroleum ether;Then, in methyl alcohol by 8 parts and 10 parts of the polyethylene imine dissolutions of above-mentioned product,
Reactant after freeze-thaw-Freeze-thaw cycle processing, at 42 DEG C, while being stirred to react 20h, stop reaction in confined conditions
Afterwards, reaction product elder generation rotary evaporation is removed into partial solvent, the product of concentration is settled out in petroleum ether, is centrifuged, dried and obtain
Obtain solvent;Ball milling together, ball milling condition are add to deionized water by 100 parts and 2~10 parts of mica powder of solvent are as follows: ball milling speed
For 20rad/min, temperature is 15 DEG C, and the time is 6 hours, is prepared into the suspension.
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CN108822722A (en) * | 2018-07-29 | 2018-11-16 | 湖南科技大学 | A kind of the hydrophobic polyurethane marine anti-pollution coating material and preparation method bionical based on lotus leaf |
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2019
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CN103524756A (en) * | 2013-09-27 | 2014-01-22 | 北京科技大学 | Preparation method of light/pH (potential of hydrogen) sensitive type pyrene functional polymer micelle |
CN104177622A (en) * | 2014-06-30 | 2014-12-03 | 中南大学 | Temperature-sensitive dispersing agent, temperature-sensitive suspending liquid and application of temperature-sensitive dispersing agent and temperature-sensitive suspending liquid |
CN108822722A (en) * | 2018-07-29 | 2018-11-16 | 湖南科技大学 | A kind of the hydrophobic polyurethane marine anti-pollution coating material and preparation method bionical based on lotus leaf |
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