CN105086388A - Preparation method of PET (polyethylene glycol terephthalate)-molecular sieve composite cooling masterbatch - Google Patents
Preparation method of PET (polyethylene glycol terephthalate)-molecular sieve composite cooling masterbatch Download PDFInfo
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Abstract
The invention relates to a preparation method of a high-polymer material, in particular to a preparation method of PET (polyethylene glycol terephthalate)-molecular sieve composite cooling masterbatch. The method comprises processes as follows: matrix resin slices and molecular sieves are dried; a molecular weight regulator is added to treated molecular sieves, a coupling agent and a dispersing agent for ultrasonic oscillation, and the mixture is stirred under the normal pressure in a closed manner, so that the molecular weight regulator grows in the molecular sieves until adsorption equilibrium; PET resin slices, a stabilizer and a lubricant are evenly mixed by a high-speed mixer; melting extrusion granulation is performed on the mixed material in a twin-screw extruder. With the adoption of the method, the contact area of the molecular weight regulator with polymers is increased in the micro perspective, volatilization is reduced, the utilization rate is increased, and the molecular chain degradation is fast and uniform, so that the relative molecular mass of PET is reduced, distribution is narrowed, and the fluidity is improved.
Description
Technical field
The present invention relates to a kind of Polymer materialspreparation method, particularly relate to a kind of preparation method of PET-molecular sieve composite cooling master batch.
Background technology
Cooling masterbatch is raw material with matrix resin, adds the auxiliary agents such as molecular weight regulator, stablizer, dispersion agent, lubricant, under specific processing conditions, drying, batch mixing, extrude, the step such as cooling granulation processes.Its effect mainly attacks by active group size and the molecular weight distribution that weak bond chain rupture carrys out regulate polymer molecular weight, improve the mobility of polymkeric substance, improve melt index, material also can be realized at a lower temperature well shaping, thus reduce processing temperature, avoid polymkeric substance to degrade under continuous high temperature, decrease the thermal stresses that the temperature difference is brought greatly, save energy consumption.And the sticky section of the height of low melt index equally can be spun.
Cooling masterbatch is applied to polypropylene spinning the earliest, and because polypropylene relative molecular mass is large, molecular weight distribution is wide, and melt temperature is higher, and spinning processing temperature is higher, and fibre property is not very stable, and especially additive easily decomposes.There is similar problem in polyester PET spinning, and because melt temperature (264 DEG C) Sum decomposition temperature (300 DEG C) difference of PET is less, make its processing temperature scope narrower, be unfavorable for process control, so temperature control cincture moves to low temperature more favourable in guarantee fibre property situation.Current interpolation cooling masterbatch has become the important means that improvement spinning technique prevents auxiliary agent from decomposing.
But the preparation process of cooling masterbatch also has a lot of defect, selects superoxide as molecular weight regulator, initiator activity group content is high, and speed of response is fast, and skewness can have influence on molecular chain conformation in the polymer.And its character is active, is liquid under normal pressure, controls the improper content that all can affect superoxide in cooling masterbatch with temperature of charge, mixing time, mixing velocity etc. during mixing of materials, cause its utilization ratio low, cause waste.On the other hand, after adding cooling masterbatch, PET thermostability declines, and add that dyeability own is poor, water absorbability and mechanical property also have much room for improvement, and also will add other auxiliary agents and improve.This is also the emphasis of field of polyester fiber research always.
Molecular sieve is that a class has uniform pore size, huge internal surface area and pore volume, has again the crystalline microporous material of the characteristics such as ion exchangeable simultaneously.Particle diameter is micron order size, and aperture is nano-grade size.Because it has absorption assembling characteristic, specific group of molecules can be contained in its micropore, be released again on other occasions.And molecular sieve is inorganic materials, there are the advantages such as fire-retardant, wear-resisting, Heat stability is good.Existing bibliographical information, adds the molecular sieve of suitable proportion, can make the dyeability of PET, water absorbability and mechanical property be improved significantly.But its agglomeration is comparatively serious, disperse even not in the polymer, be not fine with organic bonding force, the use of molecular sieve is still restricted.
Based on some deficiency above, through experimental study by two kinds of methods combining together, prepare a kind of PET-molecular sieve composite cooling agglomerate material, molecular sieve pore passage is utilized to carry active group, have an effect with polymkeric substance again, it is better that the existence of coupling agent simultaneously can make inorganics and organism combine, thus make up respective deficiency.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of PET-molecular sieve composite cooling master batch, the method increases the contact area of molecular weight regulator and polymkeric substance from microcosmic angle, reduce volatilization, improve its utilization ratio, molecular chain degradation speed soon and evenly, PET relative molecular mass is reduced, distribution narrow, mobility improves.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for PET-molecular sieve composite cooling master batch, described method comprises following process:
Matrix resin section is carried out drying with molecular sieve; Molecular sieve, coupling agent, dispersion agent are put into molecular weight regulator ultrasonic vibration after treatment, and normal-pressure sealed stirs, and molecular weight regulator is grown until adsorption equilibrium in molecular sieve; High-speed mixer is utilized to mix PET resin section, stablizer, lubricant; It is (being portion rate below) by mixture, adding proportion: PET resin 70-90 part; Molecular weight regulator 0.5-5 part; Molecular sieve 1-10 part; Coupling agent 0.2-2 part; Dispersion agent 1-10 part; Stablizer 0.5-2 part; Lubricant 0.5-2 part; Carry out melt extruding pelletizing in twin screw.
The preparation method of described a kind of PET-molecular sieve composite cooling master batch, described PET resin is poly terephthalic acid hexylene glycol ester, and resin properties viscosity is 0.675 ± 0.03dl/g; Molecular weight regulator is molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=(1-2) ︰ (1-2); Coupling agent is titanic acid ester; Dispersion agent is Magnesium Stearate; Stablizer is trimethyl phosphite 99; Lubricant is hexenyl bis-stearamides.
The preparation method of described a kind of PET-molecular sieve composite cooling master batch, described molecular sieve comprises the zeolite molecular sieve and mesoporous molecular sieve, 13X type molecular sieve that micropore size is 0.3-5.0nm, Y zeolite, mordenite molecular sieve, type molecular sieve, MCM-41 molecular sieve, more satisfactory pore diameter range is the molecular sieve of 0.6-3 nanometer, the granularity of molecular sieve is at 0.05-40 μm, and desirable granularity is 0.05-5 μm.
The preparation method of described a kind of PET-molecular sieve composite cooling master batch, described dry PET matrix resin section is at 120 DEG C of vacuum-drying 3-6 hour; Molecular sieve is at 120 DEG C of dry 2-5 hour.
The preparation method of described a kind of PET-molecular sieve composite cooling master batch, described dry molecular sieves, coupling agent, dispersion agent, put into molecular weight regulator after treatment, sonic oscillation 1-3 hour, makes molecular weight regulator in molecular sieve, grow 20-36 hour until adsorption equilibrium under normal pressure 40 DEG C-60 DEG C closed agitation conditions.
The preparation method of described a kind of PET-molecular sieve composite cooling master batch, the PET resin of described drying; Stablizer; Lubricant, utilizes high-speed mixer to be mixed.
The preparation method of described a kind of PET-molecular sieve composite cooling master batch, described granulation: start twin screw extruder, material adds to charging opening, material takes stage casing to feed in raw material, screw speed is slowly adjusted to 80-500r/min, feeding rotating speed 15-300r/min, fusion time 1-5 minute, extruder temperature is set as: district's temperature 250 DEG C, two district's temperature 255 DEG C, three district's temperature 260 DEG C, four district's temperature 265 DEG C, five district's temperature 265 DEG C, six district's temperature 255 DEG C, carry out melt extruding pelletizing with twin screw at temperature 240-270 DEG C.
Advantage of the present invention and effect are:
1. molecular sieve add the contact area increasing molecular weight regulator and polymkeric substance from microcosmic angle, reduce volatilization, improve its utilization ratio, molecular chain degradation speed is fast and evenly, PET relative molecular mass is reduced, distribution narrow, mobility raising.
2, for the processing of PET base inorganic nano-composite material, this method can prevent molecular sieve from reuniting in the polymer, can improve its flowing property again, improves organic and inorganic in conjunction with effect, improves its fiber spinnability.
3, add the shortcoming that molecular sieve obviously can improve the breaking tenacity decline that cooling masterbatch brings, compensate for the deficiency that cooling masterbatch performance is single in the past.
4, the synergy both performance, improves while achieving fluidity of molten and fiber over-all properties, achieves master batch multifunction, shorten manufacturing procedure, reduces raw material consumption, improves production efficiency.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
1, matrix resin section is carried out drying with molecular sieve; Molecular sieve, coupling agent, dispersion agent are put into molecular weight regulator ultrasonic vibration after treatment, and normal-pressure sealed stirs, and molecular weight regulator is grown until adsorption equilibrium in molecular sieve; High-speed mixer is utilized to mix PET resin section, stablizer, lubricant; Mixture is carried out in twin screw melt extrude pelletizing.
In technical scheme, each material adding proportion is (being portion rate below):
PET resin 70-90 part;
Molecular weight regulator 0.5-5 part;
Molecular sieve 1-10 part;
Coupling agent 0.2-2 part;
Dispersion agent 1-10 part;
Stablizer 0.5-2 part;
Lubricant 0.5-2 part;
2, preferred, described PET resin is poly terephthalic acid hexylene glycol ester, and resin properties viscosity is 0.675 ± 0.03dl/g; Molecular weight regulator is molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=(1-2) ︰ (1-2); Coupling agent is titanic acid ester; Dispersion agent is Magnesium Stearate; Stablizer is trimethyl phosphite 99; Lubricant is hexenyl bis-stearamides;
3, preferred, molecular sieve is characterized in that described molecular sieve comprises the zeolite molecular sieve and mesoporous molecular sieve, 13X type molecular sieve that micropore size is 0.3-5.0nm, Y zeolite, mordenite molecular sieve, type molecular sieve, MCM-41 molecular sieve, more satisfactory pore diameter range is the molecular sieve of 0.6-3 nanometer, the granularity of molecular sieve is at 0.05-40 μm, and desirable granularity is 0.05-5 μm.
4, as preferred, drying described in technique scheme 1 is: the section of PET matrix resin is at 120 DEG C of vacuum-drying 3-6 hour; Molecular sieve is at 120 DEG C of dry 2-5 hour.
5, as preferred, be grown to described in technique scheme 1: the dry molecular sieves in claim 2, coupling agent, dispersion agent, put into molecular weight regulator after treatment, sonic oscillation 1-3 hour, makes molecular weight regulator in molecular sieve, grow 20-36 hour until adsorption equilibrium under normal pressure 40 DEG C-60 DEG C closed agitation conditions.
6, as preferably, mix described in technique scheme 1: PET resin dry in claim 2; Stablizer; Lubricant, utilizes high-speed mixer to be mixed.
7, as preferred, granulation described in technique scheme 1: start twin screw extruder, in technical scheme 5, material adds to charging opening, in technical scheme 6, material takes stage casing to feed in raw material, screw speed is slowly adjusted to 80-500r/min, feeding rotating speed 15-300r/min, fusion time 1-5 minute, extruder temperature is set as: district's temperature 250 DEG C, two district's temperature 255 DEG C, three district's temperature 260 DEG C, four district's temperature 265 DEG C, five district's temperature 265 DEG C, six district's temperature 255 DEG C, carry out melt extruding pelletizing with twin screw at temperature 240-270 DEG C.
Last it is noted that above embodiment only in order to illustrate the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification sheets with reference to each above-mentioned embodiment to present invention has been detailed description, those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent to replace; And all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, it all should be encompassed in right of the present invention.
Reagent used in following examples is commercially available.
1, example 1
The composition of the PET-molecular sieve composite cooling master batch of embodiment 1 and parts by weight;
PET resin 90 parts;
Molecular weight regulator 2 parts;
1 part, 13X type molecular sieve;
Coupling agent titanic acid ester 1.5 parts;
Dispersion agent Magnesium Stearate 3.5 parts;
Stablizer trimethyl phosphite 99 1 part;
Lubricant hexenyl bis-stearamides 1 part.
Wherein molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=1 ︰ 1; Resin properties viscosity is 0.675 ± 0.03dl/g; The granularity of molecular sieve is for being 0.05-5 μm.
2, the concrete grammar preparing PET-molecular sieve composite cooling master batch is as follows:
1), dry: matrix resin PET is cut into slices 120 DEG C of vacuum-dryings more than 6 hours; By molecular sieve 120 DEG C of dryings 4 hours.
2), grow: molecular sieve, coupling agent and dispersion agent are put into after treatment molecular weight regulator sonic oscillation 1 hour, under normal pressure 50 DEG C of closed agitation conditions, make molecular weight regulator in molecular sieve, grow 24 hours until adsorption equilibrium.
3), mix: utilize high-speed mixer to mix PET resin, stablizer, lubricant.
4), start twin screw extruder, screw speed is slowly adjusted to 40r/min, feeding rotating speed 15r/min, in 2, material adds to charging opening, and in 1, material takes stage casing to feed in raw material.Fusion time controls at about 3 minutes, and extruder temperature is set as: district's temperature 250 DEG C, two district's temperature 255 DEG C, three district's temperature 260 DEG C, four district's temperature 265 DEG C, five district's temperature 265 DEG C, six district's temperature 255 DEG C, carry out melt extruding pelletizing with twin screw at temperature 240-270 DEG C.
Embodiment 2:
1, the composition of the PET-molecular sieve composite cooling master batch of embodiment 2 and parts by weight;
PET resin 85 parts;
Molecular weight regulator 4 parts;
3 parts, 13X type molecular sieve;
Coupling agent titanic acid ester 1 part;
Dispersion agent Magnesium Stearate 6 parts;
Stablizer trimethyl phosphite 99 0.5 part;
Lubricant hexenyl bis-stearamides 0.5 part.
Wherein molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=1 ︰ 1; Resin properties viscosity is 0.675 ± 0.03dl/g; The granularity of molecular sieve is for being 0.05-5 μm.
2, the concrete grammar of PET-molecular sieve composite cooling master batch is prepared with embodiment 1.
Embodiment 3
1, the composition of the PET-molecular sieve composite cooling master batch of embodiment 3 and parts by weight;
PET resin 85 parts;
Molecular weight regulator 4.5 parts;
5 parts, 13X type molecular sieve;
Coupling agent titanic acid ester 1.5 parts;
Dispersion agent Magnesium Stearate 3 parts;
Stablizer trimethyl phosphite 99 0.5 part;
Lubricant hexenyl bis-stearamides 0.5 part.
Wherein molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=1 ︰ 1; Resin properties viscosity is 0.675 ± 0.03dl/g; The granularity of molecular sieve is for being 0.05-5 μm.
2, the concrete grammar of PET-molecular sieve composite cooling master batch is prepared with embodiment 1.
Embodiment 4
1, the composition of the PET-molecular sieve composite cooling master batch of embodiment 4 and parts by weight;
PET resin 85 parts;
Molecular weight regulator 3 parts;
7 parts, 13X type molecular sieve;
Coupling agent titanic acid ester 1 part;
Dispersion agent Magnesium Stearate 3 parts;
Stablizer trimethyl phosphite 99 0.5 part;
Lubricant hexenyl bis-stearamides 0.5 part.
Wherein molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=1 ︰ 1; Resin properties viscosity is 0.675 ± 0.03dl/g; The granularity of molecular sieve is for being 0.05-5 μm.
2, the concrete grammar of PET-molecular sieve composite cooling master batch is prepared with embodiment 1.
Comparative example 1
1, the composition of the PET cooling masterbatch of comparative example 1 and parts by weight;
PET resin 90 parts;
Molecular weight regulator 3 parts;
Coupling agent titanic acid ester 1.5 parts;
Dispersion agent Magnesium Stearate 4.5 parts;
Stablizer trimethyl phosphite 99 0.5 part;
Lubricant hexenyl bis-stearamides 0.5 part.
Wherein molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=1 ︰ 1; Resin properties viscosity is 0.675 ± 0.03dl/g;
2, the preparation method of the PET cooling masterbatch of comparative example 1, comprises the following steps:
1) PET resin, molecular weight regulator, coupling agent, dispersion agent, stablizer, lubricant are added high-speed mixer according to proportioning raw materials and mix;
2) start twin screw extruder, mixture step 1) obtained carries out melt extruding pelletizing with twin screw at temperature 240-270 DEG C.Screw speed is slowly adjusted to 40r/min, feeding rotating speed 15r/min, and fusion time controls at about 3 minutes, extruder temperature is set as: district's temperature 250 DEG C, two district's temperature 255 DEG C, three district's temperature 260 DEG C, four district's temperature 265 DEG C, five district's temperature 265 DEG C, six district's temperature 255 DEG C.
By the PET cooling masterbatch of above-described embodiment and comparative example according to 1.4% weight ratio add to respectively in PET, then mix, use twin screw extruder granulation, test melting index, preparation standard batten test properties; In addition, the PET preparation standard batten of cooling masterbatch will do not added, by same test condition test properties and melting index; The performance test results obtained is as follows:
Table 1 the performance test results
Find out from the above results, molecular sieve add the contact area increasing molecular weight regulator and polymkeric substance from microcosmic angle, reduce volatilization, improve its utilization ratio, molecular chain degradation speed is fast and evenly, PET relative molecular mass is reduced, distribution narrow, mobility improves, for the processing of PET base inorganic nano-composite material, this method can prevent molecular sieve from reuniting in the polymer, can improve its flowing property again, improve organic and inorganic in conjunction with effect, improve its fiber spinnability.Add the shortcoming that molecular sieve obviously can improve the breaking tenacity decline that cooling masterbatch brings, compensate for the deficiency that cooling masterbatch performance is single in the past.The PET-molecular sieve composite cooling master batch of preparation is applied in PET, improves while achieving fluidity of molten and fiber over-all properties, achieve master batch multifunction, shorten manufacturing procedure, reduce raw material consumption, improve production efficiency.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (7)
1. a preparation method for PET-molecular sieve composite cooling master batch, is characterized in that, described method comprises following process:
Matrix resin section is carried out drying with molecular sieve; Molecular sieve, coupling agent, dispersion agent are put into molecular weight regulator ultrasonic vibration after treatment, and normal-pressure sealed stirs, and molecular weight regulator is grown until adsorption equilibrium in molecular sieve; High-speed mixer is utilized to mix PET resin section, stablizer, lubricant; It is (being portion rate below) by mixture, adding proportion: PET resin 70-90 part; Molecular weight regulator 0.5-5 part; Molecular sieve 1-10 part; Coupling agent 0.2-2 part; Dispersion agent 1-10 part; Stablizer 0.5-2 part; Lubricant 0.5-2 part; Carry out melt extruding pelletizing in twin screw.
2. the preparation method of a kind of PET-molecular sieve composite cooling master batch according to claim 1, it is characterized in that, described PET resin is poly terephthalic acid hexylene glycol ester, and resin properties viscosity is 0.675 ± 0.03dl/g; Molecular weight regulator is molecular weight regulator is tertbutyl peroxide: di-tert-butyl hydrogen peroxide=(1-2) ︰ (1-2); Coupling agent is titanic acid ester; Dispersion agent is Magnesium Stearate; Stablizer is trimethyl phosphite 99; Lubricant is hexenyl bis-stearamides.
3. the preparation method of a kind of PET-molecular sieve composite cooling master batch according to claim 1, it is characterized in that, described molecular sieve comprises the zeolite molecular sieve and mesoporous molecular sieve, 13X type molecular sieve that micropore size is 0.3-5.0nm, Y zeolite, mordenite molecular sieve, type molecular sieve, MCM-41 molecular sieve, more satisfactory pore diameter range is the molecular sieve of 0.6-3 nanometer, and the granularity of molecular sieve is at 0.05-40 μm, and desirable granularity is 0.05-5 μm.
4. the preparation method of a kind of PET-molecular sieve composite cooling master batch according to claim 1, is characterized in that, described dry PET matrix resin section is at 120 DEG C of vacuum-drying 3-6 hour; Molecular sieve is at 120 DEG C of dry 2-5 hour.
5. the preparation method of a kind of PET-molecular sieve composite cooling master batch according to claim 1, it is characterized in that, described dry molecular sieves, coupling agent, dispersion agent, put into molecular weight regulator after treatment, sonic oscillation 1-3 hour, under normal pressure 40 DEG C-60 DEG C closed agitation conditions, make molecular weight regulator in molecular sieve, grow 20-36 hour until adsorption equilibrium.
6. the preparation method of a kind of PET-molecular sieve composite cooling master batch according to claim 1, is characterized in that, the PET resin of described drying; Stablizer; Lubricant, utilizes high-speed mixer to be mixed.
7. the preparation method of a kind of PET-molecular sieve composite cooling master batch according to claim 1, it is characterized in that, described granulation: start twin screw extruder, material adds to charging opening, material takes stage casing to feed in raw material, screw speed is slowly adjusted to 80-500r/min, feeding rotating speed 15-300r/min, fusion time 1-5 minute, extruder temperature is set as: district's temperature 250 DEG C, two district's temperature 255 DEG C, three district's temperature 260 DEG C, four district's temperature 265 DEG C, five district's temperature 265 DEG C, six district's temperature 255 DEG C, carry out melt extruding pelletizing with twin screw at temperature 240-270 DEG C.
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| CN114536921A (en) * | 2022-03-11 | 2022-05-27 | 山东农业大学 | Preparation method of antioxidant food packaging film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114536921A (en) * | 2022-03-11 | 2022-05-27 | 山东农业大学 | Preparation method of antioxidant food packaging film |
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Application publication date: 20151125 |