A kind of evaporating and concentrating process of the cellulose solvent NMMO aqueous solution and device
Technical field
The invention belongs to evaporation technology and the device field of the recycling design in solvent method experimental branch line, specifically a kind of evaporating and concentrating process of the cellulose solvent NMMO aqueous solution and device.
Background technology
Solvent method produces chemical fibre, and be a kind of manufacturing technique method of Fresh fats, solvent for use is the aqueous solution of N-methylmorpholine-N-oxide (NMMO).The concentration of this solution after separated and dissolved fiber is 15 ~ 20%, and after concentrated, the concentration requirement of reuse is 85% or 65%.The feature of the NMMO aqueous solution is that " boiling point liter " is high, and high temperature, high dense under, can decompose, domestic still not have first and then applicable vaporising device.Have the patent No. to be 200610027723.6, name is called " method of evaporating of NMMO ", provides the method that 2 single-effect vacuum evaporator combinations are produced, remains very backward production method.Certain research institute domestic proposed the method for triple effect evaporation NMMO solution, but its energy consumption and advance can not meet the industrial needs of modernization completely.It is said, have the device of 6 effect evaporation NMMO abroad, steam-water ratio can reach 0.23, but its technology is top-secret.Therefore, be necessary to invent a kind of energy-conservation, efficient evaporating and concentrating process and device that can meet the cellulose solvent NMMO aqueous solution of modernization industry need of production.
Summary of the invention
According to the high concentration NMMO aqueous solution, there is higher boiling, labile feature, and a kind of evaporating and concentrating process and device of the cellulose solvent NMMO aqueous solution are provided.Obtain cicada NMMO elevation of boiling point rule at different concentrations and temperatures by experiment: under vacuum during concentration 91%, the elevation of boiling point is 54 degree, during concentration 82.73%, and the elevation of boiling point is 45 degree, and when concentration 65.94%, the elevation of boiling point is 34 degree.During concentration 54.82%, the elevation of boiling point is 22 degree.Under normal pressure, when concentration is 25.27%, the elevation of boiling point is 5 degree, and when concentration is 22.39%, the elevation of boiling point is only 3 degree;
The present invention utilizes the elevation of boiling point rule of NMMO solution under different temperatures, variable concentrations, design the process of " series connection preheating, an effect charging, following current evaporation, dense effect connect ", whole material is made all to enter an effect after preheating, enter two effects successively until the evaporation of n effect, concentration raises gradually, makes feed liquid in front triple effect evaporation, is all in the state that low boiling rises, due to the elevation of boiling point, the heat transfer temperature loss caused is down to minimum.Thus the evaporation of NMMO aqueous solution effect number can be made to bring up to 4 effects, five effects, six effects.6th effect low-temperature cooling water (lower than 20 DEG C) condensation indirect steam of sextuple-effect evaporation.For the NMMO aqueous solution of higher concentration, boiling point is upgraded to 48 DEG C, design is evaporated in dense effect, dense effect of the present invention, and non-usage Boiler Steam, but imitate (when n is four ~ six) evaporimeter from n-2 effect (when n is three ~ six) above or n-3 and draw a part of indirect steam as thermal source also.
The technological means that the present invention adopts is as follows:
An evaporation concentration device for the cellulose solvent NMMO aqueous solution, comprise connect in turn 1st effective evaporator, 2nd effect evaporator until n single-effect evaporator and only for 1st effective evaporator charging and the one-level preheater of preheating of connecting, secondary preheater until n level preheater; Also comprise respectively with 1st effective evaporator, 2nd effect evaporator until n single-effect evaporator be connected one imitate circulating pump, two and imitate circulating pump until n imitates circulating pump, wherein, n is one in three, four, five, six,
Under duty, the NMMO aqueous solution of pending low temperature, successively through n level preheater, n-1 level preheater until one-level preheater series connection pre-heating temperature elevation after, enter 1st effective evaporator evaporation, enter 2nd effect evaporator successively afterwards until the evaporation of n single-effect evaporator, discharge the NMMO aqueous solution after concentrating from n single-effect evaporator; The indirect steam that upper 1st effective evaporator produces enters the heater of lower 1st effective evaporator, and the indirect steam that n single-effect evaporator produces enters condensing unit; The heating steam condensed water of 1st effective evaporator enters one-level preheater, the condensed water that one-level preheater is discharged enters secondary preheater together with 2nd effect evaporator heating steam condensed water, until the condensed water that n-1 level preheater is discharged enters n level preheater together with the condensed water of n single-effect evaporator heating steam; The cryogenic condensation water that n level preheater is discharged is discharged and is used as him.
The evaporation concentration device of described a kind of cellulose solvent NMMO aqueous solution also comprises the concentrated evaporator obtaining the high concentration NMMO aqueous solution for evaporation and concentration be connected with n single-effect evaporator, and concentrated evaporator is provided with dense effect circulating pump,
Under duty, when n is four ~ six, discharge the NMMO aqueous solution after concentrating from n single-effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, the indirect steam of drawing a part of n-2 effect or n-3 single-effect evaporator enters concentrated evaporator, and concentrated evaporator heating steam condensed water enters n-1 level preheater; When n is three, discharge the NMMO aqueous solution after concentrating from triple effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, the indirect steam of drawing a part of 1st effective evaporator enters concentrated evaporator, and concentrated evaporator heating steam condensed water enters secondary preheater.
Each single-effect evaporator be provided with in the steam chamber of concentrated evaporator for stop the liquid barrier of high material casting liquid with for carrying out the silk screen be efficiently separated to the mist in indirect steam; Each effect circulating pump and dense effect circulating pump are Electromagnetic Drive without sealing circulating pump or No leakage circulating pump, to reduce the loss of the NMMO aqueous solution to greatest extent.
The structural design of each single-effect evaporator and concentrated evaporator is and flows falling film evaporator or reverse-flow falling film evaporator, thus improves heat transfer efficiency, reduces the liquid holdup of evaporimeter, shortens the time of staying of solvent in evaporimeter, alleviates pyrolytic.
Preheater at different levels is the plate type heat exchanger of full welded type.
The invention also discloses a kind of evaporating and concentrating process applying a kind of cellulose solvent NMMO aqueous solution of evaporation concentration device of the cellulose solvent NMMO aqueous solution, there is following processing step:
S1, series connection preheating: the NMMO aqueous solution of pending low temperature successively through n level preheater, n-1 level preheater until reach the high temperature close to boiling point after one-level preheater series connection pre-heating temperature elevation, wherein, n is one in three, four, five, six;
S2, an effect charging: by the NMMO aqueous solution that reaches after preheating close to the high temperature of boiling point from 1st effective evaporator charging;
S3, following current are evaporated: after 1st effective evaporator evaporation, feed liquid enters 2nd effect evaporator evaporation from an effect discharge, until enter n single-effect evaporator to discharge feed liquid, obtain the NMMO aqueous solution after concentrating,
The discharge overfall of each effect is all arranged on liquid level place, exceeds the feed liquid of liquid level and overflow, is connected with the charging aperture of aftereffect by U-shaped pipe, balances the pressure reduction between each single-effect evaporator with U-shaped pipe, and makes the level being constant of each effect;
S4, dense effect connection heat: when n is four ~ six, discharge the NMMO aqueous solution after concentrating from n single-effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, concentrated evaporator draws a part of indirect steam as thermal source from n-2 effect above or n-3 single-effect evaporator, realize the combined heat of imitating vaporising device with front n, concentrated evaporator heating steam condensed water enters n-1 level preheater; When n is three, discharge the NMMO aqueous solution after concentrating from triple effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, concentrated evaporator draws a part of indirect steam as thermal source from 1st effective evaporator above, realize the combined heat with front triple-effect evaporation plant, concentrated evaporator heating steam condensed water enters n-1 level preheater.
The absolute pressure pressure of n single-effect evaporator and concentrated evaporator is 0.0024 ~ 0.006MPa.
The indirect steam that upper 1st effective evaporator produces enters the heater of lower 1st effective evaporator, and the indirect steam that n single-effect evaporator produces enters cooling device; The heating steam condensed water of 1st effective evaporator enters one-level preheater, the condensed water that one-level preheater is discharged enters secondary preheater together with 2nd effect evaporator heating steam condensed water, until the condensed water that n-1 level preheater is discharged enters n level preheater together with the condensed water of n single-effect evaporator heating steam; The cryogenic condensation water that n level preheater is discharged is discharged and is used as him.
When n is three ~ five, described concentrated after the concentration of the NMMO aqueous solution be 65%, the concentration of the high concentration NMMO aqueous solution that described concentrated evaporator is discharged is 85%.
When n is six, the indirect steam of last evaporator passes through the sub-cooled water condensation lower than 20 DEG C; When n is one in three, four, five, the indirect steam of last evaporator passes through the circulating water condensing of air cooling tower.
The point of key of the present invention is " series connection preheating ".Series connection preheating be the waste heat of all each effect condensed waters all for the preheating of an effect charging, an effect is reached a high temperature charging, realizes the low temperature of condensed water can be converted into high temperature energy into an effect feed liquid.Reduce the intensification heat in an effect, increase heat of evaporation, to greatest extent raising one effect indirect steam amount, thus each evaporation capacity of imitating after improving, save the quantity of raw steam, reduce steam-water ratio.
The thermal source of series connection preheating is the heating steam condensed water of each effect, also with condensed water, can enter some indirect steams, to improve the temperature of an effect charging further if desired.
The heating steam condensed water of 1st effective evaporator enters one-level preheater, the condensed water that one-level preheater is discharged enters secondary preheater together with 2nd effect evaporator heating steam condensed water, until the condensed water that n-1 level preheater is discharged enters n level preheater together with the condensed water of n single-effect evaporator heating steam; The cryogenic condensation water that n level preheater is discharged is discharged and is used as him.
So the point of key of the present invention is also in design " following current evaporation ".Following current refers to that the flow direction of material is consistent with the flow direction of indirect steam: one imitates discharge enters two effects and evaporate, until enter n single-effect evaporator to discharge feed liquid." series connection preheating " makes an effect obtain the preheating of maximum temperature, " following current evaporation " makes each effect from two effects be all boiling-point feeding, the intensification heat of each effect that two effects start is all " zero ", and the heat of the indirect steam of effect input in the past, all for transpiring moisture.
So the point of key of the present invention exists, avoid material to occur high temperature, high dense situation in evaporation process simultaneously.NMMO material is dense at height, can decompose under high temperature.Technological process of the present invention is low concentration under high temperature, is high concentration under low temperature, and this is just avoided material generation decomposition reaction.
So the point of key of the present invention exists, use parallel type falling film evaporator, or reverse-flow falling film evaporator is as the main equipment of each effect vaporising device and concentrated evaporator.Because and flow falling film evaporation or countercurrent falling-film evaporation, there is very high heat transfer coefficient, there is minimum liquid holdup simultaneously.Minimum liquid of holding can reduce the time of staying of material in evaporimeter, reduces chemical breakdown, reduces production circulating fund, because the price of NMMO solution is very high, evaporimeter reduces holds liquid, just can reduce the amount of circulating funds used.
So the point of the present invention's key exists, increase concentrated evaporator, dense effect is evaporated to vacuum evaporation, evaporates under must remaining on 0.0024 ~ 0.006MPa absolute pressure.Concentrated evaporator draws a part of indirect steam as thermal source from n-2 effect (when n is three ~ six) above or n-3 effect (when n is four ~ six) evaporimeter.Evaporation and concentration can discharge the NMMO aqueous solution of high concentration.
Compared with prior art, the present invention can obtain the NMMO aqueous solution that concentration is 65%, and steam-water ratio is 0.215, and concentration is the NMMO aqueous solution of 85%, and steam-water ratio is 0.225, all leads over world level 0.23.
The present invention can the evaporating and concentrating process of recycling design in solvent method experimental branch line and device field extensively promote for the foregoing reasons.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the structural representation of the evaporation concentration device (" five effects " evaporates and flow falling liquid film device) of a kind of cellulose solvent NMMO aqueous solution in embodiments of the invention 1.
Fig. 2 is the structural representation of the evaporation concentration device (" five effects connect dense effect " evaporates and flow falling liquid film device) of a kind of cellulose solvent NMMO aqueous solution in embodiments of the invention 2.
Fig. 3 is the structural representation of the evaporation concentration device (" five effects " evaporation, countercurrent falling-film device) of a kind of cellulose solvent NMMO aqueous solution in embodiments of the invention 3.
Wherein, A is steam, B to be concentration be 15% the low temperature NMMO aqueous solution, C is condensed water, D to be concentration be 65% the NMMO aqueous solution, E to be concentration be 85% the NMMO aqueous solution.
Detailed description of the invention
An evaporation concentration device for the cellulose solvent NMMO aqueous solution, comprise connect in turn 1st effective evaporator, 2nd effect evaporator until n single-effect evaporator and only for 1st effective evaporator charging and the one-level preheater of preheating of connecting, secondary preheater until n level preheater; Also comprise respectively with 1st effective evaporator, 2nd effect evaporator until n single-effect evaporator be connected one imitate circulating pump, two and imitate circulating pump until n imitates circulating pump, wherein, n is one in three, four, five, six,
Under duty, the NMMO aqueous solution of pending low temperature, successively through n level preheater, n-1 level preheater until one-level preheater series connection pre-heating temperature elevation after, enter 1st effective evaporator evaporation, enter 2nd effect evaporator successively afterwards until the evaporation of n single-effect evaporator, discharge the NMMO aqueous solution after concentrating from n single-effect evaporator; The indirect steam that upper 1st effective evaporator produces enters the heater of lower 1st effective evaporator, and the indirect steam that n single-effect evaporator produces enters condensing unit; The heating steam condensed water of 1st effective evaporator enters one-level preheater, the condensed water that one-level preheater is discharged enters secondary preheater together with 2nd effect evaporator heating steam condensed water, until the condensed water that n-1 level preheater is discharged enters n level preheater together with the condensed water of n single-effect evaporator heating steam; The cryogenic condensation water that n level preheater is discharged is discharged and is used as him.
The evaporation concentration device of described a kind of cellulose solvent NMMO aqueous solution also comprises the concentrated evaporator obtaining the high concentration NMMO aqueous solution for evaporation and concentration be connected with n single-effect evaporator, and concentrated evaporator is provided with dense effect circulating pump,
Under duty, when n is four ~ six, discharge the NMMO aqueous solution after concentrating from n single-effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, the indirect steam of drawing a part of n-2 effect or n-3 single-effect evaporator enters concentrated evaporator, and concentrated evaporator heating steam condensed water enters n-1 level preheater; When n is three, discharge the NMMO aqueous solution after concentrating from triple effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, the indirect steam of drawing a part of 1st effective evaporator enters concentrated evaporator, and concentrated evaporator heating steam condensed water enters secondary preheater.
Each single-effect evaporator be provided with in the steam chamber of concentrated evaporator for stop the liquid barrier of high material casting liquid with for carrying out the silk screen be efficiently separated to the mist in indirect steam; Each effect circulating pump and dense effect circulating pump are Electromagnetic Drive without sealing circulating pump or No leakage circulating pump.
The structural design of each single-effect evaporator and concentrated evaporator is and flows falling film evaporator or reverse-flow falling film evaporator.
Preheater at different levels is the plate type heat exchanger of full welded type.
Apply an a kind of evaporating and concentrating process of the cellulose solvent NMMO aqueous solution of evaporation concentration device of the cellulose solvent NMMO aqueous solution, it is characterized in that there is following processing step:
S1, series connection preheating: the NMMO aqueous solution of pending low temperature successively through n level preheater, n-1 level preheater until reach the high temperature close to boiling point after one-level preheater series connection pre-heating temperature elevation, wherein, n is one in three, four, five, six;
S2, an effect charging: by the NMMO aqueous solution that reaches after preheating close to the high temperature of boiling point from 1st effective evaporator charging;
S3, following current are evaporated: after 1st effective evaporator evaporation, feed liquid enters 2nd effect evaporator evaporation from an effect discharge, until enter n single-effect evaporator to discharge feed liquid, obtain the NMMO aqueous solution after concentrating,
The discharge overfall of each effect is all arranged on liquid level place, exceeds the feed liquid of liquid level and overflow, is connected with the charging aperture of aftereffect by U-shaped pipe, balances the pressure reduction between each single-effect evaporator with U-shaped pipe, and makes the level being constant of each effect;
S4, dense effect connection heat: when n is four ~ six, discharge the NMMO aqueous solution after concentrating from n single-effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, concentrated evaporator draws a part of indirect steam as thermal source from n-2 effect above or n-3 single-effect evaporator, realize the combined heat of imitating vaporising device with front n, concentrated evaporator heating steam condensed water enters n-1 level preheater; When n is three, discharge the NMMO aqueous solution after concentrating from triple effect evaporator and obtain the high concentration NMMO aqueous solution through concentrated evaporator, concentrated evaporator draws a part of indirect steam as thermal source from 1st effective evaporator above, realize the combined heat with front triple-effect evaporation plant, concentrated evaporator heating steam condensed water enters n-1 level preheater.
The absolute pressure pressure of n single-effect evaporator and concentrated evaporator is 0.0024 ~ 0.006MPa.
The indirect steam that upper 1st effective evaporator produces enters the heater of lower 1st effective evaporator, and the indirect steam that n single-effect evaporator produces enters condensing unit; The heating steam condensed water of 1st effective evaporator enters one-level preheater, the condensed water that one-level preheater is discharged enters secondary preheater together with 2nd effect evaporator heating steam condensed water, until the condensed water that n-1 level preheater is discharged enters n level preheater together with the condensed water of n single-effect evaporator heating steam; The cryogenic condensation water that n level preheater is discharged is discharged and is used as him.
When n is three ~ five, described concentrated after the concentration of the NMMO aqueous solution be 65%, the concentration of the high concentration NMMO aqueous solution that described concentrated evaporator is discharged is 85%.
When n is six, the indirect steam of last evaporator passes through the sub-cooled water condensation lower than 20 DEG C; When n is one in three, four, five, the indirect steam of last evaporator passes through the circulating water condensing of air cooling tower.
Embodiment 1
As shown in Figure 1, " five effect " are evaporated and are flowed falling liquid film device and comprise 1st effective evaporator 1,2nd effect evaporator 2, triple effect evaporator 3, four-effect evaporator 4, quintuple effect evaporator 5 and be only one-level preheater 6, secondary preheater 7, three grades of preheaters 8, level Four preheater 9, Pyatyi preheaters 10 of 1st effective evaporator 1 charging and preheating of connecting; Also comprise be connected with 1st effective evaporator 1,2nd effect evaporator 2, triple effect evaporator 3, four-effect evaporator 4, quintuple effect evaporator 5 one imitate that circulating pump 11, two imitates circulating pump 12, triple effect cycle pump 13, quadruple effect circulating pump 14, five imitate circulating pump 15,
Under duty, pending concentration is the low temperature NMMO aqueous solution of 15%, successively after pre-heating temperature elevation connected by Pyatyi preheater 10, level Four preheater 9, three grades of preheaters 8, secondary preheater 7 and one-level preheaters 6, enter 1st effective evaporator 1 to evaporate, enter 2nd effect evaporator 2 afterwards successively, triple effect evaporator 3, four-effect evaporator 4, quintuple effect evaporator 5 evaporate, the concentration of discharging concentrate from quintuple effect evaporator 5 is the NMMO aqueous solution of 65%; The indirect steam that 1st effective evaporator 1 produces enters the heater of 2nd effect evaporator 2, the indirect steam that 2nd effect evaporator 2 produces enters the heater of triple effect evaporator 3, the indirect steam that triple effect evaporator 3 produces enters the heater of four-effect evaporator 4, and the indirect steam that four-effect evaporator 4 produces enters the heater of quintuple effect evaporator 5; The heating steam condensed water of 1st effective evaporator 1 enters one-level preheater 6, and the condensed water that one-level preheater 6 is discharged enters secondary preheater 7 together with 2nd effect evaporator 2 heating steam condensed water; The condensed water that secondary preheater 7 is discharged enters three grades of preheaters 8 together with triple effect evaporator 3 heating steam condensed water; The condensed water of three grades of preheater 8 discharges enters level Four preheater 9 together with four-effect evaporator 4 heating steam condensed water; The condensed water that level Four preheater 9 is discharged enters Pyatyi preheater 10 together with the condensed water of quintuple effect evaporator 5 heating steam; The cryogenic condensation water that Pyatyi preheater 10 is discharged is discharged and is used as him.
Be provided with in the steam chamber of 1st effective evaporator 1,2nd effect evaporator 2, triple effect evaporator 3, four-effect evaporator 4, quintuple effect evaporator 5 for stop the liquid barrier of high material casting liquid with for carrying out the silk screen be efficiently separated to the mist in indirect steam; One effect circulating pump 11, two effect circulating pump 12, triple effect cycle pump 13, quadruple effect circulating pump 14, five are imitated circulating pump 15 and are No leakage circulating pump.
The structural design of 1st effective evaporator 1,2nd effect evaporator 2, triple effect evaporator 3, four-effect evaporator 4, quintuple effect evaporator 5 is and flows falling film evaporator.
One-level preheater 6, secondary preheater 7, three grades of preheaters 8, level Four preheater 9, Pyatyi preheater 10 are the plate type heat exchanger of full welded type.
The indirect steam of quintuple effect evaporator 5 enters condenser 16 and cools, condenser 16 is provided with cooling water inlet 17 and steam jet ejector 18, the other end of steam jet ejector 18 is communicated with secondary condenser 19, secondary condenser 19 is provided with water ejector 20, one end of water ejector 20 is communicated with injector water tank 22 by water ejector working barrel 21, water ejector 20 the other end be directly communicated with injector water tank 22, condenser 16 is all communicated with water sealed tank 23 with secondary condenser 19.
Embodiment 2
As shown in Figure 2, " five effect connect dense effect " evaporate and flow falling liquid film device, evaporate and the difference flowing falling liquid film device is with " five imitate " in embodiment 1, also comprise concentrated evaporator 24 concentrated evaporator 24 and are provided with dense effect circulating pump 25,
The structural design of concentrated evaporator 24 is and flows falling film evaporator,
Under duty, concentration be 65% the NMMO aqueous solution obtain through concentrated evaporator the NMMO aqueous solution that concentration is 85%, concentrated evaporator 24 draws a part of indirect steam as thermal source from triple effect evaporator 3 above, realize imitating combined heat with the first five,, concentrated evaporator 24 heating steam condensed water enters level Four preheater 9.
Be provided with for stopping the liquid barrier of high material casting liquid and the silk screen for being separated the mist in indirect steam in the steam chamber of concentrated evaporator 24, dense effect circulating pump 24 is No leakage circulating pump.
The indirect steam of concentrated evaporator 24 enters condenser 16 condensation.
Embodiment 3
As shown in Figure 3, " five effects " evaporation, countercurrent falling-film device, evaporate with " five imitate " in embodiment 1 and the difference flowing falling liquid film device is, the structural design of 1st effective evaporator 1`, 2nd effect evaporator 2`, triple effect evaporator 3`, four-effect evaporator 4`, quintuple effect evaporator 5` is reverse-flow falling film evaporator.
The above; be only the present invention's preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.