CN105854329B - Prepare " rectifying+cryospray " drying means of PE low molecular polymer powder - Google Patents
Prepare " rectifying+cryospray " drying means of PE low molecular polymer powder Download PDFInfo
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- CN105854329B CN105854329B CN201610273581.5A CN201610273581A CN105854329B CN 105854329 B CN105854329 B CN 105854329B CN 201610273581 A CN201610273581 A CN 201610273581A CN 105854329 B CN105854329 B CN 105854329B
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- nitrogen
- cryospray
- tissuemat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention relates to a kind of " rectifying+cryospray " drying means for preparing PE low molecular polymer powder, this method comprises the following steps：(1) Tissuemat E solution and saturated vapor indirect heat exchange, solvent toluene separate with Tissuemat E；(2) after solvent toluene is cooled to liquid with cooling medium indirect heat exchange, rectifying column circulation is partly into；Remaining part is discharged；(3) Tissuemat E fused solution is divided into two parts, and a portion returns to rectifying column after saturated vapor heats, and obtains steam condensate and discharges；Another part, which is delivered in cryospray tower, forms vaporific Tissuemat E drop, and is exchanged heat with cold nitrogen, respectively obtains powder and the nitrogen containing superfine powder；Nitrogen containing superfine powder is purified, respectively obtains the nitrogen after superfine powder and purification；Nitrogen after purification returns to cryospray tower after being largely pressurized cooling, and remaining part enters exhaust treatment system.Operating process of the present invention is simple, the thermal efficiency is high.
Description
Technical field
The present invention relates to inflammable, explosive material cryospray technical field of drying, more particularly to prepare polyethylene oligomeric
" rectifying+cryospray " drying means of thing powder.
Background technology
At present, the conventional drying technique of polyethylene wax micro mist is under stress by it by the solution of Tissuemat E by nozzle
Misty liquid droplets are sprayed in drying tower, are then declined with hot nitrogen cocurrent, most of powder particles are collected by bottom of towe discharge gate, are steamed
The waste gas sent with its contained by micro powder discharged after cyclone separator separates by air exhauster, powder is again from cyclone separator
Lower end is collected.Such a method drying time is short, but when air themperature is less than 150 DEG C, because volumetric heat transfer coefficient is relatively low,
Need to use larger volume of equipment；Additionally, due to the package action of particle, the quantity of solvent carried in product is more；Gas-solid is mixed
The separation requirement of compound is higher, generally requires two-stage dedusting, and operating process is complicated, and the thermal efficiency is not high.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of operating process is simple, the thermal efficiency is high and prepare polyethylene low
" rectifying+cryospray " drying means of copolymer powder.
To solve the above problems, " rectifying+cryospray " of the present invention for preparing PE low molecular polymer powder is dried
Method, comprise the following steps：
(1) Tissuemat E solution is delivered in the middle part of rectifying column by slurry pump；Meanwhile temperature is 158 DEG C of saturated vapor
Pass through the rectifying column tower bottom reboiler and Tissuemat E solution indirect heat exchange；In thermal driving force and the effect of contraction to balance each other
Under, solvent toluene is separated with Tissuemat E, and the Tissuemat E fused solution of purity >=99.9% is gathered to the rectifier bottoms, molten
Agent toluene produces at the top of the rectifying column；
(2) the solvent toluene enters overhead condenser, meanwhile, cooling medium inputs to be carried out into the overhead condenser
Indirect heat exchange, solvent toluene is set to be discharged into after being cooled to liquid in solvent recovery tank, a part of solvent toluene is defeated through tower top circulating pump
Deliver to and enter circulation at the top of rectifying column；Remaining part solvent toluene is discharged through the tower top circulating pump and recycled；
(3) the Tissuemat E fused solution is divided into two parts, wherein：
A part of bottom through the rectifying column enters the reboiler, and essence is returned after 158 DEG C of saturated vapor heating
Tower is evaporated, while obtains 158 DEG C of steam condensate, and is discharged by drip pipe；
Another part is then delivered in cryospray tower by Melting pump, by described in high pressure fan nozzle under stress general
Tissuemat E fused solution sprays to form vaporific Tissuemat E drop；Meanwhile the circulating nitrogen gas that temperature is 30 DEG C are defeated by circulating fan
Enter to nitrogen cooler, after cooling medium indirect heat exchange in the nitrogen cooler, respectively obtain temperature be 5 DEG C cold nitrogen and
Toluene is condensed, the condensation toluene is discharged by the bottom of the nitrogen cooler；The cold nitrogen that the temperature is 5 DEG C enters described cold
Freeze in spray tower and exchanged heat with the vaporific Tissuemat E drop, respectively obtain powder and the nitrogen containing superfine powder；The powder
Drawn off by the rotated discharge valve I of the cryospray tower bottom；The nitrogen containing superfine powder is by the cryospray tower
Gas vent is discharged, and is purified into pulsed jet cloth filter, respectively obtains the nitrogen after superfine powder and purification；It is described
Superfine powder is drawn off by the rotated discharge valve II in the pulsed jet cloth filter bottom；Nitrogen after the purification largely enters
The circulating fan supercharging, remaining part enter exhaust treatment system；Nitrogen after supercharging enter the nitrogen cooler with it is cold
But medium indirect heat exchange, the nitrogen after cooling return to the cryospray tower and realize nitrogen circulation.
The cooling medium is 30 DEG C of recirculated cooling waters or -15 DEG C of chilled brines.
The gas-liquid heat exchange mode of the cryospray tower is cocurrent or countercurrent.
The pulsed jet cloth filter is replaced using cyclone separator, or is used in combination with cyclone separator.
The present invention has advantages below compared with prior art：
1st, the present invention combines the physical characteristic of Tissuemat E, first carries out rectifying purifying to Tissuemat E solution, obtains high-purity
The Tissuemat E fused solution of degree, recycle the principle of cryospray to be granulated Tissuemat E again, finally give the poly- of high-purity
Ethylene waxes micro mist, reach dry purpose.
2nd, because the drying means of conventional soln evaporative crystallization is related to the use of a large amount of organic solvents, easily cause product molten
The residual of agent, is difficult to obtain high purity product.The present invention using " rectifying+cryospray " and combined drying method, after purified
Tissuemat E fused solution carry out cryospray granulation, obtained polyethylene wax micro mist no solvent residue.
3rd, mist projection granulating process of the present invention avoids conventional polyethylene wax micro mist sky by the way of " closed circuit nitrogen circulation "
Inflammable, explosive accident potential existing for gas open circuit air-flow drying method.
4th, conventional soln evaporative crystallization is related to the removal process of solvent, and oil-containing polyethylene wax micro mist also needs further in solvent
Processing, complex steps and the consumption energy.The high-purity solvent that the present invention obtains in distillation process need not be handled, can be direct
Reuse, it is not only simple to operate, and also the thermal efficiency is high.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the process chart of the present invention.
In figure：1-slurry pump, 2-rectifying column, 3-reboiler, 4-Melting pump, 5-cryospray, 6-arteries and veins of tower
Rush 10-solvent recovery tank of sack cleaner 7-circulating fan, 8-nitrogen cooler, 9-overhead condenser 11-
Tower top circulating pump.
Embodiment
As shown in figure 1, preparing " rectifying+cryospray " drying means of PE low molecular polymer powder, comprise the following steps：
(1) Tissuemat E solution is delivered to the middle part of rectifying column 2 by slurry pump 1；Meanwhile the saturation that temperature is 158 DEG C is steamed
Vapour passes through the tower bottom reboiler 3 of rectifying column 2 and Tissuemat E solution indirect heat exchange；In thermal driving force and the effect of contraction to balance each other
Under, solvent toluene is separated with Tissuemat E, and the Tissuemat E fused solution of purity >=99.9% is gathered to the bottom of rectifying column 2, solvent first
Benzene produces from the top of rectifying column 2.
(2) solvent toluene enters overhead condenser 9, meanwhile, cooling medium inputs to be changed indirectly into overhead condenser 9
Heat, solvent toluene is set to be discharged into after being cooled to liquid in solvent recovery tank 10, a part of solvent toluene conveys through tower top circulating pump 11
Enter circulation at the top of to rectifying column；Remaining part solvent toluene is discharged through tower top circulating pump 11 and recycled.
(3) Tissuemat E fused solution is divided into two parts, wherein：
A part of bottom through rectifying column 2 enters reboiler 3, and rectifying column 2 is returned after 158 DEG C of saturated vapor heating,
158 DEG C of steam condensate is obtained simultaneously, and is discharged by drip pipe.
Another part is then delivered in cryospray tower 5 by Melting pump 4, under stress will be poly- by high pressure fan nozzle
Ethylene waxes fused solution sprays to form vaporific Tissuemat E drop；Meanwhile the circulating nitrogen gas that temperature is 30 DEG C are inputted by circulating fan 7
Into nitrogen cooler 8, with the nitrogen cooler 8 after cooling medium indirect heat exchange, respectively obtain temperature be 5 DEG C cold nitrogen and
Toluene is condensed, the condensation toluene is discharged by the bottom of nitrogen cooler 8；Temperature is that 5 DEG C of cold nitrogen enters cryospray tower 5
In, exchanged heat with vaporific Tissuemat E drop, Tissuemat E drop is solidified rapidly, be under spherical freedom by the cohesive force of itself
Fall, respectively obtain powder and the nitrogen containing superfine powder；Powder is drawn off by the rotated discharge valve I in the bottom of cryospray tower 5；Containing super
The nitrogen of fine powder material is discharged by the gas vent of cryospray tower 5, and is purified into pulsed jet cloth filter 6, respectively
Nitrogen to after superfine powder and purification；Superfine powder is drawn off by the rotated discharge valve II in the bottom of pulsed jet cloth filter 6；Purification
Nitrogen afterwards is largely pressurized into circulating fan 7, and remaining part enters exhaust treatment system；Nitrogen after supercharging enters nitrogen
Cooler 8 and cooling medium indirect heat exchange, the nitrogen after cooling return to cryospray tower 5 and realize nitrogen circulation.
Wherein：
Cooling medium is 30 DEG C of recirculated cooling waters or -15 DEG C of chilled brines.
The gas-liquid heat exchange mode of cryospray tower 5 is cocurrent or countercurrent.
Pulsed jet cloth filter 6 is replaced using cyclone separator, or is used in combination with cyclone separator.
Claims (4)
1. preparing " rectifying+cryospray " drying means of PE low molecular polymer powder, comprise the following steps：
(1) Tissuemat E solution is passed through into slurry pump（1）It is delivered to rectifying column（2）Middle part；Meanwhile the saturation that temperature is 158 DEG C is steamed
Vapour passes through the rectifying column（2）Tower bottom reboiler（3）With Tissuemat E solution indirect heat exchange；In thermal driving force and the pact to balance each other
Under Shu Zuoyong, solvent toluene is separated with Tissuemat E, and the Tissuemat E fused solution of purity >=99.9% is gathered to the rectifying column
（2）Bottom, solvent toluene is from the rectifying column（2）Top produces；
(2) the solvent toluene enters overhead condenser（9）, meanwhile, cooling medium is inputted to the overhead condenser（9）In enter
Row indirect heat exchange, solvent toluene is set to be discharged into solvent recovery tank after being cooled to liquid（10）In, a part of solvent toluene follows through tower top
Ring pump（11）It is delivered at the top of rectifying column and enters circulation；Remaining part solvent toluene is through the tower top circulating pump（11）Discharge recovery
Utilize；
(3) the Tissuemat E fused solution is divided into two parts, wherein：
A part is through the rectifying column（2）Bottom enter the reboiler（3）, returned after 158 DEG C of saturated vapor heating
Rectifying column（2）, while 158 DEG C of steam condensate is obtained, and discharged by drip pipe；
Another part then passes through Melting pump（4）It is delivered to cryospray tower（5）In, by high pressure fan nozzle under stress by institute
Tissuemat E fused solution is stated to spray to form vaporific Tissuemat E drop；Meanwhile temperature is 30 DEG C of circulating nitrogen gas by circulating fan
（7）Input to nitrogen cooler（8）, with the nitrogen cooler（8）After middle cooling medium indirect heat exchange, temperature is respectively obtained as 5
DEG C cold nitrogen and condensation toluene, the condensation toluene is by the nitrogen cooler（8）Bottom discharge；The temperature is 5 DEG C
Cold nitrogen enters the cryospray tower（5）In exchanged heat with the vaporific Tissuemat E drop, respectively obtain powder and containing ultra-fine
The nitrogen of powder；The powder is by the cryospray tower（5）The rotated discharge valve I in bottom is drawn off；It is described containing superfine powder
Nitrogen is by the cryospray tower（5）Gas vent discharge, and enter pulsed jet cloth filter（6）Purified, respectively
Nitrogen to after superfine powder and purification；The superfine powder is by the pulsed jet cloth filter（6）The rotated discharge valve in bottom
II draws off；Nitrogen after the purification largely enters the circulating fan（7）Supercharging, remaining part enter vent gas treatment system
System；Nitrogen after supercharging enters the nitrogen cooler（8）With cooling medium indirect heat exchange, the nitrogen after cooling returns described cold
Freeze spray tower（5）Realize nitrogen circulation.
2. preparing " rectifying+cryospray " drying means of PE low molecular polymer powder as claimed in claim 1, its feature exists
In：The cooling medium is 30 DEG C of recirculated cooling waters or -15 DEG C of chilled brines.
3. preparing " rectifying+cryospray " drying means of PE low molecular polymer powder as claimed in claim 1, its feature exists
In：The cryospray tower（5）Gas-liquid heat exchange mode be cocurrent or countercurrent.
4. preparing " rectifying+cryospray " drying means of PE low molecular polymer powder as claimed in claim 1, its feature exists
In：The pulsed jet cloth filter（6）Replaced using cyclone separator, or be used in combination with cyclone separator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610273581.5A CN105854329B (en) | 2016-04-28 | 2016-04-28 | Prepare " rectifying+cryospray " drying means of PE low molecular polymer powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610273581.5A CN105854329B (en) | 2016-04-28 | 2016-04-28 | Prepare " rectifying+cryospray " drying means of PE low molecular polymer powder |
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| CN105854329A CN105854329A (en) | 2016-08-17 |
| CN105854329B true CN105854329B (en) | 2017-12-01 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1883435A (en) * | 2006-07-10 | 2006-12-27 | 茂名学院 | One-step Chinese medicine spray-drying and granulating process and equipment |
| CN101037382A (en) * | 2007-04-24 | 2007-09-19 | 徐如思 | Preparation method of high-content paraformaldehyde |
| CN101874934A (en) * | 2010-07-05 | 2010-11-03 | 天津大学 | Flash evaporation feed type internal heat integration energy-saving rectifying device and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL2669001T3 (en) * | 2012-06-01 | 2015-06-30 | Procter & Gamble | Spray-drying process |
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- 2016-04-28 CN CN201610273581.5A patent/CN105854329B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1883435A (en) * | 2006-07-10 | 2006-12-27 | 茂名学院 | One-step Chinese medicine spray-drying and granulating process and equipment |
| CN101037382A (en) * | 2007-04-24 | 2007-09-19 | 徐如思 | Preparation method of high-content paraformaldehyde |
| CN101874934A (en) * | 2010-07-05 | 2010-11-03 | 天津大学 | Flash evaporation feed type internal heat integration energy-saving rectifying device and method |
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| CN105854329A (en) | 2016-08-17 |
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