CN115992399A - Preparation process of high-strength polypropylene staple fibers - Google Patents
Preparation process of high-strength polypropylene staple fibers Download PDFInfo
- Publication number
- CN115992399A CN115992399A CN202310184515.0A CN202310184515A CN115992399A CN 115992399 A CN115992399 A CN 115992399A CN 202310184515 A CN202310184515 A CN 202310184515A CN 115992399 A CN115992399 A CN 115992399A
- Authority
- CN
- China
- Prior art keywords
- castor oil
- polyoxyethylene ether
- oil polyoxyethylene
- polypropylene
- polypropylene staple
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- -1 polypropylene Polymers 0.000 title claims abstract description 131
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 77
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 75
- 239000000835 fiber Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000004359 castor oil Substances 0.000 claims abstract description 112
- 235000019438 castor oil Nutrition 0.000 claims abstract description 112
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 112
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 64
- 239000010452 phosphate Substances 0.000 claims abstract description 64
- 239000000203 mixture Substances 0.000 claims abstract description 57
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 56
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000002788 crimping Methods 0.000 claims abstract description 5
- 238000009998 heat setting Methods 0.000 claims abstract description 5
- 239000008041 oiling agent Substances 0.000 claims abstract description 5
- 238000004806 packaging method and process Methods 0.000 claims abstract description 5
- 239000000654 additive Substances 0.000 claims abstract description 4
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000010035 extrusion spinning Methods 0.000 claims abstract description 4
- 239000000155 melt Substances 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 80
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 39
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 28
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 28
- 235000011187 glycerol Nutrition 0.000 claims description 26
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 15
- 230000007062 hydrolysis Effects 0.000 claims description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims description 14
- JAJRRCSBKZOLPA-UHFFFAOYSA-M triethyl(methyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(CC)CC JAJRRCSBKZOLPA-UHFFFAOYSA-M 0.000 claims description 14
- 238000006386 neutralization reaction Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000002585 base Substances 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000007872 degassing Methods 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 17
- 239000002216 antistatic agent Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004804 winding Methods 0.000 description 9
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 8
- 239000003921 oil Substances 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 6
- 229910015900 BF3 Inorganic materials 0.000 description 5
- 125000000129 anionic group Chemical group 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 125000002091 cationic group Chemical group 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- KVFVBPYVNUCWJX-UHFFFAOYSA-M ethyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(C)C KVFVBPYVNUCWJX-UHFFFAOYSA-M 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000009849 vacuum degassing Methods 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 1
- 206010020112 Hirsutism Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- LYRKJTJQRBRDLB-UHFFFAOYSA-N [P].C1CO1 Chemical compound [P].C1CO1 LYRKJTJQRBRDLB-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000005691 triesters Chemical class 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The application relates to the technical field of functionalized polypropylene staple fibers, in particular to a preparation process of high-strength polypropylene staple fibers. The preparation process of the high-strength polypropylene short fiber is characterized by comprising the following steps of: step one, placing the polypropylene fiber forming slices and the additive into a temperature of 110-130 ℃ for preheating, continuously stirring for 20-40min, and then cooling. Drying at 120-140 ℃ for 3-4 hours to obtain a mixed master batch; step two, conveying the mixed master batch to a screw extruder, compacting and plasticizing, melting by a screw, filtering by a filter, and then entering a melt pipeline; step three, sequentially performing extrusion spinning, cooling, oiling, drafting, crimping, heat setting, cutting and packaging to obtain high-strength polypropylene staple fibers; wherein, during oiling operation, the polypropylene oiling agent is selected from castor oil polyoxyethylene ether-phosphate ester composition. The preparation process has the advantages of reducing broken filaments of the polypropylene staple fibers and improving the strength of the polypropylene staple fibers.
Description
Technical Field
The application relates to the technical field of functionalized polypropylene staple fibers, in particular to a preparation process of high-strength polypropylene staple fibers.
Background
Polypropylene, also called polypropylene fiber or PP fiber, is a fiber melt-spun from isotactic polypropylene, and has the advantages of high strength, small specific gravity, abrasion resistance, corrosion resistance and the like, so that the polypropylene fiber is widely applied to civil and industrial fields.
In actual production, the quality of the polypropylene staple fiber is affected by the process flow in addition to the quality of the raw materials. When the polypropylene is spun at a high speed, friction and static electricity generated by the mutual movement of the fibers and equipment can cause the dispersion of the tows, so that the polypropylene is promoted to generate phenomena of yarn hairiness, winding roller, yarn breakage and the like, and the prepared polypropylene short fiber has insufficient strength.
Disclosure of Invention
In order to overcome the defect of insufficient strength of the polypropylene staple fibers, the application provides a preparation process of the high-strength polypropylene staple fibers.
The preparation process of the high-strength polypropylene staple fiber provided by the application adopts the following technical scheme:
a preparation process of high-strength polypropylene short fibers comprises the following steps:
step one, placing the polypropylene fiber forming slices and the additive into a temperature of 110-130 ℃ for preheating, continuously stirring for 20-40min, and then cooling. Drying at 120-140 ℃ for 3-4 hours to obtain a mixed master batch;
step two, conveying the mixed master batch to a screw extruder, compacting and plasticizing, melting by a screw, filtering by a filter, and then entering a melt pipeline;
step three, sequentially performing extrusion spinning, cooling, oiling, drafting, crimping, heat setting, cutting and packaging to obtain high-strength polypropylene staple fibers;
wherein, during oiling operation, the polypropylene oiling agent is selected from castor oil polyoxyethylene ether-phosphate ester composition.
Castor oil polyoxyethylene ether is an ester type polyol nonionic surfactant which has excellent emulsifying property, dispersibility, softening property and antistatic property. Therefore, when the castor oil polyoxyethylene ether acts on the polypropylene fiber, the castor oil polyoxyethylene ether not only can increase the smooth and soft performance of the polypropylene fiber, but also can reduce the electrostatic influence generated by high-speed spinning of the polypropylene fiber, effectively reduce the possibility of phenomena such as yarn, winding roller and broken yarn of the polypropylene fiber, and indirectly improve the strength of the polypropylene short fiber.
The principle of the castor oil polyoxyethylene ether is that the polyoxyethylene ether can form hydrogen bond with water, so that the hygroscopicity of the fiber is increased, and the resistance of the surface of the fiber is reduced due to the improvement of the water content, so that the static electricity is easy to leak. However, the nonionic surfactant is relatively weak in antistatic property improving effect.
The phosphate is a main functional group of the anionic antistatic agent, and the phosphate also has a synergistic effect with castor oil polyoxyethylene ether as the anionic antistatic agent, so that the phosphate has high oil film strength besides excellent smooth wire and antistatic performance after being combined.
Therefore, when the phosphate functional group is added into the castor oil polyoxyethylene ether system, the obtained castor oil polyoxyethylene ether-phosphate composition can further reduce the possibility of phenomena such as yarn, winding roller, yarn breakage and the like of the polypropylene, and indirectly improve the strength of the polypropylene short fiber.
Preferably, the castor oil polyoxyethylene ether-phosphate composition comprises the following raw materials: hydrogenated castor oil, ethylene oxide, phosphorus pentoxide, catalysts and bases;
the molar ratio of the hydrogenated castor oil to the ethylene oxide to the phosphorus pentoxide is 1: (70-90): (0.5-1), the catalyst is added in an amount of 2% of the total mass, and the base adjusts the castor oil polyoxyethylene ether-phosphate composition to ph=8.
When the molar ratio of the hydrogenated castor oil to the ethylene oxide is adopted, the prepared castor oil polyoxyethylene ether-phosphate composition has higher molecular weight, so that higher heat resistance and oil film strength are obtained, the possibility of phenomena such as yarn, winding, yarn breakage and the like of the polypropylene is further reduced, and the strength of the polypropylene short fiber is indirectly improved.
When the molar ratio of the hydrogenated castor oil, the ethylene oxide and the phosphorus pentoxide is adopted, the prepared castor oil polyoxyethylene ether-phosphate composition can obtain monoester with more specific gravity, but compared with diester or triester, the monoester can promote the castor oil polyoxyethylene ether-phosphate composition to obtain more excellent antistatic performance.
Preferably, the preparation method of the castor oil polyoxyethylene ether-phosphate composition comprises the following steps:
s1, mixing hydrogenated castor oil with a catalyst, stirring, heating and dehydrating, adding ethylene oxide, heating for reaction, and finally cooling, degassing, decoloring and filtering to obtain castor oil polyoxyethylene ether;
s2, slowly adding phosphorus pentoxide into the castor oil polyoxyethylene ether for 1-2h, then adding quantitative water for hydrolysis for 2-3h, and finally adding alkali for neutralization at 50-60 ℃ to obtain the castor oil polyoxyethylene ether-phosphate composition.
Preferably, in S2, after the phosphorus pentoxide is added, the temperature is firstly increased to 80-90 ℃, the reaction is carried out for 3-5 hours under the heat preservation, and then the hydrolysis is carried out.
When the castor oil polyoxyethylene ether and phosphorus pentoxide are required to react, the temperature and the heat preservation time promote the content of monoester to be increased, and the reaction time is shorter and the color of the product is lighter at the temperature.
Preferably, the base is aqueous methyl triethylammonium hydroxide.
Methyl triethylammonium hydroxide is a quaternary ammonium base that is readily soluble in water and is strongly basic, and therefore, methyl triethylammonium hydroxide can also be used for neutralization of castor oil polyoxyethylene ether-phosphate compositions. Furthermore, after neutralization, the quaternary ammonium salt groups in the methyltriethylammonium hydroxide can also be loaded into the castor oil polyoxyethylene ether-phosphate composition. The quaternary ammonium salt group belongs to the functional group of the cationic antistatic agent, and the cationic antistatic agent has the most excellent antistatic effect, so that the antistatic performance of the castor oil polyoxyethylene ether-phosphate composition is further improved.
Preferably, the raw materials of the castor oil polyoxyethylene ether-phosphate composition further comprise glycerin, and the mol ratio of the glycerin to the hydrogenated castor oil is 1: (1-2).
The addition of the glycerol can promote the castor oil polyoxyethylene ether-phosphate composition to additionally contain the glycerol group, and the glycerol group can promote the castor oil polyoxyethylene ether-phosphate composition to have better hydrophilicity, so that the antistatic performance of the castor oil polyoxyethylene ether-phosphate composition is further improved.
Preferably, the molar ratio of the hydrogenated castor oil, the glycerol, the ethylene oxide and the phosphorus pentoxide is 1:1.5:8:0.75.
when the molar ratio of the hydrogenated castor oil, the glycerol, the ethylene oxide and the phosphorus pentoxide is adopted, castor oil polyoxyethylene ether, the glycerol, the phosphate and the quaternary ammonium salt are balanced, so that the prepared castor oil polyoxyethylene ether-phosphate composition has the most excellent smoothness, antistatic performance and oil film strength, the possibility of phenomena such as yarn breakage, winding roll and yarn breakage of polypropylene fibers is effectively reduced, and the strength of the polypropylene short fibers is indirectly improved.
Preferably, the preparation method of the castor oil polyoxyethylene ether-phosphate composition comprises the following steps:
s1, mixing hydrogenated castor oil, glycerol and concentrated sulfuric acid with the total mass of 3%, then preserving heat at 100-110 ℃ for 2-3 hours, then mixing with a catalyst, stirring, heating and dehydrating, then adding ethylene oxide, heating and reacting, and finally cooling, degassing, decolorizing and filtering to obtain castor oil glycerol polyoxyethylene ether;
s2, slowly adding phosphorus pentoxide into the castor oil glycerol polyoxyethylene ether for 1-2h, then heating to 80-90 ℃, carrying out heat preservation reaction for 3-5h, then adding quantitative water for hydrolysis for 2-3h, and finally adding a methyl triethyl ammonium hydroxide aqueous solution for neutralization at 50-60 ℃ to obtain the castor oil polyoxyethylene ether-phosphate composition.
In summary, the present application has the following beneficial effects:
1. the phosphate can be used as an anionic antistatic agent to have a synergistic effect with castor oil polyoxyethylene ether, so that when the two agents are combined, the antistatic agent has excellent smooth wire and antistatic performance, and also has higher oil film strength, the possibility of phenomena such as yarn, winding roller and yarn breakage of polypropylene is further reduced, and the strength of the polypropylene short fiber is indirectly improved.
2. Methyl triethylammonium hydroxide can be used for neutralization of castor oil polyoxyethylene ether-phosphate compositions. And after neutralization, the quaternary ammonium salt group in the methyltriethylammonium hydroxide can be loaded in the castor oil polyoxyethylene ether-phosphate composition, so that the antistatic performance of the castor oil polyoxyethylene ether-phosphate composition is further improved.
3. The addition of the glycerol can promote the castor oil polyoxyethylene ether-phosphate composition to additionally contain the glycerol group, and the glycerol group can promote the castor oil polyoxyethylene ether-phosphate composition to have better hydrophilicity, so that the antistatic performance of the castor oil polyoxyethylene ether-phosphate composition is further improved.
Detailed Description
The present application is described in further detail below in connection with examples 1-12 and comparative example 1.
Raw materials
Polypropylene slice PP BH Langang petrochemical; hydrogenated castor oil CAS:8001-78-3; ethylene oxide CAS:75-21-8; phosphorus pentoxide CAS:1314-56-3; methyl triethylammonium hydroxide CAS:109334-81-8; glycerol CAS:56-81-5; boron trifluoride CAS:7637-07-2; potassium hydroxide CAS:1310-58-3.
Examples
Example 1
A preparation process of high-strength polypropylene short fibers comprises the following steps:
step one, the polypropylene fiber forming slice and the additive are placed at the temperature of 120 ℃ (preferably 110-130 ℃) to be preheated and continuously stirred for 30min (preferably 20-40 min), and then cooled. Drying at 130deg.C (preferably 120-140deg.C) for 3.5 hr (preferably 3-4 hr) to obtain mixed master batch;
wherein, the polypropylene fiber forming slice and the addition amount or class of the addition auxiliary agent can be selected according to the actual requirement; in this example, in order to reduce the influence of the addition of the auxiliary agent on the subsequent test, only polypropylene fiber-forming chips were added;
step two, conveying the mixed master batch to a screw extruder, compacting and plasticizing, melting by a screw, filtering by a filter, and then entering a melt pipeline;
and thirdly, sequentially performing extrusion spinning, cooling, oiling, drafting, crimping, heat setting, cutting and packaging to obtain the high-strength polypropylene staple fiber.
Wherein, the mesh number of the filter is 200 meshes (180-220 meshes are suitable), and the temperature of the five zones of the screw is respectively: a region: 305 ℃; two areas: 300 ℃; three regions: 295 deg.c; four regions: 280 ℃; five regions: 275 ℃. Flange zone 275 ℃, elbow zone: 270 ℃, spinning manifold: 267 ℃, annular blowing speed: 0.45m/min, wind temperature: spinning speed at 16 deg.c: 750m/min, pre-spinning oiling: 1.5%; oil wet rate of the precursor: 15%.
Total denier bundled: 66 ten thousand denier, total draft: 4, a step of; stretching speed: 90m/min, stretching temperature: oil bath 56 ℃, superheated steam: 110 ℃, crimping machine main pressure: 1.8kg/cm2, back pressure: 1.2kg/cm2, heat setting four zone temperature: a region: 100 ℃, two areas: 115 ℃, three regions: 125 ℃, four regions: 95 ℃; cutting and packaging at 95deg.C, and cutting length of 35mm.
In addition, during oiling operation, the polypropylene oiling agent is selected from castor oil polyoxyethylene ether-phosphate ester compositions.
The castor oil polyoxyethylene ether-phosphate composition is prepared by reacting hydrogenated castor oil, ethylene oxide, phosphorus pentoxide, catalyst-boron trifluoride and potassium hydroxide, wherein the molar ratio of the hydrogenated castor oil to the ethylene oxide to the phosphorus pentoxide is 1:80:0.75, the addition amount of the catalyst-boron trifluoride is 2% of the total mass, and the potassium hydroxide is used for adjusting the castor oil polyoxyethylene ether-phosphate composition to pH=8.
The preparation method of the castor oil polyoxyethylene ether-phosphate composition comprises the following steps:
s1, pumping hydrogenated castor oil and 20g of catalyst boron trifluoride into a condensation kettle, sequentially opening a stirring and heating valve, dehydrating at the temperature of 90 ℃ in a vacuum environment, adding ethylene oxide, reacting for 3 hours at the temperature of 105 ℃, cooling to 100 ℃ and carrying out vacuum degassing for 20min, decoloring, dehydrating and filtering to obtain castor oil polyoxyethylene ether;
s2, filling castor oil polyoxyethylene ether into a three-neck flask provided with a stirrer, a spherical condenser and a thermometer, then starting the stirrer, then slowly adding phosphorus pentoxide, wherein the molar ratio of hydrogenated castor oil to phosphorus pentoxide is 1:0.75, the charging time is 1.5h (1-2 h is suitable), then adding 100g of water for hydrolysis for 2.5h (2-3 h), and finally adding a potassium hydroxide aqueous solution (1 mol/L) for neutralization at 55 ℃ (50-60 ℃ is suitable), thus obtaining the castor oil polyoxyethylene ether-phosphate composition with the total mass of 1 kg+/-50 g.
Examples 2 to 5
The difference from example 1 is that the molar ratios of hydrogenated castor oil, ethylene oxide and phosphorus pentoxide are different, as shown in Table 1.
Table 1 molar ratio of the components in examples 2-5
| Hydrogenated castor oil | Ethylene oxide | Phosphorus pentoxide | |
| Example 1 | 1 | 80 | 7.5 |
| Example 2 | 1 | 70 | 7.5 |
| Example 3 | 1 | 90 | 7.5 |
| Example 4 | 1 | 80 | 0.5 |
| Example 5 | 1 | 80 | 1 |
Example 6
The difference from example 1 is that in S2, after the addition of phosphorus pentoxide was completed, the temperature was first raised to 85℃and the reaction was continued for 4 hours, followed by hydrolysis.
Example 7
The difference from example 6 is that in S2, after the addition of phosphorus pentoxide was completed, the temperature was first raised to 80℃and the reaction was continued for 3 hours, followed by hydrolysis.
Example 8
The difference from example 6 is that in S2, after the addition of phosphorus pentoxide is completed, the temperature is first raised to 90℃and the reaction is continued for 5 hours, followed by hydrolysis.
Example 9
The difference from example 6 is that the aqueous potassium hydroxide solution was replaced with an aqueous solution of trimethylethylammonium hydroxide of the same concentration.
Example 10
The difference from example 9 is that the raw material of the castor oil polyoxyethylene ether-phosphate composition further comprises glycerin, and the molar ratio of glycerin to hydrogenated castor oil is 1:1.5.
the preparation method of the castor oil polyoxyethylene ether-phosphate composition comprises the following steps:
s1, mixing hydrogenated castor oil, glycerol and 30g of concentrated sulfuric acid solution (70 wt%) and then preserving heat at 105 ℃ (100-110 ℃ is suitable) for 2.5h (2-3 h is suitable), then pumping the mixture and 20g of catalyst-boron trifluoride into a condensation kettle, sequentially opening a stirring and heating valve, dehydrating at a vacuum environment and a temperature of 90 ℃, adding ethylene oxide and reacting at 105 ℃ for 3h, finally cooling to 100 ℃ and carrying out vacuum degassing for 20min, decoloring, dewatering and filtering to obtain castor oil glycerol polyoxyethylene ether;
s2, filling castor oil polyoxyethylene ether into a three-neck flask with a stirrer, a spherical condenser and a thermometer, then starting the stirrer, slowly adding phosphorus pentoxide, wherein the molar ratio of hydrogenated castor oil to phosphorus pentoxide is 1:0.75, the charging time is 1.5h (1-2 h is proper), heating to 85 ℃, preserving the heat for 4h, then adding 100g of water for hydrolysis for 2.5h (2-3 h), and finally adding a trimethyl ethyl ammonium hydroxide aqueous solution (1 mol/L) for neutralization at 55 ℃ (50-60 ℃ is proper), thus obtaining the castor oil polyoxyethylene ether-phosphate composition with the total mass of 1 kg+/-50 g.
Example 11
The difference from example 10 is that the molar ratio of glycerol to hydrogenated castor oil is 1:1.
example 12
The difference from example 10 is that the molar ratio of glycerol to hydrogenated castor oil is 1:2.
comparative example
Comparative example 1
The difference from example 1 is that phosphorus pentoxide is no longer added to S2.
Performance test
Detection method
1. Elongation at break test
Three samples of high strength polypropylene staple fibers were taken from examples 1-12 and comparative example 1, respectively, and the samples were then tested for breaking strength by reference to GB/T14337-1993 method for test of breaking Strength and elongation at break of synthetic staple fibers, and averaged.
2. Antistatic Performance test
Three high-strength polypropylene staple fiber samples were taken from examples 1 to 12 and comparative example 1, respectively, and then the specific resistance values of the samples were measured by a YG321 fiber specific resistance meter, and an average value was taken.
The test data of examples 1 to 12 and comparative example 1 are shown in Table 2.
TABLE 2 detection data sheet for examples 1-12 and comparative example 1
| Breaking strength (g/denier) | Specific resistance value (10) 7 Ω) | |
| Example 1 | 4.8 | 0.90 |
| Example 2 | 4.5 | 0.91 |
| Example 3 | 4.7 | 0.88 |
| Example 4 | 4.6 | 0.95 |
| Example 5 | 4.9 | 0.89 |
| Example 6 | 5.2 | 0.84 |
| Example 7 | 5.0 | 0.86 |
| Example 8 | 5.1 | 0.84 |
| Example 9 | 5.4 | 0.71 |
| Example 10 | 5.9 | 0.67 |
| Example 11 | 5.7 | 0.69 |
| Example 12 | 5.6 | 0.70 |
| Comparative example 1 | 4.3 | 1.10 |
Referring to examples 1 to 5 and comparative example 1 in combination with Table 2, it can be seen that the specific resistance values of examples 1 to 5 are significantly reduced, and the breaking strength of examples 1 to 5 is significantly improved, compared with comparative example 1, thereby demonstrating that the addition of phosphorus pentoxide to a oiling agent can effectively improve the strength of the polypropylene staple fiber.
The reason for this is that when phosphorus pentoxide is added into the castor oil polyoxyethylene ether, phosphorus pentoxide and the castor oil polyoxyethylene ether will undergo a phosphorus esterification reaction, thereby loading the phosphate group on the castor oil polyoxyethylene ether. The phosphate group is a main functional group of the anionic antistatic agent, and the phosphate is used as the anionic antistatic agent to have a synergistic effect with castor oil polyoxyethylene ether, so that the phosphate has high oil film strength besides excellent smooth wire and antistatic performance after the phosphate and the castor oil polyoxyethylene ether are combined.
Therefore, when the phosphate functional group is added into the castor oil polyoxyethylene ether system, the obtained castor oil polyoxyethylene ether-phosphate composition can further reduce the possibility of phenomena such as yarn, winding roller, yarn breakage and the like of the polypropylene, and indirectly improve the strength of the polypropylene short fiber.
Among them, the specific resistance values of examples 2 to 3 were not substantially changed as compared with example 1, but the breaking strength of examples 2 to 3 was significantly reduced, thereby indicating that the addition amount of ethylene oxide in the castor oil polyoxyethylene ether-phosphate composition had substantially no effect on the antistatic properties of the polypropylene staple fiber, but was related to the strength of the polypropylene staple fiber as a whole.
The reason is that when the addition amount of the ethylene oxide is large, the prepared castor oil polyoxyethylene ether-phosphate composition can obtain higher molecular weight, so that higher heat resistance and oil film strength are obtained, the possibility of phenomena such as yarn breakage, winding, yarn winding and the like of the polypropylene is further reduced, and the strength of the polypropylene short fiber is indirectly improved. However, if the amount of ethylene oxide added is too large, ethylene oxide will hinder the formation of monoester, but will affect the antistatic properties of the polypropylene staple fiber, resulting in a slight decrease in the strength of the polypropylene staple fiber.
Whereas the specific resistance of example 4 was significantly improved compared to example 1, the breaking strength of example 4 was significantly reduced. The specific resistance of example 5 was slightly lowered, and the breaking strength of example 5 was slightly raised, thus indicating that the addition amount of phosphorus pentoxide had an effect on both the antistatic properties and the breaking strength of the polypropylene staple fibers.
The reason for this is that when the molar ratio of hydrogenated castor oil, ethylene oxide and phosphorus pentoxide is used in example 1, the castor oil polyoxyethylene ether-phosphate composition prepared will obtain more monoesters with specific gravity, and the monoesters can promote the castor oil polyoxyethylene ether-phosphate composition to obtain more excellent antistatic performance.
Referring to examples 1 and 6-8, and referring to Table 2, it can be seen that, compared with example 1, the specific resistance of examples 6-8 is significantly reduced, and the breaking strength of examples 6-8 is significantly improved, so that the temperature raising and heat preserving operation before the hydrolysis operation can effectively improve the antistatic performance and breaking strength of the polypropylene staple fiber. The reason is that the temperature rising and maintaining operation before the hydrolysis operation can effectively increase the monoester content in the castor oil polyoxyethylene ether-phosphate composition.
Compared with example 6, the specific resistance values of examples 7-8 are relatively high, and the breaking strength of examples 7-8 is relatively low, so that the fact that the content of monoester in the castor oil polyoxyethylene ether-phosphate composition is relatively high when the data of example 6 are adopted in the heating and heat preservation operation before the hydrolysis operation is shown, the possibility that filaments of the polypropylene staple fibers break is effectively reduced, and the strength of the polypropylene staple fibers is indirectly improved.
Referring to example 6 and example 9 in combination with Table 2, it can be seen that the specific resistance of example 9 is significantly reduced, and the breaking strength of example 9 is significantly improved, compared with example 6, thereby demonstrating that the antistatic performance and strength of the polypropylene staple fiber can be significantly improved by replacing the aqueous solution of potassium hydroxide with the aqueous solution of trimethyl ethylammonium hydroxide of the same concentration.
The reason for this is that methyltriethylammonium hydroxide is a quaternary ammonium base which is readily soluble in water and strongly basic, and therefore methyltriethylammonium hydroxide can also be used for neutralization of castor oil polyoxyethylene ether-phosphate compositions.
Furthermore, after neutralization, the quaternary ammonium salt groups in the methyltriethylammonium hydroxide can also be loaded into the castor oil polyoxyethylene ether-phosphate composition. The quaternary ammonium salt group belongs to the functional group of the cationic antistatic agent, and the cationic antistatic agent has the most excellent antistatic effect, so that the antistatic performance of the castor oil polyoxyethylene ether-phosphate composition is further improved.
Referring to examples 9-12 in combination with Table 2, it can be seen that the specific resistance values of examples 10-12 were slightly decreased and the breaking strength of examples 10-12 was slightly increased relative to example 9, thus demonstrating that the addition of glycerol effectively improved the antistatic properties and strength of the polypropylene staple fibers.
The reason is that the addition of the glycerol can promote the castor oil polyoxyethylene ether-phosphate composition to additionally contain the glycerol group, and the glycerol group can promote the castor oil polyoxyethylene ether-phosphate composition to have better hydrophilicity, so that the antistatic performance of the castor oil polyoxyethylene ether-phosphate composition is further improved.
Whereas examples 11-12 have a relatively large specific resistance value relative to example 10, examples 11-12 have a relatively small breaking strength, thus demonstrating that the glycerol groups can be more efficiently loaded in the castor oil polyoxyethylene ether-phosphate composition when the molar ratio of glycerol to hydrogenated castor oil is the ratio of example 10.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. The preparation process of the high-strength polypropylene short fiber is characterized by comprising the following steps of:
step one, placing the polypropylene fiber forming slices and the additive into a temperature of 110-130 ℃ for preheating, continuously stirring for 20-40min, and then cooling. Drying at 120-140 ℃ for 3-4 hours to obtain a mixed master batch;
step two, conveying the mixed master batch to a screw extruder, compacting and plasticizing, melting by a screw, filtering by a filter, and then entering a melt pipeline;
step three, sequentially performing extrusion spinning, cooling, oiling, drafting, crimping, heat setting, cutting and packaging to obtain high-strength polypropylene staple fibers;
wherein, during oiling operation, the polypropylene oiling agent is selected from castor oil polyoxyethylene ether-phosphate ester composition.
2. The process for preparing high-strength polypropylene staple fibers according to claim 1, wherein the castor oil polyoxyethylene ether-phosphate composition comprises the following raw materials: hydrogenated castor oil, ethylene oxide, phosphorus pentoxide, catalysts and bases;
the molar ratio of the hydrogenated castor oil to the ethylene oxide to the phosphorus pentoxide is 1: (70-90): (0.5-1), the catalyst is added in an amount of 2% of the total mass, and the base adjusts the castor oil polyoxyethylene ether-phosphate composition to ph=8.
3. The process for preparing high-strength polypropylene staple fiber according to claim 2, wherein the process for preparing the castor oil polyoxyethylene ether-phosphate composition comprises the following steps:
s1, mixing hydrogenated castor oil with a catalyst, stirring, heating and dehydrating, adding ethylene oxide, heating for reaction, and finally cooling, degassing, decoloring and filtering to obtain castor oil polyoxyethylene ether;
s2, slowly adding phosphorus pentoxide into the castor oil polyoxyethylene ether for 1-2h, then adding quantitative water for hydrolysis for 2-3h, and finally adding alkali for neutralization at 50-60 ℃ to obtain the castor oil polyoxyethylene ether-phosphate composition.
4. The process for preparing high-strength polypropylene staple fiber according to claim 2, wherein: in S2, after the phosphorus pentoxide is added, firstly heating to 80-90 ℃, carrying out heat preservation reaction for 3-5h, and then carrying out hydrolysis.
5. The process for preparing high-strength polypropylene staple fiber according to claim 2, wherein: the base is aqueous methyl triethyl ammonium hydroxide.
6. The process for preparing high-strength polypropylene staple fiber according to claim 2, wherein: the castor oil polyoxyethylene ether-phosphate composition also comprises glycerin, wherein the mol ratio of the glycerin to the hydrogenated castor oil is 1: (1-2).
7. The process for preparing high-strength polypropylene staple fiber according to claim 6, wherein: the molar ratio of the hydrogenated castor oil to the glycerol to the ethylene oxide to the phosphorus pentoxide is 1:1.5:8:0.75.
8. the process for preparing high-strength polypropylene staple fiber according to claim 7, wherein the process for preparing the castor oil polyoxyethylene ether-phosphate composition comprises the following steps:
s1, mixing hydrogenated castor oil, glycerol and concentrated sulfuric acid with the total mass of 3%, then preserving heat at 100-110 ℃ for 2-3 hours, then mixing with a catalyst, stirring, heating and dehydrating, then adding ethylene oxide, heating and reacting, and finally cooling, degassing, decolorizing and filtering to obtain castor oil glycerol polyoxyethylene ether;
s2, slowly adding phosphorus pentoxide into the castor oil glycerol polyoxyethylene ether for 1-2h, then heating to 80-90 ℃, carrying out heat preservation reaction for 3-5h, then adding quantitative water for hydrolysis for 2-3h, and finally adding a methyl triethyl ammonium hydroxide aqueous solution for neutralization at 50-60 ℃ to obtain the castor oil polyoxyethylene ether-phosphate composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310184515.0A CN115992399A (en) | 2023-03-01 | 2023-03-01 | Preparation process of high-strength polypropylene staple fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310184515.0A CN115992399A (en) | 2023-03-01 | 2023-03-01 | Preparation process of high-strength polypropylene staple fibers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115992399A true CN115992399A (en) | 2023-04-21 |
Family
ID=85992112
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310184515.0A Pending CN115992399A (en) | 2023-03-01 | 2023-03-01 | Preparation process of high-strength polypropylene staple fibers |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115992399A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212299A (en) * | 1997-09-24 | 1999-03-31 | 山东虎山实业集团有限公司 | Process for producing fine denier polypropylene fiber short-staple |
| CN101046059A (en) * | 2007-04-12 | 2007-10-03 | 苏州大学 | Cationic polypropylene spinning oil prepn |
| CN101279984A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Alkyl phenol sulfonic polyoxyethylene ether phosphate salt and preparation thereof |
| CN101886334A (en) * | 2009-05-15 | 2010-11-17 | 中国石油天然气股份有限公司 | Oil for polypropylene spinning |
| CN105685056A (en) * | 2016-03-22 | 2016-06-22 | 江西巴菲特化工有限公司 | 50 percent of difenoconazole-propiconazole emulsion in water and preparation method thereof |
| CN106978726A (en) * | 2017-04-25 | 2017-07-25 | 上海新浦特种助剂有限公司 | A kind of polypropylene fiber spinning oil |
| CN108866652A (en) * | 2018-08-24 | 2018-11-23 | 湖北博韬合纤有限公司 | A kind of processing method of thick denier polypropylene short fiber |
| CN114574985A (en) * | 2022-03-25 | 2022-06-03 | 湖北博韬合纤有限公司 | Production process of regenerated polypropylene short fiber |
-
2023
- 2023-03-01 CN CN202310184515.0A patent/CN115992399A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1212299A (en) * | 1997-09-24 | 1999-03-31 | 山东虎山实业集团有限公司 | Process for producing fine denier polypropylene fiber short-staple |
| CN101279984A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Alkyl phenol sulfonic polyoxyethylene ether phosphate salt and preparation thereof |
| CN101046059A (en) * | 2007-04-12 | 2007-10-03 | 苏州大学 | Cationic polypropylene spinning oil prepn |
| CN101886334A (en) * | 2009-05-15 | 2010-11-17 | 中国石油天然气股份有限公司 | Oil for polypropylene spinning |
| CN105685056A (en) * | 2016-03-22 | 2016-06-22 | 江西巴菲特化工有限公司 | 50 percent of difenoconazole-propiconazole emulsion in water and preparation method thereof |
| CN106978726A (en) * | 2017-04-25 | 2017-07-25 | 上海新浦特种助剂有限公司 | A kind of polypropylene fiber spinning oil |
| CN108866652A (en) * | 2018-08-24 | 2018-11-23 | 湖北博韬合纤有限公司 | A kind of processing method of thick denier polypropylene short fiber |
| CN114574985A (en) * | 2022-03-25 | 2022-06-03 | 湖北博韬合纤有限公司 | Production process of regenerated polypropylene short fiber |
Non-Patent Citations (1)
| Title |
|---|
| 沈一丁: "《表面活性剂原理与应用》", vol. 1, 中国轻工业出版社, pages: 268 - 270 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100378267C (en) | Oil agent used for polyester industrial filament | |
| CN101929068A (en) | Polyester POY spinning finish and production method thereof | |
| CN111206427A (en) | High-temperature oil agent for polyester industrial yarn and preparation method thereof | |
| CN110923844B (en) | Preparation method of spandex easy to unwind | |
| CN113969436A (en) | Chinlon spinning oil and preparation method thereof | |
| CN108505342A (en) | It is a kind of continuously to spin viscose filament yarn finish and its preparation method and application | |
| US2676924A (en) | Textile lubricant | |
| CN113774510B (en) | Preparation method of expanded graphite polyester flame-retardant fabric | |
| CN115992399A (en) | Preparation process of high-strength polypropylene staple fibers | |
| CN115651177B (en) | Hydrophilic polyester granules and preparation method thereof | |
| CN113584639B (en) | Polyester fully drawn yarn oiling agent | |
| CN107574502B (en) | Preparation method of superfine denier polyester FDY (fully drawn yarn) for high-density fabric | |
| CN112176722B (en) | Poly (p-phenylene benzobisoxazole) fiber spinning oil and preparation method thereof | |
| CN102619084B (en) | Polypropylene spinning oil composition for cigarette and preparation method thereof | |
| CN115058789A (en) | Preparation method of flexible antistatic polylactic acid fiber | |
| CN114351450A (en) | Oil agent for semi-continuous spinning viscose filament yarn and preparation method and application thereof | |
| CN111321597B (en) | Modified polyester slurry and preparation method thereof | |
| CN114150403A (en) | PBS spinning oil, production method and application thereof | |
| CN115595685B (en) | Hydrophilic polyester fiber and preparation method and application thereof | |
| US3381075A (en) | Process for preparation of viscose regenerated cellulose fibers | |
| CN112694609B (en) | Surfactant for high-temperature level dyeing of polyester fibers and preparation method thereof | |
| KR102576568B1 (en) | Spinning oil composition for polyester full draw yarns, Spinning oil using the same and Manufacturing method thereof | |
| CN116752251A (en) | Ultra-high-speed spinning FDY (fully drawn yarn) oiling agent and preparation method thereof | |
| CN106884220A (en) | FDY high strength polyester filament yarns | |
| CN113913957A (en) | Processing method for online adding flame-retardant anti-dripping polyester fiber in melt direct spinning |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20230421 |