CN111978651A - Flame-retardant antistatic soft polyvinyl chloride composite material and preparation method thereof - Google Patents

Flame-retardant antistatic soft polyvinyl chloride composite material and preparation method thereof Download PDF

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CN111978651A
CN111978651A CN202010803799.3A CN202010803799A CN111978651A CN 111978651 A CN111978651 A CN 111978651A CN 202010803799 A CN202010803799 A CN 202010803799A CN 111978651 A CN111978651 A CN 111978651A
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polyvinyl chloride
flame
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平海龙
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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
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
    • C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
    • C08L23/286—Chlorinated polyethylene
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • C08L2201/04—Antistatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/18—Applications used for pipes

Abstract

The invention discloses a flame-retardant antistatic soft polyvinyl chloride composite material and a preparation method thereof, wherein the material comprises the following raw material components in parts by weight: 60-70 parts of chlorinated polyethylene; 30-40 parts of polyvinyl chloride; 5-10 parts of a stabilizer; 27-42 parts of a plasticizer; 10-15 parts of a flame retardant; 5.5-6.5 parts of a lubricant; 15-33 parts of conductive filler; the conductive filler comprises specially conductive carbon black and conductive graphite powder; the material has excellent antistatic performance, good flame retardant performance, excellent weather resistance and good mechanical property.

Description

Flame-retardant antistatic soft polyvinyl chloride composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of polyvinyl chloride composite materials, and particularly relates to a flame-retardant antistatic soft polyvinyl chloride composite material and a preparation method thereof.
Background
The traditional PVC is widely applied to the field of water supply and drainage and has the advantages of acid resistance, alkali resistance, corrosion resistance, internal pressure bearing and the like. However, the traditional PVC has poor mechanical property and mechanical property, is not antistatic, is easy to become brittle at low temperature, has insufficient flame retardance, generates smoke during combustion, is not aging-resistant and is easy to generate electrostatic sparks, and the defects are not beneficial to the application of PVC materials in the coal mine fields of coal mine gas extraction, ventilation and the like. First, PVC can be classified into three types, soft, hard and semi-hard, depending on the amount of plasticizer added. With the annual increase of the utilization rate of soft PVC, the application field of the soft PVC is wider and wider. However, the soft PVC is added with a large amount of plasticizer in the processing process, so that the processing performance and plasticity of the PVC are improved to a certain extent, but the hardness of the PVC is reduced, the flame retardant property of the soft PVC is seriously influenced, and even the soft PVC becomes a flammable material. The soft PVC can be generated along with a large amount of thick smoke in the combustion process, secondary damage is easily generated, the life and property safety of people is seriously harmed, the green environment which people rely on for survival is destroyed, and the safety of the soft PVC in application is greatly reduced; secondly, in order to meet the requirement of antistatic property, a large amount of conductive carbon black needs to be added into the PVC material, so that the PVC material becomes hard and brittle, the mechanical property and mechanical property of the material are greatly influenced, and the use requirement of industrial related fields cannot be met.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides the flame-retardant antistatic soft polyvinyl chloride composite material and the preparation method thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the flame-retardant antistatic soft polyvinyl chloride composite material comprises the following raw material components in parts by weight:
60-70 parts of chlorinated polyethylene; 30-40 parts of polyvinyl chloride; 5-10 parts of a stabilizer; 27-42 parts of a plasticizer; 10-15 parts of a flame retardant; 5.5-6.5 parts of a lubricant; 15-33 parts of conductive filler.
Further, the conductive filler comprises specially conductive carbon black and conductive graphite powder, and the mass ratio of the specially conductive carbon black to the conductive graphite powder in the conductive filler is (5-6): 1 to 3.
Furthermore, the mesh number of the conductive graphite powder is 5000-10000 meshes.
Further, the stabilizer is one or a mixture of more than two of a lead salt stabilizer, calcium stearate, lead stearate or a rare earth composite stabilizer.
Further, the plasticizer is one or a mixture of more than two of dioctyl phthalate, dioctyl adipate and pentaerythritol oleate.
Further, the lubricant is one or a mixture of more than two of oxidized polyethylene wax, paraffin wax, stearic acid or polyethylene wax.
Further, the polyvinyl chloride is SG-3 type.
Further, the flame retardant is HT-105.
Flame-retardant antistatic soft polyvinyl chloride composite material with surface resistance less than 1x106Omega, oxygen index 30%.
A preparation method of a flame-retardant antistatic soft polyvinyl chloride composite material comprises the following steps:
firstly, weighing chlorinated polyethylene, polyvinyl chloride, a stabilizer, a lubricant and conductive filler according to parts by weight, and then stirring at a high speed to completely mix the materials uniformly; when the material temperature reaches 86-90 ℃, adding a plasticizer, and continuing to stir at a high speed; when the material temperature reaches 100 ℃, stirring at a low speed; when the material temperature reaches 110-120 ℃, controlling the material mixing time to be 17-20 min, putting the materials into a cold mixer, continuously mixing the materials in the cold mixer, and cooling the materials to 50-60 ℃ to obtain a mixed material;
and step two, extruding and granulating the mixed material obtained in the step one by using a double-screw extruder, controlling the processing temperature of the extrusion and granulation within the range of 130-170 ℃, and fully cooling the granules to obtain the composite material.
Compared with the prior art, the invention has the following beneficial effects:
the composite material has reasonable formula compatibility, selects the chlorinated polyethylene as a matrix, and leads the surface resistance of the composite material to be less than 1X10 by adding the conductive carbon black and the conductive graphite powder6Omega, the material has excellent antistatic performance, flame retardant performance, weather resistance and mechanical performance.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to examples, but the scope of the present invention is not limited thereto.
The flame-retardant antistatic soft polyvinyl chloride composite material comprises the following raw material components in parts by weight: 60-70 parts of chlorinated polyethylene; 30-40 parts of polyvinyl chloride; 5-10 parts of a stabilizer; 27-42 parts of a plasticizer; 10-15 parts of a flame retardant; 5.5-6.5 parts of a lubricant; 15-25 parts of conductive filler.
The main raw material chlorinated polyethylene adopted by the invention is a saturated elastomer material, is nontoxic and tasteless, and has excellent thermal-oxidative aging resistance, ozone aging resistance, acid and alkali resistance and chemical medicine resistance. The chlorinated polyethylene contains chlorine element, and has flame retardant property and anti-dripping property. And the chlorinated polyethylene is nontoxic, does not contain heavy metal and PAHS (PAHS is a carcinogenic polycyclic aromatic hydrocarbon), and completely meets the requirement of environmental protection.
The polyvinyl chloride is SG-3 type, and the material has excellent strength, rigidity, toughness, heat resistance, low temperature resistance and other properties.
The stabilizer is one or a mixture of more than two of a lead salt stabilizer, calcium stearate, lead stearate or a rare earth composite stabilizer in any proportion. The heat stabilizer is added in too small amount, so that the heat stability in the mixing and processing processes and the use of products is poor, the heat stabilizer is easy to decompose, and excessive heat stabilizer can cause precipitation.
The plasticizer is one or a mixture of more than two of dioctyl phthalate (DOP), dioctyl adipate (DOA) or pentaerythritol oleate in any proportion. The above plasticizers can be used in combination to increase the flexibility of the plastic resin, improve the processability, reduce the melt viscosity and lower the glass transition temperature.
The type of the flame retardant is antimony trioxide HT-105.
The lubricant is one or a mixture of more than two of oxidized polyethylene wax (OPE), paraffin, stearic acid or polyethylene wax in any proportion. Preference is given to oxidized polyethylene waxes, paraffins or stearic acid, in combination with lubricants, too low amounts of which adversely affect the processing flowability and too high amounts of which adversely affect the mechanical and flame-retardant properties.
The conductive filler comprises specially conductive carbon black and conductive graphite powder, and the mass ratio of the specially conductive carbon black to the conductive graphite powder in the conductive filler is (5-6): 1 to 3. The mesh number of the conductive graphite powder is 5000-10000 meshes.
The conductive filler is prepared by mixing the special conductive carbon black and the conductive graphite powder, the conductivity of the conductive graphite powder is higher than that of the traditional conductive carbon black, and the conductivity of the material can be improved6Omega. If the traditional conductive carbon black is used as the conductive filler, a large amount of conductive carbon black needs to be added to achieve the conductive performance of the invention, which can cause the tensile property of the whole polyvinyl chloride composite material to be greatly reduced, and the qualified soft polyvinyl chloride composite material cannot be made.
Example 1
70 parts of chlorinated polyethylene material, 30 parts of polyvinyl chloride resin, 12 parts of dioctyl adipate (DOA), 2 parts of calcium stearate, 4 parts of lead stearate, 4 parts of paraffin, 1.5 parts of polyethylene oxide wax (OPE), 20 parts of specially-conductive carbon black (HG-IP), 4 parts of conductive graphite powder and 10 parts of flame retardant are weighed according to the parts by weight, poured into a high-speed mixer, started and stirred at a high speed.
Adding 15 parts by weight of dioctyl phthalate (DOP) when the material temperature reaches 90 ℃, continuously stirring at a high speed, changing to low-speed stirring when the material temperature reaches 100 ℃, mixing for 16min when the material temperature reaches 115 ℃, discharging into a cold mixer, cooling the material to 55 ℃ in the cold mixer, and discharging the material to obtain a mixed material. The obtained mixture was processed by a twin-screw extruder at a heating temperature of 170 ℃ to form a phi 50 hose, and after the hose was sufficiently cooled, a ring shape having a width of 30mm was cut out from the hose, and then various parameter tests as listed in the attached table 1 were performed.
Example 2
68 parts by weight of chlorinated polyethylene material, 32 parts by weight of polyvinyl chloride resin, 15 parts by weight of dioctyl adipate (DOA), 3 parts by weight of calcium stearate, 3 parts by weight of lead stearate, 4 parts by weight of paraffin, 2.5 parts by weight of polyethylene oxide wax (OPE), 25 parts by weight of specially-conductive carbon black (HG-IP), 6 parts by weight of conductive graphite powder and 11 parts by weight of flame retardant are weighed according to the parts by weight, poured into a high-speed mixer, started and stirred at high speed.
When the material temperature reaches 86 ℃, adding 18 parts by weight of dioctyl phthalate (DOP), continuously stirring at a high speed, changing to low-speed stirring when the material temperature reaches 100 ℃, mixing for 15min when the material temperature reaches 120 ℃, discharging into a cold mixer, cooling the material to 55 ℃ in the cold mixer, and discharging the material to obtain a mixed material. The obtained mixture was processed by a twin-screw extruder at a heating temperature of 170 ℃ to form a phi 50 hose, and after the hose was sufficiently cooled, a ring shape having a width of 30mm was cut out from the hose, and then various parameter tests as listed in the attached table 1 were performed.
Example 3
65 parts by weight of chlorinated polyethylene material, 35 parts by weight of polyvinyl chloride resin, 17 parts by weight of pentaerythritol oleate, 2 parts by weight of lead salt stabilizer, 4 parts by weight of rare earth composite stabilizer, 3 parts by weight of stearic acid, 3.5 parts by weight of oxidized polyethylene wax (OPE), 23 parts by weight of specially-conductive carbon black (HG-IP), 5 parts by weight of conductive graphite powder and 15 parts by weight of flame retardant are weighed according to the parts by weight, poured into a high-speed mixer, started and stirred at high speed.
When the material temperature reaches 95 ℃, adding 20 parts by weight of dioctyl phthalate (DOP), continuously stirring at a high speed, changing to low-speed stirring when the material temperature reaches 105 ℃, mixing for 15min when the material temperature reaches 115 ℃, discharging into a cold mixer, cooling the material to 55 ℃ in the cold mixer, and discharging the material to obtain a mixed material. The obtained mixture was processed by a twin-screw extruder at a heating temperature of 170 ℃ to form a phi 50 hose, and after the hose was sufficiently cooled, a ring shape having a width of 30mm was cut out from the hose, and then various parameter tests as listed in the attached table 1 were performed.
Example 4
62 parts of chlorinated polyethylene material, 40 parts of polyvinyl chloride resin, 20 parts of pentaerythritol oleate, 4 parts of lead salt stabilizer, 2 parts of rare earth composite stabilizer, 4.5 parts of stearic acid, 1.5 parts of oxidized polyethylene wax (OPE), 27 parts of special conductive carbon black (HG-IP), 6 parts of conductive graphite powder and 13 parts of flame retardant are weighed according to the parts by weight, poured into a high-speed mixer, started and stirred at a high speed.
Adding 22 parts by weight of dioctyl phthalate (DOP) when the material temperature reaches 90 ℃, continuously stirring at a high speed, changing to low-speed stirring when the material temperature reaches 110 ℃, mixing for 15min when the material temperature reaches 125 ℃, discharging into a cold mixer, cooling the material to 55 ℃ in the cold mixer, and discharging the material to obtain a mixed material. The obtained mixture was processed by a twin-screw extruder at a heating temperature of 170 ℃ to form a phi 50 hose, and after the hose was sufficiently cooled, a ring shape having a width of 30mm was cut out from the hose, and then various parameter tests as listed in the attached table 1 were performed.
Example 5
70 parts of chlorinated polyethylene material, 30 parts of polyvinyl chloride resin, 12 parts of pentaerythritol oleate, 6 parts of calcium stearate, 4 parts of lead stearate, 3 parts of paraffin, 3.5 parts of polyethylene oxide wax (OPE), 18 parts of ultra-conductive carbon black (HG-IP), 9 parts of conductive graphite powder and 13 parts of flame retardant are weighed according to the parts by weight, poured into a high-speed mixer, started and stirred at a high speed.
Adding 19 parts by weight of dioctyl phthalate (DOP) when the material temperature reaches 88 ℃, continuously stirring at a high speed, changing to low-speed stirring when the material temperature reaches 100 ℃, discharging the materials into a cold mixer for 20min when the material temperature reaches 110 ℃, cooling the materials to 50 ℃ in the cold mixer, and discharging the materials to obtain a mixed material: soft polyvinyl chloride (PVC) with flame retardant, antistatic properties.
Processing the obtained mixture by a double-screw extruder at the heating temperature of 180 ℃ to form a hose.
Example 6
63 parts by weight of chlorinated polyethylene material, 35 parts by weight of polyvinyl chloride resin, 18 parts by weight of pentaerythritol oleate, 6 parts by weight of calcium stearate, 4 parts by weight of lead stearate, 3 parts by weight of paraffin, 3.5 parts by weight of polyethylene oxide wax (OPE), 12 parts by weight of specially-conductive carbon black (HG-IP), 4 parts by weight of conductive graphite powder and 12 parts by weight of flame retardant are weighed, poured into a high-speed mixer, started and stirred at high speed.
When the material temperature reaches 90 ℃, adding 20 parts by weight of dioctyl phthalate (DOP), continuously stirring at a high speed, changing to low-speed stirring when the material temperature reaches 100 ℃, discharging the materials into a cold mixer when the material temperature reaches 120 ℃, cooling the materials to 60 ℃ in the cold mixer, and discharging the materials to obtain a mixed material: soft polyvinyl chloride (PVC) with flame retardant, antistatic properties.
Flame retardant property: the flame combustion time is less than or equal to 3 seconds, and the flameless combustion time is less than or equal to 10 seconds. The oxygen index of the composite material is 30 percent. Antistatic performance: surface resistance < 1X106Omega; can completely meet the requirements of the standards of the Ministry of coal, MT181-1988, MT 558.1-2005 and AQ 1071-2009.
TABLE 1 test data
Figure 96630DEST_PATH_IMAGE001
As can be seen from the above table, the soft polyvinyl chloride (PVC) composite material with flame retardant and antistatic properties has excellent comprehensive properties. The soft polyvinyl chloride (PVC) composite material with flame retardant and antistatic properties is granular, and the basic color is black.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. The flame-retardant antistatic soft polyvinyl chloride composite material is characterized by comprising the following raw material components in parts by weight: 60-70 parts of chlorinated polyethylene; 30-40 parts of polyvinyl chloride; 5-10 parts of a stabilizer; 27-42 parts of a plasticizer; 10-15 parts of a flame retardant; 5.5-6.5 parts of a lubricant; 15-33 parts of conductive filler.
2. The flame-retardant antistatic soft polyvinyl chloride composite material as claimed in claim 1, which is characterized by comprising the following raw material components in parts by weight:
62-68 parts of chlorinated polyethylene; 32-35 parts of polyvinyl chloride; 6 parts of a stabilizer; 33-37 parts of a plasticizer; 13-14 parts of a flame retardant; 6-6.5 parts of a lubricant; 15-25 parts of conductive filler.
3. The flame-retardant antistatic soft polyvinyl chloride composite material as claimed in claim 1 or 2, wherein the conductive filler comprises specially conductive carbon black and conductive graphite powder, and the mass ratio of the specially conductive carbon black to the conductive graphite powder in the conductive filler is 5-6: 1 to 3.
4. The flame-retardant antistatic flexible polyvinyl chloride composite material as claimed in claim 3, wherein the mesh number of the conductive graphite powder is 5000-10000 meshes.
5. The flame-retardant antistatic flexible polyvinyl chloride composite material as claimed in claim 1, wherein the stabilizer is one or a mixture of more than two of lead salt stabilizer, calcium stearate, lead stearate or rare earth composite stabilizer.
6. The flame-retardant antistatic flexible polyvinyl chloride composite material according to claim 1, wherein the plasticizer is one or a mixture of two or more of dioctyl phthalate, dioctyl adipate and pentaerythritol oleate.
7. The flame-retardant antistatic flexible polyvinyl chloride composite material according to claim 1, wherein the lubricant is one or a mixture of more than two of oxidized polyethylene wax, paraffin wax, stearic acid or polyethylene wax.
8. The flame-retardant antistatic flexible polyvinyl chloride composite material as claimed in claim 1, wherein the surface resistance of the material is less than 1x106Omega, oxygen index 30%.
9. The preparation method of the flame-retardant antistatic soft polyvinyl chloride composite material is characterized by comprising the following steps of:
firstly, weighing chlorinated polyethylene, polyvinyl chloride, a stabilizer, a lubricant and conductive filler according to parts by weight, and then stirring at a high speed to completely mix the materials uniformly; when the material temperature reaches 86-90 ℃, adding a plasticizer, and continuing to stir at a high speed; when the material temperature reaches 100 ℃, stirring at a low speed; when the material temperature reaches 110-120 ℃, controlling the material mixing time to be 17-20 min, putting the materials into a cold mixer, continuously mixing the materials in the cold mixer, and cooling the materials to 50-60 ℃ to obtain a mixed material;
and step two, extruding and granulating the mixed material obtained in the step one by using a double-screw extruder, controlling the processing temperature of the extrusion and granulation within the range of 130-170 ℃, and fully cooling the granules to obtain the composite material.
CN202010803799.3A 2020-08-11 2020-08-11 Flame-retardant antistatic soft polyvinyl chloride composite material and preparation method thereof Pending CN111978651A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101096587A (en) * 2007-06-18 2008-01-02 大连工业大学 Antistatic masterbatch and manufacturing method of high-strength polyvinyl chloride pipe for coal mine
CN102061044A (en) * 2010-12-10 2011-05-18 河南理工大学 High shock resistance type inflaming retarding antistatic polyvinyl chloride composition and preparation method thereof
CN103012997A (en) * 2012-12-28 2013-04-03 大连亚泰科技新材料股份有限公司 Smoke-suppression magnesium-series halogen-free flame retardant material special for conveying belt and preparation method thereof
CN106947188A (en) * 2017-04-27 2017-07-14 安徽国登管业科技有限公司 Flame-retardant and anti-static PVC and preparation method thereof
CN108485092A (en) * 2018-04-18 2018-09-04 潍坊亚星化学股份有限公司 Flame-retardant and anti-static CPE Composites and preparation method thereof applied to gas drainage pipeline

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101096587A (en) * 2007-06-18 2008-01-02 大连工业大学 Antistatic masterbatch and manufacturing method of high-strength polyvinyl chloride pipe for coal mine
CN102061044A (en) * 2010-12-10 2011-05-18 河南理工大学 High shock resistance type inflaming retarding antistatic polyvinyl chloride composition and preparation method thereof
CN103012997A (en) * 2012-12-28 2013-04-03 大连亚泰科技新材料股份有限公司 Smoke-suppression magnesium-series halogen-free flame retardant material special for conveying belt and preparation method thereof
CN106947188A (en) * 2017-04-27 2017-07-14 安徽国登管业科技有限公司 Flame-retardant and anti-static PVC and preparation method thereof
CN108485092A (en) * 2018-04-18 2018-09-04 潍坊亚星化学股份有限公司 Flame-retardant and anti-static CPE Composites and preparation method thereof applied to gas drainage pipeline

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