CN112694554A - Synthesis method and production equipment of SMA resin - Google Patents
Synthesis method and production equipment of SMA resin Download PDFInfo
- Publication number
- CN112694554A CN112694554A CN202110029643.9A CN202110029643A CN112694554A CN 112694554 A CN112694554 A CN 112694554A CN 202110029643 A CN202110029643 A CN 202110029643A CN 112694554 A CN112694554 A CN 112694554A
- Authority
- CN
- China
- Prior art keywords
- kettle
- solvent
- condenser
- maleic anhydride
- styrene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/02—Methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/10—Dissolving using driven stirrers
-
- 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
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a synthesis method of SMA resin and production equipment thereof, wherein styrene and maleic anhydride are reacted in a solvent at room temperature to prepare the SMA resin. Specifically, the synthesis method of the SMA resin comprises the following steps: at room temperature, adding styrene and maleic anhydride into a solvent, stirring to dissolve the styrene and the maleic anhydride, and adding an initiator to prepare a raw material solution; putting a solvent into a reaction bottle, and heating to a reaction temperature; slowly dripping the raw material solution into the reaction bottle, and then preserving the temperature for a period of time at the reaction temperature after dripping; the solvent is evaporated off, and the tablets are poured out when the solution is hot. The invention has the following beneficial effects: the solvent polymerization method is adopted, the temperature is stable in the reaction process, and the molecular weight distribution is narrow; styrene, maleic anhydride and an initiator are prepared into a solution in advance, and then dropwise added, so that the composition of a product is uniform; the reaction temperature is higher, and the product SMA is ensured to be a random copolymer; the reaction is fast, the raw material accumulation in the solution is less, the reaction heat release is stable, the reaction temperature is easy to control, and the safety is high; the molecular weight distribution is narrow.
Description
Technical Field
The invention belongs to the technical field of resin synthesis, and particularly relates to a synthetic method of SMA resin and production equipment thereof.
Background
Styrene-maleic anhydride copolymer (SMA) is a polymer with excellent heat resistance, rigidity and dimensional stability, and is widely used in the fields of latex paints, water treatment agents, modifiers of adhesives, emulsifiers for pesticides, textile aids, printing inks, composite materials, curing agents for epoxy resins, and the like.
Styrene-maleic anhydride copolymers can be classified into two types according to the difference in copolymer composition and sequence structure: one is an alternating copolymer of styrene and maleic anhydride (A-SMA) in a molar ratio close to 1:1, and the other is a random copolymer of low maleic anhydride content (R-SMA). Styrene-maleic anhydride alternating copolymers cannot be used as thermoplastic materials because they absorb water easily and are difficult to mold. The styrene-maleic anhydride random copolymer is a novel material developed in the later stage of the 70 th 20 th century, has good heat resistance, low melt viscosity and excellent processing performance, can be blended and modified with various high polymer materials, and has good chemical stability, foaming performance, transparency and high hardness. Further, the adhesive property, plating property and coloring property are also good.
At present, SMA production methods mainly include precipitation polymerization, bulk polymerization, and solution polymerization. The solution polymerization method uses a solvent as a medium, is easy to transfer reaction heat, is beneficial to controlling production, and the obtained SMA product has a regular structure and narrow molecular weight distribution and is beneficial to improving the performance of the SMA product. Therefore, the solution polymerization method is the most widely applied method in SMA synthesis.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a synthetic method of SMA resin and production equipment thereof, so as to solve the problems in the prior art.
The technical scheme for solving the technical problems is as follows: a synthesis method of SMA resin is characterized in that styrene and maleic anhydride react in a solvent at room temperature, and the reaction process is as follows:
the invention is further configured such that the method of synthesizing SMA resin comprises the steps of:
(1) at room temperature, adding styrene and maleic anhydride in a weight ratio of 1: 1-8: 1 into a solvent, stirring to dissolve the styrene and the maleic anhydride, and adding an initiator to prepare a raw material solution;
(2) continuously adding the solvent, and heating to the reaction temperature;
(3) continuously and slowly dripping the raw material solution, and then preserving the temperature for a period of time at the reaction temperature after dripping;
(4) the solvent is evaporated off, and the tablets are poured out when the solution is hot.
The invention is further provided that the solvent is one or more selected from toluene, xylene, ethylbenzene, propylbenzene, isopropylbenzene, trimethylbenzene, butylbenzene, isobutylbenzene and diethylbenzene, and the initiator is a free radical initiator, including peroxide initiators and azo initiators.
The invention is further set in that in the step (2), the reaction temperature is 130-230 ℃.
The invention is further set that the amount of the initiator is 0.1-20% of the total mass of the styrene and the maleic anhydride.
The invention is further set in that in the step (3), the dripping time is 2-10 hours, and the heat preservation time is 1-6 hours.
The invention is further set as that a catalyst is added, the catalyst is a mixture of aluminum trichloride, phenetole and methylchlorosilane, the content of the catalyst is 0.2-0.6% of the total mass of styrene and maleic anhydride, and the mass ratio of the aluminum trichloride, the phenetole and the methylchlorosilane is (0.2-0.8): 1: (0.4-0.8); the diameter of the aluminum trichloride is 3-4 mm.
The invention is further set in that the aluminum trichloride, the phenetole and the methyl chlorosilane are mixed and heated before being put into the reactor, and the temperature is kept at 130-230 ℃.
The invention also provides equipment for producing the SMA resin, which comprises a batching kettle, a polymerization kettle, a dissolution kettle and a devolatilization kettle which are connected in sequence, wherein stirring devices are arranged in the batching kettle, the polymerization kettle, the dissolution kettle and the devolatilization kettle; the bottom discharge port of the batching kettle is connected with the top feed port of the polymerization kettle, the bottom discharge port of the polymerization kettle is connected with the top feed port of the dissolution kettle, and the bottom discharge port of the dissolution kettle is connected with the top feed port of the devolatilization kettle;
the top of the dissolution kettle is connected with a first condenser, the first condenser is connected with a first buffer tank, and the first buffer tank is connected with a vacuum pump;
the top of the devolatilization kettle is connected with a second condenser, the second condenser is connected with a second buffer tank, and the second buffer tank is connected with a vacuum pump;
the first condenser and the second condenser are also connected with a receiving groove.
The invention is further provided that the receiving tank is connected with a solvent pump, and the solvent pump is connected with the batching kettle; a metering pump is arranged between the batching kettle and the polymerization kettle; and a flaker is arranged behind the receiving groove.
The invention is further provided that a receiving tank is connected to each of the first condenser and the second condenser, and another receiving tank having a larger volume is connected to each of the first condenser and the second condenser, and the larger volume receiving tank is connected to the solvent pump.
The invention is further provided that the receiving tank has a volume of 2000L and the receiving tank with a larger volume has a volume of 15000L.
The invention is further arranged in such a way that a feed inlet is arranged on the batching kettle, a first heat source inlet and outlet jacket is arranged on the outer layer of the batching kettle, a second heat source inlet and outlet jacket is arranged on the outer layer of the polymerization kettle, a third heat source inlet and outlet jacket is arranged on the outer layer of the dissolution kettle, and a fourth heat source inlet and outlet jacket is arranged on the outer layer of the devolatilization kettle.
The invention is further provided that steam, water or heat conducting oil is introduced into water of the first heat source inlet and outlet jacket, the second heat source inlet and outlet jacket, the third heat source inlet and outlet jacket and the fourth heat source inlet and outlet jacket.
The invention is further provided that the volume of the batching kettle is 4000L, the volume of the polymerization kettle is 5000L, the volume of the dissolution kettle is 5000L, and the volume of the devolatilization kettle is 1500L.
In conclusion, the invention has the following beneficial effects:
(1) the invention adopts a solvent polymerization method, and has stable temperature and narrow molecular weight distribution in the reaction process.
(2) In the invention, styrene, maleic anhydride and an initiator are prepared into a solution in advance and then are dripped, and the composition of the product is relatively uniform.
(3) The reaction temperature is higher, so that the product SMA is ensured to be a random copolymer; the reaction speed is high, the raw material accumulation in the solution is less, the reaction heat release is stable, the reaction temperature is easy to control, and the safety is high; the molecular weight distribution is narrow.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of the stripping vessel;
FIG. 3 is a schematic diagram of the devolatilizer kettle structure.
Wherein, 1, a batching kettle; 2. a polymerization kettle; 3. a stripping kettle; 4. a devolatilization kettle; 5. a first condenser; 6. a first buffer tank; 7. a vacuum pump; 8. a second condenser; 9. a second buffer tank; 10. a vacuum pump; 11. a receiving groove; 12. a receiving groove; 13. a solvent pump; 14. a metering pump.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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 invention.
The invention provides a synthesis method of SMA resin, which is prepared by reacting styrene and maleic anhydride in a solvent at room temperature, and the specific synthesis method comprises the following steps:
(1) at room temperature, adding styrene and maleic anhydride into a solvent, stirring to dissolve the styrene and the maleic anhydride, and adding an initiator to prepare a raw material solution;
(2) continuously adding the solvent, and heating to the reaction temperature;
(3) continuously and slowly dripping the raw material solution for 2-10 hours, and then preserving the temperature for a period of time at the reaction temperature after dripping, wherein the preserving time is 1-6 hours;
(4) the solvent is evaporated off, and the tablets are poured out when the solution is hot.
The ratio of styrene to maleic anhydride is 1: 1-8: 1.
Wherein, the mass of the solvent is 1 to 10 times, preferably 3 to 7 times of the total mass of the styrene and the maleic anhydride, and the maleic anhydride and the initiator are generally ensured to be fully dissolved.
Wherein the solvent is selected from one or more of toluene, xylene, ethylbenzene, propylbenzene, isopropylbenzene, trimethylbenzene, butylbenzene, isobutylbenzene and diethylbenzene. Preferably, the solvent is selected from higher boiling solvents such as propylbenzene, isopropylbenzene, trimethylbenzene, butylbenzene, isobutylbenzene, diethylbenzene, and the like.
Wherein the initiator is a free radical initiator and comprises a peroxide initiator and an azo initiator. Preferably, the initiator is an organic peroxide, such as benzoyl peroxide, dicumyl peroxide, cumene hydroperoxide, and the like. The amount of the initiator is 0.1-20% of the total mass of the styrene and the maleic anhydride, and the specific amount is determined by the molecular weight of a target product and the reaction temperature.
The reaction temperature is 130-230 ℃. Preferably, the reaction temperature is 150-200 ℃. More preferably, the initiator half-life is at a temperature below 5 minutes.
As a more preferable embodiment, a catalyst is also added, the catalyst is a mixture of aluminum trichloride, phenetole and methylchlorosilane, and the content of the catalyst is 0.2-0.6 percent of the total mass of styrene and maleic anhydride. The mass ratio of the aluminum trichloride to the phenetole to the methylchlorosilane is (0.2-0.8): 1: (0.4-0.8). The diameter of the aluminum trichloride is 3-4 mm. Mixing and heating aluminum trichloride, phenetole and methyl chlorosilane before adding, and keeping the temperature at 130-230 ℃.
Example 1
(1) 300g of xylene were placed in a compounding kettle equipped with a thermometer, a dropping channel and a condenser, and heated to 135 ℃ in an oil bath.
(2) 49g of maleic anhydride, 156g of styrene and 300g of xylene are added and stirred until the maleic anhydride is completely dissolved. Adding 17.4g of Benzoyl Peroxide (BPO) into 35g of dimethylbenzene, stirring until the Benzoyl Peroxide (BPO) is completely dissolved, standing, removing a water layer, adding a xylene layer into a solution of maleic anhydride and styrene dimethylbenzene, stirring and mixing uniformly, and preparing a raw material solution.
(3) Weighing 1g of BPO, dissolving in 2g of water, separating the water layer, and averagely dividing into 2 parts.
(4) And (3) injecting the raw material solution into a polymerization kettle by using a metering pump, controlling the injection time to be 4 hours, keeping the reaction temperature at 135 ℃, preserving the heat for 0.5 hour after the injection is finished, adding 1 part of the BPO solution, preserving the heat for 0.5 hour, adding the rest 1 part of the BPO solution, and preserving the heat for reaction for 2 hours.
(5) And after the heat preservation is finished, raising the temperature, distilling the dimethylbenzene, gradually pulling vacuum for distillation in the later period, and finally, when the temperature reaches 180 ℃, completely distilling the dimethylbenzene under high vacuum to obtain 204g of SMA resin.
Example 2
(1) 300g of xylene were placed in a compounding kettle equipped with a thermometer, a dropping channel and a condenser, and heated to 135 ℃ in an oil bath.
(2) 19.6g of maleic anhydride, 166.4g of styrene and 300g of xylene were continuously added and stirred until all the maleic anhydride was dissolved. Adding 9.3g of Benzoyl Peroxide (BPO) into 20g of dimethylbenzene, stirring until the Benzoyl Peroxide (BPO) is completely dissolved, standing, removing a water layer, adding a xylene layer into a solution of maleic anhydride and styrene dimethylbenzene, stirring and mixing uniformly to prepare a raw material solution.
(3) Weighing 1g of BPO, dissolving in 2g of water, separating the water layer, and averagely dividing into 2 parts.
(4) And (3) injecting the raw material solution into a polymerization kettle by using a metering pump, controlling the injection time to be 4 hours, keeping the reaction temperature at 135 ℃, preserving the heat for 0.5 hour after the injection is finished, adding 1 part of the BPO solution, preserving the heat for 0.5 hour, adding the rest 1 part of the BPO solution, and preserving the heat for reaction for 2 hours.
(5) After the heat preservation is finished, the temperature is raised, the dimethylbenzene is distilled, vacuum distillation is gradually carried out in the later period, the final temperature reaches 180 ℃, and the dimethylbenzene is completely distilled under high vacuum, so that 182.2g of SMA resin is obtained.
Example 3
(1) 300g of butylbenzene was put into a compounding kettle with a thermometer, a dropping passage and a condenser tube, and heated to 175 ℃ in an oil bath.
(2) 24.5g of maleic anhydride, 156g of styrene and 200g of butylbenzene are continuously added and stirred until the maleic anhydride is completely dissolved. Then 4.5g of dicumyl peroxide is added and stirred until the dicumyl peroxide is completely dissolved, and the raw materials are uniformly mixed to prepare a raw material solution.
(3) The raw material solution is injected into a polymerization kettle by a metering pump, the injection time is controlled to be 4 hours, the reaction temperature is kept at 175 ℃, and the reaction is kept for 2 hours after the injection.
(4) And after the heat preservation is finished, raising the temperature, pulling vacuum distillation butylbenzene, and pulling vacuum distillation step by step in the later period, wherein the final temperature reaches 180 ℃, and butylbenzene is evaporated completely under high vacuum to obtain 178.2g of SMA resin.
Example 4
On the basis of the embodiment 1, before the raw material solution is injected into the batching kettle, the catalyst is added into the batching kettle at the dropping speed of 2 drops per second, the mass of the catalyst is 0.2 percent of the total mass of the styrene and the maleic anhydride, and the mass ratio of the aluminum trichloride to the phenetole to the methylchlorosilane is 0.2: 1: 0.8, the diameter of the aluminum trichloride is 4 mm. Finally, 217g of SMA resin is obtained.
Example 5
On the basis of the embodiment 2, before the raw material solution is injected into the batching kettle, the catalyst is added into the batching kettle at the dropping speed of 3 drops per second, the mass of the catalyst is 0.4 percent of the total mass of the styrene and the maleic anhydride, and the mass ratio of the aluminum trichloride to the phenetole to the methylchlorosilane is 0.5: 1: 0.8, the diameter of the aluminum trichloride is 4 mm. Finally obtaining 205g of SMA resin.
Example 6
On the basis of the embodiment 3, before the raw material solution is injected into the batching kettle, the catalyst is added into the batching kettle at the dropping speed of 4 drops per second, the mass of the catalyst is 0.6 percent of the total mass of the styrene and the maleic anhydride, and the mass ratio of the aluminum trichloride to the phenetole to the methylchlorosilane is 0.8: 1: 0.4, the diameter of the aluminum trichloride is 3 mm. The total yield of 191g of SMA resin was finally obtained.
Example 7
As an apparatus capable of realizing the method, the SMA resin production apparatus is used for producing SMA resin, and is shown in the figures 1-3, and comprises a batching kettle 1, a polymerization kettle 2, a dissolution kettle 3 and a devolatilization kettle 4 which are connected in sequence. The bottom discharge port of the batching kettle 1 is connected with the top feed port of the polymeric kettle 2, the bottom discharge port of the polymeric kettle 2 is connected with the top feed port of the dissolution kettle 3, and the bottom discharge port of the dissolution kettle 3 is connected with the top feed port of the devolatilization kettle 4. In order to facilitate the uniform mixing of the materials, stirring devices are arranged in the batching kettle 1, the polymerization kettle 2, the dissolution and volatilization kettle 3 and the volatilization kettle 4. For the convenience of metering, a metering pump 14 is provided between the compounding tank 1 and the polymerization tank 2.
The top of the stripping kettle 3 is connected with a first condenser 5, the first condenser 5 is connected with a first buffer tank 6, and the first buffer tank 6 is connected with a vacuum pump 7. The top of the devolatilization kettle 4 is connected with a second condenser 8, the second condenser 8 is connected with a second buffer tank 9, and the second buffer tank 9 is connected with a vacuum pump 10. The first condenser 5 and the second condenser 8 are also connected to receiving grooves 11.
As another example, the receiving tank 11 is connected to a solvent pump 13, and the solvent pump 13 is connected to the batch kettle 1.
Further, the first condenser 5 and the second condenser 8 are respectively connected with one receiving tank 11, the two receiving tanks 11 are connected with another receiving tank 12 with a larger volume, and the receiving tank 12 with the larger volume is connected with a solvent pump 13.
Specifically, a feed inlet is arranged on the batching kettle 1, a first heat source inlet and outlet jacket is arranged on the outer layer of the batching kettle 1, a second heat source inlet and outlet jacket is arranged on the outer layer of the polymeric kettle 2, a third heat source inlet and outlet jacket is arranged on the outer layer of the dissolution kettle 3, and a fourth heat source inlet and outlet jacket is arranged on the outer layer of the devolatilization kettle 4. Optionally, steam, water or heat conducting oil is introduced into water of the first heat source inlet and outlet jacket, the second heat source inlet and outlet jacket, the third heat source inlet and outlet jacket and the fourth heat source inlet and outlet jacket.
As an embodiment, the receiving groove may have a volume of 2000L and the receiving groove having a larger volume may have a volume of 15000L. The volume of the batching kettle 1 is 4000L, the volume of the polymerization kettle 2 is 5000L, the volume of the dissolution kettle 3 is 5000L, and the volume of the devolatilization kettle 4 is 1500L.
And further, a flaker is arranged behind the receiving groove, and the materials are placed into the flaker to be flaked.
The synthesis of the SMA resin by using the above-mentioned equipment comprises the following steps:
(1) preparing feed liquid in a material preparing kettle 1: adding styrene and maleic anhydride into the solvent for dissolving in sequence, stirring to dissolve completely, adding the solvent, and stirring and mixing uniformly.
(2) Polymerization reaction in polymerizer 2: and (4) pumping the prepared feed liquid into the kettle, and controlling the temperature.
(3) Desolventizing in a desolventizing kettle 3: after the reaction is carried out under the condition of heat preservation, the materials are transferred to a stripping kettle 3, cooled, vacuum distilled and the distillation temperature is controlled.
(4) Devolatilization in devolatilization kettle 4: after most of the solvent is evaporated, the materials in the kettle become thick, the discharging speed becomes slow, and the materials are transferred to a devolatilization kettle 4. The temperature was slowly raised and the vacuum degree was increased. Raising the temperature, fully drawing the vacuum, if the distillation speed is slow, switching to high vacuum, and distilling until no fraction is discharged.
(5) Discharging the materials to a flaker for flakiness.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A synthetic method of SMA resin is that styrene and maleic anhydride react in solvent at room temperature; the method is characterized by comprising the following steps:
(1) at room temperature, adding styrene and maleic anhydride in a weight ratio of 1: 1-8: 1 into a solvent, stirring to dissolve the styrene and the maleic anhydride, and adding an initiator to prepare a raw material solution;
(2) continuously adding the solvent, and heating to the reaction temperature;
(3) continuously and slowly dripping the raw material solution, and then preserving the temperature for a period of time at the reaction temperature after dripping;
(4) the solvent is evaporated off, and the tablets are poured out when the solution is hot.
2. The method for synthesizing the SMA resin according to claim 1, wherein the solvent is one or more selected from toluene, xylene, ethylbenzene, propylbenzene, isopropylbenzene, trimethylbenzene, butylbenzene, isobutylbenzene, diethylbenzene, and the initiator is a radical initiator including a peroxide initiator and an azo initiator.
3. The method for synthesizing the SMA resin according to claim 1, wherein in the step (2), the reaction temperature is 130-230 ℃.
4. The method for synthesizing the SMA resin according to claim 1, wherein the amount of the initiator is 0.1-20% of the total mass of the styrene and the maleic anhydride.
5. The method for synthesizing the SMA resin according to claim 1, wherein in the step (3), the dropping time is 2-10 hours, and the holding time is 1-6 hours.
6. The method for synthesizing the SMA resin according to claim 1, wherein a catalyst is further added, the catalyst is a mixture of aluminum trichloride, phenetole and methylchlorosilane, the content of the catalyst is 0.2-0.6% of the total mass of styrene and maleic anhydride, and the mass ratio of the aluminum trichloride, the phenetole and the methylchlorosilane is (0.2-0.8): 1: (0.4-0.8); the diameter of the aluminum trichloride is 3-4 mm.
7. The method for synthesizing the SMA resin of claim 6, wherein the aluminum trichloride, the phenetole and the methylchlorosilane are mixed and heated before being added, and the temperature is kept at 130-230 ℃.
8. The equipment for producing the SMA resin is characterized by comprising a batching kettle, a polymerization kettle, a dissolution kettle and a devolatilization kettle which are sequentially connected, wherein stirring devices are arranged in the batching kettle, the polymerization kettle, the dissolution kettle and the devolatilization kettle; the bottom discharge port of the batching kettle is connected with the top feed port of the polymerization kettle, the bottom discharge port of the polymerization kettle is connected with the top feed port of the dissolution kettle, and the bottom discharge port of the dissolution kettle is connected with the top feed port of the devolatilization kettle;
the top of the dissolution kettle is connected with a first condenser, the first condenser is connected with a first buffer tank, and the first buffer tank is connected with a vacuum pump;
the top of the devolatilization kettle is connected with a second condenser, the second condenser is connected with a second buffer tank, and the second buffer tank is connected with a vacuum pump;
the first condenser and the second condenser are also connected with a receiving groove.
9. The apparatus for producing SMA resin according to claim 8, wherein the receiving tank is connected to a solvent pump connected to an ingredient kettle; a metering pump is arranged between the batching kettle and the polymerization kettle; and a flaker is arranged behind the receiving groove.
10. The apparatus for manufacturing SMA resin according to claim 8, wherein one receiving groove is connected to each of the first condenser and the second condenser, and another receiving groove having a larger volume is connected to each of the first condenser and the second condenser, and the solvent pump is connected to the receiving groove having a larger volume.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110029643.9A CN112694554A (en) | 2021-01-11 | 2021-01-11 | Synthesis method and production equipment of SMA resin |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110029643.9A CN112694554A (en) | 2021-01-11 | 2021-01-11 | Synthesis method and production equipment of SMA resin |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112694554A true CN112694554A (en) | 2021-04-23 |
Family
ID=75513736
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110029643.9A Pending CN112694554A (en) | 2021-01-11 | 2021-01-11 | Synthesis method and production equipment of SMA resin |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112694554A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113402648A (en) * | 2021-07-26 | 2021-09-17 | 上海微陌新材料科技有限公司 | Mother liquor for preparing styrene-maleic anhydride copolymer by photo-initiation polymerization, copolymer preparation method and equipment |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4328327A (en) * | 1979-10-15 | 1982-05-04 | Daicel Chemical Industries, Ltd. | Continuous bulk polymerization process for preparing copolymer of aromatic vinyl monomer and maleic anhydride |
CN101580564A (en) * | 2009-06-19 | 2009-11-18 | 北京化工大学 | Synthetic method of high molecular weight (HMW) alternating copolymer of styrene and maleic anhydride |
CN102250273A (en) * | 2011-06-02 | 2011-11-23 | 北京化工大学 | Preparation method of styrene-maleic anhydride random copolymer |
CN102653578A (en) * | 2011-03-04 | 2012-09-05 | 武陟县智辉化工有限责任公司 | Method for synthesizing styrene-maleic anhydride polymer through precipitation |
CN103193932A (en) * | 2012-01-09 | 2013-07-10 | 上海飞凯光电材料股份有限公司 | Low-molecular-weight styrene-maleic anhydride alternating copolymer synthesis method |
CN105175598A (en) * | 2015-08-12 | 2015-12-23 | 莘县阳光包装材料有限公司 | Synthesis method of SMA resin with low molecular weight |
CN108239187A (en) * | 2017-12-14 | 2018-07-03 | 成都斯伯里科技有限公司 | The process units of acrylonitrile-styrene random copolymer |
CN109776710A (en) * | 2018-12-27 | 2019-05-21 | 苏州世名科技股份有限公司 | Structure containing phenylethylene-maleic anhydride and the waterborne pigment dispersant and preparation method thereof of graft modification |
CN111234081A (en) * | 2020-03-06 | 2020-06-05 | 长春工业大学 | Low-molecular-weight narrow-distribution styrene-maleic anhydride copolymer and preparation method thereof |
CN111763281A (en) * | 2020-07-04 | 2020-10-13 | 博立尔化工(扬州)有限公司 | Equipment and method for preparing acrylic resin for powder coating by continuous body process |
-
2021
- 2021-01-11 CN CN202110029643.9A patent/CN112694554A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4328327A (en) * | 1979-10-15 | 1982-05-04 | Daicel Chemical Industries, Ltd. | Continuous bulk polymerization process for preparing copolymer of aromatic vinyl monomer and maleic anhydride |
CN101580564A (en) * | 2009-06-19 | 2009-11-18 | 北京化工大学 | Synthetic method of high molecular weight (HMW) alternating copolymer of styrene and maleic anhydride |
CN102653578A (en) * | 2011-03-04 | 2012-09-05 | 武陟县智辉化工有限责任公司 | Method for synthesizing styrene-maleic anhydride polymer through precipitation |
CN102250273A (en) * | 2011-06-02 | 2011-11-23 | 北京化工大学 | Preparation method of styrene-maleic anhydride random copolymer |
CN103193932A (en) * | 2012-01-09 | 2013-07-10 | 上海飞凯光电材料股份有限公司 | Low-molecular-weight styrene-maleic anhydride alternating copolymer synthesis method |
CN105175598A (en) * | 2015-08-12 | 2015-12-23 | 莘县阳光包装材料有限公司 | Synthesis method of SMA resin with low molecular weight |
CN108239187A (en) * | 2017-12-14 | 2018-07-03 | 成都斯伯里科技有限公司 | The process units of acrylonitrile-styrene random copolymer |
CN109776710A (en) * | 2018-12-27 | 2019-05-21 | 苏州世名科技股份有限公司 | Structure containing phenylethylene-maleic anhydride and the waterborne pigment dispersant and preparation method thereof of graft modification |
CN111234081A (en) * | 2020-03-06 | 2020-06-05 | 长春工业大学 | Low-molecular-weight narrow-distribution styrene-maleic anhydride copolymer and preparation method thereof |
CN111763281A (en) * | 2020-07-04 | 2020-10-13 | 博立尔化工(扬州)有限公司 | Equipment and method for preparing acrylic resin for powder coating by continuous body process |
Non-Patent Citations (2)
Title |
---|
张钦文: "苯乙烯-马来酸酐共聚探讨", 《科技信息》 * |
海关总署关税征管司: "《危险化学品归类指南》", 31 August 2017, 中国海关出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113402648A (en) * | 2021-07-26 | 2021-09-17 | 上海微陌新材料科技有限公司 | Mother liquor for preparing styrene-maleic anhydride copolymer by photo-initiation polymerization, copolymer preparation method and equipment |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US3954722A (en) | Manufacture of uniform polymers | |
US5753784A (en) | Continuous preparation of polymers and apparatus for this purpose | |
JP2659722B2 (en) | Method for producing molding materials from monomer mixtures | |
CA1079898A (en) | Continuous bulk polymerisation process | |
KR100427376B1 (en) | Process for Preparing Polymer | |
EP2160422B1 (en) | Maleimide-alpha-alkylstyrene-based terpolymer with low molten viscosity and continuous bulk process for producing it | |
GB715666A (en) | Continuous method for making solid polymeric materials | |
TW307773B (en) | ||
CN109232787B (en) | Methyl methacrylate-styrene copolymer resin, preparation method and application thereof | |
EP2066708A1 (en) | Maleimide-alpha-alkylstyrene-based tetrapolymer with low molten viscosity and continuous bulk process for producing it | |
EP0027274B1 (en) | Continuous bulk polymerization process for preparing a copolymer of an aromatic vinyl monomer and maleic anhydride | |
US2496653A (en) | Continuous bulk polymerization of styrene | |
EP0087165B1 (en) | Production of copolymers of alpha-methylstyrene | |
GB843896A (en) | Improved moulding grade copolymers and process for preparing the same | |
CN112694554A (en) | Synthesis method and production equipment of SMA resin | |
US3337650A (en) | Process for preparing graft polymers having high impact strength | |
CN107257808B (en) | Continuous process for preparing high heat resistant copolymers | |
KR101151062B1 (en) | Alpha methyl styrene-acrylonitrile-methylmethacrylate copolymer having excellent heat resistance and processibility, and a method of preparation thereof | |
US6488898B1 (en) | Process for preparing acrylonitrile-styrene copolymer | |
JPS6211710A (en) | Production of thermoplastic polymer | |
JPS5818363B2 (en) | Renzoku Kaiji Youji Yugohouhou | |
CZ279474B6 (en) | Process for removing volatile waste products from raw polymerization product | |
KR100874030B1 (en) | Manufacturing method of copolymer of styrene monomer and acrylonitrile monomer | |
CN214599017U (en) | A equipment for synthesizing SMA resin | |
JPH05331212A (en) | Production of acrylic resin |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210423 |