CN105061802A - Preparation method of foamed polyester slurry - Google Patents
Preparation method of foamed polyester slurry Download PDFInfo
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- CN105061802A CN105061802A CN201510452900.4A CN201510452900A CN105061802A CN 105061802 A CN105061802 A CN 105061802A CN 201510452900 A CN201510452900 A CN 201510452900A CN 105061802 A CN105061802 A CN 105061802A
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Abstract
The invention discloses a preparation method of foamed polyester slurry, and belongs to the technical field of water soluble polyester slurry. The invention aims to solve the problems that in the prior art, the cutter is damaged easily, and the slurry dissolution wastes too much energy and time. The preparation method is characterized by comprising the following steps: mixing recycled polyester, glycol, water soluble monomers, and a catalyst according to a certain ratio, then throwing the mixture into a pre-melting kettle to carry out pre-melting; then introducing the mixture to a final polymerization kettle, gradually increasing the vacuum degree in the kettle until the pressure in the kettle reaches an absolute pressure of 133 Pa or less; keeping on raising the temperature in the kettle, wherein the reactions are finished when the kettle temperature reaches 275 +/- 2 DEG C, and the stirring power is 10 KW or so; introducing high-purity nitrogen gas into the kettle to break the vacuum state until the pressure in the kettle reaches 0.1-0.2 MPa, keeping on stirring for 5 to 10 minutes, discharging polymer to a hopper; naturally cooling the polymer, and breaking the foamed blocks into powder by a powerful pulverizer. The provided preparation method has the advantages of the breaking difficulty is reduced, the dissolution speed is accelerated, and the energy and material consumption is reduced, and is mainly used to produce foamed polyester slurry.
Description
Technical field
The invention belongs to water-soluble polyurethane preparing technical field, be specifically related to a kind of preparation method of expansion type polyester pulp.
Background technology
In the common production technique of polyester (PET) product; by vacuumizing ethylene glycol more than needed in removal system, to reach raising molecular weight, reach the object of condensation polymerization; after polymerization terminates; extrusion is cooled to particle or bulk, and polymkeric substance is fine and close, is also conducive to product in follow-up melt production; facilitate compacting material; produce qualified polyester product (comprising chemical fibre, sheet material, film material etc.).The production of polyester pulp, has continued to use the production technique of usual polyester, and product is fine and close, such product, and is unfavorable for dissolving, and at broken process, because product is fine and close, intensity is comparatively large, increases broken difficulty, consumes mass energy.
In the production, application process of other material, there is foaming treatment process, to meet different product requirements, as: Chinese patent: CN201110192218.8, a kind of preparation method of polyester for foaming.Chinese patent: CN201110259267.9, a kind of preparation of waterborne polyurethane foaming slurry.In prior art, expanded polyester is described above, and purposes is different from this patent object, and implementation method more complicated.
In prior art, polyester pulp is described above, shortcoming clearly: (1) pulverizing process often damages cutter; (2) dissolvingization slurry process, at substantial steam, changes the slurry time longer.
Summary of the invention
The object of the invention is for above-mentioned deficiency, a kind of preparation method of expansion type polyester pulp is provided, carry out foaming process in process of production, can comminution energy conssumption be reduced; Expanded polyester slurry, increases the specific surface area of material, increases the contact area of product and aqueous solvent, is more conducive to product and dissolves.
Technical solution of the present invention is: a kind of preparation method of expansion type polyester pulp, it is characterized in that comprising following processing step:
(1) by Pillar recovery, account for the ethylene glycol of this Pillar recovery weight part 5 ~ 10%, m-phthalic acid-5-sulfonate or derivatives thereof, the m-phthalic acid of 3 ~ 15%, the polycondensation catalyst Sb of 0.03 ~ 0.15% of 10 ~ 20% respectively
2o
3mixing is also together put in fritting still, static normal pressure heats up, this process reaction still fractionation capital temperature initial stage controls below 130 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture and/or methyl alcohol when reaching 90 ~ 100% of theoretical quantity of distillate, then in raising, temperature, to 250-260 DEG C, distills out unnecessary ethylene glycol;
(2) after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, heating is stopped when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum tightness in still and finally reach within 133Pa, still temperature reaches 275 ± 2 DEG C, be polymerized under power of agitator 10KW condition, and then obtain water-soluble polyurethane melt;
(3) stop vacuumizing, with high pure nitrogen releasings vacuum is carried out to polymeric kettle and pressurising to 0.1 ~ 0.2MPa, keep at this pressure stirring 5-10 minute, after stirring stopping, opening bottom valve, polymkeric substance is released to the melt material block being cooled to foaming in hopper;
(4), after naturally cooling, melt material block is made to become dead front type foam material;
(5) with strong crusher foamed material block is broken into Powdered after, test, measure, pack.
This product is before starching, and dissolve completely under the effect of stirring with the tap water of 95 ~ 98 DEG C, solubleness is between 6% ~ 25%, and according to different products, concentration is difference slightly.
In (1) step described in technical solution of the present invention, the reactor fractionation capital temperature initial stage controls between 105 DEG C ± 3 DEG C.
In (3) step described in technical solution of the present invention, high pure nitrogen passes into from polymeric kettle top.
Foamed material block is broken into strong crusher the particulate state that diameter is less than 3mm in (5) step described in technical solution of the present invention, outward appearance is faint yellow to oyster white, packing density of particle 0.82-0.84.
One of reaction conditions of condensation polymerization is under high vacuum state, by volatile component unnecessary in system as ethylene glycol is discharged in melt, reaches the object improving the polymerization degree.After reaction terminates, the viscosity of material is very large, often can reach several ten thousand even tens0000 mPa.S, now, after stirring blade, often form darker whirlpool.Now, be filled with nitrogen, under the effect of stirring, nitrogen can be imbedded in the material of thickness along with stirring whirlpool, is finally wrapped in melt.After material extrudes cooling, still exist in material, form the cavity closed one by one.After material fragmentation, cavity thereupon major part breaks, and form the concavo-concave convoluted surface pattern in hole, hole on material surface, such pattern increases the specific surface area of material.The dissolving of solid matter be first solid matter to the diffusion in liquid, undoubtedly, increase the contact area of solid-liquid, can the velocity of diffusion of accelerating solid material, thus contribute to the dissolving of solid matter.
The present invention is in production waterborne polyester slurry process, adopt simple equipment, at the end of polymerization, by the mode of inflated with nitrogen, melt inside is made to form tiny gas bag, because melt film-forming properties is better, viscosity is comparatively large, after extrusion, a large amount of gas is still deposited in internal batch, forming multiple air bag, when not having fragmentation, is dead front type foam material.During this material fragmentation, membranous wall is relatively thin, is easy to fragmentation, the semi-open type foam material of final formation.This material is compared with conventional polyester, and specific surface area increases about about 5 times.This material belongs to hydrophilic material, very little with the wetting angle of water, and therefore, in down stream dissolution operation, water is easy to infiltrate in material micropore, along with the rising of water temp, accelerates the dissolution rate of material.
Key point of the present invention is after pet reaction terminates, and by the operation of inflated with nitrogen and stirring, reaches the effect preparing expanded polyester slurry.The present invention has makes the broken difficulty of polyester pulp reduce, energy-saving and cost-reducing, increase specific surface area, increase and solvent contact area, improve the feature of dissolution rate and production efficiency.The present invention is mainly used in the preparation of expansion type polyester pulp.
Accompanying drawing explanation
Fig. 1 is foaming picture of the present invention.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1:
Preparation method comprises following processing step:
(1) within waste and old Pillar recovery plastics 750kg(water ratio 6%),
Ethylene glycol 280kg(excessive more than 200%),
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 100kg,
Sb
2O
3120g，
Above component mixing is also together put in jacketed kettle polymeric kettle at the bottom of 1.8 cubic cones, static normal pressure heats up, this process reaction still fractionation capital temperature initial stage controls between 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture and/or methyl alcohol when reaching 90 ~ 100% of theoretical quantity of distillate, then in raising, temperature, to 250-260 DEG C, distills out unnecessary ethylene glycol;
(2) after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively improves temperature in the kettle from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum tightness in still and and finally reach below absolute pressure 133Pa.Because polycondensation belongs to thermopositive reaction, and agitating friction heat-dissipating, temperature of reaction can continue to raise.Still temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains water-soluble polyurethane melt;
(3) stop vacuumizing, pass into high pure nitrogen and stir bottom terminal polymerization kettle, final maintenance still internal pressure 0.2MPa, stops after 5 minutes stirring and opening bottom valve, is released to by material on stainless steel plate, discharging time 25 minutes, is cooled to the melt material block of foaming;
(4), after naturally cooling, melt material block is made to become dead front type foam material;
(5) with strong crusher foamed material block is broken into diameter be less than 3mm Powdered after, crushing process does not stick together smoothly, and product appearance is oyster white hard foam particle, and packing density of particle 0.82, measures after the assay was approved, packs.
Adopt product prepared by above-mentioned technological process before starching, under agitation dissolve completely with 98 DEG C of tap water, dissolution time 25 minutes, solubleness 27g, solution is limpid transparent.
Embodiment 2:
Preparation method comprises following processing step:
(1) within waste and old Pillar recovery plastics 750kg(water ratio 6%),
Ethylene glycol 300kg(excessive more than 240%),
M-phthalic acid 75kg,
5-sodium sulfo isophthalate 75kg,
Sb
2O
3120g，
Above component mixing is also together put in jacketed kettle polymeric kettle at the bottom of 1.8 cubic cones, static normal pressure heats up, this process reaction still fractionation capital temperature initial stage controls between 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture and/or methyl alcohol when reaching 90 ~ 100% of theoretical quantity of distillate, then in raising, temperature, to 250-260 DEG C, distills out unnecessary ethylene glycol;
(2) after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively improves temperature in the kettle from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum tightness in still and and finally reach below absolute pressure 133Pa.Because polycondensation belongs to thermopositive reaction, and agitating friction heat-dissipating, temperature of reaction can continue to raise.Still temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains water-soluble polyurethane melt;
(3) stop vacuumizing, pass into high pure nitrogen and stir bottom terminal polymerization kettle, final maintenance still internal pressure 0.1MPa, stops after 10 minutes stirring and opening bottom valve, is released to by material on stainless steel plate, discharging time 38 minutes, is cooled to the melt material block of foaming;
(4), after naturally cooling, melt material block is made to become dead front type foam material;
(5) with strong crusher foamed material block is broken into diameter be less than 3mm Powdered after, crushing process does not stick together smoothly, and product appearance is faint yellow to oyster white hard foam particle, and packing density of particle 0.84, measures after the assay was approved, packs.
Adopt product prepared by above-mentioned technological process before starching, under agitation dissolve completely with 98 DEG C of tap water, dissolution time 28 minutes, solubleness 27g, solution is limpid transparent.
Embodiment 3:
Preparation method comprises following processing step:
(1) within waste and old Pillar recovery plastics 800kg(water ratio 6%),
Ethylene glycol 300kg(excessive more than 180%),
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 125kg,
Sb
2O
3120g，
Above component mixing is also together put in jacketed kettle polymeric kettle at the bottom of 1.8 cubic cones, static normal pressure heats up, this process reaction still fractionation capital temperature initial stage controls between 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture and/or methyl alcohol when reaching 90 ~ 100% of theoretical quantity of distillate, then in raising, temperature, to 250-260 DEG C, distills out unnecessary ethylene glycol;
(2) after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively improves temperature in the kettle from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum tightness in still and and finally reach below absolute pressure 133Pa.Because polycondensation belongs to thermopositive reaction, and agitating friction heat-dissipating, temperature of reaction can continue to raise.Interior temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains water-soluble polyurethane melt;
(3) stop vacuumizing, pass into high pure nitrogen and stir from terminal polymerization kettle top, final maintenance still internal pressure 0.2MPa, stops after 5 minutes stirring and opening bottom valve, is released to by material on stainless steel plate, discharging time 25 minutes, is cooled to the melt material block of foaming;
(4), after naturally cooling, melt material block is made to become dead front type foam material;
(5) with strong crusher foamed material block is broken into diameter be less than 3mm Powdered after, crushing process does not stick together smoothly, and product appearance is faint yellow to oyster white hard foam particle, and packing density of particle 0.83, measures after the assay was approved, packs.
Adopt product prepared by above-mentioned technological process before starching, under agitation dissolve completely with 98 DEG C of tap water, dissolution time 25 minutes, solubleness 27g, solution is limpid transparent.
Embodiment 4:
Preparation method comprises following processing step:
(1) within waste and old Pillar recovery plastics 800kg(water ratio 6%),
Ethylene glycol 320kg(excessive more than 200%),
M-phthalic acid 75kg,
5-sodium sulfo isophthalate 125kg,
Sb
2O
3120g，
Above component mixing is also together put in jacketed kettle polymeric kettle at the bottom of 1.8 cubic cones, static normal pressure heats up, this process reaction still fractionation capital temperature initial stage controls between 105 DEG C ± 3 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture and/or methyl alcohol when reaching 90 ~ 100% of theoretical quantity of distillate, then in raising, temperature, to 250-260 DEG C, distills out unnecessary ethylene glycol;
(2) after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively improves temperature in the kettle from 235 DEG C of beginnings, stop heating when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum tightness in still and and finally reach below absolute pressure 133Pa.Because polycondensation belongs to thermopositive reaction, and agitating friction heat-dissipating, temperature of reaction can continue to raise.Still temperature reaches 275 ± 2 DEG C, is polymerized under power of agitator 10KW condition, and the excessive ethylene glycol of residue removes by this process further, and then obtains water-soluble polyurethane melt;
(3) stop vacuumizing, pass into high pure nitrogen and stir from terminal polymerization kettle top, final maintenance still internal pressure 0.1MPa, stops after 5 minutes stirring and opening bottom valve, is released to by material on stainless steel plate, discharging time 40 minutes, is cooled to the melt material block of foaming;
(4), after naturally cooling, melt material block is made to become dead front type foam material;
(5) with strong crusher foamed material block is broken into diameter be less than 3mm Powdered after, crushing process does not stick together smoothly, and product appearance is faint yellow to oyster white hard foam particle, and packing density of particle 0.83, measures after the assay was approved, packs.
Adopt product prepared by above-mentioned technological process before starching, under agitation dissolve completely with 98 DEG C of tap water, dissolution time 30 minutes, solubleness 26g, solution is limpid transparent.
Comparative example 1:
In the ratio of embodiment 1, material is dropped in jacketed kettle polymeric kettle at the bottom of 1.8 cubic cones, normal vacuum condensation polymerization water-soluable sizing material polyester, at the end of reaction, stop stirring, be filled with high pure nitrogen from still top and finally keep still internal pressure 0.2MPa, open bottom valve, material is released on stainless steel plate, discharging time 25 minutes.Broken to material after naturally cooling.Adopt product prepared by above-mentioned technological process, with strong crusher, material block is broken into diameter and is less than the Powdered of 3mm, crushing process machine utilization is comparatively large, and product does not stick together, and product appearance is faint yellow particle, packing density of particle 0.98.98 DEG C of tap water dissolution times 35 minutes, solubleness 27g, solution is limpid transparent.
Comparative example 2:
In the ratio of embodiment 3, material is dropped in jacketed kettle polymeric kettle at the bottom of 1.8 cubic cones, normal vacuum condensation polymerization water-soluable sizing material polyester, at the end of reaction, stop stirring, bottom still, be filled with high pure nitrogen finally keep still internal pressure 0.2MPa, open bottom valve, material is released on stainless steel plate, melt material block surface has the hollow bubble of size about 5 millimeters once in a while, discharging time 25 minutes.Broken to material after naturally cooling.Adopt product prepared by above-mentioned technological process, with strong crusher, material block is broken into diameter and is less than the Powdered of 3mm, crushing process machine utilization is comparatively large, and product does not stick together, and product appearance is faint yellow particle, tap density 0.99.98 DEG C of tap water dissolution times 35 minutes, solubleness 27g, solution is limpid transparent.
From above several embodiment, before discharging, while stirring, no matter be filled with high pure nitrogen wherefrom, all can form closed air bag, pressure is between 0.1 ~ 0.2MPa.If be not filled with high pure nitrogen, product proportion is comparatively large, and the broken difficulty of product, energy consumption is higher, and product dissolution time is relatively long.Consider the reliability of operation, preferred scheme is filled with nitrogen from reactor top.
Claims (4)
1. a preparation method for expansion type polyester pulp, is characterized in that comprising following processing step:
(1) by Pillar recovery, account for the ethylene glycol of this Pillar recovery weight part 5 ~ 10%, m-phthalic acid-5-sulfonate or derivatives thereof, the m-phthalic acid of 3 ~ 15%, the polycondensation catalyst Sb of 0.03 ~ 0.15% of 10 ~ 20% respectively
2o
3mixing is also together put in fritting still, static normal pressure heats up, this process reaction still fractionation capital temperature initial stage controls below 130 DEG C, when in reaction, temperature reaches 235 DEG C ± 5 DEG C, the complete melting of material, distillate moisture and/or methyl alcohol when reaching 90 ~ 100% of theoretical quantity of distillate, then in raising, temperature, to 250-260 DEG C, distills out unnecessary ethylene glycol;
(2) after above fritting reaction terminates, material is imported terminal polymerization kettle, progressively temperature in the kettle is improved from 235 DEG C of beginnings, heating is stopped when interior temperature reaches 265 DEG C, while intensification, slowly progressively improve vacuum tightness in still and finally reach within 133Pa, still temperature reaches 275 ± 2 DEG C, be polymerized under power of agitator 10KW condition, and then obtain water-soluble polyurethane melt;
(3) stop vacuumizing, with high pure nitrogen releasings vacuum is carried out to polymeric kettle and pressurising to 0.1 ~ 0.2MPa, keep at this pressure stirring 5-10 minute, after stirring stopping, opening bottom valve, polymkeric substance is released to the melt material block being cooled to foaming in hopper;
(4), after naturally cooling, melt material block is made to become dead front type foam material;
(5) with strong crusher foamed material block is broken into Powdered after, test, measure, pack.
2. the preparation method of expansion type polyester pulp according to claim 1, is characterized in that: in (1) described step, the reactor fractionation capital temperature initial stage controls between 105 DEG C ± 3 DEG C.
3. the preparation method of expansion type polyester pulp according to claim 1 and 2, is characterized in that: in (3) described step, high pure nitrogen passes into from polymeric kettle top.
4. the preparation method of expansion type polyester pulp according to claim 1 and 2, it is characterized in that: in (5) described step, foamed material block is broken into strong crusher the particulate state that diameter is less than 3mm, outward appearance is faint yellow to oyster white, packing density of particle 0.82-0.84.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852117A (en) * | 2021-03-11 | 2021-05-28 | 湖北山特莱新材料有限公司 | High-temperature-resistant water-soluble polyester slurry |
| CN113185681A (en) * | 2021-04-28 | 2021-07-30 | 湖北山特莱新材料有限公司 | Preparation method of foaming type polyester slurry |
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| EP0406671A2 (en) * | 1989-06-27 | 1991-01-09 | The Seydel Companies, Inc. | Water-soluble or water-dispersible polyester sizing compositions |
| CN1834131A (en) * | 2006-04-24 | 2006-09-20 | 洛阳高新技术开发区南峰聚酯有限公司 | Water-soluable sizing material polyester and prepn. thereof |
| CN101955581A (en) * | 2010-10-10 | 2011-01-26 | 四川宏扬高分子科技有限公司 | Water-soluble polyester slurry prepared from waste polyester plastics and preparation method thereof |
| CN102295761A (en) * | 2011-07-11 | 2011-12-28 | 华润包装材料有限公司 | Method for preparing polyester for foaming |
-
2015
- 2015-07-29 CN CN201510452900.4A patent/CN105061802B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0406671A2 (en) * | 1989-06-27 | 1991-01-09 | The Seydel Companies, Inc. | Water-soluble or water-dispersible polyester sizing compositions |
| CN1834131A (en) * | 2006-04-24 | 2006-09-20 | 洛阳高新技术开发区南峰聚酯有限公司 | Water-soluable sizing material polyester and prepn. thereof |
| CN101955581A (en) * | 2010-10-10 | 2011-01-26 | 四川宏扬高分子科技有限公司 | Water-soluble polyester slurry prepared from waste polyester plastics and preparation method thereof |
| CN102295761A (en) * | 2011-07-11 | 2011-12-28 | 华润包装材料有限公司 | Method for preparing polyester for foaming |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112852117A (en) * | 2021-03-11 | 2021-05-28 | 湖北山特莱新材料有限公司 | High-temperature-resistant water-soluble polyester slurry |
| CN113185681A (en) * | 2021-04-28 | 2021-07-30 | 湖北山特莱新材料有限公司 | Preparation method of foaming type polyester slurry |
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Denomination of invention: Preparation method of foaming polyester slurry Effective date of registration: 20230404 Granted publication date: 20180116 Pledgee: Industrial Bank Co.,Ltd. Xiangyang Branch Pledgor: Hubei Santak New Material Co.,Ltd. Registration number: Y2023420000147 |
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