CN105777465B - A kind of quick washing process in synthesis ester production process - Google Patents
A kind of quick washing process in synthesis ester production process Download PDFInfo
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- CN105777465B CN105777465B CN201610218997.7A CN201610218997A CN105777465B CN 105777465 B CN105777465 B CN 105777465B CN 201610218997 A CN201610218997 A CN 201610218997A CN 105777465 B CN105777465 B CN 105777465B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B63/00—Purification; Separation; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to the quick washing process in a kind of synthesis ester production process.Its step are as follows：1) after esterification, reaction product is placed in and is neutralized in kettle, lye is added, after stirring 10-30min, obtain mixed material, for use；2) mixed material obtained by step 1) is placed in extraction tower, mixed material is placed in from above extraction tower, while being 1 by mixed material and water lotion flow-rate ratio by water lotion from extraction tower bottom injection：0.1~1:100 coutroi velocities after 20min~40min, flow out the synthetic ester that washing is completed from water scrubber discharge port.Synthetic ester through quickly washing process preparation of the invention is through detection acid value up to 0.1mgKOH/g hereinafter, complying fully with quality control requirement；Original washing Refining times for needing 2~3 days are shortened into only 6~8h of entire washing process used time, greatly increases the production efficiency, there is very big application and popularization value；This technique only can be fully completed water-washing process with one-step method, realize continuous production, efficiently produce.
Description
Technical field
The present invention relates to the quick washing process in a kind of synthesis ester production process.
Background technique
Synthetic oil of the esters base oil as a kind of function admirable, with its low pour point, high-flash, high viscosity index (HVI), fabulous
Biological degradability, be widely used in each necks such as Aeronautics and Astronautics, navigation, vehicle, heavy-duty machinery, compressor, polar region condition
Domain.Compared with other synthetic oils, Esters oil can be relatively easy to carry out molecular modification because its molecular structure is easy to hold, and lead to
It crosses and increases and decreases its molecular weight and branch number, derive the different new varieties of a large amount of purposes.
But Esters oil price can not have always been high any more, be because of its high cost of material and too low life after all
Produce efficiency.It is needed in Esters oil subtractive process plus lye neutralizes acidic catalyst and unreacted organic acid, the sodium of organic acid
Salt has extremely strong frothing capacity, can form very big emulsion layer among oil reservoir and water layer, usually abolish emulsion layer, needs
Material is stood into 20h or more, it is extremely time-consuming.And in order to which alkali extra in alkaline cleaning procedure is washed with deionized water, conventional washing
Alkali cleaning-stratification-washing-stratification of subtractive process-repetition washing-stratification-repetition washing-stratification work
Skill washes the work at most up to 5~6 times.From the point of view of entire production process, esterification stage only needs 3,4 hours, but essence
Treatment process processed but needs 3 to 4 days.Especially alkali cleaning and water-washing process, time-consuming, low efficiency, at high cost, seriously restricts conjunction
At the quality of production and scale of ester.
Therefore, it is necessory to propose a kind of scheme, for solving the above problems.
Summary of the invention
The present invention in view of the above shortcomings of the prior art, provides a kind of fast continuously, in efficient synthesis ester production process
Fast washing process.
In order to solve the above technical problems, the embodiment of the present application provides：
A kind of quick washing process in synthesis ester production process, its step are as follows：
1) after esterification, reaction product is placed in and is neutralized in kettle, lye is added, after stirring 10-30min, obtained
To mixed material, for use；
2) mixed material obtained by step 1) is placed in extraction tower, mixed material is placed in from above extraction tower, simultaneously
It is 1 by mixed material and water lotion flow-rate ratio by water lotion from extraction tower bottom injection：0.1~1:100 coutroi velocities, 20min
After~40min, the synthetic ester that washing is completed is flowed out from water scrubber discharge port.
Further, the water lotion is the mixed liquor of water and organic solvent, and the mass ratio of the water and organic solvent is
1:0.1~1:100；The organic solvent be methanol, ethyl alcohol, ether, toluene, hexamethylene, to toluene, ethyl acetate and glycerine
One or more.
Further, it is 1 that the water lotion is water, ethyl alcohol, ether and hexamethylene in mass ratio:1:0.5:0.2 ratio
Mixed mixed liquor.
Further, it is 1 that the water lotion is water, toluene, ethyl alcohol and hexamethylene in mass ratio:0.7:0.3:0.2 ratio
The mixed liquor of example mixing.
Further, the water lotion is water, methanol, ether, ethyl alcohol are 1 in mass ratio:0.2:0.3:0.4 ratio is mixed
The mixed liquor of conjunction.
Further, the lye be sodium hydrate aqueous solution, aqueous sodium carbonate, it is a kind of in sodium bicarbonate aqueous solution or
It is several.
Further, the mass concentration of the lye is 1%~20%.
Further, the dosage of the lye is 0.01~10 times of reaction product quality.
The present invention also provides a kind of production technology of synthetic ester, step includes：Esterification reaction is carried out first；It uses again
Quick washing process in above-mentioned synthesis ester production process, completes the preparation of synthetic ester.
The present invention also provides a kind of synthetic ester produced using above-mentioned technique, the acid value of the synthetic ester is at most
0.1mgKOH/g, yield are at least 90%.
Quick washing process in synthesis ester production process of the invention, compared with prior art, advantage is as follows：
1, the synthetic ester through quickly washing process preparation of the invention is detected acid value up to 0.1mgKOH/g hereinafter, complete symbol
Close quality control requirement；
2, original washing Refining times for needing 2~3 days are shortened into only 6~8h of entire washing process used time, greatly mentioned
High production efficiency, has very big application and popularization value；
3, this technique only can be fully completed water-washing process with one-step method, realize continuous production, efficiently produce.
Specific embodiment
Quick washing process in a kind of synthesis ester production process of the present invention, its step are as follows：
1) after esterification, reaction product is placed in and is neutralized in kettle, lye is added, after stirring 10-30min, obtained
To mixed material, for use；
2) mixed material obtained by step 1) is placed in extraction tower, mixed material is placed in from above extraction tower, simultaneously
It is 1 by mixed material and water lotion flow-rate ratio by water lotion from extraction tower bottom injection：0.1~1:100 coutroi velocities, 20min
After~40min, the synthetic ester that washing is completed is flowed out from water scrubber discharge port.
Wherein, the preparation of the water lotion in the present invention is weight for the completion quickly washed in synthesis ester production process
It wants.The water lotion is the mixed liquor of water and organic solvent, and the mass ratio of the water and organic solvent is 1:0.1~1:100；
The organic solvent be methanol, ethyl alcohol, ether, toluene, hexamethylene, to the one or more of toluene, ethyl acetate and glycerine.
As an embodiment of the present invention, it is 1 that the water lotion is water, ethyl alcohol, ether and hexamethylene in mass ratio:1:0.5:0.2
Ratio mixing mixed liquor；As another embodiment of the invention, the water lotion is water, toluene, ethyl alcohol and hexamethylene
It is in mass ratio 1:0.7:0.3:The mixed liquor of 0.2 ratio mixing；As another embodiment of the invention, the water lotion
It is in mass ratio 1 for water, methanol, ether, ethyl alcohol:0.2:0.3:The mixed liquor of 0.4 ratio mixing.
In addition, the working method of the water washing device in the present invention, the i.e. working method of extraction tower, for synthesizing ester production process
In the completion quickly washed also be important.It refers specifically to：First is that flow-rate ratio, is 1 by mixed material and water lotion flow-rate ratio：
0.1~1:100 coutroi velocities, preferably flow-rate ratio are 1：10；Second is that extraction tower feed liquor mode, mixed material is from extraction tower
Side's merging, water lotion are injected from extraction tower bottom.
As an embodiment of the present invention, the lye is sodium hydrate aqueous solution, aqueous sodium carbonate, sodium bicarbonate
It is one or more of in aqueous solution.The mass concentration of the lye is 1%~20%.The dosage of the lye is reaction product quality
0.01~10 times, before wherein lye is added, first measure the acid value of reaction product, lye dosage need to be added in calculating, preferably：Alkali
The dosage of liquid is 0.1~1 times of reaction product quality.
The quick washing process in present invention synthesis ester production process is further illustrated below by specific embodiment.
Embodiment one：
It takes 100kg esterification reaction product to be added in 150L and in kettle, 5% sodium hydroxide solution 20L is added, stir
30min stops stirring, obtains mixed material；Mixed material is injected from water scrubber upper end；By water, ethyl alcohol, ether, hexamethylene
It is in mass ratio 1:1:0.5:0.2 ratio is uniformly mixed, and obtains water lotion, which is injected from water scrubber lower end；Control
The flow-rate ratio of system mixing upper end material and lower end water lotion is 1:7, after after upper end, mixed material is added, stop that water lotion is added；
After 6h, the as clear as crystal synthetic ester of 95kg is obtained.
It is 0.05mgKOH/g, yield 95% through detection acid value.
Embodiment two：
It takes 100kg esterification reaction product to be added in 150L and in kettle, 10% sodium carbonate liquor 10L is added, stir
30min stops stirring, obtains mixed material；Mixed material is injected from water scrubber upper end；By water, toluene, ethyl alcohol, hexamethylene
It is in mass ratio 1:0.7:0.3:0.2 ratio is uniformly mixed, and obtains water lotion, which is injected from water scrubber lower end；
The flow-rate ratio for controlling upper end mixed material and lower end water lotion is 1:5, after after upper end, mixed material is added, stop that washing is added
Liquid；After 6.5h, the as clear as crystal synthetic ester of 93kg is obtained.
It is 0.07mgKOH/g, yield 93% through detection acid value.
Embodiment three：
It takes 100kg esterification reaction product to be added in 150L and in kettle, 8% sodium bicarbonate solution 25L is added, stir
30min stops stirring, obtains mixed material；Mixed material is injected from water scrubber upper end；Water, methanol, ether, ethyl alcohol are pressed
Mass ratio is 1:0.2:0.3:0.4 ratio is uniformly mixed, and obtains water lotion, which is injected from water scrubber lower end；Control
The flow-rate ratio of upper end mixed material processed and lower end water lotion is 1:6, after after upper end, mixed material is added, stop that water lotion is added；
After 7h, the as clear as crystal synthetic ester of 94kg is obtained.
It is 0.04mgKOH/g, yield 94% through detection acid value.
A kind of production technology of synthetic ester of the present invention, step include：Esterification reaction is carried out first；Above-mentioned reality is used again
The quick washing process in the synthesis ester production process of example one, embodiment two or embodiment three is applied, the preparation of synthetic ester is completed.Institute
The acid value for stating synthetic ester is at most 0.1mgKOH/g, and yield is at least 90%.
The present invention can be summarized with others without prejudice to the concrete form of spirit or essential characteristics of the invention.Therefore, nothing
By from the point of view of which point, the embodiment above of the invention can only all be considered the description of the invention and cannot limit this hair
Bright, claims indicate the scope of the present invention, and above-mentioned explanation does not point out the scope of the present invention, therefore, with this
Any change in the comparable meaning and scope of claims of invention is all considered as including in claim of the invention
In the range of book.
Claims (5)
1. the quick washing process in a kind of synthesis ester production process, which is characterized in that its step are as follows：
1) after esterification, reaction product is placed in and is neutralized in kettle, lye is added, after stirring 10-30min, mixed
Material is closed, for use；
2) mixed material obtained by step 1) is placed in extraction tower, mixed material is placed in from above extraction tower, while by water
Washing lotion is 1 by mixed material and water lotion flow-rate ratio from extraction tower bottom injection：0.1~1:100 coutroi velocities, 20min~
After 40min, the synthetic ester that washing is completed is flowed out from extraction tower discharge port；
The water lotion is：Water, ethyl alcohol, ether and hexamethylene are 1 in mass ratio:1:0.5:The mixed liquor of 0.2 ratio mixing,
Water, toluene, ethyl alcohol and hexamethylene are 1 in mass ratio:0.7:0.3:The mixed liquor of 0.2 ratio mixing, Yi Jishui, methanol, second
Ether, ethyl alcohol are 1 in mass ratio:0.2:0.3:One of the mixed liquor of 0.4 ratio mixing.
2. the quick washing process in synthesis ester production process as described in claim 1, which is characterized in that the lye is hydrogen
It is aqueous solution of sodium oxide, aqueous sodium carbonate, one or more of in sodium bicarbonate aqueous solution.
3. the quick washing process in synthesis ester production process as claimed in claim 2, which is characterized in that the matter of the lye
Measuring concentration is 1%~20%.
4. the quick washing process in synthesis ester production process as claimed in claim 3, which is characterized in that the use of the lye
Amount is 0.01~10 times of reaction product quality.
5. a kind of production technology of synthetic ester, which is characterized in that step includes：Esterification reaction is carried out first；Again using power
Benefit requires the quick washing process in the described in any item synthesis ester production process of 1-4, completes the preparation of synthetic ester.
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| CN201610218997.7A CN105777465B (en) | 2016-04-08 | 2016-04-08 | A kind of quick washing process in synthesis ester production process |
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| CN201610218997.7A CN105777465B (en) | 2016-04-08 | 2016-04-08 | A kind of quick washing process in synthesis ester production process |
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| CN105777465A CN105777465A (en) | 2016-07-20 |
| CN105777465B true CN105777465B (en) | 2018-11-16 |
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