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Process for polymerization preparation of macromolecular emulsion without heating

A technology of polymer emulsion and emulsion polymerization, which is applied in the field of preparation of polymer emulsion polymerization, can solve the problems of complex polymerization process, decrease of polymer molecular weight, and high equipment investment, so as to reduce process operation, improve polymerization efficiency, and ensure stable quality Effect

Inactive Publication Date: 2006-09-27
ANHUI UNIVERSITY
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Problems solved by technology

However, this technique obviously has some disadvantages: during the dropping process, the monomer concentration in the reaction system is always at a low level, and the reaction temperature is relatively high, which is not conducive to improving the molecular weight of the polymer from the principle of polymerization, and at the same time The continuous introduction of polymerization inhibitors (inhibitors, impurities, oxygen, etc. in the monomer) into the monomer emulsion that is added will also lead to a decrease in the molecular weight of the polymer.
Emulsion polymerization is usually the main industrial method for us to pursue high molecular weight polymers. In many applications, the molecular weight of polymers plays an important role in determining the properties of latex. Therefore, the performance of latex produced by semi-continuous method is limited to a certain extent.
At the same time, due to the use of ionic initiators, it is easy to produce some oligomers when the monomer concentration is very low. These oligomers generally have surface activity. many adverse effects
Another problem with the traditional emulsion polymerization process is that heating equipment is generally required, because the monomer emulsion polymerization of unsaturated olefins is usually initiated by free radical polymerization
Among them, the photolysis and radiation initiation of initiators can initiate emulsion polymerization at a very wide temperature, but because the polymerization process is too complicated, the equipment investment is too high, and the application is limited. At present, there are few successful industrial examples.
Initiator thermal decomposition is an important method of traditional emulsion polymerization. The disadvantage is that the decomposition temperature of the initiator is generally relatively high. For example, the commonly used persulfate triggers emulsion polymerization. If you want to observe an obvious polymerization process, the temperature should not be lower than 50 ° C. Obviously, even at such temperature, heating is unavoidable for the polymerization process, because the ambient temperature is usually below 30 °C
The redox decomposition of the initiator can initiate emulsion polymerization in a very wide temperature range. However, among the methods introduced by industry and patents, there are many methods whose initiation temperature has dropped to 30°C, which can meet the requirements of the ambient temperature. However, during the polymerization process Due to process design issues, heating is still required to complete the polymerization process
At the same time, when the ambient temperature is lower, or when the heat release of the polymerization system is relatively high, the method is limited, and a two-step method is required to obtain a polymer emulsion with a conventional solid content, which is obviously unfavorable for the synthesis of polymer emulsions.

Method used

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  • Process for polymerization preparation of macromolecular emulsion without heating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] see attached figure 1 , raw material selection: methyl acrylate (MA), butyl acrylate (BA), acrylonitrile (AN), acrylic acid (AA), N,N-methylenebisacrylamide (NNMBAN), diisooctyl succinate sulfonate Sodium (AOT), Potassium Persulfate (PPS), Ascorbic Acid (LAAS), Ammonia (AW).

[0021] Process: Mix 17 parts MA, 5.5 parts BA, 5.5 parts AN, 0.9 parts AA, 0.00035 parts NNMBAN, 1.5 parts AOT, 0.25 parts AW and water. Emulsify at high speed for 15 minutes. Start stirring, and deoxygenate with nitrogen for 5 minutes. 0.13 parts of PPS were added, and at room temperature of 15°C, 0.04 parts of LAAS were added. After nine minutes, the temperature of the emulsion system reached 69°C, and cooling water was started. When the temperature reached 78°C, the temperature was stopped and the cooling was stopped. After fifteen minutes, the temperature of the emulsion system was 74°C, and the cooling was continued until the temperature of the emulsion system was 65°C. A solution of 0.04...

Embodiment 2

[0024] Raw material selection: methyl acrylate (MA), butyl acrylate (BA), 2-ethylhexyl acrylate (IOA), acrylic acid (AA), nonylphenol polyoxyethylene ammonium sulfate (PAS), N,N-sulfite Methylbisacrylamide (NNMBAN), hydrogen peroxide (POH), ascorbic acid (LAAS), ammonia water (AW).

[0025] Process: Mix 33.5 parts BA, 22.5 parts IOA, 2.5 parts AA, 2.2 parts PAS, 0.5 parts AW, 0.0018 parts NNMBAN and water. Emulsify at high speed for 25 minutes. Start stirring, and deoxygenate with nitrogen for 4 minutes. 0.085 part of POH was added, and at room temperature 25°C, 0.04 part of LAAS was added. Ten minutes later, the temperature of the emulsion system reached 65°C, and cooling water was started. When the temperature reached 78°C, the temperature stopped rising, and cooling was stopped. 0.004 part of MA was added, and 0.025 part of LAAS 10% solution was added in about 70 minutes. The reaction was completed for another 10 minutes, 0.27 part of AW was added, the temperature of the...

Embodiment 3

[0028] Raw material selection: methyl acrylate (MA), ethyl acrylate (EA), methacrylic acid (MAA), N-hydroxymethylene acrylamide (NHMAM), nonylphenol polyoxyethylene ammonium sulfate (PAS), peroxide Hydrogen (POH), Erythorbic Acid (DAAS), Ammonia (AW).

[0029] Process: Mix 16 parts EA, 11 parts MAA, 0.065 parts NHMAM, 1.4 parts PAS, 0.18 parts AW and water. Emulsify at high speed for 18 minutes. Start stirring and deoxygenate with nitrogen for 3 minutes. 0.092 parts of POH were added, and at room temperature 10°C 0.043 parts of DAAS were added. After four minutes, the temperature of the emulsion system reached 55 °C, and the cooling water was started. After the maximum temperature reached 82 °C, the cooling was stopped for ten minutes. After fifteen minutes, the temperature of the emulsion system was 70 °C, and the temperature of the emulsion system was 65 °C. parts MA, 0.042 parts of LAAS 10% solution was added over an hour or so. The reaction was completed for another 15...

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Abstract

The invention discloses a polymeric preparing method of macromolecular emulsion without heating, which comprises the following steps: acting 15-62 percent unsaturated olefin, 0.5-15 percent emulsifying agent, 0-8 percent pH adjustant and 82-33 percent water together at atmosphere temperature with oxidant and reducer; forming macromolecular emulsion through emulsion polymeric parttern. The invention improves the polymeric efficiency, which saves large amount of cool water.

Description

Technical field: [0001] The invention relates to a preparation method for polymer emulsion polymerization without heating or heating. Background technique: [0002] Emulsion polymerization is an important method for synthesizing polymers. There are three main methods: continuous method, semi-continuous method and batch method. The most commonly used method is the semi-continuous method, which is usually initiated by persulfate and polymerized at a temperature of 65 to 90 °C. The advantage of this polymerization is that the polymerization process is simple to control, the reaction can be kept relatively stable, and the quality is relatively stable. However, this process obviously has some disadvantages: in the dropwise addition process, the monomer concentration in the reaction system is always at a low level, and the reaction temperature is relatively high, which is not conducive to increasing the molecular weight of the polymer in terms of polymerization principle, and at ...

Claims

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Application Information

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IPC IPC(8): C08F2/22C08F20/00C08F4/40
Inventor 吴志超
Owner ANHUI UNIVERSITY
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