CN111702982A - Preparation method of high-MFR polypropylene melt-blown special material - Google Patents

Preparation method of high-MFR polypropylene melt-blown special material Download PDF

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Publication number
CN111702982A
CN111702982A CN202010398770.1A CN202010398770A CN111702982A CN 111702982 A CN111702982 A CN 111702982A CN 202010398770 A CN202010398770 A CN 202010398770A CN 111702982 A CN111702982 A CN 111702982A
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polypropylene
melt
blown
special material
material according
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CN202010398770.1A
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Inventor
黄振
申乾成
申辉
申暮春
黄自豪
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Anhui Guanhong Plastic Industry Co ltd
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Anhui Guanhong Plastic Industry Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/02Making granules by dividing preformed material
    • B29B9/06Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00Conditioning or physical treatment of the material to be shaped
    • B29B13/10Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/14Peroxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/315Compounds containing carbon-to-nitrogen triple bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/36Sulfur-, selenium-, or tellurium-containing compounds
    • C08K5/45Heterocyclic compounds having sulfur in the ring
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/12Applications used for fibers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a preparation method of a high MFR polypropylene melt-blown special material, which relates to the technical field of melt-blown non-woven fabric processing, takes polypropylene as a base material, cuts molecular chains of low MFR polypropylene by adding peroxide, reduces the molecular weight, improves the fluidity of a melt, thereby producing the polypropylene melt-blown special material with the MFR being as high as 1500g/10min, simultaneously, the volatile component is less than 0.05 percent, and the ash content is less than 0.02 percent, and the polypropylene melt-blown special material is suitable for being used as a processing raw material of the melt-blown non-woven fabric.

Description

Preparation method of high-MFR polypropylene melt-blown special material
The technical field is as follows:
the invention relates to the technical field of melt-blown non-woven fabric processing, in particular to a preparation method of a high-MFR polypropylene melt-blown special material.
Background art:
the melt-blown non-woven fabric is widely applied to the fields of filter materials, medical and health materials, environmental protection materials, clothing materials, battery diaphragm materials and the like. At this stage, due to the emergence of new coronavirus pneumonia, melt-blown nonwoven fabrics are more and more well known. The melt-blown non-woven fabric has good filtering performance and plays an important role in the mask.
The higher the Melt Flow Rate (MFR) of the material used to produce the meltblown nonwoven fabric, the finer the meltblown fibers and the better the filtration performance of the resulting meltblown nonwoven fabric, and the MFR generally required for materials used to produce meltblown nonwoven fabrics is above 800g/10 min. At present, in order to save cost and simplify the process, polypropylene with low melt index is mostly used as a raw material, and a peroxide controlled degradation method is adopted to produce a melt-blown material with high MFR. Patent CN201610375131.7 discloses an additive for producing meltblown nonwoven fabrics, comprising fatty acid amide and di-t-butyl peroxide, but does not provide MFR value of meltblown produced by the additive, so it is difficult to objectively judge the effect of the additive on MFR value improvement. Patent CN201910197622.0 discloses a melt-blown copolymer and a process for its production, but MFR values in the range of 35 to 140g/10min do not give melt-blown material of high MFR.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation method of a high-MFR polypropylene melt-blown special material, which is used for preparing the high-MFR polypropylene melt-blown special material with low volatile and ash content by improving the preparation method of the polypropylene melt-blown material and is suitable for processing high-quality melt-blown non-woven fabrics.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of a high MFR polypropylene melt-blown special material comprises the following preparation steps:
(1) freezing polypropylene at low temperature, crushing, ball milling and sieving to obtain polypropylene powder;
(2) adding polypropylene powder, peroxide and a dispersing agent into a mixer, and mixing at a high speed to obtain a premix;
(3) adding the premix into a double-screw extruder, heating and melting, enabling the melt to flow out of a die head of the extruder, cooling, granulating, and sieving to obtain the special melt-blown material.
The low-temperature freezing temperature is-15 to-10 ℃, and the time is 12 to 24 hours.
The invention obtains the particle size of the polypropylene particles by freezing, crushing and ball milling, thereby being beneficial to the uniform blending of the polypropylene and the peroxide.
The mass ratio of the polypropylene powder, the peroxide and the dispersant is (80-100) to (5-20) to (1-10).
The polypropylene is homo-or co-polypropylene, and the MFR is 0.5-40g/10 min.
The peroxide is 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane. The peroxide is used as a degradation agent, has excellent safety performance and degradation efficiency and extremely low odor compared with other existing degradation agents, and is a preferred peroxide for degrading polypropylene.
The good dispersibility of peroxide in polypropylene is a necessary condition for the narrow molecular weight distribution of polypropylene, and conversely, the peroxide and the polypropylene have heterogeneous reaction, which causes severe local degradation and broaden the molecular weight distribution.
The addition of the dispersing agent can prevent the degradation agent from being adsorbed on the surface of the polypropylene powder, thereby improving the dispersibility of the peroxide in the polypropylene and improving the MFR value of the polypropylene; moreover, the addition of the dispersing agent can also enhance the mechanical properties of the polypropylene.
The dispersant is N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxy acrylamide. The invention takes N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxy acrylamide as a dispersant, and improves the dispersibility of peroxide in polypropylene and enhances the mechanical property of the polypropylene by utilizing the affinity of the dispersant to the polypropylene and the peroxide.
The dispersant is 5- (5-ethyl thiophene-3-yl) -4- (tetrahydrofuran-2-ylmethyl) -4H-1,2, 4-triazole-3-thiol.
The invention also uses 5- (5-ethyl thiophene-3-yl) -4- (tetrahydrofuran-2-ylmethyl) -4H-1,2, 4-triazole-3-thiol as a dispersant, and tests show that the technical effect obtained by the invention is better than that of N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxy acrylamide.
The extruder temperature was 200 ℃ and 250 ℃.
The die temperature was 200 ℃ and 250 ℃.
The cooling adopts a water cooling tank.
The invention has the beneficial effects that: the invention takes polypropylene as a base material, cuts molecular chains of low MFR polypropylene by adding peroxide, reduces molecular weight, improves the fluidity of melt, thereby producing the special polypropylene material with MFR as high as 1500g/10min, simultaneously, the volatile content is less than 0.05 percent, the ash content is less than 0.02 percent, and the polypropylene material is suitable for being used as a processing raw material of melt-blown non-woven fabrics.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The polypropylene in the examples and comparative examples was shanghai seiki S2040 PP.
Example 1
(1) Freezing polypropylene at-12 ℃ for 12h, crushing, ball-milling, and sieving with a 300-mesh sieve to obtain polypropylene powder;
(2) adding 100g of polypropylene powder, 8g of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane and 5g of N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxy acrylamide into a mixer, and mixing at high speed to obtain a premix;
(3) adding the premix into a double-screw extruder, heating and melting, enabling the melt to flow out of a die head of the extruder, cooling by a water cooling tank at 20 ℃, pelletizing and sieving by a 120-mesh sieve, wherein the temperatures of all sections of the extruder are 210 ℃, 220 ℃, 230 ℃ and 220 ℃, the temperature of the die head is 230 ℃ and the temperature of the die head is 20 ℃, so as to obtain the special material for melt-blown.
Example 2
Example 2 differs from example 1 only in that the amount of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane used was adjusted to 12 g.
(1) Freezing polypropylene at-12 ℃ for 12h, crushing, ball-milling, and sieving with a 300-mesh sieve to obtain polypropylene powder;
(2) adding 100g of polypropylene powder, 12g of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane and 5g N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxy acrylamide into a mixer, and mixing at high speed to obtain a premix;
(3) adding the premix into a double-screw extruder, heating and melting, enabling the melt to flow out of a die head of the extruder, cooling by a water cooling tank at 20 ℃, pelletizing and sieving by a 120-mesh sieve, wherein the temperatures of all sections of the extruder are 210 ℃, 220 ℃, 230 ℃ and 220 ℃, the temperature of the die head is 230 ℃ and the temperature of the die head is 20 ℃, so as to obtain the special material for melt-blown.
Example 3
Example 3 differs from example 1 only in that the dispersant is replaced with an equal amount of 5- (5-ethylthiophen-3-yl) -4- (tetrahydrofuran-2-ylmethyl) -4H-1,2, 4-triazole-3-thiol.
(1) Freezing polypropylene at-12 ℃ for 12h, crushing, ball-milling, and sieving with a 300-mesh sieve to obtain polypropylene powder;
(2) adding 100g of polypropylene powder, 8g of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane and 5g of 5- (5-ethylthiophene-3-yl) -4- (tetrahydrofuran-2-ylmethyl) -4H-1,2, 4-triazole-3-thiol into a mixer, and mixing at high speed to obtain a premix;
(3) adding the premix into a double-screw extruder, heating and melting, enabling the melt to flow out of a die head of the extruder, cooling by a water cooling tank at 20 ℃, pelletizing and sieving by a 120-mesh sieve, wherein the temperatures of all sections of the extruder are 210 ℃, 220 ℃, 230 ℃ and 220 ℃, the temperature of the die head is 230 ℃ and the temperature of the die head is 20 ℃, so as to obtain the special material for melt-blown.
Comparative example
The comparative example differs from example 1 only in that the dispersant N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxyacrylamide was not added.
(1) Freezing polypropylene at-12 ℃ for 12h, crushing, ball-milling, and sieving with a 300-mesh sieve to obtain polypropylene powder;
(2) adding 100g of polypropylene powder and 8g of 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane into a mixer, and mixing at high speed to obtain a premix;
(3) adding the premix into a double-screw extruder, heating and melting, enabling the melt to flow out of a die head of the extruder, cooling by a water cooling tank at 20 ℃, pelletizing and sieving by a 120-mesh sieve, wherein the temperatures of all sections of the extruder are 210 ℃, 220 ℃, 230 ℃ and 220 ℃, the temperature of the die head is 230 ℃ and the temperature of the die head is 20 ℃, so as to obtain the special material for melt-blown.
The melt-blown special materials prepared in the above examples and comparative examples were subjected to the performance test, and the test methods and the test results are shown in table 1.
TABLE 1
Figure BDA0002488664480000041
Figure BDA0002488664480000051
As can be seen from Table 1, the addition of the peroxide of the present invention can significantly increase the melt index of the polypropylene melt-blown special material but reduce the tensile stress at break and the tensile stress at yield, while the addition of the dispersant can simultaneously increase the melt index, the tensile stress at break and the tensile stress at yield of the polypropylene melt-blown special material.
The volatile components and ash contents of the polypropylene melt-blown special material prepared in the above examples 1-3 were measured according to GB/T2914 (110 ℃) and GB/T9345.1 (850 ℃), and the results were: the volatile content is less than 0.05 percent, and the ash content is less than 0.02 percent.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (9)

1. A preparation method of a high MFR polypropylene melt-blown special material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) freezing polypropylene at low temperature, crushing, ball milling and sieving to obtain polypropylene powder;
(2) adding polypropylene powder, peroxide and a dispersing agent into a mixer, and mixing at a high speed to obtain a premix;
(3) adding the premix into a double-screw extruder, heating and melting, enabling the melt to flow out of a die head of the extruder, cooling, granulating, and sieving to obtain the special melt-blown material.
2. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the low-temperature freezing temperature is-15 to-10 ℃, and the time is 12 to 24 hours.
3. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the mass ratio of the polypropylene powder, the peroxide and the dispersant is (80-100) to (5-20) to (1-10).
4. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the polypropylene is homo-or co-polypropylene, and the MFR is 0.5-40g/10 min.
5. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the peroxide is 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane.
6. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the dispersant is N- [ 4-cyano-3- (trifluoromethyl) phenyl ] methyl epoxy acrylamide.
7. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the extruder temperature was 200 ℃ and 250 ℃.
8. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the die temperature was 200 ℃ and 250 ℃.
9. The method for preparing high MFR polypropylene melt-blown special material according to claim 1, wherein: the cooling adopts a water cooling tank.
CN202010398770.1A 2020-05-12 2020-05-12 Preparation method of high-MFR polypropylene melt-blown special material Withdrawn CN111702982A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112795097A (en) * 2021-01-05 2021-05-14 中广核俊尔(浙江)新材料有限公司 High-flexibility low-odor polypropylene material, preparation method thereof and application thereof in manufacturing melt-blown fabric

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112795097A (en) * 2021-01-05 2021-05-14 中广核俊尔(浙江)新材料有限公司 High-flexibility low-odor polypropylene material, preparation method thereof and application thereof in manufacturing melt-blown fabric

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