CN1663982A - Redispersible polyarylethersulphones micropowder and method for preparing same - Google Patents
Redispersible polyarylethersulphones micropowder and method for preparing same Download PDFInfo
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Abstract
The invention relates to redispersable polyarylether sulfone micro-powder and the preparing method, belonging to the high molecular polymer field.The elementary composition is polyarylideneethersulfone with repetitive units or polyarylideneethersulfone with repetitive units and with side group, containing surface active agent, the average granule diameter is 0.01~10mum.The preparing process comprising putting the polyarylether sulfone into the mixed solution of organic solvent and assisting solvent; putting the ionic surface active agent into water for rapid dispersion, dispersing the solution of polyarylethersulfone, and getting the emulsion of polyarylethersulfone; evaporating the organic solvent, and then spraying for drying. Prepared product can be used as heat resisting paint or coating polymer. The invention enlarges the application area of the polyarylethersulfone, which is a kind of engineering material, and adapted for environmental protection; and benefits the maintain and application because of its redispersable.
Description
Technical field
The invention belongs to the high molecular polymer field, particularly be used for the preparation method of the redispersible polyarylethersulphonmicropowder micropowder of heat resisting coating or coating polymer.
Background technology
The prior art close with the present invention is CN1116428, and disclosed is the organic solution or the molten state polyethersulfone of polyethersulfone, and the polyethersulfone micropowder is smooth ball-type, by polyethersulfone organic solution or the preparation of molten state spraying drying.
The micropowder of poly (arylene ether) sulfone itself is known (WO91/00876 is open), the micropowder of poly (arylene ether) sulfone also can be by providing a kind of paste with a kind of liquid processing poly (arylene ether) sulfone, vigorous stirring makes latter's emulsification in water, makes the emulsion drying again and the acquisition micropowder.Mentioned preparation poly (arylene ether) sulfone emulsion (containing organic solvent N, dinethylformamide) in the patent, the content of the poly (arylene ether) sulfone in the emulsion is very low.
Disadvantages of background technology is, owing to be to be dissolved in the organic solvent, and the content of poly (arylene ether) sulfone is very low, is not fully water base, is unfavorable for redispersion, is unfavorable for environment protection.
Summary of the invention
The technical problem to be solved in the present invention is that prepared redispersible polyarylethersulphonmicropowder micropowder is not contain organic solvent; Can obtain Recovery of Organic Solvent; Prepare a kind of aqueous polyarylethersulphondispersion micro mist of environment-friendly type, have good redispersible, can be distributed to the poly (ether ketone ketone) dispersion liquid of any concentration of preparation in the water again; Being suitable for doing coating uses.
The fundamental component that redispersible polyarylethersulphonmicropowder micropowder contains is, contains the poly (arylene ether) sulfone of repeating unit or contains the poly arylidene ether sulfone that has side group of repeating unit.
The said structure that contains the poly (arylene ether) sulfone of repeating unit is:
A：-O- -S-
B：
Wherein A be-O-or-S-; Wherein B be I or/and II or/and III.Wherein the relation of A and B is that A is or/and B.
The said poly arylidene ether sulfone that has side group that contains repeating unit, its side group is: carbonyl or carboxylate salt, sulfonic group or sulfonate, amino or hydroxyl or epoxy group(ing) or thiazolinyl or alkyl or alkyl or cyano group etc.
Redispersible polyarylethersulphonmicropowder micropowder contains tensio-active agent, mainly is that Sodium dodecylbenzene sulfonate (DBS) is or/and polyvinylpyrrolidone (PVP).
Its average particulate diameter of redispersible polyether sulfone micro mist is 0.01～10 μ m.
The preparation of redispersible polyethersulfone micro mist of the present invention, used organic solvent is water-fast, and boiling point is lower than water, and suitable solvent comprises: methylene dichloride, trichloromethane, preferably trichloromethane; Solubility promoter is water-soluble and boiling point is lower than water, mainly contains methyl alcohol, ethanol, preferably methyl alcohol; Used tensio-active agent has ionic, non-ionic type and polymeric surface active agent, preferred surfactants: non-ionic type be polyvinylpyrrolidone (PVP), ionic be Sodium dodecylbenzene sulfonate (DBS).
Preparation process has preparation poly (ether ketone ketone) polymers soln, prepares emulsion, boils off organic solvent and spraying drying:
Said preparation poly (ether ketone ketone) polymers soln process is, polyether sulphone is dissolved in the mixing solutions of organic solvent and solubility promoter, and wherein, be 30% or littler by the content of mass ratio polyethersulfone; The content of solubility promoter is 12% or littler in the mixed solvent; The consumption of the tensio-active agent of non-ionic type occupies 0～5% of machine solvent by mass ratio.
Said preparation emulsion process is, pours in the high speed dispersion device ionogenic surfactant is soluble in water earlier, and the high speed dispersion device can be with colloidal mill or other dispersing apparatus, is 2～12% by the content of mass ratio tensio-active agent; Slowly pour the poly (ether ketone ketone) polymers soln into dispersion again, be prepared into poly (ether ketone ketone) emulsion.
The said organic solvent that boils off is, poly (ether ketone ketone) emulsion poured in the device (water-bath) that stirring is housed, reclaims, and feeds the pressurized air of trace, and controlled temperature is taken organic solvent out of for 50 ℃～85 ℃.
When feeding pressurized air was taken organic solvent out of, organic solvent can be used usual method, promptly obtained reclaiming by condensing works.
Said spraying drying, its processing parameter is: 90～150 ℃ of inlet temperatures, 90～125 ℃ of temperature outs, input speed 5～15r/min, air output 10～25l/min.
In preparation poly (ether ketone ketone) polymers soln process, the mixing solutions of dissolving polyether sulphone base polymer is solvent trichloromethane or methylene dichloride, solubility promoter methyl alcohol or ethanol.Preferably organic solvent mixes with solubility promoter methyl alcohol mutually with trichloromethane.The adding of solubility promoter plays hydrotropy, and the solubility promoter add-on can not be excessive.If the amount of the solubility promoter (particular methanol) that adds is too much, just do not have the effect of hydrotropy, condense easily on the contrary and precipitate, be difficult for the dissolving of polyether sulphone.
In being dissolved with the mixing solutions of polyether sulphone, the content of preferred polyether sulphone is 10～30% (mass ratioes) or littler.If the content of polyethersulfone surpasses 30% (mass ratio), the easy caking because viscosity is excessive is difficult for disperseing.
Tensio-active agent polyvinylpyrrolidone (PVP) or the polyvinyl alcohol (PVA) or the polyoxyethylene glycol (PEG) that can contain non-ionic type in organic solvent, the tensio-active agent of preferred non-ionic type is polyvinylpyrrolidone (PVP).The tensio-active agent that is dissolved in the water is the tensio-active agent of aniorfic surfactant or non-ionic type: Sodium dodecylbenzene sulfonate (DBS) or sodium laurylsulfonate (K12) or Nonyl pheno class (OP series), preferred water-soluble tensio-active agent is an anion surfactant, particularly preferably is Sodium dodecylbenzene sulfonate (DBS).
The solution that wherein contains the dissolved polyether sulphone of preparation as mentioned above added wherein contain when disperseing in the water that has dissolved tensio-active agent, can obtain the polyether sulphone emulsion.
Boiling off the organic solvent process, the removal temperature range of organic solvent is controlled at 50 ℃～85 ℃ scopes.Can, continue again to be warming up to 64～65 ℃, till not having organic solvent after 2～3 hours at 50～55 ℃ of constant temperature earlier; Be warmed up to 75～85 ℃ again, constant temperature 0.5～1 hour stops heating, discharging.When removing organic solvent, stirring velocity is slow.
Preferred drying process with atomizing parameter is: 110～115 ℃ of inlet temperatures, 92～98 ℃ of temperature outs, charging 11～13r/min, air output 20～25l/min.
The dispersing apparatus of preparation emulsion process can use various high speed pulverization, dispersion, drying plant, includes: colloidal mill, sand mill, homogenizer etc.Preferably disperse with colloidal mill.
The particle of redispersible polyethersulfone micro mist measures particle diameter≤8 μ m. by SEM, and the pattern of particle is a spheric, has aperture.The variation of the particle diameter before redispersible polyethersulfone micro mist after the spraying drying and the drying is little, can be easy to be distributed in the water, prepares the dispersion liquid of various concentration.
This redispersible polyethersulfone micro mist can be made heat resisting coating or coating polymer usefulness, and can make up with fluoro-resin, prepares various coating.For example, preparation non-stick pan coating is distributed to redispersible polyethersulfone micro mist in the water, mixes with ptfe emulsion and other additive again, makes the coating that can prepare non-stick pan.
Redispersible polyethersulfone micro mist has enlarged the range of application of poly (ether ketone ketone) engineering materials, adapts to environmental protection requirement, and is free from environmental pollution, avoided the pollution of solvent-borne type polyether sulphone emulsion to environment.Redispersible polyethersulfone micro mist has good redispersible, helps preserving and using.
Embodiment
The preparation of embodiment 1 redispersible polyethersulfone micro mist
Trichloromethane 240ml and methyl alcohol 30ml thorough mixing, 4g is dissolved in the above-mentioned solution with polyvinylpyrrolidone (PVP), polyethersulfone 140g is dissolved in above-mentioned mixing solutions is mixed with polyethersulfone solution.
The 8g Sodium dodecylbenzene sulfonate is dissolved in the 280ml deionized water; Sodium dodecyl benzene sulfonate aqueous solution is poured in the colloidal mill, again polyethersulfone solution is slowly added in the colloidal mill, disperse.
Pour the polyethersulfone emulsion that contains organic solvent of preparation into 1000 milliliters of there-necked flasks that whipping appts, condensing works are housed, in water-bath, heat, temperature controlling range 55 ℃ 3 hours, 65 ℃ 3 hours till not having solvent to steam, be warmed up to 85 ℃ again, 30 minutes.Stop to stir stopping to heat and obtain water base aqueous polyarylethersulphondispersion dispersion liquid.
The drying process with atomizing parameter is 112 ℃ of inlet temperatures, 95 ℃ of temperature outs, charging 12r/min, air output 25l/min.
The preparation of embodiment 2 redispersible polyethersulfone micro mists
Trichloromethane 240ml and methyl alcohol 20ml thorough mixing are dissolved in above-mentioned mixing solutions with polyethersulfone 90g.
The 8g Sodium dodecylbenzene sulfonate is dissolved in the 280ml deionized water.Sodium dodecyl benzene sulfonate aqueous solution is poured in the colloidal mill, again polyethersulfone solution is slowly added in the colloidal mill, disperse.
Pour the polyethersulfone emulsion that contains organic solvent of preparation into 1000 milliliters of there-necked flasks that whipping appts, condensing works are housed, in water-bath, heat, temperature controlling range 55 ℃ 3 hours 65 ℃ 3 hours till not having solvent to steam, be warmed up to 85 ℃ again, 30 minutes.Stop to stir stopping to heat and obtain water base aqueous polyarylethersulphondispersion dispersion liquid.
The drying process with atomizing parameter is 112 ℃ of inlet temperatures, 95 ℃ of temperature outs, charging 12r/min, air output 25l/min.
The preparation of embodiment 3 redispersible polyethersulfone micro mists
Trichloromethane 240ml and methyl alcohol 10ml thorough mixing are dissolved in above-mentioned mixing solutions with polyethersulfone 90g.
The 6g Sodium dodecylbenzene sulfonate is dissolved in the 280ml deionized water.Sodium dodecyl benzene sulfonate aqueous solution is poured in the colloidal mill, again polyethersulfone solution is slowly added in the colloidal mill, disperse.
Pour the polyethersulfone emulsion that contains organic solvent of preparation into 1000 milliliters of there-necked flasks that whipping appts, condensing works are housed, in water-bath, heat, temperature controlling range 55 ℃ 2 hours, 65 ℃ 3 hours till not having solvent to steam, be warmed up to 80 ℃ again, 30 minutes.Stop to stir, stop to heat and obtain water base aqueous polyarylethersulphondispersion dispersion liquid.
The drying process with atomizing parameter is 112 ℃ of inlet temperatures, 95 ℃ of temperature outs, charging 11r/min, air output 25l/min.
The preparation of embodiment 4 redispersible polyethersulfone micro mists
Trichloromethane 240ml and methyl alcohol 15ml thorough mixing are dissolved in above-mentioned mixing solutions with polyethersulfone 60g.
The 4g Sodium dodecylbenzene sulfonate is dissolved in the 280ml deionized water.The above-mentioned aqueous solution is poured in the colloidal mill, again polyethersulfone solution is slowly added in the colloidal mill, disperse
Pour the polyethersulfone emulsion that contains organic solvent of preparation into 1000 milliliters of there-necked flasks that whipping appts, condensing works are housed, in water-bath, heat, temperature controlling range 55 ℃ 2 hours 65 ℃ 3 hours till not having solvent to steam, be warmed up to 85 ℃ again, 30 minutes.Stop to stir, stop to heat and obtain water base aqueous polyarylethersulphondispersion dispersion liquid.
Drying process with atomizing: 112 ℃ of inlet temperatures, 95 ℃ of temperature outs, charging 11r/min, air output 25l/min.
The preparation of embodiment 5 redispersible polyethersulfone micro mists
Trichloromethane 240ml and methyl alcohol 20ml thorough mixing, 4g is dissolved in above-mentioned mixing solutions with polyvinylpyrrolidone (PVP), and dissolving back fully is being dissolved in above-mentioned mixing solutions with polyethersulfone 90g.
The 8g Sodium dodecylbenzene sulfonate is dissolved in the 280ml deionized water.Sodium dodecyl benzene sulfonate aqueous solution is poured in the colloidal mill, again polyethersulfone solution is slowly added in the colloidal mill, disperse.
Pour the polyethersulfone emulsion that contains organic solvent of preparation into 1000 milliliters of there-necked flasks that whipping appts, condensing works are housed, in water-bath, heat, temperature controlling range 55 ℃ 2 hours 65 ℃ 3 hours till not having solvent to steam, be warmed up to 85 ℃ again, 30 minutes.Stop to stir, heat and obtain water base aqueous polyarylethersulphondispersion dispersion liquid.
The drying process with atomizing parameter is 112 ℃ of inlet temperatures, 95 ℃ of temperature outs, charging 12r/min, air output 25l/min.
The preparation of embodiment 6 redispersible polyethersulfone micro mists
Trichloromethane 240ml, 4g is dissolved in the above-mentioned solution with polyvinylpyrrolidone (PVP), and dissolving back fully is being dissolved in above-mentioned mixing solutions with polyethersulfone 90g.
The 8g Sodium dodecylbenzene sulfonate is dissolved in the 280ml deionized water.Sodium dodecyl benzene sulfonate aqueous solution is poured in the colloidal mill, again polyethersulfone solution is slowly added in the colloidal mill, disperse.
Pour the polyethersulfone emulsion that contains organic solvent of preparation into 1000 milliliters of there-necked flasks that whipping appts, condensing works are housed, in water-bath, heat, temperature controlling range 55 ℃ 2 hours 65 ℃ 3 hours till not having solvent to steam, be warmed up to 85 ℃ again, 30 minutes.Stop to stir, heat and obtain water base aqueous polyarylethersulphondispersion dispersion liquid.
Drying process with atomizing: 112 ℃ of inlet temperatures, 95 ℃ of temperature outs, charging 11r/min, air output 25l/min.
The preparation of embodiment 7 redispersible polyethersulfone micro mists
With any poly (arylene ether) sulfone or have polyethersulfone in the poly arylidene ether sulfone alternate embodiment 1～6 of side group, can make corresponding aqueous-based dispersions.
The preparation of embodiment 8 redispersible polyethersulfone micro mists
Make the solvent of polyether sulphone base polymer with the trichloromethane in the trichloromethane alternate embodiment 1～6, perhaps make the solubility promoter of polyether sulphone base polymer with the methyl alcohol in the ethanol alternate embodiment 1～6, the effect of products obtained therefrom and embodiment 1～6 are basic identical.
The preparation of embodiment 9 redispersible polyethersulfone micro mists
Make tensio-active agent with the polyvinylpyrrolidone (PVP) in polyvinyl alcohol (PVA) or polyoxyethylene glycol (PEG) alternate embodiment 1,5,6, perhaps use the Sodium dodecylbenzene sulfonate (DBS) in sodium laurylsulfonate (K12) or Nonyl pheno class (OP series) alternate embodiment 1～6 to make tensio-active agent, the effect of products obtained therefrom and embodiment 1～6 are basic identical.
Claims (6)
1, a kind of redispersible polyarylethersulphonmicropowder micropowder is characterized in that, fundamental component is the poly arylidene ether sulfone that has side group that contains the poly (arylene ether) sulfone of repeating unit or contain repeating unit,
The said structure that contains the poly (arylene ether) sulfone of repeating unit is:
Wherein A be-O-or-S-; Wherein B be I or/and II or/and III; Wherein the relation of A and B is that A is or/and B;
The said poly arylidene ether sulfone that has side group that contains repeating unit, its side group is: carbonyl or carboxylate salt, sulfonic group or sulfonate, amino or hydroxyl or epoxy group(ing) or thiazolinyl or alkyl or alkyl or cyano group;
Also contain tensio-active agent Sodium dodecylbenzene sulfonate or sodium laurylsulfonate or Nonyl pheno class.
According to the described redispersible polyarylethersulphonmicropowder micropowder of claim 1, it is characterized in that 2, said tensio-active agent is a Sodium dodecylbenzene sulfonate, also have polyvinylpyrrolidone.
According to claim 1 or 2 described redispersible polyarylethersulphonmicropowder micropowders, it is characterized in that 3, its average particulate diameter of said redispersible polyarylethersulphonmicropowder micropowder is 0.01～10 μ m.
4, a kind of preparation method of redispersible polyarylethersulphonmicropowder micropowder, comprise spray-dired process, it is characterized in that, with poly (arylene ether) sulfone that contains repeating unit or the poly arylidene ether sulfone that has side group that contains repeating unit is basal component, also contains tensio-active agent Sodium dodecylbenzene sulfonate or sodium laurylsulfonate or Nonyl pheno class; With methylene dichloride or trichloromethane is solvent, is solubility promoter with methyl alcohol or ethanol, and preparation process has preparation poly (ether ketone ketone) polymers soln, prepares emulsion, boils off organic solvent, is spraying drying at last;
Said preparation poly (ether ketone ketone) polymers soln process is, the polyether sulphone base polymer is dissolved in the mixing solutions of organic solvent and solubility promoter, and wherein, be 4～30% by the content of mass ratio polyether sulphone base polymer; The content of solubility promoter is 12% or littler in the mixed solvent, and the consumption of the tensio-active agent of non-ionic type occupies 0～5% of machine solvent by mass ratio.；
Said preparation emulsion process is, pours in the high speed dispersion device tensio-active agent is soluble in water earlier, and be 2～12% by the content of mass ratio tensio-active agent; Slowly pour the poly (ether ketone ketone) polymers soln into dispersion again, be prepared into poly (ether ketone ketone) emulsion;
The said organic solvent that boils off is, poly (ether ketone ketone) emulsion poured in the device that stirring is housed, reclaims, and feeds pressurized air, and controlled temperature is taken organic solvent out of for 50 ℃～85 ℃;
Said spraying drying, its processing parameter is: 90～150 ℃ of inlet temperatures, 90～125 ℃ of temperature outs, input speed 5～15r/min, air output 10～25l/min.
According to the preparation method of the described redispersible polyarylethersulphonmicropowder micropowder of claim 4, it is characterized in that 5, said tensio-active agent is to add polyvinylpyrrolidone or polyvinyl alcohol or polyoxyethylene glycol in organic solvent; The tensio-active agent that is dissolved in the water is a Sodium dodecylbenzene sulfonate.
6, according to the preparation method of the described redispersible polyarylethersulphonmicropowder micropowder of claim 4, it is characterized in that said drying process with atomizing parameter is: 110～115 ℃ of inlet temperatures, 92～98 ℃ of temperature outs, charging 11～13r/min, air output 20～25l/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831177A (en) * | 2010-05-05 | 2010-09-15 | 吉林大学 | Formula and production process of water dispersible poly(ether ketone ketone) emulsion |
| CN103881118A (en) * | 2014-04-06 | 2014-06-25 | 吉林大学 | Preparation method of redispersible polyether sulphone micro powder |
| CN109705376A (en) * | 2019-01-21 | 2019-05-03 | 开封夸克新材料有限公司 | Polyether sulfone micro mist, preparation method and application |
| CN111440319A (en) * | 2020-05-13 | 2020-07-24 | 吉林省中科聚合工程塑料有限公司 | Post-treatment method of polyarylethersulfone polymer |
| CN113354834A (en) * | 2021-07-26 | 2021-09-07 | 浙江鹏孚隆新材料有限公司 | Heat-resistant hydrolysis-resistant engineering plastic dispersion liquid, and preparation method and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4945154A (en) * | 1989-07-07 | 1990-07-31 | Hexcel Corporation | Densified polyethersulfone |
| DK0678109T3 (en) * | 1993-01-08 | 1998-11-02 | Basf Ag | micro Powder |
| CN1162460C (en) * | 2001-08-14 | 2004-08-18 | 上海交通大学 | Polyester sulphone with lateral carboxylate group and its prepn |
-
2005
- 2005-03-25 CN CNB2005100166544A patent/CN1305936C/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831177A (en) * | 2010-05-05 | 2010-09-15 | 吉林大学 | Formula and production process of water dispersible poly(ether ketone ketone) emulsion |
| CN103881118A (en) * | 2014-04-06 | 2014-06-25 | 吉林大学 | Preparation method of redispersible polyether sulphone micro powder |
| CN109705376A (en) * | 2019-01-21 | 2019-05-03 | 开封夸克新材料有限公司 | Polyether sulfone micro mist, preparation method and application |
| CN111440319A (en) * | 2020-05-13 | 2020-07-24 | 吉林省中科聚合工程塑料有限公司 | Post-treatment method of polyarylethersulfone polymer |
| CN111440319B (en) * | 2020-05-13 | 2023-06-02 | 吉林省中科聚合工程塑料有限公司 | Post-treatment method of polyarylethersulfone polymer |
| CN113354834A (en) * | 2021-07-26 | 2021-09-07 | 浙江鹏孚隆新材料有限公司 | Heat-resistant hydrolysis-resistant engineering plastic dispersion liquid, and preparation method and application thereof |
| CN113354834B (en) * | 2021-07-26 | 2023-02-24 | 浙江鹏孚隆新材料有限公司 | Heat-resistant hydrolysis-resistant engineering plastic dispersion liquid, and preparation method and application thereof |
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| CN1305936C (en) | 2007-03-21 |
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