CN106832286A - A kind of sulfone birds of the same feather flock together compound industrialization blowing dispersing technology - Google Patents
A kind of sulfone birds of the same feather flock together compound industrialization blowing dispersing technology Download PDFInfo
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- CN106832286A CN106832286A CN201710116974.XA CN201710116974A CN106832286A CN 106832286 A CN106832286 A CN 106832286A CN 201710116974 A CN201710116974 A CN 201710116974A CN 106832286 A CN106832286 A CN 106832286A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/20—Polysulfones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/20—Polysulfones
- C08G75/23—Polyethersulfones
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Abstract
The present invention provides a kind of sulfone and birdss of the same feather flock together compound industrialization blowing dispersing technology, sulfone birds of the same feather flock together added after compound polymerisation terminates with polymerization solvent identical polymerization solvent, to reduce reaction temperature, terminate polymerisation, reduce reaction fluid viscosity；Being filled with inert gas all the time in kettle carries out protection against oxidation；Sulfone compound of birdsing of the same feather flock together slowly is discharged in dispersion sieve plate, during polymer after sieve forms drops in the case of freely falling body and falls into the dispersion slot equipped with dispersant and belt stirrer, polymer solvent is dissolved in the middle of deionized water dispersant；After blowing dispersion is finished, deionized water dispersant and polymerization solvent mixed solution are discharged by disperseing the screen cloth of trench bottom；Washing.The washing process difficulty of prior art presence is solved, cleaning solvent consumption is big, and disposal of pollutants is big, polymer solvent and inorganic salts residual are high, and transparency declines, the product colour depth low problem of purity.
Description
Technical field
The present invention provides a kind of sulfone and birdss of the same feather flock together compound industrialization blowing dispersing technology, is related to speciality polymer material industry metaplasia
The polymer process for dispersing of product, more particularly to the polymer blowing process for dispersing such as polysulfones, polyether sulfone, PPSU, polyarylsulfone (PAS) and set
It is standby, belong to technical field of polymer materials.
Background technology
Sulfone polymer is a series of amorphous aromatic thermoplastic macromolecule materials containing sulfone linkage in macromolecule repeat unit
Material.Industrial valuable sulfone polymer mainly includes polysulfones（English abbreviation have PSF PSU PSO etc.）, polyether sulfone（English contracting
Write PES）, PPSU（English abbreviation have PPSF PPSU PPSO etc.）Deng.Its key property is:Heat endurance is high, the transparency is good,
Hydrolytic stability is excellent, and shrinkage factor is low, good biocompatibility, electrical property and excellent in mechanical performance, to acid, alkali, alcohol, aliphatic hydrocarbon and
The excellent special engineering plastics of the patience of salting liquid, are widely used in the high-end field such as medicine equipment, space flight and aviation, electronics material
Material
Current sulfone family macromolecule polymer production process uses a step nucleophilic displacement of fluorine route, polymerisation in solution synthetic method, main segregation
Close workshop section and treatment and finishing section.
Polymerization workshop section:Primary raw material 4,4 '-dichloro diphenyl sulfone, bisphenol-A, bisphenol S, '-biphenyl diphenol, potassium carbonate or carbonic acid
Sodium, is polymerized in a solvent, and common solvent has dimethyl sulfoxide (DMSO), N, N- dimethylacetylamides, sulfolane etc., optional toluene,
Dimethylbenzene etc. is used as water entrainer.Polymerization carries out the post processing work such as dispersion, crushing, washing, drying, granulation of polymer after terminating
Section.
The dispersion of polymer:Viscous fluid after polymerization is injected the solvents different from the solvent of reaction addition as dispersion
Agent, such as deionized water, ethanol, methyl alcohol.Sulfone polymers is separated from polymer solution in dispersant.That separates is poly-
The size-reduced washing of sulfone, drying, granulation and packaging.Wherein, sulfone polymers is separated from polymer solution and washs particularly important, polymerization
Contain unreacted inorganic salts sodium carbonate or sodium acid carbonate, potassium carbonate or saleratus in polymer solution after end, and
Reaction side product chlorinated sodium or potassium chloride, unreacted raw material monomer, system and material web come colouring metal ions and its
Its mechanical admixture.They must be divided, and could obtain high-quality polysulfones
Existing dispersion technology is domestic without ripe method.It is use water sedimentation high speed comminuting method, this method more:It is anti-in polymerization
After should terminating, by the viscous fluid injection water after polymerization, while polysulfones is ground into particulate with high speed disintegrator, polymer is separated out
The inorganic salt particle of middle parcel, polymer solvent be discharged into it is molten with dispersant in dispersant be integrated, remove solvent after being separated by filtration
Recovery system.The problem that the method is present is that the polymer contour structures for obtaining are irregular, increased subsequent wash technology difficulty,
Cleaning solvent consumption is big, and disposal of pollutants is big, and polymer solvent and inorganic salts residual are high, and transparency declines, and product colour depth purity is low.
The content of the invention
The present invention provides a kind of sulfone and birdss of the same feather flock together compound industrialization blowing dispersing technology, solves the washers of prior art presence
Skill difficulty, cleaning solvent consumption is big, and disposal of pollutants is big, and polymer solvent and inorganic salts residual are high, and transparency declines, product colour depth
The low problem of purity.
The present invention provide a kind of sulfone birds of the same feather flock together compound industrialization blowing dispersing technology, comprise the following steps：
1）Compound polymerisation of sulfone birdsing of the same feather flock together is added and polymerization solvent identical polymerization solvent after terminating, to reduce reaction
Temperature, the polymerisation that terminates, reduction reaction fluid viscosity；The addition of polymerization solvent is that polymerization pre-polymerization reaction dissolvent is added
The 10% ~ 50% of amount, control material temperature is at 70 DEG C ~ 200 DEG C；
2）Being filled with inert gas all the time in kettle carries out protection against oxidation；
3）By sulfone birds of the same feather flock together compound be slowly discharged to dispersion sieve plate in, the polymer after sieve forms drops simultaneously in the case of freely falling body
Fall into the dispersion slot equipped with dispersant and belt stirrer, polymer solvent is dissolved in the middle of deionized water dispersant；
4）After blowing dispersion is finished, by disperseing, the screen cloth of trench bottom discharges deionized water dispersant and polymerization solvent mixes
Solution；
5）The sulfone for precipitating compound little particle of birdsing of the same feather flock together is sent to washing procedure and is washed.
Described polymerization solvent is selected from：N, N- dimethylacetylamide（DMAC）, dimethyl sulfoxide (DMSO), sulfolane.
Step 1）Polymerisation adds polymerization solvent again after terminating, the addition of polymerization solvent is before being polymerized
10% ~ 50% for adding, is preferable over 20% ~ 30%, and control material temperature is preferable over 80 ~ 180 DEG C at 70 ~ 200 DEG C.
Step 1）Moisture content≤0.5% of the control solvent being related to；The addition of solvent is the 20% ~ 30% of the preceding addition of polymerization,
Control material temperature is at 80 ~ 180 DEG C.
Step 3）The dispersing sieve screen aperture being related to is φ 2 ~ φ 10mm, is preferable over φ 5-φ 8mm, sieve-plate aperture ratio 8 ~
20%, preferred aperture rate 10 ~ 15%；Freely falling body of the dispersion sieve plate away from dispersant liquid level is highly 0.5 ~ 2.5m, is preferable over 1 ~ 2m.
Step 4）The dispersant being related to is deionized water；In dispersion process, the temperature control of dispersant is in 15 ~ 55 DEG C of scopes
It is interior.
The positive effect of the present invention is：
Solve existing sulfone to birds of the same feather flock together in compound production process, the sticky shaped polymer dispersion of high temperature is irregular to cause washing uneven,
The low problem of product percent of pass.Using present invention production sulfone class polysulfones purity is high, physical and chemical performance stabilization, solvent recovering rate are high,
It is simple to operate, low cost, pollution-free.
Specific embodiment
By following examples further illustrate description the present invention, never in any form limit the present invention, without departing substantially from
On the premise of technical solution of the invention, easily any of realization changes those of ordinary skill in the art made for the present invention
Dynamic or change is fallen within scope of the presently claimed invention.
Embodiment 1
Polysulfones（PSF）Blowing disperses
After the reaction of 3000L polymerization reaction kettles terminates, continue to be protected to logical nitrogen in kettle, while N is rapidly joined, N- bis-
Methylacetamide（DMAC）300 L, are sufficiently stirred for 10 minutes, and polysulfones solution temperature is down to 120 DEG C, open polymerization kettle bottom valve, dilute
The reaction solution released is put into the sieve plate at the top of dispersion slot, material by designing screen-aperture for φ 4mm, sieve-plate aperture ratio 20%,
Drops is formed in the case of freely falling body and is fallen into the dispersion slot equipped with dispersant and belt stirrer, dispersant temperature control exists
Within 45 DEG C, the polymer beads of average grain diameter 5mm are obtained, stayed in the minutes of dispersion slot 20, big portion stirring is underlying
Segregation bonding solvent is dissolved in the middle of dispersant, obtains the uniform polysulfone polymer of the hardened granules after desolventizing.It is size-reduced, washing and
Dry N in post-consumer polymer, N- dimethylacetylamides（DMAC）Residual quantity is 0.0012%, and water washing pass is reduced to 8 by 10 times
Time.Product quality and detersive efficiency are improve, washing water consumption is reduced.
Embodiment 2
PPSU（PPSU）Blowing disperses
After the reaction of 3000L polymerization reaction kettles terminates, continue to be protected to logical nitrogen in kettle, while rapidly joining sulfolane
300L, is sufficiently stirred for 20 minutes, and PPSU solution temperature is down to 160 DEG C, opens polymerization kettle bottom valve, and the reaction solution of dilution is put into point
Dissipate in the sieve plate at the top of groove, material is φ 6mm, sieve-plate aperture ratio 15%, the shape in the case of freely falling body by designing screen-aperture
Into drops and fall into the dispersion slot equipped with dispersant and belt stirrer, dispersant temperature control is put down within 50 DEG C
The polymer beads of equal particle diameter 7mm, stay in the minutes of dispersion slot 15 stirring is underlying, and most of polymer solvent is dissolved in
In the middle of dispersant, the uniform polyphenylsulfone polymer of the hardened granules after desolventizing is obtained.It is size-reduced, in washing and drying post-consumer polymer
Sulfolane residual quantity is 0.0008%, and water washing pass is reduced to 8 times by 10 times.Product quality and detersive efficiency are improve, is reduced
Washing water consumption.
Embodiment 3
Polyether sulfone（PES）Blowing disperses
After the reaction of 3000L polymerization reaction kettles terminates, continue to be protected to logical nitrogen in kettle, while rapidly joining sulfolane sulfone
250L, is sufficiently stirred for 15 minutes, and polyether sulfone solution temperature is down to 150 DEG C, opens polymerization kettle bottom valve, and the reaction solution of dilution is put into point
Dissipate in the sieve plate at the top of groove, material is φ 5mm, sieve-plate aperture ratio 17%, the shape in the case of freely falling body by designing screen-aperture
Into drops and fall into the dispersion slot equipped with dispersant and belt stirrer, dispersant temperature control is put down within 40 DEG C
The polymer beads of equal particle diameter 6mm, stay in the minutes of dispersion slot 20 stirring is underlying, and most of polymer solvent is dissolved in
In the middle of dispersant, the uniform polyether sulfone polymer of the hardened granules after desolventizing is obtained.It is size-reduced, in washing and drying post-consumer polymer
Sulfolane residual quantity is 0.0015%, and water washing pass is reduced to 8 times by 10 times.Product quality and detersive efficiency are improve, is reduced
Washing water consumption.
Above example proved, the evengranular sulfone obtained using the present invention is birdsed of the same feather flock together compound discrete particles, and postmenstruation crushes
After machine washing is washed, sulfone is birdsed of the same feather flock together the physical and chemical performance stabilization of compound, solvent recovering rate high, simple to operate, low cost, pollution-free.
Claims (6)
1. a kind of sulfone birds of the same feather flock together compound industrialization blowing dispersing technology, comprise the following steps：
1）Compound polymerisation of sulfone birdsing of the same feather flock together is added and polymerization solvent identical polymerization solvent after terminating, to reduce reaction
Temperature, the polymerisation that terminates, reduction reaction fluid viscosity；Control polymerization solvent moisture content is 0.05% ~ 3%；Solvent polymeric is anti-
The addition for answering solvent is 10% ~ 50% that polymerization pre-polymerization reaction dissolvent is added, and control material temperature is at 70 DEG C ~ 200 DEG C；
2）Being filled with inert gas all the time in kettle carries out protection against oxidation；
3）Polymer was slowly photographed in dispersion sieve plate, the polymer after sieve forms drops and falls into the case of freely falling body
In dispersion slot equipped with dispersant and belt stirrer, polymer solvent is dissolved in the middle of deionized water dispersant；
4）After blowing dispersion is finished, by disperseing, the screen cloth of trench bottom discharges deionized water dispersant and polymerization solvent mixes
Solution；
5）The sulfone for precipitating compound little particle of birdsing of the same feather flock together is sent to crushing and washing procedure is crushed and washed.
2. a kind of sulfone according to claim 1 birds of the same feather flock together compound industrialization blowing dispersing technology, it is characterised in that：
Described polymerization solvent is selected from：N, N- dimethylacetylamide（DMAC）, dimethyl sulfoxide (DMSO), sulfolane.
3. a kind of sulfone according to claim 1 birds of the same feather flock together compound industrialization blowing dispersing technology, it is characterised in that：
Step 1）Moisture content≤0.5% of the control solvent being related to；The addition of polymerization solvent be polymerization before add 20% ~
30%, control material temperature is at 80 ~ 180 DEG C.
4. a kind of sulfone according to claim 1 birds of the same feather flock together compound industrialization blowing dispersing technology, it is characterised in that：
Step 3）The dispersing sieve screen aperture being related to is φ 2 ~ φ 10mm, is preferable over φ 5 ~ φ 8mm, and sieve-plate aperture ratio 8 ~ 20% is excellent
Select percent opening 10 ~ 15%.
5. a kind of sulfone according to claim 1 birds of the same feather flock together compound industrialization blowing dispersing technology, it is characterised in that；
Step 3）Freely falling body of the dispersion sieve plate being related to away from dispersant liquid level is highly 0.5 ~ 2.5m, is preferable over 1 ~ 2m.
6. a kind of sulfone according to claim 1 birds of the same feather flock together compound industrialization blowing dispersing technology, it is characterised in that：
Step 4）The dispersant being related to is deionized water；In dispersion process, the temperature control of disintegrator is in the range of 15 ~ 55 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325286A (en) * | 2017-07-27 | 2017-11-07 | 山东浩然特塑股份有限公司 | A kind of post-processing approach of sulfone resinoid dispensing laundry |
| CN107892746A (en) * | 2017-11-24 | 2018-04-10 | 江门市优巨新材料有限公司 | A kind of Industrialized synthesis method of coating level superfine powder polyaryl ether sulphone resin |
| CN111533912A (en) * | 2020-06-11 | 2020-08-14 | 万华化学集团股份有限公司 | Preparation method of low-haze sulfone polymer |
| CN113637168A (en) * | 2021-09-22 | 2021-11-12 | 山东海科创新研究院有限公司 | Preparation method of sulfone polymer |
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| CN103087309A (en) * | 2013-01-18 | 2013-05-08 | 山东浩然特塑有限公司 | High-pressure synthetic method of polyaryl sulfone resin of terpolymer and quadripolymer |
| CN103897188A (en) * | 2014-03-06 | 2014-07-02 | 上海帕斯砜材料科技有限公司 | Industrialized production process of polysulfone macromolecular material |
| CN104629055A (en) * | 2015-03-11 | 2015-05-20 | 威海帕斯砜新材料有限公司 | Method for industrially producing polysulfone polymer material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087309A (en) * | 2013-01-18 | 2013-05-08 | 山东浩然特塑有限公司 | High-pressure synthetic method of polyaryl sulfone resin of terpolymer and quadripolymer |
| CN103897188A (en) * | 2014-03-06 | 2014-07-02 | 上海帕斯砜材料科技有限公司 | Industrialized production process of polysulfone macromolecular material |
| CN104629055A (en) * | 2015-03-11 | 2015-05-20 | 威海帕斯砜新材料有限公司 | Method for industrially producing polysulfone polymer material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325286A (en) * | 2017-07-27 | 2017-11-07 | 山东浩然特塑股份有限公司 | A kind of post-processing approach of sulfone resinoid dispensing laundry |
| CN107325286B (en) * | 2017-07-27 | 2020-04-17 | 山东浩然特塑股份有限公司 | Post-treatment method for dispersing and washing sulfone resin |
| CN107892746A (en) * | 2017-11-24 | 2018-04-10 | 江门市优巨新材料有限公司 | A kind of Industrialized synthesis method of coating level superfine powder polyaryl ether sulphone resin |
| CN111533912A (en) * | 2020-06-11 | 2020-08-14 | 万华化学集团股份有限公司 | Preparation method of low-haze sulfone polymer |
| CN111533912B (en) * | 2020-06-11 | 2022-08-05 | 万华化学集团股份有限公司 | Preparation method of low-haze sulfone polymer |
| CN113637168A (en) * | 2021-09-22 | 2021-11-12 | 山东海科创新研究院有限公司 | Preparation method of sulfone polymer |
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