CN101671246B - Method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts - Google Patents
Method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts Download PDFInfo
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- CN101671246B CN101671246B CN 200910035519 CN200910035519A CN101671246B CN 101671246 B CN101671246 B CN 101671246B CN 200910035519 CN200910035519 CN 200910035519 CN 200910035519 A CN200910035519 A CN 200910035519A CN 101671246 B CN101671246 B CN 101671246B
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Abstract
The invention relates to a method for producing sodium acetate trihydrate and anhydrous sodium acetate as byproducts, which comprises the following steps: firstly, taking sodium acetate solution which is a byproduct generated in the production process of trimellitic anhydride, pouring into a material mixing kettle, stirring, and neutralizing until the pH value is 6-9; secondly, evaporating and concentrating; thirdly, putting the concentrated sodium acetate solution in a crystallization kettle, cooling to 60-57 DEG C, adding sodium acetate trihydrate crystals accounting for 0.05-0.5% by mass of the solution in the kettle to provoke the crystallization, and stirring for more than 12 hours; fourthly, centrifugally separating to obtain the solid phase which is the sodium acetate trihydrate; and fifthly, drying the sodium acetate trihydrate in a vortex drier to obtain the anhydrous sodium acetate. The method can prevent the sodium acetate solution from being supercooled, avoids the processes with high energy consumption, such as brine cooling and the like, and does not need to add other crystal nuclei so as to avoid introducing impurities into the product. The vortex drier is used for drying by one step so as to avoid the complicated energy-consuming processes of vacuum concentration, crystallization by cooling, centrifugal separation, drying and the like in the prior production technique of anhydrous sodium acetate.
Description
(1) technical field
The present invention relates to a kind of method of producing sodium acetate trihydrate and anhydrous sodium acetate, especially the method for by-product sodium acetate trihydrate and sodium acetate when producing trimellitic acid 1,2-anhydride.Belong to the organic salt production technical field.
(2) background technology
Sodium acetate (being commonly called as sodium-acetate) can be as the esterifying agent of organic synthesis, and can be used for many aspects such as photographic chemical, medicine, printing and dyeing mordant, buffer reagent, meat are anticorrosion, pigment, tanning.When it is used as Snow Agent, light compared with salt to the infringement of road.It can relax unpleasant odor and prevent the seasonings variable color, and have certain mildew-proof function as the buffer reagent of seasonings.It also can be used for producing some Chemicals, as: furfuracrylic acid and Mono Chloro Acetic Acid etc.Sodium acetate trihydrate is a kind of common chemical reagent.Anhydrous sodium acetate can be divided into pharmaceutical grade, food grade and technical grade etc. again.
Industrial production sodium acetate generally carries out replacement(metathesis)reaction with lime acetate and soda ash etc., and the sodium acetate solution of generation after filtration, can obtain sodium acetate trihydrate behind concentrated, the crystallisation by cooling of filtrate, centrifugation.Then generally the crystallization sodium acetate need to be melted again during from sodium acetate trihydrate anhydrous sodium acetate processed, through the process such as centrifugation, drying again behind the vacuum concentration, crystallisation by cooling.
Chinese patent CN101139280A has described and has utilized several chemical reagent to carry out metathesis or neutralization reaction is produced sodium acetate soln, after heating is closely done, use water dissolution, decolour with activated carbon adsorption, again solution is heated to 120～130 ℃ after the filtration, carries out concentrating under reduced pressure, cool off crystallization, obtain the method for medical sodium acetate, anhydrous after the drying.It is high that the method adopts chemical reagent to prepare the anhydrous sodium acetate cost, the competitive power that does not have suitability for industrialized production, prepare anhydrous sodium acetate from sodium acetate solution or sodium acetate trihydrate and need to pass through the processes such as concentrating under reduced pressure, cooling crystallization, drying, step is many, and energy consumption is high.And the main purpose of the method is to obtain medical sodium acetate, anhydrous, is not to be sodium acetate trihydrate.Because under normal pressure, sodium acetate trihydrate will lose crystal water in the time of 123 ℃, to be evaporated to what obtain when doing under 120～130 ℃ be the mixture of the not high sodium acetate trihydrate of purity and anhydrous sodium acetate in fact so the method is being about to reaction solution after the replacement(metathesis)reaction, rather than said Sodium acetate trihydrate in this patent.Thereafter being dissolved in water again, adding what obtain after the purification step such as activated carbon adsorption decolouring, filtration also only is the aqueous solution of sodium acetate, and then the aqueous solution from sodium acetate directly removes to make the higher anhydrous sodium acetate of purity.
Chinese patent CN1014922362A has described a kind of method of the mother liquor by-product large-particle sodium acetate that contains acetic acid of the 5-of utilization Nitrofulral diacetate, the technical scheme of taking is: with mother liquor distill, add the soda ash neutralization, decolouring, press filtration, concentrating under reduced pressure, adjusting acidity of proportional quantity, with the tap water cooling, be cooled to 5～10 ℃ with icy salt solution again, make the sodium-acetate crystallization abundant, then after centrifugation, obtain oarse-grained sodium-acetate.The problem of a maximum of the method is exactly because sodium acetate has surfusion in crystallisation process, is difficult to crystallization and goes out larger particle, so have to adopt the very large icy salt solution of energy consumption by sodium acetate solution crystallization under 5～10 ℃ temperature.The method does not relate to the process that obtains anhydrous sodium acetate from sodium acetate hydrate drying.
Industrial being dissolved in unsym-trimethyl benzene carried out liquid-phase oxidation production trimellitic acid 1,2-anhydride in the acetic acid.At oxidation operation, when the rear oxidation tower is finished in oxidation from 2.3MPa pressure release discharge, must have part acetic acid with exhaust emissions out.If this tail gas is directly emptying, acidity is very large, and tart flavour is dense, and is very large to surrounding environment influence.Therefore need to wash first tail gas with water, the most of acetic acid in the gas phase is forwarded in the liquid phase, after concentrate, flash distillation, realize the reuse of acetic acid, the acetic acid of remainder also will carry out spray-absorption with liquid caustic soda in the gas phase, is translated into sodium acetate solution.
(3) summary of the invention
The object of the invention is to overcome some shortcomings in existing sodium acetate trihydrate and the anhydrous acetic acid process for producing sodium, provide a kind of and can obtain easily sodium acetate trihydrate, can make the by-product sodium acetate trihydrate of anhydrous sodium acetate and the method for anhydrous sodium acetate from sodium acetate trihydrate very simply again.
The object of the present invention is achieved like this: a kind of sodium acetate solution that by-product in the trimellitic acid 1,2-anhydride production process is obtained is further processed the method that makes sodium acetate trihydrate and anhydrous sodium acetate, and described method mainly comprises following technological processs:
Step 1, getting the sodium acetate solution of the degree Beaume that by-product obtains in trimellitic acid 1,2-anhydride or other process of producing product 〉=12 ° of B é, pour in the batching kettle, stir, is 6～9 with its neutralization to pH with glacial acetic acid, and the sodium acetate solution after then will neutralizing pumps into evaporating kettle;
Step 2 ,-0.08～-evaporate under the vacuum of 0.04MPa and 80～110 ℃ the temperature, make sodium acetate solution concentrated, until from visor, can be observed when having solid particulate to separate out in the still liquid stopped heating;
Step 3, evaporating kettle let out vacuum after, concentrated sodium acetate solution is changed in the crystallization kettle, open and stir, with recirculated cooling water it is cooled off, when the temperature of sodium acetate solution drops to (60～57) ℃, add the sodium acetate trihydrate crystal of solution quality 0.05～0.5% in the still, then allow sodium acetate solution continue to be cooled to below 40 ℃, allow concentrated solution keep being stirred in more than the 12h, make grain growth wherein, and make the crystal of separating out in the still be unlikely to the precipitation caking;
Step 4, the material after utilizing gravity with crystallization change whizzer over to, carry out centrifugation, the solid phase that obtains namely is sodium acetate trihydrate, and after the centrifugal mother liquor of telling and the sodium acetate solution newly fetched merge, proceeds sodium acetate trihydrate evaporation, crystallization and the centrifugal process of next round;
Step 5 only needs sodium acetate trihydrate is changed in the cyclone drying machine if further make anhydrous sodium acetate, carries out drying under 120～130 ℃ temperature.
In step 5, if sodium acetate trihydrate storage period is long or heap causes caking after pressing, the crusher that available cyclone drying machine carries carries out drying behind the fragment again.
The massfraction of the sodium acetate trihydrate that makes with this method 〉=99.0%, the massfraction of anhydrous sodium acetate 〉=98.0% can satisfy the service requirements of downstream industry.
Compared with prior art, the present invention has following advantages:
1) with the acetic acid of by-product in the major product production process with sprays such as liquid caustic soda, absorb after, not only solved the environmental issue in the major product production process, and will can make sodium acetate trihydrate or anhydrous sodium acetate after the sodium acetate solution processing, and production cost is very low, and product has price competitiveness.
During 2) with concentrated sodium acetate solution crystallization, when solution cools to (60～57) ℃, add a small amount of sodium acetate trihydrate crystal as crystal seed, can prevent that sodium acetate solution is excessively cold, avoid adopting the larger processes of power consumption such as brine refrigeration, and need not add other nuclear material, avoid in product, introducing impurity.
3) the process of cooling time longer, and keep solution to be in whipped state, can be so that crystal grain looks larger, crystal grain is more even, and is unlikely to precipitation caking in still.This both can have been avoided in follow-up blowing process can preventing again tiny crystal grain disperse in the cloth eye of centrifuge filtering cloth by larger caking blocking pipe, so that centrifugal more thorough, do not need drying can obtain satisfactory sodium acetate trihydrate.
4) adopt the whirlwind dryer to prepare anhydrous sodium acetate, can save behind vacuum concentration, the crystallisation by cooling the more complicated process such as centrifugation, drying, thereby also avoided a large amount of energy consumptions of intensification-cooling-again intensification-lower the temperature again.
(4) embodiment
Step 1, the 3000kg degree Beaume that by-product in the trimellitic acid 1,2-anhydride production process is obtained are that the sodium acetate solution of 18 ° of B é is poured in the batching kettle, open and stir, and be 8 with its neutralization to pH with glacial acetic acid, the sodium acetate solution after then this being neutralized pumps into evaporating kettle;
Step 2, evaporate under-the vacuum of 0.07MPa, 92～96 ℃ temperature, make it concentrated, when having solid particulate matter to separate out when observe still liquid from visor in, stopped heating judges that according to liquid level the total mass of solution in the still is about 1200kg;
Step 3, evaporating kettle let out vacuum after, concentrated sodium acetate solution is changed in the crystallization kettle, open and stir, with recirculated cooling water it is cooled off, when the temperature of sodium acetate solution drops to 58 ℃, add 1kg sodium acetate trihydrate crystal, then allow sodium acetate solution continue to be cooled to 35 ℃, allow concentrated solution keep stirring 20h, make grain growth wherein, and make the crystal of separating out in the still be unlikely to the precipitation caking;
Valve at the bottom of step 4, the unlatching crystallization kettle still, material after utilizing gravity with crystallization changes whizzer over to, carry out centrifugation, the solid that obtains namely is sodium acetate trihydrate, be total to 770kg, after testing, the massfraction of sodium acetate trihydrate is 99.1%, and after the centrifugal mother liquor of telling can merge with the next batch sodium acetate solution, proceed sodium acetate trihydrate evaporation, crystallization and the centrifugal process of next round;
Step 5,770kg sodium acetate trihydrate obtained above is changed in the cyclone drying machine, carry out drying under 123～125 ℃, obtain the anhydrous sodium acetate of 458kg, after testing, its massfraction is 98.5%.
Claims (1)
1. the method for a by-product sodium acetate trihydrate and anhydrous sodium acetate, it is characterized in that: described method comprises following technological process:
Step 1, getting the sodium acetate solution of the degree Beaume that by-product obtains in the trimellitic acid 1,2-anhydride production process 〉=12 ° B é, pour in the batching kettle, stir, is 6～9 with its neutralization to pH with glacial acetic acid, and the sodium acetate solution after then will neutralizing pumps into evaporating kettle;
Step 2 ,-0.08～-evaporate under the vacuum of 0.04MPa and 80～110 ℃ the temperature, make sodium acetate solution concentrated, until from visor, observe when having solid particulate to separate out in the still liquid stopped heating;
Step 3, evaporating kettle let out vacuum after, concentrated sodium acetate solution is changed in the crystallization kettle, open and stir, with recirculated cooling water it is cooled off, when the temperature of sodium acetate solution drops to 60～57 ℃, add the sodium acetate trihydrate crystal of solution quality 0.05～5% in the still, then allow sodium acetate solution continue to be cooled to below 40 ℃, allow concentrated solution keep being stirred in more than the 12h, make grain growth wherein, and make the crystal of separating out in the still be unlikely to the precipitation caking;
Step 4, change the material after the crystallization over to whizzer, carry out centrifugation, the solid phase that obtains namely is sodium acetate trihydrate, and after the centrifugal mother liquor of telling and the sodium acetate solution newly fetched merge, proceeds sodium acetate trihydrate evaporation, crystallization and the centrifugal process of next round;
Step 5 changes sodium acetate trihydrate in the cyclone drying machine over to if further make anhydrous sodium acetate, carries out drying under 120～130 ℃ temperature.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102617324B (en) * | 2012-02-24 | 2014-01-08 | 浙江金科过氧化物股份有限公司 | Crystal size controllable continuous crystallization process of sodium acetate trihydrate |
| CN104788306B (en) * | 2015-04-20 | 2016-07-06 | 江苏兄弟维生素有限公司 | A kind of synthesis technique of pharmaceutical grade anhydrous sodium acetate |
| CN109734582B (en) * | 2019-01-18 | 2019-12-10 | 台山市新宁制药有限公司 | Production process of sodium acetate |
| CN110845324B (en) * | 2019-11-18 | 2022-04-26 | 浙江伊诺环保科技股份有限公司 | Preparation process of sodium acetate trihydrate |
| CN114539049B (en) * | 2022-04-06 | 2024-01-26 | 衡阳市建衡实业有限公司 | Sodium acetate production process |
| CN116003362A (en) * | 2022-12-29 | 2023-04-25 | 河北海力恒远新材料股份有限公司 | Method for treating acetic anhydride dehydration waste liquid generated by 3,3', 4' -diphenyl ether dianhydride dehydration process |
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| CN1762954A (en) * | 2005-07-13 | 2006-04-26 | 杨正学 | Furfural waste water disposal method capable of producing acetone |
| CN101092343A (en) * | 2007-07-19 | 2007-12-26 | 江苏大康实业有限公司 | Method for preparing cobalt acetate |
| CN101337953A (en) * | 2008-08-14 | 2009-01-07 | 河南宏业化工有限公司 | Method for producing furfural by cleaning hydrolysis of biomass |
| CN101492362A (en) * | 2008-01-25 | 2009-07-29 | 山东方兴科技开发有限公司 | Production process for large-particle sodium acetate |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4002648A (en) * | 1973-07-16 | 1977-01-11 | Standard Oil Company (Indiana) | Catalyzed trans-acidolysis reaction of trimellitic acid, trimellitic anhydride and 2-naphthoic acid |
| CN1762954A (en) * | 2005-07-13 | 2006-04-26 | 杨正学 | Furfural waste water disposal method capable of producing acetone |
| CN101092343A (en) * | 2007-07-19 | 2007-12-26 | 江苏大康实业有限公司 | Method for preparing cobalt acetate |
| CN101492362A (en) * | 2008-01-25 | 2009-07-29 | 山东方兴科技开发有限公司 | Production process for large-particle sodium acetate |
| CN101337953A (en) * | 2008-08-14 | 2009-01-07 | 河南宏业化工有限公司 | Method for producing furfural by cleaning hydrolysis of biomass |
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Address after: 214422, Jianshe Road, Jiangsu Province, Jiangyin Town, No. 55 Co-patentee after: Nantong hundred Sichuan new materials Co., Ltd. Patentee after: Jiangsu hundred Sichuan high science and technology new materials Limited by Share Ltd Address before: 214422, Jianshe Road, Jiangsu Province, Jiangyin Town, No. 55 Co-patentee before: Baichuan Chemical (Rugao) Co., Ltd. Patentee before: Wuxi Baichuan Chemical Industrial Co., Ltd. |