CN100412108C - Material for making toothbrush bristle and its preparation method - Google Patents
Material for making toothbrush bristle and its preparation method Download PDFInfo
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- CN100412108C CN100412108C CNB2005100281881A CN200510028188A CN100412108C CN 100412108 C CN100412108 C CN 100412108C CN B2005100281881 A CNB2005100281881 A CN B2005100281881A CN 200510028188 A CN200510028188 A CN 200510028188A CN 100412108 C CN100412108 C CN 100412108C
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- nylon
- monomer
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- tooth brush
- carbon chain
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000004677 Nylon Substances 0.000 claims abstract description 62
- 229920001778 nylon Polymers 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims description 21
- 239000000178 monomer Substances 0.000 claims description 20
- -1 amido silicon Chemical compound 0.000 claims description 10
- 125000001165 hydrophobic group Chemical group 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007334 copolymerization reaction Methods 0.000 claims description 8
- 239000003921 oil Substances 0.000 claims description 7
- 238000005453 pelletization Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001408 amides Chemical class 0.000 claims description 6
- 230000006837 decompression Effects 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229960001866 silicon dioxide Drugs 0.000 claims description 3
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims description 2
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000299 Nylon 12 Polymers 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 229920000572 Nylon 6/12 Polymers 0.000 abstract description 6
- 125000003368 amide group Chemical group 0.000 abstract description 5
- 229920002292 Nylon 6 Polymers 0.000 abstract description 3
- 229920002302 Nylon 6,6 Polymers 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract 2
- 239000002667 nucleating agent Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 description 7
- 238000001125 extrusion Methods 0.000 description 5
- 238000007380 fibre production Methods 0.000 description 5
- 210000003128 head Anatomy 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004687 Nylon copolymer Substances 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Abstract
The present invention discloses a kind of material for making toothbrush fibre and its preparation method. It is characterized by that said invention uses general nylon (nylon-6 and nylon-66) as raw material, when it is polymerized, the long carbon chain nylon resin can be added and undergone the process of amido exchange reaction, then the nucleating agent is added so as to raise nylon crystallinity and reduce its water absorption. The function of said invented product is similar to that of nylon 612 brush fibre.
Description
Technical field
The present invention relates to a kind of tooth brush monofilament material, be specifically related to a kind of nylon copolymer and synthetic method thereof that is used for toothbrush.
Background technology
Toothbrush is an apparatus inseparable in our daily life, and good head toothbrushes not only can cleaning teeth, and does not damage the oral cavity, increases the enjoyment of brushing teeth.
Along with growth in the living standard, people are more and more higher to the requirement of head toothbrushes, require head toothbrushes wear-resisting, and rebound resilience is good, and is neither too hard, nor too soft, and mouthfeel is good.This just requires more and more higher to the brush wire material of head toothbrushes.Brush wire material on the head toothbrushes mainly contains polypropylene, polyester and nylon.Wherein polypropylene is because wear resistance and rebound resilience difference can only be used as low-grade tooth brush monofilament, and polyester is because molding shrinkage is big, cause its spinning that the big and not high shortcoming of linearity of size deviation is arranged, particularly under the little situation in silk footpath, its shortcoming is just obvious all the more, is difficult to satisfy tooth brush monofilament to ultra-fine attrition resistant developing direction.Though common nylon such as nylon are 6 wear-resisting, elastic recovery is better, it is easy to suction, because water has plastification to nylon, so nylon 6 brush silks easily produce a tension set under wet environment, can not use for a long time.Nylon 612 is not only wear-resisting, the elastic recovery excellence, and also water-intake rate is low, and dimensional stability is good, and particularly its modulus is moderate, and its brush silk promptly has good mouthfeel, and the impurity in enough rigidity rejecting teeth spaces is arranged again.Therefore be commonly used for high-grade tooth brush monofilament material.But its price is expensive, has limited use range, can only be used for high-grade toothbrush and occasion that some are special, as scrubbing under the bad working environments etc.
At the shortcoming of above-mentioned brush wire material, there are a lot of researchs to wish to obtain even more ideal brush wire material by the above-mentioned shortcoming of the method improvement of material modification.These researchs mainly concentrate on the modified nylon aspect.The one, by the method for copolymerization, when nylon polymerization, add fluorochemical monomer or organosilane monomer, introduce the hydrophobic group, reduce the water-intake rate of common nylon; The 2nd, by special process, nylon is become the monofilament of skin-core structure with polyester, the comprehensive advantage of the two, the brush wire material that available can be good.With regard to first method, when polymerization, add the monomer contain the hydrophobic group, be two aspects to the influence of the water-intake rate of nylon.On the one hand, introduce the water-intake rate that the hydrophobic group helps reducing nylon, comonomer and nylon copolymerization will destroy the regularity of nylon on the other hand, reduce the crystalline probability of amide group, and not have the water-retaining capacity of crystalline amide group stronger.Therefore, limited with the water absorbing properties effect of this kind method improvement nylon.In addition, add comonomer, can reduce the modulus of nylon significantly.For second method, complex process is also very high to the requirement of equipment.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of material that is used for tooth brush monofilament and preparation method thereof, to overcome the defective that prior art exists, satisfy people's needs.
Technical conceive of the present invention is such:
The present invention utilizes amide exchange reaction by add the long carbon chain nylon resin when common nylon (nylon 6, nylon 66) polymerization, introduces the low-down long carbon chain nylon segment of water-intake rate in common nylon; And singlely can carry out end-blocking to polymeric amide with the group (as amino, carboxyl, hydroxyl etc.) and the monomer of hydrophobic group of polymeric amide copolymerization with containing; Add nucleator to improve nylon degree of crystallinity.By above-mentioned measure, reach the purpose that reduces the nylon water-intake rate.
Method of the present invention comprises the steps:
With nylon monomer, long carbon chain nylon resin, contain and singlely can carry out polymerization with the group of polymeric amide copolymerization and the monomer and the nucleator of hydrophobic group, 200～280 ℃ of polymerization temperatures, earlier 0.2MPa-10MPa pressure polymerisation 0.3～18 hour, then pressure is reduced to-0.1～0MPa, the polycondensation time is 0.3～24 hour, discharging pelletizing then promptly obtains the material that is used for tooth brush monofilament of the present invention;
Described nylon monomer is selected from nylon monomer select oneself lactan or nylon 66;
Described long carbon chain nylon resin is selected from a kind of in nylon 9, Ni Long11, nylon 12, nylon 1212 or the nylon 1010;
The weight ratio of described long carbon chain nylon resin and nylon monomer is 2～35: 100;
Described containing singlely can be selected from amido silicon oil with the group of polymeric amide copolymerization and the monomer of hydrophobic group, as Dow Corning Corporation 8460,8822,8209, the TSF4703 of General Electric Corporation, Luo Na-Rhone-Poulenc 21637,21642; A kind of among the Nikka Silicone AM of solar corona company, WR1300, the WT1650 of Brunswick company, in the weight of nylon monomer, add-on is 0.1-5wt.%.
Said nucleator is selected from silicon-dioxide, molybdenumdisulphide, titanium dioxide, talcum powder or iron sulphide, and in the weight of nylon monomer, add-on is 0.1～9wt. ‰;
Every performance of the nylon that obtains and nylon 612 are approaching, be a kind of ideal brush wire material, and cost are cheap more than nylon 612.Because material modified mainly is the long carbon chain nylon resin, and, in common nylon, introduce the long carbon chain nylon segment of a plurality of repeating units,, kept the regularity of nylon structure better than the random copolymerization between monomer by the amide group exchange; And the end-blocking of hydrophobic group and the effect that nucleator improves degree of crystallinity are arranged; Therefore can improve the water-absorbent of common nylon effectively.Make the 48h saturated water absorption of common nylon drop to 2% or lower by 7%.Also improve the molding shrinkage of common nylon in addition, kept good wear resistance of nylon and elastic recovery.Its modulus and nylon 612 are suitable, have guaranteed its brush silk under the identical situation in silk footpath, and mouthfeel is identical with nylon 612 brush silk with function.Its brush silk performance is as follows:
| Test event | Silk footpath mm | Deviation mm | Tensile strength/MPa | Rebound degree |
| Numerical value | 0.1 | ±0.005 | 700 | ≥100％ |
Embodiment
The test of product property is to adopt the method for GB standard code to carry out.
Embodiment 1
TSF4703 amido silicon oil and 0.9 kilogram of nucleator silicon-dioxide of 90 kilograms of hexanolactams, 10 kilograms of raw material nylon 9 resins, 1 kilogram of General Electric Corporation are carried out polymerization, polymerization 5 hours under 200 ℃, 0.2MPa earlier, decompression is-0.1MPa then, continue polyase 13 hour, promptly obtain the material that is used for tooth brush monofilament of the present invention, with material extrusion pelletizing, can send fiber production factory to carry out the manufacturing of tooth brush monofilament material.
The product property that obtains is as follows:
| Test event | Molding shrinkage/% | Tensile strength/MPa | Tension set/% | Modulus in tension/% | Flexural strength/MPa | Rebound degree silk footpath 0.1mm | 48h/% in water-intake rate/water |
| Numerical value | 1.1 | 62 | 300 | 2000 | 56 | ≥100％ | 2 |
Embodiment 2
8460 amido silicon oils and 0.1 kilogram of nucleator talcum powder of 93 kilograms of nylon salts, 7 kilograms of Ni Long11 resins, 0.5 kilogram of Dow Corning Corporation are carried out polymerization, polymerization 12 hours under 230 ℃, 5MPa earlier, decompression is-0.1MPa then, continue polymerization 9 hours, promptly obtain the material that is used for tooth brush monofilament of the present invention, with material extrusion pelletizing, can send fiber production factory to carry out the manufacturing of tooth brush monofilament material.The performance of material sees the following form.
| Test event | Molding shrinkage/% | Tensile strength/MPa | Tension set/% | Modulus in tension/% | Flexural strength/MPa | Rebound degree silk footpath 0.1mm | 48h/% in water-intake rate/water |
| Numerical value | 1.0 | 60 | 300 | 1950 | 54 | ≥100％ | 2 |
Embodiment 3
8460 amido silicon oils and 0.05 kilogram of nucleator titanium dioxide of 65 kilograms of hexanolactams, 35 kilograms of nylon 1212 resins, 1 kilogram of Dow Corning Corporation are carried out polymerization, polymerization 24 hours under 260 ℃, 10MPa earlier, decompression is-0.1MPa then, continue polymerization 12 hours, promptly obtain the material that is used for tooth brush monofilament of the present invention, with material extrusion pelletizing, can send fiber production factory to carry out the manufacturing of tooth brush monofilament material.The performance of material sees the following form.
| Test event | Molding shrinkage/% | Tensile strength/MPa | Tension set/% | Modulus in tension/% | Flexural strength/MPa | Rebound degree silk footpath 0.1mm | 48h/% in water-intake rate/water |
| Numerical value | 1.0 | 62 | 300 | 2000 | 56 | ≥100％ | 2 |
Embodiment 4
8460 amido silicon oils and 0.1 kilogram of nucleator titanium dioxide of 75 kilograms of nylon salts, 25 kilograms of nylon 1010 resins, 1 kilogram of Dow Corning Corporation are carried out polymerization, polymerization 18 hours under 240 ℃, 7MPa earlier, decompression is-0.1MPa then, continue polymerase 17 hour, promptly obtain the material that is used for tooth brush monofilament of the present invention, with material extrusion pelletizing, can send fiber production factory to carry out the manufacturing of tooth brush monofilament material.The performance of material sees the following form.
| Test event | Molding shrinkage/% | Tensile strength/MPa | Tension set/% | Modulus in tension/% | Flexural strength/MPa | Rebound degree silk footpath 0.1mm | 48h/% in water-intake rate/water |
| Numerical value | 1.0 | 59 | 300 | 1750 | 52 | ≥100％ | 2 |
Embodiment 5
8209 amido silicon oils and 0.08 kilogram of nucleator molybdenumdisulphide of 85 kilograms of nylon salts, 15 kilograms of Ni Long11 resins, 0.5 kilogram of Dow Corning Corporation are carried out polymerization, polymerization 18 hours under 240 ℃, 5MPa earlier, decompression is-0.1MPa then, continue polymerase 17 hour, promptly obtain the material that is used for tooth brush monofilament of the present invention, with material extrusion pelletizing, can send fiber production factory to carry out the manufacturing of tooth brush monofilament material.The performance of material sees the following form.
| Test event | Molding shrinkage/% | Tensile strength/MPa | Tension set/% | Modulus in tension/% | Flexural strength/MPa | Rebound degree silk footpath 0.1mm | 48h/% in water-intake rate/water |
| Numerical value | 1.0 | 57 | 300 | 1700 | 50 | ≥100％ | 2 |
Claims (5)
1. preparation methods that is used for tooth brush monofilament, it is characterized in that, comprise the steps: nylon monomer, long carbon chain nylon resin, contain and singlely can carry out polymerization with the group of polymeric amide copolymerization and the monomer and the nucleator of hydrophobic group, 200～280 ℃ of polymerization temperatures, polymerization pressure is 0.2MPa～10MPa, and decompression is-0.1～0MPa then, and polymerization time is 0.3～24 hour, last discharging pelletizing, i.e. acquisition is used for the material of tooth brush monofilament;
Described nylon monomer select oneself lactan or nylon salt;
Said long carbon chain nylon resin is selected from nylon 9, Ni Long11, nylon 12, nylon 1212 or nylon 1010.
2. method according to claim 1 is characterized in that, the weight ratio of described nylon monomer and long carbon chain nylon resin is 2～35: 100.
3. method according to claim 1 is characterized in that, described containing singlely can be selected from amido silicon oil with the group of polymeric amide copolymerization and the monomer of hydrophobic group, and in the weight of nylon monomer, add-on is 0.1-5wt.%.
4. method according to claim 1 is characterized in that said nucleator is selected from silicon-dioxide, molybdenumdisulphide, titanium dioxide, talcum powder or iron sulphide, and in the weight of nylon monomer, add-on is 0.1-9wt. ‰.
5. according to the material that is used for tooth brush monofilament of each method of claim 1～4 preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100281881A CN100412108C (en) | 2005-07-27 | 2005-07-27 | Material for making toothbrush bristle and its preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100281881A CN100412108C (en) | 2005-07-27 | 2005-07-27 | Material for making toothbrush bristle and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1903912A CN1903912A (en) | 2007-01-31 |
| CN100412108C true CN100412108C (en) | 2008-08-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100281881A Active CN100412108C (en) | 2005-07-27 | 2005-07-27 | Material for making toothbrush bristle and its preparation method |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037714A (en) * | 2014-12-02 | 2015-11-11 | 淮安市欣佳尼龙有限公司 | Preparation method of anti-static nylon 610 and toothbrush hair produced therefrom |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001139804A (en) * | 1999-11-12 | 2001-05-22 | Toray Ind Inc | Copolyamide, fiber and molded article |
| KR20020048240A (en) * | 2000-12-18 | 2002-06-22 | 조 정 래 | Adhesive copolyamide resin |
| CN1546570A (en) * | 2003-12-04 | 2004-11-17 | 华东理工大学 | Composite material of fibrous nanometer clay and high viscosity polyamide |
-
2005
- 2005-07-27 CN CNB2005100281881A patent/CN100412108C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001139804A (en) * | 1999-11-12 | 2001-05-22 | Toray Ind Inc | Copolyamide, fiber and molded article |
| KR20020048240A (en) * | 2000-12-18 | 2002-06-22 | 조 정 래 | Adhesive copolyamide resin |
| CN1546570A (en) * | 2003-12-04 | 2004-11-17 | 华东理工大学 | Composite material of fibrous nanometer clay and high viscosity polyamide |
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| Publication number | Publication date |
|---|---|
| CN1903912A (en) | 2007-01-31 |
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