CN112552660A - Preparation method and application of polylactic resin capable of adsorbing water and oil amphiprotic - Google Patents

Preparation method and application of polylactic resin capable of adsorbing water and oil amphiprotic Download PDF

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CN112552660A
CN112552660A CN202011307304.4A CN202011307304A CN112552660A CN 112552660 A CN112552660 A CN 112552660A CN 202011307304 A CN202011307304 A CN 202011307304A CN 112552660 A CN112552660 A CN 112552660A
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polylactic acid
polylactic
antioxidant
oil
water
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董芬芬
赵羽
孔晓东
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Anhui Yuanchen Environmental Protection Science and Technology Co Ltd
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Anhui Yuanchen Environmental Protection Science and Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/407—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties containing absorbing substances, e.g. activated carbon
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4326—Condensation or reaction polymers
    • D04H1/435—Polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/06—Biodegradable
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/12—Applications used for fibers

Abstract

The invention discloses a preparation method of polylactic resin capable of adsorbing water and oil, which comprises the following steps: adding polylactic acid into a sodium hydroxide solution, and performing ultrasonic dispersion to form a suspension; introducing the suspension into an ozone reaction tower, and introducing ozone for treatment to prepare a mixed solution; and pouring out the mixed solution after the treatment, filtering out particles, carrying out vacuum drying on the particles to obtain modified polylactic acid particles, adding sodium polyacrylate and an antioxidant, uniformly mixing, and then placing on a double-screw extruder for granulation to obtain the polylactic resin. The invention has the beneficial effects that: according to the invention, after the surface oxidation treatment is carried out on polylactic acid by using ozone, a non-polar surface is changed into a local polar surface, so that oxygen-containing functional groups on the surface of the polylactic acid are increased, mainly hydroxyl functional groups are increased, the water absorption and oil absorption functions of the prepared polylactic acid resin are obviously improved, the water absorption multiplying power distilled water index can reach more than 200g/g, and the biodegradability is kept better.

Description

Preparation method and application of polylactic resin capable of adsorbing water and oil amphiprotic
Technical Field
The invention relates to the technical field of plastic modification, in particular to a preparation method and application of polylactic resin capable of adsorbing water and oil amphiprotic substances.
Background
High oil absorption resin, polypropylene fiber, polyurethane foam and the like are common chemical synthesis oil absorption materials. In recent years, with the rapid development of the nonwoven fabric industry, nonwoven fabric-type oil absorbing materials have started to be developed, and polypropylene meltblown nonwoven fabrics have become the ideal oil absorbing materials recognized in the industry. However, with the push of national environmental protection policy, polypropylene and polyurethane oil absorption materials can not be degraded, and the application of degradable biological material PLA (polylactic acid) in oil absorption is not reported.
Patent CN105440605A discloses a polylactic acid resin, which provides a polylactic acid resin containing aliphatic-aromatic copolyester segment, and enhances the flexibility of the polylactic acid resin. Patent CN103937012A discloses a method for producing polylactic acid resin fine particles, porous polylactic acid resin fine particles having a small particle size and a high oil absorption suitable for cosmetic applications, spherical lactic acid resin fine particles having a narrow particle size distribution and smooth surface suitable for toner applications, and cosmetics using these polylactic acid resin fine particles.
The problems with the above technique are as follows: due to the fact that a large number of ester bonds are contained in polylactic acid, hydrophilicity is poor, and water absorption and water locking are to be improved.
Disclosure of Invention
The invention aims to provide a preparation method of polylactic resin which has good hydrophilicity and stable biodegradability and can absorb water and oil amphipathy.
The invention solves the technical problems through the following technical means:
a preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding polylactic acid into a sodium hydroxide solution according to the mass ratio of 1:1-1:3, and performing ultrasonic dispersion to form a suspension;
(2) introducing the suspension prepared in the step (1) into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 10-20mg/min, the flow rate is 1-3L/min, and the treatment time is 10-20min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and vacuum-drying the particles at 50-80 ℃ for 24-36h to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and an antioxidant into the modified polylactic acid granules prepared in the step (3) according to the mass ratio of 30:60:1:1-30:60:1:13, uniformly mixing, and then placing on a double-screw extruder for granulation to prepare the polylactic resin.
The invention uses ozone to carry out surface oxidation treatment on polylactic acid, changes a non-polar surface into a local polar surface, increases oxygen-containing functional groups on the surface, mainly increases hydroxyl functional groups, and the polylactic acid modified by ozone and sodium polyacrylate are granulated and melt-blown, so that the prepared polylactic acid resin has obviously improved water and oil absorption functions, the water absorption rate and distilled water index can reach more than 200g/g, and the biodegradability also keeps better.
Preferably, the polylactic acid comprises one or more of dextrorotatory polylactic acid, levorotatory polylactic acid, racemic polylactic acid and polylactic acid stereocomplex.
Preferably, the particle size of the polylactic acid is 100-300 meshes.
Preferably, the antioxidant is a main antioxidant and an auxiliary antioxidant;
the main antioxidant comprises one or more of antioxidant 168 and antioxidant 1010;
the auxiliary antioxidant comprises one or more of antioxidant 1330 and antioxidant 1076.
Preferably, the acrylic acid monomer residual amount in the sodium polyacrylate is 200-300 ppm.
Preferably, the granulation process parameters of the twin-screw extruder in the step (4) are set as follows:
Figure BDA0002788663400000031
the invention also provides an application of the polylactic resin prepared by the preparation method of the polylactic resin capable of adsorbing water and oil, which comprises the following steps:
(a) determining the size of the holes of the melt-blowing equipment, checking the single-screw melt-blowing machine, assembling a spinneret, switching on a power supply and preheating;
(b) adjusting the temperature of each section of the melt-blowing equipment to the required set temperature of 170-230 ℃, and keeping the temperature for 30 min;
(c) uniformly mixing the prepared polylactic resin and the polylactic acid flow increasing agent according to the mass ratio of 100:0.5-100: 3;
(d) and (3) opening a metering pump, starting a screw rod, adding the mixture obtained in the step (c) into a screw extruder for melting treatment, feeding the melt into a rectangular spinneret plate through the screw rod and the metering pump, feeding the melt onto a receiving device through high-pressure high-temperature hot air, cooling and solidifying to form a cloth cover, winding, and cutting into melt-blown non-woven fabrics.
Further, the size of the hole is 0.25-0.35 mm.
Further, the hot air pressure is 60-90kPa, and the temperature is 200-280 ℃.
Further, the polylactic acid resin is used in a melt-blowing process, high-speed spinning and fine fibers of a nonwoven fabric.
The invention has the following beneficial effects:
1. the invention uses ozone to carry out surface oxidation treatment on polylactic acid, changes a non-polar surface into a local polar surface, increases oxygen-containing functional groups on the surface, mainly increases hydroxyl functional groups, and the polylactic acid modified by ozone and sodium polyacrylate are granulated and melt-blown, so that the prepared polylactic acid resin has obviously improved water and oil absorption functions, the water absorption rate and distilled water index can reach more than 200g/g, and the biodegradability also keeps better.
2. The method can uniformly introduce oxygen-containing groups on the surface of a complex polymer through ozone treatment, does not need chemical reagents, does not generate polluting residual byproducts, and has simple equipment and simple operation.
3. The product prepared by using the polylactic resin can be widely applied to the field of non-woven fabrics, can ensure the processing performance and the use performance of materials in various aspects, can reduce white pollution compared with the existing polypropylene melt-blown fabric, and meets the requirement of environmental protection.
Drawings
FIG. 1 is a schematic view of the structure of an ozone treatment apparatus according to embodiment 1 of the present invention;
FIG. 2 is an infrared spectrum of the polylactic acid subjected to ozone treatment in example 5 of the present invention and the polylactic acid not subjected to ozone treatment in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
A preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding polylactic acid into a sodium hydroxide solution according to the mass ratio of 1:1-1:3, and performing ultrasonic dispersion to form a suspension;
(2) introducing the suspension prepared in the step (1) into an ozone reaction tower of an ozone treatment device, wherein the ozone treatment device is shown in figure 1, introducing ozone for treatment, the mass percentage concentration of the introduced ozone is 10-20mg/min, the flow rate is 1-3L/min, and the treatment time is 10-20min, so as to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and vacuum-drying the particles at 50-80 ℃ for 24-36h to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and an antioxidant into the modified polylactic acid granules prepared in the step (3) according to the mass ratio of 30:60:1:1-30:60:1:13, uniformly mixing, and then placing on a double-screw extruder for granulation to prepare the polylactic resin.
The polylactic acid comprises one or more of dextro-polylactic acid, levorotatory polylactic acid, racemic polylactic acid and polylactic acid stereo complex.
The particle size of the polylactic acid is 100-300 meshes.
The antioxidant is a main antioxidant and an auxiliary antioxidant;
the main antioxidant comprises one or more of antioxidant 168 and antioxidant 1010;
the auxiliary antioxidant comprises one or more of antioxidant 1330 and antioxidant 1076.
Preferably, the acrylic acid monomer residual amount in the sodium polyacrylate is 200-300 ppm.
Preferably, the granulation process parameters of the twin-screw extruder in the step (4) are set as follows:
Figure BDA0002788663400000061
example 1
A preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding 10 parts of 100-mesh polylactic acid of 110 brands produced by Zhejiang Haizhizheng biological pharmacy into 20 parts of sodium hydroxide solution, and performing ultrasonic dispersion to form suspension;
(2) introducing the prepared suspension into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 10mg/min, the flow rate is 1L/min, and the treatment time is 10min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and carrying out vacuum drying at the temperature of 50 ℃ for 24 hours to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and antioxidant into the obtained modified polylactic acid granule, wherein the particle size of the sodium polyacrylate is 20 meshes, the antioxidant 1010 is 1 part, and the antioxidant 1330 is 0.1 part; the residual amount of acrylic acid monomer in the sodium polyacrylate is 200 ppm; and after being uniformly mixed, the mixture is placed on a double-screw extruder for granulation to prepare the polylactic resin.
The granulation process parameters of the double-screw extruder are as follows:
the temperature of the material section is 90 ℃; the temperature of the first barrel area is 180 ℃, the temperature of the second barrel area is 200 ℃, the temperature of the third barrel area is 230 ℃ and the temperature of the fourth barrel area is 230 ℃; the temperature of a die head is 180 ℃; the temperature of cooling water is 20 ℃; the screw extrusion speed is 200 rpm/min; the drawing speed of the wire drawing material is 10 m/min.
Example 2
A preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding 10 parts of polylactic acid of 200 meshes of 110 brands produced by Zhejiang Haizhizheng biological pharmacy into 20 parts of sodium hydroxide solution, and performing ultrasonic dispersion to form suspension;
(2) introducing the prepared suspension into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 20mg/min, the flow rate is 1L/min, and the treatment time is 10min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and carrying out vacuum drying at the temperature of 50 ℃ for 24 hours to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and antioxidant into the obtained modified polylactic acid granule, wherein the particle size of the sodium polyacrylate is 20 meshes, the antioxidant 1010 is 1 part, and the antioxidant 1330 is 0.1 part; the residual amount of acrylic acid monomer in the sodium polyacrylate is 200 ppm; and after being uniformly mixed, the mixture is placed on a double-screw extruder for granulation to prepare the polylactic resin.
The granulation process parameters of the double-screw extruder are as follows:
the temperature of the blanking section is 90 ℃; the temperature of the first barrel area is 180 ℃, the temperature of the second barrel area is 200 ℃, the temperature of the third barrel area is 230 ℃ and the temperature of the fourth barrel area is 230 ℃; the temperature of a die head is 180 ℃; the temperature of cooling water is 20 ℃; the screw extrusion speed is 200 rpm/min; the drawing speed of the wire drawing material is 10 m/min.
Example 3
A preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding 10 parts of 300-mesh polylactic acid of 110 brands produced by Zhejiang Haizhizheng biological pharmacy into 20 parts of sodium hydroxide solution, and performing ultrasonic dispersion to form suspension;
(2) introducing the prepared suspension into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 30mg/min, the flow rate is 2L/min, and the treatment time is 10min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and carrying out vacuum drying at the temperature of 50 ℃ for 36h to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and antioxidant into the prepared modified polylactic acid granules, wherein the particle size of the sodium polyacrylate is 40 meshes, the antioxidant 1010 is 1 part, and the antioxidant 1330 is 0.1 part; the residual amount of acrylic acid monomer in the sodium polyacrylate is 200 ppm; and after being uniformly mixed, the mixture is placed on a double-screw extruder for granulation to prepare the polylactic resin.
The granulation process parameters of the double-screw extruder are as follows:
the temperature of the blanking section is 90 ℃; the temperature of the first barrel area is 180 ℃, the temperature of the second barrel area is 200 ℃, the temperature of the third barrel area is 230 ℃ and the temperature of the fourth barrel area is 230 ℃; the temperature of a die head is 180 ℃; the temperature of cooling water is 20 ℃; the screw extrusion speed is 200 rpm/min; the drawing speed of the wire drawing material is 10 m/min.
Example 4
A preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding 10 parts of 300-mesh polylactic acid of 110 brands produced by Zhejiang Haizhizheng biological pharmacy into 20 parts of sodium hydroxide solution, and performing ultrasonic dispersion to form suspension;
(2) introducing the prepared suspension into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 30mg/min, the flow rate is 1L/min, and the treatment time is 20min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and carrying out vacuum drying at the temperature of 60 ℃ for 24h to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and antioxidant into the obtained modified polylactic acid granules, wherein the particle size of the sodium polyacrylate is 60 meshes, the antioxidant 1010 is 1 part, and the antioxidant 1330 is 0.1 part; the residual amount of acrylic acid monomer in the sodium polyacrylate is 200 ppm; and after being uniformly mixed, the mixture is placed on a double-screw extruder for granulation to prepare the polylactic resin.
The granulation process parameters of the double-screw extruder are as follows:
the temperature of the blanking section is 90 ℃; the temperature of the first barrel area is 180 ℃, the temperature of the second barrel area is 200 ℃, the temperature of the third barrel area is 230 ℃ and the temperature of the fourth barrel area is 230 ℃; the temperature of a die head is 180 ℃; the temperature of cooling water is 20 ℃; the screw extrusion speed is 200 rpm/min; the drawing speed of the wire drawing material is 20 m/min.
Example 5
A preparation method of polylactic resin capable of adsorbing water and oil amphiprotic substances comprises the following steps:
(1) adding 10 parts of 300-mesh polylactic acid of 110 brands produced by Zhejiang Haizhizheng biological pharmacy into 20 parts of sodium hydroxide solution, and performing ultrasonic dispersion to form suspension;
(2) introducing the prepared suspension into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 30mg/min, the flow rate is 3L/min, and the treatment time is 30min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and carrying out vacuum drying at the temperature of 50 ℃ for 36h to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and antioxidant into the obtained modified polylactic acid granule, wherein the particle size of the sodium polyacrylate is 80 meshes, the antioxidant 1010 is 1 part, and the antioxidant 1330 is 0.1 part; the residual amount of acrylic acid monomer in the sodium polyacrylate is 200 ppm; and after being uniformly mixed, the mixture is placed on a double-screw extruder for granulation to prepare the polylactic resin.
The granulation process parameters of the double-screw extruder are as follows:
the temperature of the blanking section is 90 ℃; the temperature of the first barrel area is 180 ℃, the temperature of the second barrel area is 200 ℃, the temperature of the third barrel area is 230 ℃ and the temperature of the fourth barrel area is 230 ℃; the temperature of a die head is 180 ℃; the temperature of cooling water is 20 ℃; the screw extrusion speed is 200 rpm/min; the drawing speed of the wire drawing material is 20 m/min.
Comparative example 1
Unlike example 1, this comparative example directly melt-blown 110 parts of 300 mesh polylactic acid manufactured by Zhejiang Haizhizheng biopharmaceutical industry.
Comparative example 2
Different from the embodiment 1, in the comparative example, 10 parts of 300-mesh polylactic acid of 110 brands produced by Zhejiang Haizhizheng biological pharmacy is added into 20 parts of sodium hydroxide solution for ultrasonic dispersion to form suspension, the prepared suspension is introduced into an ozone reaction tower, ozone is introduced for treatment, the mass percentage concentration of the introduced ozone is 30mg/min, the flow rate is 3L/min, and the treatment time is 30 min; and pouring out the mixed solution after the treatment, filtering out particles, and drying in vacuum at the temperature of 50 ℃ for 36 hours to obtain the modified polylactic acid particle material.
Test data and analysis
1. The polylactic acid resins prepared in examples 1 to 5 and the products of comparative examples 1 to 2 were subjected to spinning on a melt blowing apparatus: firstly, determining the size of an eyelet of melt-blown equipment to be 0.30mm, checking a single-screw melt-blown machine, assembling a spinneret, switching on a power supply and preheating, adjusting the temperature of each section of the melt-blown equipment to the required set temperature, and keeping the temperature for 30 min; according to the mass ratio of 100: 1, respectively mixing the polylactic acid resin prepared in examples 1-5 and the product prepared in comparative examples 1-2 with a polylactic acid flow increasing agent, and uniformly mixing; opening a metering pump, starting a screw rod, adding the mixture into a screw extruder for melting treatment, feeding the melt into a rectangular spinneret plate through the screw rod and the metering pump, feeding the melt onto a receiving device through hot air with the pressure of 80kPa and the temperature of 280 ℃, cooling and solidifying to form a cloth cover, winding, and cutting into melt-blown non-woven fabrics; the melt blowing process is as shown in table 1.
Table 1 shows the melt-blown process of examples 1-5 and comparative examples 1-2
Zone 1 temperature Zone 2 temperature Zone 3 temperature Zone 4 temperature Die temperature Oven temperature
175℃ 200℃ 230℃ 230℃ 195℃ 231℃
Speed of main engine Current of the host Rotating speed of fan Current of fan Distance between mould nets Speed of mesh belt
168r/min 3.7A 828r/min 12.9A 25cm 150r/min
2. Fourier infrared spectrum detection is carried out on the polylactic acid (marked as a) subjected to ozone treatment in example 5 and the polylactic acid (marked as b) not subjected to ozone treatment, the detection results are shown in figure 2, and it can be seen that the infrared spectrum of the polylactic acid subjected to ozone treatment in example 5 of the invention is basically the same as that of the polylactic acid not subjected to ozone treatment in comparative example 1, but at 3217cm-1The absorption peak of poly-associated hydrogen bonds among the belonging molecules is obviously reduced, which shows that the hydrogen bonds among the molecules are reduced, so that more groups capable of forming the hydrogen bonds exist; and at 1759cm-1Where the stretching vibration is C ═ O, the absorption front narrows and becomes sharp, indicating that more carbonyl groups are exposed, which all contribute to the change in hydrophilicity.
3. Examples 1 to 5 and comparative examples 1 to 2 were subjected to water absorption test according to ASTM D6651-01, oil absorption test according to FZ/T01130-2016, biodegradability test according to GB/T-19277, and the results are shown in Table 2.
Table 2 shows the results of the measurement of the properties of the products of examples 1 to 5 and comparative examples 1 to 2
Figure BDA0002788663400000121
The results in table 2 show that the functional water and oil absorption functions of the product of the polylactic acid modified by ozone and the sodium polyacrylate through granulation and melt-blowing are obviously improved, the water absorption multiplying power distilled water index can reach more than 200g/g, and the biodegradability is kept better.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A preparation method of polylactic resin capable of adsorbing water and oil is characterized by comprising the following steps:
(1) adding polylactic acid into a sodium hydroxide solution according to the mass ratio of 1:1-1:3, and performing ultrasonic dispersion to form a suspension;
(2) introducing the suspension prepared in the step (1) into an ozone reaction tower, introducing ozone for treatment, wherein the mass percentage concentration of the introduced ozone is 10-20mg/min, the flow rate is 1-3L/min, and the treatment time is 10-20min to prepare a mixed solution;
(3) pouring out the mixed solution after the treatment, filtering out particles, and vacuum-drying the particles at 50-80 ℃ for 24-36h to obtain modified polylactic acid particles;
(4) adding sodium polyacrylate and an antioxidant into the modified polylactic acid granules prepared in the step (3) according to the mass ratio of 30:60:1:1-30:60:1:13, uniformly mixing, and then placing on a double-screw extruder for granulation to prepare the polylactic resin.
2. The method for preparing the polylactic acid resin capable of adsorbing the water and oil amphiphilicity according to claim 1, is characterized in that: the polylactic acid comprises one or more of dextro-polylactic acid, levorotatory polylactic acid, racemic polylactic acid and polylactic acid stereo complex.
3. The method for preparing the polylactic acid resin capable of adsorbing the water and oil amphiphilicity according to claim 1, is characterized in that: the particle size of the polylactic acid is 100-300 meshes.
4. The method for preparing the polylactic acid resin capable of adsorbing the water and oil amphiphilicity according to claim 1, is characterized in that: the antioxidant is a main antioxidant and an auxiliary antioxidant;
the main antioxidant is one or more of antioxidant 168 and antioxidant 1010;
the auxiliary antioxidant is one or more of antioxidant 1330 and antioxidant 1076.
5. The method for preparing the polylactic acid resin capable of adsorbing the water and oil amphiphilicity according to claim 1, is characterized in that: the acrylic acid monomer residual amount in the sodium polyacrylate was 200-300 ppm.
6. The method for preparing the polylactic acid resin capable of adsorbing the water and oil amphiphilicity according to claim 1, is characterized in that: the granulation process parameters of the double-screw extruder in the step (4) are set as follows:
Figure FDA0002788663390000021
7. the application of the polylactic resin prepared by the preparation method of the polylactic resin capable of adsorbing water and oil according to any one of claims 1 to 6, which is characterized by comprising the following steps:
(a) determining the size of the holes of the melt-blowing equipment, checking the single-screw melt-blowing machine, assembling a spinneret, switching on a power supply and preheating;
(b) adjusting the temperature of each section of the melt-blowing equipment to the required set temperature of 170-230 ℃, and keeping the temperature for 30 min;
(c) uniformly mixing the prepared polylactic resin and the polylactic acid flow increasing agent according to the mass ratio of 100:0.5-100: 3;
(d) and (3) opening a metering pump, starting a screw rod, adding the mixture obtained in the step (c) into a screw extruder for melting treatment, feeding the melt into a rectangular spinneret plate through the screw rod and the metering pump, feeding the melt onto a receiving device through high-pressure high-temperature hot air, cooling and solidifying to form a cloth cover, winding, and cutting into melt-blown non-woven fabrics.
8. The application of the polylactic resin prepared by the preparation method of the polylactic resin capable of adsorbing water and oil according to claim 7 is characterized in that: the size of the eyelet is 0.25-0.35 mm.
9. The application of the polylactic resin prepared by the preparation method of the polylactic resin capable of adsorbing water and oil according to claim 7 is characterized in that: the hot air pressure is 60-90kPa, and the temperature is 200-280 ℃.
10. The application of the polylactic resin prepared by the preparation method of the polylactic resin capable of adsorbing water and oil according to claim 7 is characterized in that: the polylactic resin is used in the melt-blown process, high-speed spinning and fine denier fiber of non-woven fabrics.
CN202011307304.4A 2020-11-19 2020-11-19 Preparation method and application of polylactic resin capable of adsorbing water and oil amphiprotic Withdrawn CN112552660A (en)

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