CN102050730B - Process of reducing esterification time in plasticizer production - Google Patents
Process of reducing esterification time in plasticizer production Download PDFInfo
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- CN102050730B CN102050730B CN 201010555423 CN201010555423A CN102050730B CN 102050730 B CN102050730 B CN 102050730B CN 201010555423 CN201010555423 CN 201010555423 CN 201010555423 A CN201010555423 A CN 201010555423A CN 102050730 B CN102050730 B CN 102050730B
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Abstract
The invention belongs to the technical field of plasticizer production, in particular to a process for reducing esterification time in plasticizer production. In the process, the alcohol raw materials are composed of 85%-90% of unused alcohols and 10%-15% of recovered alcohols; the unused alcohols and the recovered alcohols are separately fed; firstly the unused alcohols are fed into an esterification reaction kettle; and then the recovered alcohols that are preheated to 90 DEG C-95 DEG C are sprayed in an atomized state from the top of an esterification tower, after the temperature of the esterification reaction kettle rises to 130 DEG C-135 DEG C. The process is easy to operate, increases the exchange efficiency of the tower, shortens the esterification period, increases the yield, reduces the energy consumption and the cost, and increases the economic benefit.
Description
Technical field
The invention belongs to the plasticizer production technical field, particularly a kind of technique that reduces esterification time in plasticizer production.
Background technology
The softening agent synthesis techniques such as Phthalates, aliphatic dicarboxylic acid ester class and citric acid ester type generally are to make by the di-carboxylic acid classes such as phthalic anhydride or phthalic acid, aliphatic dicarboxylic acid, citric acid or anhydrides chemical intermediate and propyl carbinol or isopropylcarbinol esterification.This type of softening agent reaction process is reversible reaction, has water to generate, more to more difficult carrying out of reaction later stage, so, in order to improve reaction efficiency, generally to remove as far as possible the water in the reaction in the industry, to shorten esterification time.What most domestic manufacturer adopted at present is the alcohol reflux device, and the pure method of applying mechanically of recovery, fresh alcohol, recovery alcohol are dropped in the reaction kettle of the esterification together and reacts, add fresh alcohol in the reaction process, reaction throws away number of times to a certain degree carrying out back flow reaction with raising reaction efficiency, the useless alcohol of minimizing.This Technology has satisfied the requirement of manufacturer to a certain extent, but still exists following shortcoming: the one, and reclaim in the alcohol and contain saturation water, affect in the reactor and heat up; The 2nd, in the alcohol reflux process, the alcohol (containing saturation water) that is back in the esterification column can not in time be vaporized, and affects the tower effect, and in addition, water also can enter reaction kettle of the esterification with alcohol, prolongs esterification time, reduces reaction efficiency.
Summary of the invention
The object of the present invention is to provide a kind of technique that reduces esterification time in plasticizer production, solve the superfluous water that produces in the plasticizer production process, processed reclaiming alcohol, effectively to shorten esterification time, improve reaction efficiency, thereby greatly reduce production energy consumption, Decrease production cost.
The technical solution used in the present invention is as follows:
A kind of technique that reduces esterification time in plasticizer production, raw alcohol is comprised of 85%～90% fresh alcohol and 10%～15% recovery alcohol, wherein fresh alcohol and recovery alcohol add respectively, first fresh alcohol is dropped in the reaction kettle of the esterification, after the esterifying kettle temperature is raised to 130 ℃～135 ℃, will be preheated to again 90 ℃～95 ℃ recovery alcohol and be the atomizing shape by the top of esterification column and sprays into.
The present invention improves original technique, change original directly fresh alcohol, the pure technique of reacting in the reaction kettle of the esterification that drops into together of recovery, processed reclaiming alcohol, adjust the adding mode of alcohol, the alcohol that reclaims is carried out preheating before entering esterifying kettle, it is low that this has just solved the recovery alcohol temperature that enters esterifying kettle, the problem that water wherein can not in time be vaporized; And the process that need to heat up with the large section time first when intensification has also reduced esterification separately; Be the atomizing shape by the top of esterification column and spray into and will reclaim alcohol, the water that reclaims in the alcohol is removed as far as possible, thereby thereby the alcohol of having avoided being back to when refluxing in the esterification column can not in time vaporize and affect the generation that tower is imitated situation because containing saturation water.Further, reclaim the water that contains in the alcohol and can remove by rectifying section or the stripping section of reactor, thus further fast reaction speed.
Technique of the present invention is specially adapted to situation that raw alcohol is propyl carbinol or isopropylcarbinol and the production of Phthalates, aliphatic dicarboxylic acid ester class or citric acid ester plasticizer.
Concrete, reclaim alcohol and can cooperate with pump by preheater and carry out preheating and squeeze in the esterifying kettle.
The exchange efficiency that adopts the improved technique of the present invention to improve tower is esterification efficient, and esterification time has reduced 1.5-2 hour than in the past, and shorten to present every batch 5.5-6h by every crowd of original 7-8h reaction time; Improved output, day output has improved 30-35%; Reduced energy consumption, unit time ton product energy consumption reduces 20-25%; Reduced production cost.
The present invention has following advantage with respect to prior art:
Technological operation of the present invention is simple, has improved the exchange efficiency of tower, has shortened the esterification cycle, has improved output, has reduced energy consumption and cost, has increased economic benefit.
Embodiment
Take the dibutyl phthalate synthesis technique as example, following embodiment 1 is technique of the present invention, and Comparative Examples 1 is original production process.
Embodiment 1
Successively to 20m
3Reaction kettle of the esterification in add the 9t phthalic anhydride, the fresh propyl carbinol of 10t and 150kg catalyzer, heating is stirred, when rising to 130 ℃, temperature keeps constant temperature, 1.2t is reclaimed alcohol be preheated to 92 ℃ by well heater, slowly spray into from the esterification cat head by nozzle again, make it to be the atomizing shape, be heated to 140 ℃～150 ℃ back flow reaction, 4.5h rear acid number is down to 2.0mgKOH/g, esterification finishes, and makes finished product through aftertreatment again.
Comparative Examples 1
Successively to 20m
3Esterifying kettle in add the catalyzer of 9t phthalic anhydride, 10t butanols (1.2t reclaims alcohol, 8.8t fresh alcohol) and 150kg, heating, stir, when rising to 130 ℃, temperature keeps constant temperature, slowly add the fresh butanols of 1.2t, be heated to 140 ℃～150 ℃ back flow reaction, acid number is down to 2.1mgKOH/g behind the 6h, esterification finishes, and makes finished product through aftertreatment again.
The above-mentioned example of the present invention is can not limit the present invention to explanation of the present invention, requiring suitable implication and any change and the combination in the scope with claims of the present invention, all should think in the scope of claims.
Claims (2)
1. technique that reduces esterification time in plasticizer production, it is characterized in that, raw alcohol is comprised of 85%～90% fresh alcohol and 10%～15% recovery alcohol, fresh alcohol and recovery alcohol add respectively, first fresh alcohol is dropped in the reaction kettle of the esterification, after the esterifying kettle temperature is raised to 130 ℃～135 ℃, will be preheated to again 90 ℃～95 ℃ recovery alcohol and be the atomizing shape by the top of esterification column and sprays into; The top of esterification column is the water that contains in the recovery alcohol that sprays into of atomizing shape and removes by rectifying section or the stripping section of reactor.
2. the technique of minimizing esterification time in plasticizer production as claimed in claim 1 is characterized in that, described raw alcohol is propyl carbinol or isopropylcarbinol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010555423 CN102050730B (en) | 2010-11-23 | 2010-11-23 | Process of reducing esterification time in plasticizer production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010555423 CN102050730B (en) | 2010-11-23 | 2010-11-23 | Process of reducing esterification time in plasticizer production |
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| CN102050730A CN102050730A (en) | 2011-05-11 |
| CN102050730B true CN102050730B (en) | 2013-05-29 |
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| CN 201010555423 Active CN102050730B (en) | 2010-11-23 | 2010-11-23 | Process of reducing esterification time in plasticizer production |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952012A (en) * | 2012-10-17 | 2013-03-06 | 河南启瑞生物科技发展有限公司 | Method for improving quality of plasticizer |
| CN111620779A (en) * | 2020-06-08 | 2020-09-04 | 福建春达化工有限公司 | Dibutyl phthalate production process capable of preventing crystallization in esterification kettle |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105982A (en) * | 1994-08-11 | 1995-08-02 | 潍坊开发区精细化工技术开发中心 | Processing method of diethyl metabenzenediformate |
| CN1320593A (en) * | 2000-04-24 | 2001-11-07 | 仪征市化工厂 | Process for preparing dimethyl terephthalate |
| CN1474802A (en) * | 2000-11-13 | 2004-02-11 | �����ɷ� | Method for producing esters of multibasic acids |
-
2010
- 2010-11-23 CN CN 201010555423 patent/CN102050730B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105982A (en) * | 1994-08-11 | 1995-08-02 | 潍坊开发区精细化工技术开发中心 | Processing method of diethyl metabenzenediformate |
| CN1320593A (en) * | 2000-04-24 | 2001-11-07 | 仪征市化工厂 | Process for preparing dimethyl terephthalate |
| CN1474802A (en) * | 2000-11-13 | 2004-02-11 | �����ɷ� | Method for producing esters of multibasic acids |
Non-Patent Citations (4)
| Title |
|---|
| DBP生产中回收醇的再利用;乞少红;《河北化工》;20040620(第3期);第45-46页 * |
| 乞少红.DBP生产中回收醇的再利用.《河北化工》.2004,(第3期),第45-46页. |
| 杨维之 等.邻苯二甲酸二丁酯生产中酯化工艺的改进.《河北省科学院学报》.1999,第16卷(第2期),第50-52页. |
| 邻苯二甲酸二丁酯生产中酯化工艺的改进;杨维之 等;《河北省科学院学报》;19990630;第16卷(第2期);第50-52页 * |
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| CN102050730A (en) | 2011-05-11 |
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Inventor after: Song Guangxun Inventor before: Si Junjie Inventor before: Wang Yanli Inventor before: Liu Weili Inventor before: Yu Shuping Inventor before: Song Guangxun Inventor before: Cheng Shunguo Inventor before: Yao Ning Inventor before: Zhang Zuli Inventor before: Yang Zhen Inventor before: Yao Junying Inventor before: Gao Lihong Inventor before: Wang Xinzhen |
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Effective date of registration: 20160519 Address after: 451150 Henan city of Zhengzhou province Xinzheng City Road No. 218 fisherman Patentee after: Henan Tianning new Mstar Technology Ltd Address before: 451150, No. 189, Qing'an Road, Xinzheng, Henan, Zhengzhou Patentee before: Henan Qing'an Chemicals High Technology Stock Co., Ltd. |