Preparation method and application of bio-based itaconic acid diglycidyl ester

By synthesizing bio-itaconic acid diglycidyl ester with a biepoxy structure using bio-itaconic acid and epoxy chlorohydrin, the problems of strong self-polymerization tendency, low epoxy value and low grafting rate are solved, and efficient and environmentally friendly graft monomer synthesis is achieved, which improves the grafting rate and compatibility effect.

CN119613357APending Publication Date: 2025-03-14NINGBO INST OF MATERIALS TECH & ENG CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202411793960.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-06
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

In the prior art, glycidyl methacrylate (GMA) as a reaction monomer has problems such as strong self-polymerization tendency, low epoxy value, low grafting rate and poor compatibility effect. Its non-biological basis origins, complex synthesis process and low yields.

Method used

Bio-itaconic acid and epoxypropane as raw materials were used to synthesize diglycidyl bio-itaconic acid by a non-solvent method, with a double epoxy structure, and used as graft monomers to prepare graft-based compatibility agents.

Benefits of technology

The synthesis of bio-based diglycidyl itaconic acid diglycidyl ester with high purity and low self-polymerization tendency has been achieved, and a new source of graft monomers has been opened up, the use of petrochemical chemicals has been reduced, and the advantages of low carbon environmental protection and renewable are improved, and the grafting rate and compatibility effect have been improved.

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Abstract

The invention discloses a preparation method and application of bio-based itaconic acid diglycidyl ester. The preparation method comprises the following steps: carrying out first reaction on itaconic acid and a sodium source at room temperature to prepare sodium itaconate; and carrying out a second reaction on a mixed reaction system at least containing the sodium itaconate, epoxy chloropropane, a catalyst and an anti-auto-agglutination agent to prepare the bio-based itaconic acid diglycidyl ester. The main raw materials for preparing the itaconic acid diglycidyl ester are bio-based sources, no organic solvent is needed in the reaction process, few reaction byproducts are generated, the prepared itaconic acid diglycidyl ester is high in purity and higher in epoxy value, the grafting compatilizer higher in epoxy value and grafting rate is easier to prepare, and the preparation method is suitable for industrial production. And the composition has a better compatibility effect.
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Description

Technical Field

[0001] The invention belongs to the field of bio-based ester monomer synthesis and grafting compatibilizers, and specifically relates to a preparation method and application of bio-based diglycidyl itaconate. Background Art

[0002] At present, bio-based materials are becoming more and more important in the development of new materials in the future. Among them, itaconic acid is a bio-based organic acid made from plant components such as non-grain starch, sucrose, straw and corn platycodon as raw materials through special biological fermentation. Epichlorohydrin, as an important raw material for epoxy resins and epoxy oligomers, has also developed a biomass glycerol-chemical enzyme synthesis method.

[0003] Glycidyl methacrylate (GMA) has reactive carbon-carbon double bonds and ionic epoxy groups. It can be used as a coating and adhesive, and can also be used as an important reactive monomer for ionic polymerization and double bond homopolymerization or copolymerization. It is an indispensable chemical raw material. However, GMA is not bio-based, and the GMA double bond has a strong tendency to self-polymerize, and it has only one epoxy group, so its bonding effect is limited. In particular, polar monomers used as grafted two-phase compatibilizers often have disadvantages such as low grafting rate and general compatibility effect. Therefore, it will be crucial to synthesize an ester monomer with a bio-based source, weak self-polymerization tendency and multi-epoxy structure to replace traditional GMA.

[0004] So far, there are very few reports on this type of ester monomers. The current method for preparing diglycidyl itaconate requires the use of non-biobased chlorination reagents and various organic solvents, such as tetrahydrofuran, chloroform, toluene and xylene. The synthesis process is relatively complicated and the yield is low. In addition, the synthesized glycerol ester is mainly used in thermosetting epoxy resins. There is no report on the synthesis of diglycidyl itaconate using biomass itaconic acid and epichlorohydrin as raw materials, and there is no report in any relevant literature or patent using it as a grafting monomer in a grafting two-phase compatibilizer. Summary of the invention

[0005] The main purpose of the present invention is to provide a preparation method and application of bio-based diglycidyl itaconate to overcome the shortcomings of the prior art.

[0006] In order to achieve the above-mentioned invention object, the technical solution adopted by the present invention includes:

[0007] The embodiment of the present invention provides a method for preparing bio-based diglycidyl itaconate, which comprises:

[0008] Allowing itaconic acid to react with a sodium source at room temperature to produce sodium itaconate;

[0009] And, a mixed reaction system containing at least the sodium itaconate, epichlorohydrin, a catalyst, and an anti-self-polymerization agent is subjected to a second reaction to obtain bio-based diglycidyl itaconate.

[0010] The embodiment of the present invention also provides the use of the bio-based diglycidyl itaconate prepared by the aforementioned preparation method in the preparation of a grafting compatibilizer.

[0011] The embodiment of the present invention further provides a graft compatibilizer, and the raw materials for preparing the graft compatibilizer include the following components calculated by weight: 100 parts of polypropylene, 0.2-1 parts of initiator and 1-10 parts of diglycidyl itaconate;

[0012] Wherein, the diglycidyl itaconate is prepared by the aforementioned preparation method.

[0013] The embodiment of the present invention also provides a method for preparing the aforementioned graft compatibilizer, which comprises: uniformly mixing polypropylene, an initiator, and diglycidyl itaconate, and then inputting the obtained material into a twin-screw extruder for melt blending, dynamic grafting reaction extrusion, pelletizing, and homogenization to obtain a graft compatibilizer.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] (1) The present invention uses bio-based itaconic acid and epichlorohydrin, and synthesizes bio-based itaconic acid diglycidyl ester by a non-solvent method. Compared with traditional glycidyl methacrylate, the present invention is not only convenient and simple to synthesize, easy to operate and implement, with fewer side reactions, and a high purity of the obtained product, but also opens up a new source of grafting monomer raw materials, reduces petrochemical chemicals as much as possible from the source and avoids the use of organic solvents, and has the advantages of low carbon, environmental protection and renewable;

[0016] (2) The bio-based diglycidyl itaconate synthesized in the present invention has a diepoxy structure and has a higher epoxy value than GMA. As a grafting monomer, it can not only reduce the self-polymerization of the monomer during the grafting process, but also the prepared EIA-g-PP compatibilizer has a higher epoxy value and grafting rate. As a polypropylene compatibilizer, it has a better compatibility effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1This is the hydrogen nuclear magnetic resonance spectrum of the bio-based diglycidyl itaconate prepared in Example 2 of the present invention. DETAILED DESCRIPTION

[0019] In view of the defects of the prior art, the inventor of this case has proposed the technical solution of the present invention after long-term research and extensive practice. The technical solution of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] Specifically, as one aspect of the technical solution of the present invention, a method for preparing bio-based diglycidyl itaconate involves:

[0021] Allowing itaconic acid to react with sodium source at room temperature to obtain sodium itaconate;

[0022] And, a mixed reaction system containing at least the sodium itaconate, epichlorohydrin, a catalyst, and an anti-self-polymerization agent is subjected to a second reaction to obtain bio-based diglycidyl itaconate.

[0023] In some preferred embodiments, the sodium source includes any one or more combinations of sodium hydroxide, sodium carbonate, and sodium bicarbonate, but is not limited thereto.

[0024] In some preferred embodiments, the molar ratio of carboxylate in the itaconic acid to sodium atoms in the sodium source is 1:1.

[0025] In some preferred embodiments, the preparation method specifically comprises:

[0026] The sodium itaconate, epichlorohydrin, catalyst and anti-self-polymerization agent are mixed uniformly, and then stirred at room temperature for 5-30 minutes in an inert gas, and then heated to 80-120° C. for a second reaction for 1-3 hours;

[0027] And, after the second reaction is completed, the obtained product is washed with water and distilled under reduced pressure at 60-110° C. to obtain bio-based diglycidyl itaconate.

[0028] In some preferred embodiments, the mass ratio of the sodium itaconate, epichlorohydrin, catalyst and anti-self-polymerization agent is 100:600-1000:1-6:0.2-1.

[0029] In some preferred embodiments, the catalyst includes any one or more combinations of benzyltriethylammonium chloride (TEBAC), tetrabutylammonium bromide (TBAB), tetrabutylammonium chloride (TBAC), tetrabutylammonium hydrogen sulfate (THS), trioctylmethylammonium chloride (Aliquat336), dodecyltrimethylammonium chloride (DTAC), and tetradecyltrimethylammonium chloride (TTAC), and is not limited thereto.

[0030] In some preferred embodiments, the anti-self-polymerization agent includes any one or more combinations of p-benzoquinone, methylhydroquinone, p-hydroxyanisole, 2-tert-butylhydroquinone (TBHQ), and 2,5-di-tert-butylhydroquinone (DTBHQ), but is not limited thereto.

[0031] In some more specific embodiments, the method for preparing bio-based diglycidyl itaconate comprises the following steps:

[0032] a. 100 parts by mass of itaconic acid and sodium hydroxide in the same molar ratio as the carboxylate were prepared at room temperature to prepare sodium itaconate;

[0033] b. After 100 parts by mass of sodium itaconate prepared in step a, 600-1000 parts by mass of epichlorohydrin, 1-6 parts of a catalyst and 0.2-1 parts of an anti-self-polymerization agent are uniformly mixed, under inert gas protection, vigorously stirred at room temperature for 5-30 min, and then heated to 80-120 ° C, and reacted for 1-3 h;

[0034] c. After cooling to room temperature, the component obtained in b is washed with water and distilled under reduced pressure at 60-110°C to obtain bio-based diglycidyl itaconate.

[0035] The bio-based diglycidyl itaconate prepared by the present invention has the following structure:

[0036]

[0037] Another aspect of the embodiments of the present invention further provides the use of the bio-based diglycidyl itaconate prepared by the aforementioned preparation method in the preparation of a grafting compatibilizer.

[0038] For example: the grafted compatibilizer is a polypropylene compatibilizer.

[0039] Another aspect of the embodiment of the present invention further provides a graft compatibilizer, and the raw materials for preparing the graft compatibilizer include the following components calculated by weight: 100 parts of polypropylene, 0.2-1 parts of initiator and 1-10 parts of diglycidyl itaconate;

[0040] Wherein, the diglycidyl itaconate is prepared by the aforementioned preparation method.

[0041] In some preferred embodiments, the polypropylene includes any one or more combinations of homopolymer PP, random copolymer PP, and block copolymer PP, but is not limited thereto.

[0042] In some preferred embodiments, the initiator includes any one or more combinations of dicumyl peroxide, di-tert-butyl peroxide, 1,4-di-tert-butylperoxyisopropylbenzene, and tert-butyl peroxyacetate, but is not limited thereto.

[0043] Another aspect of an embodiment of the present invention also provides a method for preparing the aforementioned grafted compatibilizer, which comprises: uniformly mixing polypropylene, an initiator, and diglycidyl itaconate, and then inputting the obtained material into a twin-screw extruder for melt blending, dynamic grafting reaction extrusion, pelletizing, and homogenization to obtain a grafted compatibilizer.

[0044] In some preferred embodiments, the process parameters adopted by the twin-screw extruder include: the temperature of zone 1 is 140-160°C, the temperature of zone 2 is 165-175°C, the temperature of zone 3 is 175-180°C, the temperatures of zones 4 to 7 are independently 180-185°C, the temperatures of zones 8 to 10 are independently 175-185°C, the temperature of zone 11 is 170-175°C, the head temperature is 170-180°C, the screw aspect ratio adopted for twin-screw melt extrusion is 42:1-52:1, and the screw speed is 200-400rpm.

[0045] In some preferred embodiments, the homogenization treatment time is 2 to 4 hours.

[0046] In some more specific embodiments, the preparation method of the grafted compatibilizer (EIA-g-PP) comprises the following steps:

[0047] a. The polypropylene, initiator and diglycidyl itaconate are mixed and added to the main feed hopper of the twin-screw extruder for melt blending and dynamic grafting reaction extrusion;

[0048] b. The extruded material is water-cooled or air-cooled, and cut into particles of uniform size by a pelletizer, and finally homogenized for 2-4 hours.

[0049] The main raw materials for preparing diglycidyl itaconate in the present invention are of bio-based origin, the reaction process does not require any organic solvent, the reaction by-products are few, the prepared diglycidyl itaconate has high purity and a higher epoxy value, and it is easier to prepare a grafted compatibilizer with a higher epoxy value and grafting rate, and has a more excellent compatibility effect.

[0050] The epoxy value of diglycidyl itaconate in the present invention is much higher than that of GMA, and it is used as a grafting monomer to prepare a two-phase compatibilizer. The prepared compatibilizer has a higher epoxy value and grafting rate, and has better bonding and compatibility effects.

[0051] The technical solution of the present invention is further described in detail below in conjunction with several preferred embodiments and drawings. This embodiment is implemented on the premise of the technical solution of the invention, and a detailed implementation method and specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.

[0052] Unless otherwise specified, the experimental materials used in the following examples can be purchased from conventional biochemical reagent companies.

[0053] Example 1

[0054] Bio-based itaconate diglycidyl ester was synthesized according to the following method: 100 parts by mass of itaconic acid was reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1) to prepare sodium itaconate, 100 parts by mass of sodium itaconate, 600 parts by mass of epichlorohydrin, 1 part of benzyltriethylammonium chloride (TEBAC) and 0.2 parts of p-benzoquinone were mixed evenly, and then heated to 100°C under inert gas protection after vigorous stirring at room temperature for 5 minutes and reacted for 3 hours; then cooled to room temperature, the obtained components were washed with water, and distilled under reduced pressure at 60°C to obtain bio-based itaconate diglycidyl ester. The synthesized EIA had an epoxy value of 0.813 and a yield of 83.4%.

[0055] Example 2

[0056] Bio-based diglycidyl itaconate was synthesized according to the following method: 100 parts by mass of itaconic acid were reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1), 100 parts of sodium itaconate, 800 parts of epichlorohydrin, 4 parts of tetrabutylammonium bromide (TBAB) and 0.5 parts of methylhydroquinone were evenly mixed, and then under the protection of inert gas, the mixture was vigorously stirred at room temperature for 30 minutes and then heated to 115°C and reacted for 2 hours; then the mixture was cooled to room temperature and the obtained components were washed with water, and bio-based diglycidyl itaconate was obtained after reduced pressure distillation at 90°C. The synthesized EIA had an epoxide value of 0.825 and a yield of 84.1%.

[0057] The nuclear magnetic resonance hydrogen spectrum of the bio-based diglycidyl itaconate prepared in this example is as follows: Figure 1In 1H NMR, the characteristic chemical shifts are at 2.5-2.85ppm, 3.2-3.3ppm, 3.9-4.2ppm, 4.4-4.6ppm, 5.8ppm and 6.4ppm, combined with the highest epoxy value of 0.825, reaching 99.87% of the theoretical epoxy value (0.826) of diglycidyl itaconate, which shows that bio-based diglycidyl itaconate is successfully prepared by the non-solvent method.

[0058] Example 3

[0059] Bio-based itaconic acid diglycidyl ester was synthesized according to the following method: 100 parts by mass of itaconic acid was reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1), 100 parts of sodium itaconate, 1000 parts of epichlorohydrin, 6 parts of tetrabutylammonium chloride (TBAC) and 1 part of p-hydroxyanisole were uniformly mixed, and then the mixture was vigorously stirred at room temperature for 20 minutes under the protection of inert gas, and then the temperature was raised to 140°C and reacted for 1 hour; then the temperature was cooled to room temperature, the obtained components were washed with water, and bio-based itaconic acid diglycidyl ester was obtained after reduced pressure distillation at 110°C. The synthesized EIA had an epoxy value of 0.816 and a yield of 90.3%.

[0060] Example 4

[0061] Bio-based itaconic acid diglycidyl ester was synthesized according to the following method: 100 parts by mass of itaconic acid was reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1), 100 parts of sodium itaconate, 800 parts of epichlorohydrin, 3 parts of tetrabutylammonium hydrogen sulfate (THS) and 0.4 parts of 2-tert-butylhydroquinone (TBHQ) were uniformly mixed, and then the mixture was vigorously stirred at room temperature for 15 minutes under the protection of inert gas, and then the temperature was raised to 110°C and reacted for 2 hours; then the temperature was cooled to room temperature, the obtained components were washed with water, and bio-based itaconic acid diglycidyl ester was obtained after reduced pressure distillation at 90°C. The synthesized EIA had an epoxy value of 0.817 and a yield of 79.2%.

[0062] Example 5

[0063] Bio-based itaconic acid diglycidyl ester was synthesized according to the following method: 100 parts by mass of itaconic acid was reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1), 100 parts of sodium itaconate, 800 parts of epichlorohydrin, 4 parts of trioctylmethylammonium chloride (Aliquat 336) and 0.4 parts of 2,5-di-tert-butylhydroquinone (DTBHQ) were uniformly mixed, and then the mixture was stirred vigorously at room temperature for 15 minutes under the protection of inert gas, and then the temperature was raised to 110°C and reacted for 2 hours; then the temperature was cooled to room temperature, the obtained components were washed with water, and bio-based itaconic acid diglycidyl ester was obtained after reduced pressure distillation at 90°C. The synthesized EIA had an epoxy value of 0.820 and a yield of 75.3%.

[0064] Example 6

[0065] Bio-based itaconate diglycidyl ester was synthesized according to the following method: 100 parts by mass of itaconic acid was reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1), 100 parts of sodium itaconate, 800 parts of epichlorohydrin, 6 parts of dodecyltrimethylammonium chloride (DTAC) and 0.4 parts of p-hydroxyanisole were mixed evenly, and then the mixture was stirred vigorously at room temperature for 15 minutes under the protection of inert gas, and then the temperature was raised to 110°C and reacted for 1 hour; then the temperature was cooled to room temperature, the obtained components were washed with water, and bio-based itaconate diglycidyl ester was obtained after reduced pressure distillation at 90°C. The synthesized EIA had an epoxy value of 0.823 and a yield of 73.2%.

[0066] Example 7

[0067] Bio-based itaconic acid diglycidyl ester was synthesized according to the following method: 100 parts by mass of itaconic acid was reacted with sodium hydroxide at room temperature (the molar ratio of carboxylate to sodium atom was 1:1), 100 parts of sodium itaconate, 800 parts of epichlorohydrin, 6 parts of tetradecyltrimethylammonium chloride (TTAC) and 0.4 parts of 2-tert-butylhydroquinone (TBHQ) were uniformly mixed, and then the mixture was vigorously stirred at room temperature for 15 minutes under the protection of inert gas, and then the temperature was raised to 120°C and reacted for 1 hour; then the temperature was cooled to room temperature, the obtained components were washed with water, and bio-based itaconic acid diglycidyl ester was obtained after reduced pressure distillation at 100°C. The synthesized EIA had an epoxy value of 0.819 and a yield of 84.1%.

[0068] The raw materials, process parameters and performances used in Examples 1-7 are shown in Table 1:

[0069] Table 1

[0070]

[0071]

[0072] The application examples listed use the same extrusion process parameters for grafting reaction: the process parameters adopted by the twin-screw extruder include: zone one temperature is 150°C, zone two temperature is 170°C, zone three temperature is 175°C, zone four to seven temperature is 180°C, zone eight to ten temperature is 185°C, zone eleven temperature is 175°C, die temperature is 180°C, twin-screw melt extrusion uses a screw length-to-diameter ratio of 52:1, and a screw speed of 300rpm.

[0073] Application Example 1

[0074] The following mass parts: 100 parts of polypropylene, 0.2 parts of diisopropylbenzene peroxide, and 1 part of EIA were uniformly mixed and added to the main feeding hopper of a twin-screw extruder for melt blending and dynamic grafting reaction extrusion. The measured epoxy value after purification was 0.48, and the effective grafting rate after purification was 0.581%.

[0075] Application Example 2

[0076] According to the following mass proportions: 100 parts of polypropylene, 0.4 parts of di-tert-butyl peroxide, and 3 parts of EIA were uniformly mixed and added to the main feeding hopper of a twin-screw extruder for melt blending and dynamic grafting reaction extrusion. The measured epoxy value after purification was 0.99, and the effective grafting rate after purification was 1.198%.

[0077] Application Example 3

[0078] According to the following mass parts: 100 parts of polypropylene, 0.6 parts of 1,4-di-tert-butylperoxyisopropylbenzene, and 5 parts of EIA were uniformly mixed and added to the main feeding hopper of a twin-screw extruder for melt blending and dynamic grafting reaction extrusion. The measured epoxy value after purification was 1.16, and the effective grafting rate after purification was 1.404%.

[0079] Application Example 4

[0080] According to the following mass parts: 100 parts of polypropylene, 1 part of tert-butyl peracetate, and 10 parts of EIA were uniformly mixed and added to the main feeding hopper of a twin-screw extruder for melt blending and dynamic grafting reaction extrusion. The measured epoxy value after purification was 1.91, and the effective grafting rate after purification was 2.311%.

[0081] Application Comparative Example 1

[0082] According to the following mass proportions: 100 parts of polypropylene, 0.4 parts of di-tert-butyl peroxide, and 3 parts of GMA were uniformly mixed and added to the main feeding hopper of a twin-screw extruder for melt blending and dynamic grafting reaction extrusion. The measured epoxy value after purification was 0.495, and the effective grafting rate after purification was 0.703%.

[0083] By comparing Application Example 2 with Application Comparative Example 1, it can be found that the epoxy value of bio-based diglycidyl itaconate synthesized by the present invention grafted with polypropylene is nearly twice as high as that of GMA grafted with polypropylene under the same conditions, and the grafting rate is more than 50% higher, which proves that EIA, as a grafting monomer, has better grafting performance and higher epoxy value.

[0084] In addition, the inventors of this case also referred to the aforementioned embodiments and conducted experiments with other raw materials, process operations, and process conditions described in this specification, and obtained relatively ideal results.

[0085] It should be understood that the technical solution of the present invention is not limited to the above-mentioned specific implementation cases. Any technical deformation made according to the technical solution of the present invention without departing from the scope of protection of the purpose of the present invention and the claims shall fall within the protection scope of the present invention.

Claims

1. A method for preparing bio-based diglycidyl itaconate, characterized in that: include: Allowing itaconic acid to react with sodium source at room temperature to obtain sodium itaconate; And, a mixed reaction system containing at least the sodium itaconate, epichlorohydrin, a catalyst, and an anti-self-polymerization agent is subjected to a second reaction to obtain bio-based diglycidyl itaconate.

2. The preparation method according to claim 1, characterized in that: The sodium source includes any one or more combinations of sodium hydroxide, sodium carbonate, and sodium bicarbonate; And / or, the molar ratio of carboxylate in the itaconic acid to sodium atoms in the sodium source is 1:

1.

3. The preparation method according to claim 1, characterized in that: Specifically include: The sodium itaconate, epichlorohydrin, catalyst and anti-self-polymerization agent are mixed uniformly, and then stirred at room temperature for 5-30 minutes in an inert gas, and then heated to 80-120° C. for a second reaction for 1-3 hours; And, after the second reaction is completed, the obtained product is washed with water and distilled under reduced pressure at 60-110° C. to obtain bio-based diglycidyl itaconate.

4. The preparation method according to claim 1, characterized in that: The mass ratio of the sodium itaconate, epichlorohydrin, catalyst and anti-self-polymerization agent is 100:600-1000:1-6:0.2-1.

5. The preparation method according to claim 1, characterized in that: The catalyst includes any one or more combinations of benzyltriethylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium chloride, tetrabutylammonium hydrogen sulfate, trioctylmethylammonium chloride, dodecyltrimethylammonium chloride, and tetradecyltrimethylammonium chloride; And / or, the anti-self-polymerization agent includes any one or more combinations of p-benzoquinone, methylhydroquinone, p-hydroxyanisole, 2-tert-butylhydroquinone, and 2,5-di-tert-butylhydroquinone.

6. Use of bio-based diglycidyl itaconate prepared by the preparation method according to any one of claims 1 to 5 in the preparation of grafting compatibilizers.

7. A grafting compatibilizer, characterized in that: The raw materials for preparing the grafting compatibilizer include the following components calculated by weight: 100 parts of polypropylene, 0.2-1 parts of initiator and 1-10 parts of diglycidyl itaconate; Wherein, the diglycidyl itaconate is prepared by the preparation method described in any one of claims 1 to 5.

8. The grafting compatibilizer according to claim 7, characterized in that: The polypropylene includes any one or more combinations of homopolymer PP, random copolymer PP, and block copolymer PP; And / or, the initiator includes any one or more combinations of dicumyl peroxide, di-tert-butyl peroxide, 1,4-di-tert-butylperoxycumene, and tert-butyl peroxyacetate.

9. The method for preparing a grafted compatibilizer according to claim 7 or 8, characterized in that: include: The polypropylene, initiator and diglycidyl itaconate are uniformly mixed, and then the obtained materials are input into a twin-screw extruder for melt blending, dynamic grafting reaction extrusion, pelletizing and homogenization to obtain a grafted compatibilizer.

10. The preparation method according to claim 9, characterized in that: The process parameters adopted by the twin-screw extruder include: the temperature of zone 1 is 140-160°C, the temperature of zone 2 is 165-175°C, the temperature of zone 3 is 175-180°C, the temperatures of zones 4 to 7 are independently 180-185°C, the temperatures of zones 8 to 10 are independently 175-185°C, the temperature of zone 11 is 170-175°C, the head temperature is 170-180°C, the screw length-diameter ratio adopted by the twin-screw melt extrusion is 42:1-52:1, and the screw speed is 200-400rpm; And / or, the homogenization treatment time is 2 to 4 hours.

Citation Information

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