CN106632749A - Novel method and special device for removing solvents from chlorosulfonated polyethylene adhesive liquid - Google Patents
Novel method and special device for removing solvents from chlorosulfonated polyethylene adhesive liquid Download PDFInfo
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- CN106632749A CN106632749A CN201710088635.5A CN201710088635A CN106632749A CN 106632749 A CN106632749 A CN 106632749A CN 201710088635 A CN201710088635 A CN 201710088635A CN 106632749 A CN106632749 A CN 106632749A
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- stainless steel
- chlorosulfonated polyethylene
- roller
- glue
- csm
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/38—Sulfohalogenation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
The invention relates to a novel method and a special device for removing solvents from chlorosulfonated polyethylene (CSM) adhesive liquid. Adhesive liquid films can be obtained by means of open type normal-pressure flash evaporation drying (instant solvent flash evaporation) and can be quickly cooled (for preventing yellowing). The novel method includes directly leading the adhesive liquid into the surfaces of open type metal double rolls after CSM is completely synthesized by the aid of solution processes; carrying out flash evaporation on the solvents by the aid of the instant high temperature and the normal pressure; quickly cooking the films by the aid of cooling rolls to obtain film-shaped CSM products. The novel method and the special device have the advantages that technical difficult problems in the aspect of sealing and technical difficult problems of easiness in local adhesive burning, adhesive twining, adhesive sticking and the like can be solved by the normal-pressure open type double-roll device, vacuum can be omitted, equipment is simple, the solvents are high in recycling rate, the novel method and the special device are high in drying efficiency and can be widely applied to drying heat-sensitive and high-adhesiveness substances such as chloroprene rubber, chlorinated natural rubber and CSM rubber, and the like.
Description
Technical field
The present invention relates to polymer solution desolvation technical field, particularly relates to a kind of chlorosulfonated polyethylene (CSM) glue
The new method of liquid desolvation-open, atmospheric flashing are dried glue film (solvent moment flash distillation), and gained glued membrane is cooled down rapidly
(anti-xanthochromia)；And describe the structure and parameter of special purpose device (open, normal pressure metal double roller flash dryer).
Background technology
After solwution method synthesis chlorosulfonated polyethylene (CSM), need that for solvent removal dry products could be obtained.Current glue
Liquid desolventizing is dried post-processing approach and is broadly divided into following three kinds：
(1) wet method water vapour air lift
This method is that glue is scattered in hot water, is blown into water vapour air lift and takes away solvent (such as CCl4), glue Jing one-pots or
Many kettle cohesions, cohesion blob of viscose and the dehydration of water Jing reciprocating sieves are washed again bis- grades of screw extrudings of Jing and are drying to obtain finished product CSM.The method water is followed
Circular rector is big, and energy consumption is big, the high (Cl remained in glue of acid/inorganic salt content in finished product glue2And SO2Run into cohesion hot water, reaction life
Hydrochloric acid and sulfuric acid, small part is embedded into the CSM of cohesion, in order to neutralize remaining acid, alkali, shape must be often added in recirculated water
Into salt), of poor quality, condition is poor.
(2) closed roller drying
This method is the closed cylinder surface that CSM glues are sprayed to heating, in vacuum (to reduce solvent boiling point), compared with low temperature
Solvent is evaporated under degree, polymer is separated out with film-form and is dried, this method is also traditional handicraft, strict sealing (ensures high
Vacuum) and locally paste glue is the law technology difficult problem.If solving sealing problem, this method can also be adopted.
(3) pre-concentration twin-screw dry method extrusion desolventizing
Drying means is typically completed in two steps, first glue is carried out into pre-concentration, is typically subtracted using thin film evaporation or spinneret
Pressure evaporation desolventizing carries out pre-concentration, makes glue content from 10% concentrate to 30%～50%, enters subsequently into double screw extruder
Row depth desolventizing is dried.This method two step of palpus can just complete thorough drying, and equipment investment is big.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of new CSM desolventizings technology and special purpose device.The technology
Using open type dual-roller surface, the solvent that rapid flash goes out in thin CSM liquid films under high temperature, normal pressure, while cooling down institute rapidly
CSM films (prevent turn yellow), one-step method obtains that outward appearance condition is good, and acid content is low, the measured CSM of matter.It is simple with equipment, it is molten
The agent rate of recovery is high, the advantage such as drying efficiency height.Can be widely applied to remove the easy volatile solvent in thermal sensitivity, high viscosity substance.
The double roller of one of such device core component-heating, is commonly used for before this drying of food, thermoplastic
Plasticizing and rubber are plasticated and the occasion such as knead.Here with the addition of the chill roll of key, this quick heat is cold change for
The quick desolventizing of CSM glue films and the quality control of CSM films, it is most important.
To realize the goal of the invention of the present invention, adopt the following technical scheme that：
A kind of new technology of CSM glues desolvation --- open type dual-roller expansion drying, comprises the steps：
(1) stainless steel double roller (gap 0.05-0.5mm) surface for reversely inwardly rotating is heated into 90-180 DEG C of (two rollers
Temperature is identical), specifically with higher than the boiling point of glass transition temperature of polymer Tg and solvent, while and not causing polymer discoloration
It is defined；
(2) the CSM glues in reactor are incorporated into the V-groove that above-mentioned double roller is formed (two ends are kept off with high-temperature resistance plastice
Firmly, prevent from leaking), can be that multiple spot is introduced, or single-point is introduced.Simultaneously the in-migration draught hood above V-groove, takes away molten
Agent is simultaneously reclaimed.
Wherein, multiple spot or single-point are introduced, and refer to that glue pipe outlet is multiple (with groove parallel arrangement) or single；Exhausting
Cover, refer to be placed on double roller upside, can be taken away with negative pressure the solvent for flashing off cover (it is fixed or movable, but will
Ask wind-force big, be similar to lampblack absorber)；Take solvent away and reclaim, refer to and solvent is introduced into low-temperature space, condense into liquid solvent, with
Reach and recycle, not the purpose of pollutant atmosphere.
(3) roll surface temperature and rotating speed are adjusted, treats that roller surface forms dry film shape cladding, it is fast with the lower film of knife beveling
Speed is coated on chill roll (surface temperature 20-25 DEG C), then collects and is drawn to (distortion is into strips) on traction wheel, uses blade
Cut into bulk.Form stable glue addition --- roller rotation --- traction, rate of cutting to match.
Wherein, double roller surface temperature and rotating speed are adjusted, refer to quick, thoroughly can be flashed out with solvent, while polymerization
Thing film color is unchanged or change slight (thermal degradation causes) is principle；With the lower film of knife beveling, referring to will be adhered to scraper
Strip down in the thin polymer film of roller surface, and pull out；Chill roll, refers to the stainless steel riders that surface temperature is room temperature,
CSM films are coated to rapidly on chill roll from after thermo-roll surface stripping, can prevent CSM from turning yellow (thermal degradation)；Described traction is
The CSM films of stripping are persistently pulled out and are twisted into rope form by finger, are then cut into little bulk.Form stable glue addition --- rolling
Cylinder is rotated --- and traction, rate of cutting match.
Device of the present invention is described as follows：
A kind of special purpose device of chlorosulfonated polyethylene (CSM) glue desolvation, described device is open, normal pressure metal
Double roller flash dryer, including stainless steel double roller, cooling system, solvent recovering system and traction, cutter sweep；It is described stainless
Steel double roller is the stainless steel heating double roller for reversely inwardly rotating, and described cooling system is chill roll, the double hot-rollings of the stainless steel
Between type form V-groove, V-groove upper and lower is provided with draught hood.
Wherein, described V-groove is the V-type space of the double hot-rolling upside self-assembling formations of parallel stainless steel of IDS very little,
Blocked with high-temperature resistance plastice at two ends；The gap is 0.05-0.5mm.
Wherein, described chill roll is made up of upper chill roll and lower chill roll.Be passed through inside upper chill roll～30 DEG C originally
Water, CSM films are coated to rapidly on upper chill roll from after thermo-roll surface stripping, can prevent CSM from turning yellow (thermal degradation).Lower chill roll
Inside is passed through～10 DEG C of low temperature running water, and CSM films reach lower chill roll, can further cool down, prevent from upper cooling roller surface
CSM is not thoroughly cooled.The material of chill roll is stainless steel, in unloading position, for cooling down material and transmission material, is risen
To draw.The cooling medium of chill roll can also be air (during winter).
Wherein, stainless steel double roller, refers to material for stainless steel chromium plating, stainless steel enameling or stainless steel and covers polytetrafluoroethyl-ne
The cylindric solid or hollow roller drum of alkene.
Wherein, described high-temperature resistance plastice baffle plate material is phenoplasts.
Wherein, described draught hood, refers to and is placed on double roller upper and lower sides, can take the cover of the solvent for flashing off away with negative pressure
Son (it is fixed or movable, but require that wind-force is big, it is similar to lampblack absorber).
Wherein, described solvent recovering system is condenser and draught hood；The preferred graphite condenser of condenser.The exhausting
Cover is that, in V-groove upper and lower each, draught hood can make to form slight negative pressure in whole device, and negative pressure is generated by water-circulating pump；
Preferably, stainless steel heating roller roller size of the present invention is diameter 200-1000mm, long 200-2000mm,
As it is further preferred that selected size is diameter 600-900mm, long 1000-1200mm；Chill roll length it is identical with heating roller or
It is bigger, but diameter can reduce.
Preferably, stainless steel riders material of the present invention is stainless steel chromium plating, stainless steel enameling, stainless steel is covered
Polytetrafluoroethylene (PTFE), as it is further preferred that selected material is stainless steel chromium plating；
Preferably, stainless steel riders mode of heating of the present invention is electrical heating, steam heating, heat-conducting oil heating,
As it is further preferred that selected mode of heating is electrical heating；
Preferably, the stainless steel riders type of cooling of the present invention is：Water-cooled, air-cooled, oil cooling, as it is further preferred that institute
From the type of cooling be water-cooled, roller temperature can be controlled by water temperature or flow；
Preferably, stainless steel double roller (hot-rolling) gap of the present invention is 0.05-0.5mm, as it is further preferred that selected
Gap is 0.1-0.2mm；
Preferably, stainless steel hot roller surface heating-up temperature of the present invention is 90-180 DEG C (higher than solvent boiling point, low
In CSM decomposition temperatures)；
Preferably, stainless steel riders (containing cold and hot roller) rotating speed of the present invention is 1-5rpm, preferred 2-3rpm；
Preferably, solvent is CCl in glue of the present invention4、CHCl3、CH2Cl2、CHFCl2And its mixture, CSM
Concentration 2-10wt%, as it is further preferred that selecting CCl4And CSM concentration 8wt%；
Preferably, traction of the present invention is mechanical traction, hauling speed matches with drum rotation speed.
Compared with prior art, advantages of the present invention has：
The present invention adopts open stainless steel double roller surface, rapidly, continuously flashes off under high temperature, normal pressure (without the need for vacuum)
Solvent in thin polymer (such as CSM) liquid film, and rapidly (in case xanthochromia) is cooled down, one-step method obtains that outward appearance condition is good, and acid contains
Measure low, the measured polymer of matter.Simple with equipment, solvent recovering rate is high, the advantage such as drying efficiency height.Can be widely applied to take off
Except the easy volatile solvent in thermal sensitivity, high viscosity substance.
The technology is after solwution method synthesis CSM terminates, directly glue to be introduced into open metal double roller surface, by moment
High temperature, atmospheric flashing goes out solvent, then film is run through into chill roll and is cooled down, and obtains film-form CSM products.Compare biography
The hot water condensation technique (also known as wet method water vapour air- extraction) of system, the solvent expansion drying method of the present invention has process is simple,
Do not use recirculated water, reduce solvent eliminating water cost in production process, content is low, do not contain for products obtained therefrom acid (hydrochloric acid and sulfuric acid etc.)
Inorganic salts (CaCl2, NaCl), xanthochromia degree is little, outward appearance condition good (white or shallow milky).Compare conventional containment cylinder
Minton dryer, the double roller device of the present invention is that normal pressure is open, it is to avoid sealing and local easily paste glue, twine glue, kiss-coating
Simple with equipment without the need for vacuum Deng technical barrier, solvent recovering rate is high, the advantage such as drying efficiency height.Can be widely applied to do
Scorching quick, high viscosity substance, such as neoprene, chlorinated natural rubber, CSM rubber.
Description of the drawings
Fig. 1 is apparatus of the present invention schematic diagram
Specific embodiment
With reference to embodiment, present disclosure is further illustrated.It should be appreciated that the enforcement of the present invention is not limited to
In the following examples, any pro forma flexible and/or change made to the present invention falls within the scope of the present invention.
Embodiment 1
After open stainless steel double roller surface is warming up into 160 DEG C, the CSM/CCl that concentration is 8%4Glue introduces above-mentioned
In the V-groove that double roller is formed, it is 0.1mm to adjust the gap between two rollers.The rotating speed of two rollers is 2r/min, treats that steel roller faces are formed
Dry film shape is coated, and with the lower film of knife beveling, is coated to rapidly on the chill roll of reverse rotation, collects and be drawn to traction wheel
On, pulling speed is 3.7m/min, you can obtain the CSM finished products that outward appearance is white.
CSM finished products are refined into elastomeric compound with basic components component, formula constituent is as follows：
| Title | Specification | Formula (g) |
| CSM | 40 | 100 |
| Magnesia | 150 | 4 |
| Age resistor | NBC | 1 |
| Carbon black | 550 | 40 |
| Accelerator | Pentaerythrite | 3 |
| Accelerator | TRA | 2 |
Embodiment 2
, with example 1, it is 130 DEG C only to change double roller surface temperature for device therefor and method of operating.
Embodiment 3
Device therefor and method of operating are with example 1, but it is 4r/min to change double roller rotating speed.
Embodiment 4
Device therefor and method of operating singly eliminate chill roll with example 1, i.e., the direct Jing of CSM films peeled off from hot double roller
Surrounding air cooling is collected and is drawn on traction wheel.Gained CSM substantially turns yellow.
Embodiment 5
Using traditional hot water cohesion process：Glue (in advance plus fine particle calcium carbonate, sodium acid carbonate to neutralize acid) is scattered in into 90-95
In DEG C hot water, it is blown into water vapour air lift and takes away CCl4, glue Jing one-pots or many kettles condense, cohesion blob of viscose and the dehydration of water Jing reciprocating sieves
Bis- grades of screw extruding drying machines of Jing are washed again gets product CSM.
Claims (10)
1. a kind of special purpose device of chlorosulfonated polyethylene (CSM) glue desolvation, it is characterised in that：Described device is opening
Formula, normal pressure metal double roller flash dryer, including stainless steel double roller, cooling system, solvent recovering system and traction, cutting dress
Put；The stainless steel double roller is the double stainless steels heating double roller for reversely inwardly rotating, and described cooling system is chill roll, described
V-groove is formed between the double hot-rollings of stainless steel, V-groove upper and lower is provided with draught hood；Solvent recovering system is draught hood and condensation
Device.
2. the special purpose device of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 1, it is characterised in that：It is described
V-groove be IDS very little parallel pair of stainless steel heating roller upside self-assembling formation V-type space, two ends high-temperature resistance plastice
Block；The hot-rolling gap is 0.05-0.5mm.
3. the special purpose device of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 1, it is characterised in that：It is described
Chill roll be made up of upper chill roll and lower chill roll；Upper and lower chill roll is respectively with room temperature tap water and～10 DEG C of water at low temperature
Cooling medium；Cooling medium can also be air during winter.
4. the special purpose device of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 1, it is characterised in that：It is described
Stainless steel double roller, refer to material for stainless steel chromium plating, stainless steel enameling or stainless steel and cover the cylindric of polytetrafluoroethylene (PTFE)
Solid or hollow roller drum.
5. a kind of new method of glue liquor of chlorosulfonated polyethylene through desolventizing, it is characterised in that methods described includes step in detail below：
(1) the double stainless steel double roller surfaces for reversely inwardly rotating are heated into 90-180 DEG C, specifically with higher than polymer glass
The boiling point of transition temperature Tg and solvent, while and not causing polymer discoloration to be defined；
(2) glue in reactor is incorporated into the V-groove that above-mentioned double roller is formed, groove two ends are blocked with high-temperature resistance plastice, is prevented
Only leak；Simultaneously the in-migration draught hood above V-groove, takes solvent away and reclaims；
(3) double roller surface temperature and rotating speed are adjusted, treats that double roller surface forms dry film shape cladding, it is fast with the lower film of knife beveling
Speed is coated on chill roll, and the surface temperature of chill roll is room temperature or lower, then collects and is drawn on traction wheel and distorts
Into strips, bulk is cut into blade, forms stable glue addition --- roller rotation --- cooling --- traction, cutting phase
Matching.
6. the new method of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 5, it is characterised in that：Described
Glue liquor of chlorosulfonated polyethylene through is referred to CCl4、CHCl3、CH2Cl2、CHFCl2And its mixture be solvent, concentration 2-10wt% it is equal
Phase solution.
7. the new method of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 5, it is characterised in that：Stainless steel
Roller mode of heating is electrical heating, steam heating or heat-conducting oil heating.
8. the new method of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 5, it is characterised in that：Stainless steel
The roller type of cooling is：Water-cooled, air-cooled or oil cooling.
9. the new method of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 5, it is characterised in that：Heating roller
It is 1-5rpm with the rotating speed of chill roll.
10. the new method of a kind of glue liquor of chlorosulfonated polyethylene through desolventizing according to claim 6, it is characterised in that：It is described
Glue liquor of chlorosulfonated polyethylene through refer to CCl4For solvent, the homogeneous phase solution of concentration 8wt%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710088635.5A CN106632749A (en) | 2017-02-18 | 2017-02-18 | Novel method and special device for removing solvents from chlorosulfonated polyethylene adhesive liquid |
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| CN201710088635.5A CN106632749A (en) | 2017-02-18 | 2017-02-18 | Novel method and special device for removing solvents from chlorosulfonated polyethylene adhesive liquid |
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| CN201710088635.5A Pending CN106632749A (en) | 2017-02-18 | 2017-02-18 | Novel method and special device for removing solvents from chlorosulfonated polyethylene adhesive liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108410004A (en) * | 2018-04-04 | 2018-08-17 | 肖锦 | A kind of preparation method of chlorosulfonated polyethylene |
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| GB804535A (en) * | 1956-02-17 | 1958-11-19 | Du Pont | Isolation of chlorosulfonated polymers of ethylene |
| GB1000253A (en) * | 1960-09-30 | 1965-08-04 | Mason & Sons Ltd E N | Method of and apparatus for drying sheet material |
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| CN108410004A (en) * | 2018-04-04 | 2018-08-17 | 肖锦 | A kind of preparation method of chlorosulfonated polyethylene |
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