CN1114304A - Continuous post-treatment process and equipment for synthesizing ester compounds with high boiling points - Google Patents
Continuous post-treatment process and equipment for synthesizing ester compounds with high boiling points Download PDFInfo
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- CN1114304A CN1114304A CN 94111053 CN94111053A CN1114304A CN 1114304 A CN1114304 A CN 1114304A CN 94111053 CN94111053 CN 94111053 CN 94111053 A CN94111053 A CN 94111053A CN 1114304 A CN1114304 A CN 1114304A
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Abstract
The post-treating method for synthesizing ester compounds with high boiling points features continuous operation, use of falling-film evaporator and washing tower, full removal of solvent and high productivity and quality of product.
Description
The present invention relates to ester compounds with high boiling points synthetic post-treating method and equipment.
Typical esterification can be divided into two kinds of alcoholic acid esterification method and ester-interchange methods.No matter which kind of method of use in most of the cases, all need use solvent and various catalyzer to be beneficial to the carrying out that reacts.For this reason, after reaction is finished, must wash and slough solvent and just can obtain final product.In original synthetic post-treating method, wash and remove solvent two-step and carry out at washing still and still kettle discontinuous formula respectively suddenly.Enter the washing still after reaction is finished in the material autoreaction still and wash, after repeatedly washing reaches requirement, pump into again and distill in the still kettle or underpressure distillation.After lower boiling solvent was distilled, high boiling product was then stayed in the still, and agent content to be held reaches after certain requirement, just can stop distillation, and obtain the finished product.
There is following shortcoming in above-mentioned post-treating method:
1, washing times is limited, is difficult to thoroughly wash impurity to be removed to the greatest extent;
The extremely difficult distillation of solvent eliminates when 2, distilling, and residual solvent levels is too high;
3, to take solvent many for washing process, and solvent can not in time be recycled;
4, the material distillation time is long, and it is bad that material performance is easy to become;
5, washing and distillation plant volume are big.
Particularly above-mentioned the 4th, for those withstand high temperatures and very easily polymeric ester for a long time, as acrylate,, the shortcoming of above-mentioned treatment process is fairly obvious.Make the product of producing in this way, its performance is quite inferior inevitably.
In order to improve above-mentioned high boiling ester synthetic post-treating method, the present invention proposes that a kind of distillation time is short, solvent is removed fully, solvent load is few, can in time reclaim detersive efficiency height, the post-treating method of serialization and equipment thereof.
For achieving the above object, technical scheme of the present invention is:
Esterification reaction product is washed in the still in washing, after separation is anhydrated, pump into falling-film evaporator and carry out successive and remove the solvent operation, the solvent vapour that evaporates from falling-film evaporator is directly recycling use after condenser condenses; Material promptly obtains the high-content product through the material water cooler.
This programme has solved the key issue of the capability and performance difference of removing material heated time length in the dissolving agent process and causing.In order further to improve the continuity of treatment process, esterification reaction product can be injected washing tower and carry out the successive washing operation.Material behind the thorough washing is after centrifugation, and clarifying material pumps into falling-film evaporator again and handles.
In washing process, available multiple washings washs successively.
Accompanying drawing 1 is a process flow diagram of the present invention.
Describe the synthetic continuous post-treatment process of ester compounds with high boiling points in detail below in conjunction with accompanying drawing And equipment.
Material liquid after reaction is finished pumps into behind flow control valve 1 automatic gauge and is positioned at scrubbing tower 1 Material inlet 2, the first cleaning solutions (main cleaning solution) of below are then after the flow self controlled valve metering Enter to be positioned at the cleaning solution entrance 3 of scrubbing tower 1 top. Because the severe of material liquid and cleaning solution is poor, Feed liquid is flowing from bottom to top in tower, cleaning solution is then presented in tower and lower mobile, Both realize disperseing fully and mixing in tower, have finished washing process. At first cleaning solution The second cleaning solution entrance 4 is left in the top of entrance 3, advances for second cleaning solution of different nature Enter scrubbing tower, material is carried out the washing second time. In case of necessity more heterogeneity can be set The entrance of cleaning solution to satisfy the washing requirement. Below material inlet 2, leave colvent inlet 5, For quantitatively pumping into solvent cleaning solution is carried out last extraction. Solvent after extraction is finished is at tower Interior rising mixes the rear dilution that realizes material liquid with material liquid, so that washing process is smooth Carry out. Being positioned at the second cleaning solution entrance, 4 top parts in the scrubbing tower is upper settling section 6, through repeatedly Material liquid after the washing leaves standstill the clarification layering at this, and the material liquid of final clarification overflows through liquid outlet 7 Go out, enter whizzer 8. Being positioned at below, colvent inlet part in the tower is lower settling section 9, warp Cleaning solution after the solvent extraction leaves standstill the clarification layering at this, and the cleaning solution of final clarification goes out through the below Liquid mouth 10 is discharged, and enters waste water system.
The material that settling section liquid outlet 7 overflows on scrubbing tower is general owing to contain the thin of cleaning solution Droplet thereby not yet thoroughly clarification are rendered as opaque milky. For this reason, special with this material Liquid is put into a continuous whizzer 8, obtains clear after separating through high speed centrifugation Material liquid.
Material liquid obtained above (is needed such as the acrylic acid ester after adding various helper components 11 Add polymerization inhibitor), carry out decompression distillation among just can pumping into falling film evaporator 12. Add hot fluid Enter falling film evaporator from entrance 13, to heating material, flow out from exporting 14 afterwards, contain big The material liquid of amount solvent flows from top to bottom in evaporation tube 15 and forms film, and solvent volatilizees rapidly. After gas-liquid separation chamber's 16 interior realization gas-liquid separations, solvent evaporates through condenser 17 condensations, quilt Solvent tanker 18 receives. Solvent circulating pump 19 is obtained solvent and is pumped into scrubbing tower in basin 18 1 interior participation washing process. In evaporation tube the high boiling ester compound of volatilization gasification in gas-liquid Be collected and behind condenser 20, enter material basin 21 in the separation chamber 16 and be final products. Condensation Device 20 and 17 all is communicated with going vacuum system 22.
In sum, the present invention compares with original post-processing approach and has following advantages:
1, treating processes continuous operation.
2, the material evaporation time that is heated shortens.
3, solvent is removed fully, can in time reclaim.
4, washing operation is convenient, the efficient height.
Embodiment 1
Present embodiment is a Comparative Examples.
With traditional intermittent type post-treating method to Viscoat 295 (TMPTA) material after synthetic handle.Washings is 10%NaOH and deionized water, washing respectively, 0.2% stopper.Products obtained therefrom has related parameter as follows,
Product viscosity (CPS) 120
Product form and aspect (APHA) 100
Solvent (%) 8
Solvent-oil ratio (kg/l) 200
Embodiment 2
With method and apparatus of the present invention same material among the embodiment 1 is handled.
Trimethylolpropane tris acrylic acid ester (TMPTA) routinely technology synthetic after, the cooling reaction solution.In washing tower, put in advance and expired solvent benzol.Material liquid is pumped into the material inlet that is positioned at rotating disk washing tower below behind the flowrate control valve automatic gauge, 10% NaOH solution then pumps into the washings inlet that is positioned at rotating disk washing tower top after the metering of flow internally piloted valve.Both throughput ratios are 5: 1.Because the severe of material liquid and washings is poor, material liquid is flowing from bottom to top in tower, and washings then is top-down and flows in tower, and both realize dispersion fully through the effect of rotating disk and mix, finish washing process in tower.Above NaOH washings inlet, leave second washings inlet, from pumping into here, its flow equates with the flow of NaOH solution, so that the washing of material liquid is extremely neutral with deionized water.Below material liquid inlet, leave the colvent inlet, solvent benzol is pumped into from here, flow equates with the flow of material liquid, so that washings is carried out last extraction.Solvent after extraction is finished rises in tower, mixes the dilution of back realization to material liquid with material liquid, so that carrying out smoothly of washing process prevents the emulsification of material liquid.Being positioned at deionized water inlet top part in the washing tower is last settling section, and the material liquid after repeatedly washing leaves standstill the clarification layering at this, and the material liquid of principal defecation overflows through liquid outlet, enters tripping device.Be positioned at below, colvent inlet part in the tower and be following settling section, the washings after solvent extraction leaves standstill the clarification layering at this, and the alkaline waste water of principal defecation is discharged through the below liquid outlet, enters Waste Water Treatment.
The general not thoroughly clarification as yet owing to contain tiny water droplet of the material liquid that the settling section outlet is overflowed on the autorotation disk washing tower is rendered as opaque oyster white.For this reason, the spy puts into this material liquid among the one successive centrifuge separator, separates through high speed centrifugation, has obtained the material liquid of clear.
The above-mentioned material liquid that obtains is carried out underpressure distillation among adding 0.2% stopper (be mixed with in advance 5% solution), just can pumping into falling-film evaporator.The material liquid of the big solvent of amount flows from top to bottom in generating tube and forms film, and solvent volatilizees rapidly.Realize that in the separate chamber solvent vapour is received by solvent tanker through condenser condenses after the gas-liquid separation.The solvent cycle pump is obtained solvent and is pumped into and participates in washing process in the washing tower in basin.Not having the high boiling point esterification thing of volatilization gas to be collected in gas-liquid separation chamber in generating tube and enter the material basin after cooling is the finished product.
The related parameter that has of products obtained therefrom is:
Product viscosity (CPS) 100
Product form and aspect (APHA) 75
Solvent resultant (%) 3
Solvent-oil ratio (KG/l) 50
The product that obtains from two kinds of methods has related parameter relatively, and continuous post-treatment process has remarkable advantages.Both product viscosity appear to and are more or less the same, but because both are the test results under different solvent conditions, therefore in fact both viscosity has very big difference.
Claims (5)
1, the continuous post-treatment process of synthesizing ester compounds with high boiling points, it is characterized in that esterification reaction product is washed in the washing still, after separation is anhydrated, pump into falling-film evaporator and carry out successive and remove solvent operation, the solvent vapour that evaporates from falling-film evaporator is directly recycling use after condenser condenses; Material promptly obtains the high-content product through the material water cooler.
2, the continuous post-treatment process of ester compounds with high boiling points according to claim 1 is characterized in that esterification reaction product is injected washing tower carries out the successive washing operation.
3, method according to claim 2 is characterized in that washing successively with multiple washings.
4, the continuous finishing apparatus of synthesizing ester compounds with high boiling points comprises washing tower, whizzer and falling-film evaporator, and other necessary utility appliance.
5, equipment according to claim 5 is characterized in that washing tower is the rotating disk washing tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94111053 CN1114304A (en) | 1994-06-28 | 1994-06-28 | Continuous post-treatment process and equipment for synthesizing ester compounds with high boiling points |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94111053 CN1114304A (en) | 1994-06-28 | 1994-06-28 | Continuous post-treatment process and equipment for synthesizing ester compounds with high boiling points |
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| Publication Number | Publication Date |
|---|---|
| CN1114304A true CN1114304A (en) | 1996-01-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94111053 Pending CN1114304A (en) | 1994-06-28 | 1994-06-28 | Continuous post-treatment process and equipment for synthesizing ester compounds with high boiling points |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL1021873C2 (en) * | 2002-11-08 | 2004-05-11 | Hermanus Hendrikus Kleizen | Filter device, contains filters with parts containing small passages aligned with parts containing large passages |
-
1994
- 1994-06-28 CN CN 94111053 patent/CN1114304A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL1021873C2 (en) * | 2002-11-08 | 2004-05-11 | Hermanus Hendrikus Kleizen | Filter device, contains filters with parts containing small passages aligned with parts containing large passages |
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