CN102617324A - 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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- CN102617324A CN102617324A CN2012100430142A CN201210043014A CN102617324A CN 102617324 A CN102617324 A CN 102617324A CN 2012100430142 A CN2012100430142 A CN 2012100430142A CN 201210043014 A CN201210043014 A CN 201210043014A CN 102617324 A CN102617324 A CN 102617324A
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- Prior art keywords
- sodium acetate
- acetate trihydrate
- crystallization
- slurry
- still
- Prior art date
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- 235000017281 sodium acetate Nutrition 0.000 title claims abstract description 68
- 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 57
- 229940087562 sodium acetate trihydrate Drugs 0.000 title claims abstract description 57
- 238000002425 crystallisation Methods 0.000 title claims abstract description 55
- 230000008025 crystallization Effects 0.000 title claims abstract description 43
- 239000013078 crystal Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 50
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 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
- 230000004927 fusion Effects 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000005516 engineering process Methods 0.000 claims description 12
- 239000001632 sodium acetate Substances 0.000 claims description 11
- 239000002826 coolant Substances 0.000 claims description 8
- 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
- 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 5
- 230000008020 evaporation Effects 0.000 description 4
- 238000001704 evaporation Methods 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
- 230000000996 additive effect Effects 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000243 solution 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
- 238000002844 melting Methods 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
- 239000012141 concentrate Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 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
- 230000008018 melting Effects 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
- AYRVGWHSXIMRAB-UHFFFAOYSA-M sodium acetate trihydrate Chemical compound O.O.O.[Na+].CC([O-])=O AYRVGWHSXIMRAB-UHFFFAOYSA-M 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
Classifications
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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, the Sodium acetate trihydrate continuous crystallisation technology that particularly a kind of crystallographic dimension is controlled.
Background technology
Sodium acetate trihydrate is claimed SODIUM ACETATE TRIHYDRATE again, 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; Be a kind of purposes Chemicals very widely, can be used 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 is also waited some countries as the highway snow-melting agent, to alleviate the damage to road by Japan.
Sodium acetate trihydrate generally obtains by acetic acid or after containing waste acid water and the soda ash or the liquid caustic soda neutralization reaction of acetic acid.Because sodium acetate aqueous solution has good heat storage capacity, rate of cooling is slow; Sodium acetate trihydrate is easily sticking wall in crystallisation process, influences the solution speed of cooling and reduces crystallization rate; Sodium acetate trihydrate particulate size directly affects 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 technology is the tap water cooling, re-use the chilled brine cooling, make solution supersaturation crystallization at low temperatures; Need the manual work slurry that rolls in the crystallisation process; The single still crystallization of this technology, production efficiency is lower, has increased freezing energy consumption.Crystallization processes is mainly the cooling sodium acetate soln to hypersaturated state among the Chinese patent CN200810229404.2; Add crystal seed and lure the Sodium acetate trihydrate crystallization into; Solid is as product after the solid-liquid separation, and filtrating concentrates the back recrystallize again, the single still crystallization of this technology; Production efficiency is lower, has increased concentrated energy consumption.U.S. Pat 44513831 has been introduced additive terepthaloyl moietie USP Kosher etc. to the influence of Sodium acetate trihydrate crystalline, and Ruan Deshui has introduced the influence to crystallization rate of additive and Tc in " additive is to the influence of sodium acetate trihydrate crystallization rate ".Zhan Licai has mainly introduced the structure of sodium-acetate crystallizer tank in " transformation of sodium-acetate crystallizer tank ".Aforesaid method all exists efficient low, and energy consumption is high, and the Sodium acetate trihydrate crystallographic dimension is not allowed manageable defective.
Summary of the invention
The object of the present invention is to provide the controlled Sodium acetate trihydrate continuous crystallisation technology of a kind of crystallographic dimension, be intended to solve that Sodium acetate trihydrate periodic crystallisation production efficiency in the prior art is low, easily sticking wall causes evaporation efficiency to reduce and uncontrollable problem of product particle size in the crystallisation process.
The Sodium acetate trihydrate continuous crystallisation technology 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 get into continuously simultaneously and are equipped with in the reception still of slurry; Said slurry is for containing Sodium acetate trihydrate crystalline sodium acetate soln; Temperature is 35 ~ 45 ℃, and wherein, Sodium acetate trihydrate crystalline weight percent is 10 ~ 50%;
2) slurry gets in the crystallization interchanger through recycle pump in the reception still, cools, and the water coolant and the slurry temperature difference are 0 ~ 10 ℃ in the crystallization control interchanger;
3) slurry after cooling gets into the crystal growth still, and slurry residence time in the crystal growth still is 0.5 ~ 5 hour;
4) slurry gets into whizzer in the crystal growth still, and solid is as the Sodium acetate trihydrate packing of product after the solid-liquid separation, and liquid gets into crystallization again as mother liquor and accepts still.
5) when crystallization heat exchanger tube knot wall, switch to subsequent use heat exchange cooling process, and the Sodium acetate trihydrate of knot wall is carried out the fusion removing.
Further, the said slurry temperature of step 1 is preferably 45 ℃.
Sodium acetate trihydrate crystalline weight percent is preferably 20 ~ 30% in the step 1.
In the step 2 in the interchanger water coolant and the slurry temperature difference be preferably 1 ~ 5 ℃.
Sodium acetate trihydrate product particle of the present invention size controlled when slurry stopped in the crystal growth still 0.5 ~ 1 hour, 2 ~ 3 hours, 4 ~ 5 hours, obtains the product crystal size and is 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: the Sodium acetate trihydrate of, temperature 60 ~ 75 ℃ molten states about 100% from the acetate trihydrate sodium content of concentration section and from the mother liquor after whizzer 6 solid-liquid separation.Said slurry is for containing Sodium acetate trihydrate crystalline sodium acetate soln, and temperature is 35 ~ 45 ℃, and wherein, Sodium acetate trihydrate crystalline weight percent is 10 ~ 50%.Slurry cools through forced circulation pump 7 entering crystallization interchanger 2A in the reception still 1, loops back and receives still 1.The water coolant and the slurry temperature difference are 0 ~ 10 ℃ in the crystallization control interchanger.Slurry after cooling branches to crystal growth still 5 through the aperture of by-pass valve control 11A.Slurry residence time in crystal growth still 5 is 0.5 ~ 5 hour, forms the crystal of different-grain diameter along with the length of the residence time.Slurry gets into whizzer 6 in the crystal growth still 5, and solid is as the packing of product after the solid-liquid separation, and liquid gets into through pump 9 as mother liquor and accepts still 1.3A is the dashpot of Control Circulation water temp among the figure, through the aperture of DCS autocontrol valve 12A, 13A, regulates the circulating water temperature that interchanger 2A needs.
The Sodium acetate trihydrate crystallization is accompanied by the knot wall of tubulation among the crystallization interchanger 2A, causes the slurry evaporation efficiency is reduced.This moment, switch three-way valve 10 made slurry through crystallization interchanger 2B heat exchange, and as shown in the figure when using subsequent use heat exchange (crystallization interchanger 2B) cooling heat transferring, each valve B and pump B such as A operate.Open recycle pump 8A and interchanger 4A steam, close the recirculated water turnover valve of dashpot 3A, water in the surge tank is heated to 70 ~ 100 ℃, melt the Sodium acetate trihydrate on the crystallization interchanger 2A tubulation.The thawing of Sodium acetate trihydrate is by crystallization interchanger 2A operation on the crystallization interchanger 2B tubulation.When crystallization interchanger 2B evaporation efficiency reduces, switch to crystallization interchanger 2A again and cool off slurry, so back and forth operation realizes the continuous crystallisation production of Sodium acetate trihydrate.
The inventive method production efficiency is high, and energy consumption is low, Sodium acetate trihydrate crystallization may command, and solved the problem that easily sticking wall causes evaporation efficiency to reduce in the crystallisation process.
Description of drawings
Fig. 1 is a 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; Turn trough in 15-mother liquor; 16-valve.
Embodiment
Embodiment 1:
By-pass valve control 14 apertures, the flow of the Sodium acetate trihydrate 1t/h that molten state is following 60 ℃ get into and receive still 1.By-pass valve control 16 apertures, mother liquor 4t/h gets into and receives still 1.Slurry temperature is 45 ℃ in the reception still, and Sodium acetate trihydrate crystalline weight percent is 20%.The water coolant and the slurry temperature difference are 5 ℃ among the crystallization control interchanger 2A, and promptly temperature of cooling water is 40 ℃.The control slurry flow is that 5t/h gets into crystal growth still 5, and the residence time is 0.5 hour in still.Slurry gravity flows into whizzer 6 in the still 5, and centrifugal back solid is a product, and product sodium-acetate particle diameter is 0.4 ~ 0.5mm., mother liquor advances turn trough 15 recycleds in the mother liquor.
The stream time of crystallization interchanger 2A is 10h, behind the full 10h of non-stop run, needs to switch slurry to crystallization interchanger 2B cooling heat transferring, and Sodium acetate trihydrate melts operation on the heat exchanging device 2A tubulation then.
Embodiment 2:
By-pass valve control 14 apertures, the flow of the Sodium acetate trihydrate 1t/h that molten state is 75 ℃ get into and receive still 1.By-pass valve control 16 apertures, mother liquor 1t/h gets into and receives still 1.Slurry temperature is 45 ℃ in the reception still, and Sodium acetate trihydrate crystalline weight percent is 50%.The water coolant and the slurry temperature difference are 10 ℃ among the crystallization control interchanger 2A, and promptly temperature of cooling water is 35 ℃.The control slurry flow is that 2t/h gets into crystal growth still 5, and the residence time is 5 hours in still.Slurry gravity flows into whizzer 6 in the still 5, and centrifugal back solid is a 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, behind the full 2h of non-stop run, needs to switch slurry to interchanger 2B cooling heat transferring, and Sodium acetate trihydrate melts operation on the heat exchanging device 2A tubulation then.
Embodiment 3:
By-pass valve control 14 apertures, the flow of the Sodium acetate trihydrate 1t/h that molten state is 65 ℃ get into and receive still 1.By-pass valve control 16 apertures, mother liquor 9t/h gets into and receives still 1.Slurry temperature is 35 ℃ in the reception still, and Sodium acetate trihydrate crystalline weight percent is 10%.The water coolant and the slurry temperature difference are 1 ℃ among the crystallization control interchanger 2A, and promptly temperature of cooling water is 34 ℃.The control slurry flow is that 10t/h gets into crystal growth still 5, and the residence time is 0.5 hour in still.Slurry gravity flows into whizzer 6 in the still 5, and centrifugal back solid is a product, and product sodium-acetate particle diameter is 0.4 ~ 0.5mm.Mother liquor advances turn trough 15 recycleds in the mother liquor.
The stream time of this embodiment interchanger 2A is 48h, behind the full 48h of non-stop run, needs to switch slurry to interchanger 2B cooling heat transferring, and Sodium acetate trihydrate melts operation on the heat exchanging device 2A tubulation then.
The above is merely preferred embodiment of the present invention; Be not that the present invention is done 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 any simple modification, equivalent variations and modification, all belong in the scope of technical scheme of the present invention.
Claims (4)
1. Sodium acetate trihydrate continuous crystallisation technology 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 get into continuously simultaneously and are equipped with in the reception still of slurry; Said slurry is for containing Sodium acetate trihydrate crystalline sodium acetate soln; Temperature is 35 ~ 45 ℃, and wherein, Sodium acetate trihydrate crystalline weight percent is 10 ~ 50%;
2) slurry gets in the crystallization interchanger through recycle pump in the reception still, cools, and the water coolant and the slurry temperature difference are 0 ~ 10 ℃ in the crystallization control interchanger;
3) slurry after cooling gets into the crystal growth still, and slurry residence time in the crystal growth still is 0.5 ~ 5 hour;
4) slurry gets into whizzer in the crystal growth still, and solid is as the Sodium acetate trihydrate packing of product after the solid-liquid separation, and liquid gets into crystallization again as mother liquor and accepts still;
5) when crystallization heat exchanger tube knot wall, switch to subsequent use heat exchange cooling process, and the Sodium acetate trihydrate of knot wall is carried out the fusion removing.
2. technology as claimed in claim 1 is characterized in that, the said slurry temperature of step 1 is 45 ℃.
3. technology as claimed in claim 1 is characterized in that, Sodium acetate trihydrate crystalline weight percent is 20 ~ 30% in the step 1.
4. technology as claimed in claim 1 is characterized in that, in the step 2 in the crystallization interchanger water coolant and the slurry temperature difference be 1 ~ 5 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210043014.2A CN102617324B (en) | 2012-02-24 | 2012-02-24 | Crystal size controllable continuous crystallization process of sodium acetate trihydrate |
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| CN201210043014.2A CN102617324B (en) | 2012-02-24 | 2012-02-24 | Crystal size controllable continuous crystallization process of sodium acetate trihydrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0424804A2 (en) * | 1989-10-24 | 1991-05-02 | GLATT INGENIEURTECHNIK GmbH | Process for preparing granulated sodium acetate trihydrate |
| CN101671246A (en) * | 2009-09-23 | 2010-03-17 | 无锡百川化工股份有限公司 | Method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts |
| CN101735268A (en) * | 2009-12-07 | 2010-06-16 | 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 |
| CN102351679A (en) * | 2011-10-10 | 2012-02-15 | 东营金明工贸有限公司 | Method for producing crystalline sodium acetate with one-step method |
-
2012
- 2012-02-24 CN CN201210043014.2A patent/CN102617324B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0424804A2 (en) * | 1989-10-24 | 1991-05-02 | GLATT INGENIEURTECHNIK GmbH | Process for preparing granulated sodium acetate trihydrate |
| CN101671246A (en) * | 2009-09-23 | 2010-03-17 | 无锡百川化工股份有限公司 | Method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts |
| CN101735268A (en) * | 2009-12-07 | 2010-06-16 | 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 |
| CN102351679A (en) * | 2011-10-10 | 2012-02-15 | 东营金明工贸有限公司 | Method for producing crystalline sodium acetate with one-step method |
Non-Patent Citations (1)
| Title |
|---|
| 崔勇等: "稀醋酸制备醋酸钠试验", 《云南化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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