CN102617324B - Crystal size controllable continuous crystallization process of sodium acetate trihydrate - Google Patents
Crystal size controllable continuous crystallization process of sodium acetate trihydrate Download PDFInfo
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- CN102617324B CN102617324B CN201210043014.2A CN201210043014A CN102617324B CN 102617324 B CN102617324 B CN 102617324B CN 201210043014 A CN201210043014 A CN 201210043014A CN 102617324 B CN102617324 B CN 102617324B
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- acetate trihydrate
- sodium acetate
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- slurry
- still
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 57
- 235000017281 sodium acetate Nutrition 0.000 title claims abstract description 57
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229940087562 sodium acetate trihydrate Drugs 0.000 title claims abstract description 46
- 230000008025 crystallization Effects 0.000 title claims abstract description 45
- 239000013078 crystal Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 50
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000012452 mother liquor Substances 0.000 claims abstract description 15
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical class [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- AYRVGWHSXIMRAB-UHFFFAOYSA-M sodium acetate trihydrate Chemical compound O.O.O.[Na+].CC([O-])=O AYRVGWHSXIMRAB-UHFFFAOYSA-M 0.000 claims description 12
- 239000001632 sodium acetate Substances 0.000 claims description 11
- 239000002826 coolant Substances 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- BDKZHNJTLHOSDW-UHFFFAOYSA-N [Na].CC(O)=O Chemical class [Na].CC(O)=O BDKZHNJTLHOSDW-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000000498 cooling water Substances 0.000 abstract description 4
- 230000004927 fusion Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 14
- 229960004249 sodium acetate Drugs 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- YMBNBZFZTXCWDV-UHFFFAOYSA-N ethane-1,2-diol;propane-1,2,3-triol Chemical compound OCCO.OCC(O)CO YMBNBZFZTXCWDV-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a crystal size controllable continuous crystallization process of a sodium acetate trihydrate, which includes the steps that the sodium acetate trihydrate which is concentrated to a molten state and a saturated sodium acetate solution with a temperature of 35 DEG C to 45 DEG C are simultaneously and continuously added into a receiving kettle which contains slurries, the slurries in the receiving kettle enter a crystallization heat exchanger through a circulating pump to be cooled, temperature difference between cooling water and the slurries in the crystallization heat exchanger is controlled to be in the range from 0 DEG C to 10 DEG C, the slurries after being cooled enter a crystal growth kettle to stay for 0.5 to 5 hours, the slurries in the crystal growth kettle enter a centrifugal machine, after solid-liquid separation, a solid is packaged as a product of the sodium acetate trihydrate, a liquid serving as a mother liquor further enters a crystal receiving kettle, a standby heat exchanging cooling process is switched to be used when wall attachment in tubulation of the crystallization heat exchanger occurs, and the sodium acetate trihydrate which has wall attachment is eliminated in a fusion mode. The crystal size controllable continuous crystallization process of the sodium acetate trihydrate is high in production efficiency and low in energy consumption, crystallization of the sodium acetate trihydrate can be controlled, and the problem of reduced cooling efficiency caused by wall attachment easily generated in the crystallization process is solved.
Description
Technical field
The invention belongs to the Sodium acetate trihydrate production technical field, particularly the controlled Sodium acetate trihydrate continuous crystallisation technique of a kind of crystallographic dimension.
Background technology
Sodium acetate trihydrate claims again sodium acetate trihydrate, chemical formula CH
3cOONa3H
2o, molecular weight 136.06, white or colourless transparent crystal.Sodium acetate trihydrate is a kind of heat-retaining mass preferably, and fusing point is 58.4 ℃, and melting heat is 264kJ/kg.Sodium acetate trihydrate is soluble in water, be slightly soluble in ethanol, a kind of purposes Chemicals very widely, can be for dyeing and printing auxiliary, organic synthesis industrial raw material, civilian heat-retaining mass raw material and chemical reagent, the Sodium acetate trihydrate that reaches certain purity also can be used as a kind of auxiliary pharmaceutical drugs.In recent years, Sodium acetate trihydrate also is used as the highway snow-melting agent by some countries such as Japan, to alleviate the damage to road.
Sodium acetate trihydrate is generally by acetic acid or containing obtaining after the waste acid water of acetic acid and soda ash or liquid caustic soda neutralization reaction.Because sodium acetate aqueous solution has good heat storage capacity, rate of cooling is slow; Sodium acetate trihydrate is easily sticky wall in crystallisation process, affects the solution speed of cooling and reduces crystallization rate; The size of Sodium acetate trihydrate particle, directly affect product quality and price, and the client of special purpose has particular requirement to product cut size.
Chinese patent CN200810014204.5 has introduced a kind of oarse-grained sodium-acetate production technique, after crystallization in this technique is the tap water cooling, re-use the chilled brine cooling, make at low temperatures solution supersaturation crystallization, need the slurry that manually rolls in crystallisation process, the single still crystallization of this technique, production efficiency is lower, has increased freezing energy consumption.In Chinese patent CN200810229404.2, crystallization processes is mainly cooling sodium acetate soln to hypersaturated state, add crystal seed and lure the Sodium acetate trihydrate crystallization into, after solid-liquid separation, solid is as product, filtrate is concentrated rear recrystallize again, the single still crystallization of this technique, production efficiency is lower, has increased concentrated energy consumption.U.S. Pat 44513831 has been introduced the impact on the Sodium acetate trihydrate crystallization such as additive ethylene glycol glycerol, and Ruan Deshui has introduced the impact on crystallization rate of additive and Tc in " impact of Additives On The Linear Crystallization Velocity of Sodium Acetate Trihydrate ".Zhan Licai in " transformation of sodium-acetate crystallizer tank " article the structure of sodium-acetate crystallizer tank.Aforesaid method all exists efficiency low, and energy consumption is high, and the Sodium acetate trihydrate crystallographic dimension is not allowed manageable defect.
Summary of the invention
The object of the present invention is to provide the controlled Sodium acetate trihydrate continuous crystallisation technique of a kind of crystallographic dimension, be intended to solve that Sodium acetate trihydrate periodic crystallisation production efficiency in prior art is low, easily sticky wall causes cooling efficiency to reduce and uncontrollable problem of product particle size in crystallisation process.
The Sodium acetate trihydrate continuous crystallisation technique that a kind of crystallographic dimension is controlled is characterized in that comprising step:
1) Sodium acetate trihydrate and 35 ~ 45 ℃ of saturated acetic acid sodium solutions that are concentrated into molten state enter in the reception still that slurry is housed simultaneously continuously, described slurry is the sodium acetate soln that contains the acetate trihydrate sodium crystal, temperature is 35 ~ 45 ℃, and wherein, the weight percent of acetate trihydrate sodium crystal is 10 ~ 50%;
2) receive slurry in still and enter in the crystallization interchanger by recycle pump, cool, in the crystallization control interchanger, water coolant and the slurry temperature difference are 0 ~ 10 ℃;
3) slurry after cooling enters crystal growth still, and slurry residence time in crystal growth still is 0.5 ~ 5 hour;
4) in crystal growth still, slurry enters whizzer, and after solid-liquid separation, solid is as the Sodium acetate trihydrate packing of product, and liquid enters crystallization as mother liquor again and accepts still.
5) when crystallization heat exchanger tube knot wall, switch to standby heat exchange cooling process, and the Sodium acetate trihydrate of knot wall is carried out to the melting removing.
Further, the described slurry temperature of step 1 is preferably 45 ℃.
In step 1, the weight percent of acetate trihydrate sodium crystal is preferably 20 ~ 30%.
In step 2 in interchanger water coolant and the slurry temperature difference be preferably 1 ~ 5 ℃.
Sodium acetate trihydrate product particle size of the present invention controlled, when slurry stops 0.5 ~ 1 hour, 2 ~ 3 hours, 4 ~ 5 hours in crystal growth still, obtain the product crystal size and be respectively 0.4 ~ 0.5mm, 0.6 ~ 0.8mm, 0.8 ~ 1.0mm.
Schema as shown in Figure 1, concrete grammar of the present invention is:
The reception still 1 that contains slurry receives continuously: from the acetate trihydrate sodium content of concentration section approximately 100%, the Sodium acetate trihydrate of 60 ~ 75 ℃ of molten states of temperature, with from the mother liquor after whizzer 6 solid-liquid separation.Described slurry is the sodium acetate soln that contains the acetate trihydrate sodium crystal, and temperature is 35 ~ 45 ℃, and wherein, the weight percent of acetate trihydrate sodium crystal is 10 ~ 50%.Receive in still 1 slurry and enter crystallization interchanger 2A by forced circulation pump 7 and cool, loop back and receive still 1.In the crystallization control interchanger, water coolant and the slurry temperature difference are 0 ~ 10 ℃.Slurry after cooling branches to crystal growth still 5 by the aperture of by-pass valve control 11A.Slurry residence time in crystal growth still 5 is 0.5 ~ 5 hour, along with the length of the residence time forms the crystal of different-grain diameter.In crystal growth still 5, slurry enters whizzer 6, and after solid-liquid separation, solid is as the packing of product, and liquid enters and accepts still 1 by pump 9 as mother liquor.The dashpot that in figure, 3A is the controlled circulation water temp, by the aperture of DCS autocontrol valve 12A, 13A, regulate the circulating water temperature that interchanger 2A needs.
The Sodium acetate trihydrate crystallization is accompanied by the knot wall of tubulation in crystallization interchanger 2A, causes the slurry cooling efficiency is reduced.Now switch three-way valve 10, make slurry by crystallization interchanger 2B heat exchange, and when using standby heat exchange (crystallization interchanger 2B) cooling heat transferring, each valve B and pump B operate as A as shown in the figure.Open recycle pump 8A and interchanger 4A steam, close the recirculated water turnover valve of dashpot 3A, water in surge tank is heated to 70 ~ 100 ℃, melt the Sodium acetate trihydrate on crystallization interchanger 2A tubulation.On crystallization interchanger 2B tubulation, the thawing of Sodium acetate trihydrate is by crystallization interchanger 2A operation.When crystallization interchanger 2B cooling efficiency reduces, then switch to the next cooling slurry of crystallization interchanger 2A, operation realizes the continuous crystallisation production of Sodium acetate trihydrate and so forth.
The inventive method production efficiency is high, and energy consumption is low, and the Sodium acetate trihydrate crystallization can be controlled, and has solved the problem that in the crystallisation process, easily sticky wall causes cooling efficiency to reduce.
The accompanying drawing explanation
Fig. 1 is schema of the present invention, wherein: 1-reception still; 2A, 2B-crystallization interchanger; 3A, 3B-dashpot; 4A, 4B-interchanger; 5-crystal growth still; 6-whizzer; 7-recycle pump; 8A, 8B-recycle pump; 9-pump; 10-T-valve; 11A, 11B-valve; 12A, 12B-valve; 13A, 13B-valve; 14-valve; 15-mother liquor transfer tank; 16-valve.
Embodiment
Embodiment 1:
By-pass valve control 14 apertures, the flow of the Sodium acetate trihydrate 1t/h that molten state is lower 60 ℃ enters and receives still 1.By-pass valve control 16 apertures, mother liquor 4t/h enters and receives still 1.Receiving slurry temperature in still is 45 ℃, and the weight percent of acetate trihydrate sodium crystal is 20%.In crystallization control interchanger 2A, water coolant and the slurry temperature difference are 5 ℃, and temperature of cooling water is 40 ℃.Controlling slurry flow is that 5t/h enters crystal growth still 5, and in still, the residence time is 0.5 hour.In still 5, slurry gravity flows into whizzer 6, and centrifugal rear solid is product, and product sodium-acetate particle diameter is 0.4 ~ 0.5mm., mother liquor advances mother liquor transfer tank 15 recycleds.
The stream time of crystallization interchanger 2A is 10h, after the full 10h of non-stop run, needs the switching slurry to crystallization interchanger 2B cooling heat transferring, and then on heat exchanger 2A tubulation, Sodium acetate trihydrate melts operation.
Embodiment 2:
By-pass valve control 14 apertures, the flow of the Sodium acetate trihydrate 1t/h that molten state is 75 ℃ enters and receives still 1.By-pass valve control 16 apertures, mother liquor 1t/h enters and receives still 1.Receiving slurry temperature in still is 45 ℃, and the weight percent of acetate trihydrate sodium crystal is 50%.In crystallization control interchanger 2A, water coolant and the slurry temperature difference are 10 ℃, and temperature of cooling water is 35 ℃.Controlling slurry flow is that 2t/h enters crystal growth still 5, and in still, the residence time is 5 hours.In still 5, slurry gravity flows into whizzer 6, and centrifugal rear solid is product, and product sodium-acetate particle diameter is 0.8 ~ 1.0mm.Mother liquor advances the mother liquor tank recycled.
The stream time of this embodiment interchanger 2A is 2h, after the full 2h of non-stop run, needs the switching slurry to interchanger 2B cooling heat transferring, and then on heat exchanger 2A tubulation, Sodium acetate trihydrate melts operation.
Embodiment 3:
By-pass valve control 14 apertures, the flow of the Sodium acetate trihydrate 1t/h that molten state is 65 ℃ enters and receives still 1.By-pass valve control 16 apertures, mother liquor 9t/h enters and receives still 1.Receiving slurry temperature in still is 35 ℃, and the weight percent of acetate trihydrate sodium crystal is 10%.In crystallization control interchanger 2A, water coolant and the slurry temperature difference are 1 ℃, and temperature of cooling water is 34 ℃.Controlling slurry flow is that 10t/h enters crystal growth still 5, and in still, the residence time is 0.5 hour.In still 5, slurry gravity flows into whizzer 6, and centrifugal rear solid is product, and product sodium-acetate particle diameter is 0.4 ~ 0.5mm.Mother liquor advances mother liquor transfer tank 15 recycleds.
The stream time of this embodiment interchanger 2A is 48h, after the full 48h of non-stop run, needs the switching slurry to interchanger 2B cooling heat transferring, and then on heat exchanger 2A tubulation, Sodium acetate trihydrate melts operation.
The foregoing is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, any for breaking away from invention technical scheme content, according to technical spirit of the present invention, above embodiment is made to any simple modification, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (4)
1. the Sodium acetate trihydrate continuous crystallisation technique that crystallographic dimension is controlled is characterized in that comprising step:
1) Sodium acetate trihydrate and 35 ~ 45 ℃ of saturated acetic acid sodium solutions that are concentrated into molten state enter in the reception still that slurry is housed simultaneously continuously, described slurry is the sodium acetate soln that contains the acetate trihydrate sodium crystal, temperature is 35 ~ 45 ℃, and wherein, the weight percent of acetate trihydrate sodium crystal is 10 ~ 50%;
2) receive slurry in still and enter in the crystallization interchanger by recycle pump, cool, in the crystallization control interchanger, water coolant and the slurry temperature difference are 0 ~ 10 ℃;
3) slurry after cooling enters crystal growth still, and slurry residence time in crystal growth still is 0.5 ~ 5 hour;
4) in crystal growth still, slurry enters whizzer, and after solid-liquid separation, solid is as the Sodium acetate trihydrate packing of product, and liquid enters crystallization as mother liquor again and receives still;
5) when crystallization heat exchanger tube knot wall, switch to standby crystallization interchanger, and the Sodium acetate trihydrate of knot wall is carried out to the melting removing.
2. technique as claimed in claim 1, is characterized in that, the described slurry temperature of step 1 is 45 ℃.
3. technique as claimed in claim 1, is characterized in that, in step 1, the weight percent of acetate trihydrate sodium crystal is 20 ~ 30%.
4. technique as claimed in claim 1, is characterized in that, in step 2 in the crystallization interchanger water coolant and the slurry temperature difference be 1 ~ 5 ℃.
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| CN107686445A (en) * | 2017-09-22 | 2018-02-13 | 山西卓联锐科科技有限公司 | A kind of method for improving sodium acetate crystallographic granularity |
| CN107501082A (en) * | 2017-09-26 | 2017-12-22 | 侯马高知新生物科技有限公司 | A kind of sodium acetate crystal grain does big method |
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| DD285591A5 (en) * | 1989-10-24 | 1990-12-19 | ��������@��������@����������@���k�� | METHOD FOR THE PRODUCTION OF GRANULATED SODIUM ACETATE TRIHYDRATE |
| CN101671246B (en) * | 2009-09-23 | 2013-01-09 | 无锡百川化工股份有限公司 | Method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts |
| CN101735268B (en) * | 2009-12-07 | 2012-05-16 | 浙江嘉化集团股份有限公司 | Process for post-treatment of acephate and method for recovering waste water resources |
| CN102351679B (en) * | 2011-10-10 | 2013-09-18 | 东营金明工贸有限公司 | Method for producing crystalline sodium acetate with one-step method |
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