CN115785658A - Rat bite preventing nylon master batch and preparation method thereof - Google Patents
Rat bite preventing nylon master batch and preparation method thereof Download PDFInfo
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- CN115785658A CN115785658A CN202211693588.4A CN202211693588A CN115785658A CN 115785658 A CN115785658 A CN 115785658A CN 202211693588 A CN202211693588 A CN 202211693588A CN 115785658 A CN115785658 A CN 115785658A
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- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 84
- 239000004677 Nylon Substances 0.000 title claims abstract description 50
- 229920001778 nylon Polymers 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- YKPUWZUDDOIDPM-SOFGYWHQSA-N capsaicin Chemical compound COC1=CC(CNC(=O)CCCC\C=C\C(C)C)=CC=C1O YKPUWZUDDOIDPM-SOFGYWHQSA-N 0.000 claims abstract description 204
- 229960002504 capsaicin Drugs 0.000 claims abstract description 102
- 235000017663 capsaicin Nutrition 0.000 claims abstract description 102
- 239000004743 Polypropylene Substances 0.000 claims abstract description 40
- -1 polypropylene Polymers 0.000 claims abstract description 39
- 229920001155 polypropylene Polymers 0.000 claims abstract description 39
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 12
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 claims description 16
- 241000723346 Cinnamomum camphora Species 0.000 claims description 13
- 229960000846 camphor Drugs 0.000 claims description 13
- 229930008380 camphor Natural products 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000012745 toughening agent Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
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- 238000001035 drying Methods 0.000 claims description 6
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- 238000010992 reflux Methods 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
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- 230000002265 prevention Effects 0.000 abstract description 21
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- 239000000463 material Substances 0.000 description 8
- 241000699666 Mus <mouse, genus> Species 0.000 description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
- 241000699670 Mus sp. Species 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229940025250 camphora Drugs 0.000 description 3
- 239000010238 camphora Substances 0.000 description 3
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- 238000013461 design Methods 0.000 description 2
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- 235000000621 Bidens tripartita Nutrition 0.000 description 1
- 240000004082 Bidens tripartita Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000256602 Isoptera Species 0.000 description 1
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- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
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- 208000006637 fused teeth Diseases 0.000 description 1
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Abstract
The application relates to the technical field of high polymer materials, and particularly discloses a rat bite prevention nylon master batch and a preparation method thereof. The rat-bite-preventing nylon master batch comprises the following raw materials in percentage by mass: 1-5% of capsaicin master batch, 10-25% of flexibilizer, 0.5-2% of other auxiliary agents and the balance of nylon 6; the capsaicin masterbatch is obtained by wrapping capsaicin with polypropylene. The obtained ratproof nylon master batch has less decomposition of capsaicin and better ratproof effect.
Description
Technical Field
The application relates to the technical field of high polymer materials, in particular to a rat bite prevention nylon master batch and a preparation method thereof.
Background
Nylon is also called polyamide and has good processing performance, wear resistance, self-lubricating property and chemical corrosion resistance. Based on the good physical and chemical properties of the nylon material, the nylon material has good application in a plurality of fields.
Nylon can be used as a coating protection material for various electric wire and cable products, and generally, a certain chemical agent is added into a cable sheath material to prevent and treat fire based on the condition that the teeth bite invasion of animals such as mice and the like to the electric wire and cable easily causes power failure, communication interruption and even short circuit. The capsaicin is an effective ant-proof and rat-proof repellent, the strong pungent taste of the capsaicin is utilized, oral mucosa and gustatory nerve of the murine animals can be strongly stimulated to abandon chewing, and the capsaicin can kill termites at the same time, so that the wire and cable has wide application prospect.
In the preparation process of the rat bite prevention nylon master batch, the capsaicin is directly blended with the nylon raw material and extruded. Because capsaicin is easily decomposed at high temperature, the obtained nylon material has poor rat bite prevention effect. Therefore, it is necessary to design a nylon masterbatch which can effectively reduce the decomposition of capsaicin and has an excellent rat bite prevention effect.
Disclosure of Invention
In order to design a nylon master batch which can effectively reduce the decomposition of capsaicin and has excellent rat bite prevention effect, the application provides a rat bite prevention nylon master batch and a preparation method thereof.
In a first aspect, the application provides a ratproof nylon master batch, which adopts the following technical scheme:
the rat-bite-preventing nylon master batch comprises the following raw materials in percentage by mass: 1-5% of capsaicin master batch, 10-25% of flexibilizer, 0.5-2% of other auxiliary agents and the balance of nylon 6; the capsaicin masterbatch is obtained by wrapping capsaicin with polypropylene.
By adopting the technical scheme, the polypropylene is a better heat insulation material because the thermal conductivity coefficient is about 0.15-0.24W/(m.K), and the melting point of the polypropylene is lower, so that the processing temperature can be reduced, and the decomposition of capsaicin is effectively reduced. Therefore, the capsaicin exists in the system in the form of capsaicin masterbatch, and the polypropylene can effectively isolate high temperature in the extrusion process, thereby effectively reducing the decomposition of the capsaicin. The capsaicin in the obtained rat bite prevention nylon master batch is less influenced by a high-temperature extrusion environment, and a good rat bite prevention effect can be kept. And the dispersion effect of the polypropylene-coated capsaicin in the system is better, namely the polypropylene-coated capsaicin composite material has positive significance for promoting the nylon material to achieve a relatively uniform rat bite prevention effect.
In a specific practical implementation mode, the nylon master batch comprises the following raw materials in percentage by mass: 2.5-4% of capsaicin master batch, 15-20% of toughening agent, 0.5-1% of other auxiliary agents and the balance of nylon 6.
By adopting the technical scheme, the mass percentages of the raw materials are further optimized, and the nylon master batch has positive significance for improving the comprehensive performance of the nylon master batch.
In a specific possible embodiment, the toughening agent is POE grafted with maleic anhydride.
By adopting the technical scheme, the maleic anhydride grafted POE introduces a strong polar side group on the nonpolar molecular main chain, so that the maleic anhydride grafted POE can be used as a bridge for improving the adhesion and compatibility of polar materials and nonpolar materials, has a good toughening effect, and can effectively improve the impact resistance, the cold resistance and the molding processability of nylon.
In a particular embodiment, the other adjuvant comprises an antioxidant.
In a specific possible embodiment, the nylon 6 is extrusion grade chip with a viscosity of 2.4 to 3.0.
In a specific embodiment, the concentration of capsaicin in the capsaicin concentrate is 5-10% by mass.
In a specific embodiment, the preparation method of the capsaicin masterbatch comprises the following steps:
adding polypropylene and capsaicin into an organic solvent, and refluxing and heating until the polypropylene and the capsaicin are completely dissolved to obtain a mixed solution; and adding the mixed solution into acetone for cooling and precipitating, filtering after precipitation is finished, and cleaning filter residues to obtain the capsaicin master batch.
By adopting the technical scheme to prepare the capsaicin masterbatch, the operation is simple, the effect of wrapping capsaicin by polypropylene is good, and the industrial production prospect is achieved.
In a specific implementation mode, the filter residue is crushed and passes through a 100-mesh screen, and the screened-out product is the capsaicin masterbatch meeting the particle size requirement.
In a specific embodiment, the preparation method of the capsaicin masterbatch comprises the following steps:
adding polypropylene and capsaicin into an organic solvent, and refluxing and heating until the polypropylene and the capsaicin are completely dissolved to obtain a mixed solution; dissolving Camphora 1-2% of capsaicin in acetone, adding the mixture into acetone dissolved with Camphora, cooling and precipitating, filtering after precipitation, cleaning the filter residue, and drying the filter residue at 70-80 deg.C for 30-60min to obtain capsaicin mother granule.
By adopting the technical scheme, a proper amount of camphor is further added into the acetone, and the camphor is also wrapped by the polypropylene in the process of wrapping the capsaicin by the polypropylene; heating Camphora to sublimate and forming a plurality of pore structures in the polypropylene wrapping layer during the subsequent drying process of the filter residue at 70-80 ℃. Because the heat conductivity coefficient of the air is lower than that of the polypropylene, and is only about 0.023W/(m.K), the heat insulation performance of the wrapping layer can be effectively improved due to the existence of a plurality of pore structures in the polypropylene wrapping layer; meanwhile, the processing temperature can be reduced by matching with the characteristic of lower melting point of polypropylene, so that the condition that capsaicin is decomposed in a subsequent high-temperature extrusion environment can be further reduced.
In addition, the camphor remained in the capsaicin master batch has good expelling effect on insects, mice and other organisms, so that the obtained rat bite prevention effect of the nylon master batch is further improved.
In a second aspect, the application provides a preparation method of a rat-bite-preventing nylon master batch, which adopts the following technical scheme:
a preparation method of a ratproof nylon master batch comprises the following steps:
mixing the capsaicin master batch, the toughening agent, other auxiliaries and nylon 6 to obtain a mixture; and extruding and granulating the mixture by an extruder to obtain the ratproof nylon master batch.
In summary, the present application has the following beneficial effects:
1. capsaicin in this application adds in the system with the form of capsaicin master batch, and the polypropylene parcel layer has good heat-proof quality in the capsaicin master batch to can effectively reduce the decomposition of capsaicin in follow-up high temperature extrusion environment, the nylon master batch rat bite prevention effect that obtains is better.
2. The method for preparing the capsaicin masterbatch is simple, the obtained capsaicin masterbatch has a good effect, and the industrial production prospect is good.
3. This application is further at the in-process of preparation capsaicin master batch add camphor for capsaicin and camphor are wrapped up by polypropylene together, thereby utilize camphor to take place to sublime in follow-up drying process, at the inside porous structure that forms of polypropylene wrapping layer, further improve the heat-proof quality of polypropylene wrapping layer, further reduce the decomposition loss of capsaicin in the extrusion system.
Detailed Description
As will be described in further detail in the following with reference to examples and comparative examples, the raw materials involved in the present application are all commercially available, wherein the polypropylene is obtained from homopolymerized PP powder from Nanjing oil refinery, the brand is 150-1, and the melt index is 13-18g/10min;
the organic solvent comprises at least one of xylene, toluene and absolute ethyl alcohol, and preferably xylene.
Example 1
The rat bite prevention nylon master batch comprises the following raw materials in percentage by mass: 3kg of capsaicin master batch, 17kg of toughening agent, 0.8kg of other additives and 6.2kg of nylon;
wherein the toughening agent is POE grafted by maleic anhydride, the melt index is 0.5-5.0g/10min, and the grafting rate is 0.3% -1.5%;
the other auxiliary agent is antioxidant 1010;
the nylon 6 is an extrusion grade slice, and the viscosity is 2.4-3.0;
the preparation method of the capsaicin master batch comprises the following steps:
adding 500g of polypropylene and 43g of capsaicin into 7L of dimethylbenzene, and heating under reflux at the temperature of 150 +/-5 ℃ until the polypropylene and the capsaicin are completely dissolved to obtain a mixed solution; and (3) putting the mixed solution into acetone, cooling and precipitating at normal temperature until no precipitate exists, then filtering, cleaning filter residues, crushing the filter residues, and sieving the crushed filter residues through a 100-mesh sieve to obtain capsaicin master batches meeting the particle size requirement.
The preparation method of the ratproof nylon master batch comprises the following steps:
weighing the raw materials according to the specified mass, adding the raw materials into a high-speed mixer, mixing for 4 minutes, and discharging to obtain a mixture; adding the mixture into a double-screw extruder, and extruding and granulating to obtain the ratproof nylon master batch; the process conditions of the extruder are as follows: the temperature of the double screw extruder in the 1-2 area is 200-205 deg.c, the temperature of the 3-4 area is 205-230 deg.c, the temperature of the 5-6 area is 210-220 deg.c, the temperature of the 7-8 area is 200-210 deg.c, the temperature of the nine area and the machine head is 200-210 deg.c, and the screw rotation speed is 300 rpm.
The difference between examples 2-5 and example 1 is that the raw material ratio of the ratproof nylon masterbatch is different, which is specifically shown in the following table.
Table 1 raw material proportioning table
| Raw material/kg | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Capsaicin masterbatch | 3 | 1 | 2.5 | 5 | 4 |
| Toughening agent | 17 | 25 | 15 | 10 | 20 |
| Other auxiliaries | 0.8 | 0.5 | 1.5 | 2 | 1 |
| Nylon 6 | 79.2 | 73.5 | 81 | 83 | 75 |
Example 6
The difference between this example and example 1 is that the concentration of capsaicin in the capsaicin masterbatch is 5% by mass, i.e., the amount of capsaicin added during the preparation of the capsaicin masterbatch is 26g.
Example 7
The difference between this example and example 1 is that the concentration of capsaicin in the capsaicin masterbatch by mass is 10%, that is, the addition amount of capsaicin during the preparation of the capsaicin masterbatch is 56g.
Example 8
The difference between this example and example 1 is that the concentration of capsaicin in the capsaicin masterbatch is 2% by mass, i.e., the amount of capsaicin added during the preparation of the capsaicin masterbatch is 10g.
Example 9
The difference between the present embodiment and embodiment 1 is that the mass percentage concentration of capsaicin in the capsaicin masterbatch is 15%, that is, the addition amount of capsaicin during the preparation of the capsaicin masterbatch is 88g.
Example 10
The difference between this example and example 1 is that the preparation method of capsaicin masterbatch is as follows:
adding 500g of polypropylene and 43g of capsaicin into 7L of dimethylbenzene, and heating under reflux at the temperature of 150 +/-5 ℃ until the polypropylene and the capsaicin are completely dissolved to obtain a mixed solution; dissolving 0.7g of camphor in acetone, adding the mixed solution into the acetone dissolved with the camphor, cooling and precipitating at normal temperature until no precipitate exists, then filtering, cleaning filter residue, drying the filter residue for 50min at the temperature of 80 ℃, and screening out substances which pass through a 100-mesh screen after the filter residue is crushed, namely the capsaicin master batch meeting the requirement of the particle size.
Example 11
This example is different from example 10 in that camphor was added in an amount of 0.43g.
Example 12
This example is different from example 10 in that camphor was added in an amount of 0.86g.
Comparative example 1
This comparative example differs from example 1 in that the capsaicin masterbatch is replaced with 43g of capsaicin and the balance is made up with nylon 6.
Comparative example 2
This comparative example differs from example 1 in that 43g of capsaicin and 2957g of polypropylene were used in place of the capsaicin masterbatch.
Performance detection test method
Rat bite prevention test
1. Respectively drying the ratproof nylon master batches prepared in the examples 1-12 and the comparative examples 1-2 in a 110 ℃ blast oven for 6 hours, and performing injection molding on the dried particles on an injection molding machine to obtain a rectangular sheet sample with the size of 150mm multiplied by 30 mm;
1. respectively feeding 20 mice for tests which are half male and female and are healthy (no loss of upper and lower incisors) into mouse cages, feeding one mouse for tests into one mouse cage, and referring to the standard of GB/T29199-2012 'optical cable rat-proof performance test method' for the relevant requirements of the mouse for tests and the mouse cages;
2. placing the samples in the mouse cages, taking out the samples in 20 mouse cages after 7 days, recording the total number of tooth marks, wherein the tooth marks comprise single-tooth marks and double-tooth marks, and normally feeding test mice during a test period; the placement, the tooth trace recording and the experimental rat feeding operation of the sample refer to the standard of GB/T29199-2012 'rat-proof performance test method for optical cables'.
3. Evaluation criteria of rat-proof grade: grade 1, the total number of tooth marks is less than or equal to 5; 2 grade, 5 teeth are larger than the total number of teeth and less than or equal to 10 teeth; grade 3, 10 teeth are more than or equal to 20 teeth; 4 grades, 20 teeth marks are more than 20 and the total teeth mark number is less than or equal to 30 teeth marks; grade 5, wherein the total number of tooth marks is more than 30 and less than or equal to 50; grade 6, total number of teeth marks > 50.
TABLE 2 test data sheet
Through the detection data of the table 2, the rat-bite prevention grade of the obtained rat-bite prevention nylon master batch can reach more than grade 3, and the test results of the embodiment 1 and the comparative examples 1-2 are specifically combined, the comparative example 1 adopts a mode of directly adding capsaicin, and the obtained rat-bite prevention grade of the rat-bite prevention nylon master batch only reaches grade 6, because the directly added capsaicin is decomposed in an extruded high-temperature environment, and the rat-bite prevention effect is greatly reduced. In comparative example 2, on the basis of comparative example 1, the addition of polypropylene is retained, but the rat-bite prevention grade is still 6, which shows that the addition of polypropylene has no substantial effect on improving the rat-bite prevention effect, and that the polypropylene is used for wrapping capsaicin, namely the capsaicin is added in a capsaicin masterbatch manner.
Specifically, the test results of the embodiment 1 and the embodiment 10 are combined, the rat-bite-preventing grade of the rat-bite-preventing nylon master batch in the embodiment 10 can reach 1 grade, and the analysis is that the polypropylene wrapping layer has better heat insulation performance because the camphor is added to promote the polypropylene wrapping layer to form a porous structure inside the polypropylene wrapping layer in the embodiment 10, so that the decomposition of capsaicin in a high-temperature extrusion environment can be further reduced, and the rat-bite-preventing effect is better.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The rat-bite-preventing nylon master batch is characterized by comprising the following raw materials in percentage by mass: 1-5% of capsaicin master batch, 10-25% of flexibilizer, 0.5-2% of other auxiliary agents and the balance of nylon 6; the capsaicin masterbatch is obtained by wrapping capsaicin with polypropylene.
2. The ratproof nylon master batch according to claim 1, wherein the nylon master batch comprises the following raw materials by mass: 2.5-4% of capsaicin master batch, 15-20% of toughening agent, 0.5-1% of other auxiliary agents and the balance of nylon 6.
3. The ratproof nylon master batch according to claim 1, wherein the toughening agent is POE grafted with maleic anhydride.
4. The ratproof nylon master batch according to claim 1, wherein the other auxiliary agents comprise antioxidants.
5. The rat-bite-preventing nylon master batch according to claim 1, wherein the nylon 6 is an extrusion-grade slice with the viscosity of 2.4-3.0.
6. The rat-bite-preventing nylon masterbatch according to claim 1, wherein the mass percentage concentration of capsaicin in the capsaicin masterbatch is 5-10%.
7. The rat-bite-preventing nylon master batch according to claim 1, wherein the preparation method of the capsaicin master batch comprises the following steps:
adding polypropylene and capsaicin into an organic solvent, and refluxing and heating until the polypropylene and the capsaicin are completely dissolved to obtain a mixed solution; and adding the mixed solution into acetone for cooling and precipitating, filtering after precipitation is finished, and cleaning filter residues to obtain the capsaicin master batch.
8. The rat-bite-preventing nylon master batch as claimed in claim 7, wherein the capsaicin master batch meeting the particle size requirement is obtained by crushing filter residues and passing the filter residues through a 100-mesh screen.
9. The ratproof nylon masterbatch according to claim 7, wherein the capsaicin masterbatch is prepared by the following steps:
adding polypropylene and capsaicin into an organic solvent, and refluxing and heating until the polypropylene and the capsaicin are completely dissolved to obtain a mixed solution; dissolving camphor accounting for 1-2% of capsaicin content in acetone, adding the mixed solution into acetone dissolved with camphor, cooling and precipitating, filtering after precipitation, cleaning filter residue, and drying the filter residue at 70-80 ℃ for 30-60min to obtain capsaicin masterbatch.
10. The method for preparing the ratproof nylon masterbatch according to any one of claims 1 to 9, comprising the following steps:
mixing the capsaicin master batch, the toughening agent, other auxiliaries and nylon 6 to obtain a mixture; and extruding and granulating the mixture by an extruder to obtain the ratproof nylon master batch.
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| CN102153859A (en) * | 2011-02-23 | 2011-08-17 | 湖北科普达实业有限公司 | Environmental friendly termite-resistant and rodent-resistant nylon sheath material for special cables |
| CN105062036A (en) * | 2015-07-31 | 2015-11-18 | 大禹节水（天津）有限公司 | Rodent-resistant drip irrigation tube master batch |
| CN110467810A (en) * | 2019-08-13 | 2019-11-19 | 江门市凯生工程塑料有限公司 | A kind of preparation method of the rat-and-ant proof PA environmentally-friendly plastic of high impact |
| CN112164509A (en) * | 2020-09-25 | 2021-01-01 | 安徽德尔电气集团有限公司 | Fireproof and rat and ant bite prevention cable and preparation method thereof |
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