CN111040224A - Syndiotactic polystyrene and its preparing process - Google Patents
Syndiotactic polystyrene and its preparing process Download PDFInfo
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- CN111040224A CN111040224A CN201911399471.3A CN201911399471A CN111040224A CN 111040224 A CN111040224 A CN 111040224A CN 201911399471 A CN201911399471 A CN 201911399471A CN 111040224 A CN111040224 A CN 111040224A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/5399—Phosphorus bound to nitrogen
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention provides a syndiotactic polystyrene comprising: syndiotactic polystyrene particles having surface irregularities and a conductive metal in-situ deposited on the surfaces of the syndiotactic polystyrene particles; the syndiotactic polystyrene particles comprise syndiotactic polystyrene and hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene. According to the invention, hexaphenoxycyclotriphosphazene is used as a flame retardant of syndiotactic polystyrene, the syndiotactic polystyrene is subjected to surface treatment in an electric shock mode, and then conductive metal is deposited on the surface of the syndiotactic polystyrene, so that the syndiotactic polystyrene particles with good flame retardant property and conductivity are obtained, and the mechanical strength of the particles is not obviously reduced.
Description
Technical Field
The invention relates to the field of polystyrene, in particular to syndiotactic polystyrene and a preparation method thereof.
Background
Syndiotactic polystyrene is a kind of polystyrene, and is a crystalline polystyrene obtained by polymerizing with a highly oriented metallocene catalyst, and its main chain structure is that phenyl groups are regularly arranged at both sides of the molecular chain. Syndiotactic polystyrene, which is produced half a century later than general polystyrene, is a semi-crystalline polymer, which has excellent mechanical properties, heat resistance, solvent resistance and dimensional stability due to crystallization, and has a much higher crystallization rate than that of isotactic polystyrene, so that molding can be performed, and thus, it is being widely used as a novel engineering plastic.
As one of plastics, studies on the flame retardant properties of syndiotactic polystyrene have also been receiving wide attention. At present, the use ratio of the halogen flame retardant still accounts for a great proportion in the market, but the existence of the halogen causes indisputable damage to the environment and human bodies, so the development of the halogen-free flame retardant is also carried out vigorously, and the phosphate ester widely applied in the market at present is more and more concerned by people due to excellent flame retardant property and non-toxic action. The phosphazene compound is also a flame retardant which is greatly concerned in recent years, has more excellent flame retardance due to higher phosphorus and nitrogen elements than other organic compounds, is often used for improving the flame retardance of various plastics, is commonly used at present as hexachlorocyclotriphosphazene, and has poor environmental protection due to halogen.
Polystyrene has poor conductivity, basically has no conductivity, and the conductivity of polystyrene is rarely studied.
Disclosure of Invention
In view of this, the present invention aims to provide a syndiotactic polystyrene and a preparation method thereof, wherein the syndiotactic polystyrene provided by the present invention has good flame retardancy and electrical conductivity, and is environmentally friendly.
The present invention provides a syndiotactic polystyrene comprising: syndiotactic polystyrene particles having surface irregularities and a conductive metal in-situ deposited on the surfaces of the syndiotactic polystyrene particles;
the syndiotactic polystyrene particles comprise syndiotactic polystyrene and hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene.
The hexaphenoxycyclotriphosphazene (abbreviated as HPCTP) is used as a flame retardant, namely six chlorine atoms are replaced by phenoxy, and the hexaphenoxycyclotriphosphazene is a halogen-free, low-smoke and low-toxicity environment-friendly flame retardant, has good compatibility with high polymer and has higher flame retardant property.
In one embodiment, the syndiotactic polystyrene particles further comprise flame retardant synergistic masterbatch HT-1055 in an amount of 1 to 5 wt% of syndiotactic polystyrene.
In one embodiment, the syndiotactic polystyrene particles having surface irregularities are spherical, and the surface irregularities are produced by electrical impact.
In one embodiment, the conductive metal is selected from copper.
The syndiotactic polystyrene provided by the invention has good flame retardant property and conductivity.
The invention also provides a preparation method of the syndiotactic polystyrene, which comprises the following steps:
A) melting syndiotactic polystyrene and hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene, and molding to obtain syndiotactic polystyrene particles;
B) subjecting the syndiotactic polystyrene particles to electrical impact treatment to obtain an uneven surface;
C) and carrying out in-situ deposition of conductive metal on the surfaces of the syndiotactic polystyrene particles to obtain the syndiotactic polystyrene.
In one embodiment, the step a) specifically includes:
and melting syndiotactic polystyrene, hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene and flame-retardant synergistic master batch HT-1055 accounting for 1-5 wt% of the syndiotactic polystyrene, and then forming the spherical syndiotactic polystyrene particles.
In one embodiment, in the step B), high-frequency alternating current is adopted for electric shock treatment, and the voltage of the high-frequency alternating current is 3000-8000V/m2. In one embodiment, the voltage of the high-frequency alternating current is 5000V/m2。
In one embodiment, said step B) is followed by step C) and further comprises:
soaking the syndiotactic polystyrene particles subjected to the electric shock treatment in acid, neutralizing in alkali, and finally washing and drying.
In one embodiment, the step C) specifically includes: in situ deposition of metallic copper is performed on the surface of the syndiotactic polystyrene particles.
In one embodiment, the step C) specifically includes:
mixing syndiotactic polystyrene granules with uneven surfaces, copper sulfate, sodium potassium tartrate, glyoxylic acid and sodium hydroxide solution for reaction, washing the obtained product with water and drying the product.
Specifically, syndiotactic polystyrene particles subjected to electrical impact are mixed with a copper reduction system comprising copper sulfate, sodium potassium tartrate as a chelating agent, glyoxylic acid as a reducing agent and a sodium hydroxide solution as a reaction medium, and copper ions in the solution are reduced to metallic copper by glyoxylic acid to deposit on the surface of syndiotactic polystyrene under alkaline conditions.
In one embodiment, the copper reduction system consists of: every 2000g of the solution contains 50-100 g of copper sulfate, 50-100 g of sodium hydroxide, 50-100 g of glyoxylic acid and 100-300 g of potassium sodium tartrate. In one embodiment, the copper reduction system consists of: each 2000g of the mixture contained 79.8g of copper sulfate, 80g of sodium hydroxide, 74g of glyoxylic acid and 210g of potassium sodium tartrate.
According to the invention, hexaphenoxycyclotriphosphazene is used as a flame retardant of syndiotactic polystyrene, the syndiotactic polystyrene is subjected to surface treatment in an electric shock mode, and then conductive metal is deposited on the surface of the syndiotactic polystyrene, so that the syndiotactic polystyrene particles with good flame retardant property and conductivity are obtained, and the mechanical strength of the particles is not obviously reduced. Meanwhile, glyoxylic acid is adopted to replace formaldehyde when copper is reduced by a chemical deposition method, and glyoxylic acid radical ions exist in an alkaline solution, so that the plating speed is high, and the method is environment-friendly and pollution-free to a water body.
Detailed Description
Example 1
Material manufacturers and instrument equipment used are detailed:
syndiotactic polystyrene: dongguan Zhaohui plastics Co Ltd;
hexaphenoxycyclotriphosphazene (HPCTP): model HT-231 Jinan Taxing Fine chemical Co., Ltd;
flame-retardant synergistic master batch: model HT-1055 Jinan Taxing Fine chemical Co., Ltd;
screw extruder: germany KraussMaffei twin screw large extruder;
a granulator: a U.S. Nordson BKG underwater pelletizer;
a corona processor: model number CW4012/4015 Nantong Sanxin Plastic Equipment science and technology Co., Ltd;
oxygen index tester: model JF-3 Nanjing Bright thunder Instrument Equipment Co., Ltd;
resistivity tester: model FT-303 Ningbor instrument, Inc.;
TABLE 1 polystyrene particle formulation
| Components | A | B | C |
| Syndiotactic polystyrene | 100 | 100 | 100 |
| Hexaphenoxycyclotriphosphazene (HPCTP)% | 0 | 6％ | 10％ |
| Flame retardant synergistic master batch (HT-1055)% | 0 | 1.5％ | 2.5％ |
In table 1, the amounts of hexaphenoxycyclotriphosphazene and the flame retardant synergistic masterbatch are the mass percentages of the syndiotactic polystyrene.
Syndiotactic polystyrene was prepared according to the following procedure:
(1) the materials are uniformly mixed according to the component proportions in the table 2, and the mixture is respectively conveyed to a screw machine, the temperatures of four subareas of the screw machine are respectively 280 ℃, 285 ℃, 285 ℃ and 285 ℃, the materials are melted and mixed in the screw machine, the materials are pumped into a granulator by a gear pump, a die head of the granulator is provided with a round hole with the diameter of 2mm, the granules are cut into round granules with the diameter of about 2mm after underwater granulation, the granules are taken by a water to a spin dryer, and a finished product A, B, C is prepared by dehydration and spin-drying procedures, and the oxygen index and the tensile strength of the finished product are tested, and the results are shown in the table 2, and the table 2 is the performance test result of the syndiotactic polystyrene granules.
(2) Setting high-frequency alternating voltage 5000V/m2Carrying out electric impact treatment on the A, B, C material to generate uneven metal attachment points on the surface of the A, B, C material;
(3) soaking the prepared A, B, C material in 0.1mol/L hydrochloric acid for 8h to remove some possible stains on the surface, and then taking out and neutralizing the material with 0.1mol/L sodium hydroxide solution to make the pH value of the material close to neutral;
(4) the neutralized A, B, C particles are washed with water for 2 times respectively, then dried in an oven at 55 ℃, the dried particles are put into a mixed solution composed of copper sulfate, sodium potassium tartrate (chelating agent) and glyoxylic acid as reducing agents, wherein each 2000g of the mixed solution contains 79.8g of copper sulfate and 80g of sodium hydroxide, 74g of glyoxylic acid and 210g of sodium potassium tartrate, and under alkaline conditions, copper ions in the solution are reduced into metal copper by the glyoxylic acid and deposited on the surface.
(5) The prepared pellets were washed with water 2 times and then baked in an oven at 55 c for 8 hours, and the volume resistivity of A, B, C was measured, respectively, and the results are shown in table 2, which is a result of performance test of the syndiotactic polystyrene pellets prepared in example 1 of the present invention.
TABLE 2 results of property test of syndiotactic polystyrene particles prepared in example 1 of the present invention
As can be seen from table 2, the substantial difference between the volume resistivities of the non-conductivity treated particles and the treated particles is about two orders of magnitude, indicating that the conductivity of the conductivity treatment is greatly improved over the non-treated particles.
Comparative example 1
(1) Syndiotactic polystyrene particles A, B, C were prepared in the same manner as in step (1) of example 1;
(2) carrying out pre-etching: etching the three particle materials in a toluene solution for 20 minutes;
(3) dipping the three kinds of particles to be etched for 8 hours by using 10mol/L sulfuric acid;
(4) neutralizing with 1mol/L sodium hydroxide solution to remove residual etching agent on the surface;
(5) washing the particles obtained in the step (4) for 2 times, and in a mixed solution consisting of sodium potassium tartrate and formaldehyde, under an alkaline condition, reducing copper ions in the solution into metallic copper by formaldehyde and depositing the metallic copper on the surface;
(6) the conductive properties of the deposited particles were tested by washing with water and then drying for 8 hours, and the results are shown in table 4 and table 3, which are the conductive properties of the syndiotactic polystyrene particles prepared in comparative example 1 of the present invention.
TABLE 3 conductive Properties of syndiotactic polystyrene particles prepared in comparative example 1 of the present invention
Example 2
A, B, C pellets were prepared according to the composition shown in Table 4 (100 parts of syndiotactic polystyrene, the remainder being in weight percent of syndiotactic polystyrene), the process was the same as in example 1, and the oxygen index and tensile strength and electrical conductivity were measured, as shown in Table 5, and Table 5 shows the results of the performance test of the syndiotactic polystyrene pellets prepared in example 2 of the present invention.
TABLE 4 composition of syndiotactic polystyrene particles prepared in example 2 of the present invention
| Components | A | B | C |
| Syndiotactic polystyrene | 100 | 100 | 100 |
| Hexaphenoxycyclotriphosphazene (HPCTP)% | 0 | 6％ | 10％ |
| Flame retardant synergistic master batch (HT-1055)% | 0 | 0 | 0 |
TABLE 5 results of property test of syndiotactic polystyrene particles prepared in example 2 of the present invention
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A syndiotactic polystyrene, comprising: syndiotactic polystyrene particles having surface irregularities and a conductive metal in-situ deposited on the surfaces of the syndiotactic polystyrene particles;
the syndiotactic polystyrene particles comprise syndiotactic polystyrene and hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene.
2. The syndiotactic polystyrene in claim 1, wherein said syndiotactic polystyrene particles further comprise flame retardant synergistic masterbatch HT-1055 in an amount of 1-5 wt% of syndiotactic polystyrene.
3. The syndiotactic polystyrene in claim 1, wherein said conductive metal is selected from copper.
4. A method for preparing syndiotactic polystyrene, comprising the steps of:
A) melting syndiotactic polystyrene and hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene, and molding to obtain syndiotactic polystyrene particles;
B) subjecting the syndiotactic polystyrene particles to electrical impact treatment to obtain an uneven surface;
C) and carrying out in-situ deposition of conductive metal on the surfaces of the syndiotactic polystyrene particles to obtain the syndiotactic polystyrene.
5. The method according to claim 4, wherein step A) comprises in particular:
and melting syndiotactic polystyrene, hexaphenoxycyclotriphosphazene accounting for 5-15 wt% of the syndiotactic polystyrene and flame-retardant synergistic master batch HT-1055 accounting for 1-5 wt% of the syndiotactic polystyrene, and then forming the syndiotactic polystyrene particles.
6. The method according to claim 5, wherein in the step B), the electric shock treatment is performed by using a high-frequency alternating current having a voltage of 3000 to 8000V/m2。
7. The method of claim 6, wherein step B) is followed by step C) and further comprises:
soaking the syndiotactic polystyrene particles subjected to the electric shock treatment in acid, neutralizing in alkali, and finally washing and drying.
8. The method according to claim 7, wherein step C) comprises in particular: in situ deposition of metallic copper is performed on the surface of the syndiotactic polystyrene particles.
9. The method according to claim 8, wherein step C) comprises in particular:
mixing syndiotactic polystyrene granules with uneven surfaces, copper sulfate, sodium potassium tartrate, glyoxylic acid and sodium hydroxide solution for reaction, washing the obtained product with water and drying the product.
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2019
- 2019-12-30 CN CN201911399471.3A patent/CN111040224B/en active Active
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| CN101245148A (en) * | 2007-02-13 | 2008-08-20 | 镇江爱邦电子科技有限公司 | Monodisperse high-performance conductive silver particle |
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