CN112376123A - Microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and preparation method thereof - Google Patents
Microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and preparation method thereof Download PDFInfo
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- CN112376123A CN112376123A CN202011213927.5A CN202011213927A CN112376123A CN 112376123 A CN112376123 A CN 112376123A CN 202011213927 A CN202011213927 A CN 202011213927A CN 112376123 A CN112376123 A CN 112376123A
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- ammonium polyphosphate
- molecular weight
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- weight polyethylene
- polyethylene fiber
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- 239000004114 Ammonium polyphosphate Substances 0.000 title claims abstract description 50
- 235000019826 ammonium polyphosphate Nutrition 0.000 title claims abstract description 50
- 229920001276 ammonium polyphosphate Polymers 0.000 title claims abstract description 50
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 title claims abstract description 43
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 title claims abstract description 43
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000003063 flame retardant Substances 0.000 title claims abstract description 33
- 239000000835 fiber Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 22
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 17
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 19
- 239000008098 formaldehyde solution Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 238000009987 spinning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 8
- 238000002791 soaking Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical group C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/046—Making microcapsules or microballoons by physical processes, e.g. drying, spraying combined with gelification or coagulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent 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
- D01F6/46—Monocomponent 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and a preparation method thereof, and the microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber comprises the following component raw materials, wherein the weight ratio of an ultra-high molecular weight polyethylene fiber solution to microencapsulated ammonium polyphosphate is (70-72): 1; the microencapsulated ammonium polyphosphate comprises the following raw materials, wherein the weight ratio of ammonium polyphosphate to ethanol solution to MF prepolymer aqueous solution to dibutyltin dilaurate to hydrochloric acid is (2-4): (15-20): (5-10): (0.3-1): (2-3); the aqueous solution of the MF prepolymer comprises the following raw materials in parts by weight, wherein the weight ratio of melamine to an aqueous solution of formaldehyde to an aqueous solution of sodium carbonate is (8-12) to (3-4) to (8-10); the LOI value of the flame retardant reaches more than 27 percent, and the flame retardant has a very good flame retardant effect.
Description
Technical Field
The invention belongs to the technical field of polyethylene fibers, and particularly relates to a microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and a preparation method thereof.
Background
With the development of science and technology, the requirements of people on textiles are higher and higher. Because of the advantages of light weight, great tensile strength, good impact resistance, good wear resistance and the like, the ultra-high molecular weight polyethylene (UHWMPE) fiber is synthesized with aramid fiber and carbon fiber as three 'high-performance fibers' in the world. The product can be widely applied in the fields of textile, military, agriculture, building and the like. But the flame retardant is poor in flame retardance, the limiting oxygen index is only 17, and the flame retardant belongs to flammable fabrics, which undoubtedly causes great threat to the safety of lives and properties of people.
Chinese patent CN201710787285.1 discloses a preparation method of a flame-retardant ultra-high molecular weight polyethylene fabric, which comprises the following steps:
removing impurities on the surface of the ultra-high molecular weight polyethylene fabric, soaking the ultra-high molecular weight polyethylene fabric in absolute ethyl alcohol or acetone, performing ultrasonic treatment at 40 ℃ for 0.5-1h, and naturally drying;
step two, activating and pretreating the ultra-high molecular weight polyethylene fabric, namely soaking the ultra-high molecular weight polyethylene fabric subjected to impurity removal in a prepared activating solution, mechanically stirring for 3-4 hours at normal temperature, wherein the stirring speed is 150r/min, continuing to soak for 3-4 hours after stirring is finished, and draining the liquid on the fabric for later use after taking out;
step three, preparation of flame retardant liquid: uniformly dispersing a flame retardant into polyethylene glycol 400, adding a proper amount of tetrabutyl titanate, stirring for 0.5h at normal temperature, wherein the stirring speed is 300r/min, and the obtained flame-retardant working solution is a black suspension;
and step four, preparing the flame-retardant ultra-high molecular weight polyethylene fabric, namely soaking the activated ultra-high molecular weight polyethylene fabric in flame-retardant working solution, treating the fabric by adopting a three-soaking three-pressing method, and finally drying the treated fabric for 6 hours at 80 ℃.
The final product is obtained by modifying the ultra-high molecular weight polyethylene and dispersing the flame retardant, the limiting oxygen index is 24.0, and the flame retardant grade can be achieved.
Disclosure of Invention
The invention aims to solve the technical problem of providing a microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and a preparation method thereof, wherein the LOI value reaches more than 27 percent, and the microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber has a very good flame-retardant effect.
The invention relates to a microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber, which comprises the following raw materials of an ultra-high molecular weight polyethylene fiber solution and microencapsulated ammonium polyphosphate, wherein the weight ratio of the ultra-high molecular weight polyethylene fiber solution to the microencapsulated ammonium polyphosphate is (70-72): 1;
the microencapsulated ammonium polyphosphate comprises the following raw materials of ammonium polyphosphate, ethanol solution, MF prepolymer aqueous solution, dibutyltin dilaurate and hydrochloric acid, wherein the weight ratio of the ammonium polyphosphate to the ethanol solution to the MF prepolymer aqueous solution to the dibutyltin dilaurate to the hydrochloric acid is (2-4): 15-20): 5-10: (0.3-1): 2-3);
the aqueous solution of the MF prepolymer comprises the following raw materials in parts by weight, namely melamine, a formaldehyde solution and a sodium carbonate aqueous solution, wherein the weight ratio of the melamine to the formaldehyde solution to the sodium carbonate aqueous solution is (8-12) to (3-4) to (8-10).
The weight ratio of ammonium polyphosphate, ethanol solution, MF prepolymer aqueous solution, dibutyltin dilaurate and hydrochloric acid was 3:17:7:0.6: 2.6.
The weight ratio of the melamine to the formaldehyde solution to the sodium carbonate aqueous solution is 10:3.2: 8.3.
The mass concentration of the ultrahigh molecular weight polyethylene fiber solution (solvent is tetrahydronaphthalene) is 18.9-19.1%, the mass concentration of the formaldehyde solution is 37%, the mass concentration of the sodium carbonate aqueous solution is 10%, the mass concentration of the ethanol solution is 27.8-34.0%, and the mass concentration of the hydrochloric acid is 9.0-11.0%.
The invention provides a preparation method of an encapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber, which comprises the steps of dissolving cyanuric chloride in a formaldehyde solution, reacting for a period of time at the temperature of 30-40 ℃, adding a sodium carbonate aqueous solution, adjusting the pH value to 8.2-8.5, adjusting the temperature to 80-83 ℃, stirring, and reacting for a period of time in a heat preservation manner to obtain an MF prepolymer aqueous solution;
dispersing ammonium polyphosphate into an ethanol solution, adding an MF prepolymer aqueous solution, then adding dibutyltin dilaurate, stirring, heating to 90-100 ℃, gradually dropwise adding hydrochloric acid in the process, adjusting the pH value of the system to 4-6, keeping the temperature for a period of time, cooling to normal temperature, washing, and drying to obtain microencapsulated ammonium polyphosphate;
mixing the ultra-high molecular weight polyethylene fiber solution and the microencapsulated ammonium polyphosphate, stirring, heating to 35-38 ℃, preserving heat to form a spinning fluid, extruding by a double-screw extruder, extracting, and stretching to obtain the microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber.
Dissolving cyanuric chloride in formaldehyde solution, and reacting at 30-40 deg.C for 10-15 min. Adjusting the temperature to 80-83 ℃, stirring at the speed of 420-. Dibutyl tin dilaurate was added and stirred at a speed of 370-400 rpm. Adjusting the pH value of the system to 4-6, and keeping the temperature for 60-65 min. Stirring and heating to 35-38 deg.C, and maintaining for 2-2.2 h.
The preparation method has the beneficial effects that cyanuric chloride is dissolved in an organic solvent to obtain MF prepolymer; mixing ammonium polyphosphate, MF prepolymer and dibutyltin dilaurate to obtain microencapsulated ammonium polyphosphate, mixing the microencapsulated ammonium polyphosphate with an ultrahigh molecular weight polyethylene solution, and processing to obtain the flame-retardant ultrahigh molecular weight polyethylene fiber with the LOI value of more than 27%.
Detailed Description
Example 1
Preparation method of encapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber
(1) Adding deionized water, MEL (melamine) and formaldehyde solution (37%) into a reaction kettle with stirring and temperature regulating functions, reacting at 30-40 deg.C for 10-15min, and adding 10% Na dropwise2CO3The pH value of the aqueous solution is adjusted to 8.2-8.5. Then, the temperature is gradually adjusted to 80-83 ℃, and stirring (420-.
(2) Uniformly dispersing a certain amount of APP (ammonium polyphosphate) in a corresponding amount of ethanol solution. Then adding a proper amount of MF prepolymer aqueous solution, then adding a certain amount of catalyst DBTDL (dibutyltin dilaurate) and starting stirring (370-400rpm), gradually raising the temperature to a certain temperature (90-100 ℃), gradually dropwise adding hydrochloric acid in the process to adjust the pH value of the system to 4-6, and carrying out heat preservation reaction for 60-65 min. Then cooling to normal temperature, washing and drying to obtain the MFAPP (microencapsulated ammonium polyphosphate).
Formulation (unit kg): MEL: formaldehyde solution: na (Na)2CO3The weight ratio of (A) to (B) is 10:3.2: 8.3. APP: ethanol solution: MF aqueous prepolymer solution: DBTDL: hydrochloric acid 3:17:7:0.6: 2.6.
(3) Blending ultra-high molecular weight polyethylene solution and microencapsulated ammonium polyphosphate
Preparing an ultra-high molecular weight polyethylene solution according to a conventional method, mixing the ultra-high molecular weight polyethylene solution and microencapsulated ammonium polyphosphate in a swelling kettle according to a mass ratio of 70: 1-72: 1, continuously stirring, heating to 35-38 ℃, and preserving heat for 2-2.2 hours to form a spinning fluid, wherein the mass percentage of the ultra-high molecular weight polyethylene is 18.9-19.1%; spinning fluid is injected into the jelly precursor obtained by the double-screw extruder from the blanking kettle; and then the encapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber with the flame-retardant function is prepared through the processes of extraction, super-stretching and the like, wherein the LOI value is 27%.
Comparative example 1
Comparative example 1 differs from example 1 in that step (1) is eliminated and step (2) is: uniformly dispersing a certain amount of APP (ammonium polyphosphate) in a corresponding amount of ethanol solution. Then the appropriate amount of melamine was added, then the amount of catalyst DBTDL (dibutyltin dilaurate) was added and the stirring was turned on (370) and 400rpm), the remaining steps were the same as those of step (2). In the same manner as in example 1 in step (3), the LOI value of the ultra-high molecular weight polyethylene fiber obtained was 15%.
Claims (10)
1. A microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber is characterized by comprising the following component raw materials, ultra-high molecular weight polyethylene fiber solution and microencapsulated ammonium polyphosphate, wherein the weight ratio of the ultra-high molecular weight polyethylene fiber solution to the microencapsulated ammonium polyphosphate is (70-72): 1;
the microencapsulated ammonium polyphosphate comprises the following raw materials of ammonium polyphosphate, ethanol solution, MF prepolymer aqueous solution, dibutyltin dilaurate and hydrochloric acid, wherein the weight ratio of the ammonium polyphosphate to the ethanol solution to the MF prepolymer aqueous solution to the dibutyltin dilaurate to the hydrochloric acid is (2-4): 15-20): 5-10: (0.3-1): 2-3);
the aqueous solution of the MF prepolymer comprises the following raw materials in parts by weight, namely melamine, a formaldehyde solution and a sodium carbonate aqueous solution, wherein the weight ratio of the melamine to the formaldehyde solution to the sodium carbonate aqueous solution is (8-12) to (3-4) to (8-10).
2. The microencapsulated ammonium polyphosphate flame-retardant ultrahigh molecular weight polyethylene fiber as claimed in claim 1, wherein the weight ratio of ammonium polyphosphate, ethanol solution, MF prepolymer aqueous solution, dibutyltin dilaurate and hydrochloric acid is 3:17:7:0.6: 2.6.
3. The microencapsulated ammonium polyphosphate flame-retardant ultrahigh molecular weight polyethylene fiber as claimed in claim 1, wherein the weight ratio of melamine, formaldehyde solution and sodium carbonate aqueous solution is 10:3.2: 8.3.
4. The microencapsulated ammonium polyphosphate flame-retardant ultrahigh molecular weight polyethylene fiber as claimed in claim 1, wherein the mass concentration of the ultrahigh molecular weight polyethylene fiber solution is 18.9 to 19.1%, the mass concentration of the formaldehyde solution is 37%, the mass concentration of the sodium carbonate aqueous solution is 10%, the mass concentration of the ethanol solution is 27.8 to 34.0%, and the mass concentration of the hydrochloric acid is 9.0 to 11.0%.
5. A method for preparing the microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber as claimed in any one of claims 1 to 4, which is characterized in that cyanuric chloride is dissolved in a formaldehyde solution, reacted for a period of time at a temperature of 30 to 40 ℃, added with a sodium carbonate aqueous solution, adjusted to a pH value of 8.2 to 8.5, adjusted to a temperature of 80 to 83 ℃, stirred, and reacted for a period of time under heat preservation to obtain an MF prepolymer aqueous solution;
dispersing ammonium polyphosphate into an ethanol solution, adding an MF prepolymer aqueous solution, then adding dibutyltin dilaurate, stirring, heating to 90-100 ℃, gradually dropwise adding hydrochloric acid in the process, adjusting the pH value of the system to 4-6, keeping the temperature for a period of time, cooling to normal temperature, washing, and drying to obtain microencapsulated ammonium polyphosphate;
mixing the ultra-high molecular weight polyethylene fiber solution and the microencapsulated ammonium polyphosphate, stirring, heating to 35-38 ℃, preserving heat to form a spinning fluid, extruding by a double-screw extruder, extracting, and stretching to obtain the microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber.
6. The process according to claim 5, wherein cyanuric chloride is dissolved in a formaldehyde solution and reacted at a temperature of 30 to 40 ℃ for 10 to 15 minutes.
7. The process according to claim 5, wherein the temperature is adjusted to 80-83 ℃, the stirring is carried out at a speed of 420-450rpm, and the temperature is maintained for 20-25 min.
8. The process according to claim 5, wherein dibutyltin dilaurate is added and the mixture is stirred at a speed of 370 rpm and 400 rpm.
9. The preparation process as claimed in claim 5, wherein the pH of the system is adjusted to 4-6 and the temperature is maintained for 60-65 min.
10. The process according to any one of claims 5 to 9, wherein the temperature is raised to 35 to 38 ℃ with stirring, and the holding time is 2 to 2.2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011213927.5A CN112376123A (en) | 2020-11-04 | 2020-11-04 | Microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011213927.5A CN112376123A (en) | 2020-11-04 | 2020-11-04 | Microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and preparation method thereof |
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| CN112376123A true CN112376123A (en) | 2021-02-19 |
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2020
- 2020-11-04 CN CN202011213927.5A patent/CN112376123A/en active Pending
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| CN1712444A (en) * | 2005-07-12 | 2005-12-28 | 南京航空航天大学 | Non-halogen fire-retardant polypropylene and production thereof |
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| Title |
|---|
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Application publication date: 20210219 |