CN106674009A - Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate - Google Patents
Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate Download PDFInfo
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Abstract
The invention relates to a reaction device for synthetic production of diisooctyl sebacate, which comprises an esterification reactor, an esterification tower, an esterification condenser, a separator, a rectifying still, a rectifying tower, a rectifying condenser, an alcohol receiving tank, an ester receiving tank, a vacuum-pumping system and a pump delivery system, wherein the esterification tower is arranged on the top part of the esterification reactor; an alcohol recycling pipeline circularly communicated with the esterification reactor is arranged on the side wall of the separator; a discharge hole of the esterification reactor is connected with a feed inlet of the rectifying still through a feed pump in the pump delivery system; the rectifying tower is arranged on the top part of the rectifying still; an outlet end of the rectifying tower is connected with an inlet end of the rectifying condenser; an outlet end of the rectifying condenser is connected with the ester receiving tank through the alcohol receiving tank. According to the reaction device provided by the invention, condition parameters such temperature and pressure intensity can be adjusted at any time during a reaction process, materials are enabled to fully react, the full and reasonable utilization of the materials is realized maximally through a synthetic process method, and the quality, the yield and the purity of the finished product diisooctyl sebacate are ensured.
Description
Technical field
The present invention relates to the synthetically prepared technical field of biomass lube base oil Plexol 201, specifically
It is a kind of synthetically produced use reaction unit of Plexol 201 and Plexol 201 synthetic process.
Background technology
Plexol 201 is a kind of excellent low temperature resistant plasticizer, is usually used in polyvinyl chloride cable material, cold-resistant film
With artificial leather and the plasticising applied technical field of other resins.Meanwhile, it is as biomass-based profit that it also has an important use
The base oil of lubricating oil, the base oil, can be used as jet engine lubricating oil due to the characteristic such as its high temperature resistant, low temperature resistant, degradable
Base oil, rubber is shunk and bad to additive compatibility is lacked to improve traditional synthetic base oil poly ＆ Alpha ,-olefin oil
Fall into.Synthetically prepared for Plexol 201, traditional synthesis technique mainly has following several：
1st, the method being prepared as catalyst using sulfuric acid, this kind of method mainly has four aspect shortcomings：1.1st, esterification knot
Need to be neutralized after beam, wash, dealcoholysis, the processing step such as decolouring, complex technical process, reaction selectivity is poor, generation it is useless
Environmental pollution by water.1.2nd, because the sulphion in sulfuric acid is present, sulfur content is too high in causing the base oil of synthesis, for jet
Engine can be caused damage during engine base oil, when for high grade resins, sulfur content is high to cause catalyst to inactivate.
1.3rd, sulfuric acid has stronger corrosivity to equipment, high to equipment requirement during the course of the reaction.1.4th, reaction time is long, low yield,
Product color number is high.
2nd, the method being prepared as catalyst using solid acid, the technique is mainly referred to and published thesis in colleges and universities, only
Limit laboratory installation, does not have industrialized production application device.
3rd, the method for using tungstosilicic acid, 732 resins, ferric trichloride mix preparation to be prepared for catalyst, the method
Laboratory synthetic method is detected in, there is no industrialized production application device.
Due to being influenceed by above several respects, Plexol 201 cannot be obtained on jet engine lube base oil
To extensive use.
Meanwhile, existing Plexol 201 production synthetic reaction device deposits irrationality in structure mostly,
Easily cause that the reaction time is long, operation temperature is difficult to accurately hold, not exclusively, byproduct is more in building-up process for esterification,
Material recycle rate is low, and production efficiency is low, and the production precision of finished product is also difficult to ensure that.
Therefore, design and prepare a kind of synthetically produced use process equipment of Plexol 201, and utilize the equipment research
Go out a set of preferable Plexol 201 synthetic process actually necessary for the production of Plexol 201.
The content of the invention
In order to solve the above-mentioned technical problem, reaction unit is used the invention provides a kind of Plexol 201 is synthetically produced
And Plexol 201 synthetic process.The device can be good at realizing the condition ginseng such as temperature, pressure in course of reaction
Several adjustment at any time, it is ensured that the abundant reaction of material, synthetic process also realize to greatest extent in itself material it is abundant,
Rationally utilize, it is ensured that the quality of finished product Plexol 201, income and purity.
The present invention is in order to solve the above technical problems, the technical scheme for being used is：A kind of Plexol 201 synthesis life
Product reaction unit, the device includes esterifying kettle, esterification column, esterification condensator, separator, rectifying still, rectifying column, rectifying condensation
It is all provided with the outer surface of device, alcohol receiving tank, ester receiving tank, pumped vacuum systems and pump induction system, the esterifying kettle and rectifying still
The heat-conducting oil heating system for being heated to material in esterifying kettle or rectifying still is equipped with, the heat-conducting oil heating system is set in
Remaining position of esterifying kettle and rectifying still in addition to top, and avoid being located at the discharging opening of esterifying kettle and rectifying still bottom；
Described esterification column is arranged on the top of esterifying kettle, and the port of export of esterification column is connected with the entrance point of esterification condensator, ester
The port of export for changing condenser is connected with the entrance point of separator, is additionally provided with the side wall of separator and is connected with esterifying kettle circulation
Alcohol recovery line, the discharging opening of the esterifying kettle is connected by the material pump in pump induction system with the charging aperture of rectifying still, institute
The rectifying column stated is arranged on the top of rectifying still, and the port of export of the rectifying column is connected with the entrance point of rectifying condenser, rectifying
The port of export of condenser is connected with alcohol receiving tank and ester receiving tank.
Heat conductive oil inlet and conduction oil outlet, heat conductive oil inlet and conduction oil are provided with described heat-conducting oil heating system
Outlet is separately mounted to the top of heat-conducting oil heating system outer surface side and the bottom of opposite side.
It is additionally provided with heat-conducting oil heating system esterifying kettle or rectifying temperature in the kettle are surveyed for installs thermometer
The thermometer socket of amount.
The top of esterifying kettle is provided with sour charging aperture, alcohol charging aperture, catalyst inlet and drain.
A kind of process of Plexol 201 synthesis, comprises the following steps：
Step one, according to isooctanol and decanedioic acid mol ratio be 2:1 ratio, it is standby to weigh decanedioic acid, and takes excessive different pungent
Alcohol is added in esterifying kettle, afterwards, opens the stirring system and heat-conducting oil heating system in esterifying kettle, adjusts esterifying kettle conduction oil
The temperature of conduction oil is 70~80 DEG C in heating system, when esterification temperature in the kettle is increased to 60 DEG C, enables pumped vacuum systems pair
Esterifying kettle carries out vacuumize process, vacuum in esterifying kettle is maintained at -0.04~-0.06Mpa；
Step 2, to adding the decanedioic acid that weighs in the esterifying kettle of step one, and added decanedioic acid quality 0.5%~1% is urged
Agent butyl titanate, afterwards, closes pumped vacuum systems, and material starts reaction in esterifying kettle, when esterification temperature in the kettle is increased to
At 90~100 DEG C, the temperature of conduction oil is 200 DEG C in regulation esterifying kettle heat-conducting oil heating system, when esterification temperature in the kettle is raised
During to 165~175 DEG C, esterification condensator is opened to being condensed into material therein, when flowing back occurs in esterification condensator,
The temperature of conduction oil is warming up to 230 DEG C with the heating rate of 10~20 DEG C/h in control esterifying kettle heat-conducting oil heating system, works as ester
When change temperature in the kettle is increased to 220 DEG C, material carries out heat-insulation pressure keeping reaction 25-35min at such a temperature in control esterifying kettle, it
Afterwards, esterifying kettle heat-conducting oil heating system is closed, esterification is completed；
Step 3, by step 2 complete esterification material be delivered in rectifying still by the material pump in pump induction system, it
Afterwards, enable pumped vacuum systems carries out vacuumize process to rectifying still, make vacuum in rectifying still be maintained at -0.0985~-
0.099Mpa, and it is 200 DEG C to adjust the temperature of conduction oil in rectifying still heat-conducting oil heating system, opens rectifying condenser to entering
Material therein is condensed；
Step 4, when rectifying column tower top temperature rises to 140~160 DEG C, open alcohol receive tank valve, make alcohol receiving tank to essence
It is that 140~160 DEG C of isooctanol for distillating are collected to evaporate column overhead temperatures, when fashionable there is no liquid flow in alcohol receiving tank, is adjusted
Section rectifying still heat-conducting oil heating system in conduction oil temperature be 290 DEG C, make alcohol receiving tank continue rectifying column is distillated distillate
Thing is collected, and when rectifying column tower top temperature is increased to 240~250 DEG C, closes alcohol and receives tank valve, and open ester receiving tank
Valve, the distillate distillated when making ester receiving tank to rectifying column tower top temperature more than 240~250 DEG C is collected, ester receiving tank
Interior collected material is finished product Plexol 201.
In step 3, the step 2 complete esterification material need to when esterifying kettle temperature is down to below 180 DEG C,
Expect the conveying of pump.
Beneficial effect：
1st, a kind of synthetically produced use reaction unit structure setting of Plexol 201 of the invention is reasonable, process operability
By force, the multiple parts in reaction unit, such as esterifying kettle, rectifying still, temperature controllability are good, and easy to operate, reaction unit is whole
Body material recycle rate is high, finished product accuracy and quality better.
2nd, the heat-conducting oil heating system set in reaction unit of the invention, may be implemented in the outside of device feature in kettle
The reaction temperature for carrying out carries out controllable adjustment at any time, enhances the artificial operability of course of reaction, is easy to hold extent of reaction,
Realize preferable esterification, it is ensured that the purity and quality of finished product Plexol 201.Esterification column in reaction unit
Discharging opening connects the part connect setting of esterification condensator and separator, and unreacted alcohols material is rising in can making material
During carry the moisture that esterification is produced secretly, constantly promote esterification balance positive mobile, the alcohols that separator is recovered to
Raw material can also repetitive cycling utilize, the reaction rate that the process is improved, the also less waste of material.
3rd, a kind of Plexol 201 synthetic process of the invention is by catalyst, temperature in esterification reaction process
The adjustment and limitation of the reaction condition parameter such as degree, pressure, substantially reduce the time of esterification, reduce reaction by-product
Generation, improves production efficiency.Process integrated artistic is simple, process control, and reaction time is short, and good reaction selectivity is produced
Product quality better, high income can carry out alternative ore matter based lubricating oil base oil as renewable biomass based lubricating oil base oil, and
To not existing corrosion using equipment, it is adaptable to the harsh conditions environment such as high temperature, low temperature.After measured：Prepared by this process
Finished product Plexol 201 in colorless and transparent, color scope is 6-8, and acid number is smaller, chromatographic content 99.7-
Between 99.86%, product yield is up to more than 98.5%, the stage such as course of reaction is without neutralizing, washing, therefore, produced without waste water,
Sulfur-bearing, not pollution-free, while this product belongs to biomass-based lube base oil, with recyclability.
4th, the specifically chosen butyl titanate using added decanedioic acid quality 0.5%~1% of the present invention is used as the catalysis reacted
Agent, butyl titanate belongs to ester type compound as product, therefore the catalyst is separated without from product, reduces
Neutralization, water-washing step.The catalyst is environmentally safe, belongs to environmental protection technique.Catalyst in whole course of reaction only
Have and a small amount of water is generated in esterification process, it is to avoid neutralization water scouring water.And reduce the damage of the product in water-washing process is neutralized
Consumption.Meanwhile, the catalyst belongs to lipid material, therefore does not have any influence to this product acid number, does not influence to do lube base
Oleic acid value is limited.
5th, the present invention is specifically chosen when kettle temperature degree is down to below 180 DEG C after esterification, then conveys material and carry out down
The reaction of one step, temperature of charge is too high after effectively prevent esterification, during discharging and air contact, oxidation occurs anti-
Should, cause product color number to raise, so as to reduce product quality.
Brief description of the drawings
Fig. 1 is structural representation of the invention；
Reference：1st, esterifying kettle, 101, sour charging aperture, 102, alcohol charging aperture, 103, catalyst inlet, 104, drain, 2,
Esterification column, 3, esterification condensator, 4, separator, 5, rectifying still, 6, rectifying column, 7, rectifying condenser, 8, alcohol receiving tank, 9, ester connects
Closed cans, 10, heat-conducting oil heating system, 1001, heat conductive oil inlet, 1002, conduction oil outlet, 1003, thermometer socket, 11, material
Pump.
Specific embodiment
The present invention is described further with specific embodiment below in conjunction with the accompanying drawings：
A kind of synthetically produced use reaction unit of Plexol 201, mainly include esterifying kettle 1, esterification column 2, esterification condensator 3,
Separator 4, rectifying still 5, rectifying column 6, rectifying condenser 7, alcohol receiving tank 8, ester receiving tank 9, pumped vacuum systems and pump delivery system
System, sour charging aperture 101, alcohol charging aperture 102, catalyst inlet 103 and drain 104 are disposed with the top of esterifying kettle 1,
It is provided with the outer surface of esterifying kettle 1 and rectifying still 5 for leading for being heated to material in esterifying kettle 1 or rectifying still 5
Heating system of hot oil 10, the heat-conducting oil heating system 10 is set in remaining position of esterifying kettle 1 and rectifying still 5 in addition to top,
And avoid being located at the discharging opening of esterifying kettle 1 and the bottom of rectifying still 5, it is provided with conduction oil in described heat-conducting oil heating system 10 and enters
Mouth 1001 and conduction oil outlet 1002, heat conductive oil inlet 1001 and conduction oil outlet 1002 are separately mounted to heat-conducting oil heating system
The top of 10 outer surfaces side and the bottom of opposite side, for being circulated heating to material in kettle, in heat-conducting oil heating system
The thermometer socket 1003 for being measured to temperature in esterifying kettle 1 or rectifying still 5 is additionally provided with 10.
Described esterification column 2 is arranged on the top of esterifying kettle 1, the port of export of esterification column 2 and the entrance point of esterification condensator 3
Connection, the port of export of esterification condensator 3 is connected with the entrance point of separator 4, is additionally provided with and esterification on the side wall of separator 4
The alcohol recovery line of the circulation connection of kettle 1, the discharging opening of the esterifying kettle 1 is by the material pump 11 in pump induction system and rectifying still 5
Charging aperture connection, described rectifying column 6 is arranged on the top of rectifying still 5, and the rectifying column 6 the port of export and rectifying condenser
7 entrance point connection, the port of export of rectifying condenser 7 is connected with alcohol receiving tank 8 and ester receiving tank 9.
A kind of process of Plexol 201 synthesis, comprises the following steps：
First, esterification
Step one, according to isooctanol and decanedioic acid mol ratio be 2:1 ratio, it is standby to weigh decanedioic acid, and takes excessive different pungent
Alcohol is added in esterifying kettle 1, afterwards, opens the stirring system and heat-conducting oil heating system 10 in esterifying kettle 1, adjusts esterifying kettle 1
The temperature of conduction oil is 70~80 DEG C in heat-conducting oil heating system 10, when temperature is increased to 60 DEG C in esterifying kettle 1, enables and takes out true
Empty set system carries out vacuumize process to esterifying kettle 1, vacuum in esterifying kettle 1 is maintained at -0.04~-0.06Mpa；
Step 2, unlatching material inlet valve, to the decanedioic acid for adding step one to weigh in esterifying kettle 1, and added decanedioic acid quality
0.5%~1% catalyst butyl titanate, afterwards, close material inlet valve, close pumped vacuum systems, keep kettle in vacuum about
It is -0.05Mpa, material starts single-esterification in esterifying kettle 1, single-esterification belongs to exothermic reaction, to make single-esterification
Fully, need not now heat, when temperature is increased to 90~100 DEG C in esterifying kettle 1, now kettle temperature rises and goes up more slowly or no longer
Rise, the temperature of conduction oil is 200 DEG C in the regulation heat-conducting oil heating system 10 of esterifying kettle 1, due to the presence of vacuum, when esterifying kettle 1
When interior temperature is increased to 165~175 DEG C, esterification column discharging opening temperature rises rapidly, opens 3 pairs of entrance of esterification condensator therein
Material is circulated water cooling, when the outlet of esterification condensator 3 regards cup backflow occurs, controls esterifying kettle 1 to lead according to backflow situation
The temperature of conduction oil is warming up to 230 DEG C with the heating rate of 10~20 DEG C/h in heating system of hot oil 10, it is ensured that kettle temperature is not higher than
220 DEG C, when temperature is increased to 220 DEG C in esterifying kettle 1, material in esterifying kettle 1 is controlled to carry out heat-insulation pressure keeping at such a temperature anti-
25-35min is answered, afterwards, the heat-conducting oil heating system 10 of esterifying kettle 1 is closed, esterification is completed；The used time in esterification stage is
3~5 hours.
2nd, rectifying
Step 3, after step 2 complete esterification after, after the temperature in the kettle of kettle to be esterified 1 is down to less than 180 DEG C, by esterifying kettle 1
Interior material is delivered in rectifying still 5 by the material pump 11 in pump induction system, after the completion of conveying, enables pumped vacuum systems to rectifying
Kettle 5 carries out vacuumize process, vacuum in rectifying still 5 is maintained at -0.0985~-0.099Mpa, sets the conduction oil of rectifying still 5
The temperature of conduction oil is 200 DEG C in heating system 10, and now, temperature is 160~180 DEG C in rectifying still 5, opens rectifying condenser
7 pairs of entrance materials therein are condensed；
Step 4, when the tower top temperature of rectifying column 6 rises to 140~160 DEG C, open the valve of alcohol receiving tank 8, make alcohol receiving tank 8
It is that 140~160 DEG C of excessive isooctanol for distillating are collected to the tower top temperature of rectifying column 6, when alcohol receiving tank 8 goes out depending on cup no liquid
After now, the temperature of conduction oil is 290 DEG C in the regulation heat-conducting oil heating system 10 of rectifying still 5, and the kettle temperature of rectifying still 5 rises to 230 DEG C
When, the light component and micro isooctanol that will be esterified generation continue to be recycled in alcohol receiving tank 8, with the rising of kettle temperature, work as rectifying
When the tower top temperature of tower 6 is increased to 240~250 DEG C, the valve of alcohol receiving tank 8 is closed, and open the valve of ester receiving tank 9, feed liquid is cut
Ester receiving tank 9 is shifted to, now kettle temperature stabilization, at 260~280 DEG C, makes ester receiving tank 9 to this time of rectifying column 6 in rectifying still 5
The distillate for distillating is collected, and when ester receiving tank 9 regards cup no liquid, rectifying is completed, and the rectifying time is 4~6 hours.Ester connects
Collected material is finished product Plexol 201 in closed cans 9, and containing for Plexol 201 in finished product is obtained through chromatogram detection
Amount ＞ 99.7%, color ＜ 10, acid number ＜ 0.05, in colorless and transparent, yield is more than 99%.
Product quality is carried out to Plexol 201 prepared by Conventional processing methods and process of the invention below
Data be compared as follows：
1st, product process flow
Sulfuric acid process：Esterification-neutralization-washing-dealcoholysis-decolouring-finished product, whole production process needs 20~25 hours.
Solid acid system：Esterification-washing-dealcoholysis-decolouring-finished product, whole production process needs 17~22 hours.
Mixed catalyst method：Esterification-neutralization-washing-dealcoholysis-decolouring-finished product, whole production process needs 20~
25 hours.
The present invention：Esterification-rectifying-finished product, whole production process needs 7~11 hours.
Through knowable to above-mentioned comparing：Process processing step of the invention is few, and reaction time is short, and production efficiency is high.
2nd, product quality
Above-mentioned data result shows：The present invention is in water white transparency relative to Plexol 201 proterties prepared by other methods
Shape, chromatographic content is higher, and color number is smaller, and acid number is smaller, not sulfur-bearing.
3rd, product yield
Above-mentioned data result shows：Plexol 201 is prepared relative to other conventional methods, process of the invention is produced
Product yield is significantly improved.
4th, effect on environment aspect
Production By Sulfuric Acid Process technique is related to neutralize, washes, and often produces 4 tons of product neededs and produces 6-8 tons of waste water, waste water yield
It is 1.5-2 tons of waste water/ton product.
Solid acid system often produces 4 tons of product neededs 3-4 tons of waste water of generation due to no N-process, and waste water yield is
0.75-1 tons of waste water/ton product.
Mixed catalyst method production technology and sulfuric acid process are basically identical, therefore waste water yield and sulfuric acid process are essentially identical,
About 1.5-2 tons of waste water/ton product.
Not neutralized washing is directly entered rectifying section after the completion of present invention esterification, is produced without waste water.
Through knowable to above-mentioned comparing：Process of the invention due in the absence of neutralize, washing etc. step operation, therefore, nothing
Waste water is produced, and environmental pollution is small.
After be cooled to the material after esterification below 180 DEG C in preparation process by the present invention, then subsequent reactions are carried out,
This is that just discharging is primarily due to prevent temperature of charge too high after declining due to kettle temperature, during discharging and air contact, is held
The rising of product color number is easily caused, oxidation reaction occurs, reduce product quality.
The catalyst that the present invention is used is butyl titanate, and ester type compound, therefore the catalysis are belonged to as product
Agent is separated without from product, reduces neutralization, water-washing step.
The mainly metatitanic acid that butyl titanate works in whole course of reaction, but because metatitanic acid has certain acid
Property, making catalyst with metatitanic acid can influence oil product acid number, in addition it is also necessary to neutralize washing to remove metatitanic acid, thus not as being urged with sulfuric acid
Agent.By the author's repetition test and Theoretical Proof, finally from butyl titanate as catalyst, during the course of the reaction, titanium
Sour four butyl esters are decomposed into metatitanic acid, and metatitanic acid catalytic reaction is completed, due to isooctanol excess, when in reaction system decanedioic acid by completely anti-
Ying Hou, and as the raising of reaction temperature, metatitanic acid and four butyl esters combine production butyl titanate again.
In the selection of catalyst usage amount, because decanedioic acid and isooctanol that 1mol metatitanic acids can be catalyzed 2mol occur instead
Should, and while tracking decanedioic acid reaction rate and butyl titanate catalytic action during the course of the reaction, determine the fourth of metatitanic acid four
The consumption of ester is the 0.5%~1% of decanedioic acid quality, and when less than 0.5%, reaction rate is decreased obviously, and the reaction time is into multiplication
Plus, it is little on reaction rate influence when higher than 1%, therefore determine that the consumption of butyl titanate is decanedioic acid according to above reason
The 0.5%~1% of quality.
Plexol 201 prepared by the present invention breaks through traditional synthesis on synthesis technique, reaches product quality
Good, synthesis technique is simple, the Novel synthesis technology of high income.Plexol 201 can as biomass-based lube base oil
Complete alternative ore matter based lubricating oil base oil, makes regenerative resource.The base oil possesses high temperature resistant, low temperature tolerance characteristicses,
Still be can be used under harsh conditions.
Main advantage of the invention is to reduce reactions steps, reduces the reaction time, improves yield, reduces equipment investment.
Used catalyst is environmentally safe simultaneously, belongs to environmental protection technique.A small amount of water is only generated in esterification process, it is to avoid in
With water scouring water.And reduce the product loss in water-washing process is neutralized.The catalyst of selection belongs to lipid material, therefore to this
Product acid branch or not to do the restriction of lube base oil acid number without any influence.This product belongs to biomass-based lubrication simultaneously
Oil base oil, with recyclability.
Embodiment 1
First to adding 4400L isooctanol in esterifying kettle and opening stirring and heat-conducting oil heating, esterifying kettle heat conduction oil temperature is set
It is 70 DEG C, when kettle temperature rises to 60 DEG C, opens pumped vacuum systems, it is -0.06Mpa to keep vacuum in kettle, opens material inlet valve,
2000kg decanedioic acid is drawn in esterifying kettle by vacuum, and adds catalyst butyl titanate 10kg, close material inlet valve, closed
Close pumped vacuum systems.It is -0.05Mpa to keep vacuum in kettle.Now single-esterification starts, and it is anti-that single-esterification belongs to heat release
Should, to make single-esterification fully, need not now heat, when kettle temperature rises to 100 DEG C, temperature no longer rises, mono-esterification
Reaction is completed, and sets heat conduction oil temperature as 200 DEG C, due to the presence of vacuum, when kettle temperature rises to 165 DEG C, and esterification column discharging opening
Temperature rises rapidly, opens esterification condensator circulation cooling water, and esterification condensator outlet regards cup and backflow occurs, according to backflow feelings
Condition improves heat conduction oil temperature to 230 DEG C with 10 DEG C/h, it is ensured that kettle temperature is not higher than 220 DEG C, and when kettle temperature rises to 220 DEG C, insulation is protected
Pressure 25min, esterification section is completed.Reaction time of esterification 5 hours.Product acid number 0.05mgKOH/g.
After the completion of esterification, after kettle temperature to be esterified is down to less than 180 DEG C, material pump is opened, material in esterifying kettle is conveyed
To rectifying still, after the completion of conveying, pumped vacuum systems is opened, set rectifying still heat conduction oil temperature as 200 DEG C, kept in rectifying still
Vacuum is -0.0985Mpa, and 180 DEG C of kettle temperature during 140-160 DEG C of rectifying column tower top temperature, opens rectifying condenser to entering wherein
Material condensed, excessive isooctanol is recycled to alcohol receiving tank, regarded after cup no liquid occurs after alcohol receiving tank, essence is set
Kettle heat conduction oil temperature is evaporated for 290 DEG C, when rectifying still kettle temperature rises to 230 DEG C, will be esterified the light component and micro isooctanol of generation
It is recycled to alcohol receiving tank.With the rising of rectifying still kettle temperature, when rectifying column tower top temperature rises to 240-250 DEG C, by feed liquid
Ester receiving tank is switched to, now at 260-280 DEG C, when ester receiving tank regards cup no liquid, rectifying is completed through chromatogram kettle temperature stabilization
Detection obtains content 99.76%, and color number is 6, the water white transparency Plexol 201 of acid number=0.04mgKOH/g, yield
98.5%, 6 hours rectifying time.
Embodiment 2
First to adding 4400L isooctanol in esterifying kettle and opening esterifying kettle stirring and heat-conducting oil heating, esterifying kettle heat conduction is set
Oil temperature is 75 DEG C, when kettle kettle temperature to be esterified rises to 60 DEG C, opens pumped vacuum systems, and it is -0.06Mpa to keep vacuum in kettle,
Material inlet valve is opened, 2000kg decanedioic acid is drawn in esterifying kettle by vacuum, and add catalyst butyl titanate 15kg, closed
Material inlet valve is closed, pumped vacuum systems is closed, it is -0.05Mpa to keep vacuum in kettle, and now single-esterification starts, mono-esterification
Reaction belongs to exothermic reaction, to make single-esterification fully, need not now heat, when kettle kettle temperature to be esterified rises to 100 DEG C,
Temperature no longer rises, and single-esterification is completed, and esterifying kettle heat conduction oil temperature as 200 DEG C is set, due to the presence of vacuum, in kettle temperature
When rising to 170 DEG C, esterification column discharging opening temperature rises rapidly, opens esterification condensator circulation cooling water, and esterification condensator goes out
Mouth regards cup and backflow occurs, according to backflow situation with 20 DEG C/h raising heat conduction oil temperatures to 230 DEG C, it is ensured that kettle temperature is not high in esterifying kettle
In 220 DEG C, when kettle temperature rises to 220 DEG C, heat-insulation pressure keeping 30min, esterification section is completed.Reaction time of esterification 4 hours.Product acid number
It is 0.04mgKOH/g.
After the completion of esterification, after kettle temperature to be esterified is down to less than 180 DEG C, material pump is opened, material in esterifying kettle is conveyed
To rectifying still, after the completion of conveying, pumped vacuum systems is opened, set rectifying still heat conduction oil temperature as 200 DEG C, kept in rectifying still
Vacuum is -0.099Mpa, and 160 DEG C of kettle temperature during 140-160 DEG C of rectifying column tower top temperature, opens rectifying condenser to entering wherein
Material condensed, excessive isooctanol is recycled to alcohol receiving tank, regarded after cup no liquid occurs after alcohol receiving tank, essence is set
Kettle heat conduction oil temperature is evaporated for 290 DEG C, when rectifying still kettle temperature rises to 230 DEG C, will be esterified the light component and micro isooctanol of generation
It is recycled to alcohol receiving tank.With the rising of rectifying still kettle temperature, when rectifying column tower top temperature rises to 240-250 DEG C, by feed liquid
Ester receiving tank is switched to, now at 260-280 DEG C, when ester receiving tank regards cup no liquid, rectifying is completed rectifying still kettle temperature stabilization
Content 99.82% is obtained through chromatogram detection, color number is 7, and the water white transparency Plexol 201 of acid number=0.03mgKOH/g is produced
Product yield 98.6%, 6 hours rectifying time.
Embodiment 3
First to adding 4400L isooctanol in esterifying kettle and opening stirring and heat-conducting oil heating, esterifying kettle heat conduction oil temperature is set
Be 80 DEG C, when kettle kettle temperature to be esterified rises to 60 DEG C, open pumped vacuum systems, keep kettle in vacuum be -0.04Mpa, open into
Material valve, 2000kg decanedioic acid is drawn in esterifying kettle by vacuum, and adds catalyst butyl titanate 20kg, closes charging
Valve, closes pumped vacuum systems.It is -0.05Mpa to keep vacuum in kettle.Now single-esterification starts, single-esterification category
In exothermic reaction, to make single-esterification fully, need not now heat, when kettle kettle temperature to be esterified rises to 90 DEG C, temperature is not
Rise again, single-esterification is completed, and esterifying kettle heat conduction oil temperature as 200 DEG C is set, due to the presence of vacuum, in esterifying kettle kettle temperature
When rising to 175 DEG C, esterification column discharging opening temperature rises rapidly, opens esterification condensator circulation cooling water, and esterification condensator goes out
Mouth regards cup and backflow occurs, according to backflow situation with 15 DEG C/h raising heat conduction oil temperatures to 230 DEG C, it is ensured that kettle temperature is not higher than 220 DEG C,
When kettle temperature rises to 220 DEG C, heat-insulation pressure keeping 30min, esterification section is completed.Reaction time of esterification 3 hours.Product acid number
0.03mgKOH/g。
After the completion of esterification, after kettle temperature to be esterified is down to less than 180 DEG C, material pump is opened, material in esterifying kettle is conveyed
To rectifying still, after the completion of conveying, pumped vacuum systems is opened, set rectifying still heat conduction oil temperature as 200 DEG C, kept in rectifying still
Vacuum is -0.099Mpa, and 170 DEG C of kettle temperature, 140-160 DEG C of rectifying column tower top temperature opens rectifying condenser therein to entering
Material is condensed, and excessive isooctanol is recycled into alcohol receiving tank, after alcohol receiving tank regards the appearance of cup no liquid, sets rectifying
Kettle heat conduction oil temperature is 290 DEG C, and when rectifying still kettle temperature rises to 230 DEG C, the light component and micro isooctanol that will be esterified generation are returned
Receive to alcohol receiving tank.With the rising of rectifying still kettle temperature, when rectifying column tower top temperature rises to 240-250 DEG C, feed liquid is cut
Ester receiving tank is shifted to, now at 270-280 DEG C, when ester receiving tank regards cup no liquid, rectifying completes warp to rectifying still kettle temperature stabilization
Chromatogram detection obtains content 99.85%, and color number is 8, the water white transparency Plexol 201 of acid number=0.02mgKOH/g, product
Yield 98.7%, 5 hours rectifying time.
Embodiment 4
First to adding 4400L isooctanol in esterifying kettle and opening stirring and heat-conducting oil heating, esterifying kettle heat conduction oil temperature is set
Be 80 DEG C, when kettle kettle temperature to be esterified rises to 60 DEG C, open pumped vacuum systems, keep kettle in vacuum be -0.05Mpa, open into
Material valve, 2000kg decanedioic acid is drawn in esterifying kettle by vacuum, and adds catalyst butyl titanate 20kg, closes charging
Valve, closes pumped vacuum systems.It is -0.05Mpa to keep vacuum in kettle.Now single-esterification starts, single-esterification category
In exothermic reaction, to make single-esterification fully, need not now heat, when kettle kettle temperature to be esterified rises to 95 DEG C, temperature is not
Rise again, single-esterification is completed, and esterifying kettle heat conduction oil temperature as 200 DEG C is set, due to the presence of vacuum, in esterifying kettle kettle temperature
When rising to 170 DEG C, esterification column discharging opening temperature rises rapidly, opens esterification condensator circulation cooling water, and esterification condensator goes out
Mouth regards cup and backflow occurs, according to backflow situation with 12 DEG C/h raising heat conduction oil temperatures to 230 DEG C, it is ensured that esterifying kettle kettle temperature is not higher than
220 DEG C, when kettle kettle temperature to be esterified rises to 220 DEG C, heat-insulation pressure keeping 35min, esterification section is completed.Reaction time of esterification 3 hours.Product
Acid number 0.03mgKOH/g.
After the completion of esterification, after kettle temperature to be esterified is down to less than 180 DEG C, material pump is opened, material in esterifying kettle is conveyed
To rectifying still, after the completion of conveying, pumped vacuum systems is opened, set rectifying still heat conduction oil temperature as 200 DEG C, kept in rectifying still
Vacuum is -0.099Mpa, and 160 DEG C of kettle temperature, 140-160 DEG C of rectifying column tower top temperature opens rectifying condenser therein to entering
Material is condensed, and excessive isooctanol is recycled into alcohol receiving tank, after alcohol receiving tank regards the appearance of cup no liquid, sets rectifying
Kettle heat conduction oil temperature is 290 DEG C, and when rectifying still kettle temperature rises to 230 DEG C, the light component and micro isooctanol that will be esterified generation are returned
Receive to alcohol receiving tank.With the rising of rectifying still kettle temperature, when rectifying column tower top temperature rises to 240-250 DEG C, feed liquid is cut
Ester receiving tank is shifted to, now at 260-270 DEG C, when ester receiving tank regards cup no liquid, rectifying completes warp to rectifying still kettle temperature stabilization
Chromatogram detection obtains content 99.86%, and color number is 8, the water white transparency Plexol 201 of acid number=0.02mgKOH/g, product
Yield 99.3%, 4 hours rectifying time.
Claims (6)
1. the synthetically produced use reaction unit of a kind of Plexol 201, it is characterised in that：The device includes esterifying kettle（1）, ester
Change tower（2）, esterification condensator（3）, separator（4）, rectifying still（5）, rectifying column（6）, rectifying condenser（7）, alcohol receiving tank
（8）, ester receiving tank（9）, pumped vacuum systems and pump induction system, the esterifying kettle（1）And rectifying still（5）Outer surface on respectively
It is provided with the heat-conducting oil heating system for being heated to material in respective kettle（10）, heat-conducting oil heating system（10）It is set in
Corresponding esterifying kettle（1）Or rectifying still（5）Remaining position in addition to top, and avoid being located at esterifying kettle（1）And rectifying still（5）
The discharging opening of bottom；
Described esterification column（2）It is arranged on esterifying kettle（1）Top, esterification column（2）The port of export and esterification condensator（3）Enter
The connection of mouth end, esterification condensator（3）The port of export and separator（4）Entrance point connection, in separator（4）Side wall on also set
It is equipped with and esterifying kettle（1）The alcohol recovery line being connected, the esterifying kettle（1）Discharging opening by the material pump in pump induction system
（11）With rectifying still（5）Charging aperture connection, described rectifying column（6）It is arranged on rectifying still（5）Top, and the rectifying column
（6）The port of export and rectifying condenser（7）Entrance point connection, rectifying condenser（7）The port of export and alcohol receiving tank（8）And ester
Receiving tank（9）Connection.
2. the synthetically produced use reaction unit of a kind of Plexol 201 according to claim 1, it is characterised in that：It is described
Heat-conducting oil heating system（10）In be provided with heat conductive oil inlet（1001）And conduction oil outlet（1002）, heat conductive oil inlet
（1001）And conduction oil outlet（1002）It is separately mounted to heat-conducting oil heating system（10）The top of outer surface side and opposite side
Bottom.
3. the synthetically produced use reaction unit of a kind of Plexol 201 according to claim 1, it is characterised in that：Leading
Heating system of hot oil（10）In be additionally provided with for installing thermometer to esterifying kettle（1）Or rectifying still（5）Interior temperature is measured
Thermometer socket（1003）.
4. the synthetically produced use reaction unit of a kind of Plexol 201 according to claim 1, it is characterised in that：In ester
Change kettle（1）Top be provided with sour charging aperture（101）, alcohol charging aperture（102）, catalyst inlet（103）And drain（104）.
5. carried out with reaction unit using the Plexol 201 described in any claim in claim 1-4 is synthetically produced
The process of Plexol 201 synthesis, it is characterised in that comprise the following steps：
Step one, according to isooctanol and decanedioic acid mol ratio be 2:1 ratio, it is standby to weigh decanedioic acid, and takes excessive different pungent
Alcohol is added to esterifying kettle（1）It is interior, afterwards, open esterifying kettle（1）In stirring system and heat-conducting oil heating system（10）, adjust ester
Change kettle（1）Heat-conducting oil heating system（10）The temperature of middle conduction oil is 70~80 DEG C, works as esterifying kettle（1）Interior temperature is increased to 60 DEG C
When, pumped vacuum systems is enabled to esterifying kettle（1）Vacuumize process is carried out, makes esterifying kettle（1）Interior vacuum is maintained at -0.04~-
0.06Mpa；
Step 2, the esterifying kettle to step one（1）The decanedioic acid that interior addition is weighed, and added decanedioic acid quality 0.5%~1%
Catalyst butyl titanate, afterwards, closes pumped vacuum systems, esterifying kettle（1）Interior material starts reaction, works as esterifying kettle（1）Interior temperature
When degree is increased to 90~100 DEG C, esterifying kettle is adjusted（1）Heat-conducting oil heating system（10）The temperature of middle conduction oil is 200 DEG C, works as ester
Change kettle（1）When interior temperature is increased to 165~175 DEG C, esterification condensator is opened（3）To being condensed into material therein, when
Esterification condensator（3）When there is backflow, esterifying kettle is controlled（1）Heat-conducting oil heating system（10）The temperature of middle conduction oil is with 10~20
DEG C/heating rate of h is warming up to 230 DEG C, works as esterifying kettle（1）When interior temperature is increased to 220 DEG C, esterifying kettle is controlled（1）Interior material
Heat-insulation pressure keeping reaction 25-35min is carried out at such a temperature, afterwards, closes esterifying kettle（1）Heat-conducting oil heating system（10）, complete
Esterification；
Step 3, the material pump passed through the material of step 2 completion esterification in pump induction system（11）It is delivered to rectifying still
（5）It is interior, afterwards, pumped vacuum systems is enabled to rectifying still（5）Vacuumize process is carried out, makes rectifying still（5）Interior vacuum is maintained at-
0.0985~-0.099Mpa, and adjust rectifying still（5）Heat-conducting oil heating system（10）The temperature of middle conduction oil is 200 DEG C, is opened
Rectifying condenser（7）To being condensed into material therein；
Step 4, work as rectifying column（6）When tower top temperature rises to 140~160 DEG C, alcohol receiving tank is opened（8）Valve, receives alcohol
Tank（8）To rectifying column（6）Tower top temperature is that 140~160 DEG C of isooctanol for distillating are collected, when alcohol receiving tank（8）Inside no longer
There is liquid flow fashionable, adjust rectifying still（5）Heat-conducting oil heating system（10）The temperature of middle conduction oil is 290 DEG C, makes alcohol receiving tank
（8）Continue to rectifying column（6）The distillate for distillating is collected, and works as rectifying column（6）When tower top temperature is increased to 240~250 DEG C,
Close alcohol receiving tank（8）Valve, and open ester receiving tank（9）Valve, makes ester receiving tank（9）To rectifying column（6）Tower top temperature surpasses
Cross the distillate distillated at 240~250 DEG C to be collected, ester receiving tank（9）Interior collected material is that finished product decanedioic acid two is different pungent
Ester.
6. using a kind of Plexol 201 synthetic process described in claim 5, it is characterised in that：In step 3
In, the material that the step 2 completes esterification need to be in esterifying kettle（1）When temperature is down to less than 180 DEG C, material pump is carried out（11）
Conveying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710160940.0A CN106674009A (en) | 2017-03-17 | 2017-03-17 | Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate |
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| CN201710160940.0A CN106674009A (en) | 2017-03-17 | 2017-03-17 | Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate |
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|---|---|---|---|
| CN201710160940.0A Pending CN106674009A (en) | 2017-03-17 | 2017-03-17 | Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824720A (en) * | 2019-03-29 | 2019-05-31 | 山东泰和水处理科技股份有限公司 | A kind of dimethylphosphite is continuously synthesizing to method and device |
| CN113413858A (en) * | 2021-08-23 | 2021-09-21 | 山东蓝湾新材料有限公司 | High molecular polymer intermediate production device and process flow |
| CN114307920A (en) * | 2021-07-30 | 2022-04-12 | 江苏雷蒙新材料有限公司 | Continuous production system and production process of polyol acetate |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060052619A1 (en) * | 2002-12-10 | 2006-03-09 | Bernhard Gutsche | Method for producing linear or branched fatty acid esters by means of heterogeneously catalysed reactive rectification with an upstream reactor |
| CN102351692A (en) * | 2011-10-10 | 2012-02-15 | 山东天兴生物科技有限公司 | Preparation method for dimethyl sebacate |
| CN204589035U (en) * | 2014-10-16 | 2015-08-26 | 杭州宇田科技有限公司 | DOTP esterification compressive reaction system |
| CN105418426A (en) * | 2015-12-17 | 2016-03-23 | 安徽华业香料股份有限公司 | Device and method for synthesizing cyclohexyl salicylate by adopting solid alkali as catalyst |
| CN105566105A (en) * | 2016-02-16 | 2016-05-11 | 濮阳市盛源能源科技股份有限公司 | Production device and technology of 1,2-cyclohexanedicarboxylic acid diisobutyl ester |
| CN206624808U (en) * | 2017-03-17 | 2017-11-10 | 濮阳市盛源能源科技股份有限公司 | Plexol 201 is synthetically produced to use reaction unit |
-
2017
- 2017-03-17 CN CN201710160940.0A patent/CN106674009A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060052619A1 (en) * | 2002-12-10 | 2006-03-09 | Bernhard Gutsche | Method for producing linear or branched fatty acid esters by means of heterogeneously catalysed reactive rectification with an upstream reactor |
| CN102351692A (en) * | 2011-10-10 | 2012-02-15 | 山东天兴生物科技有限公司 | Preparation method for dimethyl sebacate |
| CN204589035U (en) * | 2014-10-16 | 2015-08-26 | 杭州宇田科技有限公司 | DOTP esterification compressive reaction system |
| CN105418426A (en) * | 2015-12-17 | 2016-03-23 | 安徽华业香料股份有限公司 | Device and method for synthesizing cyclohexyl salicylate by adopting solid alkali as catalyst |
| CN105566105A (en) * | 2016-02-16 | 2016-05-11 | 濮阳市盛源能源科技股份有限公司 | Production device and technology of 1,2-cyclohexanedicarboxylic acid diisobutyl ester |
| CN206624808U (en) * | 2017-03-17 | 2017-11-10 | 濮阳市盛源能源科技股份有限公司 | Plexol 201 is synthetically produced to use reaction unit |
Non-Patent Citations (2)
| Title |
|---|
| 廖德仲等: "《癸二酸二异辛酯的非酸催化合成》", 《岳阳大学学报》 * |
| 韩长日等: "《橡塑助剂生产工艺与技术》", 30 November 2015, 科学技术文献出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824720A (en) * | 2019-03-29 | 2019-05-31 | 山东泰和水处理科技股份有限公司 | A kind of dimethylphosphite is continuously synthesizing to method and device |
| CN114307920A (en) * | 2021-07-30 | 2022-04-12 | 江苏雷蒙新材料有限公司 | Continuous production system and production process of polyol acetate |
| CN113413858A (en) * | 2021-08-23 | 2021-09-21 | 山东蓝湾新材料有限公司 | High molecular polymer intermediate production device and process flow |
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