CN109265896B - Preparation method of waterproof water-swelling rubber - Google Patents
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Abstract
The invention provides a preparation method of waterproof water-swelling rubber, which comprises the following steps: hydrolyzing an acrylamide potassium hydroxide solution, and adding chitin xanthate, deionized water, a potassium persulfate solution and an N, N' -methylene bisacrylamide solution for heating reaction; adding the mixture into a cyclohexane solution containing alkylphenol polyoxyethylene, and heating for reaction; filtering and drying; processing in a low-temperature plasma processing device to obtain porous water-absorbing microspheres; stirring natural latex, sucrose fatty acid ester, straw cellulose, nano silica sol and sodium bisulfite; adding a sodium acrylate solution, a potassium persulfate solution and an N, N' -methylene bisacrylamide solution for reaction; drying; transferring to an open mill, sequentially adding stearic acid, zinc oxide, an accelerator DM, an anti-aging agent RD, a reinforcing agent, porous water-absorbing microspheres and sulfur after wrapping a roll, and uniformly mixing; and (4) vulcanizing to obtain the catalyst. The waterproof water-absorbing expansion rubber prepared by the method has the advantages of excellent water absorption performance, good reutilization property and good mechanical property.
Description
Technical Field
The invention relates to a preparation method of waterproof water-swelling rubber.
Background
The water-absorbing expansion rubber is a functional polymer material developed in the end of the 70 th 20 th century, has the characteristic that the rubber can expand to several times or even tens of times of the self mass or volume after absorbing water, and can keep the specific elasticity and strength of the rubber and have certain water-retaining capacity. The water-swelling rubber has the dual characteristics of elastic sealing and water proofing and water stopping through water swelling, is good in effect, safe and reliable, convenient to construct and wide in application range, and is more and more appreciated by people and known as a waterproof material with magic power and a super sealing material. In recent years, the introduction of new structures and the preparation of high-performance water-swelling rubber by using biological materials or renewable resources are the main development directions. The invention adopts chitin xanthate and straw cellulose to improve the water absorption performance.
Disclosure of Invention
The technical problem to be solved is as follows: the preparation method of the waterproof water-swelling rubber is provided, and the obtained waterproof water-swelling rubber has the advantages of good water absorption performance, good recycling performance and good mechanical property.
The technical scheme is as follows: a preparation method of waterproof water-swelling rubber comprises the following steps of:
(1) hydrolyzing 25-30 parts of acrylamide by 30-40 parts of potassium hydroxide solution, adding 2-3 parts of chitin xanthate and 30-40 parts of deionized water, and uniformly mixing;
(2) adding 9-13 parts of 10mg/mL potassium persulfate solution and 7.5-10 parts of 2mg/mLN, N' -methylene bisacrylamide solution, introducing nitrogen, stirring uniformly, and slowly heating to 35-45 ℃ for reaction for 1-2 h;
(3) adding into cyclohexane solution containing 3-5 parts of alkylphenol polyoxyethylene, heating to 60-65 deg.C, and reacting for 30-40 min;
(4) filtering, and oven drying at 50-60 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 6-9min under the conditions of power frequency of 6-8kHz, working voltage of 20kV and discharge power of 50-70W to obtain porous water-absorbing microspheres;
(6) placing 15-20 parts of natural latex into a reaction container, adding 2.5-3 parts of 0.1 wt% sucrose fatty acid ester, 1-2 parts of straw cellulose, 1-3 parts of nano silica sol and 0.3-0.5 part of sodium bisulfite, stirring, introducing nitrogen and discharging oxygen for 20-30 min;
(7) dropwise adding 25-30 parts of 2.25mol/L sodium acrylate solution, then adding 9-13 parts of 10mg/mL potassium persulfate solution and 7.5-10 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, and reacting at the temperature of 50-55 ℃;
(8) after the reaction is finished, putting the mixture into an oven, and drying the mixture at the temperature of 70-80 ℃;
(9) transferring to an open mill, sequentially adding 0.5-0.6 part of stearic acid, 0.8-1 part of zinc oxide, 0.4-0.5 part of accelerator DM, 0.8-1 part of antioxidant RD, 3-6 parts of reinforcing agent, 15-20 parts of porous water-absorbing microspheres and 0.4-0.5 part of sulfur after roll wrapping, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 140 ℃ and the temperature of 145 ℃ and under the pressure of 12-17MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
Further, the dry glue content of the natural rubber latex is 60%.
Further, the particle size of the porous water-absorbing microspheres is 200 meshes.
Further, the reinforcing agent is one or more of white carbon black, diatomite, pottery clay or fly ash.
Further, the mass fraction of the potassium hydroxide solution in the step (1) is 5-6%.
Further, in the step (5), the power supply frequency is 7kHz, and the discharge power is 60W.
Has the advantages that:
1. the invention introduces a novel structure of chitin xanthate and straw cellulose, and has important influence on improving the water absorption performance.
2. The straw cellulose has good hydrophilic hygroscopicity, can form a water absorption channel in natural latex, and has great influence on the water absorption balance time of the water-swelling rubber.
3. After the water absorption microspheres are treated by the low-temperature plasma treatment device, dense and uniform small holes are generated, and the water absorption effect is better.
4. The waterproof water-absorbing expansion rubber prepared by the invention has very good water absorption performance, the maximum water absorption rate is up to 2031%, the secondary water absorption ratio is up to 98.6%, and the waterproof water-absorbing expansion rubber has very good reusability, and simultaneously, the waterproof water-absorbing expansion rubber prepared by the invention has very good mechanical properties, the hardness is 52.2-52.5 degrees, the 300% stress at definite elongation is up to 2.37MPa, the tensile strength is up to 10.9MPa, and the elongation at break is up to 678%.
Detailed Description
Example 1
A preparation method of waterproof water-swelling rubber comprises the following steps of:
(1) hydrolyzing 25 parts of acrylamide by 30 parts of potassium hydroxide solution, adding 2 parts of chitin xanthate and 30 parts of deionized water, and uniformly mixing;
(2) adding 9 parts of 10mg/mL potassium persulfate solution and 7.5 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, introducing nitrogen, uniformly stirring, slowly heating to 35 ℃ and reacting for 1 h;
(3) adding the mixture into cyclohexane solution containing 3 parts of alkylphenol polyoxyethylene, heating to 60 ℃, and continuing to react for 30 min;
(4) filtering, and drying at 50 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 6min under the conditions of power frequency of 6kHz, working voltage of 20kV and discharge power of 50W to obtain porous water-absorbing microspheres;
(6) putting 15 parts of natural latex into a reaction container, adding 2.5 parts of 0.1 wt% sucrose fatty acid ester, 1 part of straw cellulose, 1 part of nano silica sol and 0.3 part of sodium bisulfite, stirring, introducing nitrogen and discharging oxygen for 20 min;
(7) dropwise adding 25 parts of 2.25mol/L sodium acrylate solution, then adding 9 parts of 10mg/mL potassium persulfate solution and 7.5 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, and reacting at the temperature of 50 ℃;
(8) after the reaction is finished, putting the mixture into a drying oven, and drying the mixture at the temperature of 70 ℃;
(9) transferring the mixture to an open mill, sequentially adding 0.5 part of stearic acid, 0.8 part of zinc oxide, 0.4 part of accelerator DM, 0.8 part of antioxidant RD, 3 parts of reinforcing agent, 15 parts of porous water-absorbing microspheres and 0.4 part of sulfur after coating rollers, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 140 ℃ and the pressure of 12MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
Example 2
A preparation method of waterproof water-swelling rubber comprises the following steps of:
(1) hydrolyzing 27 parts of acrylamide by 32 parts of potassium hydroxide solution, adding 2.2 parts of chitin xanthate and 33 parts of deionized water, and uniformly mixing;
(2) adding 10 parts of 10mg/mL potassium persulfate solution and 8 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, introducing nitrogen, uniformly stirring, slowly heating to 35 ℃ and reacting for 1.5 h;
(3) adding the mixture into cyclohexane solution containing 3.5 parts of alkylphenol polyoxyethylene, heating to 62 ℃, and continuing to react for 35 min;
(4) filtering, and drying at 55 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 7min under the conditions of power frequency of 7kHz, working voltage of 20kV and discharge power of 55W to obtain porous water-absorbing microspheres;
(6) placing 17 parts of natural latex into a reaction container, adding 2.7 parts of 0.1 wt% sucrose fatty acid ester, 1.3 parts of straw cellulose, 1.5 parts of nano silica sol and 0.4 part of sodium bisulfite, stirring, introducing nitrogen and discharging oxygen for 25 min;
(7) 27 parts of 2.25mol/L sodium acrylate solution is dripped, 10 parts of 10mg/mL potassium persulfate solution and 8 parts of 2mg/mLN, N' -methylene-bisacrylamide solution are added, and reaction is carried out at the temperature of 50 ℃;
(8) after the reaction is finished, putting the mixture into a drying oven, and drying the mixture at the temperature of 75 ℃;
(9) transferring the mixture to an open mill, sequentially adding 0.55 part of stearic acid, 0.85 part of zinc oxide, 0.45 part of accelerator DM, 0.85 part of antioxidant RD, 4 parts of reinforcing agent, 17 parts of porous water-absorbing microspheres and 0.45 part of sulfur after coating rollers, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 140 ℃ and the pressure of 13MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
Example 3
A preparation method of waterproof water-swelling rubber comprises the following steps of:
(1) hydrolyzing 28 parts of acrylamide by 35 parts of potassium hydroxide solution, adding 2.5 parts of chitin xanthate and 35 parts of deionized water, and uniformly mixing;
(2) adding 11 parts of 10mg/mL potassium persulfate solution and 9 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, introducing nitrogen, uniformly stirring, slowly heating to 40 ℃ and reacting for 1.5 h;
(3) adding the mixture into cyclohexane solution containing 3-5 parts of alkylphenol polyoxyethylene, heating to 63 ℃, and continuing to react for 35 min;
(4) filtering, and drying at 55 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 8min under the conditions of power frequency of 7kHz, working voltage of 20kV and discharge power of 60W to obtain porous water-absorbing microspheres;
(6) putting 18 parts of natural latex into a reaction container, adding 2.8 parts of 0.1 wt% sucrose fatty acid ester, 1.5 parts of straw cellulose, 2 parts of nano silica sol and 0.4 part of sodium bisulfite, stirring, introducing nitrogen and discharging oxygen for 25 min;
(7) 28 parts of 2.25mol/L sodium acrylate solution is dripped, 11 parts of 10mg/mL potassium persulfate solution and 9 parts of 2mg/mLN, N' -methylene bisacrylamide solution are added, and the reaction is carried out at the temperature of 53 ℃;
(8) after the reaction is finished, putting the mixture into a drying oven, and drying the mixture at the temperature of 75 ℃;
(9) transferring to an open mill, sequentially adding 0.55 part of stearic acid, 0.9 part of zinc oxide, 0.45 part of accelerator DM, 0.9 part of antioxidant RD, 4.5 parts of reinforcing agent, 18 parts of porous water-absorbing microspheres and 0.45 part of sulfur after wrapping rollers, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 145 ℃ and the pressure of 14MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
Example 4
A preparation method of waterproof water-swelling rubber comprises the following steps of:
(1) hydrolyzing 28 parts of acrylamide by using 38 parts of potassium hydroxide solution, adding 2.5 parts of chitin xanthate and 35 parts of deionized water, and uniformly mixing;
(2) adding 12 parts of 10mg/mL potassium persulfate solution and 9 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, introducing nitrogen, uniformly stirring, slowly heating to 40 ℃ and reacting for 1.5 h;
(3) adding the mixture into a cyclohexane solution containing 4.5 parts of alkylphenol polyoxyethylene, heating to 64 ℃, and continuing to react for 35 min;
(4) filtering, and drying at 55 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 8min under the conditions of power frequency of 7kHz, working voltage of 20kV and discharge power of 65W to obtain porous water-absorbing microspheres;
(6) placing 19 parts of natural latex into a reaction container, adding 2.8 parts of 0.1 wt% sucrose fatty acid ester, 1.8 parts of straw cellulose, 2.5 parts of nano silica sol and 0.45 part of sodium bisulfite, stirring, introducing nitrogen and discharging oxygen for 25 min;
(7) 29 parts of 2.25mol/L sodium acrylate solution is dripped, and then 12 parts of 10mg/mL potassium persulfate solution and 9 parts of 2mg/mLN, N' -methylene bisacrylamide solution are added for reaction at the temperature of 55 ℃;
(8) after the reaction is finished, putting the mixture into a drying oven, and drying the mixture at the temperature of 75 ℃;
(9) transferring the mixture to an open mill, sequentially adding 0.55 part of stearic acid, 0.9 part of zinc oxide, 0.45 part of accelerator DM, 0.9 part of antioxidant RD, 5 parts of reinforcing agent, 19 parts of porous water-absorbing microspheres and 0.45 part of sulfur after coating rollers, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 145 ℃ and under the pressure of 16MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
Example 5
A preparation method of waterproof water-swelling rubber comprises the following steps of:
(1) hydrolyzing 30 parts of acrylamide with 40 parts of potassium hydroxide solution, adding 3 parts of chitin xanthate and 40 parts of deionized water, and uniformly mixing;
(2) adding 13 parts of 10mg/mL potassium persulfate solution and 10 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, introducing nitrogen, uniformly stirring, and slowly heating to 45 ℃ for reaction for 2 hours;
(3) adding the mixture into a cyclohexane solution containing 5 parts of alkylphenol polyoxyethylene, heating to 65 ℃, and continuing to react for 40 min;
(4) filtering, and drying at 60 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 9min under the conditions of power frequency of 8kHz, working voltage of 20kV and discharge power of 70W to obtain porous water-absorbing microspheres;
(6) placing 20 parts of natural latex into a reaction container, adding 3 parts of 0.1 wt% sucrose fatty acid ester, 2 parts of straw cellulose, 3 parts of nano silica sol and 0.5 part of sodium bisulfite, stirring, introducing nitrogen and discharging oxygen for 30 min;
(7) dropwise adding 30 parts of 2.25mol/L sodium acrylate solution, then adding 13 parts of 10mg/mL potassium persulfate solution and 10 parts of 2mg/mLN, N' -methylene-bisacrylamide solution, and reacting at the temperature of 55 ℃;
(8) after the reaction is finished, putting the mixture into an oven, and drying the mixture at the temperature of 80 ℃;
(9) transferring the mixture to an open mill, and sequentially adding 0.6 part of stearic acid, 1 part of zinc oxide, 0.5 part of accelerator DM, 1 part of antioxidant RD, 6 parts of reinforcing agent, 20 parts of porous water-absorbing microspheres and 0.5 part of sulfur after roll wrapping, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 145 ℃ and the pressure of 17MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
Measurement of Water absorption: a standard sample of 20 mm. times.20 mm. times.2 mm in mass was weighed, immersed in distilled water, and weighed after water absorption balance, and the water absorption rate was calculated according to the following formula.
Water absorption ratio (mass after water absorption-mass before water absorption)/mass before water absorption
And (3) measuring the secondary water absorption ratio: weighing the rubber of the invention which is saturated with water, drying in a forced air drying oven at 70 ℃ until the water is completely lost, and performing the water absorption test again, wherein the percentage of the 2 nd saturated water absorption mass to the 1 st saturated water absorption mass is the secondary water absorption ratio of the water-swelling rubber.
All physical performance indexes are tested according to corresponding national standards, the stress at definite elongation, the tensile strength and the elongation at break are tested by adopting an I-type sample, the tensile rate is 500mm/min, and the tearing strength is tested by adopting a right-angle sample.
TABLE 1 Water absorption Properties of waterproof Water-swellable rubber
| Product name | Maximum Water absorption (%) | Water absorption balance time (h) | Second Water absorption ratio (%) |
| Example 1 | 2023 | 12 | 98.5 |
| Example 2 | 2027 | 12 | 98.6 |
| Example 3 | 2031 | 12 | 98.6 |
| Example 4 | 2029 | 12 | 98.5 |
| Example 5 | 2026 | 12 | 98.5 |
All physical performance indexes are tested according to corresponding national standards, the stress at definite elongation, the tensile strength and the elongation at break are tested by adopting an I-type sample, the tensile rate is 500mm/min, and the tearing strength is tested by adopting a right-angle sample.
TABLE 2 physical property indexes of the waterproof water-swelling rubber
The waterproof water-absorbing expansion rubber prepared by the invention has very good water absorption performance, the maximum water absorption rate is up to 2031%, the secondary water absorption ratio is up to 98.6%, and the waterproof water-absorbing expansion rubber has very good reusability, and simultaneously, the waterproof water-absorbing expansion rubber prepared by the invention has very good mechanical properties, the hardness is 52.2-52.5 degrees, the 300% stress at definite elongation is up to 2.37MPa, the tensile strength is up to 10.9MPa, and the elongation at break is up to 678%.
Claims (6)
1. A preparation method of waterproof water-swelling rubber is characterized by comprising the following steps: the components by weight portion comprise the following steps:
(1) hydrolyzing acrylamide with potassium hydroxide solution, adding chitin xanthate and deionized water, and mixing well;
(2) adding a potassium persulfate solution and an N, N' -methylene bisacrylamide solution, introducing nitrogen, uniformly stirring, and slowly heating to 35-45 ℃ for reaction for 1-2 hours;
(3) adding the mixture into cyclohexane solution containing alkylphenol polyoxyethylene, heating to 60-65 ℃, and continuing to react for 30-40 min;
(4) filtering, and oven drying at 50-60 deg.C;
(5) uniformly spreading on an earth electrode in a low-temperature plasma treatment device, and treating for 6-9min under the conditions of power frequency of 6-8kHz, working voltage of 20kV and discharge power of 50-70W to obtain porous water-absorbing microspheres;
(6) placing natural latex in a reaction container, adding sucrose fatty acid ester, straw cellulose, nano silica sol and sodium bisulfite, stirring, introducing nitrogen and removing oxygen for 20-30 min;
(7) dropwise adding a sodium acrylate solution, then adding a potassium persulfate solution and an N, N' -methylene bisacrylamide solution, and reacting at the temperature of 50-55 ℃;
(8) after the reaction is finished, putting the mixture into an oven, and drying the mixture at the temperature of 70-80 ℃;
(9) transferring the mixture to an open mill, sequentially adding stearic acid, zinc oxide, an accelerator DM, an anti-aging agent RD, a reinforcing agent, porous water-absorbing microspheres and sulfur after wrapping a roll, and uniformly mixing;
(10) and vulcanizing the mixed rubber material on a flat vulcanizing machine at the temperature of 140 ℃ and the temperature of 145 ℃ and under the pressure of 12-17MPa for 10min to obtain the waterproof water-absorbing expansion rubber.
2. The method for preparing a waterproof water-swelling rubber according to claim 1, wherein the method comprises the following steps: the dry rubber content of the natural rubber latex is 60%.
3. The method for preparing a waterproof water-swelling rubber according to claim 1, wherein the method comprises the following steps: the particle size of the porous water-absorbing microspheres is 200 meshes.
4. The method for preparing a waterproof water-swelling rubber according to claim 1, wherein the method comprises the following steps: the reinforcing agent is one or more of white carbon black, diatomite, argil or fly ash.
5. The method for preparing a waterproof water-swelling rubber according to claim 1, wherein the method comprises the following steps: the mass fraction of the potassium hydroxide solution in the step (1) is 5-6%.
6. The method for preparing a waterproof water-swelling rubber according to claim 1, wherein the method comprises the following steps: in the step (5), the power supply frequency is 7kHz, and the discharge power is 60W.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508756A (en) * | 2009-03-12 | 2009-08-19 | 海南大学 | Method of preparing rubber with quick water uptake high-mechanical performance water uptake expansion |
| CN102775555A (en) * | 2012-08-15 | 2012-11-14 | 内蒙古大学 | Method for synthesizing high water absorbent polymer by using potato starch xanthate and acrylamide |
| CN108250344A (en) * | 2017-12-27 | 2018-07-06 | 山东诺尔生物科技有限公司 | A kind of low bulk speed nanoscale water suction microballoon and preparation method thereof |
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2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508756A (en) * | 2009-03-12 | 2009-08-19 | 海南大学 | Method of preparing rubber with quick water uptake high-mechanical performance water uptake expansion |
| CN102775555A (en) * | 2012-08-15 | 2012-11-14 | 内蒙古大学 | Method for synthesizing high water absorbent polymer by using potato starch xanthate and acrylamide |
| CN108250344A (en) * | 2017-12-27 | 2018-07-06 | 山东诺尔生物科技有限公司 | A kind of low bulk speed nanoscale water suction microballoon and preparation method thereof |
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