CN111167395B - System and method for continuously producing hydroxyl acrylic resin aqueous dispersion - Google Patents
System and method for continuously producing hydroxyl acrylic resin aqueous dispersion Download PDFInfo
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
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- B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
Abstract
The invention discloses a system and a method for continuously producing hydroxyl acrylic resin aqueous dispersion, wherein the system comprises a prepolymerization reaction kettle, a high-speed mixer, a first static mixer, a second static mixer, a first gear pump, a second gear pump, a dispersion kettle and a finished product storage tank; in the method, a hydroxyl acrylic resin prepolymer enters a high-speed mixer through a first gear pump and a first flowmeter after being synthesized in a prepolymerization reaction kettle, a neutralizing agent and process water are mixed in a first static mixer and then enter the high-speed mixer, the prepolymer and the neutralizing agent are neutralized in the high-speed mixer, the neutralized prepolymer and the neutralizing agent enter a dispersion kettle, the neutralized prepolymer and the process water are mixed and dispersed in the dispersion kettle to form a pre-dispersion body, then the pre-dispersion body enters a second static mixer, the pre-dispersion body is further mixed and dispersed with the process water to form an aqueous dispersion body, and finally the aqueous dispersion body enters a finished product storage tank. The method can continuously produce the hydroxyl acrylic aqueous dispersion in large batch, and has high production efficiency and uniform and stable particle size distribution of the aqueous dispersion.
Description
Technical Field
The invention belongs to the technical field of continuous production of aqueous hydroxyl acrylic resin aqueous dispersion, and particularly relates to a system and a method for continuously producing aqueous hydroxyl acrylic resin dispersion.
Background
With the increasing awareness of environmental protection and the stricter environmental regulations, the problem of VOC (volatile organic compound) emission is attracting attention. The water-based hydroxy acrylic acid taking water as a dispersion medium has excellent performances such as environmental protection, light resistance, aging resistance, chemical resistance and the like, and the low production cost is developed at a high speed, so that the water-based hydroxy acrylic acid becomes a resin with the largest yield in the field of water-based paint. The paint is widely applied to coating and protection in the industrial and civil fields of airplanes, automobiles, instruments, equipment, buildings, furniture and the like. Compared with the traditional solvent-based paint, the water-based hydroxyl acrylic resin dispersoid takes water to replace an organic solvent as a dispersion medium, contains a small amount of volatile organic solvent, and is an organic polymer paint with low toxicity and low odor.
At present, the industrial production of the hydroxyl acrylic resin aqueous dispersion is mainly carried out in a batch kettle type, a hydroxyl acrylic prepolymer is synthesized in a prepolymerization reaction kettle, then is cooled, is transferred to a dispersion kettle in batches for neutralization, is gradually added with dispersion water, and is transferred to a buffer tank after being dispersed to be qualified. The production efficiency is low, the production energy consumption is high, the products in batches are different, the production is unstable, and the kettle is washed after each batch is dispersed, so that excessive kettle washing waste liquid is generated.
Patent CN 102164660B provides a continuous dispersion method, said dispersion device is capable of continuous dispersion by shearing of a stator and a rotor. The dispersion treated by the method has low viscosity, the retention time of the dispersion in the device is too short, complete phase transformation cannot be formed, the dispersed phase can be dispersed into the continuous phase only through strong shearing, the formed dispersed particle size distribution is wide, double peaks easily appear, the emulsion is unstable, and the emulsion is easy to delaminate after being stored for a long time.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a system and a method for continuously producing hydroxyl acrylic resin aqueous dispersion, which realize high-efficiency and continuous operation and have good product dispersion effect.
In order to achieve one aspect of the above purpose, the invention adopts the following technical scheme:
a system for continuously producing a hydroxyl acrylic resin aqueous dispersion comprises a prepolymerization reaction kettle, a high-speed mixer, a first static mixer, a second static mixer, a first gear pump, a second gear pump, a dispersion kettle and a finished product storage tank;
wherein the prepolymerization reactor is connected to one inlet of the high-speed mixer through the first gear pump, the first static mixer is used for mixing a neutralizing agent with a first part of process water, an outlet of the first static mixer is connected to the other inlet of the high-speed mixer, and an outlet of the high-speed mixer is connected to a feed inlet of the dispersion tank; the dispersion kettle is used for mixing and dispersing the feed from the high-speed mixer and a second part of process water, and a discharge hole of the dispersion kettle is connected to the second static mixer through a second gear pump; the second static mixer is used for uniformly mixing the feed from the dispersion kettle and a third part of process water and sending a mixed product into the finished product storage tank.
In the system of the present invention, the prepolymerization reactors can be arranged in 1 or more, preferably 2 to 4, and arranged in parallel to better realize continuous production.
In the system of the present invention, the first gear pump is connected to the high-speed mixer through a first flow meter, and the first static mixer is connected to the high-speed mixer through a second flow meter.
In order to achieve another aspect of the above objects, the present invention also provides a method for continuously producing an aqueous dispersion of a hydroxyacrylic resin using the above system, wherein the object to be subjected to the dispersion treatment to produce the dispersion is an acrylic prepolymer obtained by polymerization in the prepolymerization reaction tank.
In the present invention, all the percentages are by mass unless otherwise specified.
According to the method of the present invention, preferably, the amount of the first portion of process water (such as deionized water) entering the first static mixer is 10 to 20 wt%, such as 12 wt%, 15 wt% or 18 wt%, of the total amount of process water added in the reaction system; wherein the total added amount of the process water is the sum of the first part of the process water, the second part of the process water and the third part of the process water; in one embodiment, the neutralizing agent used is N, N-dimethylethanolamine, and it will be understood by those skilled in the art that the amount of neutralizing agent required to neutralize the prepolymer can be readily determined and thus the flow rate can be adjusted by adjusting the concentration of the aqueous solution of the neutralizing agent, which in the present invention is generally controlled at a pH of about 7 to 8, e.g., 7.5, preferably up to 100% neutralization; in one embodiment, the aqueous neutralizer solution entering the first static mixer of the high speed mixer may be at a temperature of 30 to 40 ℃ such as 35 ℃ and the prepolymer entering the high speed mixer may be at a temperature of 115 ℃ and 125 ℃ such as 120 ℃; the linear velocity of the agitation in the high speed mixer is 20-25m/s, such as 22 m/s.
According to the method of the present invention, preferably, the amount of the second portion of the process water entering the dispersion tank is 20% to 50% by weight, such as 30% or 40% by weight, of the total amount of process water added; the temperature in the dispersion kettle is 70-80 ℃, such as 75 ℃, the retention time is 10-15min, such as 12min, and the dispersion rotation speed is 1000-.
According to the method of the present invention, preferably the water temperature of the process water entering the second static mixer is from 10 ℃ to 40 ℃, such as 20 ℃ or 30 ℃, preferably from 15 ℃ to 25 ℃.
According to the process of the present invention, preferably, the total amount of process water added is 90-110 wt%, such as 100 wt%, of the discharge amount of the prepolymerization reactor.
In the present invention, the object to be subjected to the dispersion treatment to produce the dispersion is an acrylic prepolymer obtained by polymerization in the prepolymerization reactor, and in one embodiment, the reaction raw materials in the prepolymerization reactor include: 35-45 wt% of methyl methacrylate, 10-15 wt% of styrene, 10-18 wt% of hydroxyethyl acrylate, 10-15 wt% of butyl acrylate, 3-8 wt% of acrylic acid, 5-8 wt% of isobornyl methacrylate, 2-5 wt% of dibenzoyl peroxide (initiator), 10-14 wt% of propylene glycol butyl ether and 1-4 wt% of dodecyl mercaptan (chain transfer agent) based on the total weight of the reaction raw materials; during the reaction, the prepolymerization reactor is heated to 68-72 ℃, such as 70 ℃, then the mixed solution of propylene glycol butyl ether and the first part of initiator (dibenzoyl peroxide BPO) is added, the prepolymerization reactor is started to stir, nitrogen is introduced for protection, and then the temperature is raised to 148-152 ℃, such as 150 ℃: preparing a monomer mixture (a mixture of MMA, St, HEA, BA, AA and IBOMA) according to the proportion of the reaction raw materials, uniformly mixing a second part of initiator (BPO) and chain transfer agent (DDM), feeding 8-12wt percent, such as 10wt percent of the monomer mixture and the uniformly mixed initiator and chain transfer agent into the prepolymerization reaction kettle at one time after the temperature is raised to 158-162 ℃, such as 160 ℃, reacting for 40-70min, such as 60min, and then gradually adding the rest of the monomer mixture for 4-6 h, such as 5 h; after the addition, the temperature is kept for 1 to 2 hours, such as 1.5 hours, and then the light yellow transparent acrylic acid prepolymer is obtained. The first part of the initiator accounts for 10-30 wt% of the total amount of the initiator, wherein the total amount of the initiator is the sum of the first part of the initiator and the second part of the initiator.
Compared with the prior art, the invention has the following advantages:
in the invention, hydroxyl acrylic prepolymer and neutralizer from a static mixer are dispersed and neutralized by a high-speed mixer; mixing and dispersing the neutralized prepolymer with process water in a dispersion kettle to form a pre-dispersion body; then the pre-dispersion forms stable and qualified water dispersion with process water in a static mixer, and the water dispersion is pumped into a finished product storage tank, so that high-efficiency, low-energy consumption and continuous operation are realized; the method has the advantages of safety, high efficiency, great reduction of production energy consumption and production cost, overcoming the problems of difficult dispersion caused by extremely high viscosity point during mesophase transition and small single kettle yield when hydroxypropyl dispersion is carried out by adopting different dispersion forms and gradually dispersing in proper amount, avoiding the problem of high viscosity during continuous production and dispersion, along with easy dispersion, high yield, uniform and stable particle size distribution of the aqueous dispersion, and wide application of the obtained hydroxyl acrylic emulsion in the industrial and civil fields of airplanes, automobiles, instruments, equipment, buildings, furniture and the like.
Drawings
FIG. 1 is a schematic diagram of the system for continuously producing an aqueous dispersion of a hydroxyacrylic resin according to the present invention;
the system comprises a prepolymerization reaction kettle 1, a first gear pump 2, a first flowmeter 3, a first static mixer 4, a second flowmeter 5, a high-speed mixer 6, a dispersion kettle 7, a second gear pump 8, a second static mixer 9, a finished product storage tank 10, a neutralizer pipeline 11, a first static mixer process water pipeline 12, a dispersion kettle process water pipeline 13 and a second static mixer process water pipeline 14.
Detailed Description
The invention is further illustrated by the following figures and examples, without however being limited thereto.
As shown in fig. 1, the system of the present invention comprises a prepolymerization reactor 1, a high-speed mixer 6, a first static mixer 4, a second static mixer 9, a first gear pump 2, a second gear pump 8, a dispersion tank 7 and a finished product storage tank 10; the prepolymerization reactor 1 is connected to one inlet of the high-speed mixer 6 through the first gear pump 2, the first static mixer 4 is used for mixing a neutralizing agent with process water from a first static mixer process water pipeline 12, an outlet of the first static mixer 4 is connected to the other inlet of the high-speed mixer 6, and an outlet of the high-speed mixer 6 is connected to a feed inlet of the dispersion tank 7; the dispersion kettle 7 is used for mixing and dispersing the feed from the high-speed mixer 6 and the process water from a dispersion kettle process water pipeline 13, and the discharge hole of the dispersion kettle is connected to the second static mixer 9 through a second gear pump 8; the second static mixer 9 is used to mix the feed from the dispersion vessel 7 with the process water from the second static mixer process water line 14 and to feed the mixed product to the product tank 10. Wherein the first gear pump 2 is connected to the high-speed mixer 6 through a first flow meter 3, and the first static mixer 4 is connected to the high-speed mixer 6 through a second flow meter 5.
In the present invention, in operation, the aqueous solution of the neutralizing agent from the first static mixer 4 and the hydroxyacrylic acid prepolymer from the prepolymerization reactor 1 are neutralized and predispersed in the high-speed mixer 6. The neutralized prepolymer is further dispersed with process water in a dispersion vessel 7 to form a dispersion. Then the dispersion is dispersed with the process water in the static mixer 9 to form a stable and qualified aqueous dispersion, and the aqueous dispersion is pumped into a finished product storage tank, thereby realizing high-efficiency, low-energy consumption and continuous operation.
The following is further illustrated with reference to the examples.
Example 1
Heating a prepolymer reaction kettle prepolymerization kettle to 70 ℃, adding a mixed solution of propylene glycol butyl ether and a first part of initiator (30% of total dibenzoyl peroxide (BPO)) for bottoming, opening the prepolymer reaction kettle for stirring, introducing nitrogen for protection, and heating to the reflux temperature of 150 ℃: preparing monomers according to the proportion in a formula table, uniformly mixing a second part of initiator (70 percent of the total BPO) and a chain transfer agent DDM, and adding 10 percent of monomer mixture into a prepolymerization kettle at one time after the temperature is raised to 160 ℃ to serve as reaction seeds; after 1 hour, the residual monomer mixture is constantly added dropwise, and the dropwise addition is completed within about 5 hours; after the addition, the temperature is kept for 1.5h, and the light yellow transparent acrylic prepolymer A is obtained. After the temperature is reduced to 120 ℃, the mixture enters a high-speed mixer (the linear speed is 22m/s) together with a neutralizer (N, N-dimethylethanolamine) aqueous solution (containing 20% of process water and being 30 ℃) from a first static mixer at the flow rate of 1KG/min through a mass flow meter and a gear pump, the mixture enters a dispersion kettle after being neutralized (until the system PH is about 7.5), the mixture is mixed and dispersed with 30% of process water in the dispersion kettle (the temperature of the dispersion kettle is 75 ℃, the rotating speed is 1200 and the retention time is 15 minutes) to form a pre-dispersion body, the pre-dispersion body enters a second static mixer, the pre-dispersion body is mixed and dispersed with 50% of process water (23 ℃) in the second static mixer to obtain a qualified water dispersion body, and the qualified water dispersion body enters a finished product storage tank. Wherein the total addition of the process water is 100 wt% of the discharge amount of the prepolymerization reaction kettle.
Example 1 reaction raw material ratio table:
| name of raw materials | Mass fraction% |
| Methyl methacrylate (MMA, Sponger) | 35 |
| Styrene (St, Qingdao oil refining) | 13 |
| Hydroxyethyl acrylate (HEA, Ziboxing Lu) | 18 |
| Butyl acrylate (BA, Basff) | 10 |
| Acrylic acid (AA, Wanhua) | 4 |
| Isoborneol methacrylate (IBOMA, Hechuang Chemicals) | 5 |
| Dibenzoyl peroxide (BPO, Aksu) | 3 |
| Propylene glycol butyl ether (Dow chemical) | 10 |
| Dodecyl mercaptan (DDM, Dow chemical) | 2 |
Samples were taken every 5 minutes of dispersion to be fed into the finished tank, and three emulsion samples were taken in total to determine particle size.
Example 1 aqueous Hydroxypropenoic acid Dispersion A particle size of three samples
Example 2
Heating a prepolymer reaction kettle prepolymerization kettle to 72 ℃, adding a mixed solution of propylene glycol butyl ether and a first part of dibenzoyl peroxide (25% of the total BPO amount) for bottoming, opening the prepolymerization kettle for stirring, introducing nitrogen for protection, and heating to a reflux temperature of 148 ℃: preparing monomers according to the proportion in a formula table, uniformly mixing a second part of dibenzoyl peroxide (75 percent of the total amount of BPO) and a chain transfer agent DDM, and adding 8 percent of monomer mixture into a prepolymerization kettle at one time after the temperature is raised to 162 ℃ to serve as reaction seeds; after 70min, the residual monomer mixture is constantly added dropwise, and the dropwise addition is finished within about 5 hours; after the addition, the temperature is kept for 2h, and the light yellow transparent acrylic prepolymer B is obtained. After the temperature is reduced to 120 ℃, the mixture enters a high-speed mixer (the linear speed is 20m/s) together with a neutralizer (N, N-dimethylethanolamine) aqueous solution (containing 15 wt% of process water and at 35 ℃) from a first static mixer at the flow rate of 1KG/min through a mass flow meter and a gear pump, the mixture is neutralized (until the system pH is about 7.5) by the high-speed mixer and then enters a dispersion kettle (the temperature of the dispersion kettle is 80 ℃, the rotating speed is 1500 rpm and the retention time is 15 minutes), a predispersion is formed after the dispersion kettle is mixed and dispersed with 35% of process water and then enters a second static mixer, the predispersion is mixed and dispersed with 50% of process water (at 25 ℃) in the second static mixer to obtain a qualified water dispersion, and then the qualified water dispersion enters a finished product storage tank. Wherein the total addition of the process water is 90 wt% of the discharge amount of the prepolymerization reaction kettle.
Example 2 reaction raw material ratio table:
samples were taken every 5 minutes of dispersion to be fed into the finished tank, and three emulsion samples were taken in total to determine particle size.
TABLE 2 particle size of three samples of aqueous Hydroxyacrylic Dispersion B
Example 3
Heating a prepolymer reaction kettle prepolymerization kettle to 68 ℃, adding a mixed solution of propylene glycol butyl ether and a first part of dibenzoyl peroxide (20% of the total BPO amount) for bottoming, opening the prepolymerization kettle for stirring, introducing nitrogen for protection, and then heating to the reflux temperature of 152 ℃: preparing monomers according to the proportion in a formula table, uniformly mixing a second part of dibenzoyl peroxide (80 percent of the total amount of BPO) and a chain transfer agent DDM, and adding a 12 percent monomer mixture into a prepolymerization kettle at one time after the temperature is raised to 158 ℃ to serve as reaction seeds; after 50min, the residual monomer mixture is constantly added dropwise, and the dropwise addition is finished within about 5 hours; after the addition, the temperature is kept for 1.5h, and then the faint yellow transparent acrylic prepolymer C is obtained. After the temperature is reduced to 120 ℃, the mixture enters a high-speed mixer (the linear speed is 25m/s) together with a neutralizer (N, N-dimethylethanolamine) aqueous solution (containing 10 wt% of process water and 40 ℃) from a first static mixer at the flow rate of 1KG/min through a mass flow meter and a gear pump, the mixture is neutralized (until the system PH is about 7.5) through the high-speed mixer, the mixture enters a dispersion kettle (the temperature of the dispersion kettle is 70 ℃, the rotating speed is 1000 r/min, and the retention time is 15 minutes), a predispersion is formed after the dispersion kettle is mixed and dispersed with 50% of process water and then enters a second static mixer, the predispersion is mixed and dispersed with 40% of process water (23 ℃) in the second static mixer to obtain a qualified water dispersion, and then the qualified water dispersion enters a finished product storage tank. Wherein the total addition of the process water is 110 wt% of the discharge amount of the prepolymerization reaction kettle.
Example 3 reaction raw material ratio table:
| name of raw materials | Mass fraction% |
| Methyl Methacrylate (MMA) | 45 |
| Styrene (St) | 10 |
| Hydroxyethyl acrylate (HEA) | 10 |
| Butyl Acrylate (BA) | 14 |
| Acrylic Acid (AA) | 3 |
| Isoborneol methacrylate (IBOMA) | 5 |
| Dibenzoyl peroxide (BPO) | 2 |
| Propylene |
10 |
| Dodecyl Mercaptan (DDM) | 1 |
Samples were taken every 5 minutes of dispersion to be fed into the finished tank, and three emulsion samples were taken in total to determine particle size.
Particle size of three samples of aqueous Hydroxyacrylic Dispersion C of example 3
The device and the method for continuously producing the hydroxyl acrylic resin aqueous dispersion realize stable and efficient operation, reduce the energy consumption of a device for intermittent production, avoid the volatilization of volatile organic compounds to pollute the atmosphere, and completely meet the requirement of environmental protection.
And (3) comparative analysis:
the following is a comparison of the dispersion viscosities (measured with viscometer DV 2-LV) for the hydroxyacrylic acid continuous process (example 1) and the batch process (i.e.the dispersion is completed by continuous addition of water in the dispersion vessel) of prepolymer A, as follows:
as can be seen from the above table viscosity, the viscosity fluctuation of the prepolymer dispersion system is stable and the dispersion effect is good in the dispersion process of the invention.
The present invention is capable of other embodiments, and various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (12)
1. A system for continuously producing hydroxyl acrylic resin aqueous dispersion is characterized by comprising a prepolymerization reaction kettle, a high-speed mixer, a first static mixer, a second static mixer, a first gear pump, a second gear pump, a dispersion kettle and a finished product storage tank;
wherein the prepolymerization reactor is connected to one inlet of the high-speed mixer through the first gear pump, the first static mixer is used for mixing a neutralizing agent with a first part of process water, an outlet of the first static mixer is connected to the other inlet of the high-speed mixer, and an outlet of the high-speed mixer is connected to a feed inlet of the dispersion tank; the dispersion kettle is used for mixing and dispersing the feed from the high-speed mixer and a second part of process water, and a discharge hole of the dispersion kettle is connected to the second static mixer through a second gear pump; the second static mixer is used for uniformly mixing the feed from the dispersion kettle and a third part of process water and sending a mixed product into the finished product storage tank.
2. The system of claim 1, wherein the prepolymerization reaction vessels are arranged in 1 or more and in parallel.
3. The system of claim 2, wherein the prepolymerization reactors are arranged in 2-4 and are arranged in parallel.
4. The system of any one of claims 1-3, wherein the first gear pump is connected to the high-speed mixer through a first flow meter, and the first static mixer is connected to the high-speed mixer through a second flow meter.
5. The method for continuously producing an aqueous dispersion of a hydroxyacrylic resin using the system according to any one of claims 1 to 4, wherein the object to be subjected to the dispersion treatment to produce the dispersion is an acrylic prepolymer obtained by polymerization in the prepolymerization reaction tank.
6. The process of claim 5, wherein the amount of the first portion of process water entering the first static mixer is from 10 to 20 wt% of the total amount of process water added to the reaction system.
7. The method of claim 6, wherein the second portion of the process water entering the dispersion tank is in an amount of 20% to 50% by weight of the total added amount of process water; the temperature in the dispersion kettle is 70-80 ℃, the retention time is 10-15min, and the dispersion rotation speed is 1000-.
8. The method of claim 7, wherein the process water entering the second static mixer has a water temperature of 10 ℃ to 40 ℃.
9. The method of claim 8, wherein the process water entering the second static mixer has a water temperature of 15 ℃ to 25 ℃.
10. The method of claim 8 or 9, wherein the total amount of process water added is 90-110 wt% of the reactor discharge.
11. The method according to claim 10, wherein the linear velocity of the stirring in the high-speed mixer is 20 to 25m/s, and the neutralizing agent used is N, N-dimethylethanolamine.
12. The method of claim 5 or 11, wherein the reaction raw materials in the prepolymerization reactor comprise: 35-45 wt% of methyl methacrylate, 10-15 wt% of styrene, 10-18 wt% of hydroxyethyl acrylate, 10-15 wt% of butyl acrylate, 3-8 wt% of acrylic acid, 5-8 wt% of isobornyl methacrylate, 2-5 wt% of an initiator, 10-14 wt% of propylene glycol butyl ether and 1-4 wt% of a chain transfer agent based on the total weight of the reaction raw materials;
during the reaction, after the temperature of the prepolymerization reaction kettle is raised to 68-72 ℃, adding the mixed solution of propylene glycol butyl ether and the first part of initiator, starting the prepolymerization reaction kettle for stirring, introducing nitrogen for protection, and then raising the temperature to 148-152 ℃: preparing a monomer mixture according to the proportion of the reaction raw materials, uniformly mixing a second part of initiator and a chain transfer agent, adding 8-12 wt% of the monomer mixture, the uniformly mixed initiator and the chain transfer agent into the prepolymerization reaction kettle at one time after the temperature is raised to 158-162 ℃, reacting for 40-70min, gradually adding the rest monomer mixture, and finishing the addition within 4-6 hours; and preserving the heat for 1-2 hours after the addition is finished to obtain the acrylic prepolymer.
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| CN112500522A (en) * | 2020-11-24 | 2021-03-16 | 商丘市博大化工有限公司 | Aqueous hydroxyl acrylic resin dispersion and preparation method thereof |
| CN112724309B (en) * | 2020-12-21 | 2022-04-26 | 山东友泉新材料有限公司 | Continuous production method of hydroxy acrylic resin aqueous dispersion |
| CN114163563B (en) * | 2022-01-12 | 2023-05-30 | 万华化学集团股份有限公司 | Continuous production process and system of aqueous acrylic resin emulsion |
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| CN107540785B (en) * | 2017-08-25 | 2020-07-31 | 南通博亿化工有限公司 | Hydroxyl acrylic resin aqueous dispersion and preparation method thereof |
| CN108097194B (en) * | 2017-12-28 | 2020-08-28 | 万华化学（宁波）有限公司 | Continuous production system for preparing aqueous polyurethane dispersion, continuous production process for aqueous polyurethane dispersion and application |
| CN109306032A (en) * | 2018-07-13 | 2019-02-05 | 烟台宜彬新材料科技有限公司 | A kind of preparation method of double-component aqueous hydroxy acryl acid dispersion |
| CN109762103A (en) * | 2019-01-22 | 2019-05-17 | 贵州微化科技有限公司 | A kind of micro- reaction method and device continuously preparing low dispersed acrylic resin |
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