CN110950992A - Preparation method and device of styrene-acrylic resin - Google Patents
Preparation method and device of styrene-acrylic resin Download PDFInfo
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- CN110950992A CN110950992A CN201911329451.9A CN201911329451A CN110950992A CN 110950992 A CN110950992 A CN 110950992A CN 201911329451 A CN201911329451 A CN 201911329451A CN 110950992 A CN110950992 A CN 110950992A
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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Abstract
The invention relates to a preparation method of styrene-acrylic resin, which comprises the following steps: firstly, fully and uniformly mixing a styrene monomer, an acrylic monomer, a chain transfer agent and an initiator to obtain a mixed feed liquid; secondly, carrying out oxygen-expelling and temperature-reducing on the mixed feed liquid; thirdly, introducing the mixed feed liquid into an illumination reaction chamber and carrying out light irradiation on the mixed feed liquid to obtain blocky styrene-acrylic resin; and finally, granulating the blocky styrene-acrylic resin to prepare a finished styrene-acrylic resin product. Compared with the raw material prepared by a solvent method, the method for preparing the styrene-acrylic resin by using the irradiation bulk polymerization has the advantages that the problem of solvent residue is solved, the prepared styrene-acrylic resin product is pure, the synthesis process is mild and controllable, the yield is high, and the synthesis process is simple; in addition, the device for preparing the styrene-acrylic resin is characterized in that the material liquid bearing unit is arranged on the belt conveyor, and the conveying structure forms a continuous production mode and reduces the preparation cost of products.
Description
Technical Field
The invention relates to the technical field of preparation of styrene-acrylic resin, in particular to a preparation method and a preparation device of styrene-acrylic resin.
Background
The styrene-acrylic resin is a copolymer of styrene-acrylic acid and esters thereof, and the high polymer can be dissolved or swelled in water or form a highly uniformly dispersed dispersion. Generally, the molecular weight of the polycarbonate resin is low (Mn: 2000 to 9000), the molecular weight distribution is narrow, and the acid value is not less than 200. The styrene-acrylic resin is an important class of water-based high-molecular polymer, has good wear resistance, chemical resistance, weather resistance and mechanical properties under normal conditions, and is widely applied to the fields of printing ink, coating, papermaking sewage treatment, medicine, food, cosmetics and the like at present.
The traditional styrene-acrylic resin mainly adopts liquid products mainly comprising solution polymerization and emulsion polymerization, the solution polymerization is easy to prepare the styrene-acrylic resin with low molecular weight, but a large amount of organic solvents are adopted in the synthesis, the solvents have large odor, are volatile and have high toxicity, the subsequent solvent removal treatment is required, the time and the labor are consumed, and finally obtained resin samples still contain a certain amount of organic volatile components, so that the problems of inconvenience and product quality are caused to downstream application. The molecular weight of the emulsion polymerized product is generally high, and some products are even millions, the prepared resin product is also in a liquid state, and generally can be sold and transported in a solvent-containing mode, and the transportation is very inconvenient, so that the application range of customers is limited, and certain burden is brought to the transportation.
In addition, in recent years, with the national emphasis on environmental protection, the environment is seriously polluted by overhigh VOC emission; therefore, the styrene-acrylic resin gradually develops towards water-based and high-solid content in the application of coating ink and adhesive. How to design a simple and easy preparation method with controllable process and without solvent to synthesize the pure styrene-acrylic resin becomes a main problem at present.
Disclosure of Invention
The invention aims to design a simple and easy process-controllable styrene-acrylic resin synthesized by a process or a device with pure products, and provides a preparation method and a device for synthesizing styrene-acrylic resin by bulk polymerization.
In order to achieve the above object, the present application provides a method for preparing styrene-acrylic resin, comprising the steps of: s1, fully and uniformly mixing a styrene monomer, an acrylic acid monomer, a chain transfer agent and an initiator to obtain a mixed feed liquid; s2, carrying out oxygen removal and temperature reduction on the mixed material liquid in the step S1; s3, introducing the mixed material liquid obtained in the step S2 into an illumination reaction chamber and carrying out light irradiation on the mixed material liquid to obtain blocky styrene-acrylic resin; s4, granulating the blocky styrene-acrylic resin in the step S3 to prepare a finished styrene-acrylic resin product.
As a further improvement of the present application, in step S1, the acrylic monomer is any one or two or more of acrylic acid, methacrylic acid, acrylates or crotonic acid.
As a further improvement of the present application, in step S1, the chain transfer agent is any one or two of alkyl mercaptan and methyl styrene linear dimer; the initiator is one or two of azodiisobutyronitrile and benzoyl peroxide.
As a further improvement of the present application, in step S2, the temperature of the mixed feed liquid is controlled to be less than or equal to 50 ℃.
As a further improvement of the present application, in step S3, the radiation source of the light irradiation is ultraviolet lamp light or pulsed light.
As a further improvement of the present application, in step S3, the light irradiation reaction chamber is an oxygen-free environment; the temperature of the illumination reaction chamber is controlled to be less than or equal to 50 ℃.
As a further improvement of the present application, in step S3, the intensity of the light irradiation is 0.3W/m2～15.0W/m2(ii) a The distance between the irradiation source and the mixed material liquid in the light irradiation is 5-35 cm; the irradiation time in the light irradiation is 5-30 h.
In order to realize the above purpose, the application also provides a preparation styrene-acrylic resin's device, including sealed box, arrange in band conveyer and irradiation unit in the sealed box be equipped with the euphotic layer on the sealed box, make the sealed box keeps oxygen cell and the feed liquid transfer passage of oxygen-free environment be equipped with the feed liquid on the band conveyer and bear the weight of the unit.
As a further development of the application, the feed liquid carrying unit is formed by a container which is arranged on the belt of the belt conveyor and moves continuously with the belt.
As a further improvement of the application, the feed liquid bearing unit is formed by arranging the belt of the belt conveyor into a concave structure for bearing feed liquid.
The method and the device for preparing the styrene-acrylic resin by the radiation bulk polymerization method have the advantages that the problem of solvent residue cannot occur in finished product materials prepared by a solvent method, the prepared styrene-acrylic resin product is pure, the yield is high, the synthesis process is mild and controllable, the synthesis process is simple, and the preparation cost of the product is reduced.
Drawings
FIG. 1 is a flow chart of a process for preparing styrene-acrylic resin;
FIG. 2 is a block diagram of an irradiation device;
in the figure: 1. sealing the box body; 2. a belt conveyor; 3. an irradiation unit; 4. a light transmitting layer; 5. an oxygen scavenging unit; 6. a feed liquid conveying channel; 7. and the feed liquid bearing unit.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described in detail and completely with reference to the following specific embodiments of the present application and the accompanying drawings. It should be understood that the described embodiments are only a few embodiments of the present application, not all embodiments, and are not intended to limit the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The invention aims to find a method and a device for preparing styrene-acrylic resin, which have mild and controllable synthesis process, simple synthesis process and pure product, and provides a preparation method of styrene-acrylic resin, which comprises the following steps: s1, fully and uniformly mixing a styrene monomer, an acrylic acid monomer, a chain transfer agent and an initiator, wherein equipment applied in the process of mixing materials is preferably a mixing tank to obtain mixed material liquid; s2, carrying out oxygen removal and temperature reduction on the mixed material liquid in the step S1, namely: performing oxygen removal engineering on the materials in the mixing tank and simultaneously cooling the material liquid, and further in step S2, controlling the temperature of the mixed material liquid to be less than or equal to 50 ℃ after cooling, and preferably introducing nitrogen into the mixed material liquid for oxygen removal in the process of oxygen removal; s3, introducing the mixed material liquid obtained in the step S2 into an illumination reaction chamber and carrying out light irradiation on the mixed material liquid to obtain blocky styrene-acrylic resin; preferably, the radiation source of the light irradiation is an ultraviolet lamp or pulsed intense light, the inside of the illumination reaction chamber is a sealed oxygen-free environment, wherein the oxygen-free environment is macroscopic oxygen-free, is not absolute, and can be a condition with extremely low oxygen content, and the oxygen-free environment in the illumination reaction chamber is preferably kept by continuously introducing nitrogen into the illumination reaction chamber; further, in step S3, the temperature of the light reaction chamber is controlled to be less than or equal to 50 ℃, the adjustment mode is that nitrogen gas flow is introduced to adjust the temperature in the light reaction chamber during the anaerobic environment treatment of the light reaction chamber, further, nitrogen gas is continuously introduced to the light reaction chamber to realize the anaerobic environment, and then the temperature in the reaction chamber is adjusted by adjusting the flow rate of the nitrogen gas; s4, granulating the blocky styrene-acrylic resin in the step S3 to prepare a finished product of the styrene-acrylic resin.
In the present application, in step S1, the acrylic monomer is acrylic acid, methacrylic acid, acrylate or butyl acrylateAny one or two or more of olefine acids; the chain transfer agent is one or two of alkyl mercaptan, methyl styrene linear dimer (AMSD) and the like; the initiator is one or two of azodiisobutyronitrile, benzoyl peroxide and the like. In the present application, the intensity of the light irradiation is 0.3W/m2～15.0W/m2(ii) a The distance between the irradiation source and the mixed material liquid in the light irradiation is 5-35 cm; further, the distance between the irradiation source and the mixed material liquid in the light irradiation is preferably 5-25 cm; the irradiation time in the light irradiation is 5-30 h.
In order to realize that the pure styrene-acrylic resin of the product is prepared by a mild and controllable synthesis process and a simple synthesis process, the application also provides a device for preparing the styrene-acrylic resin, as shown in fig. 2, the device comprises a sealed box body 1, a belt conveyor 2 and an irradiation unit 3 which are arranged in the sealed box body 1, wherein a euphotic layer 4 is arranged on the sealed box body 1, an oxygen expelling unit 5 and a feed liquid conveying channel 6 which enable the sealed box body 1 to keep an anaerobic environment, and a feed liquid bearing unit 7 is arranged on the belt conveyor 2. In the application, the sealed box body 1 is a sealed box body assembled by plates; the belt conveyor 2 mainly comprises a variable frequency motor with adjustable speed and a belt driven by the variable frequency motor; as a preferred embodiment of the present application, the feed liquid bearing unit 7 is composed of a container which is arranged on the belt and moves along with the belt, and the container can be set into different accommodating shapes; as a preferred embodiment of the present application, the material liquid bearing unit 7 is formed by arranging the belt in a concave structure capable of bearing material liquid, further, the belt may be arranged in a structure having wave-shaped flanges at two sides and a plurality of transverse partition plates in the middle, and the belt, the wave-shaped flanges and the transverse partition plates form a containing cavity for containing material liquid; furthermore, the height of the wavy flanges is set to be suitable for containing feed liquid with a certain height.
In the present application, the structural structure of the feed liquid bearing unit 7 is preferably made of teflon, or a coating layer which is not bonded with the styrene-acrylic resin is arranged on the structural structure of the feed liquid bearing unit 7. In this application, drive the effect of oxygen unit 5 and make keep anaerobic environment in the seal box, it is further, drive the device of oxygen unit 5 for can export nitrogen gas, to continuous letting in nitrogen gas has reached anaerobic environment in the seal box 1. In the application, the light-transmitting layer arranged on the sealed box body 1 is glass or a plastic film, and the light-transmitting layer 4 and the sealed box body 1 form a sealed and air-tight structure to prevent air leakage; further, the glass can be organic glass; further, the plastic film is preferably a plastic film with a light transmittance of 90% or more, the plastic film is preferably PP, PE, PET, PS, or the like, and the film is preferably strong and easy to install and seal the reaction chamber.
In order to verify the beneficial effects of the preparation method and the device for preparing styrene-acrylic resin, the application also provides some preferred embodiments, which are proved by the following, wherein the specific embodiments are as follows:
example 1
Firstly, 100 parts by mass of styrene, 23 parts by mass of acrylic acid, 2 parts by mass of ethyl acrylate, 0.25 part by mass of AMSD and 0.3 part by mass of benzoyl peroxide are dissolved and fully and uniformly mixed to obtain mixed feed liquid; secondly, introducing nitrogen into the mixed feed liquid and cooling, wherein the time for introducing nitrogen and removing oxygen is more than 25min, and the temperature of the mixed feed liquid is controlled at 30 ℃ after cooling; meanwhile, filling nitrogen into the illumination reaction chamber to drive oxygen, and controlling the temperature at 30 ℃; thirdly, introducing the mixed feed liquid subjected to oxygen removal and temperature reduction into an illumination reaction chamber, applying ultraviolet light for irradiation, and continuously adjusting the flow of nitrogen introduced into the illumination reaction chamber to ensure that the temperature of the mixed feed liquid is constant at 30 ℃, wherein the irradiation time is 14 hours, so that the blocky styrene-acrylic resin is obtained; and finally, crushing and screening the blocky styrene-acrylic resin to prepare a finished styrene-acrylic resin product. The detection shows that the finished product does not contain organic solvent, the yield is high, and the residual quantity of the monomer is small.
Example 2
Firstly, fully dissolving 100 parts by mass of styrene, 25 parts by mass of acrylic acid, 1 part by mass of butyl acrylate, 2 parts by mass of methyl acrylate, 0.5 part by mass of AMSD and 0.02 part by mass of azobisisobutyronitrile, and uniformly mixing to obtain a mixed feed liquid; secondly, introducing nitrogen into the mixed feed liquid and cooling, wherein the time for introducing the nitrogen and removing oxygen is more than 20min, and the temperature of the mixed feed liquid is controlled to be 35 ℃ after cooling; meanwhile, filling nitrogen into the illumination reaction chamber to drive oxygen, and controlling the temperature to be 35 ℃; thirdly, introducing the mixed feed liquid after oxygen removal and temperature reduction into an illumination reaction chamber, and irradiating by using strong pulse light for 12 hours to obtain blocky styrene-acrylic resin; and finally, crushing and screening the blocky styrene-acrylic resin to prepare a finished styrene-acrylic resin product. The detection shows that the finished product does not contain organic solvent, the yield is high, and the residual quantity of the monomer is small.
In conclusion, compared with the raw material prepared by the solvent method, the method for preparing the styrene-acrylic resin by the irradiation method does not have the problem of solvent residue, the prepared styrene-acrylic resin product is pure, the yield is high, the synthesis process is mild and controllable, the synthesis process is simple, and the preparation cost of the product is reduced. The device is designed aiming at the method for preparing the styrene-acrylic resin by the irradiation method, the device can realize continuous production for preparing the styrene-acrylic resin by the irradiation method, and can prepare blocky materials with different shapes by designing different material liquid bearing structures so as to meet the subsequent application of different products.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the styrene-acrylic resin is characterized by comprising the following steps:
s1, fully and uniformly mixing a styrene monomer, an acrylic acid monomer, a chain transfer agent and an initiator to obtain a mixed feed liquid;
s2, carrying out oxygen removal and temperature reduction on the mixed material liquid in the step S1;
s3, introducing the mixed material liquid obtained in the step S2 into an illumination reaction chamber and carrying out light irradiation on the mixed material liquid to obtain blocky styrene-acrylic resin;
s4, granulating the blocky styrene-acrylic resin in the step S3 to prepare a finished styrene-acrylic resin product.
2. The method of claim 1, wherein in step S1, the acrylic monomer is any one or two or more of acrylic acid, methacrylic acid, acrylates, and crotonic acid.
3. The method of preparing a styrene-acrylic resin according to claim 1, wherein in step S1, the chain transfer agent is any one or two of alkyl mercaptan and linear methyl styrene dimer; the initiator is one or two of azodiisobutyronitrile and benzoyl peroxide.
4. The method according to claim 1, wherein in step S2, the temperature of the mixed liquor is controlled to be less than or equal to 50 ℃ after the temperature is reduced.
5. The method of preparing styrene-acrylic resin according to claim 1, wherein the irradiation source of light is an ultraviolet lamp or a pulsed strong light at step S3.
6. The method of preparing styrene-acrylic resin according to claim 1, wherein the light irradiation reaction chamber is an oxygen-free environment in step S3; the temperature of the illumination reaction chamber is controlled to be less than or equal to 50 ℃.
7. The method of preparing styrene-acrylic resin according to claim 1, wherein the intensity of said light irradiation is 0.3W/m in step S32～15.0W/m2(ii) a The distance between the irradiation source and the mixed material liquid in the light irradiation is 5-35 cm; the irradiation time in the light irradiation is 5-30 h.
8. The device for preparing the styrene-acrylic resin is applied to any one of claims 1 to 7, and is characterized by comprising a sealed box body (1), a belt conveyor (2) and an irradiation unit (3) which are arranged in the sealed box body (1), wherein a light transmission layer (4), an oxygen driving unit (5) and a feed liquid conveying channel (6) which enable the sealed box body (1) to maintain an oxygen-free environment are arranged on the sealed box body (1), and a feed liquid bearing unit (7) is arranged on the belt conveyor (2).
9. The apparatus for preparing styrene-acrylic resin according to claim 8, wherein said feed liquid bearing unit (7) is constituted by a container provided on a belt of said belt conveyor and continuously moving with said belt.
10. The apparatus for preparing styrene-acrylic resin according to claim 8, wherein said feed liquid bearing unit (7) is formed by arranging a belt of said belt conveyor in a concave structure for receiving feed liquid.
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| CN201911329451.9A CN110950992A (en) | 2019-12-20 | 2019-12-20 | Preparation method and device of styrene-acrylic resin |
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| CN201911329451.9A CN110950992A (en) | 2019-12-20 | 2019-12-20 | Preparation method and device of styrene-acrylic resin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202643607U (en) * | 2012-06-12 | 2013-01-02 | 东营市华兴化工有限责任公司 | Photo-initiation device for polyacrylamide production |
| CN106232505A (en) * | 2014-04-25 | 2016-12-14 | 松原产业株式会社 | Water-absorbing polymeric particles is polymerized the longitudinal shape of ribbon in producing |
| CN106478862A (en) * | 2016-10-24 | 2017-03-08 | 中科院合肥技术创新工程院 | The quick Actinochemical synthesis of polymer and the reaction unit for the method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202643607U (en) * | 2012-06-12 | 2013-01-02 | 东营市华兴化工有限责任公司 | Photo-initiation device for polyacrylamide production |
| CN106232505A (en) * | 2014-04-25 | 2016-12-14 | 松原产业株式会社 | Water-absorbing polymeric particles is polymerized the longitudinal shape of ribbon in producing |
| CN106478862A (en) * | 2016-10-24 | 2017-03-08 | 中科院合肥技术创新工程院 | The quick Actinochemical synthesis of polymer and the reaction unit for the method |
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Application publication date: 20200403 |