CN111892772A - Modified polypropylene master batch, modified melt-blown fabric material and improved melt-blown fabric processing method - Google Patents
Modified polypropylene master batch, modified melt-blown fabric material and improved melt-blown fabric processing method Download PDFInfo
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- -1 polypropylene Polymers 0.000 title claims abstract description 128
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 104
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 103
- 239000004744 fabric Substances 0.000 title claims abstract description 70
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000003672 processing method Methods 0.000 title claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000004698 Polyethylene Substances 0.000 claims abstract description 11
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 11
- 239000007822 coupling agent Substances 0.000 claims abstract description 11
- 239000000314 lubricant Substances 0.000 claims abstract description 11
- 229920000573 polyethylene Polymers 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 9
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 21
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 12
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 10
- 239000002667 nucleating agent Substances 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 description 22
- 239000013078 crystal Substances 0.000 description 15
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 238000004804 winding Methods 0.000 description 8
- 238000001125 extrusion Methods 0.000 description 5
- 239000007983 Tris buffer Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000007664 blowing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 3
- 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 compound 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 3
- 210000004027 cell Anatomy 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 241001391944 Commicarpus scandens Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 238000003851 corona treatment Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229940070527 tourmaline Drugs 0.000 description 2
- 229910052613 tourmaline Inorganic materials 0.000 description 2
- 239000011032 tourmaline Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 125000000649 benzylidene group Chemical group [H]C(=[*])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 208000030159 metabolic disease Diseases 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000017074 necrotic cell death Effects 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/544—Olefin series
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Filtering Materials (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Electrostatic Separation (AREA)
Abstract
The invention discloses a modified polypropylene master batch, a modified melt-blown fabric material and an improved melt-blown fabric processing method, wherein the modified polypropylene master batch comprises polypropylene, an antioxidant, low-molecular polyethylene wax, an alkyl coupling agent, electret particles, a lubricant and modified polypropylene, and the modified polypropylene at least comprises trimesoamide derivatives obtained by modifying trimesoamide. The invention provides a safer and more effective melt-blown fabric material, which can improve the crystallinity of polypropylene by adding the modified nucleating agent, and can obviously improve the capturing and charge storage stability of space charge along with the increase of the crystallinity and the size, thereby reducing the dosage of the nano electret material, reducing the potential risk, effectively increasing the charge storage amount and prolonging the charge storage time.
Description
Technical Field
The invention relates to the field of filter materials, in particular to a modified polypropylene master batch, a modified melt-blown fabric material and an improved melt-blown fabric processing method.
Background
Melt-blown polypropylene non-woven fabric, called melt-blown fabric for short, is made up by using melt extruded from polypropylene extruder, making high-temp. air flow stretch to form superfine fibre, then using honeycomb porous winding roll to wind and condense it into fibre web, and making it be bonded and reinforced in its self-molten state.
The melt-blown fabric is the most core material of the mask, polypropylene is used as a main raw material of the melt-blown fabric, and the diameter of the fiber can reach 1-5 microns. The superfine fiber with the unique capillary structure increases the number and the surface area of the fiber per unit area, so that the melt-blown fabric has good filtering property, shielding property, heat insulation property and oil absorption property. Can be used in the fields of air and liquid filtering materials, isolating materials, absorbing materials, mask materials, warm-keeping materials, oil absorbing materials, wiping cloth and the like.
However, the filtration performance of the meltblown fabric is not very high, and the barrier effect of the meltblown filter material is obviously insufficient purely by the structure of the meltblown filter material, so that the meltblown filter material generally has the price-adjusting electrostatic charge effect on the meltblown fabric through an electret process, and the filtration efficiency is improved by using an electrostatic method.
The melt-blown fabric material subjected to electret treatment simultaneously utilizes the electret property of the fiber to carry out electrostatic adsorption on dust and capture bacteria and viruses. The prior melt-blown fabric electret material is mainly prepared by adding nano-level tourmaline, silicon dioxide particles and other electret materials into raw materials and then charging the melt-blown fabric material in a corona discharge mode of a needle electrode of an electrostatic generator before rolling up the fabric.
The problem with this approach is that:
many literature data and biological experiments show that the nano material has potential risks in the use process, for example, the nano material has biological toxicity mainly reflected in interference with the respiratory system and the immune system, and microscopically mainly affects the functional structure on the cell surface, thereby causing the metabolic disorder of the whole cell, inducing apoptosis or necrosis of the cell, and the like. The amount of the nano electret material used in the melt-blown material containing the nano electret material as the core of the mask greatly affects the safety of the material, so that better filtering performance is obviously expected to be achieved on the premise of lower amount of the electret material.
Meanwhile, the melt-blown cloth can be mechanically pulled in the mask manufacturing process, so that the requirement on the elongation at break is high, and the existing electret melt-blown cloth has poor toughness and is easy to break after an electret material is added.
Disclosure of Invention
The present invention is directed to solve the above problems in the prior art, and an object of the present invention is to provide a modified polypropylene masterbatch and a modified meltblown fabric material with improved safety by adding trimesoamide derivatives to reduce the use of electret materials.
The purpose of the invention is realized by the following technical scheme:
comprises polypropylene, antioxidant, low molecular polyethylene wax, alkyl coupling agent, electret particles, lubricant and trimesoamide derivatives.
Preferably, in the modified polypropylene master batch, the trimesoamide derivative is 1,3, 5-benzoyl tri (tert-butylamine) and/or 1,3, 5-benzoyl tri (cyclohexylamine).
Preferably, the modified polypropylene master batch comprises the following raw materials in parts by weight:
preferably, the modified polypropylene masterbatch comprises a molecular weight regulator as a raw material.
Preferably, in the modified polypropylene master batch, the weight part of the molecular weight regulator is 0.1-0.5 part.
The modified melt-blown fabric material comprises polypropylene and modified polypropylene, wherein the mass percent of the polypropylene is between 96% and 98%, and the mass percent of the modified polypropylene is between 2% and 4%.
The improved melt-blown fabric processing method comprises the following steps
S1, providing modified polypropylene master batches and polypropylene master batches;
s2, uniformly mixing the modified polypropylene master batch and the polypropylene master batch according to the proportion to obtain a melt-blown raw material;
and S3, adding the melt-blown raw material into an extruder, extruding the melt-blown raw material through a die head in a molten state, and obtaining the melt-blown fabric after hot air drafting, cooling and electret treatment.
Preferably, in the processing method of the improved meltblown fabric, in S1, the modified polypropylene masterbatch is prepared by:
s11, adding polypropylene, an antioxidant, low-molecular polyethylene wax, a molecular weight regulator, trimesoamide derivatives, an alkyl coupling agent, electret particles and a lubricant in proportion and sequence, and uniformly mixing to obtain a mixture;
and S12, mixing and plasticizing the mixture, cooling, and cutting into particles to obtain the modified polypropylene master batch.
Preferably, in the improved meltblown processing method, the trimesoamide derivatives in S11 are prepared by,
0.7mol of amine compound is dissolved in 150mL of 1-methyl-2-pyrrolidone, 0.1g of anhydrous lithium chloride and 20mL of triethylamine are added and mixed with the amine compound, 0.2mol of trimesoyl chloride is added, the mixture is stirred for 4h at 85 ℃, and nitrogen is introduced for protection during stirring. After completion of stirring, it was cooled to room temperature, and the mixture was poured into 500mL of ice water. Filtering the mixture by using a glass filter to obtain a crude product, recrystallizing and purifying the obtained crude product in DMF (dimethylformamide), washing the crude product for 3 times by using deionized water, and drying the crude product in vacuum at the temperature of 50 ℃ for 24 hours to obtain a white powder product, namely 1,3, 5-benzene tricarboxy tris (cyclohexylamine);
or 0.62mol of amine compound is dissolved in 100mL of 1-methyl-2-pyrrolidone, 0.1g of anhydrous lithium chloride and 20mL of triethylamine are added and mixed with the amine compound, 0.18mol of trimesoyl chloride is added, the mixture is stirred for 4h at 85 ℃, and nitrogen is introduced for protection during stirring. After completion of stirring, it was cooled to room temperature, and the mixture was poured into 500mL of ice water. The mixture was filtered using a glass filter to obtain a crude product, which was recrystallized in DMF (dimethylformamide) for purification, washed 3 times with deionized water, and vacuum dried at 50 ℃ for 24 hours to obtain a white powder product, i.e., 1,3, 5-benzotriazolyl tris (tert-butylamine).
Preferably, in the improved meltblown fabric manufacturing method, the cooling and drawing are performed by using cold air in S3.
Preferably, in the processing method of the improved meltblown fabric, after the cooling and before the electret treatment in S3, the meltblown fabric is heat-treated at a temperature of 110 ℃ to 130 ℃, the treatment time per square meter of the meltblown fabric is between 5 seconds to 20 seconds, and the electret treatment is performed immediately after the heating.
The technical scheme of the invention has the advantages that:
the invention provides a safer and more effective melt-blown fabric material, which can improve the crystallinity of polypropylene by adding the modified nucleating agent, and can obviously improve the capturing and charge storage stability of space charge along with the increase of the crystallinity and the size, thereby reducing the dosage of the nano electret material, reducing the potential risk, effectively increasing the charge storage amount and prolonging the charge storage time.
The scheme can effectively realize that various factors such as the filtration performance, the production cost, the processing efficiency and the like of the melt-blown fabric reach the optimal condition through the design of the proportion of materials, the technological process and the technological conditions, and has high comprehensive benefit.
The modified material of the scheme has the advantages of effectively reducing the temperature required by polypropylene melt-blowing, reducing power consumption and saving cost.
According to the scheme, one heat treatment is carried out before electret treatment, the toughness of the material can be effectively improved by controlling the heat treatment temperature and time, the integral processing beat and energy consumption are considered, and the unification of multiple effects is realized.
Detailed Description
Objects, advantages and features of the present invention will be illustrated and explained by the following non-limiting description of preferred embodiments. The embodiments are merely exemplary for applying the technical solutions of the present invention, and any technical solution formed by replacing or converting the equivalent thereof falls within the scope of the present invention claimed.
The modified melt-blown fabric material disclosed by the invention is explained below, and firstly, the inventor finds out through study and research that: the common crystal forms of the formed polypropylene comprise a quasi-hexagonal crystal form and an alpha crystal form, wherein the alpha crystal form is a spiral crystal form, so the crystal form is the most stable crystal form in the polypropylene crystal forms, and the nonwoven fabric obtained by melt-spraying the polypropylene of the alpha crystal form has higher crystallinity and initial modulus from the aspect of mechanical properties, so that the melt-sprayed fabric has better toughness.
From the aspect of charge storage performance, the thermal stimulation exothermic peak of the alpha crystal form is about 40 ℃ higher than the quasi-hexagonal peak, has stronger charge binding capacity, is not easy to trap charges, and has more excellent performance of charge dissipation after electret treatment.
Therefore, the polypropylene nonwoven fabric needs to have a larger proportion of alpha crystal form and a larger grain size, and in order to achieve the purpose, the innovation of the scheme is that the melt-blown material at least comprises modified polypropylene, the modified polypropylene at least comprises trimesoamide derivatives obtained by modifying trimesamide, and the modified polypropylene is used as a nucleating agent, so that the problems that common commercial nucleating agents such as aliphatic carboxylic acid metal compounds, sorbierite benzylidene derivatives, organic phosphates and the like are narrow in application field and limited by processing technology due to poor dispersibility, low thermal stability and the like can be effectively solved.
According to the scheme, the trimesoamide derivatives obtained by modifying the trimesoamide are added into the material, so that the crystallinity of the polypropylene can be improved, the space charge capture and charge storage stability can be obviously improved along with the increase of the crystallinity and the size, the using amount of the nano electret material in the melt-blown fabric material can be reduced, the potential risk is reduced, and the filtering effect can be improved.
Wherein, the trimesoamide derivatives are 1,3, 5-benzene tricarbamoyl tri (tert-butylamine) and/or 1,3, 5-benzene tricarbamoyl tri (cyclohexylamine), and how to modify the trimesoamide to respectively obtain the 1,3, 5-benzene tricarbamoyl tri (tert-butylamine) and/or the 1,3, 5-benzene tricarbamoyl tri (cyclohexylamine) is described in detail below, which is as follows:
(1) the preparation method of the 1,3, 5-benzene tricarbamoyl tri (cyclohexylamine) comprises the following steps:
0.7mol of amine compound (cyclohexylamine) is dissolved in 150mL of 1-methyl-2-pyrrolidone, 0.1g of anhydrous lithium chloride and 20mL of triethylamine are added and mixed with the solution, 0.2mol of trimesoyl chloride is added, the mixture is stirred for 4 hours at 85 ℃, and nitrogen is introduced for protection during stirring. After completion of stirring, it was cooled to room temperature, and the mixture was poured into 500mL of ice water. Filtering the mixture with a glass filter to obtain a crude product, recrystallizing the crude product in DMF (dimethylformamide) for purification, washing with deionized water for 3 times, and vacuum drying at 50 deg.C for 24 hr to obtain a white powder product, i.e. 1,3, 5-benzene tricarbamoyl tris (cyclohexylamine)
(2) The preparation method of the 1,3, 5-benzene tricarbamoyl tri (tert-butylamine) comprises the following steps:
0.62mol of amine compound (tert-butylamine) is dissolved in 100mL of 1-methyl-2-pyrrolidone, 0.1g of anhydrous lithium chloride and 20mL of triethylamine are added and mixed with the amine compound, 0.18mol of trimesoyl chloride is added, the mixture is stirred for 4 hours at 85 ℃, and nitrogen is introduced for protection during stirring. After completion of stirring, it was cooled to room temperature, and the mixture was poured into 500mL of ice water. The mixture was filtered using a glass filter to obtain a crude product, which was recrystallized in DMF (dimethylformamide) for purification, washed 3 times with deionized water, and vacuum dried at 50 ℃ for 24 hours to obtain a white powder product, i.e., 1,3, 5-benzotriazolyl tris (tert-butylamine).
The modified polypropylene comprises polypropylene, an antioxidant, low molecular polyethylene wax, an alkyl coupling agent, electret particles and a lubricant besides the trimesoamide derivatives, wherein the electret is preferably tourmaline nanoparticles.
The modified polypropylene has the following specific formula: the preparation raw materials comprise the following components in parts by weight:
further, as the conventional melt-blowing method needs higher melt-blowing temperature, in a more preferable formula, the modified polypropylene also comprises a molecular weight regulator, and the weight part of the molecular weight regulator is 0.1-0.5 part.
The temperature required during melt blowing can be effectively reduced by adding the molecular weight regulator, and the cost is saved.
The modified polypropylene master batch is prepared by uniformly mixing the materials of the formula and then carrying out the processes of hot melting, extrusion molding, cooling, grain cutting, drying and the like, and the detailed process is as follows:
and S11, sequentially adding the polypropylene, the antioxidant, the low-molecular-weight polyethylene wax, the trimesoamide derivative, the alkyl coupling agent, the electret particles and the lubricant in parts by weight into a high-speed stirrer, and uniformly stirring and mixing to obtain a mixture, wherein the stirring time is controlled to be about 30 minutes.
And S12, mixing and plasticizing the mixture, cooling, and cutting into particles to obtain the modified polypropylene master batch. Specifically, the mixture is added into a double-screw extruder for mixing and plasticizing, and the working parameters of the extruder are as follows:
| partitioning | Region 1 | Zone 2 | Zone 3 | Zone 4 | Zone 5 | Zone 6 | Extrusion temperature |
| Setting temperature of | 125 | 135 | 140 | 145 | 150 | 150 | 150 |
And cooling and molding the melt extruded by the extruder in a water bath, winding, cutting the melt on a granulator into master batches, and finally putting the master batches into a vacuum drying oven to dry for 3 hours at 100 ℃ to obtain the modified polypropylene master batches.
The specific preparation example of the modified polypropylene master batch is as follows:
example 1
77 parts of polypropylene (melt index 1500g/10min), 5 parts of low molecular polyethylene wax, 0.5 part of molecular weight regulator, 0.1 part of antioxidant 1010, 0.2 part of antioxidant 168, 2 parts of lubricant, 0.2 part of trimesoamide derivative, 3 parts of alkyl coupling agent and 12 parts of electret particles are adopted. And sequentially placing the materials into a high-speed mixer for mixing, transferring the mixture to a double-screw co-extruder with the length-diameter ratio of 30 for melt blending and extrusion, wherein the temperature of a melting section is 125-150 ℃, and drying particles after granulation to obtain the modified multifunctional polypropylene master batch material.
Example 2
66 parts of polypropylene (melt index 1500g/10min), 10 parts of low-molecular polyethylene wax, 0.3 part of molecular weight regulator, 0.1 part of antioxidant 1010, 0.2 part of antioxidant 168, 2 parts of lubricant, 0.4 part of trimesoamide derivative, 5 parts of alkyl coupling agent and 16 parts of electret particles. And sequentially placing the materials into a high-speed mixer for mixing, transferring the mixture to a double-screw co-extruder with the length-diameter ratio of 30 for melt blending and extrusion, wherein the temperature of a melting section is 125-150 ℃, and drying particles after granulation to obtain the modified multifunctional polypropylene master batch material.
Example 3
71 parts of polypropylene (with a melt index of 1500g/10min), 8 parts of low-molecular polyethylene wax, 0.4 part of a molecular weight regulator, 0.1 part of an antioxidant 1010, 0.2 part of an antioxidant 168, 3 parts of a lubricant, 0.3 part of a trimesoamide derivative, 2 parts of an alkyl coupling agent and 15 parts of electret particles. And sequentially placing the materials into a high-speed mixer for mixing, transferring the mixture to a double-screw co-extruder with the length-diameter ratio of 30 for melt blending and extrusion, and drying the particles after granulation at the melting section temperature of 125-150 ℃ to obtain the modified multifunctional polypropylene master batch material.
When the melt-blown fabric is actually prepared, the modified polypropylene master batch is used as a material, and the conventional polypropylene master batch can be added, so that the material cost can be reduced, and the effective combination of the cost and the final improvement of the melt-blown fabric performance is realized. Namely, the modified melt-blown fabric material also comprises polypropylene, and the mass percent of the polypropylene is between 96% and 98%, and the mass percent of the modified polypropylene is between 2% and 4%.
The method for preparing improved meltblown fabric from the modified polypropylene masterbatch and the polypropylene masterbatch comprises the following steps
S1, providing modified polypropylene master batches and polypropylene master batches; the modified polypropylene master batch is prepared according to the preparation process of the modified polypropylene master batch, and the polypropylene master batch is conventional PP master batch and can be obtained by market purchase.
S2, uniformly mixing the modified polypropylene master batches and the polypropylene master batches according to the proportion to obtain the melt-blown raw material, namely mixing the modified polypropylene master batches and the polypropylene master batches according to the mass percent of 96-98% of polypropylene and the mass percent of 2-4% of modified polypropylene in a mixer to uniformly mix the materials.
And S3, adding the melt-blown raw material into an extruder, extruding the melt-blown raw material through a die head in a molten state, and obtaining the melt-blown fabric after hot air drafting, cooling and electret treatment.
Because the melt-blown fabric is mechanically pulled in the mask manufacturing process, the requirement on the elongation at break is higher, the toughness of the existing electret melt-blown fabric is deteriorated and the electret melt-blown fabric is easy to break after the electret material is added, and the inventor finds out through research that: the cooled melt-blown fabric is subjected to heat treatment at a certain temperature for a period of time, so that the toughness of the melt-blown fabric can be effectively improved.
The reason is that at a set temperature, the polypropylene with the quasi-hexagonal crystal form can be converted into the alpha crystal form, and the toughness of the final melt-blown fabric is improved due to the increase of the polypropylene with the alpha crystal form. The inventor further determines that the toughness of the melt-blown fabric can reach the optimal value when the melt-blown fabric is treated under the temperature condition of 110-130 ℃. Meanwhile, in order to ensure the winding speed, the heating device can extend from one side to the other side of the melt-blown fabric, the length of the heating device is 1.5 meters, and the heat treatment time of each square meter of the melt-blown fabric is controlled between 5s and 20 s.
In S3, the melt-blown fabric is subjected to corona discharge treatment immediately after the heat treatment, and the charge source of the electret is divided into space charge and polarization charge, and the inventor has found that the increase of the crystallinity of the polypropylene can improve the trapping ability of the space charge and increase the storage stability of the charge. Because the melting point of the crystalline region is higher than that of the amorphous region, molecular chain rearrangement can occur in the amorphous region to form a crystalline structure after a heat treatment process, and meanwhile, incomplete crystals in polypropylene can also undergo melt recrystallization, so that the space charge trapping capability and the storage stability are improved. In addition, one of the sources of the polarization charges is the freezing of the dipoles, and the corona discharge treatment is carried out immediately after the heating at 110-130 ℃, so that the larger temperature difference is favorable for the formation of the orderly orientation freezing of the dipoles.
Example 4
Adding 2% by mass of modified polypropylene master batch and 98% by mass of polypropylene master batch into a metering type master batch proportion mixer, setting parameters of the metering type master batch proportion mixer, and starting to uniformly mix to obtain the melt-blown raw material.
Melt-blown raw materials are put into an extruder, and the extruder works according to the following parameters: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 220 ℃, the fourth zone is 225 ℃, the temperature of a spinneret plate of a die head is 180 ℃, the temperature of hot air is 200 ℃, the pressure of the hot air is 0.8Mpa, a metering pump is controlled at 22-27Hz, melt-blown raw materials are melted into molten mass through hot melting and extruded from spinneret holes, the molten mass is drawn into superfine fibers through high-speed hot air flow, then the superfine fibers are cooled and further drawn through cold air on the side, and finally the superfine fibers are wound by a winding roller.
Before the melt-blown fabric is wound into a coil, the melt-blown fabric is subjected to a heat treatment process, the selected heat treatment temperature is 130 ℃, the heat treatment time is changed by increasing the length of a heating section, and the heat treatment time is about 15s per square meter of the melt-blown fabric.
The fiber web after heat treatment is immediately subjected to electret treatment by a corona discharge device, the electret voltage is 10KV, and the electret distance is 12cm, so that the melt-blown fabric with long-acting charge preservation and good toughness is finally obtained.
Example 5
Adding 3 percent by mass of modified polypropylene master batch and 97 percent by mass of polypropylene master batch into a metering type master batch proportion mixer, setting parameters of the metering type master batch proportion mixer, starting the metering type master batch proportion mixer, and uniformly mixing to obtain the melt-blown raw material.
Melt-blown raw materials are put into an extruder, and the extruder works according to the following parameters: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 220 ℃, the fourth zone is 225 ℃, the temperature of a spinneret plate of a die head is 200 ℃, the temperature of hot air is 200 ℃, the pressure of the hot air is 0.6Mpa, a metering pump is controlled at 22-27Hz, melt-blown raw materials are melted into molten mass through hot melting and extruded from spinneret holes, the molten mass is drawn to superfine fibers through high-speed hot air flow, then the superfine fibers are further drawn through cooling air at the side, and finally the superfine fibers are wound by a winding roller.
Before the melt-blown fabric is wound into a coil, a heat treatment process is carried out, the selected heat treatment temperature is 110 ℃, the heat treatment time is changed by increasing the length of a heating section, and the heat treatment time is about 20s per square meter of the melt-blown fabric.
The fiber web after heat treatment passes through a corona discharge device immediately, the voltage of the electret is 10KV, and the distance of the electret is 12cm, so that the melt-blown fabric with long-acting charge preservation and good toughness is obtained.
Example 6
Adding 4% by mass of modified polypropylene master batch and 96% by mass of polypropylene master batch into a metering type master batch proportion mixer, setting parameters of the metering type master batch proportion mixer, starting the metering type master batch proportion mixer, and uniformly mixing to obtain the melt-blown raw material.
Melt-blown raw materials are put into an extruder, and the extruder works according to the following parameters: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 220 ℃, the fourth zone is 225 ℃, the temperature of a spinneret plate of a die head is 200 ℃, the temperature of hot air is 200 ℃, the pressure of the hot air is 0.4Mpa, a metering pump is controlled at 22-27Hz, melt-blown raw materials are melted into molten mass through hot melting and extruded from spinneret holes, the molten mass is drawn to superfine fibers through high-speed hot air flow, then the superfine fibers are further drawn through cooling air at the side, and finally the superfine fibers are wound by a winding roller.
Before the melt-blown fabric is wound into a coil, a heat treatment process is carried out, the selected heat treatment temperature is 120 ℃, the heat treatment time is changed by increasing the length of a heating section, and the heat treatment time is about 10s per square meter of the melt-blown fabric.
The fiber web after heat treatment passes through a corona discharge device immediately, the voltage of the electret is 10KV, and the distance of the electret is 12cm, so that the melt-blown fabric with long-acting charge preservation and good toughness is obtained.
Example 7
Adding 3 percent by mass of modified polypropylene master batch and 97 percent by mass of polypropylene master batch into a metering type master batch proportion mixer, setting parameters of the metering type master batch proportion mixer, starting the metering type master batch proportion mixer, and uniformly mixing to obtain the melt-blown raw material.
Melt-blown raw materials are put into an extruder, and the extruder works according to the following parameters: the temperature of a spinneret plate of a die head is 180 ℃, the temperature of hot air is 200 ℃, the pressure of the hot air is 0.4Mpa, a metering pump is controlled at 22-27Hz, melt-blown raw materials are melted into molten mass through hot melting and extruded from spinneret holes, the molten mass is drawn to superfine fibers through high-speed hot air flow, then the superfine fibers are further drawn through cooling air at the side, and finally the superfine fibers are wound by a winding roller.
Before the melt-blown fabric is wound into a coil, a heat treatment process is carried out in the winding process, the selected heat treatment temperature is 120 ℃, the heat treatment time is changed by increasing the length of a heating section, and the heat treatment time is about 20s per square meter of the melt-blown fabric.
The fiber web after heat treatment passes through a corona discharge device immediately, the voltage of the electret is 12KV, and the distance of the electret is 12cm, so that the melt-blown fabric with long-acting charge preservation and good toughness is obtained.
The meltblown obtained by the above examples, when used for filtration (filtration efficiency for particles with a particle size greater than 0.3 μm), has the following properties:
due to the increase of the charge amount and the charge time of the meltblown fabric, the filtration efficiency was maintained above 99.5% at relatively low test flow rates and above 98% at relatively high test flow rates. Meanwhile, the elongation of the finally obtained melt-blown fabric is obviously improved, and the risk of breakage when the mask is processed is reduced.
The present invention may be embodied in various forms and techniques, and all technical equivalents may be used.
Claims (10)
1. The modified polypropylene master batch is characterized in that: comprises polypropylene, antioxidant, low molecular polyethylene wax, alkyl coupling agent, electret particles, lubricant and trimesoamide derivatives.
2. The modified polypropylene masterbatch according to claim 1, wherein: the trimesoamide derivatives are 1,3, 5-benzene tri-formyl tri (tert-butylamine) and/or 1,3, 5-benzene tri-formyl tri (cyclohexylamine).
3. The modified polypropylene masterbatch according to claim 1, wherein: the preparation raw materials comprise the following components in parts by weight:
60-80 parts of polypropylene
0.4 portion of antioxidant 10100.1
0.4 portion of antioxidant 1680.1
1-10 parts of low-molecular polyethylene wax
0.2-0.4 part of trimesoamide derivatives
3-5 parts of alkyl coupling agent
15-20 parts of electret particles
0.5-3 parts of a lubricant.
4. The modified polypropylene masterbatch of claim 3, wherein: the raw materials for preparing the compound also comprise a molecular weight regulator.
5. The modified polypropylene masterbatch according to claim 4, wherein: the weight portion of the molecular weight regulator is 0.1-0.5 portion.
6. The modified melt-blown cloth material is characterized in that: the polypropylene composite material comprises polypropylene and modified polypropylene, wherein the mass percent of the polypropylene is between 96% and 98%, and the mass percent of the modified polypropylene is between 2% and 4%.
7. The improved melt-blown fabric processing method is characterized by comprising the following steps: comprises the following steps
S1, providing modified polypropylene master batches and polypropylene master batches;
s2, uniformly mixing the modified polypropylene master batch and the polypropylene master batch according to the proportion to obtain a melt-blown raw material;
and S3, adding the melt-blown raw material into an extruder, extruding the melt-blown raw material through a die head in a molten state, and obtaining the melt-blown fabric after hot air drafting, cooling and electret treatment.
8. The improved meltblown processing method of claim 7, further comprising: in the step S1, the modified polypropylene masterbatch is prepared by the following steps:
s11, adding polypropylene, an antioxidant, low-molecular polyethylene wax, a molecular weight regulator, trimesoamide derivatives, an alkyl coupling agent, electret particles and a lubricant in proportion and sequence, and uniformly mixing to obtain a mixture;
and S12, mixing and plasticizing the mixture, cooling, and cutting into particles to obtain the modified polypropylene master batch.
9. The improved meltblown processing method of claim 8, further comprising: the trimesoamide derivative is prepared by the following method,
dissolving 0.7mol of amine compound in 150mL of 1-methyl-2-pyrrolidone, adding 0.1g of anhydrous lithium chloride and 20mL of triethylamine to mix with the amine compound, adding 0.2mol of trimesoyl chloride, stirring the mixture at 85 ℃ for 4 hours, and introducing nitrogen for protection in the stirring process; after stirring, cooling to room temperature, and pouring the mixture into 500mL of ice water; filtering the mixture by using a glass filter to obtain a crude product, recrystallizing and purifying the obtained crude product in DMF (dimethyl formamide), washing the crude product for 3 times by using deionized water, and performing vacuum drying at 50 ℃ for 24 hours to obtain a white powder product, namely 1,3, 5-benzene tri (cyclohexylamine);
or 0.62mol of amine compound is dissolved in 100mL of 1-methyl-2-pyrrolidone, then 0.1g of anhydrous lithium chloride and 20mL of triethylamine are added and mixed with the amine compound, then 0.18mol of trimesoyl chloride is added, the mixture is stirred for 4h at 85 ℃, and nitrogen is introduced for protection in the stirring process; after stirring, cooling to room temperature, and pouring the mixture into 500mL of ice water; filtering the mixture by using a glass filter to obtain a crude product, recrystallizing and purifying the obtained crude product in DMF (dimethyl formamide), washing the crude product for 3 times by using deionized water, and drying the crude product in vacuum at 50 ℃ for 24 hours to obtain a white powder product, namely the 1,3, 5-benzene tricarbamoyl tri (tert-butylamine).
10. The improved meltblown processing method of claim 7, further comprising: s3 includes heat treating the meltblown web after cooling and before the electret treating, at a temperature of 110 ℃ to 130 ℃ for a treatment time of between 5 seconds to 20 seconds per square meter of the meltblown web, and wherein the electret treating is performed immediately after heating.
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