CN110229441B - Permanent antistatic PVC resin composition and antistatic pipe fitting prepared from same - Google Patents

Permanent antistatic PVC resin composition and antistatic pipe fitting prepared from same Download PDF

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CN110229441B
CN110229441B CN201910549532.3A CN201910549532A CN110229441B CN 110229441 B CN110229441 B CN 110229441B CN 201910549532 A CN201910549532 A CN 201910549532A CN 110229441 B CN110229441 B CN 110229441B
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antistatic
parts
pvc
pvc resin
resin composition
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CN110229441A (en
Inventor
刘容德
王晶
张新华
刘浩
王晓敏
王秀丽
李静
裴小静
张桦
高磊
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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
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—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 halogen; Compositions of derivatives of such polymers
    • C08L27/02—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 halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04—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 halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06—Homopolymers or copolymers of vinyl chloride
    • 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
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • 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

Abstract

The invention belongs to the technical field of plastic processing, and particularly relates to a permanent antistatic PVC resin composition, and further discloses an antistatic pipe fitting prepared from the permanent antistatic PVC resin composition. The permanent antistatic PVC composition takes PVC resin, organic tin stabilizer, impact modifier, processing modified resin, antioxidant, lubricant, titanium pigment and carbon black as base materials, and is mixed by adding antistatic agent graft with better antistatic performance, and because the antistatic agent is grafted into the resin through an initiator, the antistatic agent can not migrate along with time, so that the surface of a PVC product can not accumulate static electricity, a permanent antistatic effect is achieved, and the prepared product can be used in the field of long-term antistatic pipes.

Description

Permanent antistatic PVC resin composition and antistatic pipe fitting prepared from same
Technical Field
The invention belongs to the technical field of plastic processing, and particularly relates to a permanent antistatic PVC resin composition, and further discloses an antistatic pipe fitting prepared from the permanent antistatic PVC resin composition.
Background
The plastic is a high molecular compound which is polymerized by addition polymerization or polycondensation reaction by using monomers as raw materials, and is a material or a plastic material product which can be arbitrarily kneaded into various shapes and can keep the shapes unchanged. As is known, plastics generally have high resistivity, which leads to poor conductivity, and such nonconductive property also leads to easy dust absorption and easy charge accumulation on the surface of the plastics, thereby easily causing electrostatic accidents. The defect seriously affects the application of plastic products in certain fields, and particularly, under the working conditions that strict antistatic property is required, such as plastic pipes for coal mines, the plastic products are easy to cause greater potential safety hazard. Various antistatic materials, such as PE antistatic pipes, PVC antistatic pipes, pipe fittings, etc., have been developed at present, and have been widely used in the fields of electronics industry, pipe industry, industrial packaging, home decorative panels, etc., to achieve the purpose of antistatic.
For example, the antistatic ABS/PVC/PETG alloy disclosed in chinese patent CN102807727A is prepared from ABS resin, PVC resin, PETG resin, compatibilizer, and composite antistatic agent as raw materials, especially from stearamidopropyl dimethyl- β -hydroxyethyl quaternary ammonium nitrate, sodium allylsulfonate, N-bis (2-hydroxyethyl) -N- (3 '-dodecyloxy-2' -hydroxypropyl) methyl ammonium methyl sulfate, and (3-lauramidopropyl) trimethyl ammonium methyl sulfate as raw materials, and the composite antistatic agent effectively ensures excellent antistatic property of the alloy material, and has simple preparation process, low product cost, and excellent comprehensive properties of the product. For another example, Chinese patent CN102061044A discloses a highly impact-resistant flame-retardant polyvinyl chloride pipe composition using poly (vinyl chloride)Ethylene oxide is used as antistatic agent, and when 10-18 parts of the antistatic agent is added into PVC, the surface resistivity of the antistatic agent reaches 3 x 108Below, the impact strength is more than 35KJ/m2. For another example, the flame retardant antistatic ABS/PVC alloy material disclosed in chinese patent CN102477206A is prepared from ABS, PVC, a heat stabilizer, a toughening agent, a compatibilizer, a flame retardant, an antistatic agent, a processing aid and an antioxidant as raw materials. For another example, the antistatic low-smoke flame-retardant PVC-ABS composite material disclosed in chinese patent CN102321314A mainly comprises PVC resin, ABS resin, compatibilizer, antistatic agent, smoke-suppressing flame retardant, stabilizer, processing aid and other additives, and has better antistatic property.
Although the plastic products have certain antistatic performance meeting the requirements, the antistatic agents playing an antistatic role in the plastic products represented by the materials are added in a blending mode, and the mode often has the problems of low antistatic efficiency and excessive reduction of mechanical properties due to large addition of the antistatic agents; in addition, for the antistatic agent added in a blending manner, if an efficient antistatic effect is to be achieved, the antistatic agent must have low compatibility with the base resin, and can rapidly move to the surface of a product to form an antistatic film through processes such as adsorption, and the antistatic effect is increasingly poor along with the continuous migration loss of the antistatic agent, so that the antistatic effect of the product is not durable, and the attenuation of the antistatic effect is easily caused by scraping in the using process and the prolonging of the using time. Therefore, how to effectively improve the permanent antistatic property of the plastic product has positive significance for the wide application of the plastic product.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a permanent antistatic PVC resin composition, which has high-efficiency permanent antistatic performance and can be used for preparing permanent antistatic PVC products;
the second technical problem to be solved by the invention is to provide a permanent antistatic pipe product prepared by the composition, wherein the PVC product has no accumulated static on the surface and can be used for a long time, and the pipe composition also has excellent heat resistance and mechanical property.
In order to solve the technical problems, the permanent antistatic PVC resin composition comprises the following components in parts by weight: 100 parts of PVC resin, 1.0-3 parts of organic tin stabilizer, 10-15 parts of impact modifier, 5-10 parts of processing modified resin, 0.5-1.0 part of antioxidant, 0.8-2.5 parts of lubricant, 0-2.0 parts of titanium dioxide, 0-0.005 part of carbon black and 10-20 parts of antistatic graft.
Specifically, the preparation raw materials of the antistatic graft comprise the following components in parts by weight: 80-90 parts of ABS powder, 4-8 parts of sodium allylsulfonate, 8-10 parts of sodium styrene sulfonate, 0.2-0.5 part of initiator and 5-78 parts of TAIC 3.
Specifically, the preparation method of the antistatic graft comprises the following steps:
(1) dissolving a selected amount of the initiator in an organic solvent, adding a selected amount of the TAIC, and uniformly mixing to obtain a mixed solution;
(2) uniformly mixing a selected amount of ABS powder with sodium allylsulfonate and sodium styryl sulfonate, uniformly mixing with the mixed solution obtained in the step (1), and removing the organic solvent to obtain a mixed material;
(3) and carrying out reactive extrusion granulation on the obtained mixed material on a double-screw extruder to obtain the material.
In the step (1), the organic solvent includes acetone, and the mass ratio of the initiator to the organic solvent is 1: 4-6.
The initiator includes dicumyl peroxide (DCP).
In the step (3), the length-diameter ratio of the screws of the twin-screw extruder is controlled to be 40: 1, the reactive extrusion temperature is 160-. If the extrusion temperature is too high, the auxiliary agent is easy to volatilize, so that the grafting rate of the ABS is reduced; at too low a temperature, the reactivity is low, which also leads to a reduction in the grafting yield.
Preferably, in the permanently antistatic PVC resin composition:
the PVC resin is PVC resin with the polymerization degree of less than 800, preferably PVC resin (QS-650) with the polymerization degree of 650 on average;
the organotin stabilizers include organotin stabilizer 2903;
the impact modifier comprises methacrylic acid-butadiene-styrene terpolymer MBS, such as the designation MBS-561;
the antioxidant comprises antioxidant 1010 and/or antioxidant 264; preferably, the mass ratio of the antioxidant 1010 (tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester) to the antioxidant 264(2, 6-di-tert-butyl-p-cresol) is 1: 1;
the processing modified resin comprises styrene-acrylonitrile copolymer AS resin;
the titanium dioxide comprises rutile type titanium dioxide;
the lubricant comprises stearic acid, paraffin wax, microcrystalline wax, PE wax and/or oxidized polyethylene wax.
The invention also discloses a method for preparing the permanent antistatic PVC resin composition, which comprises the steps of taking the PVC resin, the organic tin stabilizer, the impact modifier, the processing modified resin, the antioxidant, the lubricant, the titanium dioxide and the carbon black according to the selected parts by weight, mixing at the temperature of 100-120 ℃, and cooling the obtained mixture, and then adding the antistatic graft to mix.
The invention also discloses the application of the permanent antistatic PVC resin composition in preparing permanent antistatic PVC products.
Specifically, the PVC product comprises a PVC pipe fitting product.
The invention also discloses a permanent antistatic PVC product, which is prepared from the permanent antistatic PVC resin composition according to a conventional process.
The permanent antistatic PVC composition takes PVC resin, organic tin stabilizer, impact modifier, processing modified resin, antioxidant, lubricant, titanium pigment and carbon black as base materials, and is mixed by adding antistatic agent graft with better antistatic performance, and the antistatic agent is grafted into the resin through an initiator, so that the antistatic agent cannot migrate along with time, the surface of a PVC product cannot accumulate static electricity, a permanent antistatic effect is achieved, and the prepared product can be used in the field of long-term antistatic pipes; more importantly, in the PVC resin composition, the mechanical property of the PVC pipe composition lost due to the addition of a large amount of antistatic agent can be compensated by the addition of the graft, so that the pipe composition can not be influenced by external environment humidity and the like, an effective permanent antistatic effect can be achieved, and meanwhile, the pipe composition has good rigidity and toughness and can meet the industrial application requirements.
The antistatic agent graft is prepared by graft reaction of ABS powder, sodium allylsulfonate, sodium styrene sulfonate, an initiator and TAIC, and because the whole reaction process adopts the steps that the antistatic agent is extruded and grafted into carrier resin through reactivity, and then the obtained graft with the antistatic agent is grafted into the resin through the initiator instead of being added through blending, the antistatic agent cannot migrate along with time, thereby achieving the effect of permanent antistatic.
Detailed Description
Preparation example 1
The preparation raw materials of the antistatic agent graft described in this example include the following components in parts by weight: 80kg of injection molding grade high-fluidity ABS powder (Taiwan Qimei PA-756H, the same below), 8kg of sodium allyl sulfonate, 8kg of sodium styrene sulfonate, 0.5kg of initiator DCP and TAIC3 kg.
The preparation method of the antistatic agent graft described in this example comprises the following steps:
(1) weighing DCP and TAIC according to a proportion, dissolving the DCP by using acetone, wherein the proportion of the acetone to the DCP is (weight ratio) 4: 1, then mixing with TAIC;
(2) weighing ABS, sodium allylsulfonate and sodium styryl sulfonate according to a proportion, adding the weighed materials into a continuously variable speed mixer (the rotating speed of the continuously variable speed mixer is 450-;
(3) and (3) carrying out reactive extrusion granulation on the mixed material on a double-screw extruder, wherein the length-diameter ratio of a screw is 40: and 1, the reactive extrusion temperature is 160 ℃, a vacuumizing device is arranged at the rear section of the extruder, the negative pressure is 0.2MPa, and unreacted small molecular substances are discharged through vacuumizing, so that the material is obtained.
Preparation example 2
The preparation raw materials of the antistatic agent graft described in this example include the following components in parts by weight: 90kg of injection molding grade high-fluidity ABS powder, 4kg of sodium allylsulfonate, 10kg of sodium styrene sulfonate, 0.2kg of initiator DCP and 5kg of TAIC.
The preparation method of the antistatic agent graft described in this example comprises the following steps:
(1) weighing DCP and TAIC according to a proportion, dissolving the DCP by using acetone, wherein the proportion of the acetone to the DCP is (weight ratio) 6: 1, then mixing with TAIC;
(2) weighing ABS, sodium allylsulfonate and sodium styryl sulfonate according to a proportion, adding the weighed materials into a continuously variable speed mixer (the rotating speed of the continuously variable speed mixer is 450-;
(3) and (3) carrying out reactive extrusion granulation on the mixed material on a double-screw extruder, wherein the length-diameter ratio of a screw is 40: and 1, the reactive extrusion temperature is 220 ℃, a vacuumizing device is arranged at the rear section of the extruder, the negative pressure is 0.2MPa, and unreacted small molecular substances are discharged through vacuumizing, so that the material is obtained.
Preparation example 3
The preparation raw materials of the antistatic agent graft described in this example include the following components in parts by weight: 85kg of injection molding grade high-fluidity ABS powder, 6kg of sodium allylsulfonate, 9kg of sodium styrene sulfonate, 0.4kg of initiator DCP and TAIC4 kg.
The preparation method of the antistatic agent graft described in this example comprises the following steps:
(1) weighing DCP and TAIC according to a proportion, dissolving the DCP by using acetone, wherein the proportion of the acetone to the DCP is (weight ratio) 5: 1, then mixing with TAIC;
(2) weighing ABS, sodium allylsulfonate and sodium styryl sulfonate according to a proportion, adding the weighed materials into a continuously variable speed mixer (the rotating speed of the continuously variable speed mixer is 450-;
(3) and (3) carrying out reactive extrusion granulation on the mixed material on a double-screw extruder, wherein the length-diameter ratio of a screw is 40: and 1, the reactive extrusion temperature is 200 ℃, a vacuumizing device is arranged at the rear section of the extruder, the negative pressure is 0.2MPa, and unreacted small molecular substances are discharged through vacuumizing to obtain the reactive extrusion material.
Examples 1 to 8
The following examples 1 to 8 according to the invention were used to prepare the permanently antistatic PVC resins described, the raw materials and material ratios of which are shown in Table 1 below. The preparation method of the PVC resin comprises the following steps: putting the selected amounts of the PVC resin, the organic tin stabilizer, the impact modifier, the processing modified resin, the antioxidant, the lubricant, the titanium dioxide and the carbon black into a high-speed mixer for mixing, wherein the rotating speed of the mixer is 800-1500 turns, the mixing temperature is 100-120 ℃, and the mixing time is 5-10 minutes; and then putting the mixed material into a low-speed mixer for cooling, adding the antistatic graft, mixing for 5 minutes, and discharging the material to obtain the antistatic graft.
In examples 1-8 below:
the product prepared in preparation example 3 is selected as the antistatic graft;
the PVC resin is QS-650 or S-700;
the organotin stabilizer is organotin stabilizer 2903;
the impact modifier is MBS-561 (Japanese Brillouin product);
the antioxidant is prepared from the following components in a mass ratio of 1: 1 a mixture of antioxidant 1010 and antioxidant 264;
the processing modified resin comprises styrene-acrylonitrile copolymer AS resin (brand PN 107);
the titanium dioxide is rutile type titanium dioxide;
the lubricants were stearic acid (examples 1-4), paraffin wax (examples 5-8), respectively.
Table 1 compositions of raw materials of examples 1 to 8 of the present invention
Figure GDA0003352608730000071
Comparative examples 1 to 6
The following comparative examples 1 to 6 of the present invention were used for the preparation of PVC resins, and the preparation raw materials and material ratios thereof are shown in table 2 below, and the specific preparation method was: weighing the materials according to a certain proportion, placing the materials into a high-speed mixer for mixing, wherein the rotating speed of the mixer is 800-1500 turns, the mixing temperature is 100-120 ℃, the mixing time is 5-10 minutes, then placing the mixed materials into a low-speed mixer for cooling, and discharging the materials after cooling to 40-50 ℃.
In comparative examples 1 to 6 below:
the PVC resin is QS-650 or S-700;
the organotin stabilizer is organotin stabilizer 2903;
the impact modifier is MBS-561 (Japanese Brillouin product);
the antioxidant is prepared from the following components in a mass ratio of 1: 1 a mixture of antioxidant 1010 and antioxidant 264;
the processing modified resin comprises styrene-acrylonitrile copolymer AS resin (brand PN 107);
the titanium dioxide is rutile type titanium dioxide;
the lubricant is stearic acid.
TABLE 2 comparative examples 1-6 raw material compositions
Figure GDA0003352608730000081
Note: the sodium allylsulfonate used in the comparative example was ATMER190 produced by gasoline purification of Switzerland, and MBS-561 was a Japanese Brillouin product.
Examples of the experiments
The PVC resin compositions obtained in examples 1 to 8 and comparative examples 1 to 6 were extruded at 160 ℃ to 200 ℃ into a phi 63 pipe using a twin-screw extruder, the surface resistivity was measured using a multimeter, a sample was taken from the pipe, and a tensile impact specimen was prepared and placed in a laboratory for 48 hours for testing. Specific performance test results are shown in table 3 below.
TABLE 3 results of performance test of examples and comparative examples
Figure GDA0003352608730000091
Note: the long-term antistatic properties were measured after the samples were left in an outdoor natural environment for 12 months.
As can be seen from the data in the table above, the long-term antistatic effect of the PVC product prepared by adopting the antistatic graft is obviously superior to that of the product prepared by the conventional antistatic additive in the prior art, the effective and durable antistatic effect can be achieved, and meanwhile, the pipe fitting composition has good rigidity and toughness and can meet the industrial application requirements.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (8)

1. The permanent antistatic PVC resin composition is characterized by comprising the following components in parts by weight: 100 parts of PVC resin, 1.0-3 parts of organic tin stabilizer, 10-15 parts of impact modifier, 5-10 parts of processing modified resin, 0.5-1.0 part of antioxidant, 0.8-2.5 parts of lubricant, 0-2.0 parts of titanium dioxide, 0-0.005 part of carbon black and 10-20 parts of antistatic graft;
the preparation raw materials of the antistatic graft comprise the following components in parts by weight: 80-90 parts of ABS powder, 4-8 parts of sodium allylsulfonate, 8-10 parts of sodium styrene sulfonate, 0.2-0.5 part of initiator and 5-78 parts of TAIC 3;
the preparation method of the antistatic graft comprises the following steps:
(1) dissolving a selected amount of the initiator in an organic solvent, adding a selected amount of the TAIC, and uniformly mixing to obtain a mixed solution;
(2) uniformly mixing a selected amount of ABS powder with sodium allylsulfonate and sodium styryl sulfonate, uniformly mixing with the mixed solution obtained in the step (1), and removing the organic solvent to obtain a mixed material;
(3) and carrying out reactive extrusion granulation on the obtained mixed material on a double-screw extruder to obtain the material.
2. The permanently antistatic PVC resin composition of claim 1, wherein in the step (1), the organic solvent comprises acetone, and the mass ratio of the initiator to the organic solvent is 1: 4-6.
3. The permanently antistatic PVC resin composition according to claim 2, wherein in said step (3), the screw length-diameter ratio of said twin-screw extruder is controlled to 40: 1, the reactive extrusion temperature is 160-.
4. A permanent antistatic PVC resin composition according to any one of claims 1 to 3, characterized in that:
the PVC resin is PVC resin with the polymerization degree of less than 800;
the organotin stabilizer is organotin stabilizer 2903;
the impact modifier is methacrylic acid-butadiene-styrene terpolymer MBS;
the antioxidant is antioxidant 1010 and/or antioxidant 264;
the processing modified resin is styrene-acrylonitrile copolymer AS resin;
the titanium dioxide is rutile type titanium dioxide;
the lubricant is stearic acid, paraffin wax, microcrystalline wax, PE wax and/or oxidized polyethylene wax.
5. A method for preparing the permanent antistatic PVC resin composition as defined in any one of claims 1-4, characterized in that the PVC resin, the organotin stabilizer, the impact modifier, the processing modified resin, the antioxidant, the lubricant, the titanium dioxide and the carbon black are taken according to selected parts by weight, mixed at a temperature of 100 ℃ and 120 ℃, and the obtained mixture is cooled and then added to the antistatic graft for mixing.
6. Use of the permanently antistatic PVC resin composition as claimed in any of claims 1 to 4 for the preparation of permanently antistatic PVC articles.
7. Use according to claim 6, characterized in that the PVC article is a PVC pipe product.
8. A permanently antistatic PVC article, characterized in that it is obtained from the permanently antistatic PVC resin composition according to any one of claims 1 to 4 by conventional processes.
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