CN116065259A - Milk ES large biological fiber and preparation method thereof - Google Patents

Abstract

The invention discloses a milk ES large biological fiber and a preparation method thereof, wherein the raw materials of the fiber comprise milk PE master batch and PP master batch with the mass ratio of 6:4.5-5.5, the preparation method comprises the steps of preparing diatomite particles loaded with milk components, preparing the milk PE master batch and preparing the fiber, the fiber has good antibacterial performance, the inhibition rate of staphylococcus aureus is 99.6-99.7%, the inhibition rate of escherichia coli is 99.3-99.7%, and the inhibition rate of candida albicans is 91.2-91.4%.

Description

A kind of milk ES large biological fiber and preparation method thereof

Technical Field

The invention relates to milk ES large biological fiber and a preparation method thereof, belonging to the field of ES fibers.

Background Art

ES fiber, a striking polyolefin fiber developed by Chisso Corporation of Japan, is a new type of thermally bonded composite fiber, that is, a low-melting-point two-component composite fiber. It is a type of differentiated fiber. It is usually made by slicing two raw materials with different melting points (such as polypropylene PP/polyethylene PE), extruding them through a twin-screw extruder, and then using a composite spinning method. The cross-section of the fiber generally has two types: "skin-core type" and "parallel type". Due to the different melting points of the two components, the surface melts under certain heating conditions but the core layer does not melt, so that non-woven fabrics and other products can be produced without adhesives.

ES fiber is particularly suitable for the production of sanitary materials, thermal insulation filling materials, filter materials and other products. Due to the impact of the epidemic in recent years, the demand for sanitary products such as masks remains high, and the market demand for ES fiber non-woven fabrics is huge.

ES fiber has a certain heat resistance, and the product can be sterilized at a temperature above 100°C. However, after multiple high-temperature sterilizations, the physical properties of the fiber are still affected to a certain extent. If the fiber itself can obtain antibacterial properties, the change of physical properties can be avoided. Milk is rich in protein, mainly phosphorus-containing protein, albumin and globulin. These three proteins contain all essential amino acids, including lysine, tryptophan, methionine, leucine, isoleucine, phenylalanine, valine, etc. In addition, HMO is a component in milk and belongs to oligosaccharides. It has the functions of regulating immunity and regulating intestinal flora. It is generally used as an added ingredient in high-end milk powder. In in vitro experiments, HMO has an inhibitory effect on the adhesion of Escherichia coli, Salmonella and other bacteria. Through specific processes, milk protein and HMO can be added to ES fiber as antibacterial functional components to make ES fiber obtain lasting antibacterial properties.

When preparing ES fiber, it needs to be melt-extruded through a twin-screw extruder, and then a series of operations such as spinning are performed. This requires the protection of the antibacterial components of milk, otherwise they will denature and lose their antibacterial effect. Diatomaceous earth has good hygroscopic properties. Adding it to ES fiber can solve its large shrinkage rate. In addition, its porous structure can load antibacterial substances, so that ES fiber can obtain lasting antibacterial properties. At the same time, it can also avoid the destructive effect of antibacterial substances due to high-temperature melting during the granulation process. However, in order to ensure the antibacterial performance, if too much diatomaceous earth is added, the breaking strength of the ES fiber will decrease.

In summary, the ES fiber in the prior art can load and protect the antibacterial components of milk through diatomaceous earth, which can improve the antibacterial properties of the ES fiber, but will cause the breaking strength of the ES fiber to decrease.

Summary of the invention

The technical problem to be solved by the present invention is to overcome the defects of the prior art by preparing diatomaceous earth particles loaded with milk components, further preparing milk PE masterbatch, and finally preparing fibers, thereby improving the antibacterial properties of ES fibers and at the same time improving the breaking strength of ES fibers.

In order to solve the above technical problems, the present invention adopts the following technical solutions:

A milk ES large biological fiber, characterized in that the raw materials of the fiber include milk PE masterbatch and PP masterbatch, and the mass ratio is 6:4.5-5.5.

The following are further improvements to the above technical solution:

A method for preparing milk ES large biological fiber, the preparation method comprising preparing diatomaceous earth particles loaded with milk components, preparing milk PE masterbatch, and preparing fiber;

The steps of preparing diatomaceous earth particles loaded with milk components include betaine organic treatment and loading with milk components;

The betaine organic treatment method comprises the following steps: calcining diatomite at 440-460° C. for 170-180 min, naturally cooling, mixing with deionized water, and uniformly dispersing the diatomite, controlling the temperature to be 51-53° C., soaking the diatomite for 140-160 min, adding cocamidopropyl hydroxysulfobetaine after soaking, stirring the diatomite for 85-95 min, filtering, washing with water, and drying the diatomite organically treated with betaine.

The mass ratio of the diatomaceous earth, deionized water and cocamidopropyl hydroxysulfonyl betaine is 23-27:270-330:10-12.

The particle size of the diatomaceous earth is 180-250 nm.

The method for loading the milk component comprises the following steps: mixing the diatomaceous earth organically treated with betaine with deionized water, stirring to make it dispersed evenly, then adding HMO and concentrated milk, controlling the ultrasonic frequency to be 17-19 kHz, performing ultrasound for 20-30 minutes, stirring after ultrasound for 30-40 minutes, controlling the temperature to be 48-52° C., performing concentration and drying until the water content is 0%, and passing all the products through a 500-mesh sieve to obtain diatomaceous earth particles loaded with the milk component.

The mass ratio of the betaine organically treated diatomaceous earth, deionized water, HMO, and concentrated milk is 24-26:130-170:4.5-5.5:45-55;

The protein content of the concentrated milk is 5.0-5.3 g/100 mL.

The method for preparing milk PE masterbatch is as follows: heating the PE masterbatch until it is melted, then adding aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, and 3-aminopropyltrimethoxysilane, and mixing them for 30-40 minutes, then adding diatomaceous earth particles loaded with milk components, and continuing to mix them for 20-30 minutes. After mixing, the mixture is extruded and granulated to obtain the milk PE masterbatch.

The mass ratio of the PE masterbatch, aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, 3-aminopropyltrimethoxysilane, and diatomaceous earth particles loaded with milk components is 85-115:3.5-4.5:7-9:1.8-2.2:2.5-3.5:6-8.

The method for preparing the fiber comprises the following steps: respectively feeding milk PE masterbatch and PP masterbatch into a screw extruder to obtain an outer layer PE material melt and an inner layer PP material melt, feeding the outer layer PE material melt and the inner layer PP material melt into a composite spinning machine for spinning, spraying sheath-core type fibers through a spinneret, and then winding, stretching, cooling, oiling, and curling to obtain milk ES large biological fibers.

The linear density of the ES fiber is 1.62 dtex.

Compared with the prior art, the present invention achieves the following beneficial effects:

The ES fiber of the present invention has good antibacterial performance, with an inhibition rate of 99.6-99.7% for Staphylococcus aureus, 99.3-99.7% for Escherichia coli, and 91.2-91.4% for Candida albicans. After washing 50 times, the inhibition rate of Staphylococcus aureus is 94.7-95.2%, the inhibition rate of Escherichia coli is 94.0-94.5% after washing 50 times, and the inhibition rate of Candida albicans is 90.2-90.6% after washing 50 times.

The ES fiber of the present invention has good breaking performance, with a breaking strength of 8.29-8.37 cN/dtex and a breaking elongation of 181-183%;

The ES fiber of the present invention has good air permeability. The fiber of the present invention is used to prepare a non-woven fabric, and the air permeability of the non-woven fabric is tested according to the method of GB T 24218.15-2018. The air permeability is 1.20-1.25*10 ^-3 L/(cm ² ·s);

The ES fiber of the present invention has a high protein content, which is 1.52-1.56%.

DETAILED DESCRIPTION

Example 1

(1) Preparation of diatomaceous earth particles loaded with milk components

a. Betaine organic treatment

The diatomite was calcined at 440°C for 180 minutes, and after natural cooling, it was mixed with deionized water and evenly dispersed, and the temperature was controlled to be 51°C, and the soaking time was 160 minutes. After soaking, cocamidopropyl hydroxysulfonyl betaine was added, and the stirring time was 85 minutes. After stirring, it was filtered, washed with water, and dried to obtain betaine organically treated diatomite;

The mass ratio of the diatomaceous earth, deionized water and cocamidopropyl hydroxysulfobetaine is 23:270:10;

The particle size of the diatomaceous earth is 180 nm;

b. Loading milk components

The diatomaceous earth treated with betaine was mixed with deionized water, stirred to make it dispersed evenly, then HMO and concentrated milk were added, the ultrasonic frequency was controlled to be 17kHz, ultrasonication was performed, the ultrasonication time was 30min, stirring was performed after ultrasonication, the stirring time was 40min, after stirring, the temperature was controlled to be 48°C, concentrated and dried, dried to a water content of 0%, and all the products were sieved through a 500-mesh sieve to obtain diatomaceous earth particles loaded with milk components;

The mass ratio of the betaine organically treated diatomaceous earth, deionized water, HMO, and concentrated milk is 24:130:4.5:45;

The protein content of the concentrated milk is 5.0 g/100 mL.

(2) Preparation of milk PE masterbatch

The PE masterbatch is heated until it is melted, and then aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, and 3-aminopropyltrimethoxysilane are added and mixed for 30 minutes, and then diatomaceous earth particles loaded with milk components are added and mixed for 30 minutes. After mixing, the mixture is extruded and granulated to obtain the milk PE masterbatch;

The mass ratio of the PE masterbatch, aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, 3-aminopropyltrimethoxysilane, and diatomaceous earth particles loaded with milk components is 85:3.5:7:1.8:2.5:6;

(3) Preparation of fibers

The milk PE masterbatch and the PP masterbatch are respectively fed into a screw extruder to obtain an outer layer PE material melt and an inner layer PP material melt, and the outer layer PE material melt and the inner layer PP material melt are fed into a composite spinning machine for spinning, and a core-skin fiber is ejected through a spinneret, and then the milk ES large biofiber is obtained through winding, drawing, cooling, oiling and curling;

The mass ratio of the milk PE masterbatch to the PP masterbatch is 6:5.

The linear density of the ES fiber is 1.62 dtex.

Example 2

(1) Preparation of diatomaceous earth particles loaded with milk components

a. Betaine organic treatment

The diatomite was calcined at 460° C. for 170 min, cooled naturally, mixed with deionized water, and evenly dispersed, the temperature was controlled at 53° C., and the soaking time was 140 min. After soaking, cocamidopropyl hydroxysulfonyl betaine was added, and stirred for 95 min. After stirring, the mixture was filtered, washed with water, and dried to obtain betaine organically treated diatomite.

The mass ratio of the diatomaceous earth, deionized water and cocamidopropyl hydroxysulfobetaine is 27:330:12;

The particle size of the diatomaceous earth is 250nm;

b. Loading milk components

The diatomaceous earth treated with betaine was mixed with deionized water, stirred to make it dispersed evenly, then HMO and concentrated milk were added, the ultrasonic frequency was controlled to be 19kHz, ultrasonication was performed, the ultrasonication time was 20min, stirring was performed after ultrasonication, the stirring time was 30min, after stirring, the temperature was controlled to be 52°C, concentrated and dried, dried to a water content of 0%, and all the products were sieved through a 500-mesh sieve to obtain diatomaceous earth particles loaded with milk components;

The mass ratio of the betaine organically treated diatomaceous earth, deionized water, HMO, and concentrated milk is 26:170:5.5:55;

The protein content of the concentrated milk is 5.3 g/100 mL.

(2) Preparation of milk PE masterbatch

The PE masterbatch is heated until it is melted, and then aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, and 3-aminopropyltrimethoxysilane are added and mixed for 40 minutes, and then diatomaceous earth particles loaded with milk components are added and mixed for 20 minutes. After mixing, the mixture is extruded and granulated to obtain the milk PE masterbatch;

The mass ratio of the PE masterbatch, aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, 3-aminopropyltrimethoxysilane, and diatomaceous earth particles loaded with milk components is 115:4.5:9:2.2:3.5:8;

(3) Preparation of fibers

The milk PE masterbatch and the PP masterbatch are respectively fed into a screw extruder to obtain an outer layer PE material melt and an inner layer PP material melt, and the outer layer PE material melt and the inner layer PP material melt are fed into a composite spinning machine for spinning, and a core-skin fiber is ejected through a spinneret, and then the milk ES large biofiber is obtained through winding, drawing, cooling, oiling and curling;

The mass ratio of the milk PE masterbatch to the PP masterbatch is 6:4.5.

The linear density of the ES fiber is 1.60 dtex.

Example 3

(1) Preparation of diatomaceous earth particles loaded with milk components

a. Betaine organic treatment

The diatomite was calcined at 450°C for 175 minutes, and after natural cooling, it was mixed with deionized water and evenly dispersed, and the temperature was controlled to be 52°C, and the soaking time was 150 minutes. After soaking, cocamidopropyl hydroxysulfonyl betaine was added, and the stirring time was 90 minutes. After stirring, it was filtered, washed with water, and dried to obtain betaine organically treated diatomite;

The mass ratio of the diatomaceous earth, deionized water and cocamidopropyl hydroxysulfobetaine is 25:300:11;

The particle size of the diatomaceous earth is 200 nm;

b. Loading milk components

The diatomaceous earth treated with betaine was mixed with deionized water, stirred to make it dispersed evenly, then HMO and concentrated milk were added, the ultrasonic frequency was controlled to be 18kHz, ultrasonication was performed, the ultrasonication time was 25min, stirring was performed after ultrasonication, the stirring time was 35min, after stirring, the temperature was controlled to be 50°C, concentrated and dried, dried to a water content of 0%, and all the products were sieved through a 500-mesh sieve to obtain diatomaceous earth particles loaded with milk components;

The mass ratio of the betaine organically treated diatomaceous earth, deionized water, HMO, and concentrated milk is 25:150:5:50;

The protein content of the concentrated milk is 5.2 g/100 mL.

(2) Preparation of milk PE masterbatch

The PE masterbatch was heated until it was melted, and then aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, and 3-aminopropyltrimethoxysilane were added and mixed for 35 minutes, and then diatomaceous earth particles loaded with milk components were added and mixed for 25 minutes. After mixing, the mixture was extruded and granulated to obtain the milk PE masterbatch;

The mass ratio of the PE masterbatch, aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, 3-aminopropyltrimethoxysilane, and diatomaceous earth particles loaded with milk components is 100:4:8:2:3:7;

(3) Preparation of fibers

The milk PE masterbatch and the PP masterbatch are respectively fed into a screw extruder to obtain an outer layer PE material melt and an inner layer PP material melt, and the outer layer PE material melt and the inner layer PP material melt are fed into a composite spinning machine for spinning, and a core-skin fiber is ejected through a spinneret, and then the milk ES large biofiber is obtained through winding, drawing, cooling, oiling and curling;

The mass ratio of the milk PE masterbatch to the PP masterbatch is 6:5.5.

The linear density of the ES fiber is 1.64 dtex.

Comparative Example 1

Based on the embodiment, in the step of preparing diatomaceous earth particles loaded with milk components, the betaine organic treatment step is omitted, and the untreated diatomaceous earth is directly loaded with milk components. The remaining steps are the same to prepare fibers.

Comparative Example 2

On the basis of Example 1, the preparation of milk PE masterbatch was changed to the following operation:

The PE masterbatch is heated until it is melted, and then the diatomaceous earth particles loaded with milk components are added and kneaded for 25 minutes. After kneading, the milk PE masterbatch is obtained by extrusion granulation;

The mass ratio of the PE masterbatch to the diatomaceous earth particles loaded with milk components is 100:7;

The remaining steps are the same to prepare the fibers.

Example 4 Antibacterial Performance Test

The ES fibers of Examples 1-3 and Comparative Examples 1-2 were tested for their inhibition rates against Staphylococcus aureus, Escherichia coli, and Candida albicans according to the method in GB/T20944.3-2008, and the inhibition rates against Staphylococcus aureus, Escherichia coli, and Candida albicans were tested after washing 50 times. The results are shown in Table 1.

Example 5 Fracture performance test

The ES fibers of Examples 1-3 and Comparative Examples 1-2 were tested for breaking strength and breaking elongation according to the method of FZ/T 52024-2012. The results are shown in Table 2.

Example 6 Air Permeability Test

Non-woven fabrics were prepared using the ES fibers of Examples 1-3 and Comparative Examples 1-2, and the air permeability of the non-woven fabrics was tested according to the method of GB T 24218.15-2018. The results are shown in Table 3.

Example 7 Protein Quality Detection

The protein content of the ES fibers prepared in Examples 1-3 and Comparative Examples 1-2 was tested according to the method of FZ/T 50018-2013. The results are shown in Table 4.

Claims (10)

1. A milk ES large biological fiber, characterized in that the raw materials of the fiber include milk PE masterbatch and PE masterbatch, with a mass ratio of 6:4.5-5.5. 2. A method for preparing milk ES large biological fiber, characterized in that the preparation method comprises preparing diatomaceous earth particles loaded with milk components, preparing milk PE masterbatch, and preparing fiber; The steps of preparing diatomaceous earth particles loaded with milk components include betaine organic treatment and loading with milk components; The betaine organic treatment method comprises the following steps: calcining diatomite at 440-460° C. for 170-180 min, naturally cooling, mixing with deionized water, and uniformly dispersing the diatomite, controlling the temperature to be 51-53° C., soaking the diatomite for 140-160 min, adding cocamidopropyl hydroxysulfobetaine after soaking, stirring the diatomite for 85-95 min, filtering, washing with water, and drying the diatomite organically treated with betaine. 3. The method for preparing the milk ES large biological fiber according to claim 2, characterized in that: The mass ratio of the diatomaceous earth, deionized water and cocamidopropyl hydroxysulfonyl betaine is 23-27:270-330:10-12. 4. The method for preparing the milk ES large biological fiber according to claim 3, characterized in that: The particle size of the diatomaceous earth is 180-250 nm. 5. The method for preparing the milk ES large biological fiber according to claim 2, characterized in that: The method for loading the milk component comprises the following steps: mixing the diatomaceous earth organically treated with betaine with deionized water, stirring to make it dispersed evenly, then adding HMO and concentrated milk, controlling the ultrasonic frequency to be 17-19 kHz, performing ultrasound for 20-30 minutes, stirring after ultrasound for 30-40 minutes, controlling the temperature to be 48-52° C., performing concentration and drying until the water content is 0%, and passing all the products through a 500-mesh sieve to obtain diatomaceous earth particles loaded with the milk component. 6. The method for preparing the milk ES large biological fiber according to claim 5, characterized in that: The mass ratio of the betaine organically treated diatomaceous earth, deionized water, HMO, and concentrated milk is 24-26:130-170:4.5-5.5:45-55; The protein content of the concentrated milk is 5.0-5.3 g/100 mL. 7. The method for preparing the milk ES large biological fiber according to claim 2, characterized in that: The method for preparing milk PE masterbatch is as follows: heating the PE masterbatch until it is melted, then adding aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, and 3-aminopropyltrimethoxysilane, and mixing them for 30-40 minutes, then adding diatomaceous earth particles loaded with milk components, and continuing to mix them for 20-30 minutes. After mixing, the mixture is extruded and granulated to obtain the milk PE masterbatch. 8. The method for preparing the milk ES large biological fiber according to claim 7, characterized in that: The mass ratio of the PE masterbatch, aluminum sulfate, polyoxymethylene, isodecyl diphenyl phosphate, 3-aminopropyltrimethoxysilane, and diatomaceous earth particles loaded with milk components is 85-115:3.5-4.5:7-9:1.8-2.2:2.5-3.5:6-8. 9. The method for preparing the milk ES large biological fiber according to claim 2, characterized in that: The method for preparing the fiber comprises the following steps: respectively feeding milk PE masterbatch and PP masterbatch into a screw extruder to obtain an outer layer PE material melt and an inner layer PP material melt, feeding the outer layer PE material melt and the inner layer PP material melt into a composite spinning machine for spinning, spraying sheath-core type fibers through a spinneret, and then winding, stretching, cooling, oiling, and curling to obtain milk ES large biological fibers. 10. The method for preparing the milk ES large biological fiber according to claim 8, characterized in that: The linear density of the ES fiber is 1.62 dtex.