High-strength soundproof cotton and preparation method thereof

Abstract

The application relates to the technical field of sound insulation cotton, and discloses high-strength sound insulation cotton and a preparation method thereof. The sound insulation cotton is prepared by mixing, extruding, spinning and needling with polylactic acid as a base material and diatomite modifiers and the like as additives. The diatomite modifier is prepared by modifying macromolecular substances on the surface of diatomite. The macromolecular substances can act on active groups at the chain ends of polylactic acid molecules in the subsequent melt extrusion process, play a chain extension role on polylactic acid, realize organic connection between diatomite and polylactic acid molecular chains, greatly improve the interfacial compatibility between the two, effectively improve the mechanical properties of the polylactic acid sound insulation cotton, the rich pore structure of diatomite itself can improve the sound insulation effect of the polylactic acid sound insulation cotton, and in addition, the macromolecular substances contain rich nitrogen and phosphorus flame-retardant elements, so that the flame-retardant performance of the sound insulation cotton can be effectively improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of sound insulation cotton, in particular to a high-strength sound insulation cotton and a preparation method thereof. BACKGROUND

[0002] With the acceleration of urbanization, traffic noise, industrial noise and building sound environmental problems are increasingly prominent, which has a great impact on people's life, so sound insulation materials have been studied more in recent years. Traditional sound insulation materials are mainly glass fiber, mineral wool and polyurethane foam, but they have defects such as non-degradability, dust pollution and flammability. Under this background, biobased degradable materials have become a research hotspot in the field of green sound insulation. Among them, polylactic acid gradually enters the research field of sound insulation materials due to its environmental friendliness and unique physical properties.

[0003] Polylactic acid is made of renewable resources such as corn and straw through lactic acid fermentation and polymerization, and its life cycle carbon emission is reduced by more than 60% compared with petroleum-based materials. After being discarded, it can be completely degraded within 180 days under industrial composting conditions, so it will not cause environmental pollution problems. In addition, polylactic acid supports injection, extrusion, 3D printing and other molding processes, and can be used to prepare complex structure sound insulation components. However, polylactic acid has poor mechanical properties, high brittleness and low strength, which can cause micro-cracks in polylactic acid sound insulation cotton in a vibrating environment, resulting in a decrease in sound absorption effect. In addition, polylactic acid is a flammable material, and under the background of frequent fires, the flammable defect also limits its further application.

[0004] At present, inorganic reinforcing technology is commonly used to reinforce and modify polylactic acid. However, there is an interface problem between inorganic fillers and polylactic acid, and the incompatibility between them can cause the inorganic additives to fail to efficiently exert their own effectiveness. Therefore, the present application provides a polylactic acid sound insulation cotton to solve the problems in the prior art. SUMMARY

[0005] (I) Technical problems to be solved

[0006] In view of the deficiencies in the prior art, the present application provides a high-strength sound insulation cotton and a preparation method thereof.

[0007] (II) Technical solutions

[0008] A high-strength sound insulation cotton comprises the following raw materials in parts by weight:

[0009] 65-75 parts of polylactic acid;

[0010] 3-6.5 parts of diatomite modifier;

[0011] 0.5-1 part of antioxidant;

[0012] 4-8 parts of plasticizer;

[0013] lubricant 1-2 parts;

[0014] stabilizer 0.5-1.5 parts;

[0015] tin catalyst 0.1-0.5 parts.

[0016] As a further scheme of the present application, the preparation method of the diatomite modifier comprises the following steps:

[0017] Step one, diatomite is added into acetone, after addition, ultrasonic dispersion is uniform, then, surface modifier is added into the formed dispersion liquid, catalyst is added at the same time, after addition, temperature is controlled at 30-40℃, after continuous heat preservation and stirring for 3-6h, the product is discharged, centrifugation is carried out, and the product is obtained after washing and vacuum drying;

[0018] Step two, diatomite intermediate and N,N-dimethylformamide are added into a polymerization kettle, ultrasonic frequency is controlled at 80-100kHz, after ultrasonic treatment for 20-30min, reaction type phosphate derivative is added into the polymerization kettle, after stirring for 2-4h under the temperature condition of 30-40℃, 5-isocyanate isophthaloyl chloride and catalyst are added into the polymerization kettle, after continuous stirring polymerization for 12-18h, the solid material is collected after discharge, and the diatomite modifier is prepared after washing and vacuum drying treatment.

[0019] As a further scheme of the present application, the catalyst is triethylamine.

[0020] As a further scheme of the present application, the surface modifier is any one of succinyl chloride, glutaroyl chloride or adipoyl chloride.

[0021] As a further scheme of the present application, the reaction type phosphate derivative is prepared by the following method:

[0022] Diphenyl phosphinic acid oxymethylene methyl ester is added into sulfuric acid solution, after addition, stirring is started, after mixing, temperature is increased to 90-100℃, after keeping at the temperature condition for 1-2h, heating is stopped, the product is separated after natural cooling, washing is carried out until neutral, and vacuum drying treatment is carried out, so that the reaction type phosphate derivative is prepared.

[0023] As a further scheme of the present application, the pH value of the sulfuric acid solution is 2-3.

[0024] As a further scheme of the present application, the mass ratio of the diatomite intermediate, the reaction type phosphate derivative and 5-isocyanate isophthaloyl chloride is 1:0.3-0.6:0.1-0.3.

[0025] In the technical scheme, the diatomite is first surface-modified by using a surface modifier, so that the diatomite surface can carry active acyl chloride groups, and a diatomite intermediate is prepared; since the acyl chloride groups are highly active, the acyl chloride groups of the diatomite intermediate can condense with active hydroxyl groups in the structure of the reactive phosphate derivative, and simultaneously act as an intermediate to continuously condense with acyl chloride groups in the structure of 5-isocyanate isophthaloyl chloride under low temperature conditions, and then connect with the surface modification of the diatomite by an ester bond, and a macromolecular substance with the above-mentioned alternating structure is prepared, and the diatomite modifier is prepared.

[0026] The reactive phosphate derivative is prepared by using diphenyl phosphinic acid oxirane methyl ester as a raw material, and two active hydroxyl groups are formed by hydrolysis of the epoxy groups in the structure under the action of sulfuric acid.

[0027] As a further scheme of the application, the antioxidant is at least one of antioxidant 1010, antioxidant 168, antioxidant 1076 or antioxidant BHT; and the plasticizer is dioctyl phthalate or dibutyl phthalate.

[0028] As a further scheme of the application, the lubricant is polyethylene wax or liquid paraffin; the stabilizer is a calcium-zinc stabilizer; and the tin catalyst is any one of dibutyl tin dilaurate, stannous octoate, dimethyl tin mercaptide or octyl tin mercaptide.

[0029] A preparation method of high-strength soundproof cotton comprises the following steps:

[0030] In the first step, each raw material is weighed according to the weight fraction of each raw material.

[0031] In the second step, each raw material is put into a stirring machine, the temperature is controlled at 90-100 DEG C, and the materials are uniformly mixed by mechanical stirring, then the formed mixture is transferred to a double-screw extruder, the temperature is controlled at 200-220 DEG C, and the mixture is melt-extruded, then the fibers are formed by spinning through a nozzle, and the surface density is controlled at 400-500 g / m 2 The needle punching density is 260-280 needles / cm 2 The soundproof cotton is prepared by a needle punching process.

[0032] (Three) beneficial technical effects

[0033] The diatomite modifier is prepared by modifying macromolecular substances on the surface of diatomite, and the macromolecular substances contain isocyanate groups in the structure, which can react with active groups at the end of the polylactic acid molecular chain under the action of a tin catalyst in a subsequent melt extrusion process, so that the polylactic acid is chain-extended, and the organic connection between the diatomite and the polylactic acid molecular chain is realized, thereby greatly improving the interfacial compatibility between them, enabling the diatomite to be uniformly dispersed in the polylactic acid, and then efficiently exerting the advantages of the diatomite as an inorganic additive to improve the mechanical properties of the polylactic acid acoustic cotton. In addition, the diatomite itself has a rich pore structure, and sound wave energy can be converted into heat energy through mechanisms such as viscous friction, heat conduction and resonance with the pores, thereby improving the sound insulation effect of the polylactic acid acoustic cotton. In addition, the macromolecular substance structure contains rich nitrogen and phosphorus flame-retardant elements, which can quickly form an expanded carbon layer to prevent combustion from continuing, thereby effectively improving the flame-retardant properties of the acoustic cotton. DETAILED DESCRIPTION

[0034] In order to facilitate the understanding of the present application, the present application will be described more fully below. The preferred embodiments of the present application are given below. However, the present application can be realized in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the disclosure of the present application more thorough and comprehensive.

[0035] Preparation Example

[0036] Preparation of the diatomite modifier:

[0037] Step S1, 1.5g of diatomite was added to acetone, after addition, ultrasonic dispersion was uniform, then 0.5g of adipoyl chloride was added to the formed dispersion liquid, 0.1g of triethylamine was added at the same time, after addition, the temperature was controlled at 35℃, and after continuous incubation and stirring for 4h, the product was discharged and centrifuged, washed, and vacuum dried to obtain a diatomite intermediate;

[0038] Step S2, 0.3g of diphenyl phosphinic acid oxirane methyl ester was added to a sulfuric acid solution with a pH value of 2, after addition, stirring was started, and after uniform mixing, the temperature was increased to 90℃, and after keeping at this temperature for 1h, heating was stopped, and after natural cooling, the product was separated, washed to neutral, and then vacuum dried to prepare a reaction type phosphate derivative;

[0039] Step S3, 1.2 g of diatomite intermediate and N, N-dimethylformamide are added into the polymerization kettle, the ultrasonic frequency is controlled at 100 kHz, after ultrasonic treatment for 30 min, 0.6 g of reactive phosphate derivative is added into the polymerization kettle, after stirring at a temperature of 35℃ for 3 h, 0.2 g of 5-isocyanate isophthaloyl chloride and 0.1 g of triethylamine are added into the polymerization kettle, after continuous stirring polymerization for 16 h, the product is discharged, the solid material is collected, and after washing and vacuum drying treatment, the diatomite modifier is prepared.

[0040] The diatomite is purchased from Shanghai Maikelin Biochemical Technology Co., Ltd., and the product number is D858223.

[0041] Example 1: A high-strength sound insulation cotton comprises the following raw materials measured by weight fraction:

[0042] Polylactic acid 65 parts;

[0043] Diatomite modifier 3 parts;

[0044] Antioxidant 1010 0.5 parts;

[0045] Dioctyl phthalate 4 parts;

[0046] Polyethylene wax 1 part;

[0047] Calcium-zinc stabilizer 0.5 parts;

[0048] Dibutyltin dilaurate 0.1 part.

[0049] The preparation method of the sound insulation cotton comprises the following steps:

[0050] First step, according to the weight fraction of each raw material, each raw material is weighed and prepared;

[0051] Second step, each raw material is put into a stirrer, the temperature is controlled at 90℃, and mechanical stirring is carried out for uniform mixing, then the formed mixture is transferred to a twin-screw extruder, the temperature is controlled at 200℃, and melt extrusion is carried out, then spinning is carried out through a nozzle to form fibers, and the surface density is controlled at 450 g / m 2 , the needling density is 268 needles / cm 2 , and the sound insulation cotton can be prepared through the needling process.

[0052] The polylactic acid is purchased from Shanghai Maikelin Biochemical Technology Co., Ltd., and the product number is P921577; the preparation method of the diatomite modifier is shown in the preparation example, and the following are the same.

[0053] Example 2: A high-strength sound insulation cotton comprises the following raw materials measured by weight fraction:

[0054] Polylactic acid 68 parts;

[0055] Dibutyl phthalate 6 parts;

[0056] Antioxidant BHT 0.6 parts;

[0057] Dibutyl phthalate 6 parts;

[0058] Polyethylene wax 1.5 parts;

[0059] Calcium-zinc stabilizer 1 part;

[0060] Dibutyltin dilaurate 1 part.

[0061] The preparation method of the sound insulation cotton comprises the following steps:

[0062] First step, according to the weight fraction of each raw material, each raw material is weighed and prepared;

[0063] Second step, each raw material is put into a blender, the temperature is controlled at 100 DEG C, and mechanical stirring is uniformly mixed, then the formed mixture is transferred to a twin-screw extruder, the temperature is controlled at 210 DEG C, and melt extrusion is carried out, then spinning is carried out through a nozzle to form fibers, and the surface density is controlled at 450 g / m 2 , the needling density is 268 needles / cm 2 , and the sound insulation cotton can be prepared through a needling process.

[0064] Example 3: A high-strength sound insulation cotton comprises the following raw materials measured by weight fraction:

[0065] Polylactic acid 75 parts;

[0066] Dibutyl phthalate 6 parts;

[0067] Antioxidant BHT 1 part;

[0068] Dibutyl phthalate 8 parts;

[0069] Polyethylene wax 2 parts;

[0070] Calcium-zinc stabilizer 1.5 parts;

[0071] Dibutyltin dilaurate 0.5 parts.

[0072] The preparation method of the sound insulation cotton comprises the following steps:

[0073] First step, according to the weight fraction of each raw material, each raw material is weighed and prepared;

[0074] Second step, each raw material is put into the blender, the temperature is controlled at 100℃, and the mixture is uniformly mixed by mechanical stirring. Then the formed mixture is transferred to a twin-screw extruder, the temperature is controlled at 220℃, and the mixture is melt-extruded. Then the mixture is spun through a nozzle to form fibers, and the surface density is controlled at 450g / m 2 , the needling density is 268 needles / cm 2 , and the sound insulation cotton is obtained through the needling process.

[0075] Comparative Example 1

[0076] A high-strength sound insulation cotton includes the following raw materials measured by weight fraction:

[0077] 68 parts of polylactic acid;

[0078] 5.5 parts of diatomite;

[0079] 0.6 parts of antioxidant BHT;

[0080] 6 parts of dibutyl phthalate;

[0081] 1.5 parts of polyethylene wax;

[0082] 1 part of calcium-zinc stabilizer;

[0083] 1 part of dibutyltin dilaurate.

[0084] The preparation method of the sound insulation cotton includes the following steps:

[0085] First step, each raw material is weighed according to the weight fraction;

[0086] Second step, each raw material is put into the blender, the temperature is controlled at 100℃, and the mixture is uniformly mixed by mechanical stirring. Then the formed mixture is transferred to a twin-screw extruder, the temperature is controlled at 210℃, and the mixture is melt-extruded. Then the mixture is spun through a nozzle to form fibers, and the surface density is controlled at 450g / m 2 , the needling density is 268 needles / cm 2 , and the sound insulation cotton is obtained through the needling process.

[0087] Comparative Example 2

[0088] A high-strength sound insulation cotton includes the following raw materials measured by weight fraction:

[0089] 68 parts of polylactic acid;

[0090] 0.6 parts of antioxidant BHT;

[0091] 6 parts of dibutyl phthalate;

[0092] 1.5 parts of polyethylene wax;

[0093] Calcium zinc stabilizer 1 part;

[0094] Dibutyltin dilaurate 1 part.

[0095] The preparation method of the sound insulation cotton comprises the following steps:

[0096] Firstly, each raw material is weighed according to the weight fraction of each raw material;

[0097] Secondly, each raw material is put into a stirring machine, the temperature is controlled at 100 DEG C, and mechanical stirring is performed to mix uniformly, then the formed mixture is transferred to a double-screw extruder, the temperature is controlled at 210 DEG C, and melt extrusion is performed, then spinning is performed through a nozzle to form fibers, and the surface density is controlled at 450 g / m 2 , the needling density is 268 needles / cm 2 , and the sound insulation cotton can be prepared through a needling process.

[0098] Test example

[0099] According to the reference standard GB / T 18696.2-2002, the sound insulation coefficients of the sound insulation cottons in the examples and the comparative examples are tested, the thickness of the sample is 5 mm, and the frequency is 1000 Hz;

[0100] According to the reference standard GB / T 5454-1997, the oxygen index test is performed;

[0101] According to the reference standard GB / T 14337-2022, the mechanical property test is performed;

[0102] The results are shown in the following table:

[0103] According to the test results, the sound insulation cotton prepared in the examples of the present application has excellent performance, and after the diatomite modifier is replaced by diatomite, on the one hand, there is an interface problem between the diatomite and polylactic acid, which cannot be uniformly dispersed, resulting in that the modification advantage cannot be efficiently played, and therefore the performance is greatly reduced.

[0104] The principles and implementations of the present application are described herein with specific examples, and the above description of the embodiments is only used to help understand the method of the present application and its core idea, including the best mode, and also enable any person skilled in the art to practice the present application, including implementing any combined method. It should be noted that, for those skilled in the art, without departing from the principles of the present application, some improvements and modifications can be made to the present application, and these improvements and modifications also fall within the scope of protection of the claims of the present application. The scope of protection of the present application is defined by the claims, and can include other embodiments that can be conceived by those skilled in the art. If these other embodiments have structural elements similar to the textual expression of the claims, or if they include equivalent structural elements that are not substantially different from the textual expression of the claims, then these other embodiments should also be included within the scope of the claims.

[0105] According to the ideal embodiments of the present application, through the above description, relevant personnel can certainly make various changes and modifications within the scope of the technical idea of the present application. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.

Claims

1. A high-strength soundproofing cotton, characterized by, The preparation method of the diatomite modifier comprises the following steps: Step one, diatomite is added into acetone, after adding, ultrasonic dispersion is carried out uniformly, then, a surface modifier is added into the formed dispersion liquid, a catalyst is added at the same time, after adding, the temperature is controlled to be 30-40 DEG C, after continuous heat preservation and stirring for 3-6h, the product is discharged, centrifugation is carried out, and the diatomite intermediate is obtained through washing and vacuum drying; The catalyst is triethylamine; the surface modifier is any one of succinyl chloride, glutaroyl chloride or adipoyl chloride; the reactive phosphate derivative is prepared by the following method: The pH value of the sulfuric acid solution is 2-3. The mass ratio of the diatomite intermediate, the reactive phosphate derivative and 5-isocyanate isophthaloyl chloride is 1:0.3-0.6:0.1-0.

3. The antioxidant is at least one of antioxidant 1010, antioxidant 168, antioxidant 1076 or antioxidant BHT; the plasticizer is dioctyl phthalate or dibutyl phthalate. The lubricant is polyethylene wax or liquid paraffin; the stabilizer is calcium-zinc stabilizer; the tin catalyst is any one of dibutyl tin dilaurate, stannous octoate, dimethyl tin mercaptide or octyl mercaptan tin. The preparation method comprises the following steps: Step one, according to the weight fraction of each raw material, each raw material is weighed and prepared; ​ ​ ​ ​ ​ ​ ​ 2. The high-strength acoustic cotton of claim 1, wherein, ​ 3. The high strength acoustic insulation wool according to claim 1, wherein, ​ 4. The high strength acoustic insulation wool according to claim 1, wherein, ​ 5. A method of producing the high-strength soundproofing cotton according to claim 1, characterized by, ​ ​ Second step, each raw material is put into the blender, the temperature is controlled at 90-100℃, the mixture is mixed uniformly by mechanical stirring, then the formed mixture is transferred to a twin-screw extruder, the temperature is controlled at 200-220℃, melt extrusion is carried out, then spinning is carried out through a nozzle to form fibers, the areal density is controlled at 400-500g / m 2 , the needling density is 260-280 needles / cm 2 , and the sound insulation cotton can be obtained through the needling process.

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