CN111205609A - Novel PBT and preparation method thereof - Google Patents
Novel PBT and preparation method thereof Download PDFInfo
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- CN111205609A CN111205609A CN202010178418.7A CN202010178418A CN111205609A CN 111205609 A CN111205609 A CN 111205609A CN 202010178418 A CN202010178418 A CN 202010178418A CN 111205609 A CN111205609 A CN 111205609A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention provides novel PBT, which comprises 97-99 parts of polybutylene terephthalate, 1-3 parts of calcium carbonate, 2-4 parts of modified silk, 10-14 parts of polyethylene oxide homopolymer and 0.3-0.5 part of graphene oxide in parts by weight; the preparation method of the novel PBT comprises the following steps: (1) pouring polybutylene terephthalate into an extruder according to a proportion for plasticizing; (2) in the hot melting process of polybutylene terephthalate, calcium carbonate, modified silk, polyethylene oxide homopolymer and graphene oxide are added in proportion and uniformly mixed; (3) heating the mixture to a colloid state by a screw of the extruder and extruding; (4) cooling the extruded melt, and stretching; (5) and (3) placing the stretched material still to prepare the novel PBT. The novel PBT is improved from the existing formula, and the prepared string has higher durability and timbre.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to novel PBT and a preparation method thereof.
Background
At present, nylon strings are widely used in musical instruments, after the pitches of the strings are adjusted on the musical instruments, the strings are subjected to sound change and relaxation after being placed for a period of time, and the strings need to be debugged or replaced again, so that the problems of insufficient lingering sound and fullness, insufficient low-frequency brightness, insufficient middle-high frequency fullness and compaction and the like in playing are caused by the inherent characteristics of the traditional nylon strings such as large elasticity, low tensile strength, large creep and high hygroscopicity.
CN106221145B discloses a musical instrument string, which comprises 97 to 99.9 weight percent of polybutylene terephthalate and 0.1 to 3 weight percent of calcium carbonate. Polybutylene terephthalate (PBT nylon) is modified by adding calcium carbonate, and then the internal stress of the internal molecular structure of the material and the creep deformation is changed, so that the stability of the material is improved, the creep resistance is improved, the defects of long string tuning time and fast tuning of the traditional nylon material are overcome, the novel special material for musical instrument strings is produced by utilizing the modified PBT nylon, and the advantages of the novel special material include: high strength is resistant to fracture, the extensibility is little, stable in size, prevent absorbing water so that musical instrument string tone color, tone pitch keep lasting balanced unanimity etc. characteristics in the use, but the durability and the tone quality of material still promote the space.
Disclosure of Invention
The invention provides a novel PBT and a preparation method thereof, which improves the existing formula and further improves the durability and the tone quality.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the novel PBT comprises, by weight, 97-99 parts of polybutylene terephthalate, 1-3 parts of calcium carbonate, 2-4 parts of modified silk, 10-14 parts of polyethylene oxide homopolymer and 0.3-0.5 part of graphene oxide.
Further, the modified silk fabric comprises, by weight, 98 parts of polybutylene terephthalate, 2 parts of calcium carbonate, 3 parts of modified silk, 13 parts of polyethylene oxide homopolymer and 0.4 part of graphene oxide.
Further, the polyethylene oxide homopolymer has a molecular weight of 5 to 10 ten thousand.
Further, the preparation method of the modified silk comprises the following steps: boiling silk in aqueous solution containing sodium sulfite at 100 ℃ for 2-4 hours, heating to 140-160 ℃, pressurizing to 2MPa with nitrogen, preserving heat for 2-3 hours, and cooling and dispersing.
Further, the preparation method of the modified silk comprises the following steps: boiling silk in sodium sulfite aqueous solution at 100 deg.C for 3 hr, heating to 150 deg.C, pressurizing with nitrogen to 2MPa, keeping the temperature for 2.5 hr, cooling, and dispersing.
Further, the sodium sulfite concentration of the sodium sulfite-containing aqueous solution is 2 to 4%.
Further, the mass ratio of the silk to the aqueous solution containing sodium sulfite is 30: 100.
further, the modified silk is single silk, and the length of the modified silk is controlled to be 1-2 cm.
The invention also provides a preparation method of the novel PBT, which comprises the following steps:
(1) pouring polybutylene terephthalate into an extruder according to a proportion for plasticizing;
(2) in the hot melting process of polybutylene terephthalate, calcium carbonate, modified silk, polyethylene oxide homopolymer and graphene oxide are added in proportion and uniformly mixed;
(3) heating the mixture to a colloid state by a screw of the extruder and extruding;
(4) cooling the extruded melt to 8-15 ℃, and then stretching;
(5) placing the stretched material in an incubator at 85-120 ℃ and standing for 15-60 minutes.
Further, the barrel of the extruder sequentially comprises a first temperature zone 225-.
The invention has the beneficial effects that:
in the prior art, after calcium carbonate is added into polybutylene terephthalate (PBT nylon) for modification, the internal stress of the internal molecular structure and production creep of the material is changed, so that the stability and creep resistance of the material are improved, the defects of long string sound fixing time and fast sound changing of the traditional nylon material are overcome, and the performance of the material is provided with a further improved space.
According to the invention, the modified silk, the polyethylene oxide homopolymer and the graphene oxide are added into the material taking PBT and calcium carbonate as main bodies, so that the timbre and the durability are synergistically improved. By adding calcium carbonate in the prior art, the calcium carbonate is difficult to disperse uniformly and is easy to agglomerate to cause wire drawing fracture and unbalanced mass at the same time, and the timbre of strings made by wire drawing is reduced when the strings vibrate. According to the invention, the modified silk is added, so that the stability of the silk at high temperature is greatly improved through modification, the strength and elasticity of the silk are further improved, the strength and durability of the wire drawing material can be effectively improved through the addition of the modified silk with a certain length, the internal vibration of strings can be reduced through the addition of the silk, the energy loss is reduced, and the tone is improved; the polyethylene oxide homopolymer has a strong adhesion effect, can be effectively adhered to the surface of silk, promotes the silk to disperse in a polymer system, can modify PBT, improves the compatibility of PBT and calcium carbonate, and can effectively improve the balance degree of mass distribution by polyethylene oxide, thereby effectively improving the tone; the addition of graphite alkene can effectively improve durability and improve physical properties, through adding together with silk, its high surface energy disperses on the surface of silk more easily, through the effectual improvement compatibility of the addition of polyethylene oxide homopolymer to improve whole mass distribution balance, can effectual improvement tone quality.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Any modifications that can be easily made by a person skilled in the art to the present invention without departing from the technical solutions of the present invention will fall within the scope of the claims of the present invention.
Example 1
The novel PBT comprises 98 parts of polybutylene terephthalate, 2 parts of calcium carbonate, 3 parts of modified silk, 13 parts of polyethylene oxide homopolymer and 0.4 part of graphene oxide in parts by weight; the molecular weight of the polyethylene oxide homopolymer is 5 ten thousand; the preparation method of the modified silk comprises the following steps: boiling silk in sodium sulfite aqueous solution at 100 deg.C for 3 hr, heating to 150 deg.C, pressurizing with nitrogen to 2MPa, keeping the temperature for 2.5 hr, cooling, and dispersing.
The sodium sulfite concentration of the sodium sulfite-containing aqueous solution was 3%. The mass ratio of the silk to the aqueous solution containing sodium sulfite is 30: 100. the modified silk is single silk, and the length of the modified silk is controlled to be 1-2 cm.
A preparation method of novel PBT comprises the following steps:
(1) pouring polybutylene terephthalate into an extruder according to a proportion for plasticizing;
(2) in the hot melting process of polybutylene terephthalate, calcium carbonate, modified silk, polyethylene oxide homopolymer and graphene oxide are added in proportion and uniformly mixed;
(3) heating the mixture to a colloid state by a screw of the extruder and extruding;
(4) cooling the extruded melt to 12 ℃, and stretching;
(5) the stretched material was placed in an oven at 100 ℃ and allowed to stand for 40 minutes. The machine barrel of the extruder sequentially comprises a first temperature zone 230 ℃, a second temperature zone 240 ℃, a third temperature zone 250 ℃, a fourth temperature zone 260 ℃, a fifth temperature zone 270 ℃, a sixth temperature zone 280 ℃ and a seventh temperature zone 270 ℃ according to the material conveying direction.
Example 2
The novel PBT comprises 99 parts of polybutylene terephthalate, 1 part of calcium carbonate, 4 parts of modified silk, 10 parts of polyethylene oxide homopolymer and 0.5 part of graphene oxide in parts by weight; the molecular weight of the polyethylene oxide homopolymer is 10 ten thousand; the preparation method of the modified silk comprises the following steps: boiling silk in aqueous solution containing sodium sulfite at 100 deg.C for 4 hr, heating to 140 deg.C, pressurizing with nitrogen to 2MPa, keeping the temperature for 3 hr, cooling, and dispersing.
The sodium sulfite concentration of the sodium sulfite-containing aqueous solution was 4%. The mass ratio of the silk to the aqueous solution containing sodium sulfite is 30: 100. the modified silk is single silk, and the length of the modified silk is controlled to be 1-2 cm.
The preparation method is the same as that of example 1.
Example 3
The novel PBT comprises 97 parts by weight of polybutylene terephthalate, 3 parts by weight of calcium carbonate, 2 parts by weight of modified silk, 14 parts by weight of polyethylene oxide homopolymer and 0.3 part by weight of graphene oxide; the molecular weight of the polyethylene oxide homopolymer is 5 million; the preparation method of the modified silk comprises the following steps: boiling silk in sodium sulfite aqueous solution at 100 ℃ for 2 hours, heating to 160 ℃, pressurizing to 2MPa with nitrogen, preserving heat for 2 hours, cooling and dispersing.
The sodium sulfite concentration of the sodium sulfite-containing aqueous solution was 2%. The mass ratio of the silk to the aqueous solution containing sodium sulfite is 30: 100. the modified silk is single silk, and the length of the modified silk is controlled to be 1-2 cm.
The preparation method is the same as that of example 1.
Comparative example 1
Same as example 1, except that modified silk, polyethylene oxide homopolymer, graphene oxide were not added to the raw materials.
Comparative example 2
Same as example 1 except that modified silk was not added to the raw material.
Comparative example 3
Same as example 1 except that no polyethylene oxide homopolymer was added to the feed.
Comparative example 4
Same as example 1 except that no graphene oxide was added to the raw material.
Comparative example 5
Same as example 1, except that the raw material silk was boiled and pressurized in an aqueous solution without adding sodium sulfite.
Comparative example 6
Common silk was used in place of modified silk in the same manner as in example 1.
Comparative example 7
A polymeric material was prepared according to CN106221145B example 1.
The products of examples 1-3 and comparative examples 1-7 were stretched to the same 0.65 gauge string diameter in step 4 and then tested for average decibel sound at 440 Hz; after all the strings are fixed and fixed (taking the center C as a standard), 10 ten thousand times of string plucking is carried out, the deviation of the tone marks is tested, and the data of the durability shows that the larger the deviation is, the more the strings are deformed due to the excessive use times, and the worse the durability is.
TABLE 1
As can be seen from the comparison of the data in the embodiment 1 and the data in the comparative examples 1 to 4, the modified silk, the polyethylene oxide homopolymer and the graphene oxide have a synergistic effect, and the volume can be effectively increased, the sound is brighter, the tone is better and the durability can be synergistically improved when the modified silk, the polyethylene oxide homopolymer and the graphene oxide are added under the same frequency; as can be seen from comparison of the data of example 1 and comparative examples 5 to 6, the durability can be effectively improved and the volume can be increased to a certain extent by the silk modification preparation method; as can be seen from the comparison of the data of examples 1-3 and comparative example 7, the product of the present invention can effectively improve the product performance compared with the prior art.
Claims (10)
1. A novel PBT is characterized in that: according to the weight portion, the modified silk fabric comprises 97-99 portions of polybutylene terephthalate, 1-3 portions of calcium carbonate, 2-4 portions of modified silk, 10-14 portions of polyethylene oxide homopolymer and 0.3-0.5 portion of graphene oxide.
2. The novel PBT according to claim 1, wherein: the modified silk fabric comprises, by weight, 98 parts of polybutylene terephthalate, 2 parts of calcium carbonate, 3 parts of modified silk, 13 parts of polyethylene oxide homopolymer and 0.4 part of graphene oxide.
3. The novel PBT according to claim 1 or 2, characterized in that: the molecular weight of the polyethylene oxide homopolymer is 5-10 ten thousand.
4. The novel PBT according to claim 1 or 2, characterized in that: the preparation method of the modified silk comprises the following steps: boiling silk in aqueous solution containing sodium sulfite at 100 ℃ for 2-4 hours, heating to 140-160 ℃, pressurizing to 2MPa with nitrogen, preserving heat for 2-3 hours, and cooling and dispersing.
5. The novel PBT according to claim 4, wherein the modified silk is prepared by a method comprising: boiling silk in sodium sulfite aqueous solution at 100 deg.C for 3 hr, heating to 150 deg.C, pressurizing with nitrogen to 2MPa, keeping the temperature for 2.5 hr, cooling, and dispersing.
6. The novel PBT according to claim 4, wherein: the sodium sulfite concentration of the sodium sulfite-containing aqueous solution is 2 to 4%.
7. The novel PBT according to claim 4, wherein: the mass ratio of the silk to the aqueous solution containing sodium sulfite is 30: 100.
8. the novel PBT according to claim 4, wherein: the modified silk is single silk, and the length of the modified silk is controlled to be 1-2 cm.
9. A process for the preparation of a novel PBT according to any one of claims 1 to 8, comprising the steps of:
(1) pouring polybutylene terephthalate into an extruder according to a proportion for plasticizing;
(2) in the hot melting process of polybutylene terephthalate, calcium carbonate, modified silk, polyethylene oxide homopolymer and graphene oxide are added in proportion and uniformly mixed;
(3) heating the mixture to a colloid state by a screw of the extruder and extruding;
(4) cooling the extruded melt to 8-15 ℃, and then stretching;
(5) placing the stretched material in an incubator at 85-120 ℃ and standing for 15-60 minutes.
10. The process for the preparation of the novel PBT according to claim 9, characterized in that: the machine barrel of the extruder sequentially comprises a first temperature zone 225-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010178418.7A CN111205609B (en) | 2020-03-14 | 2020-03-14 | PBT composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010178418.7A CN111205609B (en) | 2020-03-14 | 2020-03-14 | PBT composite material and preparation method thereof |
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| Publication Number | Publication Date |
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| CN111205609A true CN111205609A (en) | 2020-05-29 |
| CN111205609B CN111205609B (en) | 2022-07-12 |
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| CN202010178418.7A Active CN111205609B (en) | 2020-03-14 | 2020-03-14 | PBT composite material and preparation method thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002037991A (en) * | 2000-07-26 | 2002-02-06 | Matsushita Electric Works Ltd | Polybutylene terephthalate resin molding material and molding of the same |
| US20090183620A1 (en) * | 2007-10-29 | 2009-07-23 | Thomastik-Infeld Gesellschaft M.B.H. | Music string |
| US20090223344A1 (en) * | 2008-03-07 | 2009-09-10 | Thomastik-Infeld Gesellschaft m.b.H. | A musical string |
| CN101974596A (en) * | 2010-11-11 | 2011-02-16 | 湖北远成药业有限公司 | Extraction method of silk peptide |
| CN106221145A (en) * | 2016-08-17 | 2016-12-14 | 广州市罗曼士乐器制造有限公司 | A kind of material modified and strings for musical instruments |
| CN106751578A (en) * | 2016-12-26 | 2017-05-31 | 上海金山锦湖日丽塑料有限公司 | Biological fiber filling PBT composition and preparation method thereof |
-
2020
- 2020-03-14 CN CN202010178418.7A patent/CN111205609B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002037991A (en) * | 2000-07-26 | 2002-02-06 | Matsushita Electric Works Ltd | Polybutylene terephthalate resin molding material and molding of the same |
| US20090183620A1 (en) * | 2007-10-29 | 2009-07-23 | Thomastik-Infeld Gesellschaft M.B.H. | Music string |
| US20090223344A1 (en) * | 2008-03-07 | 2009-09-10 | Thomastik-Infeld Gesellschaft m.b.H. | A musical string |
| CN101974596A (en) * | 2010-11-11 | 2011-02-16 | 湖北远成药业有限公司 | Extraction method of silk peptide |
| CN106221145A (en) * | 2016-08-17 | 2016-12-14 | 广州市罗曼士乐器制造有限公司 | A kind of material modified and strings for musical instruments |
| CN106751578A (en) * | 2016-12-26 | 2017-05-31 | 上海金山锦湖日丽塑料有限公司 | Biological fiber filling PBT composition and preparation method thereof |
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| CN111205609B (en) | 2022-07-12 |
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