CN113861331B - Weather-resistant resin and preparation process and preparation equipment thereof - Google Patents
Weather-resistant resin and preparation process and preparation equipment thereof Download PDFInfo
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- CN113861331B CN113861331B CN202111132355.2A CN202111132355A CN113861331B CN 113861331 B CN113861331 B CN 113861331B CN 202111132355 A CN202111132355 A CN 202111132355A CN 113861331 B CN113861331 B CN 113861331B
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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
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/085—Feeding reactive fluids
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The application relates to the field of resin synthesis, and particularly discloses a weather-resistant resin, and a preparation process and preparation equipment thereof. The weather-resistant resin is prepared by mixing and reacting the following raw materials in parts by weight: 650 parts of toluene, 150 parts of butyl acetate, 450 parts of methyl acrylate, 470 parts of butyl acrylate, 230 parts of butyl acrylate, 160 parts of hydroxypropyl acrylate, 3-7 parts of acrylic acid and 10-14 parts of benzoyl peroxide. The preparation method comprises the following steps: s1, putting part of toluene and part of butyl acetate into a reaction container, mixing, and heating to 105-115 ℃; s2, mixing all methyl acrylate, butyl acrylate, hydroxypropyl acrylate, acrylic acid and part of benzoyl peroxide into a first mixed component, dropwise adding into a reaction container, and reacting for 2-3h after dropwise adding is completed; s3, mixing the residual toluene, butyl acetate and benzoyl peroxide in the total raw materials, dropwise adding into a reaction container, heating to 120-140 ℃ after dropwise adding, and carrying out heat preservation and reflux for 2-3 h. The weather-resistant resin prepared by the method has good basic performance and is low in cost.
Description
Technical Field
The invention relates to the field of resin synthesis, in particular to a preparation process of weather-resistant resin, weather-resistant resin and preparation equipment.
Background
The resin is a multipurpose synthetic material, is often used as a basic material in the field of coatings and paints, and has great influence on the effect of the coatings in the field of automobile surface coatings on the basic properties of the resin, such as hardness, glossiness, drying time and the like.
The commercially available AP-5073 type resin belongs to solvent hydroxyl polyol acrylic resin, has good basic performance, high gloss, extremely fast drying property, extremely high hardness and excellent comprehensive performance, is suitable for being used as automobile finish paint, refinishing paint and finishing varnish, but has higher cost.
With respect to the related art among the above, the inventors consider that the above-mentioned resin has good basic properties, but the cost and selling price thereof are high.
Disclosure of Invention
In order to reduce the cost while ensuring excellent basic performance, the application provides a preparation process of weather-resistant resin and the weather-resistant resin.
In a first aspect, the present application provides a weatherable resin, which adopts the following technical scheme:
the weather-resistant resin is prepared by mixing and reacting the following raw materials in parts by weight: 650 parts of toluene 610-.
By adopting the technical scheme, the raw material components and the content of the resin are tested to obtain the resin formed by the components with the content, the adopted raw materials are common raw materials, the cost is lower, the price is lower than that of AP-5073 resin, meanwhile, the acrylic resin has excellent light resistance and weather resistance, and the resin has excellent comprehensive properties such as glossiness, hardness, drying speed and the like.
Preferably, the composite nano particle also comprises 20 to 80 parts by weight of composite nano particles.
By adopting the technical scheme, the composite nanoparticles are added into the resin as the filler, so that the performance of the resin can be obviously improved, and the defects of the resin in the aspects of heat resistance and the like are overcome.
Preferably, the composite nanoparticles are nano calcium carbonate and nano silicon dioxide in a mass ratio of 2-3: 1.
By adopting the technical scheme, the nano calcium carbonate has good modification on the gloss, water resistance and other directions of the resin for the paint, the nano silicon dioxide has good effects on the adhesion force and other aspects of the resin, the matching of the nano calcium carbonate and the nano silicon dioxide has good targeted performance improvement on the performance of the resin for the vehicle surface paint, and meanwhile, the nano calcium carbonate is low in price and low in cost.
In a second aspect, the application provides a preparation method of the weather-resistant resin, which adopts the following technical scheme:
a preparation process of weather-resistant resin comprises the following steps:
s1, putting 560-580 parts by weight of toluene and 135-155 parts by weight of butyl acetate in the total raw materials into a reaction container, starting stirring, mixing and heating to 105-115 ℃;
s2, mixing methyl acrylate, butyl acrylate, hydroxypropyl acrylate, acrylic acid and 6-9 parts by weight of benzoyl peroxide in the total raw materials into a first mixed component, dropwise adding the first mixed component into a reaction container while stirring, and reacting for 2-3 hours after dropwise adding;
s3, mixing the residual toluene, butyl acetate and benzoyl peroxide in the total raw materials into a second mixed component, dropwise adding into the reaction container, stirring while dropwise adding, heating to 120-140 ℃, and carrying out heat preservation and reflux for 2-3 h.
By adopting the technical scheme, the raw materials are reasonably distributed in the preparation process, fed in batches, mixed in a uniform-speed dropwise manner, so that the reaction effect can be improved, the content and the synthesis effect of the synthetic resin are improved, the resin with proper molecular weight and uniform performance is obtained, and the basic performance of the resin is improved.
Preferably, the dropping rate in the step S2 is 78-82 g/S.
By adopting the technical scheme, the speed of the synthesis reaction is controlled by controlling the dripping speed of the raw material monomer, so that the reaction effect is controlled, the raw material of the resin is gradually dripped in the process of stirring, and the obtained resin product is uniform and consistent.
Preferably, in the step S3, the second mixed component is added dropwise 3 times, each time, one third of the total weight of the second mixed component is added dropwise, the adding speed is 75-100g/S, and after the adding, the temperature is kept for 45-60min, and the steps are repeated for 3 times.
By adopting the technical scheme, the average molecular weight of the obtained resin can be controlled by controlling the addition of the second mixed component and limiting the time of the heat preservation reaction, so that resin molecules with proper size can be obtained, and the quality of the resin can be controlled.
Preferably, after the step S3 is completed, the material is cooled to 20 to 35 ℃, and then filtered to obtain the product.
Through adopting above-mentioned technical scheme, the material that will react and accomplish is cooled down the back and is filtered, can realize good cooperation effect, improves the cooling.
Preferably, the method also comprises 20-80 parts of composite nanoparticles, the composite nanoparticles are added after the step of S1, and the stirring in the reaction vessel is started.
By adopting the technical scheme, the composite nanoparticles are added at the beginning of the reaction, so that the nanoparticles and the raw materials are uniformly mixed, the dispersion effect is good, the combination effect with the resin is good, and the basic performance of the resin can be improved.
In a third aspect, the present application provides a device for preparing a weather-resistant resin, which adopts the following technical scheme:
the utility model provides a preparation equipment of resistant resin of waiting, includes the cauldron body, be equipped with the hourglass jar on the cauldron body, be equipped with the connecting pipe jointly between hourglass jar and the cauldron body, be equipped with the flow valve on the connecting pipe, the internal agitating unit that is equipped with of cauldron, wear to be equipped with the solid inlet pipe on the cauldron body, the cauldron body is close to solid inlet pipe below and rotates and be connected with the revolving fragment, the revolving fragment is located solid inlet pipe below, the revolving fragment is by being close to the position slope of the position under the solid inlet pipe to orientation solid inlet pipe one side and setting up downwards, the revolving fragment is rotatory around the perpendicular to revolving fragment and the perpendicular line that passes the revolving fragment center.
Through adopting above-mentioned technical scheme, at the internal raw materials of putting into of cauldron, mix through agitating unit, put into the material that mixes in the hourglass jar, through the connecting pipe and the flow valve control hourglass speed on it, control monomer dropwise add speed to control reaction effect. The composite nano particle filler is fed through the solid feeding pipe, when the material falls down, the rotating sheet flies the material over against the material, and the material can gradually fall after flying, so that solid powder is reduced to be agglomerated in resin, the dispersion uniformity is improved, and the resin performance is improved.
In summary, the present application has the following beneficial effects:
1. the raw material components and the content of the resin are tested to obtain the resin consisting of the components in the content, the adopted raw materials are common raw materials, the cost is lower, the price is lower than that of AP-5073 resin, meanwhile, the acrylic resin has excellent light resistance and weather resistance, and the resin has excellent comprehensive properties such as glossiness, hardness, drying speed and the like.
2. Through with raw materials rational distribution, carry out the fed-batch with the raw materials among this application preparation technology to through mixing the component, then at the uniform velocity dropwise add mode feeding, can improve the reaction effect, thereby improve synthetic resin's content and synthetic effect, obtain suitable molecular weight and the even unanimous resin of performance, thereby realize improving the basic performance of resin.
3. The preparation equipment controls the dripping speed through the connecting pipe and the flow valve on the connecting pipe, and controls the monomer dripping speed, so that the reaction effect is controlled. The composite nano particle filler is fed through the solid feeding pipe, when the material falls down, the rotating sheet flies the material over against the material, and the material can gradually fall after flying, so that solid powder is reduced to be agglomerated in resin, the dispersion uniformity is improved, and the resin performance is improved.
Drawings
FIG. 1 is a sectional view of an apparatus for preparing a weather-resistant resin according to the present application.
1. A kettle body; 11. a stirring device; 12. a solids feed tube; 13. a rotating sheet; 131. a rotating electric machine; 2. a drip tank; 21. a connecting pipe; 22. a flow valve.
Detailed Description
The present application will be described in further detail with reference to the drawings and examples.
The application discloses preparation equipment of resistant resin of waiting.
Referring to fig. 1, the equipment for preparing the weather-resistant resin comprises a kettle body, wherein a dripping tank is arranged on the kettle body, a connecting pipe is fixedly arranged between the dripping tank and the kettle body and communicated with the dripping tank and the kettle body, and a flow valve is fixedly arranged on the connecting pipe. The kettle body is internally provided with a stirring device. Wear to be equipped with the solid inlet pipe on the cauldron body, the cauldron body is close to solid inlet pipe below and rotates and be connected with the revolving fragment, and the revolving fragment is located solid inlet pipe below, and the revolving fragment is by being close to the position under the solid inlet pipe to the position slope of towards solid inlet pipe one side and set up downwards, and the revolving fragment is rotatory around the perpendicular line that perpendicular to revolving fragment and pass the revolving fragment center. During the use, add the liquid mixed component to the thigh internal through the connecting pipe, add as required and carry out the dropwise add to liquid, carry out solid interpolation powder solid material through the solid inlet pipe, powder solid material can be broken up under the rotation of revolving fragment, and the material after breaking up is dispersed form unrestrained, can improve dispersion effect to the quality to improve resin.
The application also discloses a weather-resistant resin and a preparation process thereof.
Examples
Example 1
The raw materials of the weather-resistant resin are shown in Table 1.
Wherein the mass ratio of the composite nano particles is 2: 1 nano calcium carbonate and nano silicon dioxide.
The preparation method comprises the following steps:
s1, adding 5.6kg of toluene and 1.35kg of butyl acetate in parts by weight in the total raw materials into a reaction vessel, adding the composite nanoparticles into the reaction vessel, starting stirring in the reaction vessel, stirring and mixing, and heating to 105 ℃.
S2, mixing all methyl acrylate, butyl acrylate, hydroxypropyl acrylate and acrylic acid in the total raw materials with benzoyl peroxide in an amount of 0.06kg by weight in the total raw materials to obtain a first mixed component, and then dropwise adding the first mixed component into a reaction container at a rate of 78 g/S. Stirring is carried out while the dropwise addition is carried out, and the reaction lasts for 2.5 hours after the dropwise addition is finished.
S3, mixing the residual toluene, butyl acetate and benzoyl peroxide in the total raw materials to obtain a second mixed component, dropwise adding the second mixed component into the reaction container for 3 times, wherein the dropwise adding speed is 75g/S, the temperature is kept for 45min after dropwise adding, and the process is repeated for 3 times, and the total weight of the second mixed component is one third each time. Stirring is carried out while dripping, the temperature is raised to 125 ℃ after dripping is finished, and heat preservation and reflux are carried out for 2.3 h.
And S4, cooling the material to 25 ℃, and filtering to obtain the product.
Example 2
A weather-resistant resin is different from the weather-resistant resin in example 1 in the component content of each raw material, and is specifically shown in Table 2.
Example 3
A weather-resistant resin is different from the weather-resistant resin in example 1 in the component content of each raw material, and is specifically shown in Table 2.
Example 4
A weatherable resin, which is different from example 1 in that it is prepared by: and (S3) dropwise adding the second mixed component once at a constant dropwise adding speed, and keeping the temperature for 45min after dropwise adding.
Example 5
A weatherable resin, which is different from example 1 in that it is prepared by: the dropping rate in the step S3 was 200 g/S.
Example 6
A weatherable resin, which is different from example 1 in that nano calcium carbonate is used for all composite nanoparticles.
Example 7
A weatherable resin, which differs from example 1 in that composite nanoparticles are not added.
Example 8
A weatherable resin, differing from example 1 in that it was prepared by the following method: all the components are added simultaneously, and stirring is started to carry out mixing reaction.
Performance test
The resins prepared in examples 1 to 7 and the commercially available AP-5073 resin were tested for dryness according to GB/T1728-.
Hardness test was carried out according to GB/T6739 & 2006 Pencil method for determination of paint film hardness, and hardness was recorded.
The gloss was measured by "determination of the specular gloss of a paint film of a metallic pigment-free pigmented paint by GB/T9754-.
An artificial accelerated aging test is carried out, an ATLAS UV2000 instrument is used for carrying out an alternating test of 4h spraying and 8h illumination (intensity: 0.68w/m 2), the duration is 1200h, and the light loss rate is recorded.
TABLE 2
| Examples | Actual drying time/h | Hardness of | 60 ℃ gloss/%) | Light loss ratio/% (60 ℃) before and after aging test | Flexibility/mm |
| Example 1 | 22 | 5H | 94 | 2 | 4 |
| Example 2 | 22 | 5H | 94 | 2 | 4 |
| Example 3 | 22 | 5H | 95 | 2 | 4 |
| Example 4 | 26 | 5H | 92 | 2 | 3 |
| Example 5 | 25 | 5H | 92 | 3 | 3 |
| Example 6 | 24 | 5H | 91 | 3 | 4 |
| Example 7 | 26 | 3H | 89 | 4 | 2 |
| Example 8 | 30 | 3H | 91 | 3 | 3 |
| AP-5073 resin | 24 | 4H | 93 | 2 | 3 |
Combining the resins of examples 1-3 and AP-5073 with Table 2, it can be seen that the weatherable resins prepared herein have good basic properties, excellent hardness, drying time, gloss, flexibility and aging resistance, and low raw material cost.
Combining example 1 with example 4 and example 5 with table 2, it can be seen that the dropping speed and dropping mode of the mixed components have an influence on the performance of the finished resin product, mainly because the uniform and slow dropping during the resin synthesis process can control the molecular weight and uniformity of the resin synthesis, thereby affecting the effect of the finished resin product.
Combining example 1 with example 6 and example 7 with table 2, it can be seen that the addition of composite nanoparticles to the mixed components can improve the flexibility of the resin, while the mixture of nano calcium carbonate and nano silica can improve the gloss of the resin compared to pure calcium carbonate.
By combining the example 1 and the example 8 and the table 2, it can be seen that the preparation method in the application can significantly improve each basic property of the resin, and the synthesized resin has better properties. The preparation method can realize good matching effect by controlling the temperature, the adding sequence and the dripping speed of each barrier component, the molecular weight of the synthesized resin is uniform and consistent, and the mixing reaction effect is good.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (2)
1. The weather-resistant resin is characterized by being prepared by mixing and reacting the following raw materials in parts by weight: 650 parts of toluene, 150 parts of butyl acetate, 180 parts of methyl acrylate, 470 parts of methyl acrylate, 230 parts of butyl acrylate, 160 parts of hydroxypropyl acrylate, 3-7 parts of acrylic acid, 10-14 parts of benzoyl peroxide and 20-80 parts of composite nanoparticles, wherein the composite nanoparticles are nano calcium carbonate and nano silicon dioxide in a mass ratio of 2-3: 1;
is prepared by the following steps:
s1, putting 560-580 parts by weight of toluene and 155 parts by weight of 135-155 parts by weight of butyl acetate in the total raw materials into a reaction vessel, starting stirring and mixing, heating to 105-115 ℃, then putting 20-80 parts by weight of composite nanoparticles into the reaction vessel, and continuing stirring;
s2, mixing methyl acrylate, butyl acrylate, hydroxypropyl acrylate, acrylic acid and 6-9 parts by weight of benzoyl peroxide in the total raw materials into a first mixed component, dropwise adding into a reaction container at a dropwise adding rate of 78-82g/S while stirring, and reacting for 2-3h after dropwise adding;
s3, mixing the residual toluene, butyl acetate and benzoyl peroxide in the total raw materials into a second mixed component, then dropwise adding the second mixed component into a reaction container, wherein the dropwise adding of the second mixed component is divided into 3 times, one third of the total weight of the second mixed component is dropwise added each time, the dropwise adding speed is 75-100g/S each time, stirring is carried out while dropwise adding, the temperature is increased to 140 ℃ after the dropwise adding is completed each time, warm reflux is carried out for 45-60min, and finally the temperature of the material is reduced to 20-35 ℃, and then the material is filtered to obtain the product.
2. The process for preparing a weatherable resin according to claim 1, comprising the steps of:
s1, adding 560-580 parts by weight of toluene and 155 parts by weight of butyl acetate into a reaction vessel, stirring and mixing, heating to the temperature of 105-115 ℃, adding 20-80 parts by weight of composite nanoparticles into the reaction vessel, and continuing stirring;
s2, mixing methyl acrylate, butyl acrylate, hydroxypropyl acrylate, acrylic acid and 6-9 parts by weight of benzoyl peroxide in the total raw materials into a first mixed component, dropwise adding into a reaction container at a dropwise adding rate of 78-82g/S while stirring, and reacting for 2-3h after dropwise adding;
s3, mixing the residual toluene, butyl acetate and benzoyl peroxide in the total raw materials to form a second mixed component, dropwise adding the second mixed component into the reaction container for 3 times, wherein the dropwise adding speed of each dropwise adding is 75-100g/S, stirring is carried out while dropwise adding, the temperature is raised to 140 ℃ after each dropwise adding is finished, the temperature is refluxed for 45-60min, and finally the temperature of the material is lowered to 20-35 ℃, and then the material is filtered to obtain the product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111132355.2A CN113861331B (en) | 2021-09-27 | 2021-09-27 | Weather-resistant resin and preparation process and preparation equipment thereof |
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| CN202111132355.2A CN113861331B (en) | 2021-09-27 | 2021-09-27 | Weather-resistant resin and preparation process and preparation equipment thereof |
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| EP2778195B1 (en) * | 2013-03-15 | 2017-04-05 | Rohm and Haas Company | Redox polymers for improved dirt and water resistance for elastomeric wall and roof coatings |
| CN204051640U (en) * | 2014-09-10 | 2014-12-31 | 山东普洛得邦医药有限公司 | MEAM synthesis reactor |
| CN112029362B (en) * | 2020-08-21 | 2021-11-30 | 帝斯曼先达合成树脂(佛山)有限公司 | Preparation method of core-shell structure nano particles and hardened water-based acrylic resin coating |
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Denomination of invention: A weather resistant resin and its preparation process and equipment Effective date of registration: 20230626 Granted publication date: 20220826 Pledgee: Weihai commercial bank Limited by Share Ltd. revitalization branch Pledgor: Weihai jinant coating Co.,Ltd. Registration number: Y2023980045771 |