CN103467932A - PET flame-retardant film master batch, preparation method of PET flame-retardant film master batch and PET flame-retardant film product - Google Patents
PET flame-retardant film master batch, preparation method of PET flame-retardant film master batch and PET flame-retardant film product Download PDFInfo
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Abstract
The invention discloses a PET (polyethylene glycol terephthalate) flame-retardant film master batch. Raw materials of the PET flame-retardant film master batch comprise decabromodiphenylethane, antimony trioxide, bisphenyl A bis(diphenyl phosphate), a 1010 antioxidant, a 168 antioxidant, diffusion oil, zinc borate and PBT (polybutylene terephthalate). The invention also discloses a preparation method of the PET flame-retardant film master batch and a PET flame-retardant film product. The PET flame-retardant film master batch has unique and reasonable formula design and takes a halogen and antimony synergistic flame retardance effect due to addition of the antimony trioxide and the decabromodiphenylethane; as a carrier, the PBT solves the problems of compatibility and toughness; the bisphenyl A bis(diphenyl phosphate) has effects of plastification and synergistic flame retardance; the antioxidants take an effect of reducing oxidation and degradation of the carrier and a matrix in the high temperature machining process; the diffusion oil takes an effect of improving dispersibility and compatibility; the zinc borate takes effects of carrying out synergistic flame retardance, improving incarbonization and particularly suppressing smoke and preventing drip melting; the PET flame-retardant film product prepared by adopting the PET flame-retardant film master batch has good toughness, high tensile strength and a good flame-retardant effect (which can reach the V0 grade), is low in cost, adopts a simple preparation process, is easy to implement and is beneficial to wide popularization and application.
Description
Technical field
The invention belongs to the fire-retardant film technical field, be specifically related to a kind of PET fire-retardant film master batch and preparation method thereof, PET fire-retardant film goods.
Background technology
The PET fire-retardant film at home so that the world be all a new technology and technical barrier.Truly flame-retardant V 0-stage and every mechanical property are all good in the world, only have Mitsubishi.Its technology is in the area of security monopoly position, and its product price is high.Domesticly also phosphoric acid ester is introduced in the PET molecular skeleton by the transesterify mode in research, but that actually operating is got up is very inconvenient, of a high price, and is difficult to accomplish the V0 level of real meaning, so present stage is difficult to expansion.
People attempt with the convenient and practical additive flame retardant of tradition, but exist consistency, dispersiveness, interface property and persistence poor and to operative employee's toxicity problem, and particularly poor toughness is without Practical significance.In order to address these problems, people adopt fire-retardant master granule, have the people to make carrier with PE, PP, EVA, but all have the problem of the poor and poor toughness of consistency.For this reason, people make carrier with PET, but the PET fire-retardant film of making, and poor toughness is without Practical significance.So people find various toughner, some toughner adds, and makes on the contrary its product become fragile, and some toughner adds, and make moderate progress, but effect is little, and high cost, do not have practical value.When adopting fire-retardant master granule, its adding proportion is difficult to hold in addition, and adding proportion is little, the auxiliary agent content such as requirement master batch fire retardant are many, not only doing master batch, to add man-hour very difficult, and, when film processed, dispersed uncompatibility is poor, film product is fire-retardant inhomogeneous, adding proportion is large, and master batch is many containing carrier, the oxidative degradation when the processing master batch of a lot of carriers, make the film of doing more crisp, poor practicability.
Summary of the invention
For above-mentioned deficiency, one of the object of the invention is, a kind of environmental protection, nontoxic, consistency and good dispersity are provided, and can produce the PET fire-retardant film master batch of the PET fire-retardant film of good toughness and good flame retardation effect.
Two of the object of the invention is, a kind of preparation method who prepares above-mentioned PET fire-retardant film master batch is provided, and this preparation method's technique is simple and easy, is easy to realize, production efficiency is high, has effectively improved production efficiency.
Three of the object of the invention is, a kind of PET fire-retardant film goods that adopt above-mentioned PET fire-retardant film master batch to make are provided, and good toughness, the tensile strength of these PET fire-retardant film goods are high, good flame retardation effect
For achieving the above object, technical scheme provided by the present invention is: a kind of PET fire-retardant film master batch, and its raw material comprises the component of following weight percent:
TDE 27~35 ﹪,
Antimonous oxide 10~15 ﹪,
Dihydroxyphenyl propane is two 0.1~0.5%,
1010 oxidation inhibitor 0.5~2%,
168 oxidation inhibitor 0.1~0.5%,
Diffusing oil 0.2~0.6%,
Zinc borate 0.5~2%,
PBT 48~58%。
A kind of preparation method of above-mentioned PET fire-retardant film master batch, it comprises the following steps:
(1) preparing material, raw material comprises the component of following weight percent:
TDE 27~35 ﹪,
Antimonous oxide 10~15 ﹪,
Dihydroxyphenyl propane is two 0.1~0.5%,
1010 oxidation inhibitor 0.5~2%,
168 oxidation inhibitor 0.1~0.5%,
Diffusing oil 0.2~0.6%,
Zinc borate 0.5~2%,
PBT 48~58%;
(2) TDE, antimonous oxide, dihydroxyphenyl propane is two, 1010 oxidation inhibitor, 168 oxidation inhibitor, diffusing oil and zinc borate are put into the mixer of heating;
(3) start the mixer of heating and stirred evenly the oven dry action, until dry, and stir;
(4) pour the PBT through drying in advance into the mixer of heating, until stir, then with forcing machine, make plastic grains, make PET fire-retardant film master batch goods.
As a modification of the present invention, described step is first done surface treatment with a little coupling agent to antimonous oxide and zinc borate in (2), to increase the intermiscibility between antimonous oxide, zinc borate and carrier and matrix.
As a modification of the present invention, the Temperature Setting of the mixer of heating of described step (3) is 90~110 degree, and stirring evenly drying time is 10~30 minutes.
As a modification of the present invention, the PBT of described step (4) is in advance through 120~150 degree, the drying and processing of 100~140 minutes.
As a modification of the present invention, the forcing machine of described step (4) is twin screw extruder.
A kind of PET fire-retardant film goods of making that adopt above-mentioned PET fire-retardant film master batch, its raw material comprises the component of following weight percent:
PET fire-retardant film master batch 27~35 ﹪,
PET 65~73﹪。
As a modification of the present invention, the raw material of described PET fire-retardant film master batch comprises the component of following weight percent:
TDE 27~35 ﹪,
Antimonous oxide 10~15 ﹪,
Dihydroxyphenyl propane is two 0.1~0.5%,
1010 oxidation inhibitor 0.5~2%,
168 oxidation inhibitor 0.1~0.5%,
Diffusing oil 0.2~0.6%,
Zinc borate 0.5~2%,
PBT 48~58%。
The high strength PBT of usining replaces PP, PE, EVA, PET as carrier, solves toughness and consistency, and keeps dominance and the characteristic of PET film.Using PBT as carrier, both solved the consistency of master batch and PET, the toughness of PET fire-retardant film again, also keep dominance and the characteristic of PET film.
Beneficial effect of the present invention is: the formulating of recipe uniqueness that the invention provides PET fire-retardant film master batch, rationally, take PBT as carrier, solve toughness and consistency, and dominance and the characteristic of maintenance PET film, add antimonous oxide and TDE to play the purpose of halogen antimony cooperative flame retardant, dihydroxyphenyl propane two (diphenyl phosphoester) has the purpose of plasticising and cooperative flame retardant, 1010 oxidation inhibitor and 168 oxidation inhibitor play and reduce carrier and the matrix purpose in oxidation and the degraded of high temperature process, diffusing oil plays and improves dispersed and consistency purpose, the zinc borate cooperative flame retardant improves into carbon and particularly presses down the anti-drip melt effect of cigarette, the PET fire-retardant film goods that adopt this PET fire-retardant film master batch to make, good toughness, tensile strength is high, good flame retardation effect (can reach the V0 level), preparation method's provided by the invention technique is simple and easy, be easy to realize, cost is low, and preparation efficiency is high, and the PET fire-retardant film master batch quality made is good, is beneficial to wide popularization and application.
Below in conjunction with embodiment, the invention will be further described.
Embodiment
Embodiment 1: a kind of PET fire-retardant film master batch that the present embodiment provides, its raw material comprises the component of following weight percent: TDE 27 ﹪, antimonous oxide 12.7 ﹪, dihydroxyphenyl propane two 0.5%, 1010 oxidation inhibitor 0.5%, 168 oxidation inhibitor 0.2%, diffusing oil 0.6%, zinc borate 0.5%, PBT58%.
A kind of preparation method of above-mentioned PET fire-retardant film master batch, it comprises the following steps.
(1) preparing material, raw material comprises the component of following weight percent: TDE 27 ﹪, antimonous oxide 12.7 ﹪, two 0.5%, 1010 oxidation inhibitor 0.5%, 168 oxidation inhibitor 0.2% of dihydroxyphenyl propane, diffusing oil 0.6%, zinc borate 0.5%, PBT58%.
(2) TDE, antimonous oxide, dihydroxyphenyl propane is two, 1010 oxidation inhibitor, 168 oxidation inhibitor, diffusing oil and zinc borate are put into the mixer of heating; Described step is first done surface treatment with a little coupling agent to antimonous oxide and zinc borate in (2), to increase the intermiscibility between antimonous oxide, zinc borate and carrier and matrix.
(3) start the mixer of heating and stirred evenly the oven dry action, until dry, and stir; The Temperature Setting of the mixer of heating of described step (3) is 90~110 degree, and stirring evenly drying time is 10~30 minutes.
(4) pour the PBT through drying in advance into the mixer of heating, until stir, then with forcing machine, make plastic grains, make PET fire-retardant film master batch goods.The PBT of described step (4) is in advance through 120~150 degree, the drying and processing of 100~140 minutes.
The forcing machine of described step (4) is preferably twin screw extruder, extrudes better effects if.
A kind of PET fire-retardant film goods of making that adopt above-mentioned PET fire-retardant film master batch, its raw material comprises the component of following weight percent: PET fire-retardant film master batch 29 ﹪, PET72 ﹪.
The raw material of described PET fire-retardant film master batch comprises the component of following weight percent: TDE 27 ﹪, antimonous oxide 12.7 ﹪, two 0.5%, 1010 oxidation inhibitor 0.5%, 168 oxidation inhibitor 0.2% of dihydroxyphenyl propane, diffusing oil 0.6%, zinc borate 0.5%, PBT58%.
Embodiment 2: a kind of PET fire-retardant film master batch that the present embodiment provides and preparation method thereof, PET fire-retardant film goods, it is substantially the same manner as Example 1, difference is component and the weight percent difference of PET fire-retardant film master batch, and the component of PET fire-retardant film goods and weight percent difference.
Wherein the component of PET fire-retardant film master batch and weight percent are: TDE 35 ﹪, antimonous oxide 10 ﹪, two 0.1%, 1010 oxidation inhibitor 2%, 168 oxidation inhibitor 0.5% of dihydroxyphenyl propane, diffusing oil 0.3%, zinc borate 1.1%, PBT51%.
A kind of PET fire-retardant film goods of making that adopt above-mentioned PET fire-retardant film master batch, its raw material comprises that the component of following weight percent is: PET fire-retardant film master batch 27 ﹪, PET73 ﹪.
Embodiment 3: a kind of PET fire-retardant film master batch that the present embodiment provides and preparation method thereof, PET fire-retardant film goods, it is substantially the same manner as Example 1, difference is component and the weight percent difference of PET fire-retardant film master batch, and the component of PET fire-retardant film goods and weight percent difference.
Wherein the component of PET fire-retardant film master batch and weight percent are: TDE 33.7 ﹪, antimonous oxide 15 ﹪, two 0.2%, 1010 oxidation inhibitor 0.8%, 168 oxidation inhibitor 0.1% of dihydroxyphenyl propane, diffusing oil 0.2%, zinc borate 2%, PBT48%.
A kind of PET fire-retardant film goods of making that adopt above-mentioned PET fire-retardant film master batch, its raw material comprises that the component of following weight percent is: PET fire-retardant film master batch 35 ﹪, PET65 ﹪.
Embodiment 4: a kind of PET fire-retardant film master batch that the present embodiment provides and preparation method thereof, PET fire-retardant film goods, it is substantially the same manner as Example 1, difference is component and the weight percent difference of PET fire-retardant film master batch, and the component of PET fire-retardant film goods and weight percent difference.
Wherein the component of PET fire-retardant film master batch and weight percent are: TDE 31 ﹪, antimonous oxide 13 ﹪, two 1%, 1010 oxidation inhibitor 0.3%, 168 oxidation inhibitor 0.3% of dihydroxyphenyl propane, diffusing oil 0.4%, zinc borate 1%, PBT53%.
A kind of PET fire-retardant film goods of making that adopt above-mentioned PET fire-retardant film master batch, its raw material comprises that the component of following weight percent is: PET fire-retardant film master batch 32 ﹪, PET68 ﹪.
Above-described embodiment is only the present invention's embodiment preferably, and the present invention can not enumerate out whole embodiments, and the technical scheme of one of all employing above-described embodiments, or the equivalent variations of doing according to above-described embodiment, all in protection domain of the present invention.
The formulating of recipe that the invention provides PET fire-retardant film master batch is unique, reasonable, add antimonous oxide and TDE to play the purpose of halogen antimony cooperative flame retardant, PBT solves consistency and toughness as carrier, the two purposes that plasticising and cooperative flame retardant are arranged of dihydroxyphenyl propane, 1010 oxidation inhibitor and 168 oxidation inhibitor play and reduce carrier and the matrix purpose in oxidation and the degraded of high temperature process, diffusing oil plays and improves dispersed and consistency purpose, and the zinc borate cooperative flame retardant improves into carbon and particularly presses down the anti-drip melt effect of cigarette.
The PET fire-retardant film goods that adopt this PET fire-retardant film master batch to make, good toughness, tensile strength are high, good flame retardation effect (can reach the V0 level).The high strength PBT of usining replaces PP, PE, EVA, PET as carrier, solves toughness and consistency, and keeps dominance and the characteristic of PET film.Using PBT as carrier, both solved the consistency of master batch and PET, the toughness of PET fire-retardant film again, also keep dominance and the characteristic of PET film.
Preparation method's provided by the invention technique is simple and easy, be easy to realize, cost is low, and preparation efficiency is high, and the PET fire-retardant film master batch quality made is good.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also be changed and be revised above-mentioned embodiment.Therefore, the present invention is not limited to embodiment disclosed and described above, to modifications and changes more of the present invention, also should fall in the protection domain of claim of the present invention.In addition, although used some specific terms in this specification sheets, these terms just for convenience of description, do not form any restriction to the present invention.As described in the above embodiment the present invention, adopt method same or similar with it and component and other master batch of obtaining and preparation method thereof, goods, all in protection domain of the present invention.
Claims (8)
1. a PET fire-retardant film master batch, is characterized in that, its raw material comprises the component of following weight percent:
TDE 27~35 ﹪,
Antimonous oxide 10~15 ﹪,
Dihydroxyphenyl propane is two 0.1~0.5%,
1010 oxidation inhibitor 0.5~2%,
168 oxidation inhibitor 0.1~0.5%,
Diffusing oil 0.2~0.6%,
Zinc borate 0.5~2%,
PBT 48~58%。
2. a preparation method who prepares the described PET fire-retardant film of claim 1 master batch, is characterized in that, it comprises the following steps:
(1) preparing material, raw material comprises the component of following weight percent:
TDE 27~35 ﹪,
Antimonous oxide 10~15 ﹪,
Dihydroxyphenyl propane is two 0.1~0.5%,
1010 oxidation inhibitor 0.5~2%,
168 oxidation inhibitor 0.1~0.5%,
Diffusing oil 0.2~0.6%,
Zinc borate 0.5~2%,
PBT 48~58%;
(2) TDE, antimonous oxide, dihydroxyphenyl propane is two, 1010 oxidation inhibitor, 168 oxidation inhibitor, diffusing oil and zinc borate are put into the mixer of heating;
(3) start the mixer of heating and stirred evenly the oven dry action, until dry, and stir;
(4) pour the PBT through drying in advance into the mixer of heating, until stir, then with forcing machine, make plastic grains, make PET fire-retardant film master batch goods.
3. preparation method according to claim 2, is characterized in that, described step is first done surface treatment with a little coupling agent to antimonous oxide and zinc borate in (2), to increase the intermiscibility between antimonous oxide, zinc borate and carrier and matrix.
4. preparation method according to claim 2, is characterized in that, the Temperature Setting of the mixer of heating of described step (3) is 90~110 degree, and stirring evenly drying time is 10~30 minutes.
5. preparation method according to claim 2, is characterized in that, the PBT of described step (4) is in advance through 120~150 degree, the drying and processing of 100~140 minutes.
6. preparation method according to claim 2, is characterized in that, the forcing machine of described step (4) is twin screw extruder.
7. PET fire-retardant film goods of making that adopt the described PET fire-retardant film of claim 1 master batch, is characterized in that, its raw material comprises the component of following weight percent:
PET fire-retardant film master batch 27~35 ﹪,
PET 65~73﹪。
8. PET fire-retardant film goods according to claim 7, is characterized in that, the raw material of described PET fire-retardant film master batch comprises the component of following weight percent:
TDE 27~35 ﹪,
Antimonous oxide 10~15 ﹪,
Dihydroxyphenyl propane is two 0.1~0.5%,
1010 oxidation inhibitor 0.5~2%,
168 oxidation inhibitor 0.1~0.5%,
Diffusing oil 0.2~0.6%,
Zinc borate 0.5~2%,
PBT 48~58%。
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CN106280322A (en) * | 2016-09-26 | 2017-01-04 | 高团结 | PET fire-retardant film master batch and preparation method thereof, PET fire-retardant film goods |
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