CN114075360A - Chlorinated polyethylene rubber compound and preparation method thereof - Google Patents
Chlorinated polyethylene rubber compound and preparation method thereof Download PDFInfo
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- CN114075360A CN114075360A CN202210018971.3A CN202210018971A CN114075360A CN 114075360 A CN114075360 A CN 114075360A CN 202210018971 A CN202210018971 A CN 202210018971A CN 114075360 A CN114075360 A CN 114075360A
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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
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention relates to a chlorinated polyethylene rubber compound and a preparation method thereof, wherein the chlorinated polyethylene rubber compound comprises the following raw materials in parts by weight: 100-150 parts of chlorinated polyethylene rubber, 25-35 parts of modifier, 2-5 parts of vulcanizing agent, 1-2 parts of vulcanizing aid, 15-25 parts of carbon black, 3-5 parts of calcium-zinc stabilizer, 4-5 parts of crosslinking agent, 8-10 parts of plasticizer and 0.5-1.2 parts of stearic acid; the modifier is added for mixing, the modifier is a composite material of a carrier and xylan derivatives, the xylan derivatives are dispersed and enter the interlayer of the carrier to prepare the modifier, carrier hydrotalcite has an excellent ultraviolet physical shielding function, and the xylan derivatives can absorb ultraviolet rays passing through hydrotalcite sheets, so that the modifier has an ultraviolet absorption function and good ultraviolet reflection capacity, and can remarkably improve the ageing resistance of rubber mixtures when being used as the modifier.
Description
Technical Field
The invention belongs to the technical field of rubber production, and particularly relates to a chlorinated polyethylene rubber compound and a preparation method thereof.
Background
Compared with hoses, the rubber hose is formed by extrusion molding of high molecular chemical raw materials through processes such as vulcanization and the like. The hose structure is generally divided into: an inner rubber layer, an outer rubber layer and a framework layer (or called a middle layer). The inner rubber layer directly bears the abrasion and the erosion of the conveying medium; the outer rubber layer protects the inner body of the rubber hose from being damaged and eroded by the external environment; the framework layer is a bearing layer of the rubber pipe and endows the pipe body with strength and rigidity. The working pressure of the hose depends on the material and structure of the carcass.
The chlorinated polyethylene is a saturated high polymer material, is white powder in appearance, and is non-toxic and odorless. For the rubber hose, the rubber used for the outer rubber layer is required to have good ozone aging resistance, weather resistance and the like. The rubber used by the current rubber tube generally adopts chloroprene rubber, nitrile rubber or styrene butadiene rubber and the like, the rubber has a certain oil resistance but poor aging resistance, and ethylene propylene diene monomer rubber is adopted for some rubber tubes with very strict requirements but has higher cost.
Disclosure of Invention
In order to solve the technical problems, the invention provides a chlorinated polyethylene rubber compound and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the chlorinated polyethylene rubber compound comprises the following raw materials in parts by weight: 100-150 parts of chlorinated polyethylene rubber, 25-35 parts of modifier, 2-5 parts of vulcanizing agent, 1-2 parts of vulcanizing aid, 15-25 parts of carbon black, 3-5 parts of calcium-zinc stabilizer, 4-5 parts of crosslinking agent, 8-10 parts of plasticizer and 0.5-1.2 parts of stearic acid;
the modifier is prepared by the following steps:
step S1, calcining hydrotalcite at 550 ℃ for 2h, cooling, grinding into powder, adding the powder and potassium acetate into secondary distilled water, uniformly stirring for 30min, heating to 60 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a precursor, adding ammonium polyphosphate and the precursor into the secondary distilled water, grinding for 5min, heating to 65 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a carrier, controlling the weight ratio of hydrotalcite to potassium acetate to be 2: 1, and controlling the dosage ratio of the precursor, ammonium polyphosphate and secondary distilled water to be 4.5 g: 3-5 g: 100 mL;
in step S1, calcining hydrotalcite, and blending with potassium acetate in distilled water, where acetate can be used as a pillared precursor of intercalated hydrotalcite, and the acetate can prop open the calcined hydrotalcite interlayer to increase interlayer spacing, so as to prepare a precursor, and then blending with ammonium polyphosphate in distilled water, and inserting polyphosphoric acid as a pillared agent into the hydrotalcite interlayer through ion exchange, so as to prepare a hydrotalcite carrier with large interlayer spacing, and the polyphosphoric acid on the hydrotalcite carrier can also be used as a flame retardant, so as to improve the flame retardant property of the carrier;
step S2, adding the carrier into deionized water, heating to 60 ℃, stirring at a high speed to form a suspension, adding an alcoholic solution of the xylan derivative into the suspension, uniformly stirring, placing in a 500W microwave oven, heating to 100 ℃, stirring at a constant speed, reacting for 30min to obtain a colloidal liquid, then pouring into a three-neck flask, stirring at 140 ℃ and reacting for 12h, reducing pressure and carrying out suction filtration after the reaction is finished, washing with deionized water until the filtrate is neutral, and carrying out vacuum drying to obtain the modifier, wherein the dosage ratio of the carrier, the deionized water and the alcoholic solution of the xylan derivative is controlled to be 10 g: 200 mL: 100 mL.
In the step S2, the carrier is dispersed in water, the alcoholic solution of the xylan derivative is added, the xylan derivative is dispersed and enters the interlayer of the carrier, the modifier is prepared, the modifier is a composite material, the hydrotalcite has an excellent ultraviolet physical shielding function, and the xylan derivative can absorb ultraviolet rays passing through hydrotalcite sheets, so that the modifier has an ultraviolet absorption function and good ultraviolet reflection capability, and the anti-aging performance of the rubber compound can be obviously improved when the xylan derivative is used as the modifier.
Further: the alcohol solution of the xylan derivative is formed by mixing the xylan derivative and absolute ethyl alcohol according to the weight ratio of 1: 10.
Further: the xylan derivative is prepared by the following steps:
step S21, adding xylan into dimethyl sulfoxide, adding bromobutane and pyridine after magnetic stirring for 30min, heating to 65 ℃, keeping the temperature for reaction for 4h, adding absolute ethyl alcohol while stirring after the reaction is finished, continuously stirring until no precipitate is generated, forming suspension, standing for 10h, filtering, extracting a filter cake for 48h, taking out solid, drying in vacuum, and grinding to obtain an intermediate 1, wherein the dosage ratio of xylan to dimethyl sulfoxide to bromobutane to pyridine is controlled to be 1 g: 50-60 mL: 0.5-0.8 g: 1.2 mL;
step S21, adding xylan into dimethyl sulfoxide as a solvent, adding pyridine as a catalyst, and carrying out alkylation modification on xylan and bromobutane under catalysis to prepare an intermediate 1 which is alkyl-grafted xylan;
step S22, adding the intermediate 1 into N, N-dimethylformamide, stirring at a constant speed for 15min, heating to 60 ℃, adding triethylamine and cinnamoyl chloride solution, stirring at a constant speed and reacting for 4h, adding absolute ethyl alcohol after the reaction is finished, stirring at a constant speed until no precipitate is generated, standing for 10h, performing suction filtration, and performing vacuum drying on a filter cake to obtain the xylan derivative, wherein the dosage ratio of the intermediate 1, N-dimethylformamide, triethylamine and cinnamoyl chloride solution is controlled to be 0.3-0.5g, 10mL, 0.35-0.45g and 0.15-0.2 g.
In the step S22, the intermediate 1 is added into a high-polarity solvent N, N-dimethylformamide, and xylan is subjected to alkylation modification, so that the dispersion performance of hemicellulose in the intermediate 1 can be improved, the intermediate 1 can react with cinnamoyl chloride under a homogeneous phase, triethylamine is added as an acid-binding agent, cinnamoyl groups are grafted on the intermediate 1, a xylan derivative is prepared, and the xylan derivative is endowed with ultraviolet absorption performance.
Further: the cinnamoyl chloride solution is prepared by mixing cinnamoyl chloride and N, N-dimethylformamide according to the weight ratio of 1: 10.
The preparation method of the chlorinated polyethylene rubber compound comprises the following steps:
adding chlorinated polyethylene rubber into an internal mixer, then sequentially adding a calcium-zinc stabilizer, a modifier and stearic acid, carrying out internal mixing for 3-4min, then adding carbon black and a plasticizer, continuing internal mixing for 1-2min, then adding a cross-linking agent, carrying out internal mixing for 1-2min, finally adding a vulcanizing agent and a vulcanizing assistant, carrying out internal mixing for 1-2min to prepare a rubber material, discharging, carrying out triangular bag making, thin passing, calendering and sheet making in an open mill to prepare a rubber compound, and controlling the internal mixing temperature to be 80-100 ℃.
The invention has the beneficial effects that:
the invention takes chlorinated polyethylene rubber as matrix rubber, adds a modifier for mixing, the modifier is a composite material of a carrier and a xylan derivative, the xylan derivative is dispersed and enters the interlayer of the carrier to prepare the modifier, the carrier hydrotalcite is a composite material, the hydrotalcite per se has excellent ultraviolet physical shielding function, the xylan derivative can absorb ultraviolet rays passing through a hydrotalcite sheet layer, so that the modifier has both ultraviolet absorption function and good ultraviolet reflection capability, the anti-aging performance of mixed rubber can be obviously improved by being taken as the modifier, and good flame retardant performance is endowed to the mixed rubber, and the xylan derivative takes alkyl-grafted xylan as a matrix, and the dispersibility of hemicellulose in an intermediate 1 can be improved by carrying out alkylation modification on the xylan, so that the intermediate 1 can react with cinnamoyl chloride under homogeneous phase, triethylamine is added to serve as an acid-binding agent, the cinnamoyl group is grafted on the intermediate 1, the xylan derivative is prepared, ultraviolet absorption performance is endowed to the xylan derivative, and ethylene propylene diene monomer is not added, so that cost can be reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The xylan derivative is prepared by the following steps:
step S21, adding xylan into dimethyl sulfoxide, adding bromobutane and pyridine after magnetic stirring for 30min, heating to 65 ℃, keeping the temperature for reaction for 4h, adding absolute ethyl alcohol while stirring after the reaction is finished, continuing stirring until no precipitate is generated, forming suspension, standing for 10h, filtering, extracting a filter cake for 48h, taking out solid, drying in vacuum, and grinding to obtain an intermediate 1, wherein the dosage ratio of xylan to dimethyl sulfoxide to bromobutane to pyridine is controlled to be 1 g: 50 mL: 0.5 g: 1.2 mL;
step S22, adding the intermediate 1 into N, N-dimethylformamide, stirring at a constant speed for 15min, heating to 60 ℃, adding triethylamine and cinnamoyl chloride solution, stirring at a constant speed and reacting for 4h, adding absolute ethyl alcohol after the reaction is finished, stirring at a constant speed until no precipitate is generated, standing for 10h, performing suction filtration, and performing vacuum drying on a filter cake to obtain the xylan derivative, wherein the dosage ratio of the intermediate 1, N-dimethylformamide, triethylamine and cinnamoyl chloride solution is controlled to be 0.3 g: 10 mL: 0.35 g: 0.15 g.
The cinnamoyl chloride solution is prepared by mixing cinnamoyl chloride and N, N-dimethylformamide according to the weight ratio of 1: 10.
Example 2
The xylan derivative is prepared by the following steps:
step S21, adding xylan into dimethyl sulfoxide, adding bromobutane and pyridine after magnetic stirring for 30min, heating to 65 ℃, keeping the temperature for reaction for 4h, adding absolute ethyl alcohol while stirring after the reaction is finished, continuing stirring until no precipitate is generated, forming suspension, standing for 10h, filtering, extracting a filter cake for 48h, taking out solid, drying in vacuum, and grinding to obtain an intermediate 1, wherein the dosage ratio of xylan to dimethyl sulfoxide to bromobutane to pyridine is controlled to be 1 g: 55 mL: 0.6 g: 1.2 mL;
step S22, adding the intermediate 1 into N, N-dimethylformamide, stirring at a constant speed for 15min, heating to 60 ℃, adding triethylamine and cinnamoyl chloride solution, stirring at a constant speed and reacting for 4h, adding absolute ethyl alcohol after the reaction is finished, stirring at a constant speed until no precipitate is generated, standing for 10h, performing suction filtration, and performing vacuum drying on a filter cake to obtain the xylan derivative, wherein the dosage ratio of the intermediate 1, N-dimethylformamide, triethylamine and cinnamoyl chloride solution is controlled to be 0.4 g: 10 mL: 0.40 g: 0.15 g.
The cinnamoyl chloride solution is prepared by mixing cinnamoyl chloride and N, N-dimethylformamide according to the weight ratio of 1: 10.
Example 3
The xylan derivative is prepared by the following steps:
step S21, adding xylan into dimethyl sulfoxide, adding bromobutane and pyridine after magnetic stirring for 30min, heating to 65 ℃, keeping the temperature for reaction for 4h, adding absolute ethyl alcohol while stirring after the reaction is finished, continuously stirring until no precipitate is generated, forming suspension, standing for 10h, filtering, extracting a filter cake for 48h, taking out solid, drying in vacuum, and grinding to obtain an intermediate 1, wherein the dosage ratio of xylan to dimethyl sulfoxide to bromobutane to pyridine is controlled to be 1 g: 60 mL: 0.8 g: 1.2 mL;
step S22, adding the intermediate 1 into N, N-dimethylformamide, stirring at a constant speed for 15min, heating to 60 ℃, adding triethylamine and cinnamoyl chloride solution, stirring at a constant speed and reacting for 4h, adding absolute ethyl alcohol after the reaction is finished, stirring at a constant speed until no precipitate is generated, standing for 10h, performing suction filtration, and performing vacuum drying on a filter cake to obtain the xylan derivative, wherein the dosage ratio of the intermediate 1, N-dimethylformamide, triethylamine and cinnamoyl chloride solution is controlled to be 0.5 g: 10 mL: 0.45 g: 0.2 g.
The cinnamoyl chloride solution is prepared by mixing cinnamoyl chloride and N, N-dimethylformamide according to the weight ratio of 1: 10.
Example 4
The modifier is prepared by the following steps:
step S1, calcining hydrotalcite at 550 ℃ for 2h, cooling, grinding into powder, adding the powder and potassium acetate into secondary distilled water, uniformly stirring for 30min, heating to 60 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a precursor, adding ammonium polyphosphate and the precursor into the secondary distilled water, grinding for 5min, heating to 65 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a carrier, controlling the weight ratio of hydrotalcite to potassium acetate to be 2: 1, and controlling the dosage ratio of the precursor, ammonium polyphosphate and secondary distilled water to be 4.5 g: 3 g: 100 mL;
step S2, adding the carrier into deionized water, heating to 60 ℃, stirring at a high speed to form a suspension, adding an alcoholic solution of the xylan derivative into the suspension, uniformly stirring, placing in a 500W microwave oven, heating to 100 ℃, stirring at a constant speed, reacting for 30min to obtain a colloidal liquid, then pouring into a three-neck flask, stirring at 140 ℃ and reacting for 12h, reducing pressure and carrying out suction filtration after the reaction is finished, washing with deionized water until the filtrate is neutral, and carrying out vacuum drying to obtain the modifier, wherein the dosage ratio of the carrier, the deionized water and the alcoholic solution of the xylan derivative is controlled to be 10 g: 200 mL: 100 mL.
The alcohol solution of the xylan derivative is formed by mixing the xylan derivative and absolute ethyl alcohol according to the weight ratio of 1: 10.
Example 5
The modifier is prepared by the following steps:
step S1, calcining hydrotalcite at 550 ℃ for 2h, cooling, grinding into powder, adding the powder and potassium acetate into secondary distilled water, uniformly stirring for 30min, heating to 60 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a precursor, adding ammonium polyphosphate and the precursor into the secondary distilled water, grinding for 5min, heating to 65 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a carrier, controlling the weight ratio of hydrotalcite to potassium acetate to be 2: 1, and controlling the dosage ratio of the precursor, ammonium polyphosphate and secondary distilled water to be 4.5 g: 4 g: 100 mL;
step S2, adding the carrier into deionized water, heating to 60 ℃, stirring at a high speed to form a suspension, adding an alcoholic solution of the xylan derivative into the suspension, uniformly stirring, placing in a 500W microwave oven, heating to 100 ℃, stirring at a constant speed, reacting for 30min to obtain a colloidal liquid, then pouring into a three-neck flask, stirring at 140 ℃ and reacting for 12h, reducing pressure and carrying out suction filtration after the reaction is finished, washing with deionized water until the filtrate is neutral, and carrying out vacuum drying to obtain the modifier, wherein the dosage ratio of the carrier, the deionized water and the alcoholic solution of the xylan derivative is controlled to be 10 g: 200 mL: 100 mL.
The alcohol solution of the xylan derivative is formed by mixing the xylan derivative and absolute ethyl alcohol according to the weight ratio of 1: 10.
Example 6
The modifier is prepared by the following steps:
step S1, calcining hydrotalcite at 550 ℃ for 2h, cooling, grinding into powder, adding the powder and potassium acetate into secondary distilled water, uniformly stirring for 30min, heating to 60 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a precursor, adding ammonium polyphosphate and the precursor into the secondary distilled water, grinding for 5min, heating to 65 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a carrier, controlling the weight ratio of hydrotalcite to potassium acetate to be 2: 1, and controlling the dosage ratio of the precursor, ammonium polyphosphate and secondary distilled water to be 4.5 g: 5 g: 100 mL;
step S2, adding the carrier into deionized water, heating to 60 ℃, stirring at a high speed to form a suspension, adding an alcoholic solution of the xylan derivative into the suspension, uniformly stirring, placing in a 500W microwave oven, heating to 100 ℃, stirring at a constant speed, reacting for 30min to obtain a colloidal liquid, then pouring into a three-neck flask, stirring at 140 ℃ and reacting for 12h, reducing pressure and carrying out suction filtration after the reaction is finished, washing with deionized water until the filtrate is neutral, and carrying out vacuum drying to obtain the modifier, wherein the dosage ratio of the carrier, the deionized water and the alcoholic solution of the xylan derivative is controlled to be 10 g: 200 mL: 100 mL.
The alcohol solution of the xylan derivative is formed by mixing the xylan derivative and absolute ethyl alcohol according to the weight ratio of 1: 10.
Example 7
The chlorinated polyethylene rubber compound comprises the following raw materials in parts by weight: 100 parts of chlorinated polyethylene rubber, 25 parts of modifier, 2 parts of dicumyl peroxide, 1 part of triallyl isocyanurate, 15 parts of carbon black, 3 parts of calcium-zinc stabilizer, 4 parts of benzoyl peroxide, 8 parts of dioctyl adipate and 0.5 part of stearic acid;
adding chlorinated polyethylene rubber into an internal mixer, then sequentially adding a calcium-zinc stabilizer, a modifier and stearic acid, carrying out internal mixing for 3min, then adding carbon black and dioctyl adipate, carrying out internal mixing for 1min, then adding benzoyl peroxide, carrying out internal mixing for 1min, finally adding dicumyl peroxide and triallyl isocyanurate, carrying out internal mixing for 1min to obtain a rubber material, discharging, carrying out triangular bag making, thin passing, calendering and sheet making in an open mill to obtain the rubber compound, and controlling the internal mixing temperature to be 80 ℃.
Example 8
The chlorinated polyethylene rubber compound comprises the following raw materials in parts by weight: 120 parts of chlorinated polyethylene rubber, 30 parts of a modifier, 3 parts of dicumyl peroxide, 1 part of triallyl isocyanurate, 20 parts of carbon black, 4 parts of a calcium-zinc stabilizer, 5 parts of benzoyl peroxide, 10 parts of dioctyl adipate and 1 part of stearic acid;
adding chlorinated polyethylene rubber into an internal mixer, then sequentially adding a calcium-zinc stabilizer, a modifier and stearic acid, carrying out internal mixing for 3min, then adding carbon black and dioctyl adipate, carrying out internal mixing for 1min, then adding benzoyl peroxide, carrying out internal mixing for 1min, finally adding dicumyl peroxide and triallyl isocyanurate, carrying out internal mixing for 1min to obtain a rubber material, discharging, carrying out triangular bag making, thin passing, calendering and sheet making in an open mill to obtain the rubber compound, and controlling the internal mixing temperature to be 80 ℃.
Example 9
The chlorinated polyethylene rubber compound comprises the following raw materials in parts by weight: 150 parts of chlorinated polyethylene rubber, 35 parts of modifier, 5 parts of dicumyl peroxide, 2 parts of triallyl isocyanurate, 25 parts of carbon black, 5 parts of calcium-zinc stabilizer, 5 parts of benzoyl peroxide, 10 parts of dioctyl adipate and 1.2 parts of stearic acid;
adding chlorinated polyethylene rubber into an internal mixer, then sequentially adding a calcium-zinc stabilizer, a modifier and stearic acid, carrying out internal mixing for 4min, then adding carbon black and dioctyl adipate, carrying out internal mixing for 2min, then adding benzoyl peroxide, carrying out internal mixing for 2min, finally adding dicumyl peroxide and triallyl isocyanurate, carrying out internal mixing for 2min to obtain a rubber material, discharging, carrying out triangular bag making, thin passing, calendering and sheet making in an open mill to obtain the rubber compound, and controlling the internal mixing temperature to be 100 ℃.
Comparative example 1
This comparative example compares to example 7 without the addition of a modifier.
Comparative example 2
In this comparative example, the modifier was the support prepared in example 4, in comparison to example 7.
The rubber mixtures prepared in examples 7 to 9 and comparative examples 1 to 2 were tested, and the results are shown in the following tables 1 to 2:
TABLE 1
From Table 1 above, it can be seen that the compounds prepared in examples 7 to 9 according to the invention have better processability with reduced Mooney viscosity without affecting the mechanical properties compared to comparative example 1.
TABLE 2
As can be seen from Table 2 above, the decrease in mechanical properties under UV irradiation was lower at 504h and 1008h than in comparative examples 1-2, so that the compounds prepared in examples 7-9 according to the invention had excellent UV aging resistance.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (5)
1. Chlorinated polyethylene rubber compound, which is characterized in that: the feed comprises the following raw materials in parts by weight: 100-150 parts of chlorinated polyethylene rubber, 25-35 parts of modifier, 2-5 parts of vulcanizing agent, 1-2 parts of vulcanizing aid, 15-25 parts of carbon black, 3-5 parts of calcium-zinc stabilizer, 4-5 parts of crosslinking agent, 8-10 parts of plasticizer and 0.5-1.2 parts of stearic acid;
the modifier is prepared by the following steps:
step S1, calcining hydrotalcite at 550 ℃ for 2h, cooling, grinding into powder, adding the powder and potassium acetate into secondary distilled water, uniformly stirring for 30min, heating to 60 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a precursor, adding ammonium polyphosphate and the precursor into the secondary distilled water, grinding for 5min, heating to 65 ℃, preserving heat, stirring for 3h, filtering, washing and drying to obtain a carrier;
step S2, adding a carrier into deionized water, heating to 60 ℃, stirring at a high speed to form a suspension, adding an alcoholic solution of a xylan derivative into the suspension, uniformly stirring, placing in a 500W microwave oven, heating to 100 ℃, stirring at a constant speed, reacting for 30min to obtain a colloidal liquid, then pouring into a three-neck flask, stirring at 140 ℃ and reacting for 12h, reducing pressure and performing suction filtration after the reaction is finished, washing with deionized water until the filtrate is neutral, and performing vacuum drying to obtain a modifier;
the xylan derivative is prepared by the following steps:
step S21, adding xylan into dimethyl sulfoxide, adding bromobutane and pyridine after magnetic stirring for 30min, heating to 65 ℃, keeping the temperature for reaction for 4h, adding absolute ethyl alcohol while stirring after the reaction is finished, continuously stirring until no precipitate is generated, forming suspension, standing for 10h, filtering, extracting a filter cake for 48h, taking out solid, drying in vacuum, and grinding to obtain an intermediate 1, wherein the dosage ratio of xylan to dimethyl sulfoxide to bromobutane to pyridine is controlled to be 1 g: 50-60 mL: 0.5-0.8 g: 1.2 mL;
step S22, adding the intermediate 1 into N, N-dimethylformamide, stirring at a constant speed for 15min, heating to 60 ℃, adding triethylamine and cinnamoyl chloride solution, stirring at a constant speed and reacting for 4h, adding absolute ethyl alcohol after the reaction is finished, stirring at a constant speed until no precipitate is generated, standing for 10h, performing suction filtration, and performing vacuum drying on a filter cake to obtain a xylan derivative, wherein the dosage ratio of the intermediate 1, N-dimethylformamide, triethylamine and cinnamoyl chloride solution is controlled to be 0.3-0.5g, 10mL, 0.35-0.45g and 0.15-0.2 g;
the cinnamoyl chloride solution is prepared by mixing cinnamoyl chloride and N, N-dimethylformamide according to the weight ratio of 1: 10.
2. A chlorinated polyethylene mix according to claim 1, characterized in that: the alcohol solution of the xylan derivative is formed by mixing the xylan derivative and absolute ethyl alcohol according to the weight ratio of 1: 10.
3. A chlorinated polyethylene mix according to claim 1, characterized in that: in the step S1, the weight ratio of hydrotalcite to potassium acetate is controlled to be 2: 1, the dosage ratio of the precursor, ammonium polyphosphate and secondary distilled water is 4.5 g: 3-5 g: 100mL, and the dosage ratio of the carrier, deionized water and the alcoholic solution of the xylan derivative is controlled to be 10 g: 200 mL: 100mL in the step S2.
4. A method for preparing a chlorinated polyethylene compound according to claim 1, characterized in that: the method comprises the following steps:
adding chlorinated polyethylene rubber into an internal mixer, then sequentially adding a calcium-zinc stabilizer, a modifier and stearic acid, carrying out internal mixing for 3-4min, then adding carbon black and a plasticizer, continuing internal mixing for 1-2min, then adding a cross-linking agent, carrying out internal mixing for 1-2min, finally adding a vulcanizing agent and a vulcanizing assistant, carrying out internal mixing for 1-2min to obtain a rubber material, discharging, carrying out triangular wrapping, thin passing in an open mill, calendering and sheeting to obtain the rubber compound.
5. A method of preparing a chlorinated polyethylene compound according to claim 4, characterized in that: the banburying temperature is controlled to be 80-100 ℃.
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| CN116574338A (en) * | 2023-07-12 | 2023-08-11 | 潍坊潍星联合橡塑有限公司 | High weather-resistant chlorinated polyethylene cable sheath material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116574338A (en) * | 2023-07-12 | 2023-08-11 | 潍坊潍星联合橡塑有限公司 | High weather-resistant chlorinated polyethylene cable sheath material |
| CN116574338B (en) * | 2023-07-12 | 2023-09-08 | 潍坊潍星联合橡塑有限公司 | High weather-resistant chlorinated polyethylene cable sheath material |
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| CN114075360B (en) | 2022-03-25 |
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