CN105061802B - The preparation method of expansion type polyester pulp - Google Patents
The preparation method of expansion type polyester pulp Download PDFInfo
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- CN105061802B CN105061802B CN201510452900.4A CN201510452900A CN105061802B CN 105061802 B CN105061802 B CN 105061802B CN 201510452900 A CN201510452900 A CN 201510452900A CN 105061802 B CN105061802 B CN 105061802B
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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- Polyurethanes Or Polyureas (AREA)
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Abstract
The preparation method of the entitled expansion type polyester pulp of the present invention.Belong to water-soluble polyurethane technical field.It mainly solves the problems, such as that existing product is present and crushes fragile cutter and the dissolving time-consuming power consumption of slurrying.It is mainly characterized by：Pillar recovery, ethylene glycol, water-soluble monomer and catalyst are mixed and put into fritting kettle in proportion, carries out fritting reaction；Then material is imported into terminal polymerization kettle, steps up vacuum in kettle and and be finally reached below absolute pressure 133Pa.Now temperature of reaction kettle may proceed to raise, and when kettle temperature reaches 275 ± 2 DEG C, power of agitator about 10KW, reaction terminates；Polymeric kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.1 ~ 0.2MPa, is kept stirring for 5 10 minutes, polymer is released in hopper；After natural cooling, foamed material block is broken into strong crusher powdered.The present invention has the characteristics of reducing broken difficulty, improving dissolution velocity and be energy-saving, is mainly used in the preparation of expansion type polyester pulp.
Description
Technical field
The invention belongs to water-soluble polyurethane preparing technical field, and in particular to a kind of preparation of expansion type polyester pulp
Method.
Background technology
Polyester（PET）In the common production technology of product, by vacuumizing ethylene glycol of being had more than needed in removal system, carried with reaching
HMW, reach the purpose of condensation polymerization, after polymerization terminates, extrusion is cooled to particle or bulk, and polymer is fine and close, also favorably
In product in follow-up melt production, facilitate compaction of the material, produce qualified polyester product（Including chemical fibre, sheet material, membrane material
Etc.）.The production of polyester pulp, the production technology of usual polyester is continued to use, product is fine and close, such product, is unfavorable for molten
Solution, moreover, in broken process, because product is fine and close, intensity is larger, increases broken difficulty, consumes mass energy.
In production, application process in other materials, there is foaming handling process, to meet different product requirements, such as：In
State's patent：CN201110192218.8, a kind of preparation method of polyester for foaming.Chinese patent：CN201110259267.9, one
The preparation of kind waterborne polyurethane foaming slurry.Expanded polyester is as described above, purposes is different from this patent purpose in the prior art, and
And implementation is more complicated.
In the prior art polyester pulp as described above, shortcoming clearly：（1）Pulverizing process often damages cutter；（2）It is molten
Slurrying process is solved, expends a large amount of steam, the slurrying time is longer.
The content of the invention
The purpose of the present invention is to be directed to above-mentioned deficiency, there is provided a kind of preparation method of expansion type polyester pulp, was being produced
Foaming processing is carried out in journey, comminution energy conssumption can be reduced；Expanded polyester slurry, the specific surface area of material is increased, increases product
With the contact area of aqueous solvent, product dissolving is more beneficial for.
The present invention technical solution be：A kind of preparation method of expansion type polyester pulp, it is characterised in that including such as
Lower processing step：
（1）By Pillar recovery, ethylene glycol, 10~20% isophthalic two of the Pillar recovery parts by weight 5~10% are accounted for respectively
Formic acid -5- sulfonate or derivatives thereof, 3~15% M-phthalic acid, 0.03~0.15% polycondensation catalyst Sb2O3Mixing
And together put into fritting kettle, the heating of static normal pressure, the fractionation capital temperature incipient stage control of this process reaction kettle 130 DEG C with
Under, when temperature reaches 235 DEG C ± 5 DEG C in reaction, material melts completely, distillates moisture and/or methanol reaches the 90 of theoretical quantity of distillate
When~100%, then interior temperature is raised to 250-260 DEG C, distill out unnecessary ethylene glycol；
（2）After above fritting reaction terminates, material is imported into terminal polymerization kettle, steps up temperature in the kettle since 235 DEG C, when
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and be finally reached 133Pa with
Interior, kettle temperature reaches 275 ± 2 DEG C, polymerize under the conditions of power of agitator 10KW, and then obtains water-soluble polyurethane melt；
（3）Stopping is vacuumized, and polymeric kettle is carried out releasing vacuum with high pure nitrogen and pressurising is to 0.1 ~ 0.2MPa, is pressed herein
5-10 minutes are kept stirring under power, after stirring stops, bottom valve is opened, polymer is released to the melt that foaming is cooled in hopper
Expect block；
（4）After natural cooling, melt material block is set to become enclosed type expanded material；
（5）With strong crusher by foamed material block be broken into it is powdered after, test, measure, pack.
This product is completely dissolved, solubility is 6% ~ 25% before starching with 95 ~ 98 DEG C of running water in the presence of stirring
Between, according to different products, concentration slightly has difference.
The described in the technical solution of the present invention（1）Reactor fractionation capital temperature incipient stage control exists in step
Between 105 DEG C ± 3 DEG C.
The described in the technical solution of the present invention（3）High pure nitrogen is passed through at the top of polymeric kettle in step.
The described in the technical solution of the present invention（5）Foamed material block is broken into directly with strong crusher in step
Footpath is less than 3mm graininess, and outward appearance arrives milky, packing density of particle 0.82-0.84 to be faint yellow.
One of reaction condition of condensation polymerization is under high vacuum state, by volatile component such as ethylene glycol unnecessary in system
Discharge in melt, reach the purpose for improving the degree of polymerization.Reaction terminate after, the viscosity of material is very big, often can reach it is tens of thousands of very
To ten tens of thousands of mPa.S, now, behind stirring blade, deeper whirlpool is often formed.Now, nitrogen is filled with, in stirring
Under effect, nitrogen can be embedded in sticky material with stirring whirlpool, be finally wrapped in melt.After material extrudes cooling,
There are still in material, the cavity closed one by one is formed.After material is broken, cavity largely ruptures therewith, in surface of material
Form hole and cheat concavo-concave convoluted surface pattern, such pattern increases the specific surface area of material.The dissolving of solid matter is first
Diffusion of the solid matter into liquid before this, undoubtedly, increase the contact area of solid-liquid, can accelerating solid material diffusion speed
Degree, so as to contribute to the dissolving of solid matter.
The present invention, using simple equipment, at the end of polymerization, passes through inflated with nitrogen in waterborne polyester slurry process is produced
Mode, melt is internally formed tiny gas bag, because melt film forming is preferable, viscosity is larger, and after extrusion, a large amount of gases are still
It is deposited in inside material, forms multiple air bags, is enclosed type expanded material when not broken.During this material fragmentation, membranous wall phase
To relatively thin, it is easy to it is broken, ultimately form semi-open type expanded material.The material is compared with conventional polyester, specific surface area increase
About 5 times or so.This material belongs to hydrophilic material, and the angle of wetting very little with water, therefore, in down stream dissolution process, water is easy to
Infiltration is in material micropore, with the rise of coolant-temperature gage, accelerates the dissolution velocity of material.
Key point of the present invention is after pet reaction terminates, and by inflated with nitrogen and the operation of stirring, reaches and prepares expanded polyester
The effect of slurry.The present invention, which has, makes polyester pulp crush difficulty reduction, energy-saving, increase specific surface area, increase and solvent
Contact area, improve dissolution velocity and the characteristics of production efficiency.Present invention is mainly used for the preparation of expansion type polyester pulp.
Brief description of the drawings
Fig. 1 is the foaming picture of the present invention.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1：
Preparation method comprises the technical steps that：
（1）Waste and old Pillar recovery plastics 750kg（Within moisture content 6%）、
Ethylene glycol 280kg（Excessive more than 200%）、
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 100kg,
Sb2O3120g,
Above component is mixed and together put into 1.8 cubic cone bottom jacketed kettle polymeric kettles, static normal pressure heating, this
The fractionation capital temperature incipient stage control of process reaction kettle is between 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, thing
Material melting completely, distillate moisture and/or when methanol reaches the 90~100% of theoretical quantity of distillate, then raise interior temperature to 250-260 DEG C,
Distill out unnecessary ethylene glycol；
（2）After above fritting reaction terminates, material is imported into terminal polymerization kettle, steps up temperature in the kettle since 235 DEG C, when
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and and be finally reached absolute pressure
Below power 133Pa.Due to polycondensation reaction category exothermic reaction, and agitating friction heat, reaction temperature may proceed to raise.Kettle temperature reaches
To 275 ± 2 DEG C, it polymerize under the conditions of power of agitator 10KW, this process further removes remaining excessive ethylene glycol, and then obtains
Water-soluble polyurethane melt；
（3）Stopping vacuumizes, and is passed through high pure nitrogen from terminal polymerization kettle bottom and stirs, pressure 0.2MPa in final holding kettle, and 5
Stop stirring after minute and open bottom valve, material is released on stainless steel plate, discharging time 25 minutes, be cooled to the molten of foaming
Body material block；
（4）After natural cooling, melt material block is set to become enclosed type expanded material；
（5）With strong crusher by foamed material block be broken into diameter less than 3mm it is powdered after, crushing process is not sent out smoothly
Raw adhesion, product appearance are milky hard foam particle, packing density of particle 0.82, measure, pack after the assay was approved.
The product prepared using above-mentioned technical process is completely dissolved under agitation before starching with 98 DEG C of running water, is dissolved
25 minutes, solubility 27g time, solution is limpid transparent.
Embodiment 2：
Preparation method comprises the technical steps that：
（1）Waste and old Pillar recovery plastics 750kg（Within moisture content 6%）、
Ethylene glycol 300kg（Excessive more than 240%）、
M-phthalic acid 75kg,
5-sodium sulfo isophthalate 75kg,
Sb2O3120g,
Above component is mixed and together put into 1.8 cubic cone bottom jacketed kettle polymeric kettles, static normal pressure heating, this
The fractionation capital temperature incipient stage control of process reaction kettle is between 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, thing
Material melting completely, distillate moisture and/or when methanol reaches the 90~100% of theoretical quantity of distillate, then raise interior temperature to 250-260 DEG C,
Distill out unnecessary ethylene glycol；
（2）After above fritting reaction terminates, material is imported into terminal polymerization kettle, steps up temperature in the kettle since 235 DEG C, when
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and and be finally reached absolute pressure
Below power 133Pa.Due to polycondensation reaction category exothermic reaction, and agitating friction heat, reaction temperature may proceed to raise.Kettle temperature reaches
To 275 ± 2 DEG C, it polymerize under the conditions of power of agitator 10KW, this process further removes remaining excessive ethylene glycol, and then obtains
Water-soluble polyurethane melt；
（3）Stopping vacuumizes, and is passed through high pure nitrogen from terminal polymerization kettle bottom and stirs, final to keep pressure 0.1MPa in kettle,
Stop stirring after 10 minutes and open bottom valve, material is released on stainless steel plate, discharging time 38 minutes, is cooled to foaming
Melt material block；
（4）After natural cooling, melt material block is set to become enclosed type expanded material；
（5）With strong crusher by foamed material block be broken into diameter less than 3mm it is powdered after, crushing process is not sent out smoothly
Raw adhesion, product appearance arrive milky hard foam particle to be faint yellow, packing density of particle 0.84, counted after the assay was approved
Amount, packaging.
The product prepared using above-mentioned technical process is completely dissolved under agitation before starching with 98 DEG C of running water, is dissolved
28 minutes, solubility 27g time, solution is limpid transparent.
Embodiment 3：
Preparation method comprises the technical steps that：
（1）Waste and old Pillar recovery plastics 800kg（Within moisture content 6%）、
Ethylene glycol 300kg（Excessive more than 180%）、
M-phthalic acid 50kg,
5-sodium sulfo isophthalate 125kg,
Sb2O3120g,
Above component is mixed and together put into 1.8 cubic cone bottom jacketed kettle polymeric kettles, static normal pressure heating, this
The fractionation capital temperature incipient stage control of process reaction kettle is between 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, thing
Material melting completely, distillate moisture and/or when methanol reaches the 90~100% of theoretical quantity of distillate, then raise interior temperature to 250-260 DEG C,
Distill out unnecessary ethylene glycol；
（2）After above fritting reaction terminates, material is imported into terminal polymerization kettle, steps up temperature in the kettle since 235 DEG C, when
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and and be finally reached absolute pressure
Below power 133Pa.Due to polycondensation reaction category exothermic reaction, and agitating friction heat, reaction temperature may proceed to raise.Nei Wenda
To 275 ± 2 DEG C, it polymerize under the conditions of power of agitator 10KW, this process further removes remaining excessive ethylene glycol, and then obtains
Water-soluble polyurethane melt；
（3）Stopping vacuumizes, and is passed through high pure nitrogen from terminal polymerization kettle top and stirs, pressure 0.2MPa in final holding kettle, and 5
Stop stirring after minute and open bottom valve, material is released on stainless steel plate, discharging time 25 minutes, be cooled to the molten of foaming
Body material block；
（4）After natural cooling, melt material block is set to become enclosed type expanded material；
（5）With strong crusher by foamed material block be broken into diameter less than 3mm it is powdered after, crushing process is not sent out smoothly
Raw adhesion, product appearance arrive milky hard foam particle to be faint yellow, packing density of particle 0.83, counted after the assay was approved
Amount, packaging.
The product prepared using above-mentioned technical process is completely dissolved under agitation before starching with 98 DEG C of running water, is dissolved
25 minutes, solubility 27g time, solution is limpid transparent.
Embodiment 4：
Preparation method comprises the technical steps that：
（1）Waste and old Pillar recovery plastics 800kg（Within moisture content 6%）、
Ethylene glycol 320kg（Excessive more than 200%）、
M-phthalic acid 75kg,
5-sodium sulfo isophthalate 125kg,
Sb2O3120g,
Above component is mixed and together put into 1.8 cubic cone bottom jacketed kettle polymeric kettles, static normal pressure heating, this
The fractionation capital temperature incipient stage control of process reaction kettle is between 105 DEG C ± 3 DEG C, when temperature reaches 235 DEG C ± 5 DEG C in reaction, thing
Material melting completely, distillate moisture and/or when methanol reaches the 90~100% of theoretical quantity of distillate, then raise interior temperature to 250-260 DEG C,
Distill out unnecessary ethylene glycol；
（2）After above fritting reaction terminates, material is imported into terminal polymerization kettle, steps up temperature in the kettle since 235 DEG C, when
Stop heating when interior temperature reaches 265 DEG C, while heating, slowly step up in kettle vacuum and and be finally reached absolute pressure
Below power 133Pa.Due to polycondensation reaction category exothermic reaction, and agitating friction heat, reaction temperature may proceed to raise.Kettle temperature reaches
To 275 ± 2 DEG C, it polymerize under the conditions of power of agitator 10KW, this process further removes remaining excessive ethylene glycol, and then obtains
Water-soluble polyurethane melt；
（3）Stopping vacuumizes, and is passed through high pure nitrogen from terminal polymerization kettle top and stirs, pressure 0.1MPa in final holding kettle, and 5
Stop stirring after minute and open bottom valve, material is released on stainless steel plate, discharging time 40 minutes, be cooled to the molten of foaming
Body material block；
（4）After natural cooling, melt material block is set to become enclosed type expanded material；
（5）With strong crusher by foamed material block be broken into diameter less than 3mm it is powdered after, crushing process is not sent out smoothly
Raw adhesion, product appearance arrive milky hard foam particle to be faint yellow, packing density of particle 0.83, counted after the assay was approved
Amount, packaging.
The product prepared using above-mentioned technical process is completely dissolved under agitation before starching with 98 DEG C of running water, is dissolved
30 minutes, solubility 26g time, solution is limpid transparent.
Comparative example 1：
Material is put into 1.8 cubic cone bottom jacketed kettle polymeric kettles in the ratio of embodiment 1, normal vacuum condensation polymerization
Water-soluable sizing material polyester, at the end of reaction, stop stirring, being filled with high pure nitrogen from kettle top finally keeps pressure in kettle
0.2MPa, bottom valve is opened, material is released on stainless steel plate, discharging time 25 minutes.Material is crushed after natural cooling.Adopt
The product prepared with above-mentioned technical process, it will expect that block is broken into powdered, the crushing process that diameter is less than 3mm with strong crusher
Machine utilization is larger, and product does not stick together, and product appearance is yellowish coloured particles, packing density of particle 0.98.98 DEG C of running water
Dissolution time 35 minutes, solubility 27g, solution is limpid transparent.
Comparative example 2：
Material is put into 1.8 cubic cone bottom jacketed kettle polymeric kettles in the ratio of embodiment 3, normal vacuum condensation polymerization
Water-soluable sizing material polyester, at the end of reaction, stop stirring, be filled with high pure nitrogen from bottom portion and finally keep pressure in kettle
0.2MPa, bottom valve is opened, material is released on stainless steel plate, there is the hollow gas of about 5 millimeters of size on melt material block surface once in a while
Bubble, discharging time 25 minutes.Material is crushed after natural cooling.The product prepared using above-mentioned technical process, uses powerful smashing
Machine will expect that block is broken into diameter and is less than the powdered of 3mm, and crushing process machine utilization is larger, and product does not stick together, outside product
See as yellowish coloured particles, bulk density 0.99.98 DEG C of running water dissolution times 35 minutes, solubility 27g, solution is limpid transparent.
Several embodiments more than, before discharging, while stirring, high pure nitrogen no matter is wherefrom filled with, all can
The air bag of closing is formed, pressure is between 0.1 ~ 0.2 MPa.If not being filled with high pure nitrogen, product proportion is larger, and product crushes
Difficulty, energy consumption is higher, and product dissolution time is relatively long.In view of the reliability of operation, preferred scheme is from reactor
Top is filled with nitrogen.
Claims (4)
1. a kind of preparation method of expansion type polyester pulp, it is characterised in that comprise the technical steps that：
（1）By Pillar recovery, respectively account for the ethylene glycol of the Pillar recovery parts by weight 5~10%, 10~20% M-phthalic acid-
5- sulfonate or derivatives thereof, 3~15% M-phthalic acid, 0.03~0.15% polycondensation catalyst Sb2O3Mix and together
To put into fritting kettle, static normal pressure heating, this process reaction kettle fractionation capital temperature incipient stage is controlled below 130 DEG C, when
Temperature reaches 235 DEG C ± 5 DEG C in reaction, and material melts completely, distillates moisture and/or methanol reaches the 90~100% of theoretical quantity of distillate
When, then interior temperature is raised to 250-260 DEG C, distill out unnecessary ethylene glycol；
（2）After above fritting reaction terminates, material is imported into terminal polymerization kettle, temperature in the kettle is stepped up since 235 DEG C, when interior temperature
Stop heating when reaching 265 DEG C, while heating, slowly step up vacuum in kettle and be finally reached within 133Pa, kettle
Temperature reaches 275 ± 2 DEG C, polymerize under the conditions of power of agitator 10kW, and then obtains water-soluble polyurethane melt；
（3）Stopping vacuumizes, and to polymeric kettle release vacuum and pressurising with high pure nitrogen to 0.1 ~ 0.2MPa, at this pressure
5-10 minutes are kept stirring for, after stirring stops, bottom valve is opened, polymer is released to the melt material that foaming is cooled in hopper
Block；
（4）After natural cooling, melt material block is set to become enclosed type expanded material；
（5）With strong crusher by foamed material block be broken into it is powdered after, test, measure, pack.
2. the preparation method of expansion type polyester pulp according to claim 1, it is characterised in that：Described（1）Step
Middle reactor fractionation capital temperature incipient stage control is between 105 DEG C ± 3 DEG C.
3. the preparation method of expansion type polyester pulp according to claim 1 or 2, it is characterised in that：Described（3）Step
High pure nitrogen is passed through at the top of polymeric kettle in rapid.
4. the preparation method of expansion type polyester pulp according to claim 1 or 2, it is characterised in that：Described（5）Step
Foamed material block is broken into graininess of the diameter less than 3mm with strong crusher in rapid, outward appearance arrives milky, particle to be faint yellow
Bulk density 0.82-0.84 g/cm3。
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| CN112852117B (en) * | 2021-03-11 | 2022-05-24 | 湖北山特莱新材料有限公司 | High-temperature-resistant water-soluble polyester slurry |
| CN113185681B (en) * | 2021-04-28 | 2022-08-12 | 湖北山特莱新材料有限公司 | Preparation method of foaming type polyester slurry |
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 |
-
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 |
Non-Patent Citations (1)
| Title |
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| "乙二醇醇解法回收涤纶废丝制备聚酯浆料的研究";李准准等;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20090315(第3期);B024-8 * |
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Inventor after: Chen Chunhua Inventor after: Zhou Zhongxu Inventor before: Wei Jinhong Inventor before: Chen Chunhua Inventor before: Sun Jinglun Inventor before: Zhou Zhongxu |
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Effective date of registration: 20171211 Address after: 441403 Lei Yan Avenue in Lehe Town, Yicheng, Xiangyang, Hubei Applicant after: Hubei Santak New Material Co.,Ltd. Address before: 441403 Lei Road, Lei Da Industrial Park, Lei Town, Xiangfan City, Hubei, Yicheng Applicant before: HUBEI JIATE WEAVING SLURRY Co.,Ltd. |
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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 |