CN102050730A - Process of reducing esterification time in plasticizer production - Google Patents
Process of reducing esterification time in plasticizer production Download PDFInfo
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- CN102050730A CN102050730A CN2010105554231A CN201010555423A CN102050730A CN 102050730 A CN102050730 A CN 102050730A CN 2010105554231 A CN2010105554231 A CN 2010105554231A CN 201010555423 A CN201010555423 A CN 201010555423A CN 102050730 A CN102050730 A CN 102050730A
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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 technology that reduces esterification time in the plasticizer production.
Background technology
Softening agent synthesis techniques such as phthalic acid ester class, aliphatic dicarboxylic acid ester class and citric acid ester type generally are to make by 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, all has water to generate, more to difficult more carrying out of reaction later stage, so, in order to improve reaction efficiency, generally to remove the water in the reaction as far as possible in the industry, to shorten esterification time.What at present domestic most of manufacturers adopted 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, influence 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 influences tower and imitates, 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 technology that reduces esterification time in the plasticizer production, solve the superfluous water that produces in the plasticizer production process, handled reclaiming alcohol, to shorten esterification time effectively, improve reaction efficiency, thereby greatly reduce production energy consumption, reduce production cost.
The technical solution used in the present invention is as follows:
A kind of technology that reduces esterification time in the plasticizer production, raw alcohol is made up of the recovery alcohol of 85%～90% fresh alcohol and 10%～15%, wherein fresh alcohol and recovery alcohol add respectively, earlier fresh alcohol is dropped in the reaction kettle of the esterification, after treating that the esterifying kettle temperature is raised to 130 ℃～135 ℃, will be preheated to 90 ℃～95 ℃ recovery alcohol again and be the atomizing shape by the top of esterification column and spray into.
The present invention improves original technology, change original directly fresh alcohol, the pure technology of reacting in the reaction kettle of the esterification that drops into together of recovery, handled 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 has needed elder generation to heat up when intensification has also reduced esterification separately with the big section time; 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 influence the generation of tower effect situation because of containing saturation water.Further, reclaim the water that contains in the alcohol and can remove by the rectifying section or the stripping section of reactor, thus further fast reaction speed.
Technology of the present invention is specially adapted to the situation that raw alcohol is propyl carbinol or isopropylcarbinol and the production of phthalic acid ester class, 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 technology of the present invention to improve tower is an 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
With the dibutyl phthalate synthesis technique is example, and following embodiment 1 is technology of the present invention, and Comparative Examples 1 is an original production process.
Embodiment 1
Successively to 20m
3Reaction kettle of the esterification in add the 9t phthalic anhydride, 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 ℃, slowly spray into from the esterification cat head by nozzle again, make it to be the atomizing shape by well heater, be heated to 140 ℃～150 ℃ back flow reaction, 4.5h back acid number is reduced 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 reduced 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 (4)
1. technology that reduces esterification time in the plasticizer production, it is characterized in that, raw alcohol is made up of the recovery alcohol of 85%～90% fresh alcohol and 10%～15%, fresh alcohol and recovery alcohol add respectively, earlier fresh alcohol is dropped in the reaction kettle of the esterification, after treating that the esterifying kettle temperature is raised to 130 ℃～135 ℃, will be preheated to 90 ℃～95 ℃ recovery alcohol again and be the atomizing shape by the top of esterification column and spray into.
2. the technology of esterification time is characterized in that in the minimizing plasticizer production as claimed in claim 1, and described raw alcohol is propyl carbinol or isopropylcarbinol.
3. the technology of esterification time is characterized in that in the minimizing plasticizer production as claimed in claim 1, and the top of esterification column is the water that contains in the recovery alcohol that sprays into of atomizing shape and removes by the rectifying section or the stripping section of reactor.
4. as the technology of esterification time in the described minimizing plasticizer production of one of claim 1-3, it is characterized in that described softening agent is phthalic acid ester class, aliphatic dicarboxylic acid ester class or citric acid ester plasticizer.
Priority Applications (1)
| 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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| 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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| Publication Number | Publication Date |
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| CN102050730A true CN102050730A (en) | 2011-05-11 |
| CN102050730B 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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Cited By (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)
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| 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 |
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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 (2)
| Title |
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| 乞少红: "DBP生产中回收醇的再利用", 《河北化工》 * |
| 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》 * |
Cited By (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 |
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| Publication number | Publication date |
|---|---|
| CN102050730B (en) | 2013-05-29 |
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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. |