CN111978562A - Method for emulsifying isoprene rubber glue solution - Google Patents
Method for emulsifying isoprene rubber glue solution Download PDFInfo
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- CN111978562A CN111978562A CN202010934825.6A CN202010934825A CN111978562A CN 111978562 A CN111978562 A CN 111978562A CN 202010934825 A CN202010934825 A CN 202010934825A CN 111978562 A CN111978562 A CN 111978562A
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- isoprene rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
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- Chemical Kinetics & Catalysis (AREA)
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- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
The invention belongs to the technical field of rubber preparation, and particularly relates to a method for emulsifying isoprene rubber glue solution. The pH value of a system is controlled to be 10-11 by using a potassium bicarbonate-potassium carbonate buffer solution, and tripotassium citrate obtained by reacting citric acid with potassium carbonate or potassium bicarbonate is skillfully used as a viscosity reducer for emulsifying isoprene rubber glue solution, so that the viscosity of the isoprene rubber glue solution is reduced, the average particle size of latex after desolventizing and concentrating is smaller, and the stability of the latex is improved. The emulsified latex is subjected to solvent removal and concentration, the viscosity is between 400-450 mPa.s, the particle size is between 350-400nm, the solid content is between 60-65%, and the mechanical stability is between 1500-1550 s. The latex product prepared from the latex is suitable for the field of medical products with high safety performance such as medical gloves and the like.
Description
Technical Field
The invention belongs to the technical field of rubber preparation, and particularly relates to a method for emulsifying isoprene rubber glue solution.
Background
The emulsification process is the most critical step for producing the isoprene latex, and is that the rubber solution of the isoprene rubber, deionized water and an emulsifier are sheared and emulsified together at low speed and high speed by an emulsification pump. And the emulsified material enters the next procedure to remove the solvent.
The viscosity of the isoprene rubber glue solution is high, so that the viscosity needs to be reduced during emulsification. Therefore, the composition of the emulsifier, the emulsification process and other factors are the key to the emulsification of the isoprene rubber glue solution. The granularity of the concentrated glue solution after desolventizing is also a main factor of the stability of the latex, and the quality of the prepared latex product is directly influenced.
Chinese patent CN102936346 discloses a method for directly preparing polyisoprene latex by using polyisoprene glue solution, which is characterized in that the method comprises the following four steps: the method comprises the steps of preparation of polyisoprene glue solution, emulsification of polyisoprene glue solution, solvent removal of polyisoprene latex and concentration of polyisoprene latex, and can accurately design polyisoprene glue solution with different molecular weights and narrow distribution through active anion solution polymerization. The method for preparing the polyisoprene latex disclosed by the invention is simple in process flow, and the prepared latex has excellent comprehensive performance, is pure, does not contain human allergic substances, and is applied to the fields of medicines, lives and the like with higher requirements on the safety and comprehensive performance of latex products. The emulsification method of the polyisoprene glue solution comprises the following steps: the emulsifier is composed of a main emulsifier, a co-emulsifier and a stabilizer, wherein the main emulsifier is generally selected from one or a mixture of several of anionic emulsifier and cationic emulsifier; the auxiliary emulsifier is generally selected from one or a mixture of several nonionic emulsifiers; the stabilizer is selected from one or more of sodium polyacrylate and potassium polyacrylate, and the average particle diameter of the latex is 430nm-550 nm.
At present, the method for emulsifying the isoprene rubber glue solution with low viscosity and small average particle size of the emulsified latex is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a method for emulsifying isoprene rubber glue solution, which reduces the viscosity of the isoprene rubber glue solution, reduces the average particle size of latex after desolventizing and concentrating and increases the stability of the latex.
The method for emulsifying the isoprene rubber glue solution comprises the following steps of:
(1) mixing the isoprene rubber glue solution, a main emulsifier and an auxiliary emulsifier, adding a potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, then adding water, and then adding citric acid; reacting citric acid with potassium carbonate or potassium bicarbonate to obtain tripotassium citrate as a viscosity reducer for emulsifying isoprene rubber glue solution;
(2) emulsifying the emulsion primarily and then emulsifying again;
(3) and settling to obtain the emulsified isoprene rubber latex.
The main emulsifier is a compound of sodium dodecyl benzene sulfonate and disproportionated potassium rosinate soap, and the mass ratio of the sodium dodecyl benzene sulfonate to the disproportionated potassium rosinate soap is 1: 1-2; the main emulsifier accounts for 1-2% of the mass percent of the isoprene rubber glue solution.
The auxiliary emulsifier is fatty alcohol-polyoxyethylene ether; the dosage of the auxiliary emulsifier is 5-10% of the mass percent of the main emulsifier. The coemulsifier is preferably from the peregal series, such as peregal O-20.
In the emulsifying system, the mass ratio of the oil phase to the water phase is 1: 1-1.5.
The dosage of the citric acid is 0.01-0.05% of the mass of the isoprene rubber glue solution.
The primary emulsification temperature and the secondary emulsification temperature are both 5-20 ℃.
The rotation speed of the preliminary emulsification is 1400-1500 rpm; the emulsifying time is 2-5 min.
The re-emulsification rotating speed is 2800 and 3000 rpm; the emulsifying time is 5-8 min.
The latex of the emulsified isoprene rubber is detected after solvent removal and concentration, the average particle diameter of the latex is 350-400nm, and the mechanical stability is between 1500-1550 s. The solvent can be removed by distillation under normal pressure or reduced pressure, and the concentration can be performed by centrifugation.
The mass fraction of the isoprene rubber glue solution is 10-15%.
In the isoprene rubber glue solution, the number average molecular weight of isoprene rubber is 30-50 ten thousand.
The invention has the following beneficial effects:
according to the invention, the pH value of the system is controlled to be 10-11 by using the potassium bicarbonate-potassium carbonate buffer solution, and the tripotassium citrate obtained by reacting citric acid with potassium carbonate or potassium bicarbonate is skillfully used as a viscosity reducer for emulsifying isoprene rubber glue solution, so that the viscosity of the isoprene rubber glue solution is reduced, the average particle size of latex after desolventization and concentration is smaller, and the stability of the latex is increased.
In the invention, citric acid is added, the citric acid reacts with potassium carbonate or potassium bicarbonate to obtain tripotassium citrate which is used as a viscosity reducer for emulsifying the isoprene rubber glue solution, the citric acid reacts with the potassium carbonate or potassium bicarbonate to generate carbon dioxide, the generated carbon dioxide is gas, and the carbon dioxide is discharged from the inside of the glue solution during emulsification, so that the gap in the glue solution is increased, and the viscosity of the isoprene rubber glue solution is reduced. Meanwhile, the tripotassium citrate has 3 carbonyl groups and 1 hydroxyl group, contains a plurality of oxygen and can form hydrogen bonds with latex, so that the aggregation among the latex is reduced, the latex particle dispersing effect is achieved, meanwhile, the negative charges on the surfaces of the latex particles are increased, and the tripotassium citrate has hydroxyl groups and good hydrophilicity, so that the stability of the emulsion is improved.
The emulsified latex is subjected to solvent removal and concentration, the viscosity is between 400-450 mPa.s, the particle size is between 350-400nm, the solid content is between 60-65%, and the mechanical stability is between 1500-1550 s. The latex product prepared from the latex is suitable for the field of medical products with high safety performance such as medical gloves and the like.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The number average molecular weight of the isoprene rubber in the isoprene rubber glue solution is 30-50 ten thousand, and the mass fraction of the isoprene rubber glue solution is 15%.
Adding 1000g of isoprene rubber glue solution, 7g of sodium dodecyl benzene sulfonate and 13g of disproportionated potassium rosinate soap into a reaction kettle, adding O-202 g of peregal, adding potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, adding deionized water according to the mass ratio of an oil phase to a water phase of 1:1.2, and then adding 0.1g of citric acid; performing preliminary emulsification by using a low-speed emulsification pump at the rotation speed of 1400rpm for 2min at the emulsification temperature of 10 ℃; after the emulsion is preliminarily emulsified, a high-speed emulsification pump is used for carrying out re-emulsification; the rotating speed is 2800rpm, the re-emulsification time is 5min, and the emulsification temperature is 10 ℃; the mixture was allowed to settle for 1 hour to obtain an emulsified latex of isoprene rubber.
Example 2
The isoprene rubber cement solution of example 1 was used, and the mass fraction of the isoprene rubber cement solution was 10%.
Adding 1000g of isoprene rubber glue solution, 10g of sodium dodecyl benzene sulfonate and 10g of disproportionated potassium rosinate soap into a reaction kettle, adding O-201 g of peregal, adding potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, adding deionized water according to the mass ratio of an oil phase to a water phase of 1:1.3, and then adding 0.4g of citric acid; performing preliminary emulsification by using a low-speed emulsification pump at the rotation speed of 1450rpm for 5min at the emulsification temperature of 5 ℃; after the emulsion is preliminarily emulsified, a high-speed emulsification pump is used for carrying out re-emulsification; the rotating speed is 3000rpm, the re-emulsification time is 7min, and the emulsification temperature is 5 ℃; the mixture was allowed to settle for 1 hour to obtain an emulsified latex of isoprene rubber.
Example 3
The isoprene rubber cement solution of example 1 was used, and the mass fraction of the isoprene rubber cement solution was 12%.
Adding 1000g of isoprene rubber glue solution, 5g of sodium dodecyl benzene sulfonate and 5g of disproportionated potassium rosinate soap, peregal O-200.75 g into a reaction kettle, adding potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, adding deionized water according to the mass ratio of an oil phase to a water phase of 1:1, and then adding 0.5g of citric acid; carrying out preliminary emulsification by using a low-speed emulsification pump, wherein the rotating speed is 1500rpm, the preliminary emulsification time is 2min, and the emulsification temperature is 15 ℃; after the emulsion is preliminarily emulsified, a high-speed emulsification pump is used for carrying out re-emulsification; the rotation speed is 2900rpm, the re-emulsification time is 5min, and the emulsification temperature is 15 ℃; the mixture was allowed to settle for 1 hour to obtain an emulsified latex of isoprene rubber.
Example 4
The isoprene rubber cement of example 1 was used, and the mass fraction of the isoprene rubber cement was 13%.
Adding 1000g of isoprene rubber glue solution, 4g of sodium dodecyl benzene sulfonate and 6g of disproportionated potassium rosinate soap into a reaction kettle, adding O-200.8 g of peregal, adding potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, adding deionized water according to the mass ratio of an oil phase to a water phase of 1:1.2, and then adding 0.3g of citric acid; performing preliminary emulsification by using a low-speed emulsification pump at the rotation speed of 1450rpm for 3min at the emulsification temperature of 20 ℃; after the emulsion is preliminarily emulsified, a high-speed emulsification pump is used for carrying out re-emulsification; the rotating speed is 3000rpm, the re-emulsification time is 6min, and the emulsification temperature is 20 ℃; the mixture was allowed to settle for 1 hour to obtain an emulsified latex of isoprene rubber.
Example 5
The isoprene rubber cement of example 1 was used, and the mass fraction of the isoprene rubber cement was 15%.
Adding 1000g of isoprene rubber glue solution, 7g of sodium dodecyl benzene sulfonate and 8g of disproportionated potassium rosinate soap, peregal O-201.5 g, adding potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, adding deionized water according to the mass ratio of an oil phase to a water phase of 1:1.5, and then adding 0.2g of citric acid into a reaction kettle; carrying out preliminary emulsification by using a low-speed emulsification pump, wherein the rotating speed is 1500rpm, the preliminary emulsification time is 2min, and the emulsification temperature is 15 ℃; after the emulsion is preliminarily emulsified, a high-speed emulsification pump is used for carrying out re-emulsification; the rotating speed is 3000rpm, the re-emulsification time is 8min, and the emulsification temperature is 15 ℃; the mixture was allowed to settle for 1 hour to obtain an emulsified latex of isoprene rubber.
Comparative example 1
The procedure was the same as in example 1 except that citric acid was not added.
Comparative example 2
The procedure was the same as in example 2 except that citric acid was not added.
Comparative example 3
The procedure was as in example 3 except that citric acid was not added.
Comparative example 4
The procedure was as in example 4 except that citric acid was not added.
Comparative example 5
The procedure was as in example 5 except that citric acid was not added.
The products obtained in examples 1 to 5 and comparative examples 1 to 5 were subjected to the performance test after the removal of the solvent by atmospheric distillation and centrifugal concentration, which were conventional in the art, and the results are shown in Table 1.
The latex viscosity was measured by a rotational viscometer, and the latex particle diameter was measured by a particle size meter, and a mechanical stability test was conducted. The diameter of a stirring disc adopted in the mechanical stability test is 50mm, and the rotating speed is 3000 r/min.
TABLE 1 Performance data Table
From the above, the emulsified latex of the invention is subjected to solvent removal and concentration, the viscosity is between 400-450 mPa.s, the particle size is between 350-400nm, the solid content is between 60-65%, and the mechanical stability is between 1500-1550 s. Compared with comparative examples 1 to 5, the concentrated latexes of examples 1 to 5 of the invention have a small particle size and greater mechanical stability, up to 1550 s.
Claims (10)
1. A method for emulsifying isoprene rubber glue solution is characterized by comprising the following steps:
(1) mixing the isoprene rubber glue solution, a main emulsifier and an auxiliary emulsifier, adding a potassium bicarbonate-potassium carbonate buffer solution to control the pH value to be 10-11, then adding water, and then adding citric acid; reacting citric acid with potassium carbonate or potassium bicarbonate to obtain tripotassium citrate as a viscosity reducer for emulsifying isoprene rubber glue solution;
(2) emulsifying the emulsion primarily and then emulsifying again;
(3) and settling to obtain the emulsified isoprene rubber latex.
2. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the main emulsifier is a compound of sodium dodecyl benzene sulfonate and disproportionated potassium rosinate soap, and the mass ratio of the sodium dodecyl benzene sulfonate to the disproportionated potassium rosinate soap is 1: 1-2; the main emulsifier accounts for 1-2% of the mass percent of the isoprene rubber glue solution.
3. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the auxiliary emulsifier is fatty alcohol polyoxyethylene ether; the dosage of the auxiliary emulsifier is 5-10% of the mass percent of the main emulsifier.
4. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: in the emulsifying system, the mass ratio of the oil phase to the water phase is 1: 1-1.5.
5. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the consumption of the citric acid is 0.01-0.05% of the mass of the isoprene rubber glue solution.
6. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the primary emulsification temperature and the secondary emulsification temperature are both 5-20 ℃.
7. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the rotation speed of the primary emulsification is 1400-1500 rpm; emulsifying for 2-5 min; the re-emulsification rotating speed is 2800 and 3000 rpm; the emulsifying time is 5-8 min.
8. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the latex of the emulsified isoprene rubber is detected after solvent removal and concentration, the average particle diameter of the latex is 350-400nm, and the mechanical stability is 1500-1550 s.
9. The method for emulsifying isoprene rubber cement solution according to claim 1, characterized in that: the mass fraction of the isoprene rubber glue solution is 10-15%.
10. The method for emulsifying isoprene rubber cement solution according to claim 1 or 9, characterized in that: in the isoprene rubber glue solution, the number average molecular weight of the isoprene rubber is 30-50 ten thousand.
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