CN1059449C - Preparation method for high-viscosity chloromethyl polysulphone - Google Patents
Preparation method for high-viscosity chloromethyl polysulphone Download PDFInfo
- Publication number
- CN1059449C CN1059449C CN96107032A CN96107032A CN1059449C CN 1059449 C CN1059449 C CN 1059449C CN 96107032 A CN96107032 A CN 96107032A CN 96107032 A CN96107032 A CN 96107032A CN 1059449 C CN1059449 C CN 1059449C
- Authority
- CN
- China
- Prior art keywords
- reactor
- chloromethyl
- kettle cover
- polysulphone
- polysulfones
- 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
- Separation Using Semi-Permeable Membranes (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The present invention belongs to the technical field of a separation method of semipermeable membranes and a device thereof, which discloses a preparation method for chloromethyl polysulphone with the intrinsic viscosity being from 0.51 to 0.8. The method is characterized in that the proportion and the reaction time of polysulphone, dichloroethane, chloromethyl ether and zinc chloride are controlled, and the reaction temperature is controlled by an automatic temperature controller. A discharge device whose reaction vessel body can be lifted and reaction vessel cover is fixed is used for discharge. When materials are discharged, the vessel body is fallen down; when materials are fed in, the vessel body is lifted up. The present invention solves the problem for preparing high viscosity chloromethyl polysulphone which is used for preparing hollow fibers and flat membranes without supporters.
Description
The present invention relates to separation method and equipment thereof, particularly relate to separatory membrane, promptly be used for the preparation methods of fluid different molecular weight separating substances, belong to the method and the apparatus technology thereof of physics or chemistry with semi-permeable membranes.
Polysulfones becomes chloromethyl polysulphone behind chloromethylation, its chemical structure is
Chloro-methyl group-CH
2Cl is very active, takes place crosslinkedly easily, forms the bigger molecule of molecular weight, even is cross-linked into network, becomes the polymkeric substance that is insoluble to solvent.Take place for fear of this situation, adopting limiting viscosity during polymerization usually is the following polysulfones in η=0.5.But the chloromethyl polysulphone viscosity of making like this is low, can only make the film of band supporter, and can not be spun into hollow-fibre membrane and other not with the film of propping material.In addition, common discharging method is to stir discharging in boiling water, but this method is unsuitable for the discharging of high viscosity polysulfones chloromethylation afterreaction liquid, because of it is difficult for being stirred to fragmentate very easily to stick to being difficult on the stirring rod take off.Existing background technology has following patent documentation by retrieval, do not appear in the newspapers relevant with high-viscosity chloromethyl polysulphone with the method for preparing no support film and the technology of high-viscosity chloromethyl polysulphone discharging method.Relevant document such as CN1036588A, JP04283208, SU999547, BE1005983, SU548984, R0365054, BE905179 etc.
The objective of the invention is to overcome the defective of prior art, propose to be suitable for to prepare the preparation method of high-viscosity chloromethyl polysulphone of hollow-fibre membrane and other no support film and simple and easy to do discharging method.
The present invention is achieved in that
Be limiting viscosity that 0.51 to 0.8 polysulfones dried by the fire in 60 ℃ to 90 ℃ vacuum drying oven 20 to 40 hours; Zinc chloride dried by the fire in 110 ℃ to 140 ℃ vacuum drying oven 24 to 48 hours.
The weight ratio of polysulfones, ethylene dichloride, chloromethyl ether, zinc chloride is:
Polysulfones: ethylene dichloride: chloromethyl ether: zinc chloride=(0.8～1.2): (10～15): (0.8～1.2): (0.06～0.08)
The automatic temperature control instrument transmitter is being housed, in the heated reactor of prolong and stirrer, by said ratio, is putting into the polysulfones and the ethylene dichloride of 0.51 to 0.8 limiting viscosity earlier, room temperature is stirred to block and polysulfones was dissolved fully in 2-3 hour, puts into chloromethyl ether and zinc chloride then.Temperature of reaction is controlled at 50 ℃ to 60 ℃ by automatic temperature control instrument, reacts 4 to 10 hours.Reaction finishes and makes its naturally cooling.
The invention provides a width of cloth accompanying drawing, promptly Fig. 1 is chloromethyl polysulphone drawing mechanism figure.
Prepare discharging technology process in the chloromethyl polysulphone below in conjunction with description of drawings.Drawing mechanism as shown in Figure 1, this device mainly comprises: lifting table 1, ceramic heat pot with band heating of metal film is a reactor 2, the kettle cover 3 that has three mouths, temperature controller transmitter 5 is housed in the mouth 4 on the kettle cover 3 also to be fixed, another mouthful 7 on the kettle cover 3 be as the outlet of solvent and other chemical composition, and the 3rd mouth 8 on the kettle cover 3 is equipped with thermometer 9 and as dog-house, prolong 10 and solvent collection bottle 11.The locus of kettle cover 3 is with iron shelf and clamp 6 fixed, and reactor 2 is placed on the lifting table 1 and can be shifted up and down.
In reactor 2, inject 2/3 deionized water, water temperature by the temperature controller controlled temperature between 80 ℃ to 98 ℃.Reactor 2 risen to kettle cover 3 by lifting table 1 closely fasten.When water temperature reaches required value, drop into the chloromethyl polysulphone reaction solution slowly from dog-house 8.At this moment, ethylene dichloride, chloromethyl ether and less water become that gaseous state evaporates and condense into liquid state at prolong 10, flow in the solvent collection bottle 11.Chloromethyl polysulphone is separated out because of water insoluble.No longer including liquid in the receiving flask after spending 6-10 minute splashes into.Rotate the lifting table knob reactor is lowered, chloromethyl polysulphone is taken out, then kettle is gone up, drop into the chloromethyl polysulphone reaction solution again, carry out in proper order.
Block chloromethyl polysulphone is cut into fragment, with deionized water soak, flushing, place drier to dry, natural air drying uses vacuum drying oven in 20 ℃ of-40 ℃ of oven dry more then, is loaded in the plastics bag that band seals standby.
One embodiment below is provided.
0.63,80 ℃ of baking of polysulfones viscosity 24 hours.The weight ratio of each feed composition is:
Polysulfones: ethylene dichloride: chloromethyl ether: zinc chloride=1: 12: 0.9: 0.07
56 ℃ of temperature of reaction were reacted 8 hours.Water temperature is controlled at 95 ℃ by automatic temperature control instrument in the reactor 2, and every still discharging time is 8 minutes.Chloromethyl polysulphone baking material temperature is controlled at 30 ℃, adopts above-mentioned condition to prepare and is suitable for spinning tubular fibre and the chloromethyl polysulphone for preparing no supporting body flat-plate film.
Claims (3)
1. the preparation method of a high-viscosity chloromethyl polysulphone is characterized in that
Press following weight ratio ready reaction material:
Limiting viscosity is 0.51 to 0.8 polysulfones: ethylene dichloride: chloromethyl ether: zinc chloride=(0.8-1.2): (10-15): (0.8-1.2): (0.06-0.08);
Polysulfones was dried by the fire in 60 ℃ to 90 ℃ vacuum drying oven 20 to 40 hours, and zinc chloride dried by the fire in 110 ℃ to 140 ℃ vacuum drying oven 24 to 48 hours;
In the heated reactor (2) that is equipped with automatic temperature control instrument transmitter (5), prolong (10) and agitator, put into polysulfones and ethylene dichloride earlier, at room temperature stir and polysulfones was dissolved fully in 2-3 hour, putting into the pure and mild zinc chloride of chloromethane then reacts, by the automatic temperature control instrument control reaction temperature at 50 ℃ to 60 ℃, reacted 4 to 10 hours, reaction finishes and makes its naturally cooling;
Employing comprises the drawing mechanism discharging of lifting table (1) and reactor (2), dries with drier after the discharging, again with the vacuum drying oven oven dry, is loaded in the plastics bag that band seals standby.
2. method according to claim 1, it is characterized in that this drawing mechanism comprises: lifting table (1), the ceramic heat pot reactor (2) of band heating of metal film, the kettle cover (3) that has three mouths, wherein, equip and be fixed with temperature controller transmitter (5) in the mouth (4) on kettle cover (3), on the kettle cover (3) another mouthful (7) is as the outlet of solvent and other chemical compositions, the 3rd mouth (8) on the kettle cover (3) is equipped with thermometer (9) and as dog-house, prolong (10) and solvent collection bottle (11), the locus of kettle cover (3) is with iron shelf and clamp (6) fixed, and reactor (2) is placed on the lifting table (1), can move up and down.
3. according to claim 1,2 described methods, it is characterized in that
React the end back and in reactor (2), inject the deionized water of 2/3 volume, at 80 ℃ to 90 ℃, reactor (2) is raised to and the tight fastening of kettle cover (3) with lifting table (1) by the temperature controller control water temperature;
Slowly drop into the chloromethyl polysulphone reaction solution from dog-house (8), after spending 6-10 minute, it is fashionable to no longer include fluid drips in receiving flask (11), with lifting table (1) reactor (2) is lowered, the chloromethyl polysulphone of separating out is taken out, then kettle is gone up, dropped into the chloromethyl polysulphone reaction solution again, carry out in proper order;
The block chloromethyl polysulphone of results is cut into fragment, with deionized water soak, flushing, place drier to dry, natural air drying uses vacuum drying oven in 20 ℃ of-40 ℃ of oven dry more then, is loaded in the plastics bag that band seals standby.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96107032A CN1059449C (en) | 1996-07-08 | 1996-07-08 | Preparation method for high-viscosity chloromethyl polysulphone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96107032A CN1059449C (en) | 1996-07-08 | 1996-07-08 | Preparation method for high-viscosity chloromethyl polysulphone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1139679A CN1139679A (en) | 1997-01-08 |
| CN1059449C true CN1059449C (en) | 2000-12-13 |
Family
ID=5119476
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96107032A Expired - Fee Related CN1059449C (en) | 1996-07-08 | 1996-07-08 | Preparation method for high-viscosity chloromethyl polysulphone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1059449C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101875723B (en) * | 2009-04-30 | 2012-06-20 | 比亚迪股份有限公司 | Resin and preparation method thereof, and catalyst used for preparing biodiesel and preparation method thereof |
| CN104479146B (en) * | 2014-12-04 | 2017-06-23 | 杭州水处理技术研究开发中心有限公司 | A kind of post-processing approach of chloromethyl polysulphone |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4634742A (en) * | 1984-11-08 | 1987-01-06 | The B. F. Goodrich Company | Polyarylene polyethers with pendant vinyl groups and process for preparation thereof |
| JPH0487629A (en) * | 1990-07-30 | 1992-03-19 | Tokuyama Soda Co Ltd | Production of semipermiable dual film |
| JPH04227833A (en) * | 1990-05-18 | 1992-08-17 | Tokuyama Soda Co Ltd | Semipermeable composite membrane |
| JPH05228351A (en) * | 1992-02-17 | 1993-09-07 | Tokuyama Soda Co Ltd | Production of structure resistant to solvent |
-
1996
- 1996-07-08 CN CN96107032A patent/CN1059449C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4634742A (en) * | 1984-11-08 | 1987-01-06 | The B. F. Goodrich Company | Polyarylene polyethers with pendant vinyl groups and process for preparation thereof |
| JPH04227833A (en) * | 1990-05-18 | 1992-08-17 | Tokuyama Soda Co Ltd | Semipermeable composite membrane |
| JPH0487629A (en) * | 1990-07-30 | 1992-03-19 | Tokuyama Soda Co Ltd | Production of semipermiable dual film |
| JPH05228351A (en) * | 1992-02-17 | 1993-09-07 | Tokuyama Soda Co Ltd | Production of structure resistant to solvent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1139679A (en) | 1997-01-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100447316C (en) | Phase-change energy-storage ultra-fine composite fiber and preparation method and application thereof | |
| CN106800629B (en) | A kind of porous pyrenyl organic framework material and preparation method thereof of richness hydroxyl | |
| US20060124537A1 (en) | Pervaporation Membranes and Methods of Use | |
| CN109824906A (en) | A kind of preparation method of spinning-grade polycarbosilane precusor material | |
| CN102423505A (en) | Method and apparatus for fixing bioprosthetic valve by membrane type pervaporation mode | |
| CN1059449C (en) | Preparation method for high-viscosity chloromethyl polysulphone | |
| JPS5645704A (en) | Method and apparatus for removal of volatile substances from high-viscous substance | |
| CN111690138B (en) | Low-viscosity vinyl hydroxyl silicone oil and preparation method thereof | |
| CN109651649A (en) | A kind of graphene-based antioxidant and its preparation method and application | |
| CN102489178B (en) | Method for preparing molybdenum disulfide pervaporation membrane for separating alcohol-containing wastewater | |
| CN101259387A (en) | Controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane and preparation | |
| CN106111093A (en) | A kind of remove the preparation method of the hybridized film of copper ion in water | |
| CN111205200A (en) | Method and device for preparing heptafluoroisobutyronitrile | |
| CN103212314A (en) | Modified ZSM-5 zeolite blended ethanol-permselective composite membrane and preparation method thereof | |
| CN100577271C (en) | Method for preparing organic-inorganic hybridization anion exchange membrane based on co-polymer | |
| CN1049297A (en) | Microporous barrier | |
| CN109456602A (en) | A kind of microelectronic chip package thermal conducting material and preparation method thereof | |
| CN108299200A (en) | A kind of methyl acetoacetate clean preparation method | |
| CN108034069A (en) | A kind of phenylacetyl cellulose acetate ordered porous membrane material and preparation method thereof | |
| CN209188262U (en) | A kind of pore former extraction equipment | |
| WO2011060631A1 (en) | Temperature responsive membrane and preparation method thereof | |
| CN216658521U (en) | Epoxy resin encapsulating material production dispersion devices | |
| CN112341785B (en) | Polyethylene glycol/polyethyleneimine composite solid-solid phase change material and preparation thereof | |
| CN216410850U (en) | Full-automatic multi-station nitrogen blowing instrument | |
| CN114210133B (en) | Anti-ultraviolet filter bag and preparation method thereof |
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 |