CN111606802A - DOTP esterification automatic operation process - Google Patents
DOTP esterification automatic operation process Download PDFInfo
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- CN111606802A CN111606802A CN202010506124.2A CN202010506124A CN111606802A CN 111606802 A CN111606802 A CN 111606802A CN 202010506124 A CN202010506124 A CN 202010506124A CN 111606802 A CN111606802 A CN 111606802A
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- Prior art keywords
- esterification
- alcohol
- raw materials
- octanol
- reactor
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- 238000005886 esterification reaction Methods 0.000 title claims abstract description 49
- 230000032050 esterification Effects 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 25
- BJAJDJDODCWPNS-UHFFFAOYSA-N dotp Chemical compound O=C1N2CCOC2=NC2=C1SC=C2 BJAJDJDODCWPNS-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 230000008569 process Effects 0.000 title claims abstract description 19
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 230000009471 action Effects 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000002441 reversible effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000002918 waste heat Substances 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 description 4
- 230000036632 reaction speed Effects 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003333 secondary alcohols Chemical class 0.000 description 2
- 230000009469 supplementation Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- OEIWPNWSDYFMIL-UHFFFAOYSA-N dioctyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C=C1 OEIWPNWSDYFMIL-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of DOTP esterification, and discloses an automatic operation process of DOTP esterification, which comprises the following steps: 1) preparing materials: selecting phthalic acid and octanol raw materials, and pouring the phthalic acid and octanol raw materials into an esterification reactor, so that the step two is conveniently carried out; 2) pretreatment of raw materials: feeding raw materials of terephthalic acid, octanol and a titanate catalyst into an esterification reactor according to a certain mass proportion, and adding the catalyst according to 2-5 per mill of the total material addition; 3) mixing raw materials: under the action of axial flow push-down stirring, the inner coil is used for heating. This DOTP esterifies automated operation technology, through the appropriate amount mixture ratio of phthalic acid and octanol raw and other materials for once only drop into whole raw materials alcohol and change into twice and drop into, utilize the device waste heat to preheat excessive alcohol first, then the low discharge adds in succession, through mending alcohol for the secondary, not only can guarantee that the reaction normally goes on, also can reduce steam consumption, accelerates reaction rate simultaneously, promotes output.
Description
Technical Field
The invention relates to the technical field of DOTP esterification, in particular to an automatic operation process of DOTP esterification.
Background
DOTP is prepared by the reaction of terephthalic acid and octanol, the esterification reaction is a reversible reaction, in order to promote the reaction to proceed to the positive reaction, 30% excess alcohol is added, but now the reaction alcohol and the excess alcohol are added all at once, and the alcohol gas is recycled in the system, thereby causing steam waste.
In the prior art, acid anhydride and sufficient reaction alcohol are added at one time, required steam is introduced for heating, excessive raw material alcohol carries out reaction to generate water, and particularly when the dioctyl terephthalate is produced, because the esterification reaction of the product is heterogeneous solid-liquid reaction, the reaction speed is slow, a large amount of energy is consumed in the production process, and the capacity is limited by the influence of the reaction speed.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the DOTP esterification automatic operation process, which has the advantages of reducing steam consumption, accelerating reaction speed, improving yield and the like, and solves the problems in the background art.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
1) preparing materials: selecting phthalic acid and octanol raw materials, and pouring the phthalic acid and octanol raw materials into an esterification reactor, so that the step two is conveniently carried out;
2) pretreatment of raw materials: feeding raw materials of terephthalic acid, octanol and a titanate catalyst into an esterification reactor according to a certain mass proportion, and adding the catalyst according to 2-5 per mill of the total material addition;
3) mixing raw materials: under the action of axial flow push-down stirring, an inner coil is used for heating, the reaction temperature is controlled to be slowly increased, and water and evaporated alcohol are generated in a reaction in a reactor R6313;
4) conversion to esterification column: after leaving the reactor, the mixture enters an esterification tower, after being in reverse contact with alcohol and water vapor evaporated by the reactor and circulating alcohol refluxed from the top of the tower in the esterification tower, the mixture enters an esterification condensation cooler for condensation and cooling, and then enters an alcohol-water separation tank for settlement and separation, and an alcohol phase overflows through a U-shaped pipe;
5) the manufacturing process comprises the following steps: the refined alcohol enters an esterification reactor to be used as reflux alcohol;
6) and (3) distribution planning: the water separated from the alcohol-water separation tank is sent to a neutralization water washing procedure for reuse;
7) and (3) subsequent treatment: the remaining 30% of fresh alcohol was added to the esterification reactor at a small flow (4 hours) by preheating to 175 ℃ via a medium pressure condensate.
Preferably, in the first step, the phthalic acid and octanol are poured in an excess of 30% more alcohol to promote the reaction to proceed forward.
Preferably, the total amount of phthalic acid, octanol and titanate catalyst is 70%.
Preferably, the addition amount of the catalyst is 2-5 per mill of the total material amount.
Preferably, the pressure in the reactor is controlled to be 0.6-0.8 MPa, so that the adjustment condition of the reaction temperature is guaranteed to be controlled.
Preferably, the internal temperature of the esterification reactor is 200 ℃ when the 30% fresh alcohol is added.
(III) advantageous effects
Compared with the prior art, the invention provides the DOTP esterification automatic operation process, which has the following beneficial effects:
1. this DOTP esterifies automated operation technology, through the appropriate amount mixture ratio of phthalic acid and octanol raw and other materials for once only drop into whole raw materials alcohol and change into twice and drop into, utilize the device waste heat to preheat excessive alcohol first, then the low discharge adds in succession, through mending alcohol for the secondary, not only can guarantee that the reaction normally goes on, also can reduce steam consumption, accelerates reaction rate simultaneously, promotes output.
2. This DOTP automatic operation technology that esterifies, through the setting of reactor and medium pressure lime set, the pressure control is within a definite time at 0.6 ~ 0.8MPa, and esterify the cauldron preheat to 175 ℃ time when the little flow of medium pressure lime set add mix, for esterify the cauldron secondary mend the mellow wine when reaching energy saving and consumption reduction's purpose, more alleviate the bottleneck problem of reaction cycle length, and reduce the energy consumption, practice thrift the steam quantity and reduce the effective action of product cost, the product market competitiveness has been promoted more.
Drawings
FIG. 1 is a schematic diagram of the DOTP esterification automatic operation process structure proposed by the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the DOTP esterification automatic operation process is characterized by comprising the following steps:
1) preparing materials: selecting phthalic acid and octanol raw materials, and pouring the phthalic acid and octanol raw materials into an esterification reactor, so that the step two is conveniently carried out;
2) pretreatment of raw materials: feeding raw materials of terephthalic acid, octanol and a titanate catalyst into an esterification reactor according to a certain mass proportion, and adding the catalyst according to 2-5 per mill of the total material addition;
3) mixing raw materials: under the action of axial flow push-down stirring, an inner coil is used for heating, the reaction temperature is controlled to be slowly increased, and water and evaporated alcohol are generated in a reaction in a reactor R6313;
4) conversion to esterification column: after leaving the reactor, the mixture enters an esterification tower, after being in reverse contact with alcohol and water vapor evaporated by the reactor and circulating alcohol refluxed from the top of the tower in the esterification tower, the mixture enters an esterification condensation cooler for condensation and cooling, and then enters an alcohol-water separation tank for settlement and separation, and an alcohol phase overflows through a U-shaped pipe;
5) the manufacturing process comprises the following steps: the refined alcohol enters an esterification reactor to be used as reflux alcohol;
6) and (3) distribution planning: the water separated from the alcohol-water separation tank is sent to a neutralization water washing procedure for reuse;
7) and (3) subsequent treatment: the remaining 30% of fresh alcohol was added to the esterification reactor at a small flow (4 hours) by preheating to 175 ℃ via a medium pressure condensate.
During the operation of the first step, 30% excessive alcohol is added into the phthalic acid and the octanol to promote the reaction to proceed in the forward and reverse directions.
The total content of phthalic acid, octanol and titanate catalyst is 70%.
The addition amount of the catalyst is 2-5 per mill of the total material amount.
The pressure in the reactor is controlled to be 0.6-0.8 MPa, and the adjustment condition of the reaction temperature is guaranteed to be controlled.
When 30% of fresh alcohol is added, the internal temperature of the esterification reactor is 200 DEG C
The electrical components presented in the document are all electrically connected with an external master controller and 220V mains, and the master controller can be a conventional known device controlled by a computer or the like.
In conclusion, the DOTP esterification automatic operation process changes the one-time input of all raw material alcohol into two-time input through the proper mixing proportion of phthalic acid and octanol raw materials, preheats excessive alcohol by utilizing the waste heat of a device, then continuously adds the excessive alcohol with small flow, not only can ensure the normal reaction, but also can reduce the steam consumption by changing the excessive alcohol into secondary alcohol supplementation, simultaneously quickens the reaction speed and improves the yield, through the arrangement of a reactor and a medium-pressure condensate, the pressure in the reactor is controlled within the range of 0.6-0.8 MPa, and the esterification kettle is preheated to 175 ℃ and then adds the medium-pressure condensate with small flow (4 hours) for matching, so that the bottleneck problem of long reaction period is relieved when the secondary alcohol supplementation operation achieves the purposes of energy saving and consumption reduction, the effective effects of reducing the energy consumption, the steam consumption and the product cost, and the market competitiveness of the product is further improved, (the investment of the process greatly reduces the energy consumption of the auxiliary agent production, saves 4.0MPa steam 6600 tons every year, saves 641 tons of standard coal/year, saves energy, makes a contribution to creating a conservation-minded society, is based on key points of low energy consumption, low cost, environmental protection and the like, meets the national energy-saving and environment-friendly requirements, and has better industry guiding significance after the industrialization is implemented).
The technical quality index is as follows:
technical index
Quality index
| Item | Unit of | Index (I) |
| Acid value | mgKOH | ≤0.2 |
| Excess alcohol | ％ | ≤30 |
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, the use of the verb "comprise a" to define an element does not exclude the presence of another, same element in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
- The DOTP esterification automatic operation process is characterized by comprising the following steps:1) preparing materials: selecting phthalic acid and octanol raw materials, and pouring the phthalic acid and octanol raw materials into an esterification reactor, so that the step two is conveniently carried out;2) pretreatment of raw materials: feeding raw materials of terephthalic acid, octanol and a titanate catalyst into an esterification reactor according to a certain mass proportion, and adding the catalyst according to 2-5 per mill of the total material addition;3) mixing raw materials: under the action of axial flow push-down stirring, an inner coil is used for heating, the reaction temperature is controlled to be slowly increased, and water and evaporated alcohol are generated in a reaction in a reactor R6313;4) conversion to esterification column: after leaving the reactor, the mixture enters an esterification tower, after being in reverse contact with alcohol and water vapor evaporated by the reactor and circulating alcohol refluxed from the top of the tower in the esterification tower, the mixture enters an esterification condensation cooler for condensation and cooling, and then enters an alcohol-water separation tank for settlement and separation, and an alcohol phase overflows through a U-shaped pipe;5) the manufacturing process comprises the following steps: the refined alcohol enters an esterification reactor to be used as reflux alcohol;6) and (3) distribution planning: the water separated from the alcohol-water separation tank is sent to a neutralization water washing procedure for reuse;7) and (3) subsequent treatment: the remaining 30% of fresh alcohol was added to the esterification reactor at a small flow (4 hours) by preheating to 175 ℃ via a medium pressure condensate.
- 2. The DOTP esterification process of claim 1, wherein the first step is performed by adding 30% more excess alcohol to the phthalic acid and octanol to promote the reaction forward and backward reaction.
- 3. A DOTP esterification automation process according to claim 1, characterized in that the total amount of phthalic acid, octanol and titanate catalyst is 70%.
- 4. The DOTP esterification automatic operation process according to the claim 1, characterized in that the catalyst is added in 2-5 per mill of the total material amount.
- 5. The DOTP esterification automatic operation process according to the claim 1, which is characterized in that the pressure in the reactor is controlled to be 0.6-0.8 MPa, and the adjustment condition of the reaction temperature is ensured to be controlled.
- 6. A DOTP esterification automation process according to claim 1, characterized in that the esterification reactor internal temperature at 30% fresh alcohol addition is 200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010506124.2A CN111606802A (en) | 2020-06-05 | 2020-06-05 | DOTP esterification automatic operation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010506124.2A CN111606802A (en) | 2020-06-05 | 2020-06-05 | DOTP esterification automatic operation process |
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| Publication Number | Publication Date |
|---|---|
| CN111606802A true CN111606802A (en) | 2020-09-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010506124.2A Pending CN111606802A (en) | 2020-06-05 | 2020-06-05 | DOTP esterification automatic operation process |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503831A (en) * | 2011-11-07 | 2012-06-20 | 潍坊市元利化工有限公司 | Continuous esterification production method for plasticizer |
| CN105001091A (en) * | 2015-08-31 | 2015-10-28 | 山东齐鲁增塑剂股份有限公司 | Esterification reaction process for plasticizer DOTP (dioctyl terephthalate) |
| CN105198740A (en) * | 2015-08-31 | 2015-12-30 | 山东蓝帆化工有限公司 | DOTP esterification technology |
| CN206372821U (en) * | 2017-01-03 | 2017-08-04 | 山东朗晖石油化学有限公司 | A kind of device for producing DOTP |
| CN207112776U (en) * | 2017-07-27 | 2018-03-16 | 辽宁嘉合精细化工有限公司 | A kind of steam-heating system |
-
2020
- 2020-06-05 CN CN202010506124.2A patent/CN111606802A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503831A (en) * | 2011-11-07 | 2012-06-20 | 潍坊市元利化工有限公司 | Continuous esterification production method for plasticizer |
| CN105001091A (en) * | 2015-08-31 | 2015-10-28 | 山东齐鲁增塑剂股份有限公司 | Esterification reaction process for plasticizer DOTP (dioctyl terephthalate) |
| CN105198740A (en) * | 2015-08-31 | 2015-12-30 | 山东蓝帆化工有限公司 | DOTP esterification technology |
| CN206372821U (en) * | 2017-01-03 | 2017-08-04 | 山东朗晖石油化学有限公司 | A kind of device for producing DOTP |
| CN207112776U (en) * | 2017-07-27 | 2018-03-16 | 辽宁嘉合精细化工有限公司 | A kind of steam-heating system |
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Application publication date: 20200901 |
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