CN110407699A - A kind of neutralization technique of diisobutyl phthalate production - Google Patents
A kind of neutralization technique of diisobutyl phthalate production Download PDFInfo
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- CN110407699A CN110407699A CN201910843648.8A CN201910843648A CN110407699A CN 110407699 A CN110407699 A CN 110407699A CN 201910843648 A CN201910843648 A CN 201910843648A CN 110407699 A CN110407699 A CN 110407699A
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- neutralization
- acidity
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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
Abstract
The present invention discloses a kind of neutralization technique of diisobutyl phthalate production, including Alkali liquid compounding, splicing plus alkali neutralization, stratification, chemical examination acidity, alkali waste water discharge, it is secondary neutralize, discharging.Relative to traditional neutralization technique, the present invention neutralizes technique in and has preceding configured lye, and is raised to the rate that certain temperature guarantees neutralization reaction, shortens the processing time；And examined by multiple acidity, it determines the amount of neutralization alkali, effectively controls throwing alkali number, be unlikely to form the waste of alkali；And detected by acidity after stratification, secondary neutralization has advanced optimized neutralization technique.In addition, present device investment cost is low, required space is small, can continuous processing, usage mode is flexible, greatly promotes the overall economic efficiency of enterprise.
Description
Technical field
The present invention relates to a kind of neutralization techniques of diisobutyl phthalate production.
Technical background
Diisobutyl phthalate also known as adjacent phthalandione diisobutyl ester (Diisobutyl phthalate；phthalic
Acid diisobutyl ester, abbreviation DIBP).It is colourless transparent oil liquid, not volatile, slightly aromatic odor.It can
Combustion, toxic, molecular formula C16H22O4.Synthetic method in production is to carry out normal using phthalic anhydride and isobutanol under sulfuric acid catalysis
Liquid-phase esterification is pressed, phthalic acid list isobutyl ester is firstly generated, then proceedes to be esterified, generates two isobutyl of phthalic acid
Ester.In the process reactant need it is neutralized, distillation, alcohol recycling, decoloration, filters pressing and etc. can obtain finished product.Neutralization is benefit
Acid extra in reactant is neutralized with alkaline solution, and to obtain diisobutyl phthalate, adjacent benzene not only can be improved
The yield rate of dioctyl phthalate diisobutyl ester, moreover it is possible to guarantee the safety of the waste water of later discharge.Therefore, in two isobutyl of phthalic acid
In the production process of ester, it is critically important to neutralize technique.The preparation of lye, the additional amount of lye neutralize the temperature-time etc. of hair reaction,
All influence neutralization results.Traditional neutralization technique disposably throws alkali after esterification into reaction solution, if control is not
In place, it is not thorough it will cause reaction neutralization or alkali number is superfluous, form waste.Therefore, it is necessary to excellent to technique progress is neutralized
Change, has solved the above problems.
Summary of the invention
In order to overcome the shortcomings of that tradition neutralizes present in technique, the object of the present invention is to provide a kind of phthalic acids
The neutralization technique of diisobutyl ester production, the technique have short processing time, mode are flexible, recycle diisobutyl phthalate to fill
The advantages that dividing.In order to achieve the above object, the technical solution that the present invention uses is as follows:
A kind of neutralization technique of diisobutyl phthalate production, comprises the following steps that
S1: Alkali liquid compounding: being added a certain amount of water in adding base groove, opens steam valve heating, while the soda ash got ready is added,
The specific inventory of soda ash determines that prepared lye heats up spare again according to the acid value of esterification sampling；
S2: splicing: after esterification, reaction mass after qualified, is transported to neutralization kettle by sample examination, kettle to be neutralized into
After material reaches certain liquid level, stirring is opened；
S3: add alkali neutralization: lye prepared in step S1 being introduced by lye pump and is neutralized in kettle, is stirred simultaneously, carry out
Neutralization reaction；Temperature and the reaction time of neutralization reaction are controlled therebetween；
S4: stratification: it is to be neutralized to stop stirring after reaction, make in kettle material standing sedimentation for a period of time, thus in making
With the material layering in kettle；
S5: chemical examination acidity: taking the material being layered in step S4 to carry out acidity inspection, and acidity value qualification is then directly entered step S6,
Acidity value is unqualified, enters step S7；
S6: alkali waste water discharge: the bottom for going out stratification in step S4 when chemically examining qualified through acidity in step S5 and centre
The liquid of layer drains, and the material of remaining top layer is sent into downstream process；
S7: secondary neutralization: when acidity chemical examination is unqualified, the bottom liquid that stratification in step S4 is gone out is discharged, and is then weighed
Multiple step S3 adds alkali neutralization again, the caustic dosage depending on acidity result of laboratory test in step S5, then repeatedly step S5 and
Step S6；
S8: after acidity chemical examination is qualified, neutralized obtained top layer's material discharging: is transported to the dealcoholysis kettle in downstream.
As a preferred technical scheme, in step S1, the spare alkali liquid temperature is 75~80 DEG C.
As a preferred technical scheme, in step S3, the temperature of the neutralization reaction is 70 ± 5 DEG C, and the reaction time is
10~15min.
As a preferred technical scheme, in step S4, the time of the standing sedimentation is 40~45min.
The neutralization technique of diisobutyl phthalate above-mentioned production, in step S5, acidity value≤0.05% is
It is qualified.
As a preferred technical scheme, the neutralization technique of diisobutyl phthalate above-mentioned production, step S6 and
In step S7, the bottom liquid is discharged into wastewater disposal basin in acidity disqualified upon inspection, and acidity flows back to adding base groove when examining qualified
Lye is prepared as lower batch of neutralization to use.
In addition, the neutralization technique of diisobutyl phthalate production above-mentioned, further includes preparation step, is preparing
Before lye and splicing, adding base groove and neutralization kettle need to be checked, confirm all valve state in which and instrument, tank body are
It is no intact, and correctly wear labour protection articles for use.
The utility model has the advantages that
Relative to traditional neutralization technique, the present invention neutralize technique have it is below and the utility model has the advantages that
(1) present invention has configured in and preceding lye, and is raised to the rate that certain temperature guarantees neutralization reaction, when shortening processing
Between.(2) present invention is examined by multiple acidity, is determined the amount of neutralization alkali, is effectively controlled throwing alkali number, be unlikely to form alkali
Waste.(3) it is detected by acidity after stratification, the secondary thorough solution halfway trouble of neutralization reaction of neutralization, and intermediate
Acidity detection further control reaction has advanced optimized neutralization technique generally through secondary neutralization energy complete neutralization.(4) originally
Invention only use adding base groove and neutralize kettle, equipment investment expense is low, and required space is small, can continuous processing, usage mode is flexible,
Greatly promote the overall economic efficiency of enterprise.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with embodiment, to skill of the invention
Art scheme is clearly and completely described.
A kind of neutralization technique of diisobutyl phthalate production, comprises the following steps that
S1: Alkali liquid compounding: the esterification later period (i.e. 1 hour or so before esterification qualification) need to be good by Alkali liquid compounding.It is first turned on and matches
Alkali slot inlet valve disposably adds water about 900KG；Then open steam valve heating, while be added get ready soda ash 30 ~
80KG, specific soda ash inventory are incorporated alkali slot amount according to the acid value adjustment (one bag of 40KG of soda ash) of esterification sampling；Continue to heat up, control
Alkali liquid temperature processed reaches 75~80 DEG C, stops heating, to be delivered to kettle is neutralized.
S2: splicing: first confirm that the bottom valve for neutralizing kettle, sampling valve are in close state, blow valve is in the open state；So
Whether the material of sample examination esterification is qualified afterwards, after esterification is qualified, opens and neutralizes the splicing of kettle inlet valve, receives esterification
The material finished opens stirring after reaching certain liquid level.
S3: add alkali neutralization: after neutralizing kettle splicing, closing inlet valve, open lye inlet valve；And open lye pump into
Outlet valve opens lye pump, and prepared lye in step S1 is added toward kettle is neutralized；Lye shuts down lye pump after having beaten, close
Lye pump exits and entrances valve is closed, lye inlet valve is closed；Stirring keeps its neutralization reaction abundant；And the temperature for controlling neutralization reaction is
70 ± 5 DEG C, the time of stirring is 1~15min, preferably 10 minutes min.
S4: stratification: to be neutralized stopping is stirred after reaction, makes material standing sedimentation 40min in kettle, to make
Material layering after neutralizing the neutralization in kettle.
S5: chemical examination acidity: taking the material being layered in step S4 to carry out acidity inspection, and acidity≤0.05% is qualification, then directly
It connects and enters step S6, acidity > 0.05% then enters step S7.
S6: alkali waste water discharge: through acidity acidity in step S5≤0.05% when, by stratification in step S4 go out most bottom
Layer and the liquid of middle layer drain, and the material of remaining top layer is sent into the dealcoholysis technique in downstream.
S7: secondary neutralization: the bottom through when acidity acidity > 0.05%, stratification in step S4 is gone out in step S5
Liquid discharge, then repeatedly step S3 adds alkali neutralization again, and the caustic dosage is depending on acidity result of laboratory test in step S5, so
After repeat step S5 and step S6, until the acidity after neutralizing is qualified.
S8: it discharging: chemically examines qualified material and is delivered to dealcoholysis kettle.It is closed after alkali waste water and middle layer discharge are clean and neutralizes kettle
Bottom valve closes alkali waste water vent valves；It opens and neutralizes kettle discharging pump exits and entrances valve, open and neutralize bottom valve, open dealcoholysis kettle
Inlet valve is opened and neutralizes kettle discharging pump, toward dealcoholysis kettle dnockout.Concern at any time neutralizes bottom valve view cup and neutralizes kettle during discharging
Liquid level variation after discharging, shuts down and neutralizes kettle discharging pump, close exits and entrances valve, close and neutralize bottom valve, closes dealcoholysis kettle
Inlet valve.
It should be noted that once neutralize it is unqualified put alkali waste water, salkali waste should be put into wastewater disposal basin, open and neutralize kettle bottom valve
Door opens the valve of connection wastewater disposal basin pipeline, alkali waste water is put only, pays attention to release depending on cup with kettle level condition is neutralized at any time
Middle layer and material；After neutralizing sampling qualification, the alkali waste water that will first neutralize bottom portion is discharged, then can be to dealcoholysis kettle conveying.In
After kettle sample examination acidity qualification, alkali waste water is emitted into adding base groove, does next batch materials neutralization lye.Discharge alkali waste water
When, it opens and neutralizes bottom valve, open the valve for being put into adding base groove pipeline, discharge alkali waste water.Emission request is by alkali waste water and centre
Layer is put net together, and when discharge notices that view cup and neutralization kettle level condition put net middle layer at any time；It is closed after discharge and neutralizes kettle
Bottom valve closes the valve of connection adding base groove pipeline.
In addition, work should be ready into neutralized stream Cheng Qian, check neutralize kettle, all valves of adding base groove (including are put
Empty valve) state in which；Confirmation neutralizes kettle, whether adding base groove bottom valve closes, and whether check valve, instrument, tank body are intact；Just
Really wear labour protection articles for use；And check whether neutralization kettle, each valve of adding base groove feed system are in specified states, confirm nothing
After accidentally, it can start to grasp.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive.Although in addition, it should be understood that originally
Specification is described in terms of embodiments, but only includes not one technical solution, and this narrating mode of specification is only
It is only for clarity that the skilled in the art should refer to the specification as a whole, the technical solution in embodiment can also
To be properly combined, form other embodiments that can be understood by those skilled in the art.
Claims (6)
1. a kind of neutralization technique of diisobutyl phthalate production, it is characterised in that: comprise the following steps that
S1: Alkali liquid compounding: being added a certain amount of water in adding base groove, opens steam valve heating, while the soda ash got ready is added,
The specific inventory of soda ash determines that prepared lye heats up spare again according to the acid value of esterification sampling；
S2: splicing: after esterification, reaction mass after qualified, is transported to neutralization kettle by sample examination, kettle to be neutralized into
After material reaches certain liquid level, stirring is opened；
S3: add alkali neutralization: lye prepared in step S1 being introduced by lye pump and is neutralized in kettle, is stirred simultaneously, carry out
Neutralization reaction；Temperature and the reaction time of neutralization reaction are controlled therebetween；
S4: stratification: it is to be neutralized to stop stirring after reaction, make in kettle material standing sedimentation for a period of time, thus in making
With the material layering in kettle；
S5: chemical examination acidity: taking the material being layered in step S4 to carry out acidity inspection, and acidity value qualification is then directly entered step S6,
Acidity value is unqualified, enters step S7；
S6: alkali waste water discharge: the bottom for going out stratification in step S4 when chemically examining qualified through acidity in step S5 and centre
The liquid of layer drains, and the material of remaining top layer is sent into downstream process；
S7: secondary neutralization: when acidity chemical examination is unqualified, the bottom liquid that stratification in step S4 is gone out is discharged, and is then weighed
Multiple step S3 adds alkali neutralization again, the caustic dosage depending on acidity result of laboratory test in step S5, then repeatedly step S5 and
Step S6；
S8: after acidity chemical examination is qualified, neutralized obtained top layer's material discharging: is transported to the dealcoholysis kettle in downstream.
2. the neutralization technique of diisobutyl phthalate production according to claim 1, it is characterised in that: step S1
In, the spare alkali liquid temperature is 75~80 DEG C.
3. the neutralization technique of diisobutyl phthalate production according to claim 1, it is characterised in that: step S3
In, the temperature of the neutralization reaction is 70 ± 5 DEG C, and the reaction time is 10~15min.
4. the neutralization technique of diisobutyl phthalate production according to claim 1, it is characterised in that: step S4
In, the time of the standing sedimentation is 40~45min.
5. the neutralization technique of diisobutyl phthalate production according to claim 1, it is characterised in that: step S5
In, acidity value≤0.05% is qualification.
6. the neutralization technique of diisobutyl phthalate according to claim 1 production, it is characterised in that: step S6 and
In step S7, the bottom liquid is discharged into wastewater disposal basin in acidity disqualified upon inspection, and acidity flows back to adding base groove when examining qualified
Lye is prepared as lower batch of neutralization to use.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910843648.8A CN110407699A (en) | 2019-09-06 | 2019-09-06 | A kind of neutralization technique of diisobutyl phthalate production |
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| CN201910843648.8A CN110407699A (en) | 2019-09-06 | 2019-09-06 | A kind of neutralization technique of diisobutyl phthalate production |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072366A (en) * | 2013-03-29 | 2014-10-01 | 池银萍 | Preparation method of dibutyl phthalate (DBP) |
| CN105237394A (en) * | 2015-09-18 | 2016-01-13 | 丹阳市助剂化工厂有限公司 | Preparation method of diisobutyl phthalate |
| CN105330539A (en) * | 2015-11-26 | 2016-02-17 | 山东蓝帆化工有限公司 | Production process of dibutyl phthalate plasticizer |
-
2019
- 2019-09-06 CN CN201910843648.8A patent/CN110407699A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072366A (en) * | 2013-03-29 | 2014-10-01 | 池银萍 | Preparation method of dibutyl phthalate (DBP) |
| CN105237394A (en) * | 2015-09-18 | 2016-01-13 | 丹阳市助剂化工厂有限公司 | Preparation method of diisobutyl phthalate |
| CN105330539A (en) * | 2015-11-26 | 2016-02-17 | 山东蓝帆化工有限公司 | Production process of dibutyl phthalate plasticizer |
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