CN112592267A - Environment-friendly zinc acrylate/zinc methacrylate synthesis process and device - Google Patents
Environment-friendly zinc acrylate/zinc methacrylate synthesis process and device Download PDFInfo
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- CN112592267A CN112592267A CN202011359735.5A CN202011359735A CN112592267A CN 112592267 A CN112592267 A CN 112592267A CN 202011359735 A CN202011359735 A CN 202011359735A CN 112592267 A CN112592267 A CN 112592267A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/72—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with helices or sections of helices
- B01F27/721—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with helices or sections of helices with two or more helices in the same receptacle
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/72—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with helices or sections of helices
- B01F27/726—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with helices or sections of helices with two helices with opposite pitch on the same shaft; with two helices on the same axis, driven in opposite directions or at different speeds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/181—Preventing generation of dust or dirt; Sieves; Filters
- B01F35/189—Venting, degassing or ventilating of gases, fumes or toxic vapours during mixing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
Abstract
The invention relates to an environment-friendly zinc acrylate/zinc methacrylate synthesis process, which comprises the following steps: the method comprises the following steps: adding acrylic acid/methacrylic acid into a reaction container, heating and stirring; step two: when the temperature is raised to 40-80 ℃, zinc oxide is slowly added while stirring; step three: adding the initiator for multiple times when the reaction is in an agglomerated state; step four: after the initiator is added, stirring and controlling the reaction temperature to be between 60 and 120 ℃, and reacting for 40 to 80 minutes to obtain zinc acrylate/zinc methacrylate; step five: vacuumizing until the water content of zinc acrylate/zinc methacrylate is less than or equal to 0.5%; step six: crushing to obtain zinc acrylate/zinc methacrylate powder. The method has the advantages of no need of saponification and double decomposition reaction, no wastewater generation, low energy consumption and high product purity.
Description
Technical Field
The invention belongs to the organic compound synthesis technology, and particularly relates to an environment-friendly zinc acrylate/zinc methacrylate synthesis process and device.
Background
Zinc acrylate and zinc methacrylate are multifunctional active assistant with wide application foreground in rubber industry, and the double bond and ionic bond in the structure makes the multifunctional active assistant possess excellent compatibility with polar rubber, so that it may be used as peroxide bridging assistant to raise crosslinking density, raise vulcanizing speed, shorten vulcanizing time and raise metal adhesion. The synthesis process of zinc acrylate and zinc methacrylate has few reports in literature, and as a conventional synthesis process of zinc acrylate and zinc methacrylate, zinc acrylate and zinc methacrylate are usually produced in a water phase by a saponification method, acrylic acid or methacrylic acid is slowly added into a hot water solution of sodium hydroxide or potassium hydroxide, and is subjected to sufficient saponification, cooling and precipitation, and then dehydration to obtain products with different water contents.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an environment-friendly zinc acrylate/zinc methacrylate synthesis process, which comprises the following steps:
the method comprises the following steps: adding acrylic acid/methacrylic acid into a reaction container, heating and stirring;
step two: when the temperature is raised to 40-80 ℃, zinc oxide is slowly added while stirring;
step three: adding the initiator for multiple times when the reaction is in an agglomerated state;
step four: after the initiator is added, stirring and controlling the reaction temperature to be between 60 and 120 ℃, and reacting for 40 to 80 minutes to obtain zinc acrylate/zinc methacrylate;
step five: vacuumizing until the water content of zinc acrylate/zinc methacrylate is less than or equal to 0.5%;
step six: crushing to obtain zinc acrylate/zinc methacrylate powder.
Preferably, the acrylic acid/methacrylic acid and zinc oxide molar ratio is 2: 1.
Preferably, the initiator in the third step is distilled water or hydrogen peroxide.
Preferably, the initiator is used in an amount of 3% to 15% by weight of acrylic acid/methacrylic acid.
Preferably, the initiator is added in 4-7 times in step three.
In addition, the invention also provides a device for the environment-friendly zinc acrylate/zinc methacrylate synthesis process, which comprises a reaction vessel, wherein a feeding port, a gas inlet and a gas outlet and a thermometer are arranged above the reaction vessel, a discharging port is arranged below the reaction vessel, a stirring device is arranged in the reaction vessel, the stirrer is connected with a driving device, the reaction vessel is connected with a heating device, the stirring device comprises two stirring paddles, and the two stirring paddles rotate reversely.
Preferably, the driving device comprises a motor, the motor is connected with a speed reducer through a transmission device, the speed reducer is connected with a gear transmission, and the two stirring paddles are connected with the gear transmission.
Preferably, a jacket is arranged outside the reaction vessel, a steam inlet and a steam outlet are arranged on the jacket, the steam inlet is connected with the heating device through a pipeline, the steam outlet is connected with a condenser through a pipeline, and the condenser is connected with the heating device.
The reaction process of the acrylic acid and the zinc oxide and the structural formula of the obtained product are as follows:
the structural formula of the reaction process of methacrylic acid and zinc oxide and the obtained product is as follows:
the method has the advantages of no need of saponification and double decomposition reaction, no wastewater generation, low energy consumption and high product purity. Acrylic acid/methacrylic acid and zinc oxide adopt double stirrers and double-slurry reverse shearing rotation under the initiation of distilled water or hydrogen peroxide, the structure is simple, the reaction materials are uniformly stirred and fully reacted, the distilled water or hydrogen peroxide added after the reaction and the water generated in the reaction are discharged in a steam mode, the surface attached water can reach the drying requirement through vacuumizing or natural evaporation, and then the product is obtained by directly crushing, the green and environment-friendly production process is truly embodied, and the high-quality product with high production efficiency, less energy consumption and no wastewater is produced is obtained.
Drawings
FIG. 1 is a front view of an apparatus for synthesizing zinc acrylate/methacrylate;
FIG. 2 is a top view of the apparatus for synthesizing zinc acrylate/zinc methacrylate.
In the figure: 1-a reaction vessel; 2-a feed inlet; 3-discharging port; 4-jacket; 5-gas inlet and outlet; 6-steam inlet; 7-a thermometer; 8-a steam outlet; 9-stirring paddle; 10-a motor; 11-a transmission; 12-a speed reducer; 13-a gear transmission; 14-a heating device; 15-a condenser.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to these examples.
The utility model provides a device of environment-friendly zinc acrylate/zinc methacrylate synthesis technology, including reaction vessel 1, reaction vessel 1's top is equipped with charge door 2, gas exit 5 and thermometer 7, the below of reaction vessel 1 is equipped with discharge gate 3, be equipped with agitating unit in the reaction vessel 1, agitating unit includes two stirring rake 9, two stirring rake 9 are the antiport, agitating unit is connected with drive arrangement, drive arrangement includes motor 10, motor 10 is connected with speed reducer 12 through transmission 11, transmission 11 is belt drive or gear drive etc. commonly used, speed reducer 12 is connected with gear transmission 13, two stirring rake 9 are connected with gear transmission 13.
The reaction vessel 1 is externally provided with a jacket 4, the jacket 4 is provided with a steam inlet 6 and a steam outlet 8, the steam inlet 6 is connected with a heating device 14 through a pipeline, the steam outlet 8 is connected with a condenser 15 through a pipeline, and the condenser 15 is connected with the heating device 14.
Example 1
An environment-friendly zinc acrylate/zinc methacrylate synthesis process is synthesized according to the following process that 36kg of acrylic acid is added into a reaction vessel 1 through a feed inlet 2, a heating device 15 is started, steam enters a jacket 4 from a steam inlet 6 through a pipeline, a motor 10 and a speed reducing motor 11 are started, and a stirring paddle 9 works; when the temperature is raised to 80 ℃, slowly adding zinc oxide from the feed inlet 2 while stirring, wherein the adding amount of the zinc oxide is 20.25 kg; when the reaction is aggregated, adding distilled water from the feed inlet 2 for 5 times, wherein the adding amount is 0.72kg each time, and the time interval between adding distilled water for each time is 10 minutes; after the distilled water is added, while stirring, controlling the reaction temperature between 80 ℃ and 90 ℃, reacting for 80min to obtain zinc acrylate, vacuumizing from a gas inlet and outlet 5 until the water content of the zinc acrylate is less than or equal to 0.5%, and discharging the zinc acrylate from a discharge port 3; crushing to obtain zinc acrylate powder.
Example 2
An environment-friendly zinc acrylate/zinc methacrylate synthesis process is synthesized according to the following process that 72kg of acrylic acid is added into a reaction vessel 1 through a feed inlet 2, a heating device 15 is started, steam enters a jacket 4 from a steam inlet 6 through a pipeline, a motor 10 and a speed reducing motor 11 are started, and a stirring paddle 9 works; when the temperature is raised to 80 ℃, slowly adding zinc oxide from the feed inlet 2 while stirring, wherein the adding amount of the zinc oxide is 40.5 kg; when the reaction is aggregated, adding distilled water from a feed inlet for 7 times, wherein the adding amount is 1.5kg each time, and the time interval between adding distilled water for each time is 10 minutes; after the distilled water is added, while stirring, controlling the reaction temperature between 90 ℃ and 100 ℃, reacting for 60min to obtain zinc acrylate, vacuumizing from a gas inlet and outlet 5 until the water content of the zinc acrylate is less than or equal to 0.5%, and discharging the zinc acrylate from a discharge port 3; crushing to obtain zinc acrylate powder.
Example 3
An environment-friendly zinc acrylate/zinc methacrylate synthesis process is synthesized according to the following process that 36kg of acrylic acid is added into a reaction vessel 1 through a feed inlet 2, a heating device 15 is started, steam enters a jacket 4 from a steam inlet 6 through a pipeline, a motor 10 and a speed reducing motor 11 are started, and a stirring paddle 9 works; when the temperature is raised to 80 ℃, slowly adding zinc oxide from the feed inlet 2 while stirring, wherein the adding amount of the zinc oxide is 20.25 kg; when the reaction is in an agglomerated state, adding hydrogen peroxide from the feeding port 2 for 4 times, wherein the adding amount is 0.25kg each time, and the interval time of adding hydrogen peroxide for each time is 15 minutes; after adding hydrogen peroxide, stirring, controlling the reaction temperature to be between 100 and 120 ℃, reacting for 40min to obtain zinc acrylate, vacuumizing from a gas inlet and outlet 5 until the water content of the zinc acrylate is less than or equal to 0.5%, and discharging the zinc acrylate from a discharge port 3; crushing to obtain zinc acrylate powder.
Examples 1 to 3 are the synthesis of zinc acrylate, the physicochemical properties of the synthesized acrylic acid are shown in Table 1, and the detection conditions are as follows: the temperature was 25 ℃ and the humidity was 52%.
TABLE 1 physicochemical Properties of acrylic acid synthesized in examples 1-3
| Acid value (mgKOH/g) | Purity (%) | Relative density | |
| Example 1 | 3.7 | 99.2 | 0.34 |
| Example 2 | 3.2 | 99.4 | 0.32 |
| Example 3 | 4.1 | 99.1 | 0.36 |
Example 4
An environment-friendly zinc acrylate/zinc methacrylate synthesis process comprises the following steps of adding 86kg of methacrylic acid into a reaction vessel through a feed inlet 2, starting a heating device 15, introducing steam into a jacket 4 from a steam inlet 6 through a pipeline, starting a motor 10, a reducing motor 11 and a stirring paddle 9 to work; when the temperature is raised to 40 ℃, slowly adding 40.5kg of zinc oxide from the feed inlet 2 while stirring; when the reaction is in an agglomerated state, adding hydrogen peroxide from the feeding port 2 for 5 times, wherein 1.8kg of hydrogen peroxide is added for the first 2 times, 0.78kg of hydrogen peroxide is added for the second 4 times, and the interval time of adding hydrogen peroxide for each time is 10 minutes; after the hydrogen peroxide is added, stirring and controlling the reaction temperature to be between 60 and 70 ℃, and reacting for 80min to obtain zinc methacrylate; vacuumizing from a gas inlet and a gas outlet 5 until the water content of zinc methacrylate is less than or equal to 0.5%; discharging zinc methacrylate from a discharge port 3; and crushing to obtain zinc methacrylate powder.
Example 5
An environment-friendly zinc acrylate/zinc methacrylate synthesis process comprises the following steps of adding 4.3kg of methacrylic acid into a reaction vessel through a charging hole 2, starting a heating device 15, introducing steam into a jacket 4 from a steam inlet 6 through a pipeline, starting a motor 10, a reducing motor 11 and a stirring paddle 9 to work; when the temperature is raised to 40 ℃, 2.025kg of zinc oxide is slowly added from the feed inlet 2 while stirring; when the reaction is agglomerated, adding distilled water from the feed inlet 2 for 4 times, and averagely adding 0.043kg each time; the interval time of adding distilled water is 15 minutes each time, after the distilled water is added, the reaction temperature is controlled between 65 ℃ and 75 ℃ while stirring, and the reaction is carried out for 40min, so as to obtain zinc methacrylate; obtaining zinc methacrylate; vacuumizing from a gas inlet and a gas outlet 5 until the water content of zinc methacrylate is less than or equal to 0.5%; discharging zinc methacrylate from a discharge port 3; and crushing to obtain zinc methacrylate powder.
Example 6
An environment-friendly zinc acrylate/zinc methacrylate synthesis process is synthesized according to the following process that 150kg of methacrylic acid is added into a reaction vessel through a feed inlet 2, a heating device 15 is started, steam enters a jacket 4 from a steam inlet 6 through a pipeline, a motor 10 and a reducing motor 11 are started, and a stirring paddle 9 works; when the temperature is raised to 40 ℃, slowly adding 70.64kg of zinc oxide while stirring; when the reaction is in an agglomerated state, adding hydrogen peroxide from the feeding port 2 for 6 times, wherein 3kg of hydrogen peroxide is added for the first 3 times, and 1kg of hydrogen peroxide is added for the last 3 times; the interval time of adding hydrogen peroxide is 10 minutes each time, and after the hydrogen peroxide is added, the reaction temperature is controlled between 70 ℃ and 80 ℃ while stirring, and the reaction is carried out for 60 minutes to obtain zinc methacrylate; vacuumizing from a gas inlet and a gas outlet 5 until the water content of zinc methacrylate is less than or equal to 0.5%; discharging zinc methacrylate from a discharge port 3; and crushing to obtain zinc methacrylate powder.
Examples 4 to 6 are the synthesis of zinc methacrylate, the physicochemical properties of the synthesized methacrylic acid are shown in Table 2, and the detection conditions are as follows: the temperature was 25 ℃ and the humidity was 52%.
TABLE 2 physicochemical Properties of methacrylic acid synthesized in examples 4 to 6
| Acid value (mgKOH/g) | Purity (%) | Relative density | |
| Example 4 | 6.9 | 99.5 | 0.33 |
| Example 5 | 7.3 | 99.0 | 0.31 |
| Example 6 | 7.1 | 99.2 | 0.31 |
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (8)
1. An environment-friendly zinc acrylate/zinc methacrylate synthesis process is characterized by comprising the following steps:
the method comprises the following steps: adding acrylic acid/methacrylic acid into a reaction container, heating and stirring;
step two: when the temperature is raised to 40-80 ℃, zinc oxide is slowly added while stirring;
step three: adding the initiator for multiple times when the reaction is in an agglomerated state;
step four: after the initiator is added, stirring and controlling the reaction temperature to be between 60 and 120 ℃, and reacting for 40 to 80 minutes to obtain zinc acrylate/zinc methacrylate;
step five: vacuumizing until the water content of zinc acrylate/zinc methacrylate is less than or equal to 0.5%;
step six: crushing to obtain zinc acrylate/zinc methacrylate powder.
2. The process of claim 1, wherein the molar ratio of acrylic acid/methacrylic acid to zinc oxide is 2: 1.
3. The process of claim 2, wherein the initiator in step three is distilled water or hydrogen peroxide.
4. The process of claim 3, wherein the amount of the initiator is 3-15% by weight of acrylic acid/methacrylic acid.
5. The process of claim 4, wherein the initiator is added in 4-7 times.
6. The device for the environment-friendly zinc acrylate/zinc methacrylate synthesis process as claimed in claim 1, comprises a reaction vessel, wherein a charging port, a gas inlet and outlet and a thermometer are arranged above the reaction vessel, a discharging port is arranged below the reaction vessel, a stirring device is arranged in the reaction vessel, the stirrer is connected with a driving device, the reaction vessel is connected with a heating device, and the device is characterized in that the stirring device comprises two stirring paddles, and the two stirring paddles rotate reversely.
7. The environment-friendly zinc acrylate/zinc methacrylate synthesis process device according to claim 6, wherein the driving device comprises a motor, the motor is connected with a speed reducer through a transmission device, the speed reducer is connected with a gear transmission, and the two stirring paddles are connected with the gear transmission.
8. The environment-friendly zinc acrylate/zinc methacrylate synthesis process device according to claim 7, wherein a jacket is arranged outside the reaction vessel, a steam inlet and a steam outlet are arranged on the jacket, the steam inlet is connected with a heating device through a pipeline, the steam outlet is connected with a condenser through a pipeline, and the condenser is connected with the heating device.
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| CN202011359735.5A CN112592267A (en) | 2020-11-27 | 2020-11-27 | Environment-friendly zinc acrylate/zinc methacrylate synthesis process and device |
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| CN202011359735.5A CN112592267A (en) | 2020-11-27 | 2020-11-27 | Environment-friendly zinc acrylate/zinc methacrylate synthesis process and device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979857A (en) * | 2021-11-30 | 2022-01-28 | 青岛益林原科贸有限公司 | Method for producing zinc acrylate at low temperature |
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| JP2008044207A (en) * | 2006-08-14 | 2008-02-28 | Kureha Corp | Gas-barrier rubbery molding and its manufacturing process |
| CN201470389U (en) * | 2009-07-17 | 2010-05-19 | 湖州市菱湖新望化学有限公司 | Reaction device for producing stearate by dry method |
| CN102351683A (en) * | 2011-10-26 | 2012-02-15 | 山东阳谷华泰化工股份有限公司 | Production process of zinc acrylate |
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2020
- 2020-11-27 CN CN202011359735.5A patent/CN112592267A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008044207A (en) * | 2006-08-14 | 2008-02-28 | Kureha Corp | Gas-barrier rubbery molding and its manufacturing process |
| CN201470389U (en) * | 2009-07-17 | 2010-05-19 | 湖州市菱湖新望化学有限公司 | Reaction device for producing stearate by dry method |
| CN102351683A (en) * | 2011-10-26 | 2012-02-15 | 山东阳谷华泰化工股份有限公司 | Production process of zinc acrylate |
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| YU ZHANG ET AL: "Highly transparent bulk PMMA/ZnO nanocomposites with bright visible luminescence and efficient UV-shielding capability", 《JOURNAL OF MATERIALS CHEMISTRY》, vol. 22, 3 April 2012 (2012-04-03), pages 11972 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113979857A (en) * | 2021-11-30 | 2022-01-28 | 青岛益林原科贸有限公司 | Method for producing zinc acrylate at low temperature |
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Application publication date: 20210402 |