CN114085494A - Low-noise high-elasticity 3D air fiber material and preparation method thereof - Google Patents

Abstract

The invention discloses a low-noise high-elasticity 3D air fiber material and a preparation method thereof, wherein the low-noise high-elasticity 3D air fiber material is prepared from the following components in parts by mass: 58.2-78.2 parts of thermoplastic polyester elastomer, 20-50 parts of ethylene copolymer, 1 part of chain extender, 0.2 part of catalyst, 0.5 part of antioxidant and 0.3 part of lubricant. The thermoplastic 3D air fiber material with rubber feeling and high elasticity can be obtained by adding the ethylene copolymer, and the advantage of plastic extrusion processing is not changed; the material is composed of open, semi-open and closed pore structures, and after the ethylene copolymer is added, the surface of the 3D air fiber material is rougher and has a rubber feeling, and the noise is reduced by the flow resistance and the tortuous sound wave path when the material is extruded; for the low-frequency noise generated by compression due to extrusion, the better sound absorption effect is achieved by damping the vibration and hardly generating resonance with a noise source.

Description

Low-noise high-elasticity 3D air fiber material and preparation method thereof

Technical Field

The invention relates to the technical field of high polymer materials, in particular to a low-noise high-elasticity 3D air fiber material and a preparation method thereof.

Background

The thermoplastic polyester elastomer is a block copolymer containing polyester hard segments and polyether soft segments, and is called TPEE for short. The crystalline polyester forms an amorphous phase and the hard segments of the polyester partially crystallize to form crystalline domains that act as physical crosslinks. TPEE has the elasticity of rubber and the strength of engineering plastics, and the soft segment gives it elasticity, making it like rubber; the hard segment imparts processability to it, making it plastic-like. Compared with rubber, the rubber has better processing performance and longer service life; compared with engineering plastics, it features high strength, high flexibility and dynamic mechanical performance. TPEE has the characteristics of high strength, high elasticity, oil resistance, acid and alkali resistance, high temperature resistance, radiation resistance, excellent dynamic mechanical property and the like, the use temperature range is very wide and is-50-180 ℃, and the hardness range is 25D-80D.

TPEE in a molten state is made into a layered elastomer by a spinning mode, a spinneret plate is used for extruding at a certain speed and temperature, the extruded layered elastomer falls into water for cooling, a continuous filament body is bent into a ring, contact parts are mutually welded, two sides are flattened and finally the layered elastomer is cut into a three-dimensional reticular structure with required size. The existing layered elastic body can be used for mattresses, sofa seats, high-speed rail cushions and back pillows; novel car seat, back etc. except need considering its travelling comfort, compress durability repeatedly, still need more consider people and move about on it, stand up, have the no abnormal sound when shifting position, provide a more comfortable, more humanized, more quiet use experience for people.

Disclosure of Invention

In view of the above, the invention provides a low-noise high-elasticity 3D air fiber material and a preparation method thereof, so as to solve the problems in the background art, not only ensure the high-elasticity characteristic of the material, but also reduce the noise generated when the material is extruded, and enable the mechanical properties of the material not to be affected.

In order to achieve the purpose, the invention provides the following technical scheme:

the invention discloses a low-noise high-elasticity 3D air fiber material which is prepared from the following components in parts by mass:

as a further scheme of the invention: the hardness of the thermoplastic polyester elastomer is 40-63D.

As a further scheme of the invention: the ethylene copolymer is at least one of ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate, ethylene-acrylic ester, ethylene-methyl acrylate, ethylene-styrene, ethylene-maleic anhydride, ethylene-vinyl alcohol, ethylene-propylene, ethylene-methyl methacrylate, ethylene-butyl acrylate, ethylene-methyl acrylate-glycidyl methacrylate, ethylene-methyl methacrylate-glycidyl methacrylate and ethylene-n-butyl acrylate-glycidyl methacrylate.

As a further scheme of the invention: the chain extender is at least one of epoxy chain extender, polyhydroxy compound and diisocyanate.

As a further scheme of the invention: the catalyst is a cationic metal salt or a metal oxide.

As a further scheme of the invention: the antioxidant is pentaerythritol dodecyl sulfate, 4-bis (alpha, alpha-dimethylbenzyl) diphenylamine, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, tetrakis (BETA- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid) pentaerythritol ester, tris [2, 4-di-tert-butylphenyl ] phosphite, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, pentaerythritol distearate, N-octadecyl (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, tetramethylene (3, 5-di-tert-butyl-4-hydroxyphenyl) methyl ester, bis [ ethyl-3- (3), 5-di-tert-butyl-4-hydroxyphenyl)) 2,2 oxamide, dioctadecyl tetraol diphosphite.

As a further scheme of the invention: the lubricant is at least one of ethyl dioleamide, primary unsaturated amide derivative compounds, fatty acid esters, a mixture of various amide compounds and soap salt, glycerol, ethylene stearamide, polyethylene wax, talcum powder, white carbon black, polytetrafluoroethylene and erucamide.

The invention also discloses a preparation method of the low-noise high-elasticity 3D air fiber material, which comprises the following steps:

s1: weighing the thermoplastic polyester elastomer, the ethylene copolymer, the chain extender, the antioxidant and the lubricant according to the parts by weight, adding the mixture into a high-speed mixer at the temperature of 120-130 ℃, and mixing for 50-60 minutes to obtain a mixture;

s2: putting the mixture in the S1 into a double-screw extruder for extrusion and granulation to obtain granules;

s3: and (4) putting the granules in the S2 into a solid phase polycondensation kettle for solid phase polycondensation to obtain the 3D fiber material.

As a further scheme of the invention: in the step S2, the temperature of each material cylinder of the double-screw extruder is 180-.

As a further scheme of the invention: the solid phase polycondensation comprises a first reaction stage and a second reaction stage, wherein:

the reaction temperature of the first reaction stage is 80-120 ℃, the vacuum degree is not more than 1000Pa, and the reaction time is not more than 1 hour;

the reaction temperature of the second reaction stage is 160-200 ℃, the vacuum degree is less than 100Pa, and the reaction time is 12-24 hours.

Compared with the prior art, the invention has the beneficial effects that:

the thermoplastic 3D air fiber material with rubber feeling and high elasticity can be obtained by adding the ethylene copolymer, and the advantage of plastic extrusion processing is not changed; the TPEE and ethylene copolymer can be organically linked together by adding chain extender and catalyst to form a uniform whole. The 3D air fiber material is used for preparing the layered elastomer, and is further processed into products such as mattresses, cushions, headrests and the like, because the material consists of open, semi-open and closed hole structures, after the ethylene copolymer is added, the surface of the 3D air fiber material is rougher and has rubber feeling, and the noise is reduced by flow resistance and tortuous sound wave paths when the material is extruded; for the low-frequency noise generated by compression due to extrusion, the better sound absorption effect is achieved by damping the vibration and hardly generating resonance with a noise source.

According to the invention, the reaction activity among the TPEE, the chain extender and the ethylene copolymer is further promoted through solid-phase polycondensation to form a truly uniform elastic material, the continuous stability of the high-elasticity 3D air fiber in the processing process is ensured, and the crystalline phase and the viscosity are adjusted through solid-phase reaction to obtain the thermoplastic polyester elastomer with more rubber feeling. The production formula is adjusted through resultant force, and a proper solid phase polycondensation treatment process is matched, so that the support factor of the material (namely the product comfort) is not lost under the condition of ensuring the performance of low noise, and the material has excellent processing performance, thereby having important significance.

Detailed Description

In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

The following examples and comparative examples employ the following raw material specific information:

and (2) component A: the self-made TPEE can be used,

a1 Shore hardness 40D;

a2 Shore hardness 55D;

a2 Shore hardness 63D;

the preparation method of the self-made TPEE comprises the following steps:

a1 was prepared according to the following method:

20 parts of dimethyl terephthalate, 18 parts of 1, 4-butanediol, 30 parts of polyether ester polyol, 0.1 part of 4, 4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine antioxidant, 0.25 part of tetrabutyl titanate catalyst, 0.2 part of trimethylolpropane cross-linking agent and 0.3 part of triphenyl phosphite anti-yellowing agent are added into a polymerization reaction kettle, polycondensation reaction is carried out at 250 ℃, and a polyester elastomer substrate with required intrinsic viscosity is prepared according to the change of stirring current of the reaction kettle.

A2 was prepared according to the following method:

adding 18 parts of 1, 4-butanediol of 20 parts of dimethyl terephthalate, 20 parts of polyether ester polyol, 0.1 part of 4, 4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine antioxidant, 0.25 part of tetrabutyl titanate catalyst, 0.2 part of trimethylolpropane cross-linking agent and 0.3 part of triphenyl phosphite anti-yellowing agent into a polymerization reaction kettle, carrying out polycondensation reaction at 250 ℃, and preparing the polyester elastomer substrate with the required intrinsic viscosity according to the change of stirring current of the reaction kettle.

A3 was prepared according to the following method:

20 parts of dimethyl terephthalate, 18 parts of 1, 4-butanediol, 10 parts of polyether ester polyol, 0.1 part of 4, 4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine antioxidant, 0.25 part of tetrabutyl titanate catalyst, 0.2 part of trimethylolpropane cross-linking agent and 0.3 part of triphenyl phosphite anti-yellowing agent are added into a polymerization reaction kettle, polycondensation reaction is carried out at 250 ℃, and a polyester elastomer substrate with required intrinsic viscosity is prepared according to the change of stirring current of the reaction kettle.

And (B) component: an ethylene copolymer, which is a copolymer of ethylene,

b1: is ethylene-methyl acrylate-glycidyl methacrylate with the trade name of

From dupont, usa;

b2: ethylene-methyl methacrylate-glycidyl methacrylate: from easy polymer (shanghai) ltd;

b3: ethylene-n-butyl acrylate-glycidyl methacrylate: available from the easy polymer (shanghai) ltd.

And (C) component: the chain extender is cyclohexane-1, 2-dicarboxylic acid diglycidyl ester, and the trademark TTA184 is purchased from Jiangsu Tai Er New Material science and technology Co.

And (B) component D: the catalyst was zinc stearate, available from Shandong Kogyou and Tankite Co., Ltd.

And (3) component E: an antioxidant, a surfactant,

e1: antioxidant 4, 4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine, available under the trade designation Naugard N445, available from kepi ltd;

e2: pentaerythritol distearate phosphite (619), available from Keppi, Inc.

And (F): the lubricant is polyethylene wax, and is purchased from Oimengteng New Material science and technology Co.

All materials are conventional and common products sold in the market.

It is understood that the above raw material reagents are only examples of some specific embodiments of the present invention, so as to make the technical scheme of the present invention more clear, and do not represent that the present invention can only adopt the above reagents, particularly, the scope of the claims is subject to. In addition, "parts" described in examples and comparative examples mean parts by weight unless otherwise specified.

Any range recited herein is intended to include the endpoints and any number between the endpoints and any subrange subsumed therein or defined therein.

The addition parts of the components in examples 1 to 6 and comparative examples 1 to 12 are shown in Table 1, and the preparation method is as follows:

s1: weighing the thermoplastic polyester elastomer, the polyethylene copolymer, the chain extender, the antioxidant and the lubricant according to the weight parts, adding the mixture into a high-speed mixer at the temperature of 120-130 ℃ for mixing for 50-60 minutes to obtain a mixed material;

s2: putting the mixture in the S1 into a double-screw extruder for extrusion and granulation;

s3: and (3) putting the material in the S2 into a solid phase polycondensation kettle for solid phase polycondensation:

vacuumizing at 100 ℃ for removing water for 1 hour, wherein the vacuum degree is less than or equal to 1000 Pa; and then continuously heating to 190 ℃ and keeping the vacuum degree less than 100Pa for solid-phase polycondensation, wherein the polycondensation time is 12 hours, and discharging and cooling to obtain the low-noise high-elasticity 3D air fiber material meeting the requirements.

TABLE 1 amounts of components added in examples 1-6 and comparative examples 1-9

Composition of	A1	A2	A3	B1	B2	B3	C	D	E1	E2	F
												Example 1	78.2			20			1	0.2	0.3	0.2	0.3
Example 2	68.2				30		1	0.2	0.3	0.2	0.3
												Example 3		78.2		30			1	0.2	0.3	0.2	0.3
Example 4		68.2			40		1	0.2	0.3	0.2	0.3
												Example 5			68.2			40	1	0.2	0.3	0.2	0.3
Example 6			58.2			50	1	0.2	0.3	0.2	0.3
												Comparative example 1	98.2						1	0.2	0.3	0.2	0.3
Comparative example 2	88.2			10			1	0.2	0.3	0.2	0.3
												Comparative example 3		98.2					1	0.2	0.3	0.2	0.3
Comparative example 4		88.2			10		1	0.2	0.3	0.2	0.3
												Comparative example 5		38.2				60	1	0.2	0.3	0.2	0.3
Comparative example 6			98.2				1	0.2	0.3	0.2	0.3
												Comparative example 7			88.2	10			1	0.2	0.3	0.2	0.3
Comparative example 8			38.2	60			1	0.2	0.3	0.2	0.3
												Comparative example 9			39.2	60				0.2	0.3	0.2	0.3

The low-noise high-elasticity 3D air fiber materials prepared in the comparative examples and the examples are spun by a spinneret plate, cooled and shaped to prepare air fiber blocks with the length of 100mm, the width of 100mm and the height of 100mm, and mechanical property, support factor and noise performance tests are carried out; the test criteria, conditions and results are shown in table 2.

It should be noted that the Support factor (Support factor) is a standard for evaluating elasticity and comfort of a material, that is, a ratio of a pressure value when a product is compressed to a strain of 65% to a pressure value when the product is compressed to a strain of 25%, a product with a high Support factor experiences a softer feeling in an initial stage of compression when a user just sits on the product, and experiences a harder feeling in a later stage of compression after the user sits on the product, so that a sufficient Support effect can be achieved. The supporting factor is at least more than 4, so that the comfort of the product is better.

TABLE 2 standards, conditions and results of Performance test in comparative examples and examples

Note: the method for testing the support factor comprises the following steps: at the constant temperature of 23 ℃, an air fiber block is arranged between an upper pressure plate and a lower pressure plate, the upper pressure plate falls to compress the fiber block at the test speed of 100mm/min, the pressure values of the upper pressure plate are recorded when the air limiting block is highly compressed to the strain of 65 percent and 25 percent and are respectively recorded as P_65％And P_25％The support factor Sf ═ P_65％/P_25％A total of three support factors were averaged. A higher support factor indicates a more comfortable product.

As can be seen from table 2: the thermoplastic polyester elastomer is added with the ethylene copolymer, so that the abnormal sound of the mattress and the seat can be greatly reduced; the addition amount is too small, so that the aim of low noise cannot be achieved; if the addition amount is more than 50%, no noise exists, but the comfort level of people is influenced because the supporting factor is less than 4; and a proper chain extender is added, so that the melt index of the material can be adjusted to meet different processing requirements.

The low-noise high-elasticity 3D air fiber material developed by the technology is used for seats, back pillows, mattresses and sofa cushions of high-speed rails and automobiles, has very comfortable feeling, and particularly has no abnormal sound when people move, turn over and move positions, thereby giving people a quiet feeling. Although the present description is described in terms of embodiments, not every embodiment includes only a single embodiment, and such description is for clarity only, and those skilled in the art should be able to integrate the description as a whole, and the embodiments can be appropriately combined to form other embodiments as will be understood by those skilled in the art.

Therefore, the above description is only a preferred embodiment of the present application, and is not intended to limit the scope of the present application; all changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.

Claims (10)

1. The low-noise high-elasticity 3D air fiber material is characterized by being prepared from the following components in parts by mass:

2. the low noise high elasticity 3D air fiber material according to claim 1, wherein the thermoplastic polyester elastomer has a hardness of 40-63D.

3. The low noise high elastic 3D air fiber material according to claim 1, wherein the ethylene copolymer is at least one of ethylene-vinyl acetate copolymer, ethylene-ethyl acrylate, ethylene-acrylic ester, ethylene-methyl acrylate, ethylene-styrene, ethylene-maleic anhydride, ethylene-vinyl alcohol, ethylene-propylene, ethylene-methyl methacrylate, ethylene-butyl acrylate, ethylene-methyl acrylate-glycidyl methacrylate, ethylene-methyl methacrylate-glycidyl methacrylate, ethylene-n-butyl acrylate-glycidyl methacrylate.

4. The 3D air fiber material with low noise and high elasticity of claim 1, wherein the chain extender is at least one of an epoxy chain extender, a polyol and diisocyanate.

5. The low noise, high resilience 3D air fiber material of claim 1, wherein the catalyst is a cationic metal salt or metal oxide.

6. The low-noise high-elasticity 3D air fiber material according to claim 1, wherein the antioxidant is pentaerythritol dodecathiopropyl ester, 4-bis (α, α -dimethylbenzyl) diphenylamine, bis (2, 4-di-t-butylphenyl) pentaerythritol diphosphite, pentaerythritol tetrakis (BETA- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate), tris [2, 4-di-t-butylphenyl ] phosphite, N' -bis- (3- (3, 5-di-t-butyl-4-hydroxyphenyl) propionyl) hexanediamine, pentaerythritol distearate, N-octadecyl (3, 5-di-t-butyl-4-hydroxyphenyl) propionate, tetramethylene (3, 5-di-t-butyl-4-hydroxyphenyl) methyl ester, at least one of bis [ ethyl-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) ] 2,2 oxamide and dioctadecyl tetraol diphosphite.

7. The low noise, high resilience 3D air fiber material of claim 1, wherein the lubricant is at least one of ethyl bis-oleamide, a primary unsaturated amide derivative compound, a fatty acid ester, a mixture of various amide compounds and soap salts, glycerol, ethylene stearamide, polyethylene wax, talc, white carbon black, polytetrafluoroethylene, and erucamide.

8. The method for preparing a low-noise high-elasticity 3D air fiber material according to any one of claims 1 to 7, which comprises the following steps:

s1: weighing the thermoplastic polyester elastomer, the ethylene copolymer, the chain extender, the antioxidant and the lubricant according to the parts by weight, adding the mixture into a high-speed mixer at the temperature of 120-130 ℃, and mixing for 50-60 minutes to obtain a mixture;

s2: putting the mixture in the S1 into a double-screw extruder for extrusion and granulation to obtain granules;

s3: and (4) putting the granules in the S2 into a solid phase polycondensation kettle for solid phase polycondensation to obtain the 3D fiber material.

9. The method as claimed in claim 8, wherein in step S2, the barrel temperature of the twin-screw extruder is 180-.

10. The method of claim 8, wherein the solid phase polycondensation comprises a first reaction stage and a second reaction stage, wherein:

the reaction temperature of the first reaction stage is 80-120 ℃, the vacuum degree is not more than 1000Pa, and the reaction time is not more than 1 hour;

the reaction temperature of the second reaction stage is 160-200 ℃, the vacuum degree is less than 100Pa, and the reaction time is 12-24 hours.