CN102964318A - Recycling and refining method of ETE byproducts - Google Patents
Recycling and refining method of ETE byproducts Download PDFInfo
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- CN102964318A CN102964318A CN2012104468295A CN201210446829A CN102964318A CN 102964318 A CN102964318 A CN 102964318A CN 2012104468295 A CN2012104468295 A CN 2012104468295A CN 201210446829 A CN201210446829 A CN 201210446829A CN 102964318 A CN102964318 A CN 102964318A
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- moisture eliminator
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Abstract
The invention relates to the technical field of byproduct recycling in TET synthesis technique and especially relates to a recycling and refining method of ETE byproducts and a special device for the method. The method comprises the following steps: 1. conveying reaction products of TET synthesis reaction through phase transfer catalytic reaction technology into a centrifuge to perform centrifugal separation, and separating the filtrate from filter residues after the centrifugal separation; and 2. firstly, continuously forming negative pressure in a dryer, and then conveying the centrifugally separated filter residues into the dryer. According to the invention, the materials are integrally dried and the materials can be completely treated by starting and stopping the dryer and a vacuum pump for one time, thereby effectively reducing the necessary drying time, the work load of operators and the starting and stopping times of the equipment and prolonging the service life of the equipment; and meanwhile, a compulsive cooling mode of filling cooling water through a dryer jacket is used for shortening the cooling time and improving the working efficiency.
Description
Technical field
The present invention relates to byproduct of reaction recovery technology field in the synthetic ETE technique, is a kind of purification and recover method and isolated plant thereof of ETE by product.
Background technology
Existing ETE by-product recovery technique is after reaction product is carried out centrifugation, filtrate is sent, filter residue directly enters moisture eliminator and processes, need after drying is complete to wait for after the material naturally cooling is down to normal temperature and can pack, to produce 4 batches of calculating every day, drying process need to be carried out four times, and equipment needs start-stop four times, and every batch of drying and be about six hours cooling time, the problem such as have therefore that inefficiency, operator's workload are large, the wasting of resources, equipment start-stop are frequent.
Summary of the invention
The invention provides a kind of purification and recover method of ETE by product, overcome the deficiency of above-mentioned prior art, it can effectively solve, and existing process efficiency is low, operator's workload is large, the wasting of resources, equipment start-stop problem frequently.
One of technical scheme of the present invention realizes by following measures: a kind of purification and recover method of ETE by product, carry out in the steps below: the first step: the reaction product that will adopt the phase-transfer-catalyzed reactions technology to synthesize ETE is sent into whizzer and is carried out centrifugation, separates filtrate and filter residue after the centrifugation; Second step: at first moisture eliminator is continued to take out negative pressure, then the filter residue after the centrifugation is sent in the moisture eliminator, then after passing into low-pressure steam in the chuck of moisture eliminator filter residue is carried out drying, the temperature of filter residue is 110 ℃ to 160 ℃ when dry, and be 3 hours to 5 hours time of drying; The 3rd step: enter after the gas that produces in the drying process is extracted out under the effect of taking out negative pressure and carry out condensation in the condenser, the filtrate in condensed liquid and the first step is reclaimed as liquid product simultaneously, does not have the gas of condensation to discharge; The 4th step: after vacuum-drying is finished, in the moisture eliminator chuck, pass into cold water, reclaim as solid phase prod after dried material is down to normal temperature.
The below is the further optimization and/or improvements to one of foregoing invention technical scheme:
Above-mentioned speed range when carrying out centrifugation can be 50 r/min to 1500r/min.
Above-mentioned when taking out negative-pressure operation, the pressure of moisture eliminator inside can be evacuated to-0.05MPa is to-0.1MPa.
In the above-mentioned second step, passing into temperature in the chuck of moisture eliminator, to can be 120 ℃ to 200 ℃, pressure be the low-pressure steam of 0.3MPa to 1.2MPa.
Two of technical scheme of the present invention realizes by following measures: a kind of purification and recover method isolated plant of ETE by product comprises whizzer, moisture eliminator, condenser and vacuum pump; The import of whizzer is installed with the feeding line that reaction product can be sent into whizzer, the liquid exit of whizzer is installed with the filtrate line of pipes, be installed with material between the inner casing import of the solid outlet of whizzer and moisture eliminator and send into pipeline, the inner casing outlet of moisture eliminator is installed with the discharge of materials pipeline, the chuck import of moisture eliminator is installed with steam and enters pipeline, the Jacket outlet of moisture eliminator is installed with the steam condensate outfall pipeline, be installed with gas between the inner casing pneumatic outlet of moisture eliminator and the condenser gas feed and enter pipeline, the pneumatic outlet of condenser is installed with the non-condensable gas outfall pipeline, be installed with vacuum pump on the non-condensable gas outfall pipeline, be installed with fluid-carrying lines between the liquid exit of condenser and the filtrate line of pipes.
The below is two further optimization and/or improvements to the foregoing invention technical scheme:
Above-mentioned material is sent on the pipeline can be installed with feed bin.
Can be installed with withdrawing can on the aforesaid liquid line of pipes.
Above-mentioned entering on pipeline, steam condensate outfall pipeline, the gas fluid-carrying lines before entering pipeline, non-condensable gas outfall pipeline and feed bin and on the fluid-carrying lines after the feed bin at discharge of materials pipeline, steam can be installed with respectively valve.
The present invention is dry by material is concentrated, drying machine and vacuum pump start-stop once can all be finished dealing with, effectively reduce dry work required time, operator's working load, equipment on-off frequency, improved service life of equipment, pass into the mode that water coolant is forced cooling by the moisture eliminator chuck simultaneously, shorten cooling time, improved working efficiency.
Description of drawings
Accompanying drawing 1 is the structural representation of the embodiment of the invention 2.
Coding in the accompanying drawing is respectively: 1 is whizzer, and 2 is moisture eliminator, and 3 is condenser, 4 is vacuum pump, and 5 is feeding line, and 6 is the filtrate line of pipes, 7 send into pipeline for material, and 8 is the discharge of materials pipeline, and 9 enter pipeline for steam, 10 is the steam condensate outfall pipeline, and 11 for gas enters pipeline, and 12 is the non-condensable gas outfall pipeline, 13 is fluid-carrying lines, 14 is feed bin, and 15 is withdrawing can, and 16 is valve.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme of the present invention and practical situation.Per-cent among the present invention is mass percent.
The invention will be further described below in conjunction with embodiment and accompanying drawing 1:
Embodiment 1: the purification and recover method of this ETE by product is carried out in the steps below: the first step: the reaction product that will adopt the phase-transfer-catalyzed reactions technology to synthesize ETE is sent into whizzer 1 and is carried out centrifugation, separates filtrate and filter residue after the centrifugation; Second step: at first moisture eliminator 2 is continued to take out negative pressure, then the filter residue after the centrifugation is sent in the moisture eliminator 2, then after passing into low-pressure steam in the chuck of moisture eliminator 2 filter residue is carried out drying, the temperature of filter residue is 110 ℃ to 160 ℃ when dry, and be 3 hours to 5 hours time of drying; The 3rd step: enter after the gas that produces in the drying process is extracted out under the effect of taking out negative pressure and carry out condensation in the condenser 3, the filtrate in condensed liquid and the first step is reclaimed as liquid product simultaneously, does not have the gas of condensation to discharge; The 4th step: after vacuum-drying is finished, in moisture eliminator 2 chucks, pass into cold water, reclaim as solid phase prod after dried material is down to normal temperature.When dry, by low-pressure steam material is heated and to pass into cold water after finishing with drying material is lowered the temperature, can be rapidly with dry materials and cooling, greatly shortened the cell operation time, therefore, the multiple batches of material that need to reclaim put together carry out drying, can effectively save the working hour, the start and stop frequency of reduction equipment, minimizing operator's workload is increased work efficiency.Adopt the phase-transfer-catalyzed reactions technology to synthesize in the reaction product of ETE and contain many byproducts of reaction, contain in the filter residue after the reaction product centrifugation that Potassium Bromide is about 60%, potassium hydroxide is about 25%, water 8%, recyclable ETE product are about 4%, other impurity about 3%, contained a small amount of ETE product need reclaim in the filter residue, Potassium Bromide, potassium hydroxide also have recovery value, can be as the byproduct export trade after super-dry.
Embodiment 2: preferred as above-described embodiment, the speed range when carrying out centrifugation is 50 r/min to 1500r/min.
Embodiment 3: preferred as above-described embodiment, when taking out negative-pressure operation, the pressure of moisture eliminator 2 inside is evacuated to-0.05MPa is to-0.1MPa.
Embodiment 4: preferred as above-described embodiment, in the second step, passing into temperature in the chuck of moisture eliminator 2 and be 120 ℃ to 200 ℃, pressure is the low-pressure steam of 0.3MPa to 1.2MPa.
Embodiment 5: as shown in Figure 1, a kind of purification and recover method isolated plant of ETE by product comprises whizzer 1, moisture eliminator 2, condenser 3 and vacuum pump 4; The import of whizzer 1 is installed with the feeding line 5 that reaction product can be sent into whizzer 1, the liquid exit of whizzer 1 is installed with filtrate line of pipes 6, be installed with material between the inner casing import of the solid outlet of whizzer 1 and moisture eliminator 2 and send into pipeline 7, the inner casing outlet of moisture eliminator 2 is installed with discharge of materials pipeline 8, the chuck import of moisture eliminator 2 is installed with steam and enters pipeline 9, the Jacket outlet of moisture eliminator is installed with steam condensate outfall pipeline 10, be installed with gas between the inner casing pneumatic outlet of moisture eliminator 2 and condenser 3 gas feeds and enter pipeline 11, the pneumatic outlet of condenser 2 is installed with non-condensable gas outfall pipeline 12, be installed with vacuum pump 4 on the non-condensable gas outfall pipeline 12, be installed with fluid-carrying lines 13 between the liquid exit of condenser 3 and the filtrate line of pipes 6.Vacuum pump 4 enters 11 pairs of moisture eliminator 0 inside of pipeline by non-condensable gas outfall pipeline 12, condenser 3 and gas successively and vacuumizes.
Embodiment 6: as shown in Figure 1, be that with the difference of embodiment 6 material is sent into and is installed with feed bin 14 on the pipeline 7.Because the technique of synthetic ETE is rhythmic reaction, single batch of output is less, and for reducing energy consumption, increasing work efficiency, filter residue is introduced into feed bin 14 and collects, and filter residue reaches to concentrate after a certain amount of again and carries out drying by the time.
Embodiment 7: as shown in Figure 1, be with the difference of embodiment 6 and embodiment 7, be installed with withdrawing can 15 on the fluid-carrying lines 13, in time discharge for the liquid that makes things convenient for condensation to get off on the one hand, can avoid on the other hand preventing the liquid suck-back in the vacuum, affect working efficiency.
Embodiment 8: as shown in Figure 1, enter on pipeline 9, steam condensate outfall pipeline 10, the gas fluid-carrying lines 13 before entering pipeline 11, non-condensable gas outfall pipeline 12 and feed bin and on the fluid-carrying lines 13 after the feed bin at discharge of materials pipeline 8, steam and to be installed with respectively valve 16.
Claims (10)
1. the purification and recover method of an ETE by product is characterized in that carrying out in the steps below: the first step: will adopt the reaction product of the synthetic ETE of phase-transfer-catalyzed reactions technology to send into whizzer and carry out centrifugation, and separate filtrate and filter residue after the centrifugation; Second step: at first moisture eliminator is continued to take out negative pressure, then the filter residue after the centrifugation is sent in the moisture eliminator, then after passing into low-pressure steam in the chuck of moisture eliminator filter residue is carried out drying, the temperature of filter residue is 110 ℃ to 160 ℃ when dry, and be 3 hours to 5 hours time of drying; The 3rd step: enter after the gas that produces in the drying process is extracted out under the effect of taking out negative pressure and carry out condensation in the condenser, the filtrate in condensed liquid and the first step is reclaimed as liquid product simultaneously, does not have the gas of condensation to discharge; The 4th step: after vacuum-drying is finished, in the moisture eliminator chuck, pass into cold water, reclaim as solid phase prod after dried material is down to normal temperature.
2. the purification and recover method of ETE by product according to claim 1, the speed range when it is characterized in that carrying out centrifugation is 50 r/min to 1500r/min.
3. the purification and recover method of ETE by product according to claim 1 and 2, when it is characterized in that taking out negative-pressure operation, the pressure of moisture eliminator inside is evacuated to-0.05MPa is to-0.1MPa.
4. the purification and recover method of ETE by product according to claim 1 and 2 is characterized in that in the second step, and passing into temperature in the chuck of moisture eliminator and be 120 ℃ to 200 ℃, pressure is the low-pressure steam of 0.3MPa to 1.2MPa.
5. the purification and recover method of ETE by product according to claim 3 is characterized in that in the second step, and passing into temperature in the chuck of moisture eliminator and be 120 ℃ to 200 ℃, pressure is the low-pressure steam of 0.3MPa to 1.2MPa.
6. the isolated plant of the purification and recover method of an ETE by product is characterized in that comprising whizzer, moisture eliminator, condenser and vacuum pump; The import of whizzer is installed with the feeding line that reaction product can be sent into whizzer, the liquid exit of whizzer is installed with the filtrate line of pipes, be installed with material between the inner casing import of the solid outlet of whizzer and moisture eliminator and send into pipeline, the inner casing outlet of moisture eliminator is installed with the discharge of materials pipeline, the chuck import of moisture eliminator is installed with steam and enters pipeline, the Jacket outlet of moisture eliminator is installed with the steam condensate outfall pipeline, be installed with gas between the inner casing pneumatic outlet of moisture eliminator and the condenser gas feed and enter pipeline, the pneumatic outlet of condenser is installed with the non-condensable gas outfall pipeline, be installed with vacuum pump on the non-condensable gas outfall pipeline, be installed with fluid-carrying lines between the liquid exit of condenser and the filtrate line of pipes.
7. the isolated plant of the purification and recover method of ETE by product according to claim 6 is characterized in that material is sent into to be installed with feed bin on the pipeline.
8. according to claim 6 or the isolated plant of the purification and recover method of 7 described ETE by products, it is characterized in that being installed with on the fluid-carrying lines withdrawing can.
9. according to claim 6 or the isolated plant of the purification and recover method of 7 described ETE by products, it is characterized in that entering on pipeline, steam condensate outfall pipeline, the gas fluid-carrying lines before entering pipeline, non-condensable gas outfall pipeline and feed bin and on the fluid-carrying lines after the feed bin at discharge of materials pipeline, steam and be installed with respectively valve.
10. the isolated plant of the purification and recover method of ETE by product according to claim 8 is characterized in that entering on pipeline, steam condensate outfall pipeline, the gas fluid-carrying lines before entering pipeline, non-condensable gas outfall pipeline and feed bin and on the fluid-carrying lines after the feed bin at discharge of materials pipeline, steam and is installed with respectively valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104468295A CN102964318A (en) | 2012-11-11 | 2012-11-11 | Recycling and refining method of ETE byproducts |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012104468295A CN102964318A (en) | 2012-11-11 | 2012-11-11 | Recycling and refining method of ETE byproducts |
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| CN102964318A true CN102964318A (en) | 2013-03-13 |
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| CN2012104468295A Pending CN102964318A (en) | 2012-11-11 | 2012-11-11 | Recycling and refining method of ETE byproducts |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2000771A (en) * | 1977-07-14 | 1979-01-17 | Allied Chem | Alkyl tetrahydrofurfuryl ethers |
| US5300599A (en) * | 1992-04-06 | 1994-04-05 | The Goodyear Tire & Rubber Company | Modifier for anionic polymerization of diene monomers |
| CN202376793U (en) * | 2011-12-05 | 2012-08-15 | 上海洁美环保科技有限公司 | Ammonium sulphate evaporating and crystallizing device |
-
2012
- 2012-11-11 CN CN2012104468295A patent/CN102964318A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2000771A (en) * | 1977-07-14 | 1979-01-17 | Allied Chem | Alkyl tetrahydrofurfuryl ethers |
| US5300599A (en) * | 1992-04-06 | 1994-04-05 | The Goodyear Tire & Rubber Company | Modifier for anionic polymerization of diene monomers |
| CN202376793U (en) * | 2011-12-05 | 2012-08-15 | 上海洁美环保科技有限公司 | Ammonium sulphate evaporating and crystallizing device |
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Application publication date: 20130313 |