CN115677914B - Preparation method and application of seed latex for preparing carboxylated nitrile latex - Google Patents
Preparation method and application of seed latex for preparing carboxylated nitrile latex Download PDFInfo
- Publication number
- CN115677914B CN115677914B CN202211410886.8A CN202211410886A CN115677914B CN 115677914 B CN115677914 B CN 115677914B CN 202211410886 A CN202211410886 A CN 202211410886A CN 115677914 B CN115677914 B CN 115677914B
- Authority
- CN
- China
- Prior art keywords
- latex
- carboxylated nitrile
- initiator
- aqueous solution
- reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The application relates to a preparation method and application of seed latex for preparing carboxylated nitrile latex. The method comprises the following steps: s1, heating the temperature in a reactor containing an aqueous solution of an emulsifier in a stirring state, maintaining the temperature at 80-85 ℃, and then adding the aqueous solution of itaconic acid into the reactor to be mixed with the aqueous solution of the emulsifier; s2, mixing styrene with an acrylic ester monomer to obtain a mixed solution 2; s3, adding 10-20wt% of mixed solution 2 and the aqueous solution of the first initiator into a reactor for reaction; and S4, dropwise adding the rest mixed solution 2 and an alkaline aqueous solution containing a second initiator into the reactor, and carrying out reaction after heating to obtain the seed latex. The seed latex prepared by the method is added into the preparation raw material of the carboxylated nitrile latex, so that the prepared carboxylated nitrile latex has narrow particle size distribution and excellent chemical stability and mechanical stability.
Description
Technical Field
The application relates to the technical field of synthesis of carboxylated nitrile latex, in particular to a preparation method and application of seed latex for preparing carboxylated nitrile latex.
Background
Carboxylated nitrile latex is an aqueous dispersion made primarily from emulsion polymerization of acrylonitrile, butadiene, and a carboxylic acid-containing third monomer such as acrylic acid, methacrylic acid, and the like. The modified polyurethane has the characteristics of excellent oil resistance, solvent resistance, heat resistance, chemical corrosion resistance, wear resistance and the like, and is widely applied to the fields of thick, thin, lined, unlined gloves, sealing materials and the like through proper modification.
The current synthesis process of the carboxylated nitrile latex generally comprises continuous polymerization, directly adding required raw materials, such as acrylonitrile, butadiene, methacrylic acid and the like, in the polymerization process, then adding an initiator in a stirring state, heating in a temperature stage, testing the conversion rate in the synthesis process, reaching a preset standard, cooling and stopping polymerization, and further preparing the carboxylated nitrile latex. All the raw materials are added at one time in the process, and in the initial stage of polymerization, namely in the colloidal particle generation period, colloidal particles with different sizes are randomly generated in the form of colloidal particles, so that the whole colloidal particles are widely distributed in the middle and later latex generation period, and the chemical stability and mechanical stability of the latex are reduced. Meanwhile, in the processing process, the deviation among physical property batches of the latex product is large.
The patent CN 113563515A discloses a preparation method of high-performance carboxylated nitrile latex, which adopts an emulsion polymerization process with styrene-butadiene latex as seeds, part of monomers are dripped, butadiene and acrylonitrile are used as main monomers, unsaturated carboxylic acid is adopted, and multiple double bond crosslinking monomers and other functional monomers are used as auxiliary monomers, a composite emulsifying system, namely a reactive emulsifier and a small amount of anionic emulsifier, persulfate as an initiator, alkyl mercaptan as a molecular weight regulator and other auxiliary agents are adopted during polymerization, and the carboxylated nitrile latex is obtained by dispersing by an ultrasonic homogenizer or a high-pressure homogenizer and then dripping the dispersed monomers into a reaction kettle for reaction. The patent has the defects of complex types of monomers and times of adding monomers in the production process, complex technological process operation, difficult control of reaction temperature, long reaction time and the like, and the parameters such as the particle size distribution, the stability and the like of the prepared carboxylated nitrile latex are not researched.
Therefore, it is necessary to provide a preparation method of carboxylated nitrile latex with small particle size distribution and good chemical stability and mechanical stability.
Disclosure of Invention
In order to solve the defects of the prior art, the application provides a preparation method of seed latex for preparing carboxylated nitrile latex, and the seed latex prepared by the method is added into the preparation raw material of carboxylated nitrile latex, so that the prepared carboxylated nitrile latex has narrow particle size distribution and excellent chemical stability and mechanical stability.
To this end, a first aspect of the present application provides a process for preparing a seed latex for preparing a carboxylated nitrile latex, the process comprising the steps of:
s1, heating the temperature in a reactor containing an aqueous solution of an emulsifier under a stirring state, maintaining the temperature at 80-85 ℃, and then adding the aqueous solution of itaconic acid into the reactor to be mixed with the aqueous solution of the emulsifier to obtain a mixed solution 1;
s2, mixing styrene with an acrylic ester monomer to obtain a mixed solution 2;
s3, adding 10-20wt% of the mixed solution 2 and the aqueous solution of the first initiator into a reactor for reaction to obtain a first reaction mixed solution;
and S4, dropwise adding the rest mixed solution 2 and an alkaline aqueous solution containing a second initiator into the reactor, and carrying out reaction after heating to obtain the seed latex for preparing the carboxylated nitrile latex.
In the present application, the mixed solution 2 obtained in step S2 is an oil phase, and by adding a part (10 to 20 wt%) of the mixed solution 2 to the mixed solution 1, an oil-in-water seed core can be formed by the action of the first initiator, and then the synthesis of the oil-in-water seed latex is gradually initiated by slowly adding the remaining mixed solution 2 and an alkaline aqueous solution (aqueous phase) containing the second initiator. The oil-in-water seed latex (with the particle size of about 20 nm) is added into the preparation raw material of the carboxylated nitrile latex, so that the particle size of the colloidal particles at the initial stage of polymerization can be controlled, and the temperature is stably controlled at the later stage, so that the prepared carboxylated nitrile latex has uniform particle size distribution, small particle size distribution (with the particle size distribution of about 130 nm) and narrow particle size distribution.
In the application, the alkaline aqueous solution containing the second initiator is used as active water (commonly called as alkaline potassium persulfate), and the alkaline substance in the solution can weaken the activity of the second initiator in the active water, so that the water-based shell with the reaction activity can be slowly wrapped outside the oil-type seed core, the particle size of the prepared seed latex can be controlled more conveniently, and the particle size of the prepared seed latex can be controlled to be about 20 nm.
In the present application, the reactor is always in a stirred state during the whole reaction, and the stirring speed may be 80-100 rpm.
In some embodiments, the mass ratio of itaconic acid, emulsifier, styrene, acrylate monomer, first initiator and second initiator is (1-1.5): 40-50): 15-20): 30-40): 0.8-1.2: (0.8-1.2.
In some embodiments, the mass ratio of itaconic acid, emulsifier, styrene, acrylate monomer, first initiator, and second initiator is 1.2:42:18.5:37.8:1.1:0.8.
The present application can effectively initiate the synthesis of an oil-in-water seed latex by controlling the mass ratio of itaconic acid, emulsifier, styrene, acrylate monomer, first initiator and second initiator within the above range.
In the present application, the concentration of the emulsifier in the aqueous solution of the emulsifier may be, for example, 5 to 10wt%; the preparation mode of the aqueous solution of the emulsifier can be as follows: mixing the required amount of water (deionized water) with the emulsifier under stirring. The concentration of itaconic acid in the aqueous solution of itaconic acid may be, for example, 0.5 to 1.0wt%; the preparation mode of the aqueous solution of itaconic acid can be as follows: heating the required amount of water (deionized water) to 50-60 ℃, and slowly adding itaconic acid to completely dissolve under the stirring state (50-60 rpm). The concentration of the first initiator in the aqueous solution of the first initiator may be, for example, 25 to 30wt%; the preparation mode of the aqueous solution of the first initiator can be as follows: the required amount of water (deionized water) is stirred and mixed with the first initiator. The concentration of the second initiator in the alkaline aqueous solution containing the second initiator may be, for example, 1 to 2wt%, and the concentration of the alkaline substance contained may be, for example, 0.1 to 0.5wt%; the alkaline aqueous solution containing the second initiator can be prepared by the following steps: and stirring and mixing the required amount of water (deionized water), the second initiator and the alkaline substance solution.
In some embodiments, the emulsifier is selected from at least one of sodium alkyl sulfonate, sodium alkyl benzene sulfonate, and sodium alkyl diphenyl ether disulfonate. In some embodiments, the emulsifier is sodium alkyl benzene sulfonate, specifically sodium dodecyl benzene sulfonate.
In some embodiments, the first initiator and the second initiator are each independently selected from at least one of sodium persulfate, ammonium persulfate, and potassium persulfate.
In this application, the first initiator and the second initiator may be the same or different; preferably, the first initiator and the second initiator are the same and are both sodium persulfate.
In some embodiments, the acrylate monomers include 2-ethylhexyl acrylate, methyl methacrylate, and 2-hydroxyethyl acrylate.
The inventor of the application found through research that when the acrylic ester monomer comprises 2-ethylhexyl acrylate, methyl methacrylate and 2-hydroxyethyl acrylate simultaneously, the particle size distribution of the prepared seed latex and the finally prepared carboxylated nitrile latex can be smaller, and the chemical stability and the mechanical stability of the carboxylated nitrile latex are improved.
In some embodiments, the mass ratio of 2-ethylhexyl acrylate, methyl methacrylate, and 2-hydroxyethyl acrylate is (25-35): 5-10): 1-2.
In some embodiments, the mass ratio of 2-ethylhexyl acrylate, methyl methacrylate, and 2-hydroxyethyl acrylate is 29.8:6.9:1.1.
In the present application, by controlling the mass ratio of 2-ethylhexyl acrylate, methyl methacrylate and 2-hydroxyethyl acrylate within the above range, the particle size distribution of the finally produced carboxylated nitrile latex can be further improved.
In some embodiments, in step S4, the alkaline substance in the alkaline aqueous solution is selected from at least one of sodium hydroxide and potassium hydroxide. For example, the alkaline substance may be potassium hydroxide.
In some embodiments, the mass ratio of the basic substance to the second initiator is 1 (3-5).
The mass ratio of the alkaline substance to the second initiator is controlled within the range, so that the activity of the active water can be effectively inhibited, and the particle size of the prepared seed latex can be controlled more favorably.
In the present application, the remaining mixed solution 2 and the alkaline aqueous solution containing the second initiator are slowly added to the reactor by dropwise addition, and the rate of addition may be, for example, (0.3 to 0.5) kg/min. By slowly dropping, the water-based shell having reactivity can be slowly wrapped on the outer surface of the oil-based seed core, and the oil-in-water seed latex having a narrow particle size distribution can be obtained.
In some embodiments, in step S3, the reaction time is 10 to 20 minutes.
In some embodiments, in step S4, the reaction is carried out for a period of time ranging from 1 to 2 hours, and the temperature of the reaction is from 90 to 95 ℃.
Under the above reaction conditions, an oil-in-water seed latex can be effectively synthesized.
The second aspect of the application provides a carboxylated nitrile latex, which is prepared from the following raw materials in parts by weight:
in the application, the raw material for preparing the carboxylated nitrile latex contains the seed latex prepared by the method in the first aspect, and the seed latex is used as a core to further increase the particle size of the latex, so that the particle size of the prepared latex is kept in a narrow range.
In some embodiments, the seed latex may be, for example, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, or 15 parts by weight; in some preferred embodiments, the seed latex is 8 to 12 parts by weight; in some most preferred embodiments, the seed latex is 10 parts by weight.
The present application can make the particle size distribution of the prepared carboxylated nitrile latex narrower by controlling the weight part of the seed latex within the above range.
In some embodiments of the present application, the preparation raw materials of the carboxylated nitrile latex include the following components in parts by weight:
10 parts of seed latex prepared by the method of the first aspect of the application;
26 parts of acrylonitrile;
66 parts of butadiene;
and 8 parts of a third monomer containing carboxylic acid.
In some embodiments, the carboxylic acid-containing third monomer is selected from at least one of acrylic acid, methacrylic acid, itaconic acid, fumaric acid, and maleic acid. For example, methacrylic acid and the like can be used.
In a third aspect, the present application provides a method for preparing a carboxylated nitrile latex as described in the second aspect of the present application, comprising the steps of: and adding the seed latex, acrylonitrile, butadiene and a third monomer containing carboxylic acid into a polymerization reaction kettle, and reacting under the protection of inert gas to obtain the carboxylated nitrile latex.
In some embodiments, the reaction conditions are: rotational speed: 50-100 rpm, reaction pressure: 0.3-0.5 MPa, reaction temperature: 30-40 ℃, and the reaction time is as follows: and 10-15 hours.
In some embodiments, the reaction conditions are: rotational speed: 70rpm, reaction pressure: 0.4-0.45 MPa, and the reaction temperature is: 37-38 ℃, and the reaction time is as follows: 13-15 hours.
In the present application, the carboxylated nitrile latex can be synthesized efficiently under the above-mentioned reaction conditions.
In this application, the inert gas refers to any gas or gas mixture that does not chemically react with the reactants and reaction products, such as nitrogen, helium, etc.
The beneficial technical effect of this application: according to the preparation method, the oil-in-water type seed latex with the particle size of about 20nm is prepared by adopting a specific process and raw materials, the seed latex is added into the preparation raw materials of the carboxylated nitrile latex, the seed latex is used as a core, the particle size of initial colloidal particles can be controlled, and the later stage is controlled stably by temperature, so that the prepared carboxylated nitrile latex has uniform particle size distribution, small particle size distribution (the particle size distribution is about 130 nm), narrow particle size distribution, excellent chemical stability and mechanical stability and good application prospect.
Drawings
FIG. 1 is a flow chart of seed latex preparation in example 1.
Detailed Description
In order that the present application may be more readily understood, the following examples are presented in conjunction with the following detailed description, which are intended to be illustrative only and are not intended to limit the scope of application of the present application. The starting materials or components used in the present application may be prepared by commercial or conventional methods unless specifically indicated.
Example 1: preparation of seed latex
The flow chart of the seed latex preparation in this example is shown in fig. 1, and the specific preparation method is as follows:
step 1: 400kg of deionized water and 42kg of sodium dodecylbenzenesulfonate were heated to 85℃in a jacketed 1# reactor with stirring at 100rpm to prepare an aqueous solution of sodium dodecylbenzenesulfonate (the concentration of sodium dodecylbenzenesulfonate in the solution was 9.5 wt%) for use. 133kg of deionized water was added to a 2# reactor having a jacket function, heated to 60℃under stirring at 60rpm, then 1.2kg of itaconic acid was slowly added, stirred until complete dissolution was achieved, and an aqueous solution of itaconic acid (the concentration of itaconic acid in the solution was 0.9% by weight) was prepared, and then the aqueous solution of all itaconic acid in the 2# reactor was completely transferred to a 1# reactor, to obtain a mixed solution 1. The temperature in reactor # 1 was maintained at 85 ℃.
Step 2: styrene (18.5 kg), 2-ethylhexyl acrylate (29.8 kg), methyl methacrylate (6.9 kg) and 2-hydroxyethyl acrylate (1.1 kg) (mass ratio of 2-ethylhexyl acrylate, methyl methacrylate to 2-hydroxyethyl acrylate: 29.8:6.9:1.1) were charged into a 3# reactor having a jacket function, and stirring was started at 60rpm for 5 minutes to obtain a mixed solution 2.
Step 3: 2.9kg of deionized water and 1.1kg of sodium persulfate SPS are added into a 4# reactor with a stirring function, and the mixture is stirred and completely melted to obtain an aqueous solution of sodium persulfate (the concentration of sodium persulfate in the solution is 27.5 wt%).
Step 4: 52.9kg of deionized water and 0.8kg of sodium persulfate SPS are added into a 5# reactor with a stirring function, and 0.4kg of 48wt% potassium hydroxide solution is added, and the mixture is uniformly stirred to obtain an alkaline aqueous solution containing sodium persulfate (active water, wherein the concentration of sodium persulfate in the solution is 1.5wt%, the concentration of potassium hydroxide is 0.35wt%, and the mass ratio of potassium hydroxide to sodium persulfate is 1:4.2) for standby.
Step 5: the reaction was carried out by transferring 10wt% of the mixed solution 2 from the 3# reactor to the 1# reactor while keeping the 1# reactor at 85℃and stirring at 100rpm, and then immediately transferring all of the aqueous solution of sodium persulfate in the 4# reactor to the 1# reactor, and starting the time for 15 minutes.
Step 6: the remaining mixed solution 2 in the # 3 reactor was added dropwise to the # 1 reactor at a rate of 0.4 kg/min, and the alkaline aqueous solution containing sodium persulfate in the # 5 reactor was added dropwise to the # 1 reactor at a rate of 0.4 kg/min. After the completion of the dropwise addition, the reaction was continued at 91℃for 90 minutes to obtain a seed latex. In the preparation process, the mass ratio of the itaconic acid to the emulsifier to the styrene to the acrylate monomer to the first initiator to the second initiator is 1.2:42:18.5:37.8:1.1:0.8.
Example 2: preparation of seed latex
The preparation process is basically the same as in example 1, except for step 2:18.5 kg of styrene and 37.8kg of methyl methacrylate were charged into a 3# reactor having a jacket function, and stirring was started at 60rpm for 5 minutes to obtain a mixed solution 2.
Example 3: preparation of seed latex
The preparation process is basically the same as in example 1, except for step 2:18.5 kg of styrene and 37.8kg of 2-ethylhexyl acrylate were charged into a jacketed 3# reactor, and stirring was started at 60rpm for 5 minutes to obtain a mixed solution 2.
Example 4: preparation of seed latex
The preparation process is basically the same as in example 1, except for step 2:18.5 kg of styrene and 37.8kg of 2-hydroxyethyl acrylate were charged into a 3# reactor having a jacket function, and stirring was started at 60rpm for 5 minutes to obtain a mixed solution 2.
Example 5: preparation of seed latex
The preparation process is basically the same as in example 1, except for step 2:18.5 kg of styrene, 6.9g of 2-ethylhexyl acrylate, 29.8kg of methyl methacrylate and 1.1kg of 2-hydroxyethyl acrylate (mass ratio of 2-ethylhexyl acrylate, methyl methacrylate and 2-hydroxyethyl acrylate: 6.9:29.8:1.1) were charged into a 3# reactor having a jacket function, and stirring was started at 60rpm for 5 minutes to obtain a mixed solution 2.
Example 6: preparation of seed latex
The preparation process is basically the same as in example 1, except that in step 4, 52.9kg of deionized water is added into a 5# reactor with stirring function, 0.8kg of sodium persulfate SPS is added, 0.8kg of 48wt% potassium hydroxide solution is added, and the mixture is stirred uniformly to obtain an alkaline aqueous solution containing sodium persulfate, wherein the mass ratio of potassium hydroxide to sodium persulfate in the alkaline aqueous solution is 1:2.1.
Example 7: preparation of seed latex
The preparation process is basically the same as in example 1, except that in step 4, 52.9kg of deionized water is added into a 5# reactor with stirring function, 0.8kg of sodium persulfate SPS is added, 0.3kg of 48wt% potassium hydroxide solution is added, and the mixture is stirred uniformly to obtain an alkaline aqueous solution containing sodium persulfate, wherein the mass ratio of potassium hydroxide to sodium persulfate in the alkaline aqueous solution is 1:5.6.
Example 8: preparation of seed latex
The preparation process was substantially the same as in example 1 except that in step 6, after the completion of the dropping, the reaction was continued at 80℃for 90 minutes to prepare a seed latex.
Application example 1: preparation of carboxylated nitrile latex
10kg of the seed latex prepared in example 1 was charged into a polymerization reactor, 26kg of acrylonitrile, 66kg of butadiene and 8kg of methacrylic acid were charged into the polymerization reactor, the polymerization reactor was evacuated and then filled with nitrogen gas of 99.99% purity for substitution, the pressure in the polymerization reactor was maintained at 0.4MPa, stirring was started, the rotation speed was maintained at 70rpm, the temperature was raised to 37℃and the reaction was carried out for 15 hours, thereby obtaining carboxylated nitrile latex 1.
Application examples 2-8: preparation of carboxylated nitrile latex
Application examples 2 to 8 the preparation process was basically the same as application example 1, except that 10kg of the seed latex prepared in example 1 was replaced with the seed latex prepared in examples 2 to 8, respectively, to thereby prepare carboxylated nitrile latex 2 to 8, respectively.
Application example 9: preparation of carboxylated nitrile latex
The preparation process was substantially the same as in application example 1, except that 5kg of the seed latex prepared in example 1 was charged into a polymerization reactor, and finally carboxylated nitrile latex 9 was prepared.
Application example 10: preparation of carboxylated nitrile latex
The preparation process was substantially the same as in application example 1, except that 8kg of the seed latex prepared in example 1 was charged into a polymerization reactor, and finally carboxylated nitrile latex 10 was prepared.
Application example 11: preparation of carboxylated nitrile latex
The preparation process was substantially the same as in application example 1, except that 15kg of the seed latex prepared in example 1 was charged into a polymerization reactor, and finally carboxylated nitrile latex 11 was prepared.
Test example 1
The carboxylated nitrile latices 1 to 11 obtained in application examples 1 to 11 were subjected to performance test in accordance with the following methods, and the test results are shown in Table 1.
Total solid content: SH/T1154-92
Viscosity: SH/T1152-92
Surface tension: SH/T1156-92
Particle size: malvern ZETA SIZER particle size meter
Mechanical stability: SH/T1151-92
Chemical stability: SH/T1608-95
TABLE 1
From the test data of carboxylated nitrile latex 1-5 in Table 1, it is understood that when the acrylate monomer in the preparation mixture 2 (oil phase) includes 2-ethylhexyl acrylate, methyl methacrylate and 2-hydroxyethyl acrylate at the same time, the particle size distribution of the carboxylated nitrile latex prepared by using the seed latex prepared therefrom is narrow, and the mechanical stability and chemical stability are superior; meanwhile, when the mass ratio of the 2-ethylhexyl acrylate to the methyl methacrylate to the 2-hydroxyethyl acrylate is in the range of (25-35): (5-10): (1-2), the particle size distribution of the finally prepared carboxylated nitrile latex is narrower, and the mechanical stability and the chemical stability are better. From the test data of carboxylated nitrile latex 1, 6 and 7 in Table 1, it is understood that when the mass ratio of the alkaline substance (potassium hydroxide) to the second initiator (sodium persulfate) in the alkaline aqueous solution is in the range of 1 (3 to 5), the particle size distribution of the finally produced carboxylated nitrile latex is narrower and the mechanical stability and chemical stability are better. From the test data of carboxylated nitrile latex 1, 8 in Table 1, it is known that when seed latex is prepared, if the reaction temperature is too low, the mechanical stability and chemical stability of the finally prepared carboxylated nitrile latex are significantly lowered. As is apparent from the carboxylated nitrile latex 1, 9-11 in Table 1, when the weight part of the seed latex is 8-12 parts, it is more advantageous to improve the mechanical stability and chemical stability of the carboxylated nitrile latex when the carboxylated nitrile latex is prepared.
It should be noted that the above-described embodiments are only for explaining the present application, and do not constitute any limitation to the present application. The present application has been described with reference to exemplary embodiments, but it is understood that the words which have been used are words of description and illustration, rather than words of limitation. Modifications may be made to the present application as defined within the scope of the claims of the present application, and the invention may be modified without departing from the scope and spirit of the present application. Although the present application is described herein with reference to particular methods, materials and embodiments, the present application is not intended to be limited to the particular examples disclosed herein, but rather, the present application is intended to extend to all other methods and applications having the same functionality.
Claims (11)
1. A process for preparing a seed latex for preparing a carboxylated nitrile latex, the process comprising the steps of:
s1, heating the temperature in a reactor containing an aqueous solution of an emulsifier in a stirring state, maintaining the temperature at 80-85 ℃, and then adding the aqueous solution of itaconic acid into the reactor to be mixed with the aqueous solution of the emulsifier to obtain a mixed solution 1;
s2, mixing styrene with an acrylic ester monomer to obtain a mixed solution 2;
s3, adding 10-20wt% of the mixed solution 2 and the aqueous solution of the first initiator into a reactor for reaction to obtain a first reaction mixed solution;
s4, dropwise adding the rest of the mixed solution 2 and an alkaline aqueous solution containing a second initiator into the reactor, and reacting after heating to obtain the seed latex for preparing the carboxylated nitrile latex;
the acrylic ester monomer comprises 2-ethylhexyl acrylate, methyl methacrylate and 2-hydroxyethyl acrylate;
in the step S4, the reaction temperature is 90-95 ℃.
2. The method of claim 1, wherein the mass ratio of itaconic acid, emulsifier, styrene, acrylate monomer, first initiator and second initiator is (1-1.5): (40-50): (15-20): (30-40): (0.8-1.2).
3. The method according to claim 1 or 2, wherein the emulsifier is selected from at least one of sodium alkyl sulfonate, sodium alkyl benzene sulfonate and sodium alkyl diphenyl ether disulfonate; and/or
The first initiator and the second initiator are each independently selected from at least one of sodium persulfate, ammonium persulfate, and potassium persulfate.
4. The method according to claim 1 or 2, wherein the mass ratio of 2-ethylhexyl acrylate, methyl methacrylate and 2-hydroxyethyl acrylate is (25-35): 5-10): 1-2.
5. The method according to claim 1 or 2, wherein in step S4, the alkaline substance in the alkaline aqueous solution is selected from at least one of sodium hydroxide and potassium hydroxide.
6. The method according to claim 5, wherein the mass ratio of the alkaline substance to the second initiator is 1 (3-5).
7. The method according to claim 1 or 2, wherein in step S3, the reaction time is 10 to 20min; and/or
In the step S4, the reaction time is 1-2 hours.
8. The preparation method of the carboxylated nitrile latex is characterized by comprising the following raw materials in parts by weight:
5-15 parts of seed latex prepared by the method of any one of claims 1-7;
20-30 parts of acrylonitrile;
50-80 parts of butadiene;
5-10 parts of a third monomer containing carboxylic acid.
9. The carboxylated nitrile latex according to claim 8, wherein the carboxylic acid containing third monomer is selected from at least one of acrylic acid, methacrylic acid, itaconic acid, fumaric acid, and maleic acid.
10. A process for the preparation of a carboxylated nitrile latex according to claim 8 or 9, comprising the steps of: and adding the seed latex, acrylonitrile, butadiene and a third monomer containing carboxylic acid into a polymerization reaction kettle, and reacting under the protection of inert gas to obtain the carboxylated nitrile latex.
11. The method of claim 10, wherein the reaction conditions are: rotational speed: 50-100 rpm, reaction pressure: 0.3-0.5 MPa, and the reaction temperature is as follows: 30-40 ℃, and the reaction time is as follows: and (5) 10-15 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211410886.8A CN115677914B (en) | 2022-11-11 | 2022-11-11 | Preparation method and application of seed latex for preparing carboxylated nitrile latex |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211410886.8A CN115677914B (en) | 2022-11-11 | 2022-11-11 | Preparation method and application of seed latex for preparing carboxylated nitrile latex |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115677914A CN115677914A (en) | 2023-02-03 |
| CN115677914B true CN115677914B (en) | 2023-07-11 |
Family
ID=85051529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211410886.8A Active CN115677914B (en) | 2022-11-11 | 2022-11-11 | Preparation method and application of seed latex for preparing carboxylated nitrile latex |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115677914B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6447974B1 (en) * | 2001-07-02 | 2002-09-10 | Xerox Corporation | Polymerization processes |
| CN107177021A (en) * | 2016-03-11 | 2017-09-19 | 中国石油化工股份有限公司 | A kind of carboxylic acrylonitrile butadiene rubber latex and preparation method thereof |
| CN113683728A (en) * | 2021-07-02 | 2021-11-23 | 上海昶法新材料有限公司 | Preparation method of carboxylated butyronitrile latex |
| CN113831439A (en) * | 2021-11-02 | 2021-12-24 | 上海昶法新材料有限公司 | Carboxylated butyronitrile latex for papermaking and preparation method thereof |
-
2022
- 2022-11-11 CN CN202211410886.8A patent/CN115677914B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6447974B1 (en) * | 2001-07-02 | 2002-09-10 | Xerox Corporation | Polymerization processes |
| CN107177021A (en) * | 2016-03-11 | 2017-09-19 | 中国石油化工股份有限公司 | A kind of carboxylic acrylonitrile butadiene rubber latex and preparation method thereof |
| CN113683728A (en) * | 2021-07-02 | 2021-11-23 | 上海昶法新材料有限公司 | Preparation method of carboxylated butyronitrile latex |
| CN113831439A (en) * | 2021-11-02 | 2021-12-24 | 上海昶法新材料有限公司 | Carboxylated butyronitrile latex for papermaking and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Preparation of micron-size monodispersed PS/P(St/MMA) microspheres by seeded dispersion polymerization;Hong-Tao Zhang等;《Journai of Applied Polymer Science》;第99卷(第6期);第3586-3591页 * |
| 制备高固含量丁苯胶乳的小试技术研究;魏艳星;《中国优秀硕士学位论文全文数据库 工程科技I辑》(第1期);B016-799 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115677914A (en) | 2023-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4233219B2 (en) | Redispersible powder and aqueous dispersion thereof, production method and use method | |
| US4130523A (en) | High solids latexes | |
| US3563946A (en) | Process for latex manufacture | |
| CN105440219A (en) | PVC (polyvinyl chloride) paste resin and preparation method thereof | |
| CN115677914B (en) | Preparation method and application of seed latex for preparing carboxylated nitrile latex | |
| WO2006039860A1 (en) | A preparation method of small particle sized polybutadiene latex used for the production of abs | |
| JPS61215603A (en) | Production of polymer particle | |
| CN115304818B (en) | Ultralow-temperature thermal expansion microsphere prepared based on Pickering emulsion polymerization method and preparation method thereof | |
| CN103360529A (en) | Controllable synthetic method of micro-sized mono-disperse polystyrene microsphere | |
| WO2024130825A1 (en) | Synthetic method for large-particle-size polybutadiene latex | |
| CN102030867B (en) | Method for preparing vinyl chloride graft copolymer resins | |
| JP2509224B2 (en) | Method for producing high solid content emulsion polymer composition | |
| CN107778403B (en) | Styrene-acrylic latex and preparation method and application thereof | |
| JPH07238105A (en) | Particle of highly crosslinked polymer and production thereof | |
| CN105273119A (en) | Preparation method for high-polymerization-degree polyvinyl chloride resin | |
| JP3563234B2 (en) | Method for producing vinyl chloride polymer latex | |
| CN115677878B (en) | Preparation method and application of free radical polymerization catalyst based on liquid metal | |
| JP2748013B2 (en) | Method for producing powdery acrylic resin | |
| JPH08198903A (en) | Production of polymer latex | |
| CN108424485A (en) | A kind of production method of vinyl chloride-vinyl acetate interpolymer paste resin | |
| JP7511634B2 (en) | Method for producing vinyl chloride-vinyl acetate copolymer latex | |
| JPH01315454A (en) | Highly crosslinked polymer particle and production thereof | |
| JP2727330B2 (en) | Method for producing finely divided polymer | |
| CN107674140A (en) | A kind of production method of styrene-acrylic emulsion surface sizing agent | |
| JP2022549233A (en) | Method for producing vinyl chloride-acrylic copolymer latex |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |