CN1071297C - Solid sodium alcoholate producing process from liquid sodium alcoholate - Google Patents
Solid sodium alcoholate producing process from liquid sodium alcoholate Download PDFInfo
- Publication number
- CN1071297C CN1071297C CN98110297A CN98110297A CN1071297C CN 1071297 C CN1071297 C CN 1071297C CN 98110297 A CN98110297 A CN 98110297A CN 98110297 A CN98110297 A CN 98110297A CN 1071297 C CN1071297 C CN 1071297C
- Authority
- CN
- China
- Prior art keywords
- sodium
- liquid
- technology according
- ethanol
- solid sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a process for producing solid sodium alcoholate by liquid sodium alcoholate, which is characterized in that the liquid sodium alcoholate is evaporated, condensed and dried by a single step in closed drying equipment; vacuum degree is controlled within 0.09 to 0.1MPa; 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. Obtained solid sodium methoxide is white powder, sodium methoxide content reaches 90 to 95% and free alkali content is below 1.5%. Solid sodium ethoxide is white or yellowish powder, sodium ethoxide content reaches 85 to 90% and free alkali content is below 2.0%.
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.Since sodium alkoxide very easily with water reaction, 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 purpose of this invention is to provide the technology of being produced solid sodium ethanol by the liquid sodium alkoxide, 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, and the evaporation of liquid sodium alkoxide, concentrated, a dry step finish, and controlling vacuum tightness therebetween is 0.09～0.1MPa, solid sodium ethanol blowing to obtaining is packed then.
The liquid sodium alkoxide evaporates, concentrates, the temperature of control will be lower than 110 ℃ when dry, and under above-mentioned vacuum tightness, the boiling point that temperature is higher than the liquid sodium alkoxide generally at 50～110 ℃, is preferably in 90～110 ℃ at once, and being higher than 110 ℃ of materials can charing.
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, and alcohol otherwise cutting steam steams, 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: 1 bearing support, 2 supports, 3 steam-ins, 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
The evaporation of liquid sodium alkoxide, concentrate, dryly finish in stainless steel rake formula Vacuumdrier, rake formula Vacuumdrier has rake teeth and rolling bar (not shown) with superheated vapour chuck conduction heating in the kiln, and 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 0.09MPa1 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 80～110 ℃, but can not surpass 110 ℃, otherwise material can charing.Vacuum degree control is at 0.02MPa, and according to going out alcohol amount control vacuum tightness, the equal vacuum degree reaches 0.097MPa, no longer includes alcohol and steams, begin cooling, when being cooled to 25～28 ℃, the beginning inflated with nitrogen, solid sodium ethanol can not be contacted with atmosphere, and nitrogen can only be charged to normal pressure for extremely, finishes 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%.
Advantage of the present invention:
Process, the solid sodium ethanol content height that obtains, free alkali content is low. Thereby reduced transportation Expense has made things convenient for transportation, has shortened user's production cycle, has obvious economic benefit and society's effect Benefit. Through on probation, in the production of sulfamethoxine, producing every batch of sulfamethoxine needs liquid ethanol sodium 700kg, (be 4480 yuan by present price), and only need 140kg (2800 with solid sodium ethanol Unit), shorten 5～6 hours production cycles.
Solid sodium methylate is white powder, and sodium methoxide content reaches 90～95%, free alkali content≤ 1.5%. Solid sodium ethanol is white or pale yellow powder, and caustic alcohol content reaches 85～90%, trip From alkali content≤2.0%.
Claims (10)
1, a kind of technology of producing solid sodium ethanol by the liquid sodium alkoxide is characterized in that in close drying equipment, and the evaporation of liquid sodium alkoxide, concentrated, a dry step finish, and controlling vacuum tightness therebetween is 0.09～0.1MPa, then to the solid sodium ethanol blowing, and packing.
2, technology according to claim 1 is characterized in that liquid sodium alkoxide evaporation, concentrates, the exsiccant temperature is 50～110 ℃.
3, technology according to claim 2 is characterized in that liquid sodium alkoxide evaporation, concentrates, the exsiccant temperature is 90～110 ℃.
4, technology according to claim 1 and 2 is characterized in that lowering the temperature before the solid sodium ethanol blowing, charges into nitrogen to normal pressure, then the blowing packing.
5, technology according to claim 4 is characterized in that before the solid sodium ethanol blowing that temperature is reduced to 25～28 ℃ or its inflated with nitrogen when following.
6, technology according to claim 1 is characterized in that vacuum tightness controls to 0.09～0.1MPa from 0.01Mpa in close drying equipment.
7, technology according to claim 1 is characterized in that equipment used is preheated to 80～100 ℃ before the liquid sodium alkoxide feeds intake.
8, according to claim 1,6 or 7 described technologies, it is characterized in that equipment is stainless steel rake formula Vacuumdrier, in rake teeth and rolling bar are arranged.
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 |
|---|---|---|---|
| CN98110297A CN1071297C (en) | 1998-06-19 | 1998-06-19 | Solid sodium alcoholate producing process from liquid sodium alcoholate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98110297A CN1071297C (en) | 1998-06-19 | 1998-06-19 | Solid sodium alcoholate producing process from liquid sodium alcoholate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1239714A CN1239714A (en) | 1999-12-29 |
| CN1071297C true CN1071297C (en) | 2001-09-19 |
Family
ID=5220358
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98110297A Expired - Fee Related CN1071297C (en) | 1998-06-19 | 1998-06-19 | Solid sodium alcoholate producing process from liquid sodium alcoholate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1071297C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412659B (en) * | 2008-11-28 | 2012-06-06 | 曹衍军 | Production process of lithium alcoholate |
| CN103949155B (en) * | 2014-05-13 | 2016-05-18 | 武汉钢铁(集团)公司 | For reducing Cl-Ammonia process of desulfurization evaporative crystallization technique and the device of concentration |
| 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 |
| CN112337111A (en) * | 2020-09-18 | 2021-02-09 | 安徽金邦医药化工有限公司 | A desicator for producing sodium methoxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2104383B2 (en) * | 1971-01-30 | 1978-12-07 | Metallgesellschaft Ag, 6000 Frankfurt | |
| JPH0236138A (en) * | 1988-07-25 | 1990-02-06 | Toho Titanium Co Ltd | Production of high-purity alkoxybarium |
-
1998
- 1998-06-19 CN CN98110297A patent/CN1071297C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2104383B2 (en) * | 1971-01-30 | 1978-12-07 | Metallgesellschaft Ag, 6000 Frankfurt | |
| JPH0236138A (en) * | 1988-07-25 | 1990-02-06 | Toho Titanium Co Ltd | Production of high-purity alkoxybarium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1239714A (en) | 1999-12-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102875329B (en) | A kind of heat pump distillation is separated technique and the device of primary isoamyl alcohol isomers | |
| CN101734703A (en) | Device and method for preparing high-purity nano polyaluminium chloride with high efficiency, energy saving and environmental protection | |
| CN102294124B (en) | Spray drying method and device based on absorption heat pipe | |
| CN102847332A (en) | Steam condensate residual heat recovery process for vacuum flasher and recovery system thereof | |
| CN202860150U (en) | System for recycling afterheat of steam condensed water of vacuum flash tank | |
| CN1071297C (en) | Solid sodium alcoholate producing process from liquid sodium alcoholate | |
| CN105066602A (en) | Double-drying-chamber multifunctional drying device | |
| CN203525333U (en) | MVR (Mechanical Vapor Recompression) evaporator | |
| CN111039536A (en) | Energy-efficient sludge heat drying dewatering device | |
| CN207562379U (en) | A kind of absorption compression heat pump distillation system | |
| CN106672931A (en) | Method and equipment for producing polyphosphoric acid with wet process phosphoric acid | |
| CN1116261C (en) | Technological process producing high-purity sodium alcoholate from liquid sodium alcoholate | |
| CN207493230U (en) | A kind of steam condensation evaporation device | |
| CN210214856U (en) | Energy-efficient surplus aqueous ammonia distillation plant | |
| CN204944069U (en) | A kind of two drying chambers multifunctional drying apparatus | |
| CN109775789B (en) | Heat pipe vacuum drying system and application thereof | |
| CN107869857A (en) | One kind is based on the second kind absorption type mixing heat pump | |
| CN101550065B (en) | Energy-saving and water-saving type high-low pressure double-tower process for preparing dimethyl ether by rectifying methanol | |
| CN207193154U (en) | A kind of recycling treatment system of the recovery of the rectifying from ethanol, water and oily mixed liquor ethanol | |
| CN203922784U (en) | The two-way refining plant of the mixed bath of oilfield sewage and boiler smoke | |
| CN206276399U (en) | A kind of preparation system of giantreed biomass carbon adsorbent | |
| CN103060498A (en) | Blast furnace cinder flushing water residual heat power generation system | |
| CN207950711U (en) | Energy-saving methanol rectifying system | |
| CN206334364U (en) | Enclosed compression heat pump vapo(u)rization system | |
| CN106439766A (en) | Steam production device and direct compression type heat pump system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |