A process for the preparation of a high strength chlorinated polyethylene resin
By preparing chlorinated polyethylene resin through specific combinations and processes, the problems of low strength and poor corrosion resistance were solved, achieving high strength and high toughness, while improving the corrosion resistance of chlorinated polyethylene resin.
Patent Information
- Application Number
- CN202511441258.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-10
- Publication Date
- 2025-12-30
- Estimated Expiration
- 2045-10-10
AI Technical Summary
Existing chlorinated polyethylene resin preparation technologies suffer from low strength and poor corrosion resistance, resulting in insufficient performance, especially in applications such as chemical corrosion-resistant pipelines and high-end automotive weather-resistant components.
Chlorinated polyethylene resin was prepared by combining chlorinated polyethylene, chlorinated polyethylene graft copolymer, modified nano-silica, polyamide 6 micro powder and mixed solvent through specific process steps, including the preparation of chlorinated polyethylene graft copolymer, solution mixing and dispersion and crosslinking reaction, and finally obtained high-strength chlorinated polyethylene resin.
The prepared chlorinated polyethylene resin exhibited a notched impact strength of 26.8-31.2 KJ/m2, a tensile strength of 37.2-39.1 MPa, and an elongation at break of 676-713% at 23℃. It also showed excellent corrosion resistance in toluene and NaCl solutions, with mass growth rates of 1.25-1.79% and 0.27-0.38%, respectively.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of chlorinated polyethylene preparation technology, and specifically to a method for preparing high-strength chlorinated polyethylene resin. Background Technology
[0002] Chlorinated polyethylene resin, as an important polymer modified material, is widely used in wire and cable sheathing, building material pipes, automotive seals, and anti-corrosion coatings due to its excellent weather resistance, processability, and compatibility with other resins. With the continuous improvement of material performance requirements in the industrial sector, especially in applications such as chemical anti-corrosion pipelines, high-end automotive weather-resistant components, and sealing materials for marine engineering, higher standards are being set for the mechanical properties and corrosion resistance of chlorinated polyethylene resin.
[0003] However, existing chlorinated polyethylene resin preparation technologies still have significant limitations: in the traditional aqueous suspension method, the chlorination reaction is not uniform, and localized low-chlorine content areas easily form within the resin, leading to large fluctuations in mechanical properties and generally low tensile strength. Simultaneously, plasticizers or fillers often added to improve processing fluidity reduce the bonding force between resin molecular chains, thus decreasing corrosion resistance. Prior art CN114213561B discloses a method for preparing high-rigidity chlorinated polyethylene resin. While this prior art improves rigidity and impact resistance through "secondary polymerization + pulsed current post-treatment," the increase in tensile strength is limited, and a balance between strength and toughness is lacking. Prior art CN118459902A discloses a method for preparing high-elongation-at-break chlorinated polyethylene. The core objective of this prior art is to improve the elongation-at-break of chlorinated polyethylene, but it lacks improvements in strength and corrosion resistance.
[0004] In summary, although the existing technical solutions have improved some properties of chlorinated polyethylene resin to a certain extent, the following technical problems still exist: low strength and poor corrosion resistance. Summary of the Invention
[0005] In order to solve the above-mentioned problems in the prior art, the present invention provides a method for preparing high-strength chlorinated polyethylene resin, and achieves the following objective: to prepare high-strength chlorinated polyethylene resin with excellent corrosion resistance.
[0006] To achieve the above objectives, the following technical solution is adopted:
[0007] A method for preparing high-strength chlorinated polyethylene resin, comprising the following raw materials by weight: 50-65 parts chlorinated polyethylene, 8-13 parts chlorinated polyethylene graft copolymer, 4-5 parts polyamide 6 micro powder, 8-10 parts modified nano silica, 65-75 parts mixed solvent, and 0.8-1 parts hexamethylene diisocyanate.
[0008] The chlorine content of the chlorinated polyethylene is 30%-35% (by mass).
[0009] The chlorinated polyethylene graft copolymer is an allyl glycidyl ether graft copolymer of chlorinated polyethylene.
[0010] The modified nano-silica is nano-silica with a silane coupling agent surface modified, and the silane coupling agent selected is KH560.
[0011] The mixed solvent is obtained by mixing toluene and dioxane, with a mass ratio of toluene to dioxane of (80-85):(15-20).
[0012] The particle size of the polyamide 6 micro powder is 1-10 μm.
[0013] A method for preparing high-strength chlorinated polyethylene resin, comprising the following steps:
[0014] Step 1: Preparation of chlorinated polyethylene graft copolymer
[0015] Add chlorinated polyethylene to anhydrous toluene at a mass ratio of chlorinated polyethylene to anhydrous toluene of 1:(14-16). Purge with nitrogen gas at a flow rate of 50 mL / min for 10-15 min. Then start stirring at 200-300 rpm and heat to 80-90℃, holding for 1-2 h. Add allyl glycidyl ether at a mass ratio of (1-3):2 to chlorinated polyethylene. Add an initiator at a mass of 1-2% of the chlorinated polyethylene mass. Stir for 10-20 min at a stirring speed of 300-400 rpm. 00 rpm; then heat to 110-130℃, increase stirring speed to 400-500 rpm, reflux reaction for 4-6 h under nitrogen protection to obtain reaction solution; slowly cool to 60-70℃, slowly pour reaction solution into anhydrous ethanol, the volume ratio of reaction solution to anhydrous ethanol is 1:(5-6), let stand for 30-40 min, filter to collect precipitate, wash with anhydrous ethanol 3-4 times, then vacuum dry at -0.095 MPa and 70-80℃ for 8-12 h to obtain chlorinated polyethylene graft copolymer.
[0016] The chlorinated polyethylene has a chlorine content of 30%-35% (by mass); the initiator is dicumyl peroxide.
[0017] Step 2: Solution mixing and dispersion and cross-linking reaction
[0018] Add the modified nano-silica to 1 / 6 volume of the mixed solvent, stir for 30-40 minutes at a stirring speed of 800-900 rpm, and then sonicate for 1-1.5 hours at a power of 400-500W to form a silica suspension.
[0019] Add the dried chlorinated polyethylene to the remaining 5 / 6 volume of the mixed solvent, purge with nitrogen at a flow rate of 0.5-0.6 L / min, heat to 120-130℃, and stir until the chlorinated polyethylene is completely dissolved; then cool to 100-110℃, add the chlorinated polyethylene graft copolymer, and stir for 1-1.5 h at a speed of 500-600 rpm; add the dried polyamide 6 micro powder and continue stirring for 30-40 min; then slowly add the silica suspension, heat to 110-120℃, increase the stirring speed to 800-900 rpm, and stir for 1.5-2 h, while simultaneously turning on ultrasonic-assisted dispersion at a power of 200-300 W, sonicating for 10 min every 30 min; add hexamethylene diisocyanate, reduce the stirring speed to 600-700 rpm, and stir the reaction for 2-2.5 h to obtain the reaction mixture.
[0020] Step 3: Obtain chlorinated polyethylene resin
[0021] Cool the reaction mixture to 50-60℃ and slowly pour it into acetone while stirring at 1000-1100 rpm. The volume ratio of the reaction mixture to acetone is 1:(5-8). Let it stand for 30-40 minutes, filter and collect the precipitate, wash it with acetone 3-4 times, and then vacuum dry it at a vacuum degree of -0.095 MPa and a temperature of 70-80℃ for 10-12 hours to obtain chlorinated polyethylene resin.
[0022] The beneficial effects of this invention are as follows:
[0023] (1) The high-strength chlorinated polyethylene resin of the present invention has excellent mechanical properties. The notched impact strength of the prepared chlorinated polyethylene resin at 23°C is 26.8-31.2 KJ / m. 2 The tensile strength reaches 37.2-39.1 MPa, and the elongation at break is 676-713%.
[0024] (2) The high-strength chlorinated polyethylene resin of the present invention has excellent corrosion resistance. The prepared chlorinated polyethylene resin has a mass growth rate of 1.25-1.79% after being soaked in toluene for 48 hours; and a mass growth rate of 0.27-0.38% after being soaked in 5% NaCl solution for 48 hours. Attached Figure Description
[0025] Appendix Figure 1 This is the Fourier transform infrared spectrum of chlorinated polyethylene and chlorinated polyethylene graft copolymer. Detailed Implementation
[0026] To make the objectives, technical solutions, and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below. It should be understood that the specific embodiments described herein are for illustrative and explanatory purposes only and are not intended to limit the scope of the invention.
[0027] Example 1: A method for preparing high-strength chlorinated polyethylene resin
[0028] A method for preparing high-strength chlorinated polyethylene resin, comprising the following raw materials by weight: 50 parts chlorinated polyethylene, 13 parts chlorinated polyethylene graft copolymer, 5 parts polyamide 6 micro powder, 10 parts modified nano silica, 65 parts mixed solvent, and 0.8 parts hexamethylene diisocyanate.
[0029] The chlorine content of the chlorinated polyethylene is 30%-35% (by mass).
[0030] The modified nano-silica is nano-silica with a silane coupling agent surface modified, and the silane coupling agent selected is KH560.
[0031] The mixed solvent is obtained by mixing toluene and dioxane, with a mass ratio of toluene to dioxane of 80:20; the particle size of the polyamide 6 micro powder is 1-10 μm.
[0032] A method for preparing high-strength chlorinated polyethylene resin, comprising the following steps:
[0033] Step 1: Preparation of chlorinated polyethylene graft copolymer
[0034] Chlorinated polyethylene was added to anhydrous toluene at a mass ratio of 1:14. Nitrogen gas was introduced at a flow rate of 50 mL / min for 10 min, followed by stirring at 200 rpm. The temperature was raised to 80°C and maintained for 2 h. Allyl glycidyl ether was added at a mass ratio of 1:2 to chlorinated polyethylene. An initiator was added at a concentration of 1% of the mass of chlorinated polyethylene. The mixture was stirred for 10 min at 400 rpm. The temperature was then raised to 110°C, and the stirring speed was increased to 500 rpm. The mixture was refluxed under nitrogen protection for 6 h to obtain a reaction solution. The temperature was slowly lowered to 60°C, and the reaction solution was slowly poured into anhydrous ethanol at a volume ratio of 1:5. The mixture was allowed to stand for 30 min, and the precipitate was collected by filtration. The precipitate was washed three times with anhydrous ethanol and then vacuum dried at -0.095 MPa and 70°C for 12 h to obtain the chlorinated polyethylene graft copolymer.
[0035] The chlorinated polyethylene has a chlorine content of 30%-35% (by mass); the initiator is dicumyl peroxide.
[0036] Step 2: Solution mixing and dispersion and cross-linking reaction
[0037] Modified nano-silica was added to 1 / 6 volume of the mixed solvent, stirred for 30 minutes at a stirring speed of 900 rpm, and then sonicated for 1 hour at a power of 500 W to form a silica suspension.
[0038] Dry chlorinated polyethylene was added to the remaining 5 / 6 volume of the mixed solvent, nitrogen gas was introduced to purge air at a flow rate of 0.5 L / min, the temperature was raised to 120 °C, and the mixture was stirred until the chlorinated polyethylene was completely dissolved. Then the temperature was lowered to 100 °C, the chlorinated polyethylene graft copolymer was added, and the mixture was stirred for 1 h at a speed of 600 rpm. Dry polyamide 6 micro powder was added, and the mixture was stirred for another 30 min. Then silica suspension was slowly added, the temperature was raised to 110 °C, the stirring speed was increased to 900 rpm, and the mixture was stirred for 1.5 h. At the same time, ultrasonic-assisted dispersion was turned on at a power of 200 W, and ultrasonication was performed for 10 min every 30 min. Hexamethylene diisocyanate was added, the stirring speed was reduced to 700 rpm, and the mixture was stirred for 2 h to obtain the reaction mixture.
[0039] Step 3: Obtain chlorinated polyethylene resin
[0040] The reaction mixture was cooled to 50°C and slowly poured into acetone while stirring at 1000 rpm. The volume ratio of the reaction mixture to acetone was 1:5. After standing for 40 minutes, the precipitate was collected by filtration, washed three times with acetone, and then vacuum dried at -0.095 MPa and 70°C for 12 hours to obtain chlorinated polyethylene resin.
[0041] Example 2: A method for preparing high-strength chlorinated polyethylene resin
[0042] A method for preparing a high-strength chlorinated polyethylene resin, comprising the following raw materials by weight: 60 parts chlorinated polyethylene, 10 parts chlorinated polyethylene graft copolymer, 5 parts polyamide 6 micro powder, 9 parts modified nano silica, 70 parts mixed solvent, and 1 part hexamethylene diisocyanate.
[0043] The chlorine content of the chlorinated polyethylene is 30%-35% (by mass).
[0044] The modified nano-silica is nano-silica with a silane coupling agent surface modified, and the silane coupling agent selected is KH560.
[0045] The mixed solvent is obtained by mixing toluene and dioxane, with a mass ratio of toluene to dioxane of 83:18.
[0046] The particle size of the polyamide 6 micro powder is 1-10 μm.
[0047] A method for preparing high-strength chlorinated polyethylene resin, comprising the following steps:
[0048] Step 1: Preparation of chlorinated polyethylene graft copolymer
[0049] Chlorinated polyethylene was added to anhydrous toluene at a mass ratio of 1:15. Nitrogen gas was introduced at a flow rate of 50 mL / min for 12 min, followed by stirring at 300 rpm. The temperature was raised to 85°C and maintained for 1.5 h. Allyl glycidyl ether was added at a mass ratio of 2:2 to chlorinated polyethylene. An initiator was added at a concentration of 1.5% of the mass of chlorinated polyethylene. The mixture was stirred for 15 min at 400 rpm. The temperature was then raised to 120°C, and the stirring speed was increased to 500 rpm. The mixture was refluxed under nitrogen protection for 5 h to obtain a reaction solution. The temperature was slowly lowered to 70°C, and the reaction solution was slowly poured into anhydrous ethanol at a volume ratio of 1:6. The mixture was allowed to stand for 40 min, and the precipitate was collected by filtration. The precipitate was washed four times with anhydrous ethanol and then vacuum dried at -0.095 MPa and 80°C for 10 h to obtain the chlorinated polyethylene graft copolymer.
[0050] The chlorinated polyethylene has a chlorine content of 30%-35% (by mass); the initiator is dicumyl peroxide.
[0051] Step 2: Solution mixing and dispersion and cross-linking reaction
[0052] Modified nano-silica was added to 1 / 6 volume of the mixed solvent, stirred for 40 min at 900 rpm, and then sonicated for 1.5 h at 400 W to form a silica suspension.
[0053] Dry chlorinated polyethylene was added to the remaining 5 / 6 volume of the mixed solvent, nitrogen gas was introduced to purge air at a flow rate of 0.6 L / min, the temperature was raised to 130 °C, and the mixture was stirred until the chlorinated polyethylene was completely dissolved. Then the temperature was lowered to 110 °C, the chlorinated polyethylene graft copolymer was added, and the mixture was stirred for 1.5 h at a speed of 500 rpm. Dry polyamide 6 micro powder was added, and the mixture was stirred for another 40 min. Then silica suspension was slowly added, the temperature was raised to 120 °C, the stirring speed was increased to 900 rpm, and the mixture was stirred for 2 h. At the same time, ultrasonic-assisted dispersion was turned on at a power of 300 W, and ultrasonication was performed for 10 min every 30 min. Hexamethylene diisocyanate was added, the stirring speed was reduced to 700 rpm, and the mixture was stirred for 2.5 h to obtain the reaction mixture.
[0054] Step 3: Obtain chlorinated polyethylene resin
[0055] The reaction mixture was cooled to 60°C and slowly poured into acetone while stirring at 1000 rpm. The volume ratio of the reaction mixture to acetone was 1:6. After standing for 40 minutes, the precipitate was collected by filtration, washed four times with acetone, and then vacuum dried at -0.095 MPa and 80°C for 12 hours to obtain chlorinated polyethylene resin.
[0056] Example 3: A method for preparing high-strength chlorinated polyethylene resin
[0057] A method for preparing a high-strength chlorinated polyethylene resin, comprising the following raw materials by weight: 65 parts chlorinated polyethylene, 8 parts chlorinated polyethylene graft copolymer, 4 parts polyamide 6 micro powder, 8 parts modified nano silica, 75 parts mixed solvent, and 1 part hexamethylene diisocyanate, all of which are parts by weight.
[0058] The chlorine content of the chlorinated polyethylene is 30%-35% (by mass).
[0059] The modified nano-silica is nano-silica with a silane coupling agent surface modified, and the silane coupling agent selected is KH560.
[0060] The mixed solvent is obtained by mixing toluene and dioxane, with a mass ratio of toluene to dioxane of 85:15.
[0061] The particle size of the polyamide 6 micro powder is 1-10 μm.
[0062] A method for preparing high-strength chlorinated polyethylene resin, comprising the following steps:
[0063] Step 1: Preparation of chlorinated polyethylene graft copolymer
[0064] Chlorinated polyethylene was added to anhydrous toluene at a mass ratio of 1:16. Nitrogen gas was introduced at a flow rate of 50 mL / min for 15 min, followed by stirring at 300 rpm. The temperature was raised to 90 °C and maintained for 1 h. Allyl glycidyl ether was added at a mass ratio of 3:2 to chlorinated polyethylene. An initiator was added at a concentration of 2% of the mass of chlorinated polyethylene. The mixture was stirred for 20 min at 300 rpm. The temperature was then raised to 130 °C, and the stirring speed was increased to 400 rpm. The mixture was refluxed under nitrogen protection for 4 h to obtain a reaction solution. The temperature was slowly lowered to 70 °C, and the reaction solution was slowly poured into anhydrous ethanol at a volume ratio of 1:6. The mixture was allowed to stand for 40 min, and the precipitate was collected by filtration. The precipitate was washed four times with anhydrous ethanol and then vacuum dried at -0.095 MPa and 80 °C for 8 h to obtain the chlorinated polyethylene graft copolymer.
[0065] The chlorinated polyethylene has a chlorine content of 30%-35% (by mass); the initiator is dicumyl peroxide.
[0066] Step 2: Solution mixing and dispersion and cross-linking reaction
[0067] Modified nano-silica was added to 1 / 6 volume of the mixed solvent, stirred for 40 min at 800 rpm, and then sonicated for 1.5 h at 400 W to form a silica suspension.
[0068] Dry chlorinated polyethylene was added to the remaining 5 / 6 volume of the mixed solvent, nitrogen gas was introduced to purge air at a flow rate of 0.6 L / min, the temperature was raised to 130 °C, and the mixture was stirred until the chlorinated polyethylene was completely dissolved. Then the temperature was lowered to 110 °C, the chlorinated polyethylene graft copolymer was added, and the mixture was stirred for 1.5 h at a speed of 500 rpm. Dry polyamide 6 micro powder was added, and the mixture was stirred for another 40 min. Then silica suspension was slowly added, the temperature was raised to 120 °C, the stirring speed was increased to 800 rpm, and the mixture was stirred for 2 h. At the same time, ultrasonic-assisted dispersion was turned on at a power of 300 W, and ultrasonication was performed for 10 min every 30 min. Hexamethylene diisocyanate was added, the stirring speed was reduced to 600 rpm, and the mixture was stirred for 2.5 h to obtain the reaction mixture.
[0069] Step 3: Obtain chlorinated polyethylene resin
[0070] The reaction mixture was cooled to 60°C and slowly poured into acetone while stirring at 1100 rpm. The volume ratio of the reaction mixture to acetone was 1:8. After standing for 30 minutes, the precipitate was collected by filtration, washed four times with acetone, and then vacuum dried at -0.095 MPa and 80°C for 10 hours to obtain chlorinated polyethylene resin.
[0071] Comparative Example 1
[0072] A method for preparing high-strength chlorinated polyethylene resin, comprising the following raw materials by weight: 70 parts chlorinated polyethylene, 5 parts polyamide 6 micro powder, 9 parts modified nano silica, 70 parts mixed solvent, and 1 part hexamethylene diisocyanate.
[0073] The chlorine content of the chlorinated polyethylene is 30%-35% (by mass).
[0074] The modified nano-silica is nano-silica with a silane coupling agent surface modified, and the silane coupling agent selected is KH560.
[0075] The mixed solvent is obtained by mixing toluene and dioxane, with a mass ratio of toluene to dioxane of 83:18.
[0076] The particle size of the polyamide 6 micro powder is 1-10 μm.
[0077] A method for preparing chlorinated polyethylene resin, comprising the following steps:
[0078] Step 1: Solution mixing and dispersion and cross-linking reaction
[0079] Modified nano-silica was added to 1 / 6 volume of the mixed solvent, stirred for 40 min at 900 rpm, and then sonicated for 1.5 h at 400 W to form a silica suspension.
[0080] Dry chlorinated polyethylene was added to the remaining 5 / 6 volume of the mixed solvent, nitrogen gas was introduced to purge air at a flow rate of 0.6 L / min, the temperature was raised to 130°C, and the mixture was stirred until the chlorinated polyethylene was completely dissolved. Then the temperature was lowered to 110°C, dry polyamide 6 micro powder was added, and the mixture was stirred at 500 rpm for 40 min. Then silica suspension was slowly added, the temperature was raised to 120°C, the stirring speed was increased to 900 rpm, and the mixture was stirred for 2 h. At the same time, ultrasonic-assisted dispersion was turned on at a power of 300 W, and ultrasonication was performed for 10 min every 30 min. Hexamethylene diisocyanate was added, the stirring speed was reduced to 700 rpm, and the mixture was stirred for 2.5 h to obtain the reaction mixture.
[0081] Step 2: Obtaining chlorinated polyethylene resin
[0082] This step is the same as the "Preparation of chlorinated polyethylene resin" step in Example 2.
[0083] Comparative Example 2
[0084] A method for preparing high-strength chlorinated polyethylene resin, comprising the following raw materials by weight: 60 parts chlorinated polyethylene, 10 parts chlorinated polyethylene graft copolymer, 5 parts polyamide 6 micro powder, 9 parts modified nano silica, and 70 parts mixed solvent.
[0085] The chlorine content of the chlorinated polyethylene is 30%-35% (by mass).
[0086] The modified nano-silica is nano-silica with a silane coupling agent surface modified, and the silane coupling agent selected is KH560.
[0087] The mixed solvent is obtained by mixing toluene and dioxane, with a mass ratio of toluene to dioxane of 83:18.
[0088] The particle size of the polyamide 6 micro powder is 1-10 μm.
[0089] A method for preparing chlorinated polyethylene resin, comprising the following steps:
[0090] Step 1: Preparation of chlorinated polyethylene graft copolymer
[0091] This step is the same as the "Preparation of Chlorinated Polyethylene Graft Copolymer" step in Example 2.
[0092] Step 2: Solution mixing and dispersion and cross-linking reaction
[0093] Modified nano-silica was added to 1 / 6 volume of the mixed solvent, stirred for 40 min at 900 rpm, and then sonicated for 1.5 h at 400 W to form a silica suspension.
[0094] Dry chlorinated polyethylene was added to the remaining 5 / 6 volume of the mixed solvent, nitrogen gas was introduced to purge air at a flow rate of 0.6 L / min, the temperature was raised to 130 °C, and the mixture was stirred until the chlorinated polyethylene was completely dissolved. Then the temperature was lowered to 110 °C, the chlorinated polyethylene graft copolymer was added, and the mixture was stirred for 1.5 h at a speed of 500 rpm. Dry polyamide 6 micro powder was added, and the mixture was stirred for another 40 min. Then silica suspension was slowly added, the temperature was raised to 120 °C, the stirring speed was increased to 900 rpm, and the mixture was stirred for 2 h. At the same time, ultrasonic-assisted dispersion was turned on at a power of 300 W, and ultrasonication was performed for 10 min every 30 min to obtain the reaction mixture.
[0095] Step 3: Obtain chlorinated polyethylene resin
[0096] This step is the same as the "Preparation of chlorinated polyethylene resin" step in Example 2.
[0097] Example 4 Performance Testing
[0098] (a) The chlorinated polyethylene resins obtained in Examples 1-3 and Comparative Examples 1-2 were subjected to notched impact strength tests at 23°C according to the test methods specified in GB / T 1043.1-2008; and tensile strength and elongation at break were tested according to the test methods specified in GB / T 1040-2018. The specific test results are shown in Table 1.
[0099] Table 1
[0100]
[0101] As shown in Table 1, the notched impact strength of the chlorinated polyethylene resins prepared in Examples 1-3 at 23°C is 26.8-31.2 KJ / m. 2 The tensile strength reached 37.2-39.1 MPa and the elongation at break was 676-713%, which proves that the chlorinated polyethylene resin prepared by this invention has excellent mechanical properties and achieves a synergistic improvement in high strength and high toughness.
[0102] (II) The corrosion resistance of the chlorinated polyethylene resins prepared in Examples 1-3 and Comparative Examples 1-2 was tested. The chlorinated polyethylene resins were immersed in toluene and a 5% NaCl solution, respectively, for 48 hours at a temperature of 25°C. After immersion, they were dried, and the mass growth rate was calculated. The specific test results are shown in Table 2.
[0103] Table 2
[0104]
[0105] As shown in Table 2, the chlorinated polyethylene resins prepared in Examples 1-3 exhibited a mass increase of 1.25-1.79% after immersion in toluene for 48 hours, and a mass increase of 0.27-0.38% after immersion in 5% NaCl solution for 48 hours. This demonstrates that the chlorinated polyethylene resin prepared in this invention possesses excellent corrosion resistance.
[0106] Obviously, there are many other possible implementation methods under the concept of this invention. It should be stated here that any changes made under the inventive concept of this invention will fall within the protection scope of this invention.
Claims
1. A process for the preparation of a high-strength chlorinated polyethylene resin, characterized by: The raw material weight parts of the chlorinated polyethylene resin are: chlorinated polyethylene 50-65 parts, chlorinated polyethylene graft copolymer 8-13 parts, polyamide 6 micro powder 4-5 parts, modified nano silicon dioxide 8-10 parts, mixed solvent 65-75 parts, hexamethylene diisocyanate 0.8-1 part; The modified nano silicon dioxide is silane coupling agent surface modified nano silicon dioxide, and the silane coupling agent is selected from KH560. The mixed solvent is obtained by mixing toluene and dioxane, and the mass ratio of toluene to dioxane is (80-85):(15-20). The preparation method comprises the steps of preparing a chlorinated polyethylene graft copolymer, solution mixing and dispersion and crosslinking reaction, and preparing a chlorinated polyethylene resin. The chlorinated polyethylene graft copolymer is prepared by adding chlorinated polyethylene into anhydrous toluene, passing nitrogen for 10-15 min, starting stirring, heating to 80-90 DEG C, and keeping the temperature for 1-2 h; then adding allyl glycidyl ether and an initiator, and stirring for 10-20 min; then heating to 110-130 DEG C, and increasing the stirring speed to 400-500 rpm, and refluxing for 4-6 h under nitrogen protection to obtain a reaction solution; slowly cooling to 60-70 DEG C, slowly pouring the reaction solution into anhydrous ethanol, standing for 30-40 min, filtering and collecting the precipitate, and then washing and drying to obtain the chlorinated polyethylene graft copolymer. The solution mixing and dispersion and crosslinking reaction are performed by dissolving chlorinated polyethylene, cooling to 100-110 DEG C, adding the chlorinated polyethylene graft copolymer, stirring for 1-1.5 h, adding dry polyamide 6 micro powder, and continuing to stir for 30-40 min; then slowly adding a silicon dioxide suspension, heating to 110-120 DEG C, increasing the stirring speed to 800-900 rpm, stirring for 1.5-2 h, and simultaneously starting ultrasonic auxiliary dispersion; then adding hexamethylene diisocyanate, reducing the speed to 600-700 rpm, and stirring for 2-2.5 h to obtain a reaction mixture. The chlorinated polyethylene resin is prepared by cooling the reaction mixture to 50-60 DEG C, slowly pouring it into acetone while stirring, standing for 30-40 min, filtering and collecting the precipitate, washing it with acetone for 3-4 times, and then vacuum drying to obtain the chlorinated polyethylene resin.
2. The process for preparing a high-strength chlorinated polyethylene resin according to claim 1, characterized by: The mass ratio of chlorinated polyethylene to anhydrous toluene is 1:(14-16).
3. The process for preparing a high strength chlorinated polyethylene resin according to claim 1, characterized by: The mass ratio of allyl glycidyl ether to chlorinated polyethylene is (1-3):
2.
4. The process for preparing a high strength chlorinated polyethylene resin according to claim 1, characterized by: The initiator is dicumyl peroxide, and the amount of the initiator is 1-2% of the mass of chlorinated polyethylene.
5. The process for preparing a high strength chlorinated polyethylene resin according to claim 1, characterized by: The volume ratio of the reaction solution to anhydrous ethanol is 1:(5-6).
6. The process for preparing a high strength chlorinated polyethylene resin according to claim 1, characterized by: The volume ratio of the reaction mixture to acetone is 1:(5-8).
Citation Information
Patent Citations
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