CN114456576A - CPVC heat-resistant alloy ternary composition and preparation method thereof - Google Patents

CPVC heat-resistant alloy ternary composition and preparation method thereof Download PDF

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CN114456576A
CN114456576A CN202011138446.2A CN202011138446A CN114456576A CN 114456576 A CN114456576 A CN 114456576A CN 202011138446 A CN202011138446 A CN 202011138446A CN 114456576 A CN114456576 A CN 114456576A
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cpvc
ternary composition
superalloy
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CN114456576B (en
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王金刚
李静
张桦
许志东
王凤海
郭爱花
孙培培
桂俊杰
侯斌
盛梅
孙高远
李素真
孙丽朋
张新华
王晶
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China Petroleum and Chemical Corp
Qilu Petrochemical Co of Sinopec
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Qilu Petrochemical Co of Sinopec
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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
    • C08L73/00—Compositions of macromolecular compounds obtained by reactions forming a linkage containing oxygen or oxygen and carbon in the main chain, not provided for in groups C08L59/00 - C08L71/00; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L35/00—Compositions 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 a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L35/06—Copolymers with vinyl aromatic monomers
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

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Abstract

The invention relates to a CPVC heat-resistant alloy ternary composition and a preparation method thereof, belonging to the technical field of chlorinated polyvinyl chloride modification. The CPVC heat-resistant alloy ternary composition comprises the following components in parts by mass: 30-34 parts of CPVC component, 10-14 parts of N-phenylmaleimide terpolymer and 52-60 parts of POK component. The CPVC heat-resistant alloy ternary composition has high heat-resistant Vicat softening temperature and good injection molding processing fluidity; the invention also provides a simple and feasible preparation method.

Description

CPVC heat-resistant alloy ternary composition and preparation method thereof
Technical Field
The invention relates to a CPVC heat-resistant alloy ternary composition and a preparation method thereof, belonging to the technical field of chlorinated polyvinyl chloride modification.
Background
Chlorinated polyvinyl chloride (CPVC) is a product of chlorinated polyvinyl chloride (PVC), the mass fraction of chlorine-containing elements is about 65-71%, the physical properties and mechanical properties, particularly heat resistance, solvent resistance, flame retardance and the like of the chlorinated polyvinyl chloride (CPVC) are greatly improved compared with PVC, and the Vicat softening temperature is 30-40 ℃ higher than that of the PVC. The CPVC is widely applied to manufacturing various pipes, plates, sections, injection molding parts, foam materials, anticorrosive coatings and the like, and has a wide market prospect.
The CPVC has the defects of increased structure, poor thermal stability, increased intermolecular interaction force, high melt viscosity and poor flowability during processing due to the increased chlorine content. For injection molding of CPVC, the first way to improve the heat resistance of the material itself is to increase the chlorine content in the CPVC resin, usually the chlorine content of the CPVC resin is increased by 1 percentage point, the vicat softening temperature of the pipe is increased by about 2 ℃, and when the chlorine content of the resin is higher than 68%, the thermal stability is sharply reduced, and the injection back pressure is sharply increased due to the increase of the melt viscosity, so that the injection molding is difficult. Therefore, the Vicat softening temperature of a single CPVC material can only be controlled between 105 ℃ and 110 ℃.
The improvement of vicat softening temperature and processability of CPVC materials by means of physical modification and chemical modification has been a hot point of research in the plastic processing industry:
the invention patent CN108373570 discloses a PVC and CPVC blending modified colloidal particle with high Vicat softening temperature, and the Vicat softening temperature of the invention reaches 95 ℃ under the condition of meeting the requirements of good processability and impact toughness of materials.
The invention patent CN110423424A discloses a highly heat-resistant and anti-aging CPVC power cable protection tube and a preparation method thereof, the formula of the patent also adopts a PVC and CPVC blending method to improve the processing fluidity of the formula of the cable protection tube, and the Vicat softening temperature of the developed cable protection tube reaches 95 ℃.
The invention patent CN105218990A discloses a highly heat-resistant CPVC formula, the main formula component of the CPVC formula is a ternary blending system of PVC/CPVC/CPE (25: 70: 3), the heat-resistant temperature reaches 125 ℃, but the patent does not mention the chlorine content of the CPVC, and does not have a specific scheme that the Vicat softening temperature of the ternary blending system is increased to 125 ℃.
The invention patent CN110734615A discloses a heat-resistant and corrosion-resistant composition for CPVC filler rings, which adopts CPVC resin with average polymerization degree of 1000 and chlorine content of 69.7, develops a material for the filler rings and reaches a Vicat softening temperature of 139 ℃, but the patent does not mention the processing flow property of the composition for the filler rings.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and providing a CPVC heat-resistant alloy ternary composition which has good injection molding processing flow property while keeping high heat-resistant Vicat softening temperature; the invention also provides a simple and feasible preparation method.
The CPVC heat-resistant alloy ternary composition comprises the following components in parts by mass:
30-34 parts of CPVC component
10-14 parts of N-phenylmaleimide terpolymer
52-60 parts of POK component.
Preferably, the CPVC component comprises the following raw materials in parts by weight:
Figure BDA0002737508420000021
preferably, the CPVC resin is prepared by performing chlorination modification on a PVC resin by a micro-suspension polymerization method; the average polymerization degree of the PVC resin is 630-670, and the mass fraction of chlorine element in the prepared CPVC resin is 66-68%.
Preferably, the antioxidant is a composite antioxidant system of a high-melting-point hindered phenol antioxidant and a high-melting-point thioester antioxidant, and the composite mass ratio is 55-75% to 25-45%. More preferably, the high-melting-point hindered phenol antioxidant is 1,3, 5-trimethyl-2, 4, 6-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene; the high-melting-point thioester antioxidant is dioctadecyl thiodipropionate.
Preferably, the organotin stabilizer is dibutyltin dilaurate in a solid state.
Preferably, the impact modifier MBS is an emulsion-polymerized methacrylate-butadiene-styrene ternary graft copolymer with a core-shell structure, the mass fraction of butadiene in the core layer butadiene-styrene polymer is 12% to 16%, preferably 13 to 14%, and the mass ratio of the shell layer methyl methacrylate to the butyl methacrylate is 1.5 to 2.5: 2.5-3.5, preferably 1: 2.5.
preferably, the lubricant is a compound of pentaerythritol stearate and polymerized oxidized polyethylene wax, and the compound mass ratio is 3: 5. Wherein the number average molecular weight of the polymerized oxidized polyethylene wax is 4500, the molecular weight distribution is 1.35, and the melting point is 113 ℃.
Preferably, the pigment is a mixture of aurora C and Ciba yellow 3G, the mixing part by mass of the aurora C and Ciba yellow 3G is preferably 0.33, the mass ratio is 1.65:0.83, and the color of the prepared heat-resistant alloy ternary composition meets the color difference requirement of standard color card RAL 2011.
Preferably, the filler is titanate surface coupling activated light calcium carbonate with the average particle size of 2500 meshes, and the mass part is preferably 40 parts.
The chlorinated polyvinyl chloride composition is physically and uniformly mixed, then is mixed for 6min on a double-roll mixing mill at the temperature of 195-210 ℃, the plasticized material is pressed into a 4mm sheet on a flat vulcanizing press, and the Vicat softening temperature of the chlorinated polyvinyl chloride composition is 111 ℃ by a B50 method.
Preferably, the CPVC composition is prepared by the following process:
adding 100 parts of CPVC resin at the rotating speed of 800 revolutions per minute of the plastic mixer, and regulating the speed of the mixer to 1200 revolutions per minute; when the temperature is raised to 65 ℃, the organic tin is added, and the heat stabilizer is added at the temperature, so that the organic tin molecules can be quickly absorbed by the CPVC resin particles, the decomposition of the resin in the subsequent heating process is reduced, and the quality of the product is improved. When the temperature is raised to 85 ℃, adding an impact modifier MBS; the temperature is raised to 90 ℃, and calcium carbonate filler, antioxidant, lubricant, pigment and other auxiliary agents are added. The auxiliary agent with smaller particle size is added after the impact modifier with larger particles is added, so that the gap of the impact modifier particles can be prevented from being filled by the auxiliary agent with smaller size, thereby ensuring the contact area between the impact modifier MBS and the raw materials and ensuring the effect of the impact modifier; after the temperature had risen to 130 ℃, the mixing was complete. And transferring the mixture in the high-speed mixer into a cooling mixer, continuously stirring at a low speed, cooling to 50 ℃, and finishing discharging to obtain the CPVC composition.
Preferably, the N-phenylmaleimide terpolymer has a melting point of 91 ℃ and a Vicat softening temperature of 124 ℃.
The preparation process of the N-phenylmaleimide terpolymer is as follows:
(1) preparation of N-phenylmaleimide: in a dry, clean 500mL three-necked flask equipped with a stirrer, 22.5 g (0.22mol) of maleic anhydride, 170mL of toluene, and 11.4mL of DMF were added and stirred to dissolve the maleic anhydride, and then 18mL (about 0.2 mol 1) of aniline was slowly added to the reaction system via a dropping funnel to gradually form a pale yellow product, and the temperature was controlled not to exceed 35 ℃. The aniline was added dropwise for about half an hour and the reaction was continued for 1 hour with the temperature maintained. Then 1.9 g of p-toluic acid was added, heated to about l10 deg.C, refluxed for about 5 hours, and water generated during the reaction was removed with a water separator until the system became a transparent solution. Evaporating toluene, pouring the residual solution into cold water to obtain a large amount of yellow solid, filtering, washing with 5% sodium carbonate aqueous solution, washing with deionized water for several times, recrystallizing with 1:2 ethanol aqueous solution to obtain pale yellow needle-shaped N-Phenylmaleimide (PMI) crystals, and determining the melting point to be 91 ℃ by DSC method.
(2) Emulsion copolymerization of N-phenylmaleimide/ethyl methacrylate/styrene terpolymer:
the monomer ratio is PMI/MMA/St 55:25: 20.
The copolymerization conditions were as follows:
300mL of distilled water, 300g of mixed monomer and 5% by mass of sodium dodecyl sulfate in the mixed monomer are sequentially added into a 1000mL four-mouth bottle provided with a stirrer, a thermometer and a spherical reflux condenser, and the temperature is raised under stirring. When the temperature rises to 80 ℃ set temperature, adding an initiator potassium persulfate with the mass ratio of the mixed monomers of 0.5 percent, and maintaining the set temperature for reaction for 8.5 hours. And after the reaction is finished, cooling the reaction materials to room temperature, discharging the materials, demulsifying by using a 2.5% aluminum sulfate aqueous solution, washing for 2-4 times by using distilled water, filtering, and drying in vacuum to constant weight to obtain the powdery N-phenylmaleimide terpolymer. The terpolymer is mixed for 4min on a double-roll mixing mill at 195-210 ℃, the plasticized material is pressed into 4mm sheets on a flat vulcanizing press, and the Vicat softening temperature is 124 ℃ by the method B50.
The POK component in the ternary alloy composition is POK of Korea Xiaoxing company with the mark of M710F. The melting point was 196 ℃ by DSC method and the Vicat softening temperature was 155 ℃ by B50 method.
The preparation method of the CPVC heat-resistant alloy ternary composition comprises the following steps:
the method comprises the following steps of (1) crushing POK M710F resin particles into POK powder which is sieved by a 50-mesh sieve by using a plastic pulverizer, weighing the prepared CPVC composition powder, POK powder and N-phenyl maleimide terpolymer powder according to the mass ratio determined by the invention, mixing for 6-8 minutes at the rotating speed of 500 revolutions per minute of a plastic mixer, stirring by using a three-layer paddle type in the plastic mixer, controlling the temperature of a material to be not more than 80 ℃, and preventing the temperature of the material from rising to adhere to the wall of a kettle and a stirring paddle; and after discharging, carrying out water cooling brace granulation on a special double-screw extrusion granulator for the mixed CPVC with the length-diameter ratio of 36: 1. The granulating temperature of the double-screw extruder is controlled between 180 ℃ and 205 ℃.
The CPVC composition powder, the POK powder and the N-phenylmaleimide terpolymer powder are preferably used in a mass ratio of 32:12: 56.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the process of preparing the CPVC composition, the invention provides the matching use proportion of the high-melting-point organic tin and the antioxidant, can effectively improve the processing thermal stability of the CPVC composition, and finally ensures the melt mixing of the heat-resistant CPVC alloy composition and the smooth processing and forming of products;
(2) the CPVC composition disclosed by the invention provides the MBS impact modifier with a specific composition, so that the Vicat softening temperature of the CPVC composition is effectively improved, and the impact toughness of the heat-resistant CPVC alloy composition is improved;
(3) according to the invention, the N-phenylmaleimide terpolymer is selected as an interface compatilizer between the CPVC composition and the POK M710F, so that the problem of uniform dispersion between the CPVC composition and the POK M710F in the melting and mixing process is effectively solved, and the comprehensive physical and mechanical properties of the CPVC composition/N-phenylmaleimide terpolymer/POK M710F ternary blend are greatly improved;
(4) the heat-resistant CPVC alloy composition prepared by the invention is suitable for injection molding of a self-control electronic circuit board of a mining heading machine, and meets the requirements of rigidity and toughness balance, flame retardance, acid and alkali resistance and good melt fluidity required by the circuit board.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
For the raw material compositions in examples 1-6, see table 1.
For the raw material compositions in comparative examples 1 to 3, see table 2.
The products prepared in examples 1-6 were tested in relation to each other and are detailed in table 3.
The products prepared in comparative examples 1-3 were tested in the relevant manner and are described in Table 4.
The CPVC component is prepared from the following raw materials in parts by mass:
Figure BDA0002737508420000041
Figure BDA0002737508420000051
the mass fraction of chlorine element in the CPVC resin accounts for 68 percent.
The melting point of the N-phenylmaleimide terpolymer is 91 ℃, and the Vicat softening temperature is 124 ℃.
POK M710F, manufactured by Xiaoxing, Korea.
TABLE 1
Figure BDA0002737508420000052
TABLE 2
Figure BDA0002737508420000053
TABLE 3
Figure BDA0002737508420000054
Figure BDA0002737508420000061
Acid resistance test: the national standard curved sample specimens were placed in a closed container at 80 ℃ in a 1% hydrochloric acid solution for 168 hours, and then the appearance change of the sample specimens was observed.
Alkali resistance test: the national standard curved sample strips were placed in a closed container at 80 ℃ for 168 hours in a 10% NaOH solution, and then the appearance change of the sample strips was observed.
As seen in examples 1-3, the heat resistant CPVC alloy composition is three-part, CPVC composition: n-phenylmaleimide terpolymer: when the mass ratio of the POK M710F is 30-34:10-14:52-60 and the mass ratio is preferably 32:12:56, the POK M710F in the ternary blend is in a continuous phase state, the CPVC composition is in a dispersed phase state, and the N-phenylmaleimide ternary copolymer plays a role of an interface compatilizer between two phases, so that the mechanical property, the flame retardant property and the acid and alkali resistance of the ternary blend material can achieve the best effect.
From examples 4-6, it can be seen that when the mass ratio of the POK M710F is in the range of 30%, 45% and 45%, the corresponding mass ratio of the CPVC composition is in the range of 30%, 40% and 30%, and the ternary blend material is in the dispersed phase, the tensile stress at break of the formulation of examples 4-6 is low, the impact strength of the simple beam notch is low, and the results of the acid and alkali resistance tests of examples 4-6 are not satisfactory because the contents of the POK M710F component and the CPVC composition are unable to form the ternary blend material into the continuous phase.
TABLE 4
Figure BDA0002737508420000071
It is seen from comparative examples 1-3 that, compared with examples 1-3, the flame retardant property of the material does not reach V0 level by using pure POK M710F, the flame retardant property does not reach V0 level by using pure N-phenyl maleimide terpolymer, the mechanical property, acid and alkali resistance and Vicat softening temperature of the material do not meet the requirements, and the Vicat softening temperature and acid and alkali resistance of the material do not meet the requirements by using the heat-resistant CPVC alloy composition by using the CPVC composition alone.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (10)

1. A ternary composition of CPVC heat-resistant alloy is characterized in that: the paint comprises the following components in parts by mass:
30-34 parts of CPVC component
10-14 parts of N-phenylmaleimide terpolymer
52-60 parts of POK component.
2. A CPVC superalloy ternary composition according to claim 1, wherein: the CPVC component comprises the following raw materials in parts by weight:
Figure FDA0002737508410000011
3. a CPVC superalloy ternary composition according to claim 2, wherein: the CPVC resin is prepared by performing chlorination modification on PVC resin by a micro suspension polymerization method; the average polymerization degree of the PVC resin is 630-670, and the mass fraction of chlorine element in the prepared CPVC resin is 66-68%.
4. A CPVC superalloy ternary composition according to claim 2, wherein: the antioxidant is a composite antioxidant system of high-melting-point hindered phenol antioxidant and high-melting-point thioester antioxidant, and the composite mass ratio is 55-75% and 25-45%.
5. A CPVC superalloy ternary composition according to claim 2, wherein: the impact modifier MBS is a methacrylate-butadiene-styrene ternary graft copolymer with a core-shell structure and emulsion polymerization, the mass fraction of butadiene in the butadiene-styrene polymer of the core layer is 12-16%, and the mass ratio of the methyl methacrylate and the butyl methacrylate of the shell layer is 1.5-2.5: 2.5-3.5.
6. A CPVC superalloy ternary composition according to claim 2, wherein: the lubricant is a compound of pentaerythritol stearate and polymerized oxidized polyethylene wax, and the compound mass ratio is 3: 5.
7. A CPVC superalloy ternary composition according to claim 2, wherein: the CPVC composition is prepared as follows:
firstly, adding CPVC resin, and regulating the speed of a mixer to 1200 revolutions per minute; when the temperature is raised to 65 ℃, adding an organic tin stabilizer; when the temperature is raised to 85 ℃, adding an impact modifier MBS; heating to 90 deg.C, adding filler, antioxidant, lubricant and colorant; and after the temperature is raised to 130 ℃, mixing, transferring the mixture in the high-speed mixer into a cooling mixer for continuously stirring, and after the mixture is cooled to 50 ℃, discharging to obtain the CPVC composition.
8. A CPVC superalloy ternary composition according to claim 1, wherein: the melting point of the N-phenylmaleimide terpolymer is 91 ℃, and the Vicat softening temperature is 124 ℃.
9. A method of making a CPVC superalloy ternary composition as claimed in any of claims 1 to 8, wherein: the method comprises the following steps:
crushing POK M710F resin particles by using a plastic mill, sieving, weighing the prepared CPVC composition powder, POK powder and N-phenylmaleimide terpolymer powder according to a ratio, and mixing for 6-8 minutes at the rotating speed of 500 revolutions per minute of a plastic mixer; after discharging, water cooling, bracing and granulating are carried out on a double-screw extrusion granulator.
10. A method of making a CPVC heat-resistant alloy ternary composition according to claim 9, wherein: the length-diameter ratio of the double-screw extruder is 36: 1; the granulation temperature is 180-205 ℃.
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Citations (4)

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Publication number Priority date Publication date Assignee Title
US20080194736A1 (en) * 2007-02-13 2008-08-14 Minqiu Lu PVC nanocomposite manufacturing technology and applications
CN102127273A (en) * 2010-12-22 2011-07-20 山东舜天力塑胶有限公司 Polrvinyl chloride heat-resistance modifier and preparation method thereof
CN108350116A (en) * 2015-10-23 2018-07-31 开米森聚合物与助剂股份公司 Vinyl chloride polymers and compositions for additive manufacturing
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Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080194736A1 (en) * 2007-02-13 2008-08-14 Minqiu Lu PVC nanocomposite manufacturing technology and applications
CN102127273A (en) * 2010-12-22 2011-07-20 山东舜天力塑胶有限公司 Polrvinyl chloride heat-resistance modifier and preparation method thereof
CN108350116A (en) * 2015-10-23 2018-07-31 开米森聚合物与助剂股份公司 Vinyl chloride polymers and compositions for additive manufacturing
US20200157335A1 (en) * 2017-09-27 2020-05-21 Sekisui Chemical Co., Ltd. Resin composition for molding

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
马建华;郑化安;付东升;雷瑞;李欣;袁聪;孙欣新;: "共混改性制备高耐热PVC复合材料的研究进展", 材料导报, no. 2, 25 November 2014 (2014-11-25), pages 331 - 333 *

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