CN115886034A - Preparation method of superfine natural oyster shell powder for polyester fibers - Google Patents
Preparation method of superfine natural oyster shell powder for polyester fibers Download PDFInfo
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- CN115886034A CN115886034A CN202211356423.8A CN202211356423A CN115886034A CN 115886034 A CN115886034 A CN 115886034A CN 202211356423 A CN202211356423 A CN 202211356423A CN 115886034 A CN115886034 A CN 115886034A
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- 239000000843 powder Substances 0.000 title claims abstract description 89
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 86
- 239000000835 fiber Substances 0.000 title claims abstract description 30
- 229920000728 polyester Polymers 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000001694 spray drying Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000428 dust Substances 0.000 claims abstract description 11
- 238000009826 distribution Methods 0.000 claims abstract description 5
- 239000004744 fabric Substances 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 241000237502 Ostreidae Species 0.000 claims description 4
- 235000020636 oyster Nutrition 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 239000003242 anti bacterial agent Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 241000276489 Merlangius merlangus Species 0.000 claims 3
- 238000005119 centrifugation Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000000703 high-speed centrifugation Methods 0.000 claims 1
- 238000010902 jet-milling Methods 0.000 claims 1
- 238000002386 leaching Methods 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 238000001238 wet grinding Methods 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 9
- 230000003385 bacteriostatic effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
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- 238000004806 packaging method and process Methods 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 230000001954 sterilising effect Effects 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 239000011701 zinc Substances 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 239000004576 sand Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004594 Masterbatch (MB) Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000015170 shellfish Nutrition 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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- 239000002910 solid waste Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
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Abstract
The present invention belongs to the field of chemical technology. The invention relates to a preparation technology of high-dispersity natural oyster shell powder for polyester fiber. The natural oyster shell powder contains a large amount of zinc element, can be used as a natural antibacterial additive to be added into the polyester chemical fiber to play a role in sterilization and bacteriostasis, and has a certain mite prevention effect. Due to the technological requirements of polyester fiber application, natural oyster shell powder must be prepared into oyster shell powder master batches in advance through a screw machine. The slurry of the superfine oyster shell powder can not be directly used and must be prepared into powder with low water content and high dispersibility. The invention uses a spray drying method to instantly dry the superfine oyster shell powder water slurry with the concentration of about 40 percent, and then collects the superfine oyster shell powder water slurry through pulse dust removal; and crushing the collected dry powder through airflow, and then packaging for later use. The prepared superfine oyster shell powder has the particle size distribution of 1.3-10 um, the average particle size of 3.0-4.0 um and excellent dispersibility, can be directly granulated by a double screw and is used for a polyester fiber slicing method. The superfine oyster shell powder is added into the polyester fiber according to a certain proportion for use, so that the antibacterial and bacteriostatic ability of the fiber can be obviously improved; and can improve the spinnability of the fiber to a certain extent and reduce the generation of static electricity.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to high-dispersity superfine natural oyster shell powder and a dispersing preparation method thereof.
Background
Oyster shell, also known as oyster shell, is a shellfish solid waste with high yield in coastal areas. In recent years, as the market demand for marine shellfish products has been expanding, the scale of shellfish culture and the production and processing ability, as typified by oysters, have been greatly improved. However, while satisfying and improving people's lives, the huge oyster market is also hidden with various environmental pollution and potential safety hazards caused by oyster shell waste. A considerable portion of the large amount of shell waste produced is not effectively utilized and properly disposed of. Therefore, development, processing and utilization of oyster shells have become a research focus and an environmental issue in recent years.
The oyster shell powder has natural antibacterial effect by using metal oxide such as zinc oxide. With the recent increasing demand for health and hygiene, the demand for antibacterial fibers has increased dramatically. Oyster shell powder has been gradually recognized as a natural antibacterial ingredient. As a good substitute of zinc oxide antibacterial agent, the inventor already patents that superfine oyster shell powder aqueous slurry is prepared by aiming at viscose fiber application. The aqueous oyster shell powder slurry can be directly used in viscose fibers (added by melt) or other aqueous coatings to improve the long-acting antibacterial property and the bacteriostatic action of the fibers or coatings.
The use of aqueous slurries is limited by many processes, such as polyester fiber, which is the largest market in the fiber industry. The polyester fiber is obtained by combining PTA and ethylene glycol at high temperature without any addition of water. Therefore, the development of ultrafine oyster shell powder for polyester fibers is becoming urgent.
In conclusion, the prepared special high-dispersity ultrafine oyster shell powder is vital to improving the antibacterial and bacteriostatic performance of the polyester fiber product, and is also beneficial to reducing the use of industrially prepared zinc oxide and reducing the fiber cost. The superfine oyster shell powder has great market potential demand. However, the processing of the oyster shell powder in China is only in the starting stage at present, the particles of the oyster shell powder are relatively thick and wide in distribution, and the oyster shell powder is mainly used in agriculture, forestry, fishery and grazing industries and building material industries. At present, few patent documents are reported on ultrafine oyster shell powder dispersion research, particularly oyster shell powder for polyester fibers. However, there have been reported cases of applying natural oyster shell powder for antibacterial polyester fiber. The technology hopes to make up the blank of domestic natural oyster shell powder in the polyester fiber industry and develop the differential and functional application of the natural oyster shell powder.
Disclosure of Invention
The invention aims to provide high-dispersity ultrafine oyster shell powder for polyester fibers and a preparation method thereof.
The superfine oyster shell powder slurry used by the invention consists of deionized water, natural oyster shell coarse powder, a dispersing agent and a coating agent, and the contents of the components are as follows: :
wherein, the oyster shell powder is crushed and cleaned coarse powder (50-100 um), the dispersant is a hydrophilic anionic dispersant, and the organic coating agent is a neutral high-molecular-weight coating agent.
The preparation method of the high-dispersity natural oyster shell powder for the polyester fiber comprises the following specific steps:
(1) Preparing water dispersion slurry of superfine oyster shell powder: mixing 40wt% of oyster shell powder, water, all the coating agents and the dispersing agents according to the formula, and circularly sanding the mixture through a horizontal sand mill to obtain the superfine oyster shell powder slurry. The slurry has average particle size of 400-900nm and maximum particle size less than 3000nm. The obtained slurry has a viscosity of 2000-4000 cps. And (4) throwing the sanded slurry into a preparation tank, and stirring at a low speed to keep uniform.
(2) Plate and frame filter pressing and washing: because of the excess dispersant in the slurry, the slurry needs to be washed to control its conductivity. A semi-automatic plate-and-frame filter press is adopted, wherein the filter cloth is 10000mm 60mm, the filter cloth is polyester long-fiber filter cloth, and the air permeability of the filter cloth is 20. And (3) dehydrating the superfine oyster shell powder slurry in the preparation tank through a plate-and-frame filter press, adding the obtained oyster shell powder filter cake into a washing tank, and adding deionized water to stir and soak for 4-8 hours. The operation is carried out twice, and finally deionized water is used for blending to 40% concentration, and the conductivity is detected to be qualified when the conductivity is less than 300 us/cm. If the conductivity is not qualified, the washing steps are continuously repeated until the conductivity is qualified, and the washing is finished.
(3) And (3) spray drying process: and (4) pumping qualified oyster shell powder slurry obtained by plate-and-frame filter pressing and washing into a spray tank. Drying and dehydrating by a spray drying tower, wherein the spray drying tower adopts saturated steam as a heat source, the steam pressure is 8-12 kg/cm < 2 >, the height of the spray drying tower is 8-12 meters, and the centrifugal rotating speed is 10000-15000 rpm. During the drying process, the change of the steam pressure is monitored, and incomplete drying and excessive moisture content can be caused by excessively low pressure. In addition, the inner wall of the spray tower needs to be cleaned regularly, so that the wall sticking phenomenon of powder is reduced as much as possible. And (3) periodically cleaning and collecting oyster shell powder aggregates or large particles falling from the spraying tower, returning to the sand milling process, and re-grinding to prepare the oyster shell powder water dispersion slurry.
(4) Pulse dust removal and collection: the cloth bag is made of 400-mesh needled felt antistatic filter cloth, the diameter of the cloth bag is 120 × 1000mm, the number of the cloth bags is 32, and the filter area is 12.5m 2 . Periodically sampling and testing the water content of the dried superfine oyster shell powder-<0.2％.
(5) And (3) airflow crushing process: after spray drying, certain oyster shell powder is still agglomerated. In order to further reduce the formation of large particle aggregates and improve the usability of the powder in the subsequent granulation process, the dried oyster shell powder is crushed by a jet type airflow crushing device. Adjusting the pressure of a feed nozzle to 0.3-0.4 MPa by an air compressor; the pressure of the crushing nozzle is about 0.6 MPa. The feed rate can be adjusted. And finally, collecting through a cyclone dust collector. The average grain diameter of the oyster shell powder is 3.0-4.0 um, and the maximum grain diameter is less than 10um.
It is shown that after drying, the superfine oyster shell powder still generates a certain aggregate. However, the aggregate treated by the process of the invention is easy to disperse in a polyester system under the double-screw dispersion condition, and can be made into a superfine oyster shell powder master batch with the concentration of 10-20%. The master batch can be prepared into the oyster shell powder modified polyester fiber together with PET chip particles in a chip spinning mode.
The superfine oyster shell powder prepared by the invention has the following advantages:
(1) the superfine natural oyster shell powder prepared by the invention is mainly distributed in 1.3-10 um, has the average grain diameter of 3.0-4.0 um and narrow grain diameter distribution, and the maximum grain diameter is not more than 10um. As shown in fig. 1.
(2) The superfine natural oyster shell powder prepared by the invention is easy to disperse and process, and can be prepared into master batches with the concentration of 10-20% together with PET slices in a double-screw granulation process. The master batch is added into polyester fiber slices for long-acting antibacterial and bacteriostatic effects.
(3) The superfine natural oyster shell powder prepared by the invention has low water content of less than 0.2 percent.
Drawings
FIG. 1 is a diagram showing the results of particle size tests of the ultrafine oyster shell slurry prepared according to the present invention.
FIG. 2 is a flow chart of a preparation process of ultrafine oyster shell powder
Detailed Description
(1) Preparing water dispersion slurry of superfine oyster shell powder: mixing 40wt% of oyster shell powder, water, all the coating agents and the dispersing agents according to the formula, and circularly sanding the mixture through a horizontal sand mill to obtain the superfine oyster shell powder slurry. The slurry has average particle size of 400-900nm and maximum particle size less than 3000nm. The obtained slurry has a viscosity of 2000-4000 cps. And (4) throwing the sanded slurry into a preparation tank, and stirring at a low speed to keep uniform.
(2) Plate and frame filter pressing and washing: because of the excess dispersant in the slurry, the slurry needs to be washed to control its conductivity. A semi-automatic plate-and-frame filter press is adopted, wherein the filter cloth is 10000mm 60mm, the filter cloth is polyester long-fiber filter cloth, and the air permeability of the filter cloth is 20. And (3) dehydrating the superfine oyster shell powder slurry in the preparation tank through a plate-and-frame filter press, adding the obtained oyster shell powder filter cake into a washing tank, and adding deionized water to stir and soak for 4-8 hours. The operation is carried out twice, and finally deionized water is used for blending to 40% concentration, and the conductivity is detected to be qualified when the conductivity is less than 300 us/cm. If the conductivity is not qualified, the washing steps are continuously repeated until the conductivity is qualified, and the washing is finished.
(3) And (3) spray drying process: and (4) pumping the qualified oyster shell powder slurry obtained by plate-and-frame filter pressing and washing into a spraying tank. Drying and dehydrating by a spray drying tower, wherein the spray drying tower adopts saturated steam as a heat source, the steam pressure is 8-12 kg/cm < 2 >, the height of the spray drying tower is 8-12 meters, and the centrifugal rotating speed is 10000-15000 rpm. During the drying process, the change of the steam pressure is monitored, and incomplete drying and excessive moisture content can be caused by excessively low pressure. In addition, the inner wall of the spray tower needs to be cleaned regularly, so that the wall sticking phenomenon of powder is reduced as much as possible. And (3) periodically cleaning and collecting oyster shell powder aggregates or large particles falling from the spraying tower, returning to the sand milling process, and re-grinding to prepare the oyster shell powder water dispersion slurry.
(4) Pulse dust removal and collection: the cloth bag is made of 400-mesh needled felt antistatic filter cloth, the diameter of the cloth bag is 120 × 1000mm, the number of the cloth bags is 32, and the filter area is 12.5m 2 . Regular sampling is carried out to test the water content-<0.2％.
(5) And (3) airflow crushing process: after spray drying, certain oyster shell powder is still agglomerated. In order to further reduce the formation of large particle aggregates and improve the usability of the powder in the subsequent granulation process, the dried oyster shell powder is crushed by a jet type airflow crushing device. Adjusting the pressure of a feed nozzle to 0.3-0.4 MPa by an air compressor; the pressure of the crushing nozzle is about 0.6 MPa. The feed rate can be adjusted. And finally, collecting through a cyclone dust collector. The average grain diameter of the oyster shell powder is 3.0-4.0 um, and the maximum grain diameter is less than 10um.
Claims (9)
1. A high-dispersity superfine natural oyster shell powder is obtained by carrying out spray drying, pulse dust collection and airflow crushing on superfine natural oyster shell powder slurry prepared by carrying out wet grinding on my oyster, wherein the superfine natural oyster shell powder slurry consists of natural oyster shell powder coarse powder (50-100 um), a coating agent, a dispersing agent and deionized water, and is characterized by comprising the following components in percentage by weight:
wherein the oyster shell powder is crushed and cleaned coarse powder (50-100 um), the dispersant is a hydrophilic anionic dispersant, and the organic coating agent is a neutral high-molecular-weight coating agent.
2. The preparation of the highly dispersible natural oyster shell powder according to claim 1 comprises the following steps of (1) preparing an ultrafine oyster shell powder slurry: firstly, preparing slurry of ultrafine oyster shell powder with the concentration of 40wt% in water by sanding, detecting that the median particle size distribution reaches the requirement of 400-900nm, and then pumping the slurry into a preparation tank;
(2) Plate and frame filter pressing and washing: dehydrating the superfine oyster shell powder slurry in the preparation tank through a plate-and-frame filter press, adding the obtained oyster shell powder filter cake into a washing tank, adding deionized water, stirring, leaching and washing for 4-8 hours, performing the operation twice, and finally blending to 40% concentration by using the deionized water, and detecting that the conductivity is qualified when the conductivity is less than 300 us/cm;
(3) And (3) spray drying: pumping the oyster shell powder slurry washed in the step (2) into a spray tank through a pressure pump, and keeping stirring at a low speed; drying the slurry by a spray drying tower, wherein the steam pressure is 8-12 kg/cm < 2 > and the height of the spray tower is 8-12 m;
(4) Pulse dust removal and collection: collecting dry powder from a spray tower by a pulse dust removal belt, wherein the material of a cloth bag is 400-mesh needled felt anti-static filter cloth, and the water content of the place is less than 0.2% in a sampling test;
(5) Airflow crushing: the superfine oyster shell powder collected in the previous step is subjected to the last step of crushing by a jet mill, so that the superfine oyster shell powder is prevented from agglomerating in the drying process, and finally collected by a cyclone collector and a bag-type dust collector and then packaged.
3. The highly stable and highly dispersible natural oyster shell whiting slurry according to claim 1 is characterized by comprising natural oyster shell whiting coarse powder (50-100 um), a coating agent, a dispersing agent and deionized water, and is characterized in that the contents of the components are as follows:
4. the highly stable and highly dispersible aqueous dispersion of natural oyster shell whiting according to claim 2, wherein the dispersion has a median particle size distribution of 400 to 900nm and a viscosity of 2000 to 4000cps (1 cps = 1mpas).
5. The plate-and-frame filter-press cleaning method according to claim 2, wherein the semi-automatic plate-and-frame filter press is 1000mm by 60mm, and the filter cloth is polyester filament filter cloth.
6. The spray-drying process according to claim 2, wherein the spray-drying is carried out by high-speed centrifugation using saturated steam as a heat source, the steam pressure being 8 to 12kg/cm2, the height of the spray tower being 8 to 12 m, and the centrifugation speed being 10000 to 15000rpm.
7. The pulse dust collector as claimed in claim 2, wherein the cloth bag is made of 400-mesh needle felt antistatic filter cloth, the diameter of the cloth bag is 120 x 1000mm, the number of the cloth bags is 32, and the filtering area is 12.5m 2 。
8. The jet milling process as claimed in claim 2, wherein the ultra-fine oyster shell powder is collected by a jet mill, a cyclone collector and a bag-type dust collector, and the average particle size of the ultra-fine oyster shell powder is 3.0-4.0 um, and the maximum particle size is less than 10um.
9. The highly dispersible natural oyster shell powder according to claim 1 or 2, which can be processed by twin screw and then added to polyester fiber, and then spun to form the long-acting antibacterial agent for fiber.
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| CN202211356423.8A CN115886034A (en) | 2022-11-01 | 2022-11-01 | Preparation method of superfine natural oyster shell powder for polyester fibers |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117683374A (en) * | 2024-02-01 | 2024-03-12 | 爱可比(苏州)新材料有限公司 | Superfine natural oyster shell powder slurry, preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117683374A (en) * | 2024-02-01 | 2024-03-12 | 爱可比(苏州)新材料有限公司 | Superfine natural oyster shell powder slurry, preparation method and application thereof |
| CN117683374B (en) * | 2024-02-01 | 2024-05-03 | 爱可比(苏州)新材料有限公司 | Superfine natural oyster shell powder slurry, preparation method and application thereof |
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