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CN107383395A - Preparation method of graphene color master batch of PET material - Google Patents

Preparation method of graphene color master batch of PET material Download PDF

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Publication number
CN107383395A
CN107383395A CN201710272459.0A CN201710272459A CN107383395A CN 107383395 A CN107383395 A CN 107383395A CN 201710272459 A CN201710272459 A CN 201710272459A CN 107383395 A CN107383395 A CN 107383395A
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pet
graphene
color masterbatch
buffer
grapheme
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劳富文
柯良节
梁思敬
司徒若祺
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/223Packed additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02Polyesters derived from dicarboxylic acids and dihydroxy compounds

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

本发明公开一种PET材料的石墨烯色母料制作方法,包括以下实现步骤:将PET原料进行粉碎,在达到50‑80目的PET粉末之后,开始与石墨烯材料混合,连续搅拌;待石墨烯材料均匀分布于PET粉末上,将混合物料送入循环锅炉中进行加热处理,并加入缓冲剂提高分散渗透效果;将循环锅炉内的温度进一步升高并不断搅拌,使石墨烯材料均匀分散与溶解;将溶解完成的色母料浆液冷却造粒,即形成色母料成品。石墨烯与PET材料结合后,可让PET拉出的织品丝线具有更好的刚性与柔韧性,每条丝线可承受的拉力均可增加50%‑75%。不同比例的色母料混合搭配,可以制作出不同的物理性能标准。

The present invention discloses a method for preparing a graphene masterbatch of PET material, comprising the following implementation steps: crushing the PET raw material, and after reaching 50-80 mesh PET powder, starting to mix with the graphene material and stirring continuously; after the graphene material is evenly distributed on the PET powder, sending the mixed material into a circulating boiler for heating treatment, and adding a buffer to improve the dispersion and penetration effect; further increasing the temperature in the circulating boiler and stirring continuously to evenly disperse and dissolve the graphene material; cooling and granulating the dissolved masterbatch slurry to form a masterbatch finished product. After the graphene is combined with the PET material, the fabric thread drawn from the PET can have better rigidity and flexibility, and the tension that each thread can withstand can be increased by 50%-75%. Masterbatches of different proportions can be mixed and matched to produce different physical performance standards.

Description

PET材料的石墨烯色母料制作方法Graphene masterbatch preparation method of PET material

技术领域technical field

本发明涉及石墨烯的技术领域,尤其涉及一种PET材料的石墨烯色母料制作方法。The invention relates to the technical field of graphene, in particular to a method for preparing a graphene color masterbatch of PET material.

背景技术Background technique

聚对苯二甲酸乙二醇酯,化学式为COC6H4COOCH2CH2O。(英文:Polyethyleneterephthalate,简称PET),由对苯二甲酸二甲酯与乙二醇酯交换或以对苯二甲酸与乙二醇酯化先合成对苯二甲酸双羟乙酯,然后再进行缩聚反应制得。属结晶型饱和聚酯,为乳白色或浅黄色、高度结晶的聚合物,表面平滑有光泽。是生活中常见的一种树脂,可以分为APET、RPET和PETG。Polyethylene terephthalate, the chemical formula is COC6H4COOCH2CH2O. (English: Polyethyleneterephthalate, PET for short), synthesize bishydroxyethyl terephthalate by transesterification of dimethyl terephthalate and ethylene glycol or esterification of terephthalic acid and ethylene glycol, and then polycondensate The reaction is made. It is a crystalline saturated polyester, a milky white or light yellow, highly crystalline polymer with a smooth and shiny surface. It is a common resin in daily life, which can be divided into APET, RPET and PETG.

在较宽的温度范围内具有优良的物理机械性能,长期使用温度可达120℃,电绝缘性优良,甚至在高温高频下,其电性能仍较好,但耐电晕性较差,抗蠕变性,耐疲劳性,耐摩擦性、尺寸稳定性都很好。It has excellent physical and mechanical properties in a wide temperature range. The long-term use temperature can reach 120 ° C. It has excellent electrical insulation. Even at high temperature and high frequency, its electrical properties are still good, but its corona resistance is poor. Creep resistance, fatigue resistance, friction resistance and dimensional stability are all very good.

涤纶是合成纤维中的一个重要品种,是我国聚酯纤维的商品名称。它是以精对苯二甲酸(PTA)或对苯二甲酸二甲酯(DMT)和乙二醇(EG)为原料经酯化或酯交换和缩聚反应而制得的成纤高聚物——聚对苯二甲酸乙二醇酯(PET),经纺丝和后处理制成的纤维。Polyester is an important variety of synthetic fibers and is the trade name of polyester fibers in my country. It is a fiber-forming high polymer prepared from purified terephthalic acid (PTA) or dimethyl terephthalate (DMT) and ethylene glycol (EG) through esterification or transesterification and polycondensation reactions— - Polyethylene terephthalate (PET), fibers made by spinning and post-processing.

涤纶酯纤维被广泛利用与日常生活,如:衣裤,帽子,外套,床单,计算机鼠标垫板等等。工业用聚酯材料如一些纤维,绳子绳索还用于传送带的面料,安全带,涂层织物等等。酯纤维还用于家具填充物,填充枕头等等。从以上的日常生活当中可得到,我们的衣食住行都离不开这种材料,这种材料在不知不觉之间支撑着我们的生活。由于在日常家具中和我们面对的衣物和布料等应用非常广泛,所以提升PET材料的应用和改革是必然的。Polyester fiber is widely used in daily life, such as: underwear, hats, coats, bed sheets, computer mouse pads and so on. Industrial polyester materials such as some fibers, ropes and ropes are also used in fabrics for conveyor belts, safety belts, coated fabrics and more. Ester fibers are also used in furniture stuffing, stuffing pillows, and more. It can be seen from the above daily life that our basic necessities of life are inseparable from this material, and this material supports our life unconsciously. Since it is widely used in daily furniture and the clothing and fabrics we face, it is inevitable to improve the application and reform of PET materials.

发明内容Contents of the invention

针对上述技术中存在的不足之处,本发明提供一种制造方便、性能完善的PET材料的石墨烯色母料制作方法。Aiming at the deficiencies in the above-mentioned technologies, the present invention provides a method for making a graphene color masterbatch of PET material with convenient manufacture and perfect performance.

为了达到上述目的,本发明一种PET材料的石墨烯色母料制作方法,包括以下实现步骤:In order to achieve the above object, a method for preparing a graphene color masterbatch of PET material of the present invention comprises the following steps:

S1、PET原料与石墨烯的混合:将PET原料进行粉碎,在达到50-80目的PET粉末之后,开始与石墨烯材料混合,连续搅拌;S1. Mixing of PET raw material and graphene: crush the PET raw material, and start mixing with the graphene material after reaching 50-80 mesh PET powder, and continuously stir;

S2、加热反应:待石墨烯材料均匀分布于PET粉末上,将混合物料送入循环锅炉中进行加热处理,并加入缓冲剂提高分散渗透效果;S2. Heating reaction: After the graphene material is evenly distributed on the PET powder, the mixed material is sent to a circulating boiler for heat treatment, and a buffer is added to improve the dispersion and penetration effect;

S3、升温分散:将循环锅炉内的温度进一步升高并不断搅拌,使石墨烯材料均匀分散与溶解;S3. Temperature rise and dispersion: further increase the temperature in the circulating boiler and keep stirring, so that the graphene material is evenly dispersed and dissolved;

S4、冷却成粒:将溶解完成的色母料浆液冷却造粒,即形成色母料成品。S4. Cooling and granulation: cooling and granulating the dissolved color masterbatch slurry to form the finished color masterbatch.

其中,在S1中PET原料与石墨烯的混合比例为,1kg PET原料对应添加300g~800g石墨烯材料。Wherein, in S1, the mixing ratio of PET raw material and graphene is such that 1kg of PET raw material corresponds to 300g~800g of graphene material.

其中,在S2中加入的缓冲剂为耐高温的非离子化合物,缓冲剂与混合物料的质量比为1:10000~1:1000。Among them, the buffering agent added in S2 is a high temperature resistant non-ionic compound, and the mass ratio of the buffering agent to the mixed material is 1:10000~1:1000.

其中, 在S2中的缓冲剂包括塑料石油副产物、亲油亲水的非离子材料以及非离子螯合剂。Wherein, the buffering agent in S2 includes plastic petroleum by-products, lipophilic and hydrophilic non-ionic materials and non-ionic chelating agents.

其中,在S3中进一步加热的温度为150~350℃,反复混合分散2~3小时。Wherein, the temperature for further heating in S3 is 150-350°C, and the mixing and dispersion are repeated for 2-3 hours.

其中,在S1中使用的石墨烯材料为具有完整晶格的2D结构晶体。Among them, the graphene material used in S1 is a 2D crystal with a complete lattice.

本发明还公开了一种PET材料的石墨烯色母料,包括以下成分:The invention also discloses a graphene color masterbatch of PET material, comprising the following components:

聚对苯二甲酸乙二醇酯材料;polyethylene terephthalate material;

以及石墨烯材料。and graphene materials.

其中,所述聚对苯二甲酸乙二醇酯材料与石墨烯材料的质量配比为10:3~10:8。Wherein, the mass ratio of the polyethylene terephthalate material to the graphene material is 10:3 to 10:8.

其中,所述石墨烯材料为具有完整晶格的2D结构晶体;该石墨烯色母料还包括缓冲剂,缓冲剂为耐高温的非离子化合物,具体包括塑料石油副产物、亲油亲水的非离子材料以及非离子螯合剂。Wherein, the graphene material is a 2D structure crystal with a complete crystal lattice; the graphene color masterbatch also includes a buffer, which is a high temperature resistant non-ionic compound, specifically including plastic petroleum by-products, lipophilic and hydrophilic Nonionic materials and nonionic chelating agents.

本发明还公开了一种PET材料的石墨烯色母料的应用,用于军备用品士兵的抗菌衣服、防弹衣、航母的飞机应用绳索上。The invention also discloses an application of the graphene color masterbatch of PET material, which is used for the antibacterial clothes, bulletproof vests of military supplies soldiers, and aircraft application ropes of aircraft carriers.

本发明的有益效果是:The beneficial effects of the present invention are:

与现有技术相比,石墨烯与PET材料相结合,可以改善PET材料的性能,并使色母料增添多样化的功能。石墨烯与PET材料结合后,可让PET拉出的织品丝线具有更好的刚性与柔韧性,每条丝线可承受的拉力均可增加50%-75%。不同比例的色母料混合搭配,可以制作出不同的物理性能标准。添加石墨烯的PET材料,拉出的丝线做布料可有效提升布料的保温作用以及抗菌功能。本发明的石墨烯色母料为PET色母料提供了一种全新的发展方向。Compared with the existing technology, the combination of graphene and PET materials can improve the performance of PET materials and add diversified functions to the color masterbatch. The combination of graphene and PET materials can make the fabric threads drawn from PET have better rigidity and flexibility, and the tensile force that each thread can withstand can increase by 50%-75%. Different proportions of color masterbatches can be mixed and matched to produce different physical performance standards. Adding graphene to the PET material, the pulled silk thread can effectively improve the thermal insulation and antibacterial function of the fabric. The graphene color masterbatch of the present invention provides a kind of brand-new development direction for PET color masterbatch.

附图说明Description of drawings

图1为本发明一种PET材料的石墨烯色母料制作方法的工艺流程图。Fig. 1 is the process flow diagram of the graphene color masterbatch production method of a kind of PET material of the present invention.

具体实施方式detailed description

为了更清楚地表述本发明,下面结合附图1对本发明作进一步地描述。In order to express the present invention more clearly, the present invention will be further described below in conjunction with accompanying drawing 1 .

本发明一种PET材料的石墨烯色母料制作方法,包括以下实现步骤:A kind of graphene masterbatch preparation method of PET material of the present invention comprises following realization steps:

S1、PET原料与石墨烯的混合:将PET原料进行粉碎,在达到50-80目的PET粉末之后,开始与石墨烯材料混合,连续搅拌;PET原料与石墨烯的混合比例为,1kg PET原料对应添加300g~800g石墨烯材料;缓冲剂为耐高温的非离子化合物,缓冲剂与混合物料的质量比为1:10000~1:1000,具体的缓冲剂包括塑料石油副产物、亲油亲水的非离子材料以及非离子螯合剂;S1. Mixing of PET raw material and graphene: crush the PET raw material, and after reaching 50-80 meshes of PET powder, start mixing with graphene material and continue stirring; the mixing ratio of PET raw material and graphene is 1kg PET raw material Add 300g~800g graphene material; the buffer is a high temperature resistant non-ionic compound, the mass ratio of the buffer to the mixed material is 1:10000~1:1000, the specific buffer includes plastic petroleum by-products, lipophilic and hydrophilic Non-ionic materials and non-ionic chelating agents;

S2、加热反应:待石墨烯材料均匀分布于PET粉末上,将混合物料送入循环锅炉中进行加热处理,并加入缓冲剂提高分散渗透效果;S2. Heating reaction: After the graphene material is evenly distributed on the PET powder, the mixed material is sent to a circulating boiler for heat treatment, and a buffer is added to improve the dispersion and penetration effect;

S3、升温分散:将循环锅炉内的温度进一步升高并不断搅拌,使石墨烯材料均匀分散与溶解;升温的温度为150~350℃,反复混合分散2~3小时;S3. Warming up and dispersing: further raise the temperature in the circulating boiler and keep stirring, so that the graphene material is uniformly dispersed and dissolved; the temperature for heating up is 150~350°C, and the mixture is repeatedly mixed and dispersed for 2~3 hours;

S4、冷却成粒:将溶解完成的色母料浆液冷却造粒,即形成色母料成品。S4. Cooling and granulation: cooling and granulating the dissolved color masterbatch slurry to form the finished color masterbatch.

本发明还公开了一种PET材料的石墨烯色母料,包括以下成分:The invention also discloses a graphene color masterbatch of PET material, comprising the following components:

聚对苯二甲酸乙二醇酯材料10份;10 parts of polyethylene terephthalate material;

以及石墨烯材料3份,石墨烯材料为具有完整晶格的2D结构晶体。And 3 parts of graphene material, graphene material is a 2D structure crystal with a complete lattice.

在本实施例中,该石墨烯色母料还包括缓冲剂,缓冲剂为耐高温的非离子化合物,具体包括塑料石油副产物、亲油亲水的非离子材料以及非离子螯合剂。In this embodiment, the graphene color masterbatch also includes a buffer, which is a high temperature resistant non-ionic compound, specifically including plastic petroleum by-products, lipophilic and hydrophilic non-ionic materials, and non-ionic chelating agents.

本发明还公开了一种PET材料的石墨烯色母料,包括以下成分:The invention also discloses a graphene color masterbatch of PET material, comprising the following components:

聚对苯二甲酸乙二醇酯材料10份;10 parts of polyethylene terephthalate material;

以及石墨烯材料8份,石墨烯材料为具有完整晶格的2D结构晶体。And 8 parts of the graphene material, the graphene material is a 2D structure crystal with a complete lattice.

在本实施例中,该石墨烯色母料还包括缓冲剂,缓冲剂为耐高温的非离子化合物,具体包括塑料石油副产物、亲油亲水的非离子材料以及非离子螯合剂。In this embodiment, the graphene color masterbatch also includes a buffer, which is a high temperature resistant non-ionic compound, specifically including plastic petroleum by-products, lipophilic and hydrophilic non-ionic materials, and non-ionic chelating agents.

相较于现有技术,石墨烯与PET材料相结合,可以改善PET材料的性能,并使色母料增添多样化的功能。石墨烯与PET材料结合后,可让PET拉出的织品丝线具有更好的刚性与柔韧性,每条丝线可承受的拉力均可增加50%-75%。不同比例的色母料混合搭配,可以制作出不同的物理性能标准。添加石墨烯的PET材料,拉出的丝线做布料可有效提升布料的保温作用以及抗菌功能。本发明的石墨烯色母料为PET色母料提供了一种全新的发展方向。Compared with the existing technology, the combination of graphene and PET materials can improve the performance of PET materials and add diversified functions to the color masterbatch. The combination of graphene and PET materials can make the fabric threads drawn from PET have better rigidity and flexibility, and the tensile force that each thread can withstand can increase by 50%-75%. Different proportions of color masterbatches can be mixed and matched to produce different physical performance standards. Adding graphene to the PET material, the pulled silk thread can effectively improve the thermal insulation and antibacterial function of the fabric. The graphene color masterbatch of the present invention provides a kind of brand-new development direction for PET color masterbatch.

石墨烯是2D结构的晶体,具有良好的传热性,天然性的石墨烯可带有特殊性的天然波,在阳光照射下可激发石墨烯发出带有7hz波频放大的光波,这种光波条件下,可对人体有很大的帮助;石墨烯本身带有透光性和滤光作用,一般单层石墨烯的透光率达到97%,可有效降低紫外光的照射,避免了紫外光的伤害。与此同时石墨烯本身是六角形结构的碳原子而成的大份子,而六角形结构物是一种非常好的抗菌材料,所以作物受细菌感染的机会大大减轻、促进人类健康。另外天然石墨烯本身除带有光波外,还带有本身的远红外线特点。因石墨烯是一种非常好的远红外线材料,远红外线是非常容易让生物细胞分化和促进新陈代谢的能量。石墨烯PET材料的应用非常广泛,此发明希望为PET材料增加上崭新科技的色母料原材料。Graphene is a crystal with 2D structure, which has good heat transfer properties. Natural graphene can have special natural waves, which can excite graphene to emit light waves with 7hz wave frequency amplification under sunlight. This light wave Under certain conditions, it can be of great help to the human body; graphene itself has light transmission and filtering effects. Generally, the light transmittance of single-layer graphene reaches 97%, which can effectively reduce the irradiation of ultraviolet light and avoid ultraviolet light. s damage. At the same time, graphene itself is a large molecule made of carbon atoms with a hexagonal structure, and the hexagonal structure is a very good antibacterial material, so the chances of crops being infected by bacteria are greatly reduced and human health is promoted. In addition, natural graphene itself not only has light waves, but also has its own far-infrared characteristics. Because graphene is a very good far-infrared material, far-infrared rays are very easy to differentiate biological cells and promote metabolism. Graphene PET materials are widely used. This invention hopes to add a new technological color masterbatch raw material to PET materials.

本发明还公开了一种PET材料的石墨烯色母料的应用,用于军备用品士兵的抗菌衣服、防弹衣、航母的飞机应用绳索上。The invention also discloses an application of the graphene color masterbatch of PET material, which is used for the antibacterial clothes, bulletproof vests of military supplies soldiers, and aircraft application ropes of aircraft carriers.

以上公开的仅为本发明的几个具体实施例,但是本发明并非局限于此,任何本领域的技术人员能思之的变化都应落入本发明的保护范围。The above disclosures are only a few specific embodiments of the present invention, but the present invention is not limited thereto, and any changes conceivable by those skilled in the art shall fall within the protection scope of the present invention.

Claims (10)

1. the graphene color masterbatch preparation method of a kind of PET material, it is characterised in that including implemented below step:
The mixing of S1, PET raw material and graphene:PET raw materials are crushed, after the PET powder of 50-80 mesh is reached, opened Beginning mixes with grapheme material, continuously stirs;
S2, heating response:Treat that grapheme material is uniformly distributed on PET powder, mixed material is sent into combined-circulation once-through boiler and carried out Heat, and add buffer and improve scattered osmotic effect;
S3, heating are scattered:Temperature in combined-circulation once-through boiler is further raised and is stirred continuously, make grapheme material it is dispersed with Dissolving;
S4, cooling granulating:The color masterbatch slurries cooling granulation completed will be dissolved, that is, form color masterbatch finished product.
2. the graphene color masterbatch preparation method of PET material according to claim 1, it is characterised in that PET is former in S1 Expect that with the mixed proportion of graphene be that 1kg PET raw materials correspondingly add 300g ~ 800g grapheme materials.
3. the graphene color masterbatch preparation method of PET material according to claim 1, it is characterised in that added in S2 Buffer be resistant to elevated temperatures non-ionic compound, the mass ratio of buffer and mixed material is 1:10000~1:1000.
4. the graphene color masterbatch preparation method of PET material according to claim 3, it is characterised in that slow in S2 Electuary includes the hydrophilic non-ionic material of plastics petroleum by-products, oleophylic and nonionic chelating agent.
5. the graphene color masterbatch preparation method of PET material according to claim 1, it is characterised in that enter one in S3 The temperature of step heating is 150 ~ 350 DEG C, and mixing is scattered 2 ~ 3 hours repeatedly.
6. the graphene color masterbatch preparation method of PET material according to claim 1, it is characterised in that used in S1 Grapheme material be the 2D structure crystals with perfect lattice.
7. the graphene color masterbatch of a kind of PET material, it is characterised in that including following component:
Pet material;
And grapheme material.
8. the graphene color masterbatch of PET material according to claim 7, it is characterised in that the poly terephthalic acid second The quality proportioning of naphthalate material and grapheme material is 10:3~10:8.
9. the graphene color masterbatch of PET material according to claim 8, it is characterised in that the grapheme material is tool There are the 2D structure crystals of perfect lattice;The graphene color masterbatch also includes buffer, and buffer is resistant to elevated temperatures nonionic chemical combination Thing, specifically include the hydrophilic non-ionic material of plastics petroleum by-products, oleophylic and nonionic chelating agent.
A kind of 10. application of the graphene color masterbatch of PET material, it is characterised in that antibacterial clothes for army standby soldier, Flak jackets, aircraft carrier aircraft application rope on.
CN201710272459.0A 2017-04-24 2017-04-24 Preparation method of graphene color master batch of PET material Pending CN107383395A (en)

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CN110012820A (en) * 2018-11-27 2019-07-16 劳富文 Graphene polyester fiber planting mat and method of making the same
CN110024673A (en) * 2018-11-27 2019-07-19 劳富文 Cotton and preparation method thereof is planted in the cultivation of graphene polyester fiber water

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CN109912291A (en) * 2018-11-27 2019-06-21 劳富文 Graphene polyester fiber soil cultivation and planting soil and preparation method thereof
CN110012820A (en) * 2018-11-27 2019-07-16 劳富文 Graphene polyester fiber planting mat and method of making the same
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Application publication date: 20171124