CN1116261C - Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate - Google Patents
Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate Download PDFInfo
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- CN1116261C CN1116261C CN 00111039 CN00111039A CN1116261C CN 1116261 C CN1116261 C CN 1116261C CN 00111039 CN00111039 CN 00111039 CN 00111039 A CN00111039 A CN 00111039A CN 1116261 C CN1116261 C CN 1116261C
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Abstract
The present invention relates to a process for producing high-purity solid sodium alcoholate using liquid sodium alcoholate, which is characterized in that the evaporation, the condensation and the drying of the liquid sodium alcoholate are completed by one step in closed drying equipment; a solvent is added into the closed drying equipment; vacuum degree is controlled within 0.09 to 0.1MPa and temperature is controlled within 110 to 200 DEG C; then, the obtained solid sodium alcoholate is discharged to be packaged; the solid sodium alcoholate is cooled before being discharged and nitrogen is filled for protection. The closed drying equipment is a stainless steel harrow type vacuum drier. The process is suitable for the production of sodium methoxide or sodium ethoxide. The obtained solid sodium methoxide is white powder, the sodium methoxide content reaches 96 to 98% and free alkali content is below 1.0%. Solid sodium ethoxide is white or yellowish powder, sodium ethoxide content reaches 96 to 98% and free alkali content is below 1.5%.
Description
The present invention relates to the production technique of a kind of solid sodium ethanol, particularly sodium methylate or sodium ethylate.
Sodium methylate or sodium ethylate are a kind of important organic synthesis intermediates, are widely used in industries such as medicine, chemical industry, agricultural chemicals, dyestuff.Because sodium alkoxide very easily reacts with water, domestic production producer produces liquid first, sodium ethylate.National Specification liquid methanol sodium be meant that sodium methylate content is at 27.5～35% methanol solution; Liquid ethanol sodium is meant that sodium ethylate content is at 16.5～23% ethanolic soln.Utilize liquid first, sodium ethylate not only to increase traffic capacity and trucking costs, and can prolong the production cycle of Application Areas.If can direct production solid sodium methylate and sodium ethylate, its economic and social benefit is conspicuous, can reduce trucking costs, shortens user's production cycle, save energy or the like.
The inventor in first to file, application number is 98110297.2, by the technology that the liquid sodium alkoxide is produced solid sodium ethanol, solved the problem of being produced solid sodium ethanol by the liquid sodium alkoxide, but the content of its solid sodium ethanol that obtains is up to 95%, can't practical requirement.
The purpose of this invention is to provide the technology of being produced the high-purity solid sodium alkoxide by the liquid sodium alkoxide, purity reaches more than 95%, and quality is good, and free alkali content is low, is particularly suitable for producing solid sodium methylate by liquid methanol sodium, and liquid ethanol sodium is produced solid sodium ethanol.
The present invention is produced the technology of solid sodium ethanol by the liquid sodium alkoxide, its major technique characteristics are in close drying equipment, the evaporation of liquid sodium alkoxide, concentrated, a dry step finish, add solvent therebetween, control vacuum tightness is 0.09～0.1MPa, temperature is 110～200 ℃, then to the solid sodium ethanol blowing, and packing.
The liquid sodium alkoxide evaporates, concentrates, the temperature height of control when dry, is preferably in 110～180 ℃.
Solvent of the present invention can be before the liquid sodium alkoxide begins crystallization to occur adding whenever.If add with raw material, contained the solvent height by in the alcohol that steams, the aftertreatment complexity, the cost height, effect is not best.Preferably disposable adding when the liquid sodium alkoxide begins crystallization to occur, it is more abundant, complete that alcohol in the crystalline sodium alkoxide is gradually proposed, and aftertreatment is simple.When the liquid sodium alkoxide began crystallization to occur, the amount that general alcohol is steamed was about 40% of liquid sodium alkoxide weight.The add-on of solvent is 22～25% of a liquid sodium alkoxide weight.
Solvent of the present invention can be not have reaction and dissolve pure alkanes solvent with raw material, preferably adopts hexanaphthene.
Temperature preferably was reduced to earlier about 50～120 ℃ of half an hour after the present invention added solvent, made sodium alkoxide and solvent thorough mixing even, was warming up to 110～200 ℃ then.
The characteristics of above-mentioned technology also are, the evaporation of liquid sodium alkoxide, concentrate, drying finishes, and when no longer including alcohol and steaming, begins cooling, charges into nitrogen to normal pressure, then the blowing packing.Preferably temperature is reduced to 25～28 ℃ or its when following, charges into nitrogen, because in whole technology, sodium alkoxide is isolated with air, so needs nitrogen protection before the blowing, and solid sodium ethanol easily catches fire simultaneously, must cooling back blowing.
The liquid sodium alkoxide is in evaporation, in the concentration process, alcohol otherwise cutting steam steams, and in order to make the abundant condensation when the recovery of the alcohol that steams, vacuum tightness preferably controls to 0.09～0.1MPa gradually from 0.01MPa in equipment.
Equipment used is preheated to 80～100 ℃ earlier before the liquid sodium alkoxide feeds intake.The one, prevent air admission, the liquid sodium alkoxide is evaporated immediately.
Technology of the present invention is suitable for the preparation of sodium methylate or sodium ethylate most, promptly produces solid sodium methylate by liquid methanol sodium, and liquid ethanol sodium is produced solid sodium ethanol.Also applicable to production as sodium propylate, sodium butylate.
Illustrate below in conjunction with embodiment:
Fig. 1 is the structural representation of stainless steel rake formula Vacuumdrier.
Among the figure: 4 vacuum meters, 5 discharge ports, 6 kilns, 7 condensation-water drains, 8 bases, 9 master wheels, 10 pinion(gear)s, 11 step-down gears, 12 motors, 13 vacuum pumps, 14 condensers, 15 fly-ash separators, 16,17 vacuum valves, 18 opening for feeds, 19 housings of 1 bearing support, 2 supports, 3 steam-ins
The evaporation of liquid sodium alkoxide, concentrate, dryly in stainless steel rake formula Vacuumdrier, finish.Rake formula Vacuumdrier has rake teeth and rolling bar (not shown) with superheated vapour chuck conduction heating in the kiln, its structure is a prior art.Rolling bar has two, can effectively the crystalline solid sodium ethanol be pulverized, and behind the solid sodium ethanol blowing, powder cooling rear surface temperature is more even, avoids catching fire.In order to increase the stopping property of rake formula Vacuumdrier better, graphite and tetrafluoroethylene mixed fillers can be adopted in the two ends of rake formula Vacuumdrier.The concrete operations step of this technology is as follows:
1, the stopping property of monitoring device: will harrow the formula Vacuumdrier and clear up the oven dry of reducing pressure only, negative pressure of vacuum remained on 0.09MPal hour, check that whether vacuum tightness is also at 0.09MPa, if any decline, also have leak source on the devices illustrated, must inspection can not feed intake to there being leak source.
2, equipment cleaning, drying: will harrow the formula Vacuumdrier and add water to completely, heated and boiled 0.5～1 hour, water is rinsed well again, carries out hot air dries then.
3, to harrow the formula Vacuumdrier when heating to 80～100 ℃, the liquid sodium alkoxide will be squeezed into pump from the vapor lamp on rake formula Vacuumdrier top is disposable, close the charging valve, begin to heat up, the vapor pressure of rake formula Vacuumdrier interlayer is controlled at 0.1～0.2MPa.
4, when rake formula Vacuumdrier begins alcohol, rake teeth is opened, after 2 hours, decompression, temperature is controlled at 110～200 ℃.Vacuum degree control is at 0.02MPa, and according to going out alcohol amount control vacuum tightness, vacuum tightness reaches 0.097MPa gradually, observe by the visor on the rake formula Vacuumdrier, when the liquid sodium alkoxide begins crystallization, the disposable solvent hexanaphthene of squeezing into, the amount of hexanaphthene is 22～25% of a liquid sodium alkoxide weight.Steam Deng no longer including alcohol, begin cooling, when being cooled to 25～28 ℃, the beginning inflated with nitrogen can not contact solid sodium ethanol with atmosphere, and nitrogen can only be charged to normal pressure for extremely, end by the gross.
5, beginning blowing, finished product packing.
This process liquid sodium alkoxide is meant the industrial goods of national standard, be that liquid methanol sodium is that sodium methylate content is 27.5～35%, the methanol solution of free alkali content≤0.05%, liquid ethanol sodium be sodium ethylate content 16.5～23%, the ethanolic soln of free alkali content≤0.05%.
The production of sodium ethylate: by above-mentioned technology, the evaporation, concentrated, dry in rake formula Vacuumdrier of the liquid ethanol sodium of 2400kg national standard when beginning crystallization to occur, adds the 600kg hexanaphthene, the solid sodium ethanol that obtains, and assay is as follows:
Sample for the first time: sodium ethylate content: 97.37%, free alkali sodium hydroxide: 1.06%
Sample for the second time: sodium ethylate content: 97.42%, free alkali sodium hydroxide: 1.20%
Advantage of the present invention:
Process, the solid sodium ethanol content height that obtains, free alkali content is low. Thereby reduced freight, made things convenient for fortune Fail, shortened user's production cycle, have obvious economic benefit and social benefit.
Solid sodium methylate is white powder, and sodium methoxide content reaches 96～98%, free alkali content≤1%. Solid sodium ethanol is White or pale yellow powder, caustic alcohol content reaches 96～98%, free alkali content≤1.5%.
Claims (10)
1, a kind of technology of producing the high-purity solid sodium alkoxide by the liquid sodium alkoxide, it is characterized in that in close drying equipment, the evaporation of liquid sodium alkoxide, concentrated, a dry step finish, add the alkanes solvent therebetween as solvent, control vacuum tightness is 0.09～0.1MPa, temperature is 110～200 ℃, then to the solid sodium ethanol blowing, and packing.
2, technology according to claim 1 is characterized in that solvent adds before the liquid sodium alkoxide begins crystallization to occur.
3, technology according to claim 1 is characterized in that solvent adds when the liquid sodium alkoxide begins crystallization to occur.
4, according to claim 1 or 3 described technologies, the add-on that it is characterized in that solvent is 22～25% of a liquid sodium alkoxide weight.
5,, it is characterized in that solvent is a hexanaphthene according to claim 1 or 2 or 3 described technologies.
6, technology according to claim 3, it is characterized in that adding solvent after temperature be reduced to 50～120 ℃ of half an hour earlier, be warming up to 110～200 ℃ then.
7, technology according to claim 1, inflated with nitrogen is to normal pressure when following to it is characterized in that before the solid sodium ethanol blowing temperature being reduced to 25～28 ℃ or its, and blowing is packed then.
8, technology according to claim 1 is characterized in that vacuum tightness controls to 0.09～0.1MPa gradually from 0.01MPa in equipment.
9, technology according to claim 1 is characterized in that sodium alkoxide is meant sodium methylate or sodium ethylate.
10, technology according to claim 9, it is characterized in that liquid methanol sodium is meant that sodium methylate content is 27.5～35%, the methanol solution of free alkali content≤0.05%, liquid ethanol sodium are meant sodium ethylate content 16.5～23%, the ethanolic soln of free alkali content≤0.05%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00111039 CN1116261C (en) | 2000-05-10 | 2000-05-10 | Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00111039 CN1116261C (en) | 2000-05-10 | 2000-05-10 | Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate |
Publications (2)
| Publication Number | Publication Date |
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| CN1322702A CN1322702A (en) | 2001-11-21 |
| CN1116261C true CN1116261C (en) | 2003-07-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 00111039 Expired - Fee Related CN1116261C (en) | 2000-05-10 | 2000-05-10 | Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105884578B (en) * | 2016-04-21 | 2018-11-27 | 赖明空 | A kind of method and device thereof of high temperature and pressure production sodium methoxide |
| CN106316789A (en) * | 2016-08-24 | 2017-01-11 | 安徽金邦医药化工有限公司 | Production process of solid sodium methoxide |
| CN106542967A (en) * | 2016-11-02 | 2017-03-29 | 宁夏佰斯特医药化工有限公司 | A kind of solid sodium methylate preparation method |
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