CN102173991A - Continuous alcohol-removing device and alcohol-removing method of di-sec-octyl phthalate - Google Patents
Continuous alcohol-removing device and alcohol-removing method of di-sec-octyl phthalate Download PDFInfo
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- CN102173991A CN102173991A CN2011100353086A CN201110035308A CN102173991A CN 102173991 A CN102173991 A CN 102173991A CN 2011100353086 A CN2011100353086 A CN 2011100353086A CN 201110035308 A CN201110035308 A CN 201110035308A CN 102173991 A CN102173991 A CN 102173991A
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Abstract
The invention discloses a continuous dealcoholizing device and dealcoholizing method of di-sec-octyl phthalate. The dealcoholizing device comprises an dealcoholizing tower and a stripping tower which are connected in series. The dealcoholizing method comprises the following steps: the material obtained through esterification enters the dealcoholizing tower first to re-dealcoholize under the conditions that the material temperature is 160-180 DEG C, the relative pressure is from -0.08MPa to -0.09 MPa, the top gas-phase temperature is more than 90 DEG C and the relative pressure is no more than -0.084MPa; the re-dealcoholized material enters the stripping tower to dealcoholize under the conditions that the material temperature is 160-180 DEG C, the relative pressure is from -0.083MPa to -0.09MPa, the top gas-phase temperature is 120-170 DEG C and the relative pressure is no more than -0.088MPa; and introducing saturated steam in a saturated steam distributor to perform stripping. In the invention, the continuous dealcoholizing production method is adopted; and the residence time of the material in the device is short, the energy consumption is low, the product purity is high, the quality is stable, and the quality and production efficiency of di-sec-octyl phthalate can be increased.
Description
Technical field
The present invention relates to the plasticizer production technical field, be specifically related to the continuous dealcoholization device in the di-sec-octyl phthalate production process and use this device to carry out the method for continuous dealcoholysis.
Background technology
Di-sec-octyl phthalate (DCP) belongs to a kind of softening agent, it is a kind of good softening agent, have good comprehensive performances, its performance that mixes is good, the plasticizing efficiency height, performance classes is similar to o-phthalic acid dibutyl ester (DOP), and thermotolerance, photostabilization, weathering resistance and electrical insulating property are better, can be used as the substitute of DOP usually, are specially adapted in the plastipaste, viscosity stability is good, is widely used in the processing of CABLE MATERIALS, adhesive tape and polyvinyl chloride (PVC) RESINS etc.The existing domestic employing of the production method of di-sec-octyl phthalate (DCP) intermittently dealcoholysis mode is produced, its production technique is to adopt phthalic anhydride and secondary octanol to carry out esterification under the catalyzer existence condition to generate di-sec-octyl phthalate, after esterification finishes, add an amount of basic solution and neutralize unreacted intact monoesters and catalyzer, separate waste water through layering, enter the dealcoholysis of dealcoholysis still after the washing, under the condition of decompression, remove excessive unreacted secondary octanol.Add activated carbon decolorizing again, filter and obtain the finished product.The dealcoholysis operation is a batch operation in the production process, uses still kettle by material being heated the alcohol deviate from the material, and the dealcoholysis time was generally 2 hours.
There are following shortcoming in existing intermittent type dealcoholization device and dealcoholysis production technique: (1) is long heat-up time, and the quality product fluctuation is big, fluctuation of service; (2) equipment, technology fall behind, and labor strength is big; (3) dealcoholysis weak effect, feed purity is low; (4) intermittent type dealcoholysis energy consumption height, small scale can't be accomplished scale production, and has restricted the development of di-sec-octyl phthalate.
Summary of the invention
First technical problem to be solved by this invention is: the deficiency at prior art exists provides a kind of production efficiency height, energy consumption is low, product purity is high, can realize the continuous dealcoholization device in the quantity-produced di-sec-octyl phthalate production process.
Second technical problem to be solved by this invention is: the deficiency at prior art exists provides a kind of production efficiency height, energy consumption is low, product purity is high, can realize the continuous method for dealcoholized in the quantity-produced di-sec-octyl phthalate production process.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
The continuous dealcoholization device of di-sec-octyl phthalate, described dealcoholization device comprises dealcoholize column and stripping tower, described dealcoholize column and stripping tower are respectively equipped with the material inlet on top, the material outlet of bottom and the gaseous phase outlet at top, the material outlet of described dealcoholize column is communicated with the material inlet of described stripping tower, the top of described dealcoholize column is provided with filler, the bottom is provided with vaporizer, the top of described stripping tower is provided with filler, the bottom is provided with thin-film evaporator, and described filler is provided with the saturation steam sparger with between the thin-film evaporator.
The gaseous phase outlet of described dealcoholize column and stripping tower is communicated with condenser and dealcoholysis receiving tank successively, and the gaseous phase outlet of described stripping tower is communicated with condenser and stripping receiving tank successively, and the material outlet of described stripping tower is communicated with finished product storage tank.
As a kind of improvement, described dealcoholysis receiving tank and described stripping receiving tank are respectively equipped with parallel with one another at least two, and described finished product storage tank is provided with parallel with one another at least two.
Preferably, described thin-film evaporator is a falling-film evaporator.
Wherein, described filler is a metal structured packing.
Described saturation steam sparger is to have the vapour pipe that some steam portal.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
The method of utilizing the continuous dealcoholization device of di-sec-octyl phthalate to carry out dealcoholysis may further comprise the steps:
(1) material that esterification is obtained enters from the material inlet on dealcoholize column top, temperature of charge is 160～180 ℃ in dealcoholize column, relative pressure is-0.08～-0.09MPa, dealcoholize column top gas phase temperature＞90 ℃, relative pressure≤-carry out pre-dealcoholysis during 0.084MPa, unreacted secondary octanol is removed in advance.
(2) material inlet of material through stripping tower top that the pre-dealcoholysis in dealcoholize column bottom is finished enters stripping tower, temperature of charge is 160～180 ℃ in stripping tower, relative pressure is-0.083～-0.09MPa, 120～170 ℃ of stripping tower top gas phase temperatures, relative pressure≤-carry out dealcoholysis during 0.088MPa, the self-saturation steam distributor feeds saturation steam and carries out stripping, and stripping finishes the back material and discharges from the material outlet of stripping tower.
The described unreacted secondary octanol steam of deviating from from the gaseous phase outlet of dealcoholize column enters the dealcoholysis receiving tank after condenser condenses, follow the mixing steam of less water to enter the stripping receiving tank after condenser condenses from the secondary octanol that the gaseous phase outlet of stripping tower is deviate from, the part octanol of deviating from reclaims the back and returns esterification step participation esterification.
Preferably, after dealcoholize column bottom material liquid level reaches 800mm, the material inlet of material through stripping tower top entered stripping tower.
Preferably, after stripping tower bottom material liquid level reaches 400mm, begin to feed saturation steam and carry out stripping.
Material after described stripping finishes enters first finished product storage tank at least two finished product storage tank parallel with one another, and liquid level reaches at 80% o'clock in first finished product storage tank, switches to second finished product storage tank parallel with one another.
Absolute pressure 〉=the 1.0MPa of the saturation steam that feeds during described stripping.
Owing to adopted technique scheme, the invention has the beneficial effects as follows:
1, continuous dealcoholization device of the present invention comprises that mutual placed in-line dealcoholize column with stripping tower, not only can realize continuous dealcoholysis, and be provided with saturation steam sparger and thin-film evaporator in the stripping tower that dealcoholysis is effective, product purity height after the dealcoholysis.
2, dealcoholysis receiving tank of the present invention and stripping receiving tank are respectively equipped with parallel with one another at least two, and finished product storage tank also is provided with parallel with one another at least two, and the finished product that helps in the dealcoholysis process the pure and mild dealcoholysis of deviating from being finished switches continuously.
3, method for dealcoholized of the present invention adopts continuous dealcoholysis production method, material is short heat-up time, the dealcoholysis time by 2 hours of prior art shorten to＜10 minutes, reduced production energy consumption, and constant product quality is even, the acidity of product is low after the dealcoholysis, purity is high, has improved the quality and the production efficiency of di-sec-octyl phthalate.
4, the present invention adopts continuous dealcoholysis, because technology is continuous and smooth running, and constant product quality, the mass discrepancy between can not occurring criticizing in the batch production and criticizing.
5, after the present invention adopts continuous dealcoholysis,, reduced heat-up time, not only greatly reduced energy consumption, and product can not cause product colourity to deepen because heated time is long because the dealcoholysis time shortens.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Accompanying drawing is the structural representation of the embodiment of the invention.
Among the figure, 1. dealcoholize column; 11. dealcoholysis material inlet; 12. dealcoholysis material outlet; 13. dealcoholysis gaseous phase outlet; 2. stripping tower; 21. stripping material inlet; 22. stripping material outlet; 23. stripping gaseous phase outlet; 3. metal structured packing; 4. vaporizer; 5. thin-film evaporator; 6. saturation steam sparger; 7. condenser; 8. dealcoholysis receiving tank; 9. stripping receiving tank; 10. finished product storage tank.
Embodiment
As shown in drawings, the continuous dealcoholization device of di-sec-octyl phthalate, described dealcoholization device comprises dealcoholize column 1 and stripping tower 2, described dealcoholize column 1 is provided with the dealcoholysis material inlet 11 on top, the dealcoholysis material outlet 12 of bottom and the dealcoholysis gaseous phase outlet 13 at top, described stripping tower 2 is provided with the stripping material inlet 21 on top, the stripping material outlet 22 of bottom and the stripping gaseous phase outlet 23 at top, described dealcoholysis material outlet 12 is communicated with described stripping material inlet 21, the top of described dealcoholize column 1 is provided with metal structured packing 3, the bottom is provided with vaporizer 4, the top of described stripping tower 2 is provided with metal structured packing 3, the bottom is provided with thin-film evaporator 5, and described metal structured packing 3 is provided with saturation steam sparger 6 with between the thin-film evaporator 5.Described dealcoholysis gaseous phase outlet 13 is communicated with condenser 7 and two dealcoholysis receiving tanks 8 parallel with one another successively, described stripping gaseous phase outlet 23 is communicated with condenser 7 and two stripping receiving tanks 9 parallel with one another successively, and described stripping material outlet 22 is communicated with two finished product storage tank 10 parallel with one another.
Principle of work of the present invention is: the material that esterification is obtained enters dealcoholize column 1 from the dealcoholysis material inlet 11 of dealcoholize column 1, utilize vaporizer 4 heating that the alcohol in the material is vaporized, in the process that in dealcoholize column 1, rises, carrying out after matter changes with cold esterification material under the effect of metal structured packing 3, discharge from dealcoholysis gaseous phase outlet 13, after condenser 7 condensations, be recycled to dealcoholysis receiving tank 8; The material of dealcoholize column 1 bottom after pre-dealcoholysis discharged from dealcoholysis material outlet 12, stripping material inlet 21 from stripping tower 2 enters stripping tower 2 then, utilize thin-film evaporator 5 to make alcohol vaporization remaining in the material, when rising under the stripping effect of the saturation steam of saturation steam sparger 6 ejections, and carrying out under the effect of metal structured packing 3 after matter changes, discharge from stripping gaseous phase outlet 23, be recycled to stripping receiving tank 9 after condenser 6 condensations, the qualified material of dealcoholysis discharges finished product storage tank 10 from stripping material outlet 22.
Further set forth the present invention below in conjunction with specific embodiment.
The vacuum system of dealcoholize column and stripping tower is opened, open the heating valve and give the vaporizer heating of dealcoholize column, the material (comprising di-sec-octyl phthalate and unreacted secondary octanol) that esterification is obtained enters from the material inlet on dealcoholize column top, inlet amount is ascending, temperature of charge is 170 ℃ in dealcoholize column, relative pressure is-0.083MPa, dealcoholize column top gas phase temperature＞90 ℃, carry out pre-dealcoholysis during relative pressure-0.084MPa, the secondary octanol of deviating from is discharged through the dealcoholysis gaseous phase outlet, be recycled to the dealcoholysis receiving tank after condenser condenses, the secondary octanol of deviating from alcohol behind standing demix returns esterification step and participates in esterification.Two dealcoholysis receiving tanks and two stripping receiving tanks parallel with one another switch use respectively.
Open stripping tower thin-film evaporator steam valve, heat to stripping tower, when dealcoholize column bottom material liquid level rises to 800mm, begin the material inlet of material through stripping tower top that the pre-dealcoholysis in dealcoholize column bottom finishes entered stripping tower, temperature of charge is 170 ℃ in stripping tower, relative pressure is-0.086MPa, 120 ℃ of stripping tower top gas phase temperatures, carry out dealcoholysis during relative pressure-0.088MPa, after stripping tower bottom material liquid level reaches 400mm, beginning self-saturation steam distributor feeding absolute pressure is that the saturation steam of 1.0MPa carries out stripping, follow the mixing steam of water to enter the stripping receiving tank after condenser condenses from the secondary octanol that the stripping gaseous phase outlet is discharged, the secondary octanol of deviating from reclaims back time esterification step and participates in esterification.Stripping tower bottom temperature of charge begins when arriving 180 ℃ from the discharging of stripping material outlet to first finished product storage tank parallel with one another, and the interior liquid level of first finished product storage tank reaches at 80% o'clock, switches to second finished product storage tank parallel with one another.
The vacuum system of dealcoholize column and stripping tower is opened, open the heating valve and give the vaporizer heating of dealcoholize column, the material (comprising di-sec-octyl phthalate and unreacted secondary octanol) that esterification is obtained enters from the material inlet on dealcoholize column top, inlet amount is ascending, temperature of charge is 172 ℃ in dealcoholize column, relative pressure is-0.085MPa, dealcoholize column top gas phase temperature＞90 ℃, carry out pre-dealcoholysis during relative pressure-0.086MPa, the secondary octanol of deviating from is discharged through the dealcoholysis gaseous phase outlet, be recycled to the dealcoholysis receiving tank after condenser condenses, the secondary octanol of deviating from reclaims the back and returns esterification step participation esterification.
Open stripping tower thin-film evaporator steam valve, heat to stripping tower, when dealcoholize column bottom material liquid level rises to 800mm, begin the material inlet of material through stripping tower top that the pre-dealcoholysis in dealcoholize column bottom finishes entered stripping tower, temperature of charge is 175 ℃ in stripping tower, relative pressure is-0.086MPa, 130 ℃ of stripping tower top gas phase temperatures, carry out dealcoholysis during relative pressure-0.088MPa, after stripping tower bottom material liquid level reaches 400mm, the saturation steam that beginning self-saturation steam distributor feeds absolute pressure 〉=1.0MPa carries out stripping, follow the mixing steam of water to enter the stripping receiving tank after condenser condenses from the secondary octanol that the stripping gaseous phase outlet is discharged, the alcohol of deviating from reclaims back time esterification step and participates in esterification.Stripping tower bottom temperature of charge begins when arriving 180 ℃ from the discharging of stripping material outlet to first finished product storage tank parallel with one another, and the interior liquid level of first finished product storage tank reaches at 80% o'clock, switches to second finished product storage tank parallel with one another.
The vacuum system of dealcoholize column and stripping tower is opened, open the heating valve and give the vaporizer heating of dealcoholize column, the material (comprising di-sec-octyl phthalate and unreacted secondary octanol) that esterification is obtained enters from the material inlet on dealcoholize column top, inlet amount is ascending, temperature of charge is 176 ℃ in dealcoholize column, relative pressure is-0.08MPa, dealcoholize column top gas phase temperature＞90 ℃, carry out pre-dealcoholysis during relative pressure-0.084MPa, the secondary octanol of deviating from is discharged through the dealcoholysis gaseous phase outlet, be recycled to the dealcoholysis receiving tank after condenser condenses, the secondary octanol of deviating from reclaims the back and returns esterification step participation esterification.
Open stripping tower thin-film evaporator steam valve, heat to stripping tower, when dealcoholize column bottom material liquid level rises to 800mm, begin the material inlet of material through stripping tower top that the pre-dealcoholysis in dealcoholize column bottom finishes entered stripping tower, temperature of charge is 173 ℃ in stripping tower, relative pressure is-0.085MPa, 140 ℃ of stripping tower top gas phase temperatures, relative pressure carries out dealcoholysis during for-0.088MPa, after stripping tower bottom material liquid level reaches 400mm, beginning self-saturation steam distributor feeding absolute pressure is that the saturation steam of 1.0MPa carries out stripping, follow the mixing steam of water to enter the stripping receiving tank after condenser condenses from the secondary octanol that the stripping gaseous phase outlet is discharged, the alcohol of deviating from reclaims back time esterification step and participates in esterification.Stripping tower bottom temperature of charge begins when arriving 180 ℃ from the discharging of stripping material outlet to first finished product storage tank parallel with one another, and the interior liquid level of first finished product storage tank reaches at 80% o'clock, switches to second finished product storage tank parallel with one another.
Embodiment 4
The vacuum system of dealcoholize column and stripping tower is opened, open the heating valve and give the vaporizer heating of dealcoholize column, the material (comprising di-sec-octyl phthalate and unreacted secondary octanol) that esterification is obtained enters from the material inlet on dealcoholize column top, inlet amount is ascending, temperature of charge is 178 ℃ in dealcoholize column, relative pressure is-0.087MPa, dealcoholize column top gas phase temperature＞90 ℃, carry out pre-dealcoholysis during relative pressure-0.084MPa, the secondary octanol of deviating from is discharged through the dealcoholysis gaseous phase outlet, be recycled to the dealcoholysis receiving tank after condenser condenses, the secondary octanol of deviating from reclaims the back and returns esterification step participation esterification.
Open stripping tower thin-film evaporator steam valve, heat to stripping tower, when dealcoholize column bottom material liquid level rises to 800mm, begin the material inlet of material through stripping tower top that the pre-dealcoholysis in dealcoholize column bottom finishes entered stripping tower, temperature of charge is 178 ℃ in stripping tower, relative pressure is-0.087MPa, 150 ℃ of stripping tower top gas phase temperatures, relative pressure carries out dealcoholysis during for-0.088MPa, after stripping tower bottom material liquid level reaches 400mm, beginning self-saturation steam distributor feeding absolute pressure is that the saturation steam of 1.0MPa carries out stripping, follow the mixing steam of water to enter the stripping receiving tank after condenser condenses from the secondary octanol that the stripping gaseous phase outlet is discharged, the alcohol of deviating from reclaims back time esterification step and participates in esterification.Stripping tower bottom temperature of charge begins when arriving 180 ℃ from the discharging of stripping material outlet to first finished product storage tank parallel with one another, and the interior liquid level of first finished product storage tank reaches at 80% o'clock, switches to second finished product storage tank parallel with one another.
Claims (10)
1. the continuous dealcoholization device of di-sec-octyl phthalate, it is characterized in that: described dealcoholization device comprises dealcoholize column and stripping tower, described dealcoholize column and stripping tower are respectively equipped with the material inlet on top, the material outlet of bottom and the gaseous phase outlet at top, the material outlet of described dealcoholize column is communicated with the material inlet of described stripping tower, the top of described dealcoholize column is provided with filler, the bottom is provided with vaporizer, the top of described stripping tower is provided with filler, the bottom is provided with thin-film evaporator, and described filler is provided with the saturation steam sparger with between the thin-film evaporator.
2. the continuous dealcoholization device of di-sec-octyl phthalate as claimed in claim 1, it is characterized in that: the gaseous phase outlet of described dealcoholize column and stripping tower is communicated with condenser and dealcoholysis receiving tank successively, the gaseous phase outlet of described stripping tower is communicated with condenser and stripping receiving tank successively, and the material outlet of described stripping tower is communicated with finished product storage tank.
3. the continuous dealcoholization device of di-sec-octyl phthalate as claimed in claim 2, it is characterized in that: described dealcoholysis receiving tank and described stripping receiving tank are respectively equipped with parallel with one another at least two, and described finished product storage tank is provided with parallel with one another at least two.
4. the continuous dealcoholization device of di-sec-octyl phthalate as claimed in claim 2, it is characterized in that: described thin-film evaporator is a falling-film evaporator.
5. the continuous dealcoholization device of the di-sec-octyl phthalate as claimed in claim 2 method of carrying out dealcoholysis is characterized in that may further comprise the steps:
(1) material that esterification is obtained enters from the material inlet on dealcoholize column top, temperature of charge is 160-180 ℃ in dealcoholize column, relative pressure is-0.08～-0.09MPa, dealcoholize column top gas phase temperature＞90 ℃, relative pressure≤-carry out pre-dealcoholysis during 0.084MPa;
(2) material inlet of material through stripping tower top that the pre-dealcoholysis in dealcoholize column bottom is finished enters stripping tower, temperature of charge is 160～180 ℃ in stripping tower, relative pressure is-0.083～-0.09MPa, 120～170 ℃ of stripping tower top gas phase temperatures, relative pressure≤-carry out dealcoholysis during 0.088MPa, the self-saturation steam distributor feeds saturation steam and carries out stripping, and stripping finishes the back material and discharges from the material outlet of stripping tower.
6. the continuous dealcoholization device of the di-sec-octyl phthalate as claimed in claim 5 method of carrying out dealcoholysis, it is characterized in that: the described pure steam of deviating from from the gaseous phase outlet of dealcoholize column enters the dealcoholysis receiving tank after condenser condenses, and the mixing steam of the alcohol of deviating from from the gaseous phase outlet of stripping tower enters the stripping receiving tank after condenser condenses.
7. the continuous dealcoholization device of the di-sec-octyl phthalate as claimed in claim 6 method of carrying out dealcoholysis is characterized in that: after dealcoholize column bottom material liquid level reaches 800mm, the material inlet of material through stripping tower top entered stripping tower.
8. the continuous dealcoholization device of the di-sec-octyl phthalate as claimed in claim 6 method of carrying out dealcoholysis is characterized in that: after stripping tower bottom material liquid level reaches 400mm, begin to feed saturation steam and carry out stripping.
9. the continuous dealcoholization device of the di-sec-octyl phthalate as claimed in claim 6 method of carrying out dealcoholysis, it is characterized in that: the material after described stripping finishes enters first finished product storage tank at least two finished product storage tank parallel with one another, liquid level reaches at 80% o'clock in first finished product storage tank, switches to second finished product storage tank parallel with one another.
10. the continuous dealcoholization device of the di-sec-octyl phthalate as claimed in claim 6 method of carrying out dealcoholysis is characterized in that: the absolute pressure 〉=1.0MPa of the saturation steam that feeds during described stripping.
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| CN2011100353086A CN102173991A (en) | 2011-01-27 | 2011-01-27 | Continuous alcohol-removing device and alcohol-removing method of di-sec-octyl phthalate |
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| CN2011100353086A CN102173991A (en) | 2011-01-27 | 2011-01-27 | Continuous alcohol-removing device and alcohol-removing method of di-sec-octyl phthalate |
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| CN112569627A (en) * | 2020-11-23 | 2021-03-30 | 福建春达化工有限公司 | Plasticizer stripping system and stripping method |
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| CN103626662A (en) * | 2013-11-09 | 2014-03-12 | 佛山市高明雄业化工有限公司 | Steam esterifying and dealcoholizing method |
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| CN103820295B (en) * | 2014-03-25 | 2016-01-20 | 周午贤 | The distillation of a kind of zero degree grape wine, sterilization, filling one production line |
| CN110698344A (en) * | 2019-11-07 | 2020-01-17 | 江苏正丹化学工业股份有限公司 | Continuous stripping dealcoholization device and method for trioctyl trimellitate |
| CN110698345A (en) * | 2019-11-07 | 2020-01-17 | 江苏正丹化学工业股份有限公司 | Continuous stripping dealcoholization method of diisooctyl terephthalate |
| CN112569627A (en) * | 2020-11-23 | 2021-03-30 | 福建春达化工有限公司 | Plasticizer stripping system and stripping method |
| CN112973607A (en) * | 2021-04-19 | 2021-06-18 | 鹤壁全丰生物科技有限公司 | Continuous production device and process of chlormequat chloride |
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