CN115403912A - Modified polysiloxane-polycarbonate composition and preparation method and application thereof - Google Patents
Modified polysiloxane-polycarbonate composition and preparation method and application thereof Download PDFInfo
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- 239000004417 polycarbonate Substances 0.000 title claims abstract description 47
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 47
- 239000000203 mixture Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 36
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 18
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920002545 silicone oil Polymers 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 239000004359 castor oil Substances 0.000 claims abstract description 10
- 235000019438 castor oil Nutrition 0.000 claims abstract description 10
- 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 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 12
- 229910001867 inorganic solvent Inorganic materials 0.000 claims description 11
- 239000003049 inorganic solvent Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 238000012544 monitoring process Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- QBDSZLJBMIMQRS-UHFFFAOYSA-N p-Cumylphenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=CC=C1 QBDSZLJBMIMQRS-UHFFFAOYSA-N 0.000 claims description 6
- NKTOLZVEWDHZMU-UHFFFAOYSA-N p-cumyl phenol Natural products CC1=CC=C(C)C(O)=C1 NKTOLZVEWDHZMU-UHFFFAOYSA-N 0.000 claims description 6
- YQUQWHNMBPIWGK-UHFFFAOYSA-N 4-isopropylphenol Chemical compound CC(C)C1=CC=C(O)C=C1 YQUQWHNMBPIWGK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims description 4
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 23
- 239000000243 solution Substances 0.000 description 7
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- -1 polysiloxane structure Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical group 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/22—General preparatory processes using carbonyl halides
- C08G64/24—General preparatory processes using carbonyl halides and phenols
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides a modified polysiloxane-polycarbonate composition, a preparation method and application thereof, and relates to the technical field of high polymer materials. Specifically, the modified polysiloxane-polycarbonate composition is prepared from the following components in parts by mass: 80-120 parts of bisphenol A, 70-90 parts of silicone oil, 15-25 parts of castor oil, 10-30 parts of sebacic acid, 90-110 parts of phosgene, 3-5 parts of triethylamine, 3-7 parts of an additive and a plurality of solvents. By adopting a one-step intermittent synthesis route, the pH value and the molecular weight of the sodium carbonate in the water phase or the polycarbonate in the oil phase are monitored in real time, and finally the reaction composition is obtained. The modified polysiloxane-polycarbonate composition has high-quality mechanical strength such as high mobile phase, strong toughness and the like, and the preparation method is simple and easy to implement, has low cost and has good application prospect.
Description
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to a modified polysiloxane-polycarbonate composition, and a preparation method and application thereof.
Background
Polycarbonate (PC) is a high molecular polymer containing carbonate groups in molecular chains, has become a universal engineering plastic with the highest growth speed among five engineering plastics due to structural particularity, and has wide application in various fields such as building materials, automobiles, medical instruments, aerospace, electronics, optics and the like. The polycarbonate is mainly prepared by the polycondensation reaction of aromatic dihydric alcohol such as bisphenol A and a carbonate precursor such as phosgene, has excellent impact strength, dimensional stability, heat resistance and transparency, and is required to prepare polycarbonate products with other characteristics in order to further expand the application field of the polycarbonate.
For example, in the invention patent with the application number of TW20170135612, a polysiloxane structure is introduced to a polycarbonate main chain, and a sebacoyl structure is introduced at the same time, so that the polycarbonate has good fluidity while having the performances of chemical corrosion resistance, low-temperature impact strength and the like. For another example, in the patent of invention with application number of CN201610079183.X, an isocyanate group-terminated polydimethylsiloxane or an epoxy group-terminated polydimethylsiloxane is added to react with hydroxyl groups on a PC molecular chain to form a block copolymer, so that a modified polycarbonate with high fluidity and low-temperature toughness is obtained. However, other technical means still exist to realize a carbonate polymer with better fluidity and stronger toughness, and the preparation method and the raw material cost are more friendly while the performance is considered.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a modified polysiloxane-polycarbonate composition, which realizes a polysiloxane-polycarbonate material with high mobile phase and strong toughness by introducing two components of silicone oil and castor oil.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the modified polysiloxane-polycarbonate composition is prepared from the following components in parts by mass:
80-120 parts of bisphenol A, 70-90 parts of silicone oil, 15-25 parts of castor oil, 10-30 parts of sebacic acid, 90-110 parts of phosgene, 3-5 parts of triethylamine, 3-7 parts of an additive and a plurality of solvents.
Preferably, the additive comprises at least one of p-cumylphenol, p-isopropylphenol, and p-tert-butylphenol;
more preferably, the additive is p-cumylphenol.
Preferably, the solvent includes an organic solvent and an inorganic solvent;
wherein the organic solvent is dichloromethane, and the inorganic solvent comprises an aqueous solution of alkaline hydroxide;
more preferably, the alkaline hydroxide includes at least one of sodium hydroxide, potassium hydroxide, ammonia monohydrate, and lithium hydroxide;
more preferably, the aqueous solution of the alkali hydroxide has a mass content of 30% to 40%.
Preferably, the mass portion of the solvent is 1800-2500 portions;
wherein the mass ratio of the organic solvent to the inorganic solvent is (14-16): (5-7).
Preferably, the silicone oil has a molecular weight of 2.3 × 10 4 ～2.5×10 4 。
A second object of the present invention is to provide a method for producing the modified polysiloxane-polycarbonate composition; the modified polysiloxane-polycarbonate composition has high mechanical property, simplifies the preparation process and is more friendly to the cost of raw materials and time.
The preparation method of the modified polysiloxane-polycarbonate composition adopts batch one-step polymerization, and synchronously carries out phosgenation reaction and polycondensation reaction, and specifically comprises the following steps:
fully mixing all components except phosgene, introducing phosgene, and synthesizing the modified polysiloxane-polycarbonate composition by adopting a one-step method; monitoring the content of sodium carbonate in the water phase in real time, and/or monitoring the molecular weight of polycarbonate in the oil phase in real time to judge the reaction end point;
side reactions become increasingly apparent as phosgene is passed into the reaction vessel until the bisphenol a reaction has reached 90%: naOH + COCl 2 ＝＝Na 2 CO 3 +NaCl+H 2 O。
Preferably, when the content of sodium carbonate in the water phase is 16 g/kg-18 g/kg, stopping introducing the phosgene and finishing the reaction;
preferably, when the molecular weight of the polycarbonate in the oil phase is 2700 to 3100, the introduction of the phosgene is stopped and the reaction is terminated.
Preferably, before the reaction starts, the pH of the reaction system is 8.8 to 9.5; after the reaction is finished, the pH value of the reaction system is 10.5-11.3.
Preferably, the aqueous solution of the alkali hydroxide is continuously added during the reaction to control the pH of the reaction system to be maintained within 8.8 to 11.3.
More preferably, the pH of the reaction system before the start of the reaction is 9.2; after the reaction is finished, the pH value of the reaction system is 10.8;
more preferably, the pH of the reaction system is 10.3 at the mid-point of the reaction, with acceptable pH fluctuations ranging from 10.5 to 11.3.
Preferably, the preparation method may specifically comprise the steps of:
(1) Mixing bisphenol A, triethylamine, an additive and an inorganic solvent to obtain a first mixed phase; mixing sebacic acid, silicone oil, castor oil and an organic solvent to obtain a second mixed phase;
(2) Dropwise adding the second mixed phase into the first mixed phase, and introducing phosgene into a closed reaction system while dropwise adding; continuously reacting for 2-5 h;
(3) Sequentially carrying out separation treatment and purification treatment on the mixed phase obtained by the reaction;
more preferably, in the step (2), the temperature of the reaction system is 15 ℃ to 60 ℃.
Preferably, the organic solvent in the invention can be recycled; however, it should be noted that the content of triethylamine in the organic solvent is detected before recycling, and the amount of fresh triethylamine is reduced according to the content of residual triethylamine, similarly to the inorganic solvent.
The third purpose of the invention is to provide the application of the modified polysiloxane-polycarbonate composition in high molecular materials; specifically, the modified polysiloxane-polycarbonate composition is applied to a high polymer material.
Drawings
While the drawings that accompany the detailed description and can be utilized for clarity in describing particular embodiments of the invention, it should be apparent that the drawings described below are illustrative of some embodiments of the invention and that other drawings can be utilized by those skilled in the art without undue inventive faculty.
FIG. 1 is a graph showing the relationship between the amount of phosgene introduced and the amount of sodium carbonate in the water phase and the molecular weight of polycarbonate in the oil phase in examples of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The modified polysiloxane-polycarbonate composition is prepared from the following components in parts by weight:
80-120 parts of bisphenol A, 70-90 parts of silicone oil, 15-25 parts of castor oil, 10-30 parts of sebacic acid, 90-110 parts of phosgene, 3-5 parts of triethylamine, 3-7 parts of an additive and 1800-2500 parts of a solvent.
As a preferred embodiment, the parts by weight of bisphenol a include, but are not limited to, 80 parts, 82 parts, 84 parts, 86 parts, 88 parts, 90 parts, 92 parts, 94 parts, 96 parts, 98 parts, 100 parts, 102 parts, 104 parts, 106 parts, 108 parts, 110 parts, 112 parts, 114 parts, 116 parts, 118 parts, 120 parts; the parts by weight of the silicone oil include, but are not limited to, 70 parts, 72 parts, 74 parts, 76 parts, 78 parts, 80 parts, 82 parts, 84 parts, 86 parts, 88 parts and 90 parts; the parts by weight of the castor oil include, but are not limited to, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts and 25 parts; the parts by weight of the sebacic acid include, but are not limited to, 10 parts, 15 parts, 20 parts, 25 parts and 30 parts; the parts by weight of the phosgene include, but are not limited to, 90 parts, 92 parts, 94 parts, 96 parts, 98 parts, 100 parts, 102 parts, 104 parts, 106 parts, 108 parts and 110 parts; the parts by weight of the triethylamine include but are not limited to 3 parts, 4 parts and 5 parts; the weight parts of the additive include but are not limited to 3 parts, 4 parts, 5 parts, 6 parts and 7 parts; the parts by weight of the solvent include, but are not limited to, 1800 parts, 1900 parts, 2000 parts, 2100 parts, 2200 parts, 2300 parts, 2400 parts, 2500 parts.
As a preferred embodiment, the solvent includes an organic solvent and an inorganic solvent; the mass ratio of the organic solvent to the inorganic solvent includes, but is not limited to, 14: 5. 14: 6. 14: 7. 15: 5. 15: 6. 15: 7. 16: 5. 16: 6. 16:7.
the preparation method of the modified polysiloxane-polycarbonate composition mainly comprises the following steps: fully mixing all the components except phosgene, introducing phosgene, and synthesizing the modified polysiloxane-polycarbonate composition by adopting a one-step method; monitoring the content of sodium carbonate in the water phase in real time, and/or monitoring the molecular weight of polycarbonate in the oil phase in real time to judge the reaction end point;
as a preferred embodiment, when the content of sodium carbonate in the aqueous phase includes, but is not limited to, 16g/kg, 17g/kg, 18g/kg, and/or when the molecular weight of the polycarbonate in the oil phase includes, but is not limited to, 2700, 2800, 2900, 3000, 3100, the phosgene feed is stopped and the reaction is terminated.
As a preferred embodiment, the pH of the reaction system at the start of the reaction includes, but is not limited to, 8.8, 8.9, 9.0, 9.1, 9.2, 9.3, 9.4, 9.5; the pH of the reaction system at the end of the reaction includes, but is not limited to, 10.5, 10.6, 10.7, 10.8, 10.9, 11.0, 11.1, 11.2, 11.3.
Examples
(1) Weighing raw materials: 100g of bisphenol A, 80g of silicone oil (with the molecular weight of 24 k), 20g of castor oil, 20g of sebacic acid, 4.9g of p-cumylphenol, 266g of 33% sodium hydroxide solution, 4.2g of triethylamine, 1489g of dichloromethane and 352g of deionized water;
(2) Mixing bisphenol A, triethylamine, p-cumylphenol, a sodium hydroxide solution and deionized water to obtain a first mixed phase; mixing sebacic acid, silicone oil, castor oil and dichloromethane to obtain a second mixed phase; independently stirring the mixed phases until the mixed phases are uniform, transferring the first mixed phase into a three-neck flask, heating and maintaining the reaction temperature at 45 ℃; dropwise adding the second mixed phase into a three-neck flask, and introducing phosgene to start reaction;
(3) Monitoring whether the pH value of the reaction system is between 8.8 and 11.3 in real time; if the pH value is too high, the flow rate of the phosgene is too high, and the pH value can be controlled to be limited in the interval by additionally adding a sodium hydroxide aqueous solution;
(4) Monitoring the content of sodium carbonate in the water phase and the molecular weight of polycarbonate in the oil phase in real time, and drawing a real-time curve graph by a computer, wherein the real-time curve graph is shown in figure 1; wherein the abscissa of FIG. 1 is the phosgene feed (in pounds), the ordinate (left) of FIG. 1 is the sodium carbonate content, and the ordinate (right) of FIG. 1 is the molecular weight of the polycarbonate. In this example, the reaction was stopped when the total mass of phosgene introduced was 4300 pounds.
(5) And centrifuging the reacted emulsion, and then eluting methylene chloride to obtain the modified polysiloxane-polycarbonate composition.
Table 1 is a table of the test results of the strength and performance indexes of the product prepared in this embodiment.
TABLE 1
| Performance index | Parameter(s) | Unit of | Test standard |
| Tensile stress, yld, type I, 50mm/min | 61 | MPa | ASTM D 638 |
| Tensile stress, brk, type I, 50mm/min | 58 | MPa | ASTM D 638 |
| Tensile modulus, 5mm/min | 2250 | MPa | ASTM D 638 |
| Bending stress, yd, 1.3mm/min,50mm span | 98 | MPa | ASTM D 790 |
| Flexural modulus, 1.3mm/min,50mm span | 2265 | MPa | ASTM D 790 |
| Hardness Rockwell hardness R | 136 | / | ASTM D 785 |
| Tensile stress, yld,50mm/min | 65 | MPa | ISO 527 |
| Tensile stress, brk,50mm/min | 62 | MPa | ISO 527 |
| Tensile modulus, 1mm/min | 2237 | MPa | ISO 527 |
Table 2 is a table of the test results of the mechanical property indexes of the product prepared in this embodiment.
TABLE 2
Table 3 is a table of the thermal performance index test results of the product prepared in this example.
TABLE 3
| Performance index | Parameter(s) | Unit | Test standard |
| Vicat softening temperature, rate B/50 | 138 | ℃ | ASTM D 1525 |
| HDT,0.45MPa,3.2mm (before annealing) | 123 | ℃ | ASTM D 648 |
| HDT,1.82MPa,3.2mm (before annealing) | 117 | ℃ | ASTM D 648 |
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the above embodiments are merely illustrative of the technical solution of the present invention and are not restrictive; those of ordinary skill in the art will understand that: modifications may be made to the above-described embodiments, or equivalents may be substituted for some or all of the features thereof without departing from the spirit and scope of the present invention; the modifications or the substitutions do not cause the essence of the corresponding technical solutions to depart from the scope of the technical solutions of the embodiments of the present invention; it is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. The modified polysiloxane-polycarbonate composition is characterized by comprising the following components in parts by mass:
80-120 parts of bisphenol A;
70-90 parts of silicone oil;
15-25 parts of castor oil;
10-30 parts of sebacic acid;
90-110 parts of phosgene;
3-5 parts of triethylamine;
3-7 parts of an additive;
and a plurality of solvents are used.
2. The modified polysiloxane-polycarbonate composition of claim 1, wherein the additive comprises at least one of p-cumylphenol, p-isopropylphenol, and p-tert-butylphenol;
preferably, the additive is p-cumylphenol.
3. The modified polysiloxane-polycarbonate composition of claim 1, wherein the solvent comprises an organic solvent and an inorganic solvent; wherein the content of the first and second substances,
the organic solvent is dichloromethane;
the inorganic solvent comprises an aqueous solution of an alkali hydroxide;
preferably, the alkaline hydroxide comprises at least one of sodium hydroxide, potassium hydroxide, ammonia monohydrate, and lithium hydroxide;
preferably, the aqueous solution of the alkaline hydroxide has a mass content of 30% to 40%.
4. The modified polysiloxane-polycarbonate composition of claim 3, wherein the solvent is used in an amount of 1800 to 2500 parts by weight; wherein the content of the first and second substances,
the mass ratio of the organic solvent to the inorganic solvent is (14-16): (5-7).
5. The modified polysiloxane-polycarbonate composition of claim 1, wherein the silicone oil has a molecular weight of 2.3 x 10 4 ～2.5×10 4 。
6. The method of preparing the modified polysiloxane-polycarbonate composition of any of claims 1-5, comprising the steps of:
fully mixing all the components except phosgene, introducing phosgene, and synthesizing the modified polysiloxane-polycarbonate composition by adopting a one-step method;
monitoring the content of sodium carbonate in the water phase in real time, and/or monitoring the molecular weight of polycarbonate in the oil phase in real time to judge the reaction end point;
preferably, when the content of sodium carbonate in the water phase is 16 g/kg-18 g/kg, stopping introducing the phosgene and finishing the reaction;
preferably, when the molecular weight of the polycarbonate in the oil phase is 2700 to 3100, the introduction of the phosgene is stopped and the reaction is terminated.
7. The method for producing a modified polysiloxane-polycarbonate composition according to claim 6, wherein the reaction system has a pH of 8.8 to 9.5 before the start of the reaction; after the reaction is finished, the pH value of the reaction system is 10.5-11.3.
8. The method for preparing a modified polysiloxane-polycarbonate composition according to claim 6, wherein the aqueous solution of the alkali hydroxide is continuously added during the reaction to control the pH of the reaction system to be within 8.8 to 11.3.
9. The method of claim 6, wherein the method comprises the steps of:
(1) Mixing bisphenol A, triethylamine, an additive and an inorganic solvent to obtain a first mixed phase; mixing sebacic acid, silicone oil, castor oil and an organic solvent to obtain a second mixed phase;
(2) Dropwise adding the second mixed phase into the first mixed phase, and introducing phosgene into a closed reaction system while dropwise adding; continuously reacting for 2-5 h;
(3) Sequentially carrying out separation treatment and purification treatment on a mixed phase obtained by the reaction;
preferably, in the step (2), the temperature of the reaction system is 15 to 60 ℃.
10. Use of the modified polysiloxane-polycarbonate composition according to any one of claims 1 to 5 in a polymeric material.
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| CN202210872480.5A Pending CN115403912A (en) | 2022-07-20 | 2022-07-20 | Modified polysiloxane-polycarbonate composition and preparation method and application thereof |
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| CN (1) | CN115403912A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150595A (en) * | 1995-09-20 | 1997-05-28 | 通用电气公司 | Method of preparing polycarbonate-polysiloxane block copolymers |
| CN114196001A (en) * | 2022-01-11 | 2022-03-18 | 万华化学集团股份有限公司 | Polycarbonate-polyorganosiloxane copolymer, manufacturing method and resin composition containing same |
| CN114752052A (en) * | 2022-03-31 | 2022-07-15 | 宁波港智新材料有限公司 | Sebacic acid block copolycarbonate, preparation method and application thereof |
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2022
- 2022-07-20 CN CN202210872480.5A patent/CN115403912A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1150595A (en) * | 1995-09-20 | 1997-05-28 | 通用电气公司 | Method of preparing polycarbonate-polysiloxane block copolymers |
| CN114196001A (en) * | 2022-01-11 | 2022-03-18 | 万华化学集团股份有限公司 | Polycarbonate-polyorganosiloxane copolymer, manufacturing method and resin composition containing same |
| CN114752052A (en) * | 2022-03-31 | 2022-07-15 | 宁波港智新材料有限公司 | Sebacic acid block copolycarbonate, preparation method and application thereof |
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