CN101007640A - Method for preparing large grain anhydrous sodium sulfate - Google Patents
Method for preparing large grain anhydrous sodium sulfate Download PDFInfo
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- CN101007640A CN101007640A CNA2007100614484A CN200710061448A CN101007640A CN 101007640 A CN101007640 A CN 101007640A CN A2007100614484 A CNA2007100614484 A CN A2007100614484A CN 200710061448 A CN200710061448 A CN 200710061448A CN 101007640 A CN101007640 A CN 101007640A
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- sodium sulfate
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- anhydrous sodium
- large grain
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Abstract
The invention discloses a making method of large-particle anhydrous sodium sulfate, which comprises the following steps: adding 0.01%-10% surface activator with one or more of dodecyl phosphate ester, dodecyl sodium benzosulfonate, dodecyl dimethyl amine oxide, phenylethene or carbowax; adding water under 60-260 deg.c; keeping the constant density of solution to react 1.5-3.0h; stopping heating; filtering; drying; obtaining 80% product over 40 order.
Description
Technical field
The present invention relates to a kind of preparation method of large grain anhydrous sodium sulfate, belong to chemosynthesis purification techniques field.
Background technology
Sodium sulfate anhydrous.min(99) formal name used at school anhydrous sodium sulphate is mainly used in washing composition, Sodium Sulphide, and bubble flower alkali, papermaking, glass, weaving, printing and dyeing vinylon is used as the toxinicide of laxative and barium salt poisoning etc. in the medicine industry.Very big to its demand both at home and abroad, but supply exceed demand always for general granularity Sodium sulfate anhydrous.min(99), and price also constantly descends but in recent years,, oarse-grained Sodium sulfate anhydrous.min(99) (anhydrous sodium sulphate) is but with its high purity, low solubility, advantages such as easy electrolysis are as the solar energy heat-storage material, the preparation cement early strength agent, and produce vitriolate of tartar etc. and supply falls short of demand, and price also is higher than general particulate Sodium sulfate anhydrous.min(99), and its market outlook are boundless.
At present the hot method production technique of domestic most employing promptly the saturated nitre liquid that makes by saltcake through purifying treatment, send into the vaporizer heating evaporation, when concentration is raised to 40%-50%, carry out thickening by wet cyclone, again after filtration, dry, can obtain the finished product Sodium sulfate anhydrous.min(99), from the Sodium sulfate anhydrous.min(99) production technique as can be seen, the size of granularity mainly is big or small decision of sodium sulfate crystal that the time is formed by evaporation, so the granularity of product is little.In order to produce large grain anhydrous sodium sulfate, the producer's control degree of supersaturation that has, reduction-effect (first stage of evaporation, be equivalent to first reactor) heating chamber pressure and increase quadruple effect evaporator room vacuum tightness, the concentration of strict clear solution, control row nitre solid-to-liquid ratio reduces the rotating speed of recycle pump etc., granularity increases to some extent, 120 orders above 75%; Reduce the speed of circulation of evaporation unit, evaporation capacity.Also have pass through to change change pH values 6-8 the time granularity increase to some extent; The enterprise that has changes feed way, and evaporation if adopt unsaturated solution (clear solution) to evaporate, then can obtain the product of larger particles at the beginning, and drying plant is changed to sulfuration bed or microwave drying.Above technological improvement has increased the granularity of Sodium sulfate anhydrous.min(99) to a certain extent, but all can not satisfy industrial requirements, and above technological transformation, has all changed original production technique and equipment, and cost is increased, and complicated operation.
Summary of the invention
The object of the present invention is to provide a kind of apparatus and process that do not change, only add a spot of tensio-active agent, prepare the method for large grain anhydrous sodium sulfate,, to the control of Sodium sulfate anhydrous.min(99) crystal formation, improve competitiveness of product in high quality to realize low cost.
The object of the present invention is achieved like this: the preparation method of this large grain anhydrous sodium sulfate, its feature comprises: the tensio-active agent that adds 0.01%-10% in the crystallisation process of saturated metabisulfite solution: 1-isobutyl-3,5-dimethylhexylphosphoric acid, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, vinylbenzene or polyoxyethylene glycol wherein one or more, adding water under temperature 60-260 ℃ condition keeps strength of solution constant, reacted 1.5-3.0 hour, stop heating, filtration, drying obtain accounting for more than 40 orders 80% large grain anhydrous sodium sulfate.
The preparation method of described large grain anhydrous sodium sulfate, its concrete technical characterictic is: stirring under the linear velocity 5m/s, in the metabisulfite solution 1000mL of 320g/L, add the 1-isobutyl-3,5-dimethylhexylphosphoric acid and the Sodium dodecylbenzene sulfonate mixture 0.064g that account for sodium sulfate weight 0.02%, the two mass ratio is 1: 1; Heating makes homo(io)thermism at 60 ℃, constantly adds entry in the reaction process to keep the constant concentration of solution; Behind the stirring reaction 1.5 hours, stop heating, solution is discharged, suction filtration is drying to obtain.
The preparation method of described large grain anhydrous sodium sulfate, its concrete technical characterictic is: stirring under the linear velocity 2m/s, in the metabisulfite solution 1000mL of 320g/L, add the vinylbenzene and the polyoxyethylene glycol mixture 3.2g that account for sodium sulfate weight 1%, the two mass ratio is 1: 1; Heating makes homo(io)thermism at 150 ℃, constantly adds entry in the reaction process to keep the constant concentration of solution; Behind the stirring reaction 2.0 hours, stop heating, solution is discharged, suction filtration is drying to obtain.
The preparation method of described large grain anhydrous sodium sulfate, its concrete technical characterictic is: stirring under the linear velocity 5m/s, in the metabisulfite solution 1000mL of 320g/L, add the dimethyl dodecyl amine oxide 1.6g that accounts for sodium sulfate weight 0.5%; Heating makes homo(io)thermism at 260 ℃, constantly adds entry in the reaction process to keep the constant concentration of solution; Behind the stirring reaction 2.0 hours, stop heating, solution is discharged, suction filtration is drying to obtain.
The preparation method of large grain anhydrous sodium sulfate provided by the invention, its theoretical foundation is to add tensio-active agent to make that increase the inductive phase of nucleation significantly in the evaporative process, under the certain condition of degree of supersaturation and stirring velocity, can increase the interfacial energy of crystal and solution significantly, thereby effectively reduce nucleation rate, created the most basic condition for generating macrocrystal.Add tensio-active agent in addition and also have the surface tension that reduces solution, change the wettability of plane of crystal, the steady sector width that is situated between is increased, can grow fast for crystal and create essential condition.
The present invention does not change apparatus and process, only adds a spot of tensio-active agent, for producer saves cost greatly, is on a good wicket in the like product competition.Used tensio-active agent all is common tensio-active agent, and price is not high, and consumption is also few.The Tc scope of application of the present invention is wide, and gained sodium sulphate content of the present invention is greater than 99.6%, and chloride ion content is less than 0.1%, calcium-magnesium content is less than 0.001%, and whiteness is greater than 80, no caking phenomenon, what product granularity 40 orders were above accounts for 80%, can satisfy industrial requirements fully.Existing Sodium sulfate anhydrous.min(99) manufacturing enterprise can make the transition according to the market requirement easily, for suitability for industrialized production large grain anhydrous sodium sulfate product provides a good selection.
Embodiment
Embodiment 1
The metabisulfite solution 1000mL of preparation 320g/L adds in the small-sized simulative generator, under the low whipping speed 5m/s, begins heating; Add the 1-isobutyl-3,5-dimethylhexylphosphoric acid and the Sodium dodecylbenzene sulfonate mixture 0.064g that account for sodium sulfate weight 0.02%, the two mass ratio is 1: 1; Homo(io)thermism is at 60 ℃.Constantly add entry in the reaction process to keep the constant concentration of solution; React after 1.5 hours, stop heating, solution is discharged, suction filtration is drying to obtain product.
Embodiment 2
The metabisulfite solution 1000mL of preparation 320g/L joins in the small-sized simulative generator, under the low whipping speed 2m/s, begins heating; Add the vinylbenzene and the polyoxyethylene glycol mixture 3.2g that account for sodium sulfate weight 1%, the two mass ratio is 10: 1; Homo(io)thermism is at 150 ℃.Constantly add entry in the reaction process to keep the constant concentration of solution; React after 2 hours, stop heating, solution is discharged, carry out suction filtration, be drying to obtain product then.
Embodiment 3
The metabisulfite solution 1000mL of preparation 320g/L joins in the small-sized simulative generator, under the low whipping speed 0.5m/s, begins heating; Add the dimethyl dodecyl amine oxide 1.6g that accounts for sodium sulfate weight 0.5%; Homo(io)thermism is at 260 ℃.Constantly add entry in the reaction process to keep the constant concentration of solution; React after 2 hours, stop heating, solution is discharged, carry out suction filtration, be drying to obtain product then.
Embodiment 4
The metabisulfite solution 1000mL of preparation 320g/L joins in the small-sized simulative generator, under the low whipping speed 2m/s, begins heating; Adding accounts for the AES of sodium sulfate weight 10% and the mixture 32g of S-11, and the two mass ratio is 1: 10; Homo(io)thermism is at 120 ℃.Constantly add entry in the reaction process to keep the constant concentration of solution; React after 3 hours, stop heating, solution is discharged, carry out suction filtration, be drying to obtain product then.
The foregoing description can be according to the weight and the concentration of metabisulfite solution, adds the single of 0.01%-10% or complexed surfactant that both are mixed in proportion, as 1-isobutyl-3,5-dimethylhexylphosphoric acid, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, TX-10, OP-10, AES, S-11, vinylbenzene, ethylene glycol bis stearic acid, polyoxyethylene glycol etc., blended ratio are 1: 10-10: 1.
Listed examples of the present invention is intended to further illustrate utilizes tensio-active agent control crystal growth to prepare the method for large grain anhydrous sodium sulfate, and protection scope of the present invention is not constituted any restriction.All can obtain large grain anhydrous sodium sulfate with the embodiment of the invention with via claims 1-4 of the present invention.
Claims (4)
1, a kind of preparation method of large grain anhydrous sodium sulfate, its feature comprises: the tensio-active agent that adds 0.01%-10% in the crystallisation process of saturated metabisulfite solution: 1-isobutyl-3,5-dimethylhexylphosphoric acid, Sodium dodecylbenzene sulfonate, dimethyl dodecyl amine oxide, vinylbenzene or polyoxyethylene glycol wherein one or more, adding water under temperature 60-260 ℃ condition keeps strength of solution constant, reacted 1.5-3.0 hour, stop heating, filtration, drying obtain accounting for more than 40 orders 80% large grain anhydrous sodium sulfate.
2, the preparation method of large grain anhydrous sodium sulfate according to claim 1, it is characterized in that: stirring under the linear velocity 5m/s, in the metabisulfite solution 1000mL of 320g/L, add the 1-isobutyl-3,5-dimethylhexylphosphoric acid and the Sodium dodecylbenzene sulfonate mixture 0.064g that account for sodium sulfate weight 0.02%, the two mass ratio is 1: 1; Heating makes homo(io)thermism at 60 ℃, constantly adds entry in the reaction process to keep the constant concentration of solution; Behind the stirring reaction 1.5 hours, stop heating, solution is discharged, suction filtration is drying to obtain.
3, the preparation method of large grain anhydrous sodium sulfate according to claim 1, it is characterized in that: stirring under the linear velocity 2m/s, in the metabisulfite solution 1000mL of 320g/L, add the vinylbenzene and the polyoxyethylene glycol mixture 3.2g that account for sodium sulfate weight 1%, the two mass ratio is 1: 1; Heating makes homo(io)thermism at 150 ℃, constantly adds entry in the reaction process to keep the constant concentration of solution; Behind the stirring reaction 2.0 hours, stop heating, solution is discharged, suction filtration is drying to obtain.
4, the preparation method of large grain anhydrous sodium sulfate according to claim 1 is characterized in that: stirring under the linear velocity 5m/s, in the metabisulfite solution 1000mL of 320g/L, add the dimethyl dodecyl amine oxide 1.6g that accounts for sodium sulfate weight 0.5%; Heating makes homo(io)thermism at 260 ℃, constantly adds entry in the reaction process to keep the constant concentration of solution; Behind the stirring reaction 2.0 hours, stop heating, solution is discharged, suction filtration is drying to obtain.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100614484A CN100450929C (en) | 2007-01-22 | 2007-01-22 | Method for preparing large grain anhydrous sodium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100614484A CN100450929C (en) | 2007-01-22 | 2007-01-22 | Method for preparing large grain anhydrous sodium sulfate |
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| Publication Number | Publication Date |
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| CN101007640A true CN101007640A (en) | 2007-08-01 |
| CN100450929C CN100450929C (en) | 2009-01-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2007100614484A Expired - Fee Related CN100450929C (en) | 2007-01-22 | 2007-01-22 | Method for preparing large grain anhydrous sodium sulfate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942809A (en) * | 2012-11-23 | 2013-02-27 | 和昌（广西）化工有限公司 | Preparation method for superfine anhydrous sodium sulphate containing organic dopants |
| CN106745081A (en) * | 2015-11-23 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | A kind of production method of large grain anhydrous sodium sulfate |
| CN106745080A (en) * | 2015-11-23 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | The anticaking agent and preparation method of a kind of glauber salt |
| CN106752088A (en) * | 2015-11-24 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | A kind of production method of superfine modified anhydrous sodium sulphate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1128104C (en) * | 2001-08-13 | 2003-11-19 | 南风集团淮安元明粉有限公司 | Automatic control method of sodium sulfate production line |
-
2007
- 2007-01-22 CN CNB2007100614484A patent/CN100450929C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942809A (en) * | 2012-11-23 | 2013-02-27 | 和昌（广西）化工有限公司 | Preparation method for superfine anhydrous sodium sulphate containing organic dopants |
| CN106745081A (en) * | 2015-11-23 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | A kind of production method of large grain anhydrous sodium sulfate |
| CN106745080A (en) * | 2015-11-23 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | The anticaking agent and preparation method of a kind of glauber salt |
| CN106752088A (en) * | 2015-11-24 | 2017-05-31 | 湖南衡阳新澧化工有限公司 | A kind of production method of superfine modified anhydrous sodium sulphate |
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| CN100450929C (en) | 2009-01-14 |
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