CN102503831A - Continuous esterification production method for plasticizer - Google Patents
Continuous esterification production method for plasticizer Download PDFInfo
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- CN102503831A CN102503831A CN2011103489444A CN201110348944A CN102503831A CN 102503831 A CN102503831 A CN 102503831A CN 2011103489444 A CN2011103489444 A CN 2011103489444A CN 201110348944 A CN201110348944 A CN 201110348944A CN 102503831 A CN102503831 A CN 102503831A
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Abstract
The invention discloses a continuous esterification production method for a plasticizer. The method comprises the following steps of: mixing phthalic anhydride and an alcohol raw material according to the molar ratio of 1:(2.5-3.0), removing water at the temperature of between 150 and 180 DEG C, and thus obtaining a pre-esterification material; heating the alcohol raw material to obtain overheating alcohol gas; and allowing the pre-esterification material to continuously pass through at least two continuous esterification reactors which are connected in series with each other and are provided with catalyst reaction beds, continuously introducing the overheating alcohol gas into the continuous esterification reactors, and taking the plasticizer out of the bottom of the continuous esterification reactor at the tail end continuously. By the continuous esterification production method for the plasticizer, production time is greatly shortened, production efficiency is improved, a large quantity of labor power and material resources are saved, the conversion efficiency of raw materials is improved, the purity of a product is improved, energy consumption is reduced, and the raw materials are saved; and the method is environment-friendly.
Description
Technical field
The present invention relates to the esterification synthesis technical field, relate in particular to a kind of continuous esterification production method of adjacent benzene class softening agent.
Background technology
Softening agent is a kind of flexibility of material or additive of material liquefaction of increasing; Softening agent various in style; Once reached more than 1000 kinds in its kind of its development period; As the softening agent of commodity production kind more than 200 only, and serve as maximum in the phthalate of petrochemical complex with raw material sources.
The existing adjacent benzene class plasticizer production technology of China all adopts esterification at intermittence mode to produce, and adopts phthalic anhydride and alcohol under the catalyzer existence condition, to carry out esterification on the technology, and reaction unit adopts a plurality of reaction kettles that are cascaded; After the reaction kettle internal reaction of front finishes fully; This reaction kettle is shut down, and reaction product is transferred to continuation reaction in the reaction kettle at the back, so repeatedly after the intermittent esterification reaction; The softening agent that extraction makes from the reaction kettle of rearmost end; There is following shortcoming in this existing batch production: (1) batch production is consuming time longer, and the quality product fluctuation is big, less stable; (2) technology falls behind, and labour intensity is big; (3) esterification at intermittence energy consumption, material consumption height, product yield is low; (4) small scale can't be accomplished scale production, and has restricted the output of softening agent.
Summary of the invention
Technical problem to be solved by this invention is: to the deficiency that prior art exists, a kind of continuous esterification production method of softening agent is provided, it shortens the PT, has improved production efficiency and quality product, thereby has addressed the above problem.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of continuous esterification production method of softening agent may further comprise the steps:
(1) with phthalic anhydride and raw polyol with the mixed in molar ratio of 1:2.5～3.0, under 150-180 ℃, carry out preparatory esterification, the water sepn that generates is removed, obtain preparatory esterification material;
(2) get raw polyol in addition and be preheated to 130～150 ℃ earlier, the overheated pure gas of reheat to 200～220 ℃;
(3) with preparatory esterification material continuously through at least two mutual placed in-line, continuous esterification devices of being provided with the catalyst reaction bed; 200～210 ℃ of the bottom temps of head end continuous esterification device wherein; 180～190 ℃ of head temperature, 210～220 ℃ of the bottom temps of terminal continuous esterification device, 185～198 ℃ of head temperature; And the temperature of each continuous esterification device raises successively; In each continuous esterification device, feed overheated pure gas continuously, on the catalyst reaction bed, carry out countercurrent reaction, continuous extraction softening agent product from terminal continuous esterification device bottom with said preparatory esterification material.
As a kind of preferred, said continuous esterification device comprises the one-level continuous esterification device and terminal secondary continuous esterification device of head end.
As a kind of improvement; Among the present invention; The middle and upper part of preparatory esterification material from one-level continuous esterification device got into continuously; Said overheated pure gas gets into from the bottom of one-level continuous esterification device, and overheated pure gas carries out countercurrent reaction with preparatory esterification material on the inner catalyst reaction bed of one-level continuous esterification device, and the softening agent work in-process that reaction generates are discharged from the bottom of said one-level continuous esterification device continuously; Said softening agent work in-process get into from the middle and upper part of secondary continuous esterification device continuously; Overheated pure gas gets into from secondary continuous esterification device bottom; Overheated pure gas and softening agent work in-process are countercurrent reaction on the inner catalyst reaction bed of secondary continuous esterification device; Excessive alcohol is discharged from one-level, secondary continuous esterification device top, and the softening agent product that obtains is reacted in secondary continuous esterification device bottom extraction continuously.
As a kind of improvement, said raw polyol is any in octanol, secondary octanol, butanols or the nonyl alcohol.
As a kind of improvement, said catalyzer is one or more in iron trichloride, tin protoxide, titanium oxide, sodium pyrosulfate or the strongly-acid solid catalyst.
As a kind of further improvement, the add-on of said catalyzer is 3～8wt% of phthalic anhydride amount.
As a kind of improvement, said one-level continuous esterification device is provided with 20 blocks of column plates, and secondary continuous esterification device is provided with 30 blocks of column plates, and said two continuous esterification device tops all are provided with scum dredger, with the water of avoiding excessive alcohol and generate softening agent is taken out of.
As a kind of improvement, the excessive alcohol of being discharged by one-level continuous esterification device top returns preparatory esterifying kettle and recycles through refining.
As a kind of improvement, the excessive alcohol of being discharged by secondary continuous esterification device top returns one-level continuous esterification device and recycles after preheating, being heated as overheated pure gas.
As a kind of improvement, the softening agent of extraction provides heat through preheater for the preheating raw polyol earlier bottom secondary continuous esterification device.
Owing to adopted technique scheme, the invention has the beneficial effects as follows:
1, the present invention adopts one-level continuous esterification device and secondary continuous esterification device that material is carried out the production of two-stage continuous esterification; Having changed traditional intermittent type esterification produces; Need not shut down in the production process and switch material, and just can excessive alcohol be reclaimed huge profit usefulness in process of production, this has just shortened the time of producing greatly; Improve production efficiency, practiced thrift lot of manpower and material resources; The present invention simultaneously is in the continuous esterification production process; Excessive alcohol is reclaimed, and it is got into the esterification production process again, and overheated pure gas and reaction mass have carried out countercurrent reaction on the catalyst reaction bed; Overheated pure gas contacts with reaction mass very fully; Esterification is complete, and feed stock conversion is high, and product purity is high.
2, the present invention feeds preparatory esterification material continuously from the middle and upper part of one-level continuous esterification device; Feed the softening agent work in-process continuously from the middle and upper part of secondary continuous esterification device; Simultaneously, get into overheated pure gas from two continuous esterification device bottoms, and the softening agent that generates is from the extraction continuously of secondary continuous esterification device bottom; Technology operates steadily, the steady quality of product.
3, will feed preheater earlier from the high temperature plasticization agent of the continuous extraction in secondary continuous esterification device bottom among the present invention, in the cooling down high-temperature softening agent, raw polyol carried out preheating, practice thrift energy consumption, reduce energy cost.
4, the present invention uses solid catalyst, with the katalysis of the form of fixed bed performance esterification, realizes reusing catalyzer, economizes in raw materials, and reduces cost.
5, excessive alcohol gets into the systemic circulation use among the present invention after refining, and no waste is discharged, friendly environment.
To sum up, softening agent continuous esterification production method provided by the invention has shortened the time of producing greatly, has improved production efficiency; Practice thrift lot of manpower and material resources, improved conversion of raw material, improved product purity; Cut down the consumption of energy simultaneously, economize in raw materials, friendly environment.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention;
Among the figure: 1. preparatory esterifying kettle, 2. one-level continuous esterification device, 3. secondary continuous esterification device, 4. preheater, 5. well heater.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect and be easy to understand and understand, below in conjunction with concrete diagram, further set forth the present invention.
Shown in accompanying drawing; A kind of continuous esterification production method of softening agent may further comprise the steps: (1) is being warming up to 150-180 ℃ in the esterifying kettle 1 in advance with phthalic anhydride and the raw polyol mixed in molar ratio with 1:2.5～3.0; The water that generates is removed from preparatory esterifying kettle 1 separation, obtained preparatory esterification material; (2) get raw polyol in addition and earlier be preheated to 130～150 ℃, be heated to 200～220 ℃ by well heater 5 again and get overheated pure gas through preheater 4; (3) middle and upper part of preparatory esterification material from one-level continuous esterification device 2 got into continuously; Said overheated pure gas gets into from the reboiler upper end of one-level continuous esterification device 2; Overheated pure gas carries out countercurrent reaction with preparatory esterification material on the catalyst reaction bed; The softening agent work in-process that reaction generates are discharged from the bottom of said one-level continuous esterification device 2 continuously, and excessive alcohol and the water that generates are discharged in the top of one-level continuous esterification device 2; (4) the softening agent work in-process that will discharge from the bottom of one-level continuous esterification device 2 get into from the middle and upper part of secondary continuous esterification device 3 continuously; Overheated pure gas gets into from the reboiler upper end of secondary continuous esterification device 3; Overheated pure gas and softening agent work in-process are countercurrent reaction on the catalyst reaction bed of secondary continuous esterification device 3; With phthalic anhydride and monoesters continuation that generates and the raw polyol reaction completely of unreacted in the one-level continuous esterification device 2; Excessive alcohol that discharge at secondary continuous esterification device 3 tops and the less water that generates, the softening agent that the continuous extraction reaction in secondary continuous esterification device 3 bottoms obtains.
Said one-level continuous esterification device 2 is provided with 20 blocks of column plates, and secondary continuous esterification device 3 is provided with 30 blocks of column plates, and said two continuous esterification device tops all are provided with scum dredger, with the water of avoiding excessive alcohol and generate softening agent is taken out of.
Phthalic anhydride and octanol with the mixed in molar ratio of 1:2.7, are warming up to 180 ℃, the water that generates are separated from preparatory esterifying kettle 1 top remove, obtain preparatory esterification material; Octanol is preheated to 150 ℃ through preheater 4 earlier, is heated to 200 ℃ by well heater 5 again and gets overheated octanol gas; The middle and upper part of preparatory esterification material from one-level continuous esterification device 2 got into continuously; Overheated octanol gas gets into from the reboiler upper end of one-level continuous esterification device 2 bottoms, and superheated octanol gas upwards carries out countercurrent reaction with the preparatory esterification material that gets into from top at the catalyst reaction bed, and catalyzer is an iron trichloride; The add-on of catalyzer is the 6wt% of phthalic anhydride amount; 210 ℃ of the bottom temps of control one-level continuous esterification device 2,190 ℃ of head temperature, the softening agent work in-process that reaction generates are discharged from the bottom of one-level continuous esterification device 2 continuously; The excessive octanol and the water of generation are discharged in the top, and octanol returns preparatory esterifying kettle 1 and recycles after refining the purification; The work in-process that to discharge from the bottom of one-level continuous esterification device 2 get into from the middle and upper part of secondary continuous esterification device 3 continuously; Heater via 5 is heated to the reboiler upper end entering of superheated octanol steam from secondary continuous esterification device 3 bottoms; Superheated octanol steam and work in-process are countercurrent reaction on the catalyst reaction bed of secondary continuous esterification device 3; Catalyzer is an iron trichloride, and the add-on of catalyzer is the 4wt% of phthalic anhydride amount, 220 ℃ of the bottom temps of control secondary continuous esterification device 3; 198 ℃ of head temperature are with unreacted continuation such as phthalic anhydride, monoesters completely and octanol reaction in the one-level continuous esterification device 2; The excessive octanol and the less water of generation are discharged in the top, return one-level continuous esterification device 2 and recycle, when the acidity of reaction mass is≤0.1 (in phthalic acid); Esterification finishes, and the softening agent esterification material that reacts completely is from the continuous extraction in secondary continuous esterification device 3 bottoms.
Phthalic anhydride and secondary octanol with the mixed in molar ratio of 1:2.8, are warming up to 170 ℃, the water that generates are separated from preparatory esterifying kettle 1 top remove, obtain preparatory esterification material; Secondary octanol is preheated to 145 ℃ through preheater 4 earlier, is heated to 210 ℃ by well heater 5 again and gets overheated secondary octanol gas; The middle and upper part of preparatory esterification material from one-level continuous esterification device 2 got into continuously; Overheated secondary octanol gas gets into from the reboiler upper end of one-level continuous esterification device 2 bottoms; The secondary octanol gas of superheated upwards carries out countercurrent reaction with the preparatory esterification material that gets into from top at the catalyst reaction bed; Catalyzer is a tin protoxide, and the add-on of catalyzer is the 8wt% of phthalic anhydride amount, 205 ℃ of the bottom temps of control one-level continuous esterification device 2; 185 ℃ of head temperature; The softening agent work in-process that reaction generates are discharged from the bottom of one-level continuous esterification device 2 continuously, and the excessive secondary octanol and the water of generation are discharged in the top, and secondary octanol returns preparatory esterifying kettle 1 and recycles after refining the purification; The work in-process that to discharge from the bottom of one-level continuous esterification device 2 get into from the middle and upper part of secondary continuous esterification device 3 continuously; Heater via 5 is heated to the reboiler upper end entering of the secondary octanol steam of superheated from secondary continuous esterification device 3 bottoms; The secondary octanol steam of superheated and work in-process countercurrent reaction on the catalyst reaction bed of secondary continuous esterification device 3; Catalyzer is a titanium oxide, and the add-on of catalyzer is the 6wt% of phthalic anhydride amount, 215 ℃ of the bottom temps of control secondary continuous esterification device 3; Phthalic anhydride, monoesters etc. continue and secondary octanol reaction completely with unreacted in the one-level continuous esterification device 2 for 190 ℃ of head temperature; The excessive secondary octanol and the less water of generation are discharged in the top, return one-level continuous esterification device 2 and recycle, when the acidity of reaction mass is≤0.1 (in phthalic acid); Esterification finishes, and the softening agent esterification material that reacts completely is from the continuous extraction in secondary continuous esterification device 3 bottoms.
Phthalic anhydride and propyl carbinol with the mixed in molar ratio of 1:2.5, are warming up to 150 ℃, the water that generates are separated from preparatory esterifying kettle 1 top remove, obtain preparatory esterification material; Propyl carbinol is preheated to 130 ℃ through preheater 4 earlier, is heated to 200 ℃ by well heater 5 again and gets overheated propyl carbinol gas; The middle and upper part of preparatory esterification material from one-level continuous esterification device 2 got into continuously; Overheated propyl carbinol gas gets into from the reboiler upper end of one-level continuous esterification device 2 bottoms; Superheated propyl carbinol gas upwards carries out countercurrent reaction with the preparatory esterification material that gets into from top at the catalyst reaction bed; Catalyzer is a titanium oxide, and the add-on of catalyzer is the 5wt% of phthalic anhydride amount, 200 ℃ of the bottom temps of control one-level continuous esterification device 2; 180 ℃ of head temperature; The softening agent work in-process that reaction generates are discharged from the bottom of one-level continuous esterification device 2 continuously, and the excessive propyl carbinol and the water of generation are discharged in the top, and propyl carbinol returns preparatory esterifying kettle 1 and recycles after refining the purification; The work in-process that to discharge from the bottom of one-level continuous esterification device 2 get into from the middle and upper part of secondary continuous esterification device 3 continuously; Heater via is heated to the reboiler upper end entering of superheated propyl carbinol steam from secondary continuous esterification device 3 bottoms; Superheated propyl carbinol steam and work in-process are countercurrent reaction on the catalyst reaction bed of secondary continuous esterification device 3, and catalyzer is a sodium pyrosulfate, and the add-on of catalyzer is the 3wt% of phthalic anhydride amount; 210 ℃ of the bottom temps of control secondary continuous esterification device 3; 185 ℃ of head temperature, with unreacted continuation such as phthalic anhydride, monoesters completely and propyl carbinol reaction in the one-level continuous esterification device 2, the excessive propyl carbinol and the less water of generation are discharged in the top; Returning one-level continuous esterification device 2 recycles; When the acidity of reaction mass was≤0.1 (in phthalic acid), esterification finished, and the softening agent esterification material that reacts completely is from the continuous extraction in secondary continuous esterification device 3 bottoms.
The present invention is not limited to above-mentioned embodiment, and all are based on technical conceive of the present invention, and the structural improvement of having done all falls among protection scope of the present invention.
Claims (10)
1. the continuous esterification production method of a softening agent is characterized in that: may further comprise the steps:
(1) with phthalic anhydride and raw polyol with the mixed in molar ratio of 1:2.5～3.0, under 150-180 ℃, carry out preparatory esterification, the water sepn that generates is removed, obtain preparatory esterification material;
(2) get raw polyol in addition and be preheated to 130～150 ℃ earlier, the overheated pure gas of reheat to 200～220 ℃;
(3) with preparatory esterification material continuously through at least two mutual placed in-line, continuous esterification devices of being provided with the catalyst reaction bed; 200～210 ℃ of the bottom temps of head end continuous esterification device wherein; 180～190 ℃ of head temperature, 210～220 ℃ of the bottom temps of terminal continuous esterification device, 185～198 ℃ of head temperature; And the temperature of each continuous esterification device raises successively; In each continuous esterification device, feed overheated pure gas continuously, on the catalyst reaction bed, carry out countercurrent reaction, continuous extraction softening agent product from terminal continuous esterification device bottom with said preparatory esterification material.
2. the continuous esterification production method of a kind of softening agent according to claim 1 is characterized in that: said continuous esterification device comprises the one-level continuous esterification device and terminal secondary continuous esterification device of head end.
3. the continuous esterification production method of a kind of softening agent according to claim 2; It is characterized in that: the esterification material gets into from the middle and upper part of one-level continuous esterification device continuously in advance; Said overheated pure gas gets into from the bottom of one-level continuous esterification device; Overheated pure gas carries out countercurrent reaction with preparatory esterification material on the inner catalyst reaction bed of one-level continuous esterification device, the softening agent work in-process that reaction generates are discharged from the bottom of said one-level continuous esterification device continuously; Said softening agent work in-process get into from the middle and upper part of secondary continuous esterification device continuously; Overheated pure gas gets into from secondary continuous esterification device bottom; Overheated pure gas and softening agent work in-process are countercurrent reaction on the inner catalyst reaction bed of secondary continuous esterification device; Excessive alcohol is discharged from one-level, secondary continuous esterification device top, and the softening agent product that obtains is reacted in secondary continuous esterification device bottom extraction continuously.
4. the continuous esterification production method of a kind of softening agent according to claim 1, it is characterized in that: said raw polyol is any in octanol, secondary octanol, butanols or the nonyl alcohol.
5. according to the continuous esterification production method of claim 1 or 2 or 3 described a kind of softening agent, it is characterized in that: said catalyzer is one or more in iron trichloride, tin protoxide, titanium oxide, sodium pyrosulfate or the strongly-acid solid catalyst.
6. the continuous esterification production method of a kind of softening agent according to claim 5, it is characterized in that: the add-on of said catalyzer is 3～8wt% of phthalic anhydride amount.
7. according to the continuous esterification production method of claim 2 or 3 described a kind of softening agent; It is characterized in that: said one-level continuous esterification device is provided with 20 blocks of column plates; Secondary continuous esterification device is provided with 30 blocks of column plates, and said two continuous esterification device tops all are provided with scum dredger.
8. the continuous esterification production method of a kind of softening agent according to claim 3 is characterized in that: the excessive alcohol that discharge at said one-level continuous esterification device top returns preparatory esterifying kettle and recycles through refining.
9. the continuous esterification production method of a kind of softening agent according to claim 3; It is characterized in that: the excessive alcohol that discharge at said secondary continuous esterification device top returns one-level continuous esterification device and recycles after preheating, being heated as overheated pure gas.
10. the continuous esterification production method of a kind of softening agent according to claim 3 is characterized in that: the softening agent of said secondary continuous esterification device bottom extraction removes step (2) preheating raw polyol.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435487A (en) * | 2013-08-13 | 2013-12-11 | 浙江合诚化学有限公司 | Preparation method of phthalic acid esters |
| CN104496818A (en) * | 2014-12-19 | 2015-04-08 | 河南奥思达新材料有限公司 | Method or producing DBP by utilizing composite Lewis acid catalysis method |
| CN105111075A (en) * | 2015-08-28 | 2015-12-02 | 华东理工大学 | Novel continuous production technique of phthalate plasticizer |
| CN107935846A (en) * | 2017-11-03 | 2018-04-20 | 中国林业科学研究院林产化学工业研究所 | A kind of apparatus and method of continuous production environment-friendlyplasticizer plasticizer |
| CN111606802A (en) * | 2020-06-05 | 2020-09-01 | 山东朗晖石油化学股份有限公司 | DOTP esterification automatic operation process |
| CN113692398A (en) * | 2019-07-04 | 2021-11-23 | 株式会社Lg化学 | Process for the continuous production of diesters |
| JP2023507541A (en) * | 2020-11-17 | 2023-02-24 | エルジー・ケム・リミテッド | Method for producing diester-based substance |
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| CN101891610A (en) * | 2010-07-03 | 2010-11-24 | 潍坊市元利化工有限公司 | Continuous esterification production method for mixed dibasic acid dimethyl ester |
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| GB1078378A (en) * | 1964-05-02 | 1967-08-09 | Kyowa Hakko Kogyo Kk | Process for the continuous production of diesters of phthalic acid |
| CN101891610A (en) * | 2010-07-03 | 2010-11-24 | 潍坊市元利化工有限公司 | Continuous esterification production method for mixed dibasic acid dimethyl ester |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435487A (en) * | 2013-08-13 | 2013-12-11 | 浙江合诚化学有限公司 | Preparation method of phthalic acid esters |
| CN104496818A (en) * | 2014-12-19 | 2015-04-08 | 河南奥思达新材料有限公司 | Method or producing DBP by utilizing composite Lewis acid catalysis method |
| CN105111075A (en) * | 2015-08-28 | 2015-12-02 | 华东理工大学 | Novel continuous production technique of phthalate plasticizer |
| CN107935846A (en) * | 2017-11-03 | 2018-04-20 | 中国林业科学研究院林产化学工业研究所 | A kind of apparatus and method of continuous production environment-friendlyplasticizer plasticizer |
| CN107935846B (en) * | 2017-11-03 | 2020-01-10 | 中国林业科学研究院林产化学工业研究所 | Device and method for continuously producing environment-friendly plasticizer |
| CN113692398A (en) * | 2019-07-04 | 2021-11-23 | 株式会社Lg化学 | Process for the continuous production of diesters |
| CN111606802A (en) * | 2020-06-05 | 2020-09-01 | 山东朗晖石油化学股份有限公司 | DOTP esterification automatic operation process |
| JP2023507541A (en) * | 2020-11-17 | 2023-02-24 | エルジー・ケム・リミテッド | Method for producing diester-based substance |
| JP7331301B2 (en) | 2020-11-17 | 2023-08-23 | エルジー・ケム・リミテッド | Method for producing diester-based substance |
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Free format text: CORRECT: APPLICANT; FROM: WEIFANG YUANLI CHEMICAL CO., LTD. TO: SHANDONG YUANLI SCIENCE AND TECHNOLOGY CO., LTD. |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120620 |