CN112662141A - Preparation method of flame-retardant hydrolysis-resistant PBT material - Google Patents
Preparation method of flame-retardant hydrolysis-resistant PBT material Download PDFInfo
- Publication number
- CN112662141A CN112662141A CN202011435710.9A CN202011435710A CN112662141A CN 112662141 A CN112662141 A CN 112662141A CN 202011435710 A CN202011435710 A CN 202011435710A CN 112662141 A CN112662141 A CN 112662141A
- Authority
- CN
- China
- Prior art keywords
- flame
- retardant
- hydrolysis
- preparation
- resistant
- 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
- 239000003063 flame retardant Substances 0.000 title claims abstract description 71
- 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 65
- 239000000463 material Substances 0.000 title claims abstract description 50
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 44
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000000835 fiber Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000001746 injection moulding Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000007605 air drying Methods 0.000 claims abstract description 9
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 9
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001125 extrusion Methods 0.000 claims abstract description 9
- 239000008187 granular material Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 35
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 30
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical group CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 27
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 235000010413 sodium alginate Nutrition 0.000 claims description 9
- 239000000661 sodium alginate Substances 0.000 claims description 9
- 229940005550 sodium alginate Drugs 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 239000000314 lubricant Substances 0.000 claims description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000008118 PEG 6000 Substances 0.000 claims description 5
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 229920001707 polybutylene terephthalate Polymers 0.000 description 43
- 230000003078 antioxidant effect Effects 0.000 description 6
- 238000007792 addition Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 description 1
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 description 1
- -1 Polybutylene terephthalate Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Injection Moulding Of Plastics Or The Like (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention provides a preparation method of a flame-retardant hydrolysis-resistant PBT material. The preparation steps are as follows: putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h; uniformly mixing the dried PBT resin, 10% of flame retardant, 3% of antimony powder, 1-2% of hydrolysis resistant agent and other processing aids in a high-speed mixer; extruding and granulating the mixed materials, wherein the extrusion temperature is 220-240 ℃, the rotating speed of a host is 350rpm, 20-30% of metal fibers are added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃; and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material. The flame-retardant hydrolysis-resistant PBT material prepared by the invention has the advantages of good mechanical property, good flame-retardant effect and strong hydrolysis resistance.
Description
Technical Field
The invention relates to the field of new materials, and particularly relates to a preparation method of a flame-retardant hydrolysis-resistant PBT material.
Background
Polybutylene terephthalate (PBT) is one of five common engineering plastics, is crystalline thermoplastic polyester, has the characteristics of excellent mechanical strength, heat resistance, electric insulativity, processability, chemical solvent resistance and the like, and is widely applied to the fields of electronic and electric appliances, automobiles and the like. With the increasingly wide application of the PBT material, the requirements on various properties of the material are higher and higher, and the flame-retardant reinforced modified PBT material is one of the main modification directions in the market at present and can be used in a plurality of industries such as automobiles, illumination, household appliances, electronics and electricity. However, because the PBT resin is a polyester material and contains ester bonds in molecules, the PBT resin is very easy to hydrolyze in a humid environment above the glass transition temperature of the PBT resin, so that the performance of the PBT resin is greatly reduced, and the use of the PBT resin is greatly limited, so that the improvement of the hydrolysis resistance of the PBT material has great research value.
During the processing of modified plastics, the interface between various additives such as flame retardants, mechanical reinforcing components, etc. and the resin also affects the hydrolysis resistance of the material. Therefore, the PBT material which has good flame retardance and hydrolysis resistance and keeps the mechanical property has important significance.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a preparation method of a flame-retardant hydrolysis-resistant PBT material, and the prepared material has good mechanical property, good flame-retardant effect and strong hydrolysis resistance.
The technical scheme is as follows: a preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of flame retardant, 3% of antimony powder, 1-2% of hydrolysis resistant agent and other processing aids in a high-speed mixer;
(3) extruding and granulating the mixed materials, wherein the extrusion temperature is 220-240 ℃, the rotating speed of a host is 350rpm, 20-30% of metal fibers are added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
Further, the flame retardant is a modified sodium alginate flame retardant or a modified magnesium hydroxide flame retardant.
Further, the metal fiber is one or a compound of more than two of stainless steel fiber, aluminum fiber, copper fiber, nickel fiber and copper alloy fiber.
Further, the preparation method of the modified sodium alginate flame retardant comprises the following steps:
1) adding a polyethylene glycol solution with the mass fraction of 0.02% into a sodium alginate solution with the mass fraction of 0.02%, and uniformly mixing;
2) adding calcium chloride solution to form a film, and repeatedly washing with sodium chloride solution;
3) and naturally drying to obtain the modified sodium alginate flame retardant.
Further, the preparation method of the modified magnesium hydroxide flame retardant comprises the following steps:
1) taking 200mL of magnesium nitrate solution and 200mL of sodium hydroxide solution respectively, wherein the concentration ratio of magnesium nitrate to sodium hydroxide is 1: 2;
2) mixing a magnesium nitrate solution and PEG6000, adding into a crystallization reactor, stirring, and then dropwise adding a sodium hydroxide solution for 30 min;
3) after the dripping is finished, stirring and filtering are continuously carried out, and filter cakes are washed for 3-4 times by deionized water;
4) washing with anhydrous ethanol for 1-2 times, drying at 120 deg.C for 2-3 hr, and grinding to obtain modified magnesium hydroxide fire retardant.
Further, the other processing aids are antioxidants, lubricants and ultraviolet-resistant agents.
Has the advantages that:
1. the modified sodium alginate flame retardant or the modified magnesium hydroxide flame retardant is adopted, so that the UL94 flame retardant grade is kept at V-0, and the mechanical property is kept unchanged.
2. The invention adopts the mechanical property of the metal fiber reinforced material, wherein the effect of the stainless steel fiber is the best.
3. The sodium alginate is a high molecular linear polymer which is formed by connecting alpha-L-guluronic acid and beta-D-mannuronic acid through 1-4 glycosidic bonds and consists of GG, MM and GM segments with different proportions. After the modified sodium alginate is modified, the viscosity of the sodium alginate is increased, when the temperature is increased, the internal structure of the sodium alginate is changed, hydroxyl-OH and oxygen are broken to form a group structure without a certain shape, the sodium alginate and the hydroxyl-OH are easy to adhere to each other, and the modified sodium alginate has a good flame retardant effect.
Detailed Description
Example 1
A preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of modified sodium alginate flame retardant, 3% of antimony powder, 1% of hydrolysis resistant agent, antioxidant, lubricant and ultraviolet resistant agent in a high-speed mixer;
(3) extruding and granulating the mixed materials, wherein the extrusion temperature is 220 ℃, the rotating speed of a main machine is 350rpm, 20 percent of stainless steel fiber is added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
The preparation method of the modified sodium alginate flame retardant comprises the following steps:
1) adding a polyethylene glycol solution with the mass fraction of 0.02% into a sodium alginate solution with the mass fraction of 0.02%, and uniformly mixing;
2) adding calcium chloride solution to form a film, and repeatedly washing with sodium chloride solution;
3) and naturally drying to obtain the modified sodium alginate flame retardant.
Example 2
A preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of modified sodium alginate flame retardant, 3% of antimony powder, 1.5% of hydrolysis resistant agent, antioxidant, lubricant and ultraviolet resistant agent in a high-speed mixer;
(3) extruding and granulating the mixed materials, wherein the extrusion temperature is 230 ℃, the rotating speed of a main machine is 350rpm, 25 percent of aluminum fiber is added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
The preparation method of the modified sodium alginate flame retardant comprises the following steps:
1) adding a polyethylene glycol solution with the mass fraction of 0.02% into a sodium alginate solution with the mass fraction of 0.02%, and uniformly mixing;
2) adding calcium chloride solution to form a film, and repeatedly washing with sodium chloride solution;
3) and naturally drying to obtain the modified sodium alginate flame retardant.
Example 3
A preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of modified sodium alginate flame retardant, 3% of antimony powder, 2% of hydrolysis resistant agent, antioxidant, lubricant and ultraviolet resistant agent in a high-speed mixer;
(3) extruding and granulating the mixed material, wherein the extrusion temperature is 240 ℃, the rotating speed of a main machine is 350rpm, 30 percent of copper fiber is added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
The preparation method of the modified sodium alginate flame retardant comprises the following steps:
1) adding a polyethylene glycol solution with the mass fraction of 0.02% into a sodium alginate solution with the mass fraction of 0.02%, and uniformly mixing;
2) adding calcium chloride solution to form a film, and repeatedly washing with sodium chloride solution;
3) and naturally drying to obtain the modified sodium alginate flame retardant.
Example 4
A preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of modified magnesium hydroxide flame retardant, 3% of antimony powder, 1% of hydrolysis resistant agent, antioxidant, lubricant and ultraviolet resistant agent in a high-speed mixer;
(3) extruding and granulating the mixed material, wherein the extrusion temperature is 220 ℃, the rotating speed of a main machine is 350rpm, 20 percent of nickel fiber is added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
The preparation method of the modified magnesium hydroxide flame retardant comprises the following steps:
1) taking 200mL of magnesium nitrate solution and 200mL of sodium hydroxide solution respectively, wherein the concentration ratio of magnesium nitrate to sodium hydroxide is 1: 2;
2) mixing a magnesium nitrate solution and PEG6000, adding into a crystallization reactor, stirring, and then dropwise adding a sodium hydroxide solution for 30 min;
3) after the dropwise addition, stirring and filtering are continued, and a filter cake is washed for 3 times by deionized water;
4) washing with anhydrous ethanol for 1 time, drying at 120 deg.C for 2 hr, and grinding to obtain modified magnesium hydroxide fire retardant.
Example 5
A preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of modified magnesium hydroxide flame retardant, 3% of antimony powder, 1.5% of hydrolysis resistant agent, antioxidant, lubricant and ultraviolet resistant agent in a high-speed mixer;
(3) extruding and granulating the mixed material, wherein the extrusion temperature is 230 ℃, the rotating speed of a main machine is 350rpm, 25 percent of copper alloy fiber is added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
The preparation method of the modified magnesium hydroxide flame retardant comprises the following steps:
1) taking 200mL of magnesium nitrate solution and 200mL of sodium hydroxide solution respectively, wherein the concentration ratio of magnesium nitrate to sodium hydroxide is 1: 2;
2) mixing a magnesium nitrate solution and PEG6000, adding into a crystallization reactor, stirring, and then dropwise adding a sodium hydroxide solution for 30 min;
3) after the dropwise addition, stirring and filtering are continued, and a filter cake is washed for 4 times by deionized water;
4) washing with anhydrous ethanol for 2 times, drying at 120 deg.C for 2.5h, and grinding to obtain modified magnesium hydroxide fire retardant.
Example 6
A preparation method of a flame-retardant hydrolysis-resistant PBT material comprises the following steps:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of modified magnesium hydroxide flame retardant, 3% of antimony powder, 2% of hydrolysis resistant agent, antioxidant, lubricant and ultraviolet resistant agent in a high-speed mixer;
(3) extruding and granulating the mixed materials, wherein the extrusion temperature is 240 ℃, the rotating speed of a main machine is 350rpm, 30 percent of stainless steel fiber is added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
The preparation method of the modified magnesium hydroxide flame retardant comprises the following steps:
1) taking 200mL of magnesium nitrate solution and 200mL of sodium hydroxide solution respectively, wherein the concentration ratio of magnesium nitrate to sodium hydroxide is 1: 2;
2) mixing a magnesium nitrate solution and PEG6000, adding into a crystallization reactor, stirring, and then dropwise adding a sodium hydroxide solution for 30 min;
3) after the dropwise addition, stirring and filtering are continued, and a filter cake is washed for 4 times by deionized water;
4) washing with anhydrous ethanol for 2 times, drying at 120 deg.C for 3 hr, and grinding to obtain modified magnesium hydroxide fire retardant.
And (3) performance testing:
the tensile property IS tested according to IS0527/2, and the tensile rate IS 50 mm/min; the bending performance IS tested according to IS0178, the bending rate IS 2mm/min, and the span wei IS 64 mm; notched impact strength tests were carried out in accordance with ISO 180.
The hydrolysis resistance of the material is tested by adopting an accelerated hydrolysis experiment method, the PBT material obtained by injection molding is immersed in a digital display constant temperature water bath kettle filled with water, the temperature of the water bath kettle is regulated to be constant at 85 ℃, and sampling is carried out after 10 days for carrying out related performance tests. The retention rate of the mechanical properties of the material after water boiling is calculated according to the following formula.
The properties of the examples are as follows:
Claims (6)
1. the preparation method of the flame-retardant hydrolysis-resistant PBT material is characterized by comprising the following steps of:
(1) putting the PBT resin into a forced air drying oven, and drying at the temperature of 140 ℃ for 4 h;
(2) uniformly mixing the dried PBT resin, 10% of flame retardant, 3% of antimony powder, 1-2% of hydrolysis resistant agent and other processing aids in a high-speed mixer;
(3) extruding and granulating the mixed materials, wherein the extrusion temperature is 220-240 ℃, the rotating speed of a host is 350rpm, 20-30% of metal fibers are added in a side feeding mode, and the granules are dried for 4 hours at the temperature of 140 ℃;
(4) and injection molding by an injection molding machine to obtain the flame-retardant hydrolysis-resistant PBT material.
2. The preparation method of the flame-retardant hydrolysis-resistant PBT material according to claim 1, wherein the flame retardant is a modified sodium alginate flame retardant or a modified magnesium hydroxide flame retardant.
3. The preparation method of the flame-retardant hydrolysis-resistant PBT material according to claim 1, wherein the metal fiber is one or a mixture of two or more of stainless steel fiber, aluminum fiber, copper fiber, nickel fiber and copper alloy fiber.
4. The preparation method of the flame-retardant hydrolysis-resistant PBT material according to claim 2, wherein the preparation method of the modified sodium alginate flame retardant comprises the following steps:
1) adding a polyethylene glycol solution with the mass fraction of 0.02% into a sodium alginate solution with the mass fraction of 0.02%, and uniformly mixing;
2) adding calcium chloride solution to form a film, and repeatedly washing with sodium chloride solution;
3) and naturally drying to obtain the modified sodium alginate flame retardant.
5. The preparation method of the flame-retardant hydrolysis-resistant PBT material according to claim 2, wherein the modified magnesium hydroxide flame retardant is prepared by the following steps:
1) taking 200mL of magnesium nitrate solution and 200mL of sodium hydroxide solution respectively, wherein the concentration ratio of magnesium nitrate to sodium hydroxide is 1: 2;
2) mixing a magnesium nitrate solution and PEG6000, adding into a crystallization reactor, stirring, and then dropwise adding a sodium hydroxide solution for 30 min;
3) after the dripping is finished, stirring and filtering are continuously carried out, and filter cakes are washed for 3-4 times by deionized water;
4) washing with anhydrous ethanol for 1-2 times, drying at 120 deg.C for 2-3 hr, and grinding to obtain modified magnesium hydroxide fire retardant.
6. The method for preparing the flame-retardant hydrolysis-resistant PBT material according to claim 1, wherein the other processing aids are antioxidants, lubricants and anti-UV agents.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011435710.9A CN112662141A (en) | 2020-12-10 | 2020-12-10 | Preparation method of flame-retardant hydrolysis-resistant PBT material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011435710.9A CN112662141A (en) | 2020-12-10 | 2020-12-10 | Preparation method of flame-retardant hydrolysis-resistant PBT material |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112662141A true CN112662141A (en) | 2021-04-16 |
Family
ID=75401753
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011435710.9A Pending CN112662141A (en) | 2020-12-10 | 2020-12-10 | Preparation method of flame-retardant hydrolysis-resistant PBT material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112662141A (en) |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1753929A (en) * | 2003-02-28 | 2006-03-29 | 三菱化学株式会社 | Polybutylene terephthalate and polybutylene terephthalate composition |
CN101165093A (en) * | 2006-10-16 | 2008-04-23 | 上海金发科技发展有限公司 | High hydrolysis resistance anti-flaming enhanced polybutylene terephthalate composition and preparation method thereof |
CN103140543A (en) * | 2010-09-29 | 2013-06-05 | 胜技高分子株式会社 | Polybutylene terephthalate resin film |
CN103525030A (en) * | 2012-07-02 | 2014-01-22 | 青岛欣展塑胶有限公司 | High-performance flame-retardant reinforced hydrolysis-resistant PBT (polybutylene terephthalate) material and preparation method thereof |
CN103694655A (en) * | 2013-12-09 | 2014-04-02 | 方万漂 | Heat-and-humidity-resistant polybutylene terephthalate |
CN104119648A (en) * | 2014-03-31 | 2014-10-29 | 东莞市美塑塑料科技有限公司 | Hydrolysis-resistant low-shrinkage glass fiber reinforced flame-retardant PBT (Polybutylene Terephthalate) and preparation method thereof |
CN110256818A (en) * | 2019-04-30 | 2019-09-20 | 南通开普乐工程塑料有限公司 | A kind of hydrolysis fiber glass reinforced PBT and preparation method thereof |
-
2020
- 2020-12-10 CN CN202011435710.9A patent/CN112662141A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1753929A (en) * | 2003-02-28 | 2006-03-29 | 三菱化学株式会社 | Polybutylene terephthalate and polybutylene terephthalate composition |
CN101165093A (en) * | 2006-10-16 | 2008-04-23 | 上海金发科技发展有限公司 | High hydrolysis resistance anti-flaming enhanced polybutylene terephthalate composition and preparation method thereof |
CN103140543A (en) * | 2010-09-29 | 2013-06-05 | 胜技高分子株式会社 | Polybutylene terephthalate resin film |
CN103525030A (en) * | 2012-07-02 | 2014-01-22 | 青岛欣展塑胶有限公司 | High-performance flame-retardant reinforced hydrolysis-resistant PBT (polybutylene terephthalate) material and preparation method thereof |
CN103694655A (en) * | 2013-12-09 | 2014-04-02 | 方万漂 | Heat-and-humidity-resistant polybutylene terephthalate |
CN104119648A (en) * | 2014-03-31 | 2014-10-29 | 东莞市美塑塑料科技有限公司 | Hydrolysis-resistant low-shrinkage glass fiber reinforced flame-retardant PBT (Polybutylene Terephthalate) and preparation method thereof |
CN110256818A (en) * | 2019-04-30 | 2019-09-20 | 南通开普乐工程塑料有限公司 | A kind of hydrolysis fiber glass reinforced PBT and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
张伟 等: "海藻酸钠阻燃剂防火性能的实验研究", 《北京石油化工学院学报》 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111087782A (en) | Flame-retardant PCABS composition | |
CN103709659A (en) | Glass fiber reinforced PBT/PET alloy material | |
CN112194893B (en) | Hydrolysis-resistant reinforced flame-retardant PA6-POK alloy material and preparation method thereof | |
CN112694708A (en) | Environment-friendly modified ABS (acrylonitrile butadiene styrene) composite plastic and preparation method thereof | |
CN104693701A (en) | Low-warpage halogen-free flame-retardant glass fiber reinforced PBT/AS alloy and preparation method thereof | |
CN108129825B (en) | high-CTI high-heat-resistance halogen-free flame-retardant PC/ABS composition and preparation method thereof | |
CN113861688A (en) | Low-dielectric polyphenylene sulfide composite material and preparation method thereof | |
CN104650558A (en) | High efficiency flame retardant reinforced grade PC/PBT alloy and preparation method thereof | |
CN104693697A (en) | High-strength flame-retardant PBT/LCP composite material and preparation method thereof | |
CN103709663A (en) | Modified PET/PBT alloy material | |
CN110452505B (en) | High-heat-resistance heat-conduction polyester composite material and preparation method thereof | |
CN112662141A (en) | Preparation method of flame-retardant hydrolysis-resistant PBT material | |
CN104151789A (en) | Low-warping high voltage resistance PBT modified material and preparation method thereof | |
CN104693748A (en) | Flame-retardant modified PC/PBT alloy and preparation method thereof | |
CN104672809A (en) | Toughened reinforced environment-friendly flame-retardant PBT/PET (polybutylene terephthalate/polyethylene terephthalate) alloy | |
CN113861687B (en) | Polyphenylene sulfide composition and preparation method thereof | |
CN114517012B (en) | High-appearance antibacterial halogen-free flame-retardant polyamide composite material and preparation method thereof | |
CN114015223A (en) | PC/PBT alloy material and preparation method and application thereof | |
CN115386200A (en) | PET composition and preparation method and application thereof | |
CN104693747A (en) | PC/PBT alloy with anti-electrostatic aging-resistant property | |
CN109627705B (en) | Acid and alkali resistant chemically modified PET composite material and preparation method thereof | |
CN104725794A (en) | Glass-fiber-reinforced flame-retardant PBT-PET alloy | |
CN113683878A (en) | Spiral substituted polyolefin and preparation method thereof, and polycarbonate composition and preparation method thereof | |
CN113667241A (en) | Preparation method of flame-retardant 90-DEG C PVC insulating material | |
KR101748243B1 (en) | Halogen-free flame-retardant polyester resin composition having high fluidity and surface gloss and molded article thereof |
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: 20210416 |