CN104496807A - Method for neutralizing coarse butyl acrylate - Google Patents
Method for neutralizing coarse butyl acrylate Download PDFInfo
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- CN104496807A CN104496807A CN201410721709.0A CN201410721709A CN104496807A CN 104496807 A CN104496807 A CN 104496807A CN 201410721709 A CN201410721709 A CN 201410721709A CN 104496807 A CN104496807 A CN 104496807A
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- ester
- mixing tank
- coarse
- thick ester
- butyl acrylate
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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
- C07C67/60—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for neutralizing coarse butyl acrylate. The method specifically comprises the following steps: putting the extracted coarse ester, water and 18% of liquid alkali together into a mixer, thoroughly neutralizing the acidic substances in the coarse ester by the liquid alkali in the mixer, next, staying in a phase splitter for 10 minutes, discharge water from the bottom and discharging the neutralized coarse ester from the top; complete neutralization of the coarse ester is guaranteed by virtue of multiple sampling and analysis of the PH value of the coarse ester and multiple addition of the alkali in the process of the mixer, and meanwhile, the alkalinity of the coarse ester cannot be too high; the turbid liquid can be discharged from the ester-water interface in the phase splitter. The method has the advantages that the dosage of the alkali is reduced, the waste water is easy to treat, the turbid liquid is reduced, the investment cost is low and the like.
Description
Technical field
The present invention relates to the technical field of method of a kind of butyl acrylate coarse ester neutralization, particularly relate to the method that butyl acrylate coarse ester that a kind of multiple spot adds alkali and multiple spot test sample neutralizes.
Background technology
After extraction tower, also there is vinylformic acid in butyl acrylate, the material of the aobvious acidity such as catalyzer in thick ester, the acidity in thick ester must be made to reach requirement by neutralization by alkali, not so can not remove butyl acrylate middle acid substance in subsequent processing units.
At present, the acid be used in neutralized crude esters is mainly neutralized by heavy ester washing tower, enter in washing tower together with the waste water that thick ester and wash tower bottoms circulate, sodium hydroxide enters heavy ester washing tower from tower, regulates the alkali adding heavy ester washing tower to keep PH=10-13 by the pH value of the recycle pump sampling and measuring waste water of bottom.Make the alkalescence in waste water too high like this, cause waste water to be difficult to process, processing costs is high.
The polymkeric substance that many turbid liquid and some viscosity are good high is had in heavy ester washing tower.Because the hole in the column plate in heavy ester washing tower is smaller, column plate is easily caused to block; Column plate is thinner simultaneously, is easily out of shape.
During pH value change, need to regulate the add-on of liquid caustic soda, because alkali adds by tower, PH meter is at the bottom of tower, so one long period such as to have could change pH value after adding alkali, easily causes alkali to add, or add inadequate.
Alkali adds and too much causes turbid liquid to increase simultaneously.
Summary of the invention
The object of the invention is the shortcoming in order to overcome above-mentioned prior art, a kind of method that butyl acrylate coarse ester neutralizes is provided, the method of this butyl acrylate coarse ester neutralization uses mixing tank and phase splitter to replace original heavy ester washing tower, makes the acidic substance in the abundant neutralized crude esters of alkali.Have the consumption reducing alkali, the advantages such as waste water easily processes, and investment cost is low, can change waste water alkalescence in traditional technology large, the shortcomings such as intractability is large, have larger industrial value.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method of butyl acrylate coarse ester neutralization, the method step is: after extraction, thick ester, water enter mixing tank together with the liquid caustic soda of 18%, acidic substance in thick ester fully neutralize by liquid caustic soda in a mixer, then enter in phase splitter and stop 10 minutes, bottom discharge, top is thick ester after going out neutralization; In mixing tank process, the pH value of the thick ester of multiple repairing weld analysis, repeatedly adds alkali, guarantees that thick ester alkalescence can not be too high simultaneously with complete in last thick ester; In phase splitter, turbid liquid can be arranged by ester water termination place.
Further, thick ester 16t/h and 0.6m after extraction
3/ h water and 0.1m
3the liquid caustic soda of/h18% enters the first mixing tank together, analyzes pH value, regulate the inlet of 18% liquid caustic soda to make pH value reach 3.5 through the first mixing tank post-sampling.
Further, after the first mixing tank, thick ester out and PH score together with the thick ester after analysing and enter the second mixing tank, analyze pH value, regulate the inlet of 18% liquid caustic soda to make pH value reach 5 through the second mixing tank post-sampling.
Further, after the first mixing tank, thick ester out and PH score together with the thick ester after analysing and enter the 3rd mixing tank, analyze pH value, regulate the inlet of 18% liquid caustic soda to make pH value reach 7 through the 3rd mixing tank post-sampling.
Further, after the first mixing tank, thick ester out and PH score together with the sample after analysing and enter the 4th mixing tank, analyze pH value, regulate the inlet of 18% liquid caustic soda to make pH value reach 9 through the 4th mixing tank post-sampling.
Further, in mixing tank in thick ester and enter phase splitter completely, layering in phase splitter, the bottom of phase splitter goes out waste water to recovery tower, and top goes out the thick ester after neutralization.
Further, turbid liquid can be observed how much also can regularly arrange turbid liquid in the glass-tube liquid level meter of phase splitter.
In sum, add effluent at the bottom of washing tower (for removing CO2) in the method for butyl acrylate coarse ester of the present invention neutralization and traditional tower to have the following advantages:
(1) method repeatedly adding alkali in a small amount makes the acidic substance in the abundant and thick ester of alkali fully react, and saves the consumption of alkali;
(2) thick ester and alkali mix soon in a mixer, and the acidic substance in alkali and thick ester are fully reacted, and regulate the add-on of liquid caustic soda can change the pH value of thick ester fast;
(3) reduce the consumption of alkali, reduce the amount of turbid liquid;
(4) use mixing tank and phase splitter to replace heavy ester washing tower, reduce the expense of investment, heavy ester washing tower can not be caused to bring column plate to block, column plate such as to become at the problem;
(5) alkalinity of waste water reduces, and reduces intractability and the cost of waste water.
Accompanying drawing explanation
Fig. 1 is the schema of the method for a kind of butyl acrylate coarse ester neutralization of the present invention;
Each symbology wherein in Fig. 1 is: the 1-the first mixing tank; 2-the second mixing tank; 3-the three mixing tank
;4-the four mixing tank.
Embodiment
Embodiment 1
The method of a kind of butyl acrylate coarse ester neutralization described by the present embodiment 1, as shown in Figure 1, thick ester 16t/h and 0.6m after extraction
3/ h water and 0.1m
3the liquid caustic soda of/h18% enters the first mixing tank together, and at the sampling analysis pH value of the first mixing tank, make pH value reach 3.5, thick ester is through elbow and 0.1m
3/ h liquid caustic soda also has the thick ester after analyzing to enter the second mixing tank, and in the second mixing tank sampling analysis, make PH reach 5, thick ester is through elbow and 0.1m
3/ h liquid caustic soda also has the thick ester after analyzing to enter the 3rd mixing tank, and in the 3rd mixing tank sampling analysis, make pH value reach 7, thick ester is through elbow and 0.1m
3/ h liquid caustic soda also has the thick ester after analyzing to enter the 4th mixing tank, in the 4th mixing tank sampling analysis, makes pH value reach 9.In mixing tank in thick ester and enter phase splitter completely, layering in phase splitter, the liquid level controlling phase splitter ester aqueous phase is maintained to the middle liquid level of phase splitter, bottom effluent goes recovery tower to reclaim, top goes out thick ester, can observe turbid liquid how many, can regularly arrange turbid liquid in glass-tube liquid level meter.
Embodiment 2
The method of a kind of butyl acrylate coarse ester neutralization described by the present embodiment 2, as shown in Figure 1, thick ester 16t/h and 0.6m after extraction
3/ h water and 0.2m
3the liquid caustic soda of/h18% enters the first mixing tank together, and at the sampling analysis pH value of the first mixing tank, make pH value reach 5, thick ester is through elbow and 0.1m
3/ h liquid caustic soda also has the thick ester after analyzing to enter the second mixing tank, and in the second mixing tank sampling analysis, make PH reach 6.8, thick ester is through elbow and 0.05m
3/ h liquid caustic soda also has the thick ester after analyzing to enter the 3rd mixing tank, and in the 3rd mixing tank sampling analysis, make pH value reach 7.5., thick ester is through elbow and 0.05m
3/ h liquid caustic soda also has the thick ester after analyzing to enter the 4th mixing tank, in the 4th mixing tank sampling analysis, makes pH value reach 9.In mixing tank in thick ester and enter phase splitter completely, layering in phase splitter, the liquid level controlling phase splitter ester aqueous phase is maintained to the middle liquid level of phase splitter, bottom effluent goes recovery tower to reclaim, top goes out thick ester, can observe turbid liquid how many, regularly can arrange turbid liquid in glass-tube liquid level meter.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to technical scheme of the present invention.Every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in the scope of technical scheme of the present invention.
Claims (7)
1. the method for a butyl acrylate coarse ester neutralization, it is characterized in that, the method step is: after extraction, thick ester, water enter mixing tank together with the liquid caustic soda of 18%, acidic substance in thick ester fully neutralize by liquid caustic soda in a mixer, then enter in phase splitter and stop 10 minutes, bottom discharge, top is thick ester after going out neutralization; In mixing tank process, the pH value of the thick ester of multiple repairing weld analysis, repeatedly adds alkali, guarantees that thick ester alkalescence can not be too high simultaneously with complete in last thick ester; In phase splitter, turbid liquid can be arranged by ester water termination place.
2. the method for a kind of butyl acrylate coarse ester neutralization according to claim 1, is characterized in that, thick ester 16t/h and 0.6m after extraction
3/ h water and 0.1m
3the liquid caustic soda of/h18% enters the first mixing tank together, analyzes pH value, regulate the inlet of 18% liquid caustic soda to make pH value reach 3.5 through the first mixing tank post-sampling.
3. the method for a kind of butyl acrylate coarse ester neutralization according to claim 2, it is characterized in that, after the first mixing tank, thick ester out and PH score together with the thick ester after analysing and enter the second mixing tank, analyze pH value through the second mixing tank post-sampling, regulate the inlet of 18% liquid caustic soda to make pH value reach 5.
4. the method for a kind of butyl acrylate coarse ester neutralization according to claim 3, it is characterized in that, after the first mixing tank, thick ester out and PH score together with the thick ester after analysing and enter the 3rd mixing tank, analyze pH value through the 3rd mixing tank post-sampling, regulate the inlet of 18% liquid caustic soda to make pH value reach 7.
5. the method for a kind of butyl acrylate coarse ester neutralization according to claim 4, it is characterized in that, after the first mixing tank, thick ester out and PH score together with the sample after analysing and enter the 4th mixing tank, analyze pH value through the 4th mixing tank post-sampling, regulate the inlet of 18% liquid caustic soda to make pH value reach 9.
6. the method for a kind of butyl acrylate coarse ester neutralization according to claim 1, is characterized in that, in mixing tank in thick ester and enter phase splitter completely, layering in phase splitter, the bottom of phase splitter goes out waste water to recovery tower, the thick ester after top goes out to neutralize.
7. the method for a kind of butyl acrylate coarse ester neutralization according to claim 6, is characterized in that, can observe turbid liquid and how much also can regularly arrange turbid liquid in the glass-tube liquid level meter of phase splitter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410721709.0A CN104496807A (en) | 2014-12-03 | 2014-12-03 | Method for neutralizing coarse butyl acrylate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410721709.0A CN104496807A (en) | 2014-12-03 | 2014-12-03 | Method for neutralizing coarse butyl acrylate |
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| CN104496807A true CN104496807A (en) | 2015-04-08 |
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| CN201410721709.0A Pending CN104496807A (en) | 2014-12-03 | 2014-12-03 | Method for neutralizing coarse butyl acrylate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109879471A (en) * | 2018-12-22 | 2019-06-14 | 江门谦信化工发展有限公司 | In a kind of n-butyl acrylate and COD treatment process drops in waste water drop COD processing unit and waste water |
| CN109988067A (en) * | 2018-12-21 | 2019-07-09 | 江门谦信化工发展有限公司 | A kind of novel purifying niacin dibutyl ester industrialization process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6472554B1 (en) * | 1999-07-28 | 2002-10-29 | Basf Aktiengesellschaft | Continuous preparation of alkyl esters of (meth) acrylic acid |
| CN101397504A (en) * | 2008-11-04 | 2009-04-01 | 中国科学院广州能源研究所 | Production process of biological diesel oil and apparatus |
| RU2443675C1 (en) * | 2010-08-17 | 2012-02-27 | Кенже Рамазанович Рамазанов | Method of neutralising acidic impurities during synthesis of acrylates and apparatus for realising said method |
| CN202595006U (en) * | 2012-04-11 | 2012-12-12 | 江苏雷蒙化工科技有限公司 | Neutralization and water washing continuous device for citric ester |
-
2014
- 2014-12-03 CN CN201410721709.0A patent/CN104496807A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6472554B1 (en) * | 1999-07-28 | 2002-10-29 | Basf Aktiengesellschaft | Continuous preparation of alkyl esters of (meth) acrylic acid |
| CN101397504A (en) * | 2008-11-04 | 2009-04-01 | 中国科学院广州能源研究所 | Production process of biological diesel oil and apparatus |
| RU2443675C1 (en) * | 2010-08-17 | 2012-02-27 | Кенже Рамазанович Рамазанов | Method of neutralising acidic impurities during synthesis of acrylates and apparatus for realising said method |
| CN202595006U (en) * | 2012-04-11 | 2012-12-12 | 江苏雷蒙化工科技有限公司 | Neutralization and water washing continuous device for citric ester |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988067A (en) * | 2018-12-21 | 2019-07-09 | 江门谦信化工发展有限公司 | A kind of novel purifying niacin dibutyl ester industrialization process |
| CN109879471A (en) * | 2018-12-22 | 2019-06-14 | 江门谦信化工发展有限公司 | In a kind of n-butyl acrylate and COD treatment process drops in waste water drop COD processing unit and waste water |
| CN109879471B (en) * | 2018-12-22 | 2021-12-14 | 谦信化工集团有限公司 | COD (chemical oxygen demand) reduction treatment device and COD reduction treatment process for n-butyl acrylate neutralization wastewater |
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Application publication date: 20150408 |
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