阅读说明：本技术 一种纳米碳酸钙复合再生pet色母粒制备工艺 (Preparation process of nano calcium carbonate composite regenerated PET color master batch ) 是由 杜兆芳 闫文静 顾殿宽 胡超凡 李继丰 方婷 于 2021-09-22 设计创作，主要内容包括：本发明公开了一种纳米碳酸钙复合再生PET色母粒制备工艺,包括以下步骤：(1)将再生PET母粒、纳米碳酸钙、颜料分别放入真空转鼓烘箱中干燥预处理；(2)将干燥后的再生PET母粒、纳米碳酸钙、颜料、PET扩链剂、分散剂混合均匀得到共混物；(3)将步骤(2)中的共混物通过双螺杆挤出机中熔融挤出,切粒,得到纳米碳酸钙复合再生PET色母粒。本发明的有益效果为：由本发明的方法所获得的纳米碳酸钙复合再生PET色母粒,低污染、高色牢度、功能性持久,可用于熔融纺丝制备高热稳定性、高韧性、原液着色亲水PET功能,分散剂的添加解决了颜料团聚的问题,增强了再生聚酯母粒的可纺性能,可以规模化生产、大面积应用于多功能PET的制备。(The invention discloses a preparation process of a nano calcium carbonate composite regenerated PET color master batch, which comprises the following steps: (1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the pigment into a vacuum drum oven for drying pretreatment; (2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, pigment, PET chain extender and dispersing agent to obtain a blend; (3) and (3) melting and extruding the blend obtained in the step (2) through a double-screw extruder, and pelletizing to obtain the nano calcium carbonate composite regenerated PET color master batch. The invention has the beneficial effects that: the nano calcium carbonate composite regenerated PET color master batch obtained by the method has low pollution, high color fastness and lasting functionality, can be used for preparing high-heat stability, high toughness and stock solution coloring hydrophilic PET function by melt spinning, solves the problem of pigment agglomeration by adding the dispersing agent, enhances the spinnability of the regenerated polyester master batch, and can be produced in large scale and applied to the preparation of multifunctional PET in large area.)

1. A preparation process of nano calcium carbonate composite regenerated PET color master batch is characterized by comprising the following steps: the method comprises the following steps:

(1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the pigment into a vacuum drum oven for drying pretreatment;

(2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, pigment, PET chain extender and dispersing agent to obtain a blend;

(3) and (3) melting and extruding the blend obtained in the step (2) through a double-screw extruder, and pelletizing to obtain the nano calcium carbonate composite regenerated PET color master batch.

2. The preparation process of the nano calcium carbonate composite recycled PET color master batch according to claim 1, which is characterized in that: the drying pretreatment process in the step (1) is vacuum drying at 60-80 ℃ for 4-6h, then heating to 120 ℃ and 130 ℃, and drying for 6-8 h.

3. The preparation process of the nano calcium carbonate composite recycled PET color master batch according to claim 1, which is characterized in that: the pigment in the step (1) is one or more of phthalocyanine blue, phthalocyanine green, pigment red 254 and pigment violet 29.

4. The preparation process of the nano calcium carbonate composite recycled PET color master batch according to claim 1, which is characterized in that: in the step (2), the mass ratios of the regenerated PET master batch, the nano calcium carbonate, the pigment, the PET chain extender and the dispersing agent are 77.7:2:23:0.3:2, 77.7:3:22:0.3:2, 77.7:4:21:0.3:2 and 77.7:5:20:0.3:2 respectively.

5. The preparation process of the nano calcium carbonate composite recycled PET color master batch according to claim 1, which is characterized in that: in the step (2), the dispersing agent is one or more of ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer and ethylene-butyl acrylate copolymer.

6. The preparation process of the nano calcium carbonate composite recycled PET color master batch according to claim 1, which is characterized in that: the screw rotating speed of the double-screw extruder in the step (3) is 150-.

7. The preparation process of the nano calcium carbonate composite recycled PET color master batch according to claim 1, which is characterized in that: the melting temperature in the step (3) is 240-260 ℃.

Technical Field

The invention relates to a process method of industrialized regenerated PET master batch, in particular to a preparation process of nano calcium carbonate composite regenerated PET master batch.

Background

At present, the living standard of people is continuously improved, the scientific technology is rapidly developed, and PET brings great convenience to the production and the life of people. PET has good thermal property and mechanical property, and is widely applied to the fields of chemical fibers, packaging materials, electronic equipment, manufacturing industry and the like. In recent years, PET is the only leader in the chemical fiber market, and the market occupation ratio of PET fibers in chemical fibers reaches about 80%. The polyester product brings convenience to life and production for people, but serious environmental hazards are caused due to difficult degradation, so that the treatment of the waste polyester becomes an important problem. The treatment and reutilization of the waste plastics comprise a physical method and a chemical method, and further can be divided into four methods: primary recovery, mechanical recovery (secondary recovery), chemical recovery (tertiary recovery) and energy recovery (quaternary recovery). The mechanical recovery is the only technology for recovering waste plastics on a large scale at present, and the main steps of the mechanical recovery are that the waste plastics are cleaned, crushed, melted and granulated and then are usually mixed with the same kind of original plastics to manufacture products with certain performance. However, it is difficult for such products to meet the requirements of aesthetic, functional, safety, etc. Meanwhile, the PET fiber has some problems, such as poor hygroscopicity and water absorption, low moisture regain, stuffy feeling when the polyester fabric is worn, and no sweat absorption of the polyester fabric, so that the comfort of wearing the polyester fabric is poor compared with that of the natural fabric. The waste plastic is recycled and the functional modification is carried out on the waste plastic, so that a high-performance recycled product is efficiently obtained, and the method has a great application prospect.

The nano calcium carbonate has small surface energy, large lipophilicity and high dispersibility and dispersion stability in a matrix, so that the nano calcium carbonate has higher compatibility with high polymers and is generally used as a performance reinforcing agent and a functional filler. The nano calcium carbonate has good affinity with resin when being used in plastic, can effectively increase or adjust the rigidity, toughness, bending strength and the like of materials, can improve the rheological property of a plastic processing system, reduce the plasticizing temperature, and improve the dimensional stability, heat resistance and surface smoothness of products; in rubber systems such as natural rubber, butadiene rubber, styrene butadiene rubber and the like, the rubber is easy to knead and uniformly dispersed, the colloid is soft, and the extrusion processability and the model fluidity can be improved. The nano calcium carbonate has a plurality of excellent properties, so that the nano calcium carbonate is widely applied to preparation of various novel composite materials, but most of the nano calcium carbonate utilizes the toughening and reinforcing characteristics of the nano calcium carbonate, and the nano calcium carbonate serving as a pore forming agent can provide a new idea for hydrophilic finishing of subsequent spinning.

Compared with the traditional PET fiber post-dyeing and finishing method, the method for preparing the dope-dyed hydrophilic PET functional fiber by adding the nano calcium carbonate composite regenerated PET color master batch and melt spinning has the advantages of low pollution, high color fastness, lasting functionality and the like. In order to obtain high-quality stock solution coloring hydrophilic fiber, the research on the preparation of the nano calcium carbonate composite regenerated PET color master batch is of great significance.

Disclosure of Invention

The invention aims to provide a preparation process of a nano calcium carbonate composite regenerated PET color master batch, which aims to solve the technical problems in the prior art, and can ensure good dispersibility of high-concentration pigment and nano calcium carbonate in the master batch, and processability, spinnability and fiber mechanical property of the master batch while giving consideration to good colorability and hydrophilic property.

The invention provides a preparation process of a nano calcium carbonate composite regenerated PET color master batch, which comprises the following steps:

(1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the pigment into a vacuum drum oven for drying pretreatment;

(2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, pigment, PET chain extender and dispersing agent to obtain a blend;

(3) and (3) melting and extruding the blend obtained in the step (2) through a double-screw extruder, and pelletizing to obtain the nano calcium carbonate composite regenerated PET color master batch.

The preparation process of the nano calcium carbonate composite recycled PET color master batch comprises the following steps of (1) drying at 60-80 ℃ for 4-6h in vacuum, heating to 120-130 ℃ and drying for 6-8 h.

The preparation process of the nano calcium carbonate composite recycled PET color master batch is preferably characterized in that the pigment in the step (1) is one or more of phthalocyanine blue, phthalocyanine green, pigment red 254 and pigment violet 29.

The preparation process of the nano calcium carbonate composite regenerated PET color master batch comprises the following steps of (2) preferably, the mass ratio of the regenerated PET color master batch to the nano calcium carbonate to the pigment to the PET chain extender to the dispersant is 77.7:2:23:0.3:2, 77.7:3:22:0.3:2, 77.7:4:21:0.3:2, and 77.7:5:20:0.3: 2.

In the preparation process of the nano calcium carbonate composite recycled PET color master batch, preferably, the dispersant in the step (2) is one or more of ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer and ethylene-butyl acrylate copolymer.

The preparation process of the nano calcium carbonate composite recycled PET color master batch comprises the following steps, wherein in the step (3), the screw rotating speed of the double-screw extruder is preferably 150-.

The preparation process of the nano calcium carbonate composite recycled PET color master batch is described above, wherein, the melting temperature in the step (3) is preferably 240-260 ℃.

Compared with the prior art, the invention has the beneficial effects that: the nano calcium carbonate composite regenerated PET color master batch obtained by the method has low pollution, high color fastness and lasting functionality, can be used for preparing high-heat stability, high toughness and stock solution coloring hydrophilic PET function by melt spinning, solves the problem of pigment agglomeration by adding the dispersing agent, enhances the spinnability of the regenerated polyester master batch, and can be produced in large scale and applied to the preparation of multifunctional PET in large area.

Drawings

FIG. 1 is a preparation process of the nano calcium carbonate composite regenerated PET color master batch of the invention.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.

A preparation process of a nano calcium carbonate composite regenerated PET color master batch comprises the following steps:

(1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the pigment into a vacuum drum oven for drying pretreatment;

(2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, pigment, PET chain extender and dispersing agent to obtain a blend;

(3) and (3) melting and extruding the blend obtained in the step (2) through a double-screw extruder, and pelletizing to obtain the nano calcium carbonate composite regenerated PET color master batch.

The drying pretreatment process in the step (1) is vacuum drying at 60-80 ℃ for 4-6h, then heating to 120 ℃ and 130 ℃, and drying for 6-8 h.

The pigment in the step (1) is one or more of phthalocyanine blue, phthalocyanine green, pigment red 254 and pigment violet 29.

In the step (2), the mass ratios of the regenerated PET master batch, the nano calcium carbonate, the pigment, the PET chain extender and the dispersing agent are 77.7:2:23:0.3:2, 77.7:3:22:0.3:2, 77.7:4:21:0.3:2 and 77.7:5:20:0.3:2 respectively.

In the step (2), the dispersing agent is one or more of ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer and ethylene-butyl acrylate copolymer.

The screw rotating speed of the double-screw extruder in the step (3) is 150-.

The melting temperature in the step (3) is 240-260 ℃.

Example 1 of the invention:

a preparation process of a nano calcium carbonate composite regenerated PET color master batch comprises the following steps:

(1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the pigment red 254 into a vacuum drum oven, heating the vacuum drum oven to 60 ℃ firstly, drying the vacuum drum oven for 4 hours, then heating the vacuum drum oven to 120 ℃, and drying the vacuum drum oven for 4 hours to obtain dried regenerated PET master batch, nano calcium carbonate and pigment red 254;

(2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, pigment, PET chain extender and ethylene-vinyl acetate copolymer according to a certain mass ratio of 77.7:2:23:0.3: 2;

(3) and (3) performing melt extrusion in a double-screw extruder, wherein the rotating speed of a screw of the double-screw extruder is 150r/min, the melting temperature is 240 ℃, and performing granulation to obtain the nano calcium carbonate composite regenerated PET color master batch.

Example 2 of the invention:

a preparation process of a nano calcium carbonate composite regenerated PET color master batch comprises the following steps:

(1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the pigment violet 29 into a vacuum drum oven, heating the regenerated PET master batch, the nano calcium carbonate and the pigment violet 29 to 70 ℃ in a vacuum dryer, drying for 5 hours, heating the regenerated PET master batch to 130 ℃ again, and drying for 5 hours to obtain dried regenerated PET master batch, nano calcium carbonate and pigment violet 29;

(2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, pigment violet 29, a PET chain extender and an ethylene acrylic acid copolymer according to a certain mass ratio of 77.7:3:22:0.3: 2;

(3) and (3) performing melt extrusion in a double-screw extruder, wherein the rotating speed of a screw of the double-screw extruder is 160r/min, the melting temperature is 250 ℃, and performing granulation to obtain the nano calcium carbonate composite regenerated PET color master batch.

Example 3 of the invention:

a preparation process of a nano calcium carbonate composite regenerated PET color master batch comprises the following steps:

(1) respectively putting the regenerated PET master batch, the nano calcium carbonate and the phthalocyanine blue into a vacuum drum oven, heating the vacuum drum oven to 80 ℃ firstly, drying the PET master batch for 6 hours, heating the PET master batch to 130 ℃ again, and drying the PET master batch for 6 hours to obtain dried regenerated PET master batch, nano calcium carbonate and phthalocyanine blue;

(2) uniformly mixing the dried regenerated PET master batch, nano calcium carbonate, phthalocyanine blue, a PET chain extender and a dispersing agent according to a certain mass ratio to obtain a polyester chain type hyperdispersant;

(3) and (3) performing melt extrusion in a double-screw extruder, wherein the rotating speed of a screw of the double-screw extruder is 170r/min, the melting temperature is 260 ℃, and performing granulation to obtain the nano calcium carbonate composite regenerated PET color master batch.

The construction, features and functions of the present invention are described in detail in the embodiments illustrated in the drawings, which are only preferred embodiments of the present invention, but the present invention is not limited by the drawings, and all equivalent embodiments modified or changed according to the idea of the present invention should fall within the protection scope of the present invention without departing from the spirit of the present invention covered by the description and the drawings.