CN103241748B - Process method for preparing anhydrous sodium sulphate based on flash vaporization crystallization of acid bath - Google Patents
Process method for preparing anhydrous sodium sulphate based on flash vaporization crystallization of acid bath Download PDFInfo
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- CN103241748B CN103241748B CN201310152938.0A CN201310152938A CN103241748B CN 103241748 B CN103241748 B CN 103241748B CN 201310152938 A CN201310152938 A CN 201310152938A CN 103241748 B CN103241748 B CN 103241748B
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- acid bath
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- 239000002253 acid Substances 0.000 title claims abstract description 146
- 238000002425 crystallisation Methods 0.000 title claims abstract description 76
- 230000008025 crystallization Effects 0.000 title claims abstract description 74
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 title claims abstract description 73
- 229910052938 sodium sulfate Inorganic materials 0.000 title claims abstract description 58
- 235000011152 sodium sulphate Nutrition 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title abstract description 24
- 230000008569 process Effects 0.000 title abstract description 14
- 238000009834 vaporization Methods 0.000 title abstract description 12
- 230000008016 vaporization Effects 0.000 title abstract description 12
- 238000004094 preconcentration Methods 0.000 claims abstract description 19
- 230000008719 thickening Effects 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims description 95
- 230000008020 evaporation Effects 0.000 claims description 95
- 238000007701 flash-distillation Methods 0.000 claims description 50
- 229960003010 sodium sulfate Drugs 0.000 claims description 50
- 229940056729 sodium sulfate anhydrous Drugs 0.000 claims description 50
- 239000010413 mother solution Substances 0.000 claims description 31
- 239000002562 thickening agent Substances 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 19
- 238000003672 processing method Methods 0.000 claims description 13
- 239000012452 mother liquor Substances 0.000 claims description 11
- 229920006395 saturated elastomer Polymers 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- 238000005360 mashing Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 238000005352 clarification Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000000835 fiber Substances 0.000 abstract description 3
- 229920000297 Rayon Polymers 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000005611 electricity Effects 0.000 abstract 1
- 239000010446 mirabilite Substances 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 11
- 230000008676 import Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000973497 Siphonognathus argyrophanes Species 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process method for preparing anhydrous sodium sulphate based on the flash vaporization crystallization of an acid bath. The method comprises the four main steps of: flash vaporization preconcentration and preheating, flash vaporization crystallization, thickening and separation drying. According to the method, by mainly controlling the acid intake amount of the sodium sulfate acid bath, the proportion of the sodium sulfate acid bath and other parameters, anhydrous sodium sulphate with high yield is obtained by the flash vaporization crystallization method; and by alternately controlling the flash vaporization crystallization phase and the flash vaporization concentration phase, the device is capable of normally crystallizing anhydrous sodium sulphate while being maintained under the flash vaporization running condition. Therefore, the situation that pipelines and equipment are blocked due to scaling is avoided. Compared with the traditional process, the two processes of crystallization and roasting are omitted, so that the steam and the electricity are saved substantially; the yield of anhydrous sodium sulphate is improved by 20%; and the problem of discharging a large amount of mirabilite is solved. The process method disclosed by the invention is reasonable in process and strong in operability, thereby being as a direction for improving the acid bath circulation treatment technology in the viscose fiber industry.
Description
Technical field
The present invention relates to the acid bath recovery processing technique in viscose fiber production, specifically a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization.
Background technology
The acid bath of chemical fibre factory is solidified for zehla, and in zehla process of setting, acid bath is diluted, and has increased the composition of sodium sulfate.Spent acid is bathed and is wanted recycling use, and the moisture that acid bath must be increased at zehla process of setting and sodium sulfate are removed.Existing technology is that separated moisture, then carries out subcooling concentrated acid bath with the concentrated acid bath of flash distillation plant, and crystallization goes out saltcake, and saltcake is carried out to hot melt, evaporative crystallization (being commonly called as " roasting ") again, obtains Sodium sulfate anhydrous.min(99).Current new flash crystallization technology, be by flash concentration device be designed to can flash crystallization Sodium sulfate anhydrous.min(99) device, make to remove moisture and sodium sulfate completes in flash vaporization process simultaneously.But disclosed is in recent years all the equipment of flash crystallization Sodium sulfate anhydrous.min(99), and in reparation technology method, do not do too much open, how under set flash vaporization condition, how to control the parameters such as the sour proportion of entering of acid bath, acid intake amount, crystalline mother solution proportion, crystallization goes out enough Sodium sulfate anhydrous.min(99) becomes technical problem urgently to be resolved hurrily at present.
Summary of the invention
According to the technical problem of above-mentioned proposition, and provide a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization.The present invention mainly passes through to control the processing parameter of each link, thereby obtains the Sodium sulfate anhydrous.min(99) of high yield.
The technique means that the present invention adopts is as follows:
Based on acid bath flash crystallization, produce a processing method for Sodium sulfate anhydrous.min(99), it is characterized in that comprising the steps:
1. flash distillation pre-concentration and preheating: pending sodium sulfate acid bath is carried out to pre-concentration with default flash distillation plant, and described default flash distillation plant is the flash concentration device outside this flash crystallization device, i.e. traditional flash distillation plant; The proportion γ of the sodium sulfate acid bath after pre-concentration is 1.35～1.43; Sodium sulfate acid bath after pre-concentration enters from the final stage flash distillation mixing tank of flash crystallization device, and from the crystalline mother solution of thickener inspiration, mixes, is pumped into preheating in flash distillation preheater flash distillation;
The acid intake amount of sodium sulfate acid bath is L
v, L
vfor the volumetric flow rate of acid intake amount, L
vmeet:
L
v=L/γ，
Wherein, the weight rate that L is acid intake amount;
Preferably, enter the proportion γ of sodium sulfate acid bath of flash crystallization device the most suitable between 1.38～1.41;
The weight rate L of described sodium sulfate acid bath acid intake amount meets:
L=W/β
z，
Wherein: W is the steam output of flash crystallization device, β
zfor sodium sulfate acid bath total evaporation rate, β
zalso meet:
β
z=β
j（1-β
b）+β
b，
Wherein: β
bfor saturated rate of evaporation, β
jfor crystallization and evaporation rate, β
jbetween 10%～15%.
Saturated rate of evaporation β
bdetermine with sodium sulfate acid bath proportion, form relevant, the composition that need be averaged sodium sulfate acid bath carries out evaporation experiment, while being determined at different rate of evaporation, the variation of sodium sulfate acid bath proportion, until sodium sulfate is saturated in sodium sulfate acid bath, be evaporated to the saturated rate of evaporation that the rate of evaporation of sodium sulfate when saturated is sodium sulfate acid bath, record the sodium sulfate acid bath proportion of sodium sulfate when saturated;
Crystallization and evaporation rate β
jdetermine relevantly with the evaporation terminal requiring, evaporation terminal is spent and is limited with the crystalline mother solution elevation of boiling point 9.Should the crystallization control mother liquor elevation of boiling point, the elevation of boiling point can reduce steam output, increase steam consumption, so restriction that the terminal of crystallization and evaporation is risen by boiling point, make exactly boiling point rise too not high, the elevation of boiling point is 9 while spending, and crystallization and evaporation rate, in 15% left and right, surpasses 9 degree, heat transfer to flash crystallization device has considerable influence, so determine crystallization and evaporation rate β
jbe between 10～15%;
2. flash crystallization: the sodium sulfate acid bath after preheating enters heater heats, enter again flashing chamber flash concentration, then enter in flash evaporation crystallizer, crystallisate circulates at flash evaporation crystallizer inner suspension, particle is grown up, and from upper level flash evaporation crystallizer, discharge and enter next stage flash evaporation crystallizer continuation crystallization continuously, finally by final stage flash evaporation crystallizer, be drained in thickener; The secondary steam that the flash evaporation crystallizer of final stage is discharged enters condenser condenses;
3. thickening: the suspension continuous sedimentation in thickener that contains Sodium sulfate anhydrous.min(99) crystallisate particle, thickening is to discharge after Sodium sulfate anhydrous.min(99) slurry; After upper strata crystalline mother solution clarification in thickener, be preferentially inhaled in final stage flash distillation mixing tank, with the sodium sulfate acid bath mixed flash boiling through pre-concentration newly entering reenter step 1. in; All the other crystalline mother solutions enter concentrated acid tank; The proportion of crystalline mother solution is γ
j, γ
jbe controlled between 1.45～1.47; The secondary steam that final stage flash distillation mixing tank is discharged enters condenser condenses;
4. separated dry: the acid Sodium sulfate anhydrous.min(99) slurry of discharge adds alkali lye neutralization, separating and dehydrating, dry through anticorrosion vacuum filter separated mother liquor, hydro-peening, after blotting, and obtains Sodium sulfate anhydrous.min(99) finished product.
Further, the output of the Sodium sulfate anhydrous.min(99) finished product that described step obtains in is 4. G, and G meets:
G=0.453ρ（W-L*β
b），
Wherein, the rate that obtains that ρ is Sodium sulfate anhydrous.min(99), ρ is between 80%～92%, and the knot wall of its numerical value and container, pipeline is, change damage, alternate cycle and the Sodium sulfate anhydrous.min(99) of concentrated alternately operating particle when separated runs off relevant.
Further, the flash crystallization of described step in 2. and two kinds of evaporation modes of flash concentration are for hocketing, and the time cycle ratio of flash crystallization and flash concentration alternate run is 5～21:3.In alternate run, clean fouling in effect pipe, flash evaporation crystallizer but evaporative process uninterrupted, continued transpiring moisture among alternately.Alternate run excessive cycle, the increase of crystallization dirt piece is dropped, and easily causes equipment, line clogging.In addition, alternate cycle and the particle wastage of knot wall situation, crystallization and the concentration operation of the rate that the obtains ρ of Sodium sulfate anhydrous.min(99) during with flash crystallization are relevant, because replace at every turn, in the fouling of undersaturated sodium sulfate acid bath in dissolving pipeline, equipment, also change the Sodium sulfate anhydrous.min(99) particle damaging in suspension.In addition, in order to extend alternate cycle, the connecting tube between crystallizer and the material of crystallizer, outside corrosion-resistant, heatproof require, also will select smooth surface, have the not less scaling material making of viscosity.
The present invention is controlled at flash vaporization point in 110-50 ℃ of region, belongs to the phase region that anhydrous sodium sulphate (being Sodium sulfate anhydrous.min(99)) is separated out; Find that its key is that sodium sulfate acid bath will carry out pre-concentration, improve the sodium sulfate acid bath proportion that enters flash crystallization device, preferably be controlled between 1.38～1.41, when proportion is low, Sodium sulfate anhydrous.min(99) crystallization content is few, and proportion is too high, increase the difficulty of sodium sulfate acid bath pre-concentration and sodium sulfate acid bath allotment.Enter the Sodium sulfate anhydrous.min(99) quantity that sour proportion should needed separation in sodium sulfate acid bath balance and decide, while requiring separated quantity many, specific gravity control adjustable height.
Further, the pre-concentration of described sodium sulfate acid bath, refer to that acid bath is before entering flash crystallization device, should pass through default flash distillation plant, the present invention is that to utilize original traditional flash concentration device be between 1.38～1.41 by sodium sulfate acid bath pre-concentration to proportion, to produce more Sodium sulfate anhydrous.min(99).The flash crystallization device that the present invention adopts has following structure: comprise 5～12 grades of flash distillation preheaters, well heater, 0～5 grade of flashing chamber, multistage flash evaporation crystallizer, final stage flash distillation mixing tank, condenser, thickener, recycle pump, vacuum filter, in and stirrer, mashing pump, separating machine and moisture eliminator;
Described multistage flash evaporation crystallizer comprises that at least 5 grades by pipeline successively connected flash evaporation crystallizer, is generally 5～13 grades of flash evaporation crystallizers, and described flash evaporation crystallizer is vertical, cone bottom structure; Wherein, the acid inlet of flash evaporation crystallizer and the acid discharge mouth of well heater that are positioned at the first step are connected by pipeline, the acid discharge mouth of every grade of flash evaporation crystallizer is connected by pipeline with the tangential acid inlet that is positioned at its next stage flash evaporation crystallizer respectively, and the acid discharge mouth of most end one-level flash evaporation crystallizer is connected by pipeline with the feed-pipe interface of thickener; The secondary steam outlet of the every grade of flash evaporation crystallizer respectively steam inlet of flash distillation preheater is corresponding thereto connected by pipeline, is positioned at the secondary steam outlet of most end one-level flash evaporation crystallizer and the secondary steam of final stage flash distillation mixing tank and exports and all by pipeline, be connected with the steam inlet of condenser;
Described thickener is provided with acid discharge overflow port, is also provided with the suction acid mouthful of the crystalline mother solution of clarification on described thickener, and described suction acid mouthful is inserted under crystalline mother solution liquid level, in the settling section of crystalline mother solution, inhales acid mouthful and is connected with the acid inlet of described final stage flash distillation mixing tank;
The plasma discharge mouth of described thickener is connected with the opening for feed of vacuum filter, the discharge opening of vacuum filter with in be connected with the opening for feed of stirrer, in be connected with the opening for feed of whizzer by mashing pump with the discharge port of stirrer, the discharge port of whizzer is connected with the opening for feed of moisture eliminator; The separated mother liquor outlet of described whizzer with described in and the separated mother liquor import of stirrer be connected, the mother liquor of separating from whizzer enters and in stirrer, dilute the sour nitre filter cake unloading from filter, neutralized stirring.
The slurry that thickener is discharged enters vacuum filter and inhales worry, hydro-peening, and separated mother liquor adds alkali lye neutralization with stirrer during filter cake enters, and be pressed into whizzer separating and dehydrating, and it is dry to enter moisture eliminator, is packaged as Sodium sulfate anhydrous.min(99) product through mashing pump.As preferably, the slurry that thickener is discharged adopts drum filter or belt vacuum filter separating acid nitre, and than separated better with whizzer, protection against corrosion easily and price is low, hydro-peening is effective, filtrate is clear, maintenance cost is low.
Further, described flashing chamber is the higher level's evaporation concentration equipment that is positioned at the 1st grade of flash evaporation crystallizer, the acid inlet of the flashing chamber of the 1st grade is connected by pipeline with the acid discharge mouth of well heater, the acid discharge mouth of every grade of flashing chamber is connected by pipeline with the tangential acid inlet that is positioned at its next stage flashing chamber or flash evaporation crystallizer respectively, and the steam inlet of the secondary steam outlet difference of every grade of flashing chamber preheater is corresponding thereto connected by pipeline.
The internal circulating load of flash crystallization device of the present invention all remains unchanged in flash concentration or flash crystallization process.Because internal circulating load is large, acid intake amount is little, not enough part utilizes final stage flash distillation mixing tank to draw from the clear liquid of thickener upper strata crystalline mother solution, and after mixed flash boiling, together by recycle pump, is pressed in flash distillation preheater and is preheated in final stage flash distillation mixing tank with the pre-concentration sodium sulfate acid bath of newly entering.
Compared with prior art, compare, the present invention has saved crystallization saltcake, the large technological process of roasting Sodium sulfate anhydrous.min(99) two, by the control of the parameters in sodium sulfate acid bath flash crystallization process, make under set flash vaporization amount condition, crystallization goes out enough Sodium sulfate anhydrous.min(99), make sodium sulfate acid bath circulating treatment procedure simplify simultaneously, save in a large number construction investment, energy consumption and productive expense.In traditional technology, meet fault in production and will discharge saltcake, managing good chemical fiber factory also has 20% saltcake discharge, the discharge in a large number of enterprise that management is poor, the present invention does not produce the stage of saltcake, has thoroughly stopped saltcake exhaust emission environmental problem.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is that the present invention is process flow sheet and the setting drawing of 11 grades of flash crystallization techniques.
In figure: A9～A1, flash distillation preheater;
H, well heater;
V1～V2, flashing chamber;
V3～V10, flash evaporation crystallizer;
V11, final stage flash distillation mixing tank;
MK1～MK2, condenser;
ZC, thickener;
ZG, vacuum filter;
ZJ, in and stirrer;
L, whizzer;
UP, recycle pump;
J, mashing pump;
The import of A-steam inlet B-acid bath import C-spray washing import D-alkali lye;
100,104,108,112,116,120,124,128 is the secondary steam outlet of flash evaporation crystallizer V3～V10;
101,105,109,113,117,121,125 is the steam inlet of flash distillation preheater A3～A9;
102,106,110,114,118,122,126,130 is the acid discharge mouth of flash evaporation crystallizer V3～V10;
103,107,111,115,119,123,127 is the acid inlet of flash evaporation crystallizer V4～V10;
129,135, the steam inlet of condenser MK2 and MK1;
131, thickener feed-pipe interface;
132, the crystalline mother solution of thickener is inhaled acid mouthful;
133, the crystalline mother solution import of final stage flashing chamber V11;
134, the secondary steam of final stage flashing chamber V11 outlet;
136, the acid discharge mouth of final stage flashing chamber V11;
137, thickener plasma discharge mouth;
138, the opening for feed of vacuum filter ZG;
139, the discharge port of vacuum filter ZG;
140, in and the opening for feed of stirrer ZJ;
141, in and the discharge port of stirrer ZJ;
142, the opening for feed of whizzer L;
143, the separated mother liquor outlet of whizzer L
144, mother liquor import separated with stirrer ZJ in
Embodiment
As shown in Figure 1, a kind of 11 grades of flash crystallization devices of take are example, A1～A9 is flash distillation preheater, V1, V2 are that flashing chamber, V11 are final stage flash distillation mixing tank, V3～V10 is flash evaporation crystallizer, adopt flash evaporation crystallizer vertical, the cone end, so that crystallisate is pressed into next stage crystallizer by cone bottom tube mouth, and can in crystallizer, not deposit.Sodium sulfate acid bath is through flash distillation preheater A9～A1 and heater H stepped heating, enter into flashing chamber V1～V2, flash evaporation crystallizer V3～V10 and final stage flash distillation mixing tank V11, moisture consecutive evaporation is concentrated, crystallisate circulates at flash evaporation crystallizer inner suspension, particle is grown up, and from upper level flash evaporation crystallizer, discharges and enter next stage flash evaporation crystallizer continuous crystallisation continuously; Sodium sulfate acid bath is concentrated in flashing chamber V1～V2, reaches sodium sulfate saturated or approach saturatedly, from flash evaporation crystallizer V3(, also can delay crystallization) start crystallization.Flash evaporation crystallizer V3～V10 inner edge turn round and round (preventing from tying wall), limit transpiring moisture, limit crystallization separated secondary steam.Its pipeline connects as follows: the secondary steam outlet 100 of flash evaporation crystallizer V3 is connected with the steam inlet 101 of flash distillation preheater A3, and acid discharge mouth 102 is connected with the acid inlet 103 of flash evaporation crystallizer V4, the secondary steam outlet 104 of flash evaporation crystallizer V4 is connected with the steam inlet 105 of flash distillation preheater A4, its acid discharge mouth 106 is connected with the acid inlet 107 of flash evaporation crystallizer V5, the secondary steam outlet 108 of flash evaporation crystallizer V5 is connected with the steam inlet 109 of flash distillation preheater A5, its acid discharge mouth 110 is connected with the acid inlet 111 of flash evaporation crystallizer V6, the secondary steam outlet 112 of flash evaporation crystallizer V6 is connected with the steam inlet 113 of flash distillation preheater A6, its acid discharge mouth 114 is connected with flash evaporation crystallizer V7 acid inlet 115, the secondary steam outlet 116 of flash evaporation crystallizer V7 is connected with the steam inlet 117 of flash distillation preheater A7, its acid discharge mouth 118 is connected with flash evaporation crystallizer V8 acid inlet 119, the secondary steam outlet 120 of flash evaporation crystallizer V8 is connected with the steam inlet 121 of flash distillation preheater A8, its acid discharge mouth 122 is connected with flash evaporation crystallizer V9 acid inlet 123, the secondary steam outlet 124 of flash evaporation crystallizer V9 is connected with the steam inlet 125 of flash distillation preheater A9, its acid discharge mouth 126 is connected with flash evaporation crystallizer V10 acid inlet 127, the secondary steam outlet 128 of flash evaporation crystallizer V10 is connected with the steam inlet 129 of condenser MK2, its acid discharge mouth 130 is connected with the feed-pipe interface 131 of thickener, the suspension that contains Sodium sulfate anhydrous.min(99) crystallisate particle flows out in acid discharge mouth 130, by thickener feed-pipe interface 131, enter in thickener ZC, after in thickener ZC, thickening is Sodium sulfate anhydrous.min(99) slurry, by thickener plasma discharge mouth 137, be connected with the opening for feed 138 of vacuum filter ZG and enter into vacuum filter ZG and filter and use spray washing C hydro-peening, again the discharge port 139 by vacuum filter ZG with in be connected with the opening for feed 140 of stirrer ZJ and enter into and stirrer ZJ carries out alkali lye neutralization, slurry after neutralization from and the discharge port 141 of stirrer ZJ through mashing pump J, enter into the opening for feed 142 of whizzer L, separated and to enter into moisture eliminator dry in whizzer, obtain Sodium sulfate anhydrous.min(99) finished product, wherein, the separated mother liquor of whizzer L outlet 143 with in and the separated mother liquor import 144 of stirrer ZJ be connected, make separated Recycling Mother Solution return in and in stirrer ZJ, dilute acid nitre filter cake, neutralization stirring.
On described thickener ZC, be also provided with clarification crystalline mother solution suction acid mouth 132, described crystalline mother solution is inhaled acid mouth 132 and is communicated with the crystalline mother solution import 133 of final stage flashing chamber V11; And the eo-acid entering with new sodium sulfate acid bath import from final stage flash distillation mixing tank V11 mixes (in as figure shown in B), flash distillation, by recycle pump UP, carry out the circulation of flash crystallization device.Recycle acid only need be controlled volumetric flow rate, and needn't control proportion, because controlled proportion and the volumetric flow rate of the pre-concentration sodium sulfate acid bath that enters final stage flash distillation mixing tank V11, controlled internal circulating load, just must inspiration crystalline mother solution quantitative, that proportion is 1.45～1.47, the proportion of recycle acid is exactly a fixed number.Flash crystallization device only needs regulating and controlling to enter sour proportion, enters sour flow, the outlet liquid temperature of internal circulating load, final stage flash distillation mixing tank V11 liquid temperature, heater H, has just controlled steam output and the Sodium sulfate anhydrous.min(99) output of flash distillation plant.As needs improve Sodium sulfate anhydrous.min(99) output, the proportion γ that must make the acid bath of pre-concentration sodium sulfate is in 1.35～1.43 high-end part 1.40 left and right; Pre-concentration sodium sulfate acid bath proportion and enter sour flow, internal circulating load meets the requirements, the proportion γ of crystalline mother solution
jinevitable between 1.45～1.47, without control.In addition, the secondary steam of final stage flashing chamber V11 outlet 134 is connected with the steam inlet 135 of condenser MK1.
Below by enumerating the beneficial effect that design parameter example brings processing method of the present invention, be described further.
Embodiment 1
11 grades of flash crystallization devices (as shown in Figure 1), its steam output W is 20 tons per hour, and entering sour sodium sulfate acid bath proportion γ is 1.38, and experiment obtains saturated rate of evaporation table β
bbe 12.05%, crystallization and evaporation rate β
jchoose in the middle of 10～15%, require, in situation that output is not bery high, to get β
jbe 10%, it is 80% that Sodium sulfate anhydrous.min(99) is obtained rate ρ,
Total evaporation rate β
z=β
j(1-β
b)+β
b=0.1(1-0.1205)+0.1205=20.85%;
The weight rate L=W/ β of acid intake amount per hour
z=20/0.2085=95.47t/h;
Sodium sulfate anhydrous.min(99) output G=(W-L* β
b) 0.453*80%=3.08t/h of 0.453* ρ=(20-95.47*12.05%);
The volumetric flow rate L of acid intake amount per hour
v=L/ γ=95.47/1.38=69.2m
3/ h;
Crystalline mother solution proportion γ
jfor 1.45g/l;
It is 8 ℃ that crystalline mother solution boiling point rises Δ.
Embodiment 2
14 grades of flash crystallization devices,, compared with 11 grades of corresponding flash distillation preheater and flash evaporation crystallizers of having increased of flash crystallization device, final stage flash distillation mixing tank is V14, other pipelines connect postpones successively.14 and the steam output W of flash crystallization device be 25 tons per hour, entering sour sodium sulfate acid bath proportion γ is 1.39, saturated rate of evaporation table β
bbe 10.2%, crystallization and evaporation rate β
jget 13%, due to the improvement of equipment pipe material, alleviate wall fouling, alternate cycle extends, and Sodium sulfate anhydrous.min(99) is obtained rate ρ and got 84%:
Total evaporation rate β
z=β
j(1-β
b)+β
b=0.13 (1-0.102)+0.102=21.87%;
The weight rate L=W/ β of acid intake amount per hour
z=25/0.2187=114.3t/h;
Sodium sulfate anhydrous.min(99) output G=(W-L* β
b) 0.453*0.84=5.08t/h of 0.453* ρ=(25-114.3*0.102);
The volumetric flow rate L of acid intake amount per hour
v=L/ γ=114.3/1.39=82.2m
3/ h;
Crystalline mother solution proportion γ
j=1.46g/l;
It is 8.4 ℃ that crystalline mother solution boiling point rises Δ.
Embodiment 3
11 grades of flash crystallization devices, its steam output is that W is 12 tons per hour, entering sour sodium sulfate acid bath proportion γ is 1.40, saturated rate of evaporation β
bbe 8.5%, crystallization and evaporation rate β
jget 13%, crystallizer and pipeline have adopted the material of good antiscale property, and fouling situation alleviates, alternate run cycle stretch-out, and Sodium sulfate anhydrous.min(99) is obtained rate ρ and is got 84%:
Total evaporation rate β
z=β
j(1-β
b)+β
b=0.13(1-0.085)+0.085=20.4%;
Per hourly enter sour weight rate L=W/ β
z=12/0.204=58.8t/h;
Sodium sulfate anhydrous.min(99) output G=(W-L* β
b) 0.453*0.84=2.66t/h of 0.453* ρ=(12-58.8*0.085);
The volumetric flow rate L of acid intake amount per hour
v=L/ γ=58.8/1.4=42m
3/ h;
Crystalline mother solution proportion γ
jfor 1.46g/l;
It is 8.4 ℃ that crystalline mother solution boiling point rises Δ.
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; according to technical scheme of the present invention and inventive concept thereof, be equal to replacement or changed, within all should being encompassed in protection scope of the present invention.
Claims (8)
1. based on acid bath flash crystallization, produce a processing method for Sodium sulfate anhydrous.min(99), it is characterized in that comprising the steps:
1. flash distillation pre-concentration and preheating: pending sodium sulfate acid bath is carried out to pre-concentration with default flash distillation plant; The proportion γ of the sodium sulfate acid bath after pre-concentration is 1.35～1.43; Sodium sulfate acid bath after pre-concentration enters from the final stage flash distillation mixing tank of flash crystallization device, and from the crystalline mother solution of thickener inspiration, mixes, is pumped into preheating in flash distillation preheater flash distillation;
The acid intake amount of sodium sulfate acid bath is L
v, L
vfor the volumetric flow rate of acid intake amount, L
vmeet:
L
v=L/γ，
Wherein, the weight rate that L is acid intake amount;
2. flash crystallization: the sodium sulfate acid bath after preheating enters heater heats, enter again flashing chamber flash concentration, then enter in flash evaporation crystallizer, crystallisate circulates at flash evaporation crystallizer inner suspension, particle is grown up, and after the discharge of upper level flash evaporation crystallizer enters next stage flash evaporation crystallizer continuation crystallization, is drained in thickener continuously;
3. thickening: the suspension continuous sedimentation in thickener that contains Sodium sulfate anhydrous.min(99) crystallisate particle, thickening is to discharge after Sodium sulfate anhydrous.min(99) slurry; After upper strata crystalline mother solution clarification in thickener, be preferentially inhaled in final stage flashing chamber, mix with the sodium sulfate acid bath through pre-concentration newly entering reenter step 1. in; All the other crystalline mother solutions enter concentrated acid tank; The proportion of crystalline mother solution is γ
j, γ
jbe controlled between 1.45～1.47;
4. separated dry: the acid Sodium sulfate anhydrous.min(99) slurry of discharge adds alkali lye neutralization, separating and dehydrating, dry through anticorrosion vacuum filter separated mother liquor, hydro-peening, after blotting, and obtains Sodium sulfate anhydrous.min(99) finished product.
2. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 1, is characterized in that: described step enters the proportion γ of sodium sulfate acid bath of flash crystallization device in 1. between 1.38～1.41.
3. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 1, is characterized in that: the weight rate L of the sodium sulfate acid bath acid intake amount of described step in 1. meets:
L=W/β
z，
Wherein: W is the evaporated water per hour of flash crystallization device, β
zfor sodium sulfate acid bath total evaporation rate, β
zalso meet:
β
z=β
j（1-β
b）+β
b，
Wherein: β
bfor saturated rate of evaporation, β
jfor crystallization and evaporation rate, β
jbetween 10%～15%.
4. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 2, is characterized in that: the output of the Sodium sulfate anhydrous.min(99) finished product that described step obtains in is 4. G, and G meets:
G=0.453ρ（W-L*β
b），
Wherein, the rate that obtains that ρ is Sodium sulfate anhydrous.min(99), ρ is between 80%～92%.
5. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 1, it is characterized in that: the flash crystallization of described step in 2. and two kinds of evaporation modes of flash concentration are for hocketing, and the time cycle ratio of flash crystallization and flash concentration alternate run is 5～21:3.
6. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 1, is characterized in that: described flash crystallization device comprise 5～12 grades of flash distillation preheaters, well heater, 0～5 grade of flashing chamber, multistage flash evaporation crystallizer, final stage flash distillation mixing tank, condenser, thickener, recycle pump, vacuum filter, in and stirrer, mashing pump, separating machine and moisture eliminator;
Described multistage flash evaporation crystallizer comprises that at least 5 grades by pipeline successively connected flash evaporation crystallizer, and described flash evaporation crystallizer is vertical, cone bottom structure; Wherein, the acid inlet of flash evaporation crystallizer and the acid discharge mouth of well heater that are positioned at the first step are connected by pipeline, the acid discharge mouth of every grade of flash evaporation crystallizer is connected by pipeline with the tangential acid inlet that is positioned at its next stage flash evaporation crystallizer respectively, and the acid discharge mouth of most end one-level flash evaporation crystallizer is connected by pipeline with the feed-pipe interface of thickener; The secondary steam outlet of the every grade of flash evaporation crystallizer respectively steam inlet of flash distillation preheater is corresponding thereto connected by pipeline, is positioned at the secondary steam outlet of most end one-level flash evaporation crystallizer and the secondary steam of final stage flash distillation mixing tank and exports and all by pipeline, be connected with the steam inlet of condenser;
Described thickener is provided with acid discharge overflow port, is also provided with the suction acid mouthful of the crystalline mother solution of clarification on described thickener, and described suction acid mouthful is inserted under crystalline mother solution liquid level, in the settling section of crystalline mother solution, inhales acid mouthful and is connected with the acid inlet of described final stage flash distillation mixing tank;
The plasma discharge mouth of described thickener is connected with the opening for feed of vacuum filter, the discharge opening of vacuum filter with in be connected with the opening for feed of stirrer, in be connected with the opening for feed of whizzer by mashing pump with the discharge port of stirrer, the discharge port of whizzer is connected with the opening for feed of moisture eliminator.
7. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 1, is characterized in that: the vacuum filter of described step in is 4. drum filter or belt vacuum filter.
8. a kind of processing method of producing Sodium sulfate anhydrous.min(99) based on acid bath flash crystallization according to claim 1, it is characterized in that: described flashing chamber is the higher level's evaporation concentration equipment that is positioned at the 1st grade of flash evaporation crystallizer, the acid inlet of the flashing chamber of the 1st grade is connected by pipeline with the acid discharge mouth of well heater, the acid discharge mouth of every grade of flashing chamber is connected by pipeline with the tangential acid inlet that is positioned at its next stage flashing chamber or flash evaporation crystallizer respectively, and the steam inlet of the secondary steam outlet difference of every grade of flashing chamber preheater is corresponding thereto connected by pipeline.
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| CN111470560A (en) * | 2019-01-24 | 2020-07-31 | 山东雅美科技有限公司 | Method for recycling acid wastewater in viscose fiber production |
| CN110330039B (en) * | 2019-07-16 | 2021-05-07 | 南通三圣石墨设备科技股份有限公司 | Production system and production process for continuously preparing anhydrous sodium sulphate by acid bath |
| CN112408431B (en) * | 2020-11-25 | 2023-01-17 | 赛得利(九江)纤维有限公司 | Method for preparing anhydrous sodium sulphate by acid bath evaporation of viscose |
| CN112704900B (en) * | 2020-12-17 | 2023-05-02 | 唐山三友集团兴达化纤有限公司 | Acid bath treatment method in modal fiber production process |
| CN113955773B (en) * | 2021-11-05 | 2023-10-10 | 唐山三友集团兴达化纤有限公司 | System and method for separating sodium sulfate in modal fiber acid bath |
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Effective date of registration: 20201030 Address after: Room 38-12, Room 501, building 6-2, Yingchun street, Huayuankou Economic Zone, Dalian City, Liaoning Province, 116000 Patentee after: Dalian North South Chemical New Technology Co.,Ltd. Address before: 116000, Liaoning, Dalian, Zhongshan District, Jiefang Road sea school compound No. 697, 2-3-1 Patentee before: Xu Daren |